Title of Invention

TIN-DOPED INDIUM OXIDE MICROPARTICLE DISPERSION, PROCESS FOR PRODUCING THE SAME, INTERLAYER FOR LAMINATED GLASS HAVING HEAT-RAY BLOCKING PROPERTY PRODUCED WITH THE DISPERSION, AND LAMINATED GLASS

Abstract A dispersion of tin-doped indium oxide fine particles has tin-doped indium oxide fine particles, a plasticizer for an interlayer film, an organic solvent containing alcohols as a main component, and a dispersion stabilizer, wherein under measuring conditions of a concentration of tin-doped indium oxide fine particles of 0.7% by weight and an optical path length of a glass cell of 1 mm, a visible light transmittance is 80% or more, a solar radiation transmittance at a wavelength within a range from 300 nm to 2100 nm is 3/4 or less of the visible light transmittance, a haze value is 1.0% or less, and a reflection yellow index is -20 or more.
Full Text DESCRIPTION
TIN-DOPED INDIUM OXIDE MICROPARTICLE DISPERSIOM, PROCESS FOR
PRODUCING THE SAME, INTERLAYE1 FOR LAMINATED GLASS HAVING HEAT-RAY
BLOCKIIG PROPERTY PRODUCED WITH THE DISPERSION, AND LAMINATED GLASS

TECHNICAL FIELD
The present invention relates to a dispersion of tin-
doped indium oxide fine particles, which can be used in the
manufacture of an interlayer film for laminated glass, to a
method for manufacturing the dispersion, to an interlayer
film for laminated glass with heat ray shield properties,
and a laminated glass therewith.
This application claims priority on Japanese Patent
Application No. 2003-427446 filed on December 24, 2003, the
contents of which are incorporated herein by reference.
BACKGROUND ART
In general, a laminated glass has a structure
obtained by interposing an interlayer film for laminated
glass (hereinafter also referred to simply as an interlayer
film) including a polyvinyl acetal resin such as polyvinyl
butyral resin plasticized by a plasticizer between at least
a pair of glass sheets, and integrating them. The laminated
glass having such a structure is excellent in safety
because fragments of glass hardly scatter when broken by an

exterior impact, and therefore it is widely used as a
window glass for vehicles such as automobiles and aircrafts,
and for buildings.
However, such a laminated glass including an
interlayer film was excellent in safety, but was inferior
in heat shield properties. In general, infrared radiation
having a wavelength of 780 nm or more, which is longer than
that of visible light, is referred to as heat ray because,
inspite of its small energy amount such as about 10% as
compared with ultraviolet radiation, it has a large thermal
action and is released as heat to cause temperature rise
when absorbed by a substance. A laminated glass capable of
effectively shielding this heat ray has been required. When
it becomes possible to shield infrared radiations having a
large thermal action among light rays incident upon
automotive front and side glasses, heat shield properties
are enhanced and thus temperature rise in the automobile
can be suppressed. Since the area of the automotive glass
portion tends to increase, recently, it has become
necessary to enhance heat shield properties of the
laminated glass, thereby imparting a heat ray shield
function to the glass opening portion.
As the laminated glass having enhanced heat shield
properties, for example, there has been known a laminated
glass including an interlayer film having a transparent
resin mixed with a plasticizer containing tin-doped indium

oxide fine particles (hereinafter also referred to as ITO
fine particles) to a transparent resin (see Patent Document
1: Japanese Patent No. 3,040,681). This publication
discloses, as the interlayer film for laminated glass, an
interlayer film obtained by mixing ITO fine particles
having a particle size limited to 0.1 urn or less so as not
to impair transparency, an anionic surfactant and phthalic
acid di-2-ethylhexyl as a plasticizer to prepare a
dispersion of ITO fine particles containing ITO fine
particles dispersed therein, kneading the dispersion with a
polyvinyl butyral resin, and forming the kneaded mixture
into a film.
As an interlayer film composition for laminated glass
having heat shield properties, there has been known a
composition obtained by mixing a dispersion containing ITO
fine particles, a higher fatty acid ester, and a
plasticizer with a resin (see Patent Document 2: Japanese
Patent Application, First Publication No. 2001-233643) . In
the case of this interlayer film composition, the higher
fatty acid ester such as polyglycerin fatty acid ester is
added so as to enhance dispersibility of ITO fine particles,
However, a conventional interlayer film for laminated
glass composition, or a dispersion of ITO fine particles
used for the interlayer film composition may be inferior in
transparency because clouding occurs at a certain angle,
inspite of the same haze value as an indicator of

transparency. Also, there is a problem in that, when using
a conventional dispersant in the case of dispersing ITO
fine particles in the plasticizer, it becomes difficult to
control the degree of adhesion at the interface between the
glass and the interlayer film of the laminated glass. Also,
there is a problem in that it becomes difficult to control
a variation in the degree of adhesion between the glass and
the interlayer film due to a change in moisture of the
interlayer film. Furthermore, there is a problem in that,
when the dispersion of ITO fine particles is diluted with a
plasticizer for an interlayer film, ITO fine particles are
converted into agglomerated particles due to poor
dispersion, that is, so-called solvent shock phenomenon
arises and thus transparency is lowered.
There have been known a composition obtained by
adding triethylene glycol di-2-hexanoate (3G0) as a
plasticizer to a solution containing ITO fine particles
dispersed in polyphosphate ester and acetylacetone (see
Patent Document 3: Japanese Patent Application, First
Publication No. 2002-293583) and a composition obtained by
further mixing the composition with 2-ethylhexanoic acid
(see Patent Document 4: Japanese Patent Application, First
Publication No. 2001-302289). However, all of these
compositions have a drawback in that they are free of
alcohols and have high hydrophobicity, and thus ITO fine
particles are inferior in affinity with the solution and

solvent shock may arise. Also, there is a drawback in that
dispersion proprety drastically vary depending on the kind
of the plasticizer for the interlayer film.
The present invention has been made so as to solve
the above problems of the prior art with respect to a
dispersion of ITO fine particles having heat ray shield
properties, and an interlayer film including the dispersion.
The present invention provides a dispersion of ITO fine
particles having excellent transparency and heat shield
properties by adjusting the haze value to a fixed value or
less, and controlling a reflection value measured by a
goniophotometric measurement as an indicator and a
reflection yellow index (YI) having a correlation with the
measured reflection value as an indicator within a fixed
range, and also provides an interlayer film including the
dispersion of ITO fine particles, and a heat ray shield
laminated glass including the interlayer film.
Furthermore, the present invention provides a
dispersion of ITO fine particles which easily adjusts the
degree of adhesion due to a combination of dispersion
stabilizers, which is excellent in dispersibility of ITO
fine particles, which easily suppresses a variation in the
degree of adhesion at the interface between the glass and
the interlayer film due to a change in moisture of the
interlayer film, and which is also less likely to cause
solvent shock, and also provides an interlayer film

including the dispersion of ITO fine particles, and a heat
ray shield laminated glass including the interlayer film.
DISCLOSURE OF THE INVENTION
The present invention relates to the following
dispersion of tin-doped indium oxide fine particles, and to
a method for manufacturing the same.
(1) A dispersion of tin-doped indium oxide fine
particles, the dispersion includes tin-doped indium oxide
fine particles, a plasticizer for an interlayer film, an
organic solvent containing alcohols as a main component,
and a dispersion stabilizer, wherein under measuring
conditions of the concentration of tin-doped indium oxide
fine particles of 0.7% by weight and an optical path length
of a glass cell of 1 mm, a visible light transmittance is
80% or more, a solar radiation transmittance at a
wavelength within a range from 300 nm to 2100 nm is 3/4 or
less of the visible light transmittance, a haze value is
1.0% or less, and a reflection yellow index is -20 or more.
In this case, there can be obtained a dispersion of
tin-doped indium oxide fine particles which is excellent in
dispersibility of tin-doped indium oxide fine particles and
has high transparency at a certain angle, and which is also
less likely to cause solvent shock and maintains good
dispersion state of tin-doped indium oxide fine particles
when the dispersion is mixed with the resin. This

dispersion of tin-doped indium oxide fine particles is
suited for the manufacture of an interlayer film for
laminated glass, and an interlayer film for laminated glass
with excellent heat ray shield properties and a laminated
glass including the same can be obtained by using the
dispersion.
(2) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein instead of the
reflection yellow index being -20 or more, or with the
reflection yellow index being -20 or more, under measuring
conditions of an optical path length of a glass cell of 1
mm, a reflection value measured at 0 degrees among
reflected light distribution at an incidence angle of 45
degrees measured by a goniophotometric measurement is 30 or
less.
(3) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein the plasticizer for an
interlayer film is at least one selected from the group
consisting of dihexyl adipate, triethylene glycol di-2-
ethylhexanoate, tetraethylene glycol di-2-ethylhexanoate,
triethylene glycol di-2-ethyl butyrate, tetraethylene
glycol di-2-ethyl butyrate, tetraethylene glycol di-
heptanoate, and triethylene glycol di-heptanoate.
(4) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein the alcohols include at
least one selected from the group consisting of methanol,

ethanol, propanol, isopropanol, n-butanol, isobutanol, sec-
butanol, tert-butanol, lauryl alcohol, diacetone alcohol,
cyclohexanol, ethylene glycol, diethylene glycol and
triethylene glycol.
(5) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein the dispersion
stabilizer is a compound having at least one atom selected
from the group consisting of nitrogen, phosphorus, and
chalcogen atoms.
(6) The dispersion of tin-doped indium oxide fine
particles according to (5), wherein the dispersion
stabilizer is at least one selected from the group
consisting of sulfate ester-based compound, phosphate
ester-based compound, ricinoleic acid, polyricinoleic acid,
polycarboxylic acid, polyhydric alcohol type surfactant,
polyvinyl alcohol, and polyvinyl butyral.
(7) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein the dispersion
stabilizer is at least one selected from the group
consisting of chelate, inorganic acid and organic acid.

