Title of Invention

AN IMPROVED DEVICE TO MEASURE VISCOSITY, PHASE TRANSFORMATION AND CRYSTALLIZATION IN LIQUID MELTS AT A TEMPERATURE UP TO 1450 O C.

Abstract The improved ultrasonic device comprises of a melting unit, a buffer rod/sample holder, a cooling unit, and an ultrasonic testing system. The buffer rod/sample holder can be configured as a vertical rod with a port on the top to hold the sample positioned inside a vertical tubular furnace. A sample is kept in a port/chamber at top end of the buffer rod/sample holder, which can be inserted into the furnace from the bottom. The bottom end of the buffer rod/sample holder is water cooled at which the ultrasonic transducers are kept for ultrasonic measurements. In an alternative embodiment, the sample will be inserted through a buffer rod with a port at its first end through the side walls of a box type or through one end of a horizontal tubular furnace. The second end accommodating transducers at which the ultrasonic measurements are to be taken will be water cooled.
Full Text 1
Title: A novel design of an ultrasonic viscometer to measure viscosity, phase transformation and crystallization in liquid melts at temperature up to 1450° C
FIELD OF INVENTION
The present invention relates to an improved ultrasonic viscometer to transmit and receive ultrasonic normal incidence shear including longitudinal waves in molten fluxes/slags/metals/polymers at temperature up to 1450°C. More particularly, the invention relates to an improved device for measuring viscosity, phase transformation and crystallization in molten solids at temperatures upto 1450°C.
BACKGROUND OF THE INVENTION
The ultrasonic viscometer can be used to measure physical and thermo physical properties of liquids such as viscosity (h), density (r), at both room temperature and elevated temperatures.
The basic underlined principle of the current invention is the sensitiveness of ultrasonic shear waves to the variations of the properties like viscosity (h), density (r) of a liquid medium. The product of viscosity (h) and density (r) is correlated with the reflection coefficient of these waves. The longitudinal ultrasonic waves are also related with density of the liquid. If the density of the liquid is obtained using the longitudinal waves, the viscosity of the liquid can be determined.

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The presently available conventional high temperature viscometers comprise a number of rotating components which are prone to frequent damage under high temperature conditions. Due to absence of the rotating parts in the proposed ultrasonic viscometer such problems have been eliminated. However the main constraint in determination of viscosity in molten fluxes/slags/glasses using the proposed ultrasonic viscometer is their high melting temperature which poses problem in transmitting ultrasonic waves in the hot liquid medium. This high temperature problem for transmitting ultrasonic waves has been solved by applying a cooling system near the end of the buffer rod where ultrasonic transducer has been positioned.
The special feature of the proposed viscometer is the design of a port made at the other end of the buffer rod to hold the powdered sample. Using this viscometer the ultrasonic waves can be transmitted in the hot liquid (molten fluxes/slags/glasses) through buffer rods made of materials capable to withstand the temperature of 1500°C.
The main feature of this viscosity measuring device is that there is no rotating part like that in conventional HAAKE viscometer used for this purpose.
OBJECTIVE OF THE INVENTION
The objective of the present invention is to propose an improved ultrasonic device to determine viscosity of molten fluxes/slags/glasses and low melting metals and alloys such as Pb, Zn etc.

3 SUMMARY OF THE INVENTION
The improved ultrasonic device comprises of a melting unit, a buffer rod/sample holder, a cooling unit, and an ultrasonic testing system. The buffer rod/sample holder can be configured as a vertical rod with a port on the top to hold the sample positioned inside a vertical tubular furnace. A sample is kept in a port/chamber at top end of the buffer rod/sample holder, which can be inserted into the furnace from the bottom. The bottom end of the buffer rod/sample holder is water cooled at which the ultrasonic transducers are kept for ultrasonic measurements.
In an alternative embodiment, the sample will be inserted through a buffer rod with a port at its first end through the side walls of a box type or through one end of a horizontal tubular furnace. The second end accommodating transducers at which the ultrasonic measurements are to be taken will be water cooled.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
The invention can now be described in detail with the help of the figures of the accompanying drawings in which:
Figure 1 shows schematic diagram of an improved ultrasonic device with a vertical buffer rod/sample holder inside a vertical tubular furnace with a cooling means, probe positioning and display of interfacial echoes, according to a first embodiment of the invention.
Figure 2 shows the details of the furnace and the buffer rod/sample holder as shown in Figure 1.