(8) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein the dispersion of tin-
doped indium oxide fine particles contains, as the
dispersion stabilizer, three components of phosphate ester-
based compound, organic acid, and chelate.
(9) The dispersion of tin-doped indium oxide fine

particles according to (1), wherein a concentration of the
ITO fine particles is from 0.1 to 95% by weight, a content
of the plasticizer for an interlayer film is from 1 to
99.9% by weight, a content of the organic solvent
containing alcohols as a main component is from 0.02 to 25%
by weight, and a content of the dispersion stabilizer is
from 0.0025 to 30% by weight.
(10) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein the dispersion of tin-
doped indium oxide fine particles is obtained by diluting a
dispersion of tin-doped indium oxide fine particles which
contains tin-doped indium oxide fine particles, a
plasticizer for an interlayer film, an organic solvent
containing alcohols as a main component, and a dispersion
stabilizer, and in which a concentration of the tin-doped
indium oxide fine particles is from 0.1 to 95% by weight,
with a plasticizer for an interlayer film, or a plasticizer
for an interlayer film containing an organic solvent
containing alcohols as a main component and/or a dispersion
stabilizer.
(11) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein, when a concentration
of the tin-doped indium oxide fine particles is adjusted to
10.0% by weight by diluting a dispersion of tin-doped
indium oxide fine particles having the concentration of the
tin-doped indium oxide fine particles of 10.0% by weight or

more, or when a concentration of the tin-doped indium oxide
fine particles is adjusted to 40.0% by weight by diluting a
dispersion of tin-doped indium oxide fine particles having
the concentration of the tin-doped indium oxide fine
particles of 40.0% by weight or more, a mean volume
particle size of the tin-doped indium oxide fine particles
is 80 nm or less, and a particle size at 90% accumulation
(D90) is 160 nm or less.
(12) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein a primary average
particle size of the tin-doped indium oxide fine particles
is 0.2 urn or less.
(13) The dispersion of tin-doped indium oxide fine
particles according to (1), wherein a lattice constant of a
tin-doped indium oxide fine particle crystal is from 10.11
to 10.16 A.
(14) A method for manufacturing the dispersion of
tin-doped indium oxide fine particles of any one of (1) to
(13), includes mixing an organic solvent containing
alcohols as a main component, a dispersion stabilizer, tin-
doped indium oxide fine particles and plasticizer for an
interlayer film, thereby dispersing the tin-doped indium
oxide fine particles.
(15) The method for manufacturing a dispersion of
tin-doped indium oxide fine particles according to (14),
wherein a mixed solution containing the organic solvent

containing the alcohols as a main component, the dispersion
stabilizer, and the tin-doped indium oxide fine particles
is prepared, and this mixed solution is mixed with the
plasticizer for an interlayer film to obtain a dispersion
of tin-doped indium oxide fine particles.
(16) The method for manufacturing a dispersion of
tin-doped indium oxide fine particles according to (15),
wherein the mixed solution containing the organic solvent
containing the alcohols as a main component, the dispersion
stabilizer, and the tin-doped indium oxide fine particles
is prepared, and this mixed solution is added to the
plasticizer for an interlayer film, or the plasticizer for
an interlayer film is added to this mixed solution, thereby
dispersing the tin-doped indium oxide fine particles.
(17) The method for manufacturing a dispersion of
tin-doped indium oxide fine particles according to (15),
wherein a plasticizer containing an organic solvent
containing alcohols as a main component or a dispersion
stabilizer is used as the plasticizer for an interlayer
film.
Also, the present invention relates to the following
interlayer film for laminated glass with heat ray shield
properties, and to a laminated glass therewith
(18) An interlayer film for heat shield laminated
glass, is formed by using a resin composition of a mixture
of the dispersion of tin-doped indium oxide fine particles

of any one of (1) to (13) and a resin, wherein, under the
measuring conditions in which the interlayer film having a
thickness of 0.76 mm is interposed between clear glass
sheets having a thickness of 2.5 mm, electromagnetic wave
shield properties at a frequency of 0.1 MHz to 26.5 GHz is
lOdB or less, a haze value is 1.0% or less, a visible light
transmittance is 70% or more, a solar radiation
transmittance at a wavelength within a range from 300 to
2100 nm is 80% or less of the visible light transmittance,
and a reflection yellow index is -12 or more.
(19) The interlayer film for laminated glass
according to (18), wherein instead of the reflection yellow
index being -12 or more or with the reflection yellow index
being -12 or more, a reflection value at 0 degrees among
reflected light distribution at an incidence angle of 45
degrees measured by a goniophotometric measurement is 25 or
less.
(20) The interlayer film for laminated glass
according to (18), wherein 20 to 60 parts by weight of the
plasticizer for an interlayer film and 0.1 to 3 parts by
weight of the tin-doped indium oxide fine particles based
on 100 parts by weight of a polyvinyl acetal resin are
contained.
(21) The interlayer film for laminated glass
according to (20), wherein the polyvinyl acetal resin is a
polyvinyl butyral resin,

(22) The interlayer film for laminated glass
according to (18), wherein the resin composition obtained
by mixing the dispersion of tin-doped indium oxide fine
particles with the resin further contains an alkali metal
salt and/or an alkali earth metal salt as an adhesion
adjustor.
(23) The interlayer film for laminated glass
according to (18), wherein the tin-doped indium oxide fine
particles have an average particle size of 80 nm or less
and are dispersed such that a number of particles having a
particle size of 100 nm or more is one per um2 or less.
(24) A laminated glass includes the interlayer film
for laminated glass of any one of (18) to (23)
(25) The laminated glass according to (24) wherein
the laminated glass has heat ray shield properties in which
electromagnetic wave shield performance at a frequency of
0.1 MHz to 26.5 GHz is 10 dB or less, a haze value is 1.0%
or less, a visible light transmittance is 70% or more, a
solar radiation transmittance at a wavelength within a
range from 300 to 2100 nm is 80% or less of the visible
light transmittance, and a reflection yellow index is -12
or more.
(26) The laminated glass according to (25), wherein
instead the reflection yellow index being -12 or more, or
with the reflection yellow index being -12 or more, a
reflection value at 0 degrees among reflected light

distribution at an incidence angle of 45 degrees measured
by a goniophotometric measurement is 25 or less.
The present invention will now be described in detail.
The dispersion of tin-doped indium oxide fine
particles of the present invention is a dispersion of tin-
doped indium oxide fine particles (hereinafter also
referred to as a dispersion of ITO fine particles)
including tin-doped indium oxide fine particles, a
plasticizer for an interlayer film, an organic solvent
containing alcohols as a main component (hereinafter also
referred to as an alcohol solvent), and a dispersion
stabilizer, wherein under measuring conditions of the
concentration of tin-doped indium oxide fine particles is
0.7% by weight and an optical path length of a glass cell
of 1 mm, a visible light transmittance is 80% or more, a
solar radiation transmittance at a wavelength within a
range from 300 to 2100 nm is 3/4 or less of the visible
light transmittance, a haze value is 1.0% or less, and a
reflection yellow index is -20 or more.
In the dispersion of ITO fine particles of the
present invention, instead of the reflection yellow index
being -20 or more, or with the reflection yellow index
being -20 or more, a reflection value at 0 degrees among
reflected light distribution at an incidence angle of 45
degrees measured by a goniophotometric measurement is 30 or
less.

The ITO fine particles preferably have a primary
average particle size of 0.2 um or less. In the case in
which the primary average particle size is more than 0.2 um,
the haze value of the resulting interlayer film, in its
turn, the haze value of the laminated glass becomes worse,
or clouding may be caused by scattering of visible light
due to ITO fine particles. The primary average particle
size is more preferably 0.1 um or less, and still more
preferably 0.08 um or less. In the ITO fine particles, a
lattice constant of its crystal is preferably in a range
from 10.11 to 10.16 A. In the case in which the lattice
constant is not within the above range, sufficient heat ray
shield effect may not be exerted.
The method for manufacturing the ITO fine particles
is not specifically limited. For example, there can be
exemplified a method for manufacturing ITO fine particles,
which includes reacting an aqueous solution containing a
water-soluble salt of indium chloride and a small amount of
tin chloride with an alkali, thereby coprecipitating a
hydroxide of indium and tin, and annealing the
coprecipitate as a material with heating in nitrogen free
of oxygen to convert the coprecipitate into an oxide.
In the dispersion of ITO fine particles of the
present invention, the plasticizer for an interlayer film
functions as a dispersion medium for dispersing the ITO
fine particles. This plasticizer for an interlayer film is

not specifically limited as long as it is conventionally
used for a polyvinyl acetal resin, and a known plasticizer
which is generally used as a plasticizer for an interlayer
film can be used. For example, there can be used organic
ester-based plasticizers such as monobasic acid ester and
polybasic acid ester; and phosphoric acid-based
plasticizers such as organic phosphoric acid-based and
organic phosphorous acid-based plasticizers.
Among the above organic ester-based plasticizers, the
monobasic acid ester includes, for example, glycol-based
esters obtained by reacting triethylene glycol with organic
acids such as butyric acid, isobutyric acid, caproic acid,
2-ethylbutyric acid, heptanoic acid, n-octylic acid, 2-
ethylhexylic acid, pelargonic acid (n-nonylic acid), and
decylic acid; and esters of tetraethylene glycol or
tripropylene glycol with the above organic acids. The
polybasic acid ester includes, for example, esters of
organic acids such as adipic acid, sebacic acid, and
azelaic acid with a linear or branched alcohol having 4 to
8 carbon atoms.
Specific examples of the organic ester-based
plasticizer include triethylene glycol di-2-ethyl butyrate,
triethylene glycol di-2-ethyl hexoate, triethylene glycol
dicapriate, triethylene glycol di-n-octoate, triethylene
glycol di-n-heptoate, tetraethylene glycol di-n-heptoate,
dibutyl sebacate, dioctyl azelate, dibutylcabitol adipate,

ethylene glycol di-2-ethyl butyrate, 1,3-propylene glycol
di-2-ethyl butyrate, 1,4-propylene glycol di-2-ethyl
butyrate, 1,4-butylene glycol di-2-ethyl butyrate, 1,2-
butylene glycol di-2-ethylene butyrate, diethylene glycol
di-2-ethyl butyrate, diethylene glycol di-2-ethyl hexoate,
dipropylene glycol di-2-ethyl butyrate, triethylene glycol
di-2-ethyl pentoate, tetraethylene glycol di-2-ethyl
butyrate, and diethylene glycol dicapriate.
Examples of the phosphoric acid-based plasticizer
include tributoxyethyl phosphate, isodecylphenyl phosphate,
and triisopropyl phosphite.
Among these plasticizers for interlayer film, at
least one selected from the group consisting of dihexyl
adipate (DHA), triethylene glycol di-2-ethylhexanoate (3G0),
tetraethylene glycol di-2-ethylhexanoate (4G0), triethylene
glycol di-2-ethyl butyrate (3GH), tetraethylene glycol di-
2-ethyl butyrate (4GH), tetraethylene glycol di-heptanoate
(4G7), and triethylene glycol di-heptanoate (3G7) is
preferable because the addition of a metal salt of a
carboxylic acid having 5 to 6 carbon atoms, as an adhesion
adjustor, makes it possible to prevent deterioration of
adhesion between the interlayer film and the glass and to
reconcile prevention of whitening and prevention of
deterioration of adhesion over time. Among these
plasticizers, triethylene glycol di-2-ethylhexanoate (3G0),
triethylene glycol di-2-ethyl butyrate (3GH), tetraethylene

glycol di-2-ethylhexanoate (4G0), and dihexyl adipate (DHA)
are particularly preferable because hydrolysis is less
likely to occur.
In the present invention, an organic solvent
containing alcohols as a main component is used. The
alcohols are not specifically limited. For example, at
least one selected from the group consisting of methanol,
ethanol, propanol, isopropanol, n-butanol, isobutanol, sec-
butanol, tert-butanol, lauryl alcohol, diacetone alcohol,
cyclohexanol, ethylene glycol, diethylene glycol, and
triethylene glycol is preferable. In the case in which the
organic solvent containing alcohols as a main component
(i.e., alcohol solvent) contains a small amount of
components other than alcohols, methyl ethyl ketone,
isopropyl acetate, ethyl lactate, 2-pyrrolidone, and ethyl
acetoacetate can be used as the component.
Since the organic solvent containing alcohols as a
main component is excellent in affinity with ITO fine
particles and is also excellent in compatibility with the
plasticizer for an interlayer film, the reflection value
measured by a goniophotometric measurement can be reduced
to 30 or less, and preferably 25 or less. Here, the
reflection value measured by a goniophotometric measurement
is a value obtained by subtracting a reference value which
is a measured value of a plasticizer filled in a glass cell
having an optical path length 1 mm with, from a raw data of

a dispersion of ITO fine particles measured at 0 degrees
among reflected light distribution at an incidence angle of
45 degrees. Furthermore, a reflection yellow index having a
correlation with the measured reflection value can be
increased to -20 or more. Also, effect of preventing
solvent shock is exerted. Furthermore, effect of
suppressing a variation in a dispersion property caused by
the kind of the plasticizer for an interlayer film is
exerted.
The dispersion stabilizer is preferably a compound
containing at least one atom selected from the group
consisting of nitrogen, phosphorus, and chalcogen atoms.
These atoms are excellent in affinity with ITO fine
particles and good dispersion effect can be exerted.
Examples of the compound include (I) anionic surfactants
such as carboxylic acid salt, sulfonic acid salt, sulfate
ester salt, phosphate ester salt, polymerization type
polymer, and polycondensation type polymer; (II) nonionic
surfactants such as ether, ester, ester ether, and
nitrogen-containing one; (III) cationic surfactants such as
primary amine salt or tertiary amine salt, quaternary
ammonium salt and polyethylenepolyamine derivative; and
(IV) amphoteric surfactants such as carboxybetaine,
aminocarboxylic acid salt, sulfobetaine, aminosulfate ester,
and imidazoline. Among these compounds, at least one
selected from sulfate ester-based compound, phosphate

ester-based compound, ricinoleic acid, polyricinoleic acid,
polycarboxylic acid, polyhydric alcohol type surfactant,
polyvinyl alcohol, and polyvinyl butyral is particularly
preferable.
Examples of the phosphate ester-based compound
include polyoxyethylene alkyl ether phosphoric acid ester,
alkyl ether phosphoric acid ester, and polyoxyethylene
alkyl phenyl ether phosphoric acid ester.
The dispersion stabilizer is preferably at least one
selected from the group consisting of chelate, inorganic
acid, and organic acid. The chelate is not specifically
limited, and for example, ethylenediaminetetraacetic acids
(EDTA) and (3-diketones can be used. Among these chelates,
(3-diketones are preferable because of excellent
compatibility with the plasticizer for an interlayer film
and the resin, and acetylacetone is particularly preferable.
As the (3-diketones, for example, benzoyltrifluoroacetone
and dipivaloylmethane may also be used. These chelates
prevent agglomeration of ITO fine particles and reduce the
reflection value measured by a goniophotometric measurement,
and also can enhance the reflection yellow index having a
correlation with the measured reflection value.
The inorganic acid is not specifically limited. For
example, hydrochloric acid and nitric acid can be used.
Also, the organic acid is not specifically limited. For
example, aliphatic carboxylic acid, aliphatic dicarboxylic

acid, aromatic carboxylic acid, and aromatic dicarboxylic
acid can be used. Specific examples thereof include benzoic
acid, phthalic acid, and salicylic acid. Among these, a C2-
C18 aliphatic carboxylic acid is preferable and a C2-C10
aliphatic carboxylic acid is more preferable. Examples of
the C2-C10 aliphatic carboxylic acid include acetic acid,
propionic acid, n-butyric acid, 2-ethylbutyric acid, n-
hexanoic acid, 2-ethylhexanoic acid, and n-octanoic acid.
These inorganic and organic acids prevent agglomeration of
ITO fine particles and reduce the reflection value measured
by a goniophotometric measurement, also can enhance the
reflection yellow index having a correlation with the
measured reflection value.
In the dispersion of ITO particles of the present
invention, in order to exhibit initial optical performances
by high dispersion of ITO fine particles, a combination of
the plasticizer for an interlayer film, which serves as a
dispersion medium, and a dispersion stabilizer is very
important. For example, in the case of using triethylene
glycol di-2-ethylhexanoate (3G0) as the plasticizer for an
interlayer film, when alcohols are used as the solvent and
three components of the above phosphate ester-based
compound, the organic acid such as 2-ethylhexanoic acid,
and the chelate such as acetylacetone are used in
combination as the dispersion stabilizer, ITO fine
particles can be dispersed with high concentration and high

dispersibility and the reflection value measured by a
goniophotometric measurement can be reduced, and also the
reflection yellow index having a correlation with the
measured reflection value can be enhanced. Furthermore,
solvent shock can be prevented in the case of diluting with
the plasticizer for an interlayer film. In this case,
alcohols are preferably methanol, ethanol, isopropanol and
diacetone alcohol.
There have been known compositions obtained by adding
3G0 as the plasticizer to a solution containing ITO fine
particles dispersed in polyphosphate ester and
acetylacetone and a composition obtained by further mixing
the composition with 2-ethylhexanoic acid. However, these
compositions have a drawback in that they are free of
alcohols and have high hydrophobicity, and thus ITO fine
particles are inferior in affinity with the solution and
solvent shock may arise. Also, the dispersion proprety
drastically vary depending on the kind of the plasticizer
for an interlayer film and it is hard to control the
dispersion proprety.
The dispersion system, in which three components of
the above phosphate ester-based compound, the organic acid
such as 2-ethylhexanoic acid, and the chelate such as
acetylacetone are used in combination, also has excellent
effect of easily controlling the degree of adhesion at the
interface between the interlayer film and the glass. In the

laminated glass, in the case in which the degree of
adhesion at the interface between the interlayer film and
the glass is too low, exfoliation occurs at the interface
between the glass and the interlayer film. On the other
hand, in the case in which the degree of adhesion is too
high, penetration resistance of the laminated glass is
lowered. Therefore, an advantage of easily controlling the
degree of adhesion at the interface between the interlayer
film and the glass is very useful. Also, there is an
advantage that a variation in the degree of adhesion at the
interface between the glass and the interlayer film caused
by a change in moisture of the interlayer film is easily
suppressed.
The dispersion stabilizer, other than the chelate,
the organic acid, and the inorganic acid, functions as a
surfactant for enhancing an interaction between an organic
interface and an inorganic interface, and therefore
enhances the degree of adhesion at the interface between
the interlayer film and the glass. As a result, it is hard
to properly control the degree of adhesion between the
glass and the interlayer film only by an adhesion adjustor
such as an alkali metal salt and/or an alkali earth metal
salt, and it is particularly hard to control the degree of
adhesion to be a low value. However, when the above three
components are used in combination, it is believed that
these components cordinate to the adhesion adjustor such as

the alkali metal salt and/or the alkali earth metal salt
which is for controlling the degree of adhesion at the
interface between the interlayer film and the glass,
thereby controllability of the adhesion adjustor is
enhanced. As a result, as described above, the degree of
adhesion can be controlled even under the conditions in
which the degree of adhesion at the interface between the
glass and the interlayer film is increased by the
dispersion stabilizer.
In the dispersion of ITO fine particles of the
present invention, when measured under the conditions in
which the concentration of ITO fine particles is 0.7% by
weight, and a glass cell having an optical path length of 1
mm is used, a visible light transmittance is 80% or more, a
solar radiation transmittance at a wavelength within a
range from 300 to 2100 nm is 3/4 or less of the visible
light transmittance, a haze value is 1.0% or less, and a
reflection yellow index is -20 or more. Alternatively, the
reflection value measured by a goniophotometric measurement
under the above measuring conditions is 30 or less.
Among these, each of the haze value, the reflection
yellow index, and the reflection value measured by a
goniophotometric measurement reflects the dispersion state
of ITO fine particles in the dispersion of ITO fine
particles. The relation between the visible light
transmittance and the solar radiation transmittance

reflects heat shield properties of the ITO fine particles
themselves. The visible light transmittance and the solar
radiation transmittance can be measured by the method
defined in Japanese Industrial Standard (JIS R 3106). The
haze value can be measured by the method defined in
Japanese Industrial Standard (JIS K 7105).
In the dispersion of ITO fine particles of the
present invention, in the case in which the visible light
transmittance is less than 80%, the resulting interlayer
film, in its turn, the laminated glass may have low visible
light transmittance. In the case in which the solar
radiation transmittance at a wavelength within a range from
300 to 2100 nm is more than 3/4 of the visible light
transmittance, the resulting interlayer film, in its turn,
the laminated glass may be inferior in heat shield
properties.
In the dispersion of ITO fine particles of the
present invention, the reflection yellow index is -20 or
more. The reflection yellow index can be calculated by the
following equation defined in Japanese Industrial Standard
(JIS K 7103). In the equation, X, Y and Z denote tristimus
values due to the measurement of reflection of test samples
in standard illuminant C.
Reflection yellow index = 100(1.28X - 1.06Z)/Y
As a result of secondary agglomeration of ITO fine
particles, scattering of visible light in a short

wavelength range occurs and clouding of the dispersion
system is induced under a light source. The reason is
believed to be as follows: when the ITO fine particles
causes secondary agglomeration, the particle size increases,
thereby causing scattering of visible light in a short
wavelength range. In proportion to a large number of
agglomerates, the reflectance of visible light in a short
wavelength range becomes higher and clouding increases.
Here, it is believed that the reflectance (Z) of visible
light in a short wavelength range of the dispersion of ITO
fine particles and the interlayer film containing ITO fine
particles is proportional to clouding of the ITO fine
particles in the dispersion system. That is, it is believed
that the reflectance (Z) of visible light in a short
wavelength range is proportional to the degree of secondary
agglomeration of the ITO fine particles, and in the case in
which the dispersibility is poor, the reflectance (Z) of
visible light in a short wavelength range becomes higher.
In the case of the same ITO concentration, absorption of
visible light in a medium wavelength range is almost the
same as that of visible light in a long wavelength range,
and thus X and Y are almost the same. Therefore, in the
case of the same ITO concentration, as the reflectance (Z)
of visible light in a short wavelength range becomes higher,
the value of the reflection yellow index decreases and
clouding increases. Therefore, the use of the reflection

yellow index (YI) as an indicator makes it possible to
grasp dispersibility of the ITO fine particles and to grasp
transparency of the dispersion of ITO fine particles and
the interlayer film containing ITO fine particles. In the
case of ITO fine particles having different concentrations,
since the values of X and Y change and the level of the
reflection yellow index increases, a relative comparison
cannot be made simply.
In the case in which the haze value of the dispersion
of ITO fine particles is more than 1.0% or the reflection
yellow index is less than -20, the ITO fine particles are
not sufficiently dispersed and the resulting interlayer
film, in its turn, the laminated glass has poor haze value
and poor reflection yellow index. In the case in which the
reflection value measured by a goniophotometric measurement
is more than 30, clouding occurs at a certain angle,
resulting in poor transparency.
In the dispersion of ITO fine particles of the
present invention, as long as the visible light
transmittance (Tv), the solar radiation transmittance (Ts),
the haze value, the reflection yellow index, and the
reflectance as determined by a goniophotometer are within
the above range, the concentration of the ITO fine
particles is not specifically limited. The dispersion may
contain a plasticizer for an interlayer film, an organic
solvent containing alcohols as a main component and a