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Figure 3 shows an alternate embodiment box type furnace and a buffer rod/sample holder inserted through the side walls of the furnace.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT OF THE INVENTION
Figure 1 is a schematic diagram of a proposed device showing a tubular vertical furnace (1) with at least two heating elements (2) in the refractory walls (3). A buffer rod (4) holding a powdered sample (S) has been inserted from the bottom (5) of the furnace (1). The filling of the powdered sample in a port (6) of the buffer rod (4) should be such that the sample after melting, the molten slag touches a reflector's surface (RS). When the furnace (1) is on, the temperature of the powder (S) rises, it melts and in molten condition at a desired temperature (that is 1300°C for mold fluxes for continuous casting of steel) the ultrasonic parameters like reflection coefficient or shear waves and ultrasonic velocity of longitudinal waves in molten slag is measured. The bottom part of the buffer rod (4) is water cooled by means of a water jacket (7) as shown in Figure 1. As shown in Figure 1, the reflection coefficient of shear waves is measured from the amplitude of the echo from the buffer rod/molten slag interface (RS), whereas the ultrasonic velocity of the longitudinal waves is measured from the transit time between the echo from the buffer rod/molten slag interface (RS) and that from molten slag/reflector interface (SS). The interfacial echoes can be displayed in an ultrasonic display means (14).
The transducers (8) are placed at the bottom end of the buffer rod/sample holder (4). The furnace (1) will have thermocouple (11). The water jacket (7) provided with water inlet (12) and a water outlet (13).

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Figure 2 shows the dimensional details of the vertical tubular furnace along with the position of the buffer rod/sample holder (4) in a device. The dimensional details of the furnace (1) details are given in Table 1.
Table 1. Dimensional Details vertical tubular furnace.
SI. No Dimension in mm
Height (H) 500
Inner Diameter (ID) 100
Outer Diameter (OD) 400
Refractory (3) thickness in top and bottom cover 25
Height of bottom stand (10) 425
The heating elements (2) are made of silicon carbide or graphite and positioned
in the vertical walls of the furnace. The furnace body (9) including the support
members (10) for the furnace (1) and the buffer rod/sample holder (4) can be made
of stainless steel.
Table 2 shows the dimensional details of the buffer rod/sample holder (4), reflector
and the port (6) in the buffer rod (4) in the case of vertical tubular furnace.

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Table 2. The dimensional details of buffer rod/sample holder (4), reflector (RS) and the port (6) in it.
Items Material Diameter, Length, Height,
mm mm mm
Buffer Alumina AD-94/Direct 50 500 -
Rod (4) Sintered Silicon
Carbide DS-SC/
Tungsten (W)/
Molybdenum (Mo)/
Titanium (Ti)
Port (6) -DO 30 100
Reflector -DO- 10
(RS)
Length of the buffer rod/sample holder (4) outside the furnace (1) = 200 mm Figure 3 shows the dimensional details of a box type furnace (2) along with the position of the buffer rod/sample holder (4) in the device. Table 1. Dimensional Details of Box type furnace (2).
SI. No Dimension in mm
Length (L) 400
Width (W) 400
Height (H) 500
Refractory (3) thickness in top and bottom cover 25
Height of bottom stand (10) 425

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Table 2. The dimensional details of buffer rod/sample holder (4), reflector (RS) and the port (6) in it.
Items Material Diameter, Length, Height,
mm mm mm
Buffer Alumina AD-94 or 50 500 -
Rod (4') Direct Sintered Silicon
Carbide DS-SC or Mo
or W or Ti
Port (6) -DO- 30 100
Reflector -DO- 10
(RS)
Refractory (3) thickness in top, bottom cover and side alls = 50 mm Height of the bottom stands (10) = 400 mm. The heating elements (2) are silicon carbide or graphite placed on the three vertical walls and on the roof.
Dimensional details of the buffer rod/sample holder (4) are
Cross section = 50 x 50 mm; Length = 300 mm;
Material of the buffer rod/sample holder;
Alumina AD-94 or Direct Sintered Silicon Carbide DS-SC or Mo or W or Ti
Dimension of the port made in buffer rod/sample holder;
Length = 70m; Width = 30 mm; Height = 30 mm.
ADVANTAGES OF THE PRESENT INVENTION
1. Unlike conventional viscometers (HAKEE VISCOMETER), due to the absence of rotating parts at high temperature, the frequent material damage problems are eliminated.