dispersion stabilizer, and each content is not specifically
limited.
The lower limit of the concentration of ITO fine
particles is preferably 0.1% by weight and the upper limit
is preferably 95.0% by weight. In the case in which the
concentration of the ITO fine particles is not within the
above range, it may become difficult to uniformly disperse
the ITO fine particles. The lower limit of the
concentration of ITO fine particles is more preferably 10%
by weight and the upper limit is more preferably 60% by
weight.
The content of the plasticizer for an interlayer film
is preferably from about 1 to 99.9% by weight, the content
of the organic solvent containing alcohols as a main
component is preferably from about 0.02 to 25% by weight,
and the content of the dispersion stabilizer is preferably
from about 0.0025 to 30% by weight. The concentration of
the ITO fine particles is more preferably from about 10 to
60% by weight, the content of the plasticizer for an
interlayer film is more preferably from about 10 to 85% by
weight, the content of the organic solvent containing
alcohols as a main component is more preferably from about
0.5 to 10% by weight, and the content of the dispersion
stabilizer is more preferably from about 0.02 to 20% by
weight.
In the dispersion of ITO fine particles of the

present invention, when the dispersion of ITO fine
particles having an ITO fine particles of 10.0 to 95.0% by
weight is allowed to stand for a long period, or diluted
with the plasticizer for an interlayer film so as to adjust
the concentration of the ITO fine particles to 40.0% by
weight, the mean volume particle size of the ITO fine
particles is preferably 80 nm or less and the particle size
at 90% accumulation (D90) is preferably 160 nm or less. In
the case in which the mean volume particle size is more
than 80 nm or D90 is more than 160 nm, when mixing with the
resin to manufacture an interlayer film, the average
particle of the ITO fine particles in the interlayer film
may increase, resulting in poor transparency. In the
dispersion of ITO fine particles of the present invention,
even when the concentration of the ITO fine particles is
decreased to 10.0% by weight by dilution, the mean volume
particle size of the ITO fine particles is more preferably
80 nm or less and D90 is more preferably 160 nm or less.
Even if the dispersion of ITO fine particles is partially
or entirely solidified, fluidity is recovered by vigorous
stirring or shaking, and the mean volume particle size
becomes 80 nm or less and the particle size at 90%
accumulation (D90) becomes 160 nm or less.
The method for manufacturing the dispersion of ITO
fine particles of the present invention is not specifically
limited, but is preferably a method for mixing the organic

solvent containing alcohol as a main component (i.e.
alcohol solvent), the dispersion stabilizer, the ITO fine
particles, and the plasticizer for an interlayer film, and
dispersing the ITO fine particles. The present invention
includes this method for manufacturing the dispersion of
ITO fine particles.
In the method for manufacturing the dispersion of ITO
fine particles of the present invention, as a specific
aspect of mixing the alcohol solvent, the dispersion
stabilizer, the ITO fine particles, and the plasticizer for
an interlayer film, these components may be simultaneously
mixed, or a mixed solution containing the alcohol solvent,
the dispersion stabilizer, and the tin-doped indium oxide
fine particles may be previously prepared and the mixed
solution may be added to the plasticizer for an interlayer
film, thereby dispersing the tin-doped indium oxide fine
particles in the plasticizer for an interlayer film, or the
tin-doped indium oxide fine particles may be dispersed in
the plasticizer for an interlayer film by adding the
plasticizer for an interlayer film to the mixed solution.
As the plasticizer for an interlayer film, a plasticizer
containing an alcohol solvent and/or a dispersion
stabilizer may be used. The composition ratio of the
dispersion may be adjusted by evaporation until the
concentration of the organic solvent containing alcohols as
a main component reaches a predetermined concentration.

In the dispersion of ITO fine particles of the
present invention, a mixed solution containing a high
concentration of ITO fine particles dispersed therein may-
be previously prepared and the mixed solution may be
diluted with the plasticizer for an interlayer film, or a
plasticizer for an interlayer film containing the alcohol
solvent and the dispersion stabilizer until the
concentration of the ITO fine particles reach a
predetermined concentration. In the dispersion of ITO fine
particles of the present invention, such a dilution process
makes it possible to obtain a dispersion of ITO fine
particles free of solvent shock, wherein the mean volume
particle size of ITO fine particles is 80 nm or less, and
the particle size at 90% accumulation (D90) is 160 nm or
less, by appropriately selecting the plasticizer for an
interlayer film, the alcohol solvent, and the dispersion
stabilizer.
In the method for manufacturing the dispersion of ITO
fine particles of the present invention, an apparatus used
for mixing and dispersion is not specifically limited. For
example, extruder, plastograph, ball mill, beads mill, sand
grinder, kneader, Banbury mixer, and calendering roll can
be used.
By using a resin composition obtained by mixing the
dispersion of ITO fine particles of the present invention
with the resin, an interlayer film for laminated glass with

heat ray shield properties can be manufactured. This
laminated glass can have excellent optical characteristics
and excellent heat shield properties because the ITO fine
particles are highly dispersed.
In the interlayer film, the ITO fine particles are
preferably dispersed such that the average particle size is
80 nm or less. In the case in which the average particle
size is more than 80 nm, severe scattering of visible light
due to the ITO fine particles occurs and the resulting
interlayer film may be inferior in transparency. As a
result, the haze value becomes worse when the laminated
glass is assembled and thus it becomes impossible to obtain
high transparency required to a front glass of automobiles.
In the interlayer film, the ITO fine particles are
preferably dispersed such that the number of particles
having a particle size of 100 nm or more is one per urn2 or
less. That is, the ITO fine particles are commonly
dispersed such that, when a heat ray shield interlayer film
for laminated glass is photographed and observed by a
transmission electron microscope, ITO fine particles having
a particle size of 100 nm or more are not found or, if any,
the number of ITO fine particles having a particle size of
100 nm or more is only one per urn2. When a laminated glass
is manufactured by using the interlayer film in such a
dispersion state, the resulting laminated glass has low
haze value and is excellent in transparency and heat shield

properties. The observation is conducted using a
transmission electron microscope (Model H-7100FA,
manufactured by Hitachi, Ltd.) at an acceleration voltage
of 100 kV.
The resin to be mixed with the dispersion of ITO fine
particles of the present invention is not specifically
limited. For example, it may be a known resin which is
generally used as a transparent resin of the interlayer
film for laminated glass. Specific examples of the resin
include polyvinyl acetal resin, polyurethane resin,
ethylene-vinyl acetate resin, acrylic copolymer resin
including, as a constituent unit, acrylic acid or
methacrylic acid, or derivatives thereof, and vinyl
chloride-ethylene-glycidyl methacrylate copolymer resin.
Among these resins, polyvinyl acetal resin is preferable.
These resins can be easily manufactured by a known method
or a method analogous to the known method.
The polyvinyl acetal resin is not specifically
limited as long as it is a polyvinyl acetal resin obtained
by acetalizing polyvinyl alcohol with aldehyde, and is
particularly preferably polyvinyl butyral. The polyvinyl
alcohol is usually obtained by saponifying vinyl
polyacetate, and polyvinyl alcohol having a saponification
degree of 80 to 99.8 mol% is generally used.
A molecular weight and a molecular weight
distribution of the polyvinyl acetal resin are not

specifically limited. In view of formability and physical
properties, the lower limit of the polymerization degree of
the polyvinyl alcohol resin as a material is preferably 200
and the upper limit is preferably 3000. In the case in
which the polymerization degree is less than 200, the
resulting laminated glass may be inferior in penetration
resistance. On the other hand, in the case in which the
polymerization degree is more than 3000, the resin film is
inferior in formability and also the resin film has too
high rigidity, resulting in poor processability. The lower
limit of the polymerization degree is more preferably 500
and the upper limit is more preferably 2000.
Also, the aldehyde used for acetalization is not
specifically limited. In general, aldehyde having 1 to 10
carbon atoms is used. Examples thereof include n-
butylaldehyde, isobutylaldehyde, n-valeraldehyde, 2-
ethylbutylaldehyde, n-hexylaldehyde, n-octylaldehyde, n-
nonylaldehyde, n-decylaldehyde, formaldehyde, acetaldehyde
and benzaldehyde. Among these aldehydes, n-butylaldehyde,
n-hexylaldehyde, and n-valeraldehyde are preferable, and
butylaldehyde having 4 carbon atoms is particularly
preferable.
The polyvinyl acetal is preferably polyvinyl butyral
acetalized by butylaldehyde. Taking account of required
physical properties, these acetal resins may be
appropriately blended in combination. Furthermore, a

copolyvinyl acetal resin may be appropriately used in
combination with aldehyde on acetalization. The lower limit
of the acetalization degree of the polyvinyl acetal resin
used in the present invention is preferably 40% and the
upper limit is preferably 85%. The lower limit is more
preferably 60% and the upper limit is more preferably 75%.
When a polyvinyl acetal resin is used as the resin,
the resin composition preferably contains 20 to 60 parts by
weight of a plasticizer for an interlayer film and 0.1 to 3
parts by weight of ITO fine particles based on 100 parts by
weight of the polyvinyl acetal resin. In the case in which
the amount of the plasticizer for an interlayer film is
less than 20 parts by weight, penetration resistance may be
lowered. On the other hand, in the case in which the amount
is more than 60 parts by weight, bleed-out of the
plasticizer occurs and transparency or adhesion of the heat
ray shield interlayer film for laminated glass is lowered,
and thus the resulting laminated glass may have large
optical strain. The lower limit of the amount of the
plasticizer for an interlayer film is more preferably 30
parts by weight and the upper limit is more preferably 60
parts by weight. In the case in which the amount of the ITO
fine particles is less than 0.1 parts by weight, sufficient
heat ray shield effect may not be exerted. On the other
hand, in the case in which the amount is more than 3.0
parts by weight, visible light transmittance may be lowered

and the haze value may increase.
Preferably, the resin composition further contains an
adhesion adjustor. The adhesion adjustor is not
specifically limited, and an alkali metal salt and/or an
alkali earth metal salt are preferably used. The alkali
metal salt and/or the alkali earth metal salt are not
specifically limited and examples thereof include salts of
potassium, sodium, and magnesium. The acid constituting the
salts is not specifically limited and examples thereof
include organic acids, for example, carboxylic acids such
as octylic acid, hexylic acid, butyric acid, acetic acid,
and formic acid; and inorganic acids such as hydrochloric
acid and nitric acid.
Among the above alkali metal salt and/or the alkali
earth metal salt, an alkali metal salt and an alkali earth
metal salt of an organic acid having 2 to 16 carbon atoms
are preferable, and a magnesium salt of carboxylic acid
having 2 to 16 carbon atoms, and a potassium salt of
carboxylic acid having 2 to 16 carbon atoms are preferable.
The magnesium or potassium salt of carboxylic acid
having 2 to 16 carbon atoms is not specifically limited,
and for example, magnesium acetate, potassium acetate,
magnesium propionate, potassium propionate, magnesium 2-
ethylbutanoate, potassium 2-ethylbutanoate, magnesium 2-
ethylhexanoate and potassium 2-ethylhexanoate are
preferably used. These salts may be used alone or in