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2. Unique design of a port made at the end of a buffer rod/sample holder allows
the ultrasonic measurement by positioning the ultrasonic probes at one end
only rather positioning at both the ends.
3. The buffer rod/sample holder with a port made at one end (which remains
inside the furnace during measurement) serves both as a sample holder as
well as transmitter of ultrasonic waves in liquid at temperatures up to 1450°C.
4. Careful selection of advanced ceramic materials like Alumina AD-94 or Direct
Sintered Silicon carbide (DS-SC) or Mo, W or Ti for making buffer rod/sample
holder. This allows easy transmission of ultrasonic waves into the molten
materials at temperature upto 1450°C through the buffer rod/sample holder.
5. The use of the above buffer rod/sample holder allows to measure reflection
coefficients of ultrasonic transverse waves and transmit time of ultrasonic
longitudinal
waves in the liquid at high temperature. From reflection coefficient viscosity and from transmit time density of the liquid is determined.
6. During cooling, crystallization and phase transformations can be indicated by
abrupt change in the ultrasonic velocity or attenuation.
7. The presence of a box type cooling chamber near the measuring end
(projected outside furnace) allows the probe position to cool down and avoids
the probe damage due to high temperature.
8. The dimensional details of tubular vertical furnace and box type furnace to
suit the ultrasonic measurements.

9 We Claim
1. An improved device adaptable to furnaces, to measure viscosity, phase transformation and crystallization in liquid melts at temperatures upto 1450°C, the furnace can be selected as a vertical tubular furnace or a box type furnace, and comprising at least two heating elements (2) in its refractory walls (3), and a thermocouple (11), the furnace (1) being disposed on stainless steel support (10) and encased in stainless steel casing (9), the device comprising: -
- A buffer rod/sample holder (4) having a port (6) at a first end to hold a
powdered sample (S) which when inserted into the furnace (1) from a
bottom (5), allows the powdered material to produce molten slag
which touches the surface of a reflector (RS) of the rod (4);
- At least one transducer (8) attached at a second end of the buffer
rod/sample holder (4), which is being projected out of the furnace and
disposed in a cooling unit (7) having one each water inlet (12) and
water outlet (13). The transducer (8) acquires data from the buffer rod
/ molten slag interface (12) to measure reflection coefficient of shear
waves, and the transit time between the echo from the buffer
rod/reflector interface (SS) to determine the ultrasonic velocity of the
longitudinal waves; and
- An ultrasonic display device (14) to display the interfacial echoes
generated by the transducer (8).

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2. The device as claimed in claim 1, wherein the buffer rod/sample holder (4)
comprises ceramic materials for example, Alumina AD 94 or Direct Sintered
Silicon Carbide SC-DS or Mo or W or Ti selectively chosen for high
temperature application upto 1450° C.
3. The device as claimed in claim 1, wherein the vertical tubular furnace can be
selected to have a dimensional relationship of H:ID:OD=5:1:4
Where,
H = Height, ID = Internal diameter, and OD = outside diameter.
4. The device as claimed in claim 1 or 3, wherein the buffer rod/sample holder
(4) is correspondingly configured to have a dimensional relationship of Length
(L) and diameter (D), for example, L = H, and D = 0.5 ID.
5. The device as claimed in claim 1, 3 or 4, wherein the port (6) of the buffer
rod/sample holder (4) is configured to have diameter (D1) and height (H1)
relationship as D1 = 0.6D, H1 = 0.2H.
6. The device as claimed in claim 1, wherein the box type furnace (1) can be
selected to have dimensional relationship between Length (L'), Width (W) and
Height (H1) at a ratio of 1:1:1.25.
7. The device as claimed in claim 1 or 6, wherein the buffer rod/sample holder
(4) is correspondingly configured to have a cross-section (CS) and Length
(L1) for example, L1= 0.75 W, and CS = 0.125 W x 0.125 W.