combination.
The amount of the alkali metal salt and/or the alkali
earth metal salt is not specifically limited. For example,
when the resin is a polyvinyl acetal resin, the lower limit
of the amount is preferably 0.001 parts by weight based on
100 parts by weight of the polyvinyl acetal resin, and the
upper limit is preferably 1.0 parts by weight. In the case
in which the amount is less than 0.001 parts by weight, the
degree of adhesion in the vicinity of the heat ray shield
interlayer film for laminated glass may be lowered under a
high humidity atmosphere. In the case in which the amount
is more than 1.0 parts by weight, the degree of adhesion
may be excessively lowered and transparency of the heat ray
shield interlayer film for laminated glass may be lost. The
lower limit of the amount is more preferably 0.01 parts by
weight and the upper limit is more preferably 0.2 parts by
weight.
Preferably, the resin composition further contains an
antioxidant. The antioxidant is not specifically limited
and examples of the phenolic antioxidant include 2,6-Di-
tert-butyl-p-cresol (BHT) ("Sumilizer BHT", manufactured by
Sumitomo Chemical Industries Co., Ltd.) and tetrakis-
[methylene-3-(3'-5'-di-t-butyl-4'-hydroxyphenyl)propionate]
methane (Irganox 1010, manufactured by Ciba Geigy Ltd.).
These antioxidants may be used alone or in combination. The
amount of the antioxidant is not specifically limited. For

example, when the resin is a polyvinyl acetal resin, the
lower limit of the amount is preferably 0.01 parts by
weight based on 100 parts by weight of the polyvinyl acetal
resin, and the upper limit is preferably 5.0 parts by
weight.
Preferably, the resin composition further contains an
ultraviolet absorber. The ultraviolet absorber is not
specifically limited and examples thereof include
benzotriazole-based compound, benzophenone-based compound,
triazine-based compound, and benzoate-based compound.
The benzotriazole-based compound is not specifically
limited and examples thereof include 2-(2'-hydroxy-5'-
methylphenyl)benzotriazole (Tinuvin P, manufactured by Ciba
Geigy Ltd.), 2- (2'-hydroxy-3',5'-di-t-
butylphenyl)benzotriazole (Tinuvin 320, manufactured by
Ciba Geigy Ltd.), 2-(2'-hydroxy-3'-t-butyl-5'-
methylphenyl)-5-chlorobenzotriazole (Tinuvin 326,
manufactured by Ciba Geigy Ltd.) and 2-(2'-hydroxy-3',5'-
di-amylphenyl)benzotriazole (Tinuvin 328, manufactured by
Ciba Geigy Ltd.).
The benzophenone-based compound is not specifically
limited, and examples thereof include octabenzone
(Chimassorb 81, manufactured by Ciba Geigy Ltd.). The
triazine-based compound is not specifically limited and
examples thereof include 2-(4,6-diphenyl-l,3,5-triazin-2-
yl)-5-[(hexyl)oxy]-phenol (Tinuvin 1577FF, manufactured by

Ciba Geigy Ltd.)- Furthermore, the benzoate-based compound
is not specifically limited and examples thereof include
2,4-di-tert-butylphenyl-3,5-di-tert-butyl-4-hydroxybenzoate
(Tinuvin 120, manufactured by Ciba Geigy Ltd.).
The amount of the ultraviolet absorber is not
specifically limited. For example, when the resin is a
polyvinyl acetal resin, the lower limit of the amount is
preferably 0.01 parts by weight based on 100 parts by
weight of the polyvinyl acetal resin, and the upper limit
is preferably 5.0 parts by weight. In the case in which the
lower limit is less than 0.01 parts by weight, the effect
of absorbing ultraviolet radiation may be hardly exerted.
In the case in which the upper limit is more than 5.0 parts
by weight, weatherability of the resin may be deteriorated.
The lower limit is more preferably 0.05 parts by weight and
the upper limit is more preferably 1.0 parts by weight.
If necessary, the interlayer film for laminated glass
including the resin composition may contain additives such
as photostabilizers, surfactants, flame retardants,
antistatic agents, moisture resistant agents, colorants,
heat ray reflecting agents, and heat ray absorbers.
Although the entire amount of the dispersion stabilizer
contained in the resin composition may be derived from the
dispersion of ITO fine particles of the present invention,
the dispersion stabilizer may be separately added when the
amount is insufficient. In this case, the same dispersion

stabilizer as that described above can be used.
The method for manufacturing the interlayer film for
laminated glass of the present invention is not
specifically limited and includes, for example, a method
for mixing the ITO resin dispersion of the present
invention with the above resin, and a plasticizer for an
interlayer film and/or additives, which are optionally
added, such that the final concentration of the ITO fine
particles is within an expected range to obtain a resin
composition, and forming the mixture into a film using a
conventional film forming method such as extrusion method,
calendering method or pressing method. Among these methods,
an extruding method using extruding machine in which two
axes are arranged in parallel is preferable and can further
enhance the haze value. Using the resulting interlayer film
for laminated glass, a laminated glass having excellent
heat ray shield properties can be manufactured. The method
for manufacturing the laminated glass may be a
conventionally known method.
The interlayer film for laminated glass of the
present invention is conventionally used in the state of
being interposed between laminated glasses. As the glass,
for example, high heat ray absorption glass, clear glass,
and green glass are used. The high heat ray absorption
glass as used herein refers to a heat ray absorption glass
wherein the visible light transmittance is 75% or more and

the transmittance is 65% or less in an entire wavelength
range within a range from 900 to 1300 nm.
The interlayer film and the laminated glass of the
present invention has heat ray shield properties, for
example, under measuring conditions in which an interlayer
film having a thickness of 0.76 mm is interposed between
clear glass sheets having a thickness of 2.5 mm, the
electromagnetic wave shield properties at a frequency of
0.1 MHz to 26.5 GHz are 10 dB or less, the haze value is
1.0% or less, the visible light transmittance is 70% or
more, the solar radiation transmittance at a wavelength
within a range from 300 to 2100 nm is 80% or less of the
visible light transmittance, and the reflection yellow
index is -12 or more, which is preferably -10 or more, and
more preferably -8 or more.
The electromagnetic wave shield properties act as an
indicator which represents the degree of attenuation when
an electromagnetic wave at a measured frequency penetrates
through the interlayer film or the laminated glass. In the
case in which the electromagnetic wave shield properties
are 10 dB or less, when using this laminated glass for the
front glass of automobiles, the latest mobile communication
equipment can be used in the automobile without causing any
problem.
The haze value of the interlayer film or the
laminated glass of the present invention is 1.0% or less.

In the case in which the haze value is 1.0% or more,
transparency of the interlayer film or the laminated glass
becomes insufficient for practical use.
In the interlayer film or the laminated glass of the
present invention, the visible light transmittance is 70%
or more. In the case in which the visible light
transmittance is less than 70%, transparency of the
interlayer film or the laminated glass becomes insufficient
for practical use. Therefore, it becomes impossible to pass
the automotive front glass regulation, and thus good
visibility is adversely affected.
In the interlayer film or laminated glass of the
present invention, the solar radiation transmittance at a
wavelength within a range from 300 to 2100 nm is 80% or
less of the visible light transmittance. In the case in
which the visible light transmittance is more than 80%,
transparency of the interlayer film or the laminated glass
becomes insufficient for practical use.
In the interlayer film or laminated glass of the
present invention, the reflection yellow index is -12 or
more, preferably -10 or more, and more preferably -8 or
more. This means that scattering of visible light due to
ITO fine particles is less likely to occur, resulting in
less clouding. Here, when the concentration and the
dispersion state are the same, the reflection yellow index
depends on the optical path length of the ITO fine

particles dispersion, the dispersion medium, and quality of
the glass. The reflection yellow index of the dispersion of
ITO fine particles is -20 or more under the measuring
conditions due to the above dispersion medium using a glass
cell having an optical path length of 1 mm. When the
laminated glass was assembled, the optical path length is
shorter than that described above and the medium contains
the polyvinyl acetal resin. Therefore, the reflection
yellow index of the laminated glass is preferably -12 or
more.
In the interlayer film or laminated glass of the
present invention, the measured reflection value at 0
degrees among reflected light distribution at an incidence
angle of 45 degrees measured by a goniophotometric
measurement is 25 or less, preferably 20 or less, and more
preferably 15 or less. This means that scattering of
visible light due to secondary agglomeration of ITO fine
particles is less likely to occur, resulting in less
clouding. In the case in which the measured reflection
value is more than 25, clouding may occur and the
transparency of the resulting laminated glass becomes
insufficient for practical use. Here, the reflection value
measured by a goniophotometric measurement is a value
obtained by subtracting a measured reflection value, as a
reference, of a laminated glass obtained by interposing an
interlayer film containing no ITO fine particles dispersed

therein between two clear glass sheets, from a raw data of
the interlayer film or the laminated glass measured at 0
degrees among reflected light distribution at an incidence
angle of 45 degrees.
BEST MODE FOR CARRYING OUT THE INVENTION
The present invention will now be described in more
detail by way of examples. The measurement and evaluation
were conducted by the following procedures.
(A) Primary average particle size of ITO fine particles
The primary average particle size was calculated from
the measured value of the specific surface area (BET) by
the following eguation. It has been confirmed that the
average particle size thus determined from the specific
surface area nearly agrees with the particle size
determined by directly observing using a transmission
electron microscope. The specific surface area due to a BET
method was measured by using a Betasorb automatic surface
area meter, Model 4200, manufactured by Microtrac Inc.
a (urn) = 6/ (pxB)
(a: average particle size, p: true specific gravity, B:
specific surface area (m2/g))
(B) Crystal lattice constant of ITO fine particles
The lattice constant was determined by the following
procedure. Using an automatic X-ray diffractometer MO3X
equipped with monochrometer, correction was conducted by a

high-purity silicon single crystal (99.9999%) and spacing
was calculated from a peak attributed to a plane index
(hkl), and then the lattice constant was determined by the
least-square method.
(C) Tv and Ts of dispersion of ITO fine particles
Using a dispersion of ITO fine particles for
evaluation (0.7% by weight) charged in a glass cell having
an optical path length of 1 mm, the transmittance at a
wavelength within a range from 300 to 2100 nm was measured
by an autographic spectrophotometer (U-4000, manufactured
by Hitachi, Ltd.) and visible light transmittance (Tv) at a
wavelength within a range from 380 to 780 nm and a solar
radiation transmittance (Ts) at a wavelength within a range
from 300 to 2100 nm were determined in accordance with
Japanese Industrial Standard (JIS R 3106).
(D) Reflection yellow index of dispersion of ITO fine
particles
Using the same dispersion, measuring cell and
autographic spectrophotometer as those used in (C), the
reflectance at a wavelength within a range from 380 to 780
nm was measured and the reflection yellow index was
calculated in accordance with Japanese Industrial Standard
(JIS K 7103).
(E) Haze value of dispersion of ITO fine particles
Using the same dispersion and measuring cell as those
used in (C), the haze value was measured by a turbidimeter

with integrating sphere (manufactured by Tokyo Denshoku Co.,
Ltd.) in accordance with Japanese Industrial Standard (JIS
K 7105) .
(F) Goniophotometric measurement of ITO fine particles
Using the same dispersion and measuring cell as those
used in (C), reflected light distribution at an incidence
angle of 45 degrees was measured by an automatic
goniophotometer (GP-200, manufactured by Murakami Color
Research Laboratory) using a halogen lamp as the light
source. Light is received at an angle within a range from -
90 to 90 degrees and a value was measured at 0 degrees
among reflected light distribution. After measuring a
laminated glass obtained by interposing an interlayer film
containing no ITO fine particles dispersed therein between
two clear glass sheets, the value at 0 degrees was
determined and the resulting value was taken as a reference.
The measurement of the dispersion was conducted in the same
manner and the value obtained by subtracting the reference
from the measured value was taken as a measured reflection
value. The measurement was conducted under the following
conditions.
Light source intensity: 12V, 50W
Type of measurement: measurement of reflection
Light receiver: photomultiplier
Tilt angle of sample: 2.5 degrees
Conditions of light receiver:

SENSITIVITY ADJ: 999
HIGH VOLT ADJ: 999
(G) Particle size of ITO fine particles in dispersion of
ITO fine particles
Using a microtrac UPA particle size analyzer
manufactured by NIKKISO Co., Ltd., particle size
distribution of ITO fine particles in a dispersion of ITO
fine particles having a concentration of ITO fine particles
of 10% by weight was determined.
(H) Tv and Ts of laminated glass
Using an autographic spectrophotometer (U-4000,
manufactured by Hitachi, Ltd.), the transmittance at a
wavelength within a range from 300 to 2100 nm of the
laminated glass was measured and then the visible light
transmittance (Tv) at a wavelength within a range from 380
to 780 nm and the solar radiation transmittance (Ts) at a
wavelength within a range from 300 to 2100 nm were measured
in accordance with Japanese Industrial Standard (JIS R 3106
"Testing method on transmittance, reflectance, and
emittance of flat glasses, and evaluation of solar heat
gain coefficient").
(I) Reflection yellow index of laminated glass
Using an autographic spectrophotometer (U-4000,
manufactured by Hitachi, Ltd.), the reflectance at a
wavelength within a range from 380 to 780 nm was measured
and then the reflection yellow index was calculated in

accordance with Japanese Industrial Standard (JIS K 7103).
(J) Haze value of laminated glass
Using a turbidimeter with integrating sphere
(manufactured by Tokyo Denshoku Co., Ltd.), the haze value
of the laminated glass was measured in accordance with
Japanese Industrial Standard (JIS K7105).
(K) Electromagentic wave shield properties (AdB) of
laminated glass
In accordance with the KEC method (method for testing
the electromagnetic wave shield effect in a near field),
the reflection loss (dB) for electromagnetic wave within
the range of 0.1 to 10 MHz of the laminated glass and that
of a common float sheet glass with the thickness of 2.5 mm
were measured respectively and were compared, and the
minimum and maximum differences between their reflection
loss (dB) were described. With respect to the reflection
loss (dB) for electromagnetic wave within the range of 2 to
26.5 GHz, after standing a 600 mm-square sample between a
pair of transreceiver antennas, radio waves from a radio
signal generating apparatus were received by a spectrum
analyzer and electromagentic wave shield properties of the
sample were evaluated (method for testing the
electromagnetic wave in a remote field) .
(L) Goniophotometric measurement of interlayer film and
laminated glass
Using an automatic goniophotometer (GP-200,

manufactured by Murakami Color Research Laboratory) and
using a halogen lamp as the light source, reflected light
distribution at an incidence angle of 45 degrees was
determined. Light is received at an angle within a range
from -90 to 90 degrees and a value was measured at 0
degrees among reflected light distribution. After measuring
a laminated glass obtained by interposing an interlayer
film containing no ITO fine particles dispersed therein
between two clear glass sheets, the value at 0 degrees was
determined and the resulting value was taken as a reference,
The measurement of the laminated glass for evaluation was
conducted and the value obtained by subtracting the
reference from the measured value was taken as a measured
reflection value. The measurement was conducted under the
following conditions.
Light source intensity: 12V, 50W
Type of measurement: measurement of reflection
Light receiver: photomultiplier
Tilt angle of sample: 2.5 degree
Conditions of light receiver:
SENSITIVITY ADJ: 999
HIGH VOLT ADJ: 999
(M) Dispersion state of ITO fine particles in interlayer
film
After preparing ultra-flake of the interlayer film by
using a microtome, the distribution of ITO fine particles

were photographed and observed under the following
conditions by using a transmission election microscope (TEM,
Model H-7100FA, manufactured by Hitachi, Ltd.). The
photographing was carried out in the range of 3 um * 4 urn
at 20,000 magnifications and enlarged at the time of
printing. Obtained image was subjected to a visual
observation, particle sizes of all ITO fine particles in
the above observed scope are measured, and the average
particle size was calculated as an mean volume particle
size. Here, the particle size of ITO fine particle was
decided to be the longest one of the ITO fine particle.
Also, counting the number of the fine particles having a
particle size of 100 nm or more within the above-mentioned
observed scope, dividing them by 12 um2 of an observed space
to calculate the number of the particles per um2.
(N) Adhesion of interlayer film
The adhesion of the interlayer film to the glass was
evaluated in terms of a pummel value. It is to be
understood that the larger the pummel value, the higher the
degree of adhesion to the glass, while the smaller the
pummel value, the lower the degree of adhesion to the glass.
The test method is as follows. First, the laminate glass
was allowed to stand at a temperature of -18 ± 0.6°C for 16
hours and then crushed with a hammer having a head weighing
0.45 kg until the glass fragments became 6 mm or less in
diameter. The degree of exposure of the film after partial

exfoliation of glass was estimated by comparison with
graded limit samples and the result was expressed in the
pummel value according to the schedule shown below in Table
3. The degree of adhesion of the interlayer film to the
glass is preferably adjusted such that the pummel value is
within a range from 3 to 6.
EXAMPLES
Example 1
(Preparation of dispersion of ITO fine particles)
10 Parts by weight ITO fine particles (primary
average particle size: 20 nm, crystal lattice constant:
10.12 A), 1 part by weight of a polyoxyethylene alkyl ether
phosphoric acid ester compound as the dispersant, 2 parts
by weight of 2-ethylhexanoic acid, 3 parts by weight of
acetylacetone, 4 parts by weight of ethanol as the organic
solvent, and 80 parts by weight of triethylene glycol di-2-
hexanoate (3GO) were mixed and dispersed to prepare a
dispersion of ITO fine particles. This composition is shown
in Table 1. This dispersion of ITO fine particles was
diluted with triethylene glycol di-2-hexanoate (3GO) so as
to adjust the concentration of the ITO fine particles to
0.7% by weight to obtain a dispersion of ITO fine particles
for evaluation. The visible light transmittance (Tv) , the
solar radiation transmittance (Ts), the haze value, the
reflection yellow index, the reflection value measured by a

goniophotometric measurement of the dispersion having an
ITO concentration of 0.7% by weight are shown in Table 2.
With respect to the dispersion having an ITO concentration
of 10% by weight, the mean volume particle size and
particle size at 90% accumulation of the ITO fine particles
are shown in Table 2 (Sample No. la).
34.5 Parts by weight of ITO fine particles, and a
polyoxyethylene alkyl ether phosphoric acid ester compound,
2-ethylhexanoic acid, acetylacetone, ethanol, and 3GO, each
of which amount is shown in Table 1, were mixed to prepare
a dispersion of ITO fine particles and then the dispersion
of ITO fine particles was diluted with 3GO to obtain a
dispersion having an ITO concentration of 0.7% by weight
and a dispersion having an ITO concentration of 10% by
weight. In the same manner as in the case of the Sample No.
la, physical properties of these dispersions were
determined. The results are shown in Table 2 (Sample No.
1b) .
Furthermore, 25 parts by weight of ITO fine particles,
and a polyoxyethylene alkyl ether phosphoric acid ester
compound, 2-ethylhexanoic acid, acetylacetone, ethanol, and
3G0 each of which amount is shown in Table 1, were mixed to
prepare a dispersion of ITO fine particles, and then the
dispersion of ITO fine particles was diluted with 3GO to
obtain a dispersion having an ITO concentration of 0.7% by
weight and a dispersion having an ITO concentration of 10%

by weight. In the same manner as in the case of the Sample
No. la, physical properties of these dispersions were
determined. The results are shown in Table 2 (Sample No.
lc) .
(Synthesis of polyvinyl butyral)
275g of polyvinyl alcohol having an average
polymerization degree of 1700 and a saponification degree
of 99.2 mol% was added to 2890g of pure water and then
dissolved with heating. After the temperature of the
solution was controlled to 15°C, 201g of hydrochloric acid
having a concentration of 35% by weight and 157g of n-
butylaldehyde were added, and then the mixed solution was
maintained at 15°C, thereby precipitating a reaction
product. After the reaction was completed by maintaining
the reaction system at 60°C for 3 hours, the reaction
mixture was washed with an excess amount of water for
washing away unreacted n-butyraldehyde, neutralized with
sodium hydroxide, which is the common neutralizing agent,
moreover washed with an excessive amount of water for 2
hours and dried to provide polyvinyl butyral resin as a
white powder with an average butyralization degree of 68.5
mol%.
(Production of heat ray shield interlayer film for
laminated glass)
To 100 parts by weight of a polyvinyl butyral resin,
2.8 parts by weight of a dispersion of ITO fine particles

(ITO concentration: 10% by weight, Sample No. la) shown in
Table 1 was added, and 3GO was added so as to adjust the
ITO concentration to 0.2% by weight. Then magnesium 2-
ethylbutyrate and magnesium acetate were added
appropriately to be 60 ppm as magnesium content to the
reaction mixture. The mixture was melt-kneaded thoroughly
with a mixing roll and press-molded with a press-molding
machine at 150°C for 30 minutes to provide an interlayer
film for laminated glass having an average thickness of
0.76 mm.
(Production of laminated glass)
The resulting interlayer film was interposed between
two transparent float sheet glasses (30cm * 30cm x 2.5mm
thickness) and the assembly was placed in a rubber bag and
deaerated under a vacuum of 2660Pa for 20 minutes. The
deaerated assembly was transferred to an oven under suction
and pressed under vacuum at 90°C for 30 minutes. The
prebonded laminated glass thus obtained was subjected to
post-bonding in an autoclave at 135°C and 118N/cm2 for 20
minutes to provide a laminated glass. Physical properties
of the laminated glass were determined. The results are
shown in Table 2 (Sample No. la).
An dispersion of ITO fine particles (ITO
concentration: 34.5% by weight, Sample No. lb) shown in
Table 1 was mixed with polyvinyl butyral resin and then
magnesium was added in the same amount as that in the case

of the Sample No. la to prepare interlayer films
(thickness: 0.76mm) wherein the concentration of the ITO
fine particles is 0.7% by weight and 0.2% by weight. Using
the resulting interlayer films, a laminated glass was
manufactured in the same manner as in the case of the
Sample No. la. Physical properties of the laminated glass
were determined. The results are shown in Table 2 (Sample
No. lb).
Example 2
In the same manner as in Example 1, except that ITO
fine particles having a primary particle size and a lattice
constant shown in Table 1 were used and three kinds of
dispersion stabilizers and alcohols were used, and also the
respective components were used in the amounts shown in
Table 1, a dispersion of ITO fine particles was prepared.
The components of this dispersion are shown in Table 1. An
interlayer film was manufactured by diluting the dispersion
with a plasticizer for an interlayer film shown in Table 1
so as to adjust to the ITO concentration to the value shown
in Table 2, and then a laminated glass was manufactured by
using the interlayer film. Physical properties of the
dispersion of ITO fine particles and the laminated glass
were determined and evaluated. The results are shown in
Table 2 (Samples No. 2 to No. 9).
Example 3
In the same manner as in Example 1, except that a

compound shown in Table 1 was used as the plasticizer for
an interlayer film and the respective components were used
in the amounts shown in Table 1, a dispersion of ITO fine
particles was prepared. The components of this dispersion
are shown in Table 1. An interlayer film was manufactured
by diluting the dispersion with a plasticizer for an
interlayer film shown in Table 1 so as to adjust to the ITO
concentration to the value shown in Table 2, and then a
laminated glass was manufactured by using the interlayer
film. Physical properties of the dispersion of ITO fine
particles and the laminated glass were determined and
evaluated. The results are shown in Table 2 (Samples No. 10
to No. 12).
(Test Example)
Using ITO fine particles, a plasticizer for an
interlayer film, a dispersion stabilizer and alcohols shown
in Table 1 in the amount shown in Table 1, a dispersion of
ITO fine particles was manufactured. An interlayer film was
manufactured by diluting the dispersion with a plasticizer
for an interlayer film shown in Table 1 so as to adjust to
the ITO concentration to the value shown in Table 2, and
then a laminated glass was manufactured by using the
interlayer film. Physical properties of the dispersion of
ITO fine particles and the laminated glass were determined
and evaluated. The results are shown in Table 2 (Samples No.
13 to No. 14).

Comparative Example
Using ITO fine particles having a slightly large
lattice constant and using a plasticizer for an interlayer
film, a dispersion stabilizer, and alcohols shown in Table
1 in the amount shown in Table 1, a dispersion of ITO fine
particles was manufactured. Using ITO fine particles, a
plasticizer for an interlayer film, a dispersion stabilizer,
and alcohols shown in Table 1 in the amount shown in Table
1, a dispersion of ITO fine particles was manufactured. A
laminated glass was manufactured by using these dispersions.
Physical properties of the dispersion of ITO fine particles
and the laminated glass were determined and evaluated. The
results are shown in Table 2 (Samples No. 15 to No. 18).
In the same manner as in Example 1, except that a
dispersion stabilizer and alcohols were not used and only a
plasticizer for an interlayer film was used, a dispersion
of ITO fine particles was prepared. The components of this
dispersion are shown in Table 1. A laminated glass was
manufactured using the dispersion. Physical properties of
the dispersion of ITO fine particles and the laminated
glass were determined and evaluated. The results are shown
in Table 2 (Sample No. 19).
In the same manner as in Example 1, except that
alcohols were not used and one kind of sulfate ester or n-
butyric acid was used as the dispersion stabilizer, a
dispersion of ITO fine particles was prepared. The

components of this dispersion are shown in Table 1. A
laminated glass was manufactured using the dispersion.
Physical properties of the dispersion of ITO fine particles
and the laminated glass were determined. The results are
shown in Table 2 (Samples No. 20 to No. 21).
In the same manner as in Example 1, except for using
the components of the Samples No. la, No. 2, and No. 12
shown in Table 1, excluding alcohols, a dispersion of ITO
fine particles was prepared. A laminated glass was
manufactured using the dispersion. Physical properties of
the dispersion of ITO fine particles and the laminated
glass were determined. The results are shown in Table 2
(Samples No. 22, No. 23, and No. 24).
In the same manner as in Example 1, except that a
dispersion stabilizer was not used and a plasticizer and
alcohols were used, a dispersion of ITO fine particles was
prepared. The components of this dispersion are shown in
Table 1. A laminated glass was manufactured using the
dispersion. Physical properties of the dispersion of ITO
fine particles and the laminated glass were determined. The
results are shown in Table 2 (Sample No. 25).
In the same manner as in Example 1, except that the
same ITO fine particles and plasticizer for an interlayer
film as those in Example 1 and also an anionic surfactant
or a higher fatty acid ester was used as shown in Table 1,
a dispersion of ITO fine particles was prepared. The

components of this dispersion are shown in Table 1. A
laminated glass was manufactured using the dispersion.
Physical properties of the dispersion of ITO fine particles
and the laminated glass were determined. The results are
shown in Table 2 (Samples No. 26 to No. 27).
As shown in Table 1 and Table 2, the dispersion of
ITO fine particles and laminated glasses of Examples (No. 1
to No. 12) of the present invention show high visible light
transmittance (Tv), low haze value, and high absolute value
of the reflection yellow index as compared with Comparative
Samples (No. 16 to No. 21, No. 25 to No. 27). The laminated
glasses of Examples (No. 1 to No. 12) of the present
invention show extremely low value measured by a
goniophotometric measurement, extremely low mean volume
particle size, and extremely low number of particles having
a particle size larger than 100 nm as compared with the
Comparative Samples (No. 16 to No. 21, No. 25 to No. 27).
In all samples, the pummel value was 4 and was controlled
within a preferable range.
The Sample No. 13 containing no n-butyric acid as the
dispersion stabilizer and the Sample No. 14 containing no
acetylacetone as the dispersion stabilizer are excellent in
visible light transmittance, solar radiation transmittance,
haze value, reflection yellow index, reflection value
measured by a goniophotometric measurement, and pummel
value.

In the case of the Comparative Sample No. 15 wherein
ITO fine particles have a slightly large lattice constant,
a ratio of the solar radiation transmittance to the visible
light transmittance is not within the range of the present
invention. In the case of the Comparative Samples (No. 16
to No. 21, No. 25 to No. 27), the haze value of the
dispersion of ITO fine particles is more than 1.0% and the
reflection yellow index is considerably less than -20 and
also the reflection value measured by a goniophotometric
measurement is more than 40. The haze value of the
interlayer film for laminated glass is more than 1.0% and
the reflection yellow index is within a range from -15 to -
18 and also the reflection value measured by a
goniophotometric measurement is within a range from 29 to
66, and thus all of them are not within the range of the
present invention.
In the case of the Comparative Samples No. 22 to No.
24, the haze value of the dispersion of ITO fine particles
is more than 1.0% and the reflection yellow index is less
than -20 and also the reflection value measured by a
goniophotometric measurement is more than 50. In the case
of the Samples No. 22 and No. 23, the haze value of the
interlayer film for laminated glass is 1.0% or less, while
the haze value is more than 1.0% in the case of the Sample
No. 24. The reflection yellow index is within a range from
-14 to -18 and the reflection value measured by a

goniophotometric measurement is within a range from 38 to
66, and thus none of them are within the range of the
present invention.































Table 3
INDUSTRIAL APPLICABILITY
The dispersion of tin-doped indium oxide fine
particles of the present invention is excellent in
dispersibility of tin-doped indium oxide fine particles and
has high transparency at a certain angle, and is also less
likely to cause solvent shock and maintains good dispersion
state of tin-doped indium oxide fine particles when the
dispersion is mixed with the resin. This dispersion of tin-
doped indium oxide fine particles is suited for the
manufacture of an interlayer film for laminated glass, and
an interlayer film for laminated glass with excellent heat
ray shield properties and a laminated glass including the
same can be obtained by using the dispersion.

WE CLAIM :
1. A dispersion of tin-doped indium oxide fine particles, the dispersion
comprising tin-doped indium oxide tine particles, a plasticizer for an interlayer
film, an organic solvent containing at least one alcohol as a main component, and a
dispersion stabilizer.
wherein under measuring conditions of a concentration of the tin-doped
indium oxide fine particles of 0.7° o by weight and an optical path length of a glass
cell of 1 mm.
a visible light transmittance is 80% or more.
a solar radiation transmittance at a wavelength within a range from 300
nm to 2100 nm is 3 4 or less of the visible light transmittance.
a haze value is 1.0°oor less.
a reflection yellow index is -20 or more.
the dispersion stabilizer comprises chelate. organic acid, and phosphate
ester-based compound.
the content of the dispersion stabilizer is from 6 to 20.7°o by weight, and
the concentration of the tin-doped indium oxide fine particles is IO'\> hweight or more.
2. The dispersion of tin-doped indium oxide fine particles -as claimed in
claim I.
wherein instead of the reflection yellow index being -20 or more, or with
the reflection yellow index being -20 or more.
under measuring conditions of the optical path length of the glass cell of 1
mm. a reflection value at 0 degrees among reflected light distribution at an
incidence angle of 45 degrees measured by a goniophotometer is 30 or less.
3. The dispersion of tin-doped indium oxide tine particles as claimed in
claim 1.
wherein the plasticizer for an interlayer film is at least one selected from
the group consisting of dihexyl adipate. triethylene glycol di-2-ethylhexanoate.
tetraethylene glycol di-2-ethylhexanoate. triethylene glycol di-2-ethyl butyrate.

tetraethylene glycol di-2-ethyl butyrate. tetraethylene glycol di-heptanoate. and
triethy lene glycol di-heptanoate.
4. The dispersion of tin-doped indium oxide tine particles as claimed in
claim I.
wherein the alcohols comprise at least one selected from the group
consisting of methanol. ethanol. propanol. isopropanol. n-butanol. isohutanol. sec-
butanol. tert-butanol. lauryl alcohol, diacetone alcohol. cyclohexanol. ethylene
glycol. diethylene glycol. and triethylene glycol.
5. The dispersion of tin-doped indium oxide tine particles as claimed in
claim 1.
wherein the dispersion stabilizer is a compound having at least one
selected from the group consisting of nitrogen, phosphorus, and chalcogen atoms.
6. The dispersion of tin-doped indium oxide tine particles as claimed in
claim 1.
wherein a concentration of the tin-doped indium oxide tine particles is
from 10to95°ob\ weight.
a content of the plasticizer for an interlayer film is from 1 to 85% by
weight, and
a content of the organic solvent containing alcohols as a main component
is from 0.02 to 25% by weight
7. The dispersion of tin-doped indium oxide fine particles as claimed in
claim 1.
wherein the dispersion of tin-doped indium oxide fine particles is obtained
by diluting a dispersion of tin-doped indium oxide fine particles which contains tin-
doped indium oxide tine particles, a plasticizer for an interlayer film, an organic
solvent containing alcohols as a main component, and a dispersion stabilizer, and
in which a concentration of the tin-doped indium oxide fine particles is from 0.1 to
95% by weight, with a plasticizer for an interlayer film, or a plasticizer for an
interlayer film containing an organic solvent containing alcohols as a main
component and 'or a dispersion stabilizer.

8. The dispersion of tin-doped indium oxide fine particles -as claimed in
claim 1.
wherein, when a concentration of the tin-doped indium oxide fine particles
is adjusted to 10.0% by weight by diluting a dispersion of tin-doped indium oxide
fine particles having the concentration of the tin-doped indium oxide fine particles
of 10.0% by weight or more, or when a concentration of the tin-doped indium
oxide fine particles is adjusted to 40.0% by weight by diluting a dispersion of tin-
doped indium oxide tine particles having the concentration of the tin-doped indium
oxide fine particles of 40.0% by weight or more.
a mean volume particle size of the tin-doped indium oxide tine particles is
80 nm or less, and
a particle size at 90% accumulation (D90) is 160 nm or less.
9. The dispersion o( tin-doped indium oxide fine particles as claimed in
claim 1.
wherein a primary a\erage particle size of the tin-doped indium oxide fine
particles is 0.2 urn or less.
10. The dispersion of tin-doped indium oxide fine particles as claimed in
claim 1.
wherein a lattice constant of a tin-doped indium oxide fine particle crystal
is from 10.1 I to 10.16 A.
11. A method for manufacturing the dispersion of tin-doped indium oxide fine
particles as claimed in claim 1.
the method comprising mixing an organic solvent containing at least one
alcohol as a main component, a dispersion stabilizer, tin-doped indium oxide fine
particles, and plasticizer for an interlayer film, thereby dispersing the tin-doped
indium oxide fine particles.
wherein the dispersion stabilizer comprises chelate. organic acid, and
phosphate ester-based compound.
the content of the dispersion stabilizer is from 6 to 20.7% by weight, and
the concentration of the tin-doped indium oxide fine particles is 10% by

weight or more.
12. The method for manufacturing a dispersion of tin-doped indium oxide fine
particles as claimed in claim 1 1.
wherein a mixed solution containing the organic solvent containing the
alcohols as a main component, the dispersion stabilizer, and the tin-doped indium
oxide tine particles is prepared, and
this mixed solution is mixed with the plasticizer for an interlayer film to
obtain a dispersion of tin-doped indium oxide fine particles.
13. The method for manufacturing a dispersion of tin-doped indium oxide tine
particles as claimed in claim 12.
wherein the mixed solution containing the organic solvent containing the
alcohols as a main component, the dispersion stabilizer, and the tin-doped indium
oxide tine particles is prepared, and
this mixed solution is added to the plasticizer for an interlayer film, or the
plasticizer for an interlayer film is added to this mixed solution, thereby dispersing
the tin-Joped indium oxide fine particles.
14. The method for manufacturing a dispersion of tin-doped indium oxide fine
particles as claimed in claim 1 2.
wherein a plasticizer containing an organic solvent containing alcohols as
a main component or a dispersion stabilizer is used as the plasticizer for an
interlayer film.
15. An interlayer film for heat shield laminated glass, which is formed by
using a resin composition of a mixture of the dispersion of tin-doped indium oxide
fine particles as claimed in claim 1 and a resin.
wherein, under measuring conditions in which the interlayer film having a
thickness of 0.76 mm is interposed between clear glass sheets having a thickness of
2.5 mm.
electromagnetic wave shield properties at a frequency of 0.1 MHz to 26.5
GHz is lOdBorless.
a haze value is 1.0% or less.

a visible light transmittance is 70% or more.
a solar radiation transmittance at a wavelength within a range from 300 to
2100 nm is 80° o or less of the visible light transmittance. and
a reflection yellow index is -12 or more.
16. The interlayer film for laminated glass as claimed in claim 15.
wherein instead of the reflection yellow index being -12 or more or with
the reflection yellow index being -12 or more.
a reflection value at 0 degrees among reflected light distribution at an
incidence angle of 45 degrees measured by a goniophotometric measurement is 25
or less.
1 7. The interlay er film for laminated glass as claimed in claim I 5.
wherein 20 to 60 parts by weight of the plasticizer for an interlayer film
and 0.1 to 3 parts by weight of the tin-doped indium oxide fine particles based on
100 parts by weight of a poly\ inyl acetal resin are contained.
1 8. The interlay cr film lor laminated glass as claimed in claim 1 7.
wherein the polyvinyl acetal resin is a polyvinyl butyral resin.
19. The interlayer film for laminated glass as claimed in claim 15.
wherein the resin composition obtained by mixing the dispersion of tin-
doped indium oxide fine particles with the resin further contains an alkali metal salt
and .'or an alkali earth metal salt as an adhesion adjuster.
20. The interlayer film for laminated glass as claimed in claim 15.
wherein the tin-doped indium oxide fine particles have an average particle
size of SO nm or less and are dispersed such that a number of particles having a
particle size of 100 nm or more is one per unr or less.
21. A laminated glass comprising the interlayer film for laminated glass as
claimed in claim 1 5.
22. The laminated "lass as claimed in claim 21.

wherein the laminated glass has heat ray shield properties in which
electromagnetic wave shield performance at a frequency of 0.1 MHz to 26.5 GHz
is 10 dB or less, a haze value is 1.0% or less, a visible light transmittance is 70° o or
more, a solar radiation transmittance at a wavelength within a range from 300 to
2100 nm is 80% or less of the visible light transmittance. and a reflection yellow
index is -12 or more.
23. The laminated glass as claimed in claim 22.
wherein instead of the reflection yellow index being —12 or more, or with
the reflection yellow index being -12 or more.
a reflection value measured at 0 degrees among reflected light distribution
at an incidence angle of 45 degrees measured by a goniophotometric measurement
is 25 or less.


A dispersion of tin-doped indium oxide fine particles
has tin-doped indium oxide fine particles, a plasticizer
for an interlayer film, an organic solvent containing
alcohols as a main component, and a dispersion stabilizer,
wherein under measuring conditions of a concentration of
tin-doped indium oxide fine particles of 0.7% by weight and
an optical path length of a glass cell of 1 mm, a visible
light transmittance is 80% or more, a solar radiation
transmittance at a wavelength within a range from 300 nm to
2100 nm is 3/4 or less of the visible light transmittance,
a haze value is 1.0% or less, and a reflection yellow index
is -20 or more.

Documents:

02020-kolnp-2006 abstract.pdf

02020-kolnp-2006 claims.pdf

02020-kolnp-2006 correspondence other.pdf

02020-kolnp-2006 description(complete).pdf

02020-kolnp-2006 form1.pdf

02020-kolnp-2006 form3.pdf

02020-kolnp-2006 form5.pdf

02020-kolnp-2006 international publication .pdf

02020-kolnp-2006 priority document.pdf

02020-kolnp-2006-correspondence others-1.1.pdf

02020-kolnp-2006-correspondence-1.2.pdf

02020-kolnp-2006-form-18.pdf

02020-kolnp-2006-g.p.a.pdf

2020-KOLNP-2006-ABSTRACT 1.1.pdf

2020-kolnp-2006-assignment.pdf

2020-KOLNP-2006-CANCELLED PAGES.pdf

2020-KOLNP-2006-CLAIMS 1.1.pdf

2020-KOLNP-2006-CORRESPONDENCE 1.1.pdf

2020-kolnp-2006-correspondence-1.2.pdf

2020-KOLNP-2006-CORRESPONDENCE.pdf

2020-kolnp-2006-examination report.pdf

2020-KOLNP-2006-FORM 1.1.1.pdf

2020-kolnp-2006-form 13-1.1.pdf

2020-KOLNP-2006-FORM 13.pdf

2020-kolnp-2006-form 18.pdf

2020-KOLNP-2006-FORM 3.1.1.pdf

2020-kolnp-2006-form 3.pdf

2020-kolnp-2006-form 5.pdf

2020-KOLNP-2006-FORM-27.pdf

2020-kolnp-2006-gpa.pdf

2020-kolnp-2006-granted-abstract.pdf

2020-kolnp-2006-granted-claims.pdf

2020-kolnp-2006-granted-description (complete).pdf

2020-kolnp-2006-granted-form 1.pdf

2020-kolnp-2006-granted-specification.pdf

2020-kolnp-2006-others-1.1.pdf

2020-KOLNP-2006-OTHERS.pdf

2020-KOLNP-2006-PETITION UNDER RULE 137.pdf

2020-kolnp-2006-reply to examination report-1.1.pdf

2020-KOLNP-2006-REPLY TO EXAMINATION REPORT.pdf

2020-kolnp-2006-translated copy of priority document-1.1.pdf

2020-KOLNP-2006-TRANSLATED COPY OF PRIORITY DOCUMENT.pdf


Patent Number 247589
Indian Patent Application Number 2020/KOLNP/2006
PG Journal Number 17/2011
Publication Date 29-Apr-2011
Grant Date 26-Apr-2011
Date of Filing 18-Jul-2006
Name of Patentee MITSUBISHI MATERIALS CORPORATION
Applicant Address 5-1, OTEMACHI 1-CHOME, CHIYODA-KU, TOKYO
Inventors:
# Inventor's Name Inventor's Address
1 HAGIWARA, MASAHIRO C/O JEMCO INC., KASHIMA PLANT, 19-1, HIGASHIFUKASHIBA, KAMISU-MACHI, KASHIMA-GUN, IBARAKI-KEN
2 FUKATANI, JUICHI C/O SEKISUI CHEMICAL CO., LTD., 1259, IZUMI, MINAKUCHI-CHO, KOGA-GUN, SHIGA-KEN
3 YOSHIOKA, TADAHIKO C/O SEKISUI CHEMICAL CO., LTD., 1259, IZUMI, MINAKUCHI-CHO, KOGA-GUN, SHIGA-KEN
4 HATTA BUNGO C/O SEKISUI CHEMICAL CO., LTD., 2-1, HYAKUYAMA, SHIMAMOTO-CHO, MISHIMA-GUN, OSAKA
5 NAKAGAWA TAKESHI C/O JEMCO INC., KASHIMA PLANT, 19-1, HIGASHIFUKASHIBA, KAMISU-MACHI, KASHIMA-GUN, IBARAKI-KEN
PCT International Classification Number C03C 27/12
PCT International Application Number PCT/JP2004/008576
PCT International Filing date 2004-06-11
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 2003-427446 2003-12-24 Japan