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8. The device as claimed in claim 6 or 7, wherein the port (6) of the buffer
rod/sample holder (4') is correspondingly configured to have a dimensional
ratio relationship of width (W') = 0.075W, Length (L") = 0.175L', height (H")
= 0.06 H'.
9. An improved device adaptable to furnaces, to measure viscosity, phase
transformation and crystallization in molten solids at temperatures up to
1450°C as substantially herein described with reference to the accompanying
drawings.

The improved ultrasonic device comprises of a melting unit, a buffer rod/sample holder, a cooling unit, and an ultrasonic testing system. The buffer rod/sample holder can be configured as a vertical rod with a port on the top to hold the sample positioned inside a vertical tubular furnace. A sample is kept in a port/chamber at top end of the buffer rod/sample holder, which can be inserted into the furnace from the bottom. The bottom end of the buffer rod/sample holder is water cooled at which the ultrasonic transducers are kept for ultrasonic measurements.

In an alternative embodiment, the sample will be inserted through a buffer rod with a port at its first end through the side walls of a box type or through one end of a horizontal tubular furnace. The second end accommodating transducers at which the ultrasonic measurements are to be taken will be water cooled.

Documents:

00237-kol-2007-correspondence-1.1.pdf

00237-kol-2007-correspondence-1.2.pdf

00237-kol-2007-form-1-1.1.pdf

00237-kol-2007-form-18.pdf

0237-kol-2007 abstract.pdf

0237-kol-2007 claims.pdf

0237-kol-2007 correspondence others.pdf

0237-kol-2007 description(complete).pdf

0237-kol-2007 drawings.pdf

0237-kol-2007 form-1.pdf

0237-kol-2007 form-2.pdf

0237-kol-2007 form-3.pdf

0237-kol-2007 form-5.pdf

237-KOL-2007-(30-03-2012)-ABSTRACT.pdf

237-KOL-2007-(30-03-2012)-AMANDED CLAIMS.pdf

237-KOL-2007-(30-03-2012)-AMANDED PAGES OF SPECIFICATION.pdf

237-KOL-2007-(30-03-2012)-DESCRIPTION (COMPLETE).pdf

237-KOL-2007-(30-03-2012)-DRAWINGS.pdf

237-KOL-2007-(30-03-2012)-EXAMINATION REPORT REPLY RECEIVED.pdf

237-KOL-2007-(30-03-2012)-FORM-1.pdf

237-KOL-2007-(30-03-2012)-FORM-2.pdf

237-KOL-2007-(30-03-2012)-OTHERS.pdf

237-KOL-2007-CORRESPONDENCE 1.1.pdf

237-KOL-2007-CORRESPONDENCE 1.2.pdf

237-KOL-2007-CORRESPONDENCE OTHERS 1.3.pdf

237-KOL-2007-EXAMINATION REPORT.pdf

237-KOL-2007-FORM 1-1.2.pdf

237-KOL-2007-FORM 18.pdf

237-KOL-2007-FORM 3.pdf

237-KOL-2007-GPA.pdf

237-KOL-2007-GRANTED-ABSTRACT.pdf

237-KOL-2007-GRANTED-CLAIMS.pdf

237-KOL-2007-GRANTED-DESCRIPTION (COMPLETE).pdf

237-KOL-2007-GRANTED-DRAWINGS.pdf

237-KOL-2007-GRANTED-FORM 1.pdf

237-KOL-2007-GRANTED-FORM 2.pdf

237-KOL-2007-GRANTED-LETTER PATENT.pdf

237-KOL-2007-GRANTED-SPECIFICATION.pdf

237-KOL-2007-OTHERS.pdf

237-KOL-2007-REPLY TO EXAMINATION REPORT.pdf

723-KOL-2007-CORRESPONDANCE OTHERS-1.1.pdf

723-KOL-2007-FORM 26.pdf


Patent Number 253383
Indian Patent Application Number 237/KOL/2007
PG Journal Number 29/2012
Publication Date 20-Jul-2012
Grant Date 17-Jul-2012
Date of Filing 15-Feb-2007
Name of Patentee TATA STEEL LIMITED
Applicant Address JAMSHEDPUR 831001
Inventors:
# Inventor's Name Inventor's Address
1 J.C.PANDEY TATA STEEL LIMITED, JAMSHEDPUR-831001
PCT International Classification Number G01N11/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA