Title of Invention


Abstract In order to provide an invisible information mark on a facet of a diamond gemstone, a plasma resist is applied to the whole of the exposed surface of the gemstone, a layer of gold is applied to the facet in the region where the mark is to be formed, a selected zone .of the metal and resist layers is ablated by ultraviolet laser ablation to form a mask on the facet, an electrical connection is provided to the metal layer, and the facet is plasma etched through the mask in order to apply a mark of appropriate depth, the resist and metal layers subsequently being removed
Full Text

Marking Diamond
Background to the Invention
The present invention relates to a method of marking a surface of a diamond to produce a mark which is invisible to the naked eye, The mark may be any mark, but the invention is particularly though not exclusively directed to applying an information mark to the diamond. The diamond may be for instance an industrial diamond such as a wire-drawing die, though the invention is of particular interest in marking gemstone diamonds, for instance for applying a mark which is invisible to the naked eye or invisible to the eye using a xlO loupe, when the mark can be applied to a polished facet of the gemstone without detracting from its clarity or colour grade. When a loupe is used, the visibility is assessed under the internationally accepted conditions for clarity grading, i.e. using a lOx magnifying achromatic, aplanatic loupe under normal light, this being a white diffuse light, not a spot light. The marks can be used to uniquely identify the gemstone by a serial number or as a brand or quality mark In general, the mark should be capable of being viewed under suitable magnification and viewing conditions, and, if applied to a gemstone, should not detract from the value or appearance of the stone and should preferably not exhibit blackening, v
There is a detailed description of the nature of the marks that can be applied in
W 097/03 846, in which the marks are applied by irradiating a diamond gemstone with
ultraviolet laser radiation using a projection mask.
It is generally desirable to produce marks of improved resolution and to reduce the time required to apply the marks so that for instance serial numbers can be applied using an assembly or sequence of masks.

The Invention
According to the invention, a layer of resist is applied to the surface of the diamond, a selected zone of the resist layer is ablated to form a mask on the diamond surface, and the diamond surface is etched through the mask, wherein an electrically-conducting layer is applied to the resist layer, and an electrical connection is provided to the electrically-conducting layer to prevent charging during etching. The invention extends to a diamond whose surface has been marked by the method, and to apparatus for carrying out the method.
The preferred form of etching is plasma etching. For plasma etching, it is especially advantageous to have an electrically-conducting layer, for example metal, and provide an electrical connection to the layer, to prevent charging of the diamond, the resist can then be non-electrically-conducting. The layer of metal can for instance be a layer of gold, for instance about 0.1 microns thick. It need not be applied to the whole of the resist layer, only to a region sufficiently large to prevent charging during plasma etching The bilayer mask so formed may require different ablation conditions to a single layer, hut generally both layers are ablated substantially simultaneously It is found that the electrically-conducting layer effectively remains on the resist around the ablated zone, and thus prevents charging during plasma etching, whilst leaving the ablated zone clear of metal. The metal should have an ablation threshold no higher than that^pf the resist A metal such as gold cannot be used on its own as a resist because it does not give high enough resolution, ablating too readily and leaving poorly defined edges Furthermore, if a thicker layer of metal such as gold is used, there is a risk of the metal sputtering and redepositing in the ablated zone.
A completely dry technique can be used (with no chemical etching or stripping steps); although wet cleaning may be required after plasma etching in order to remove the mask, this is not a critical step requiring controlled conditions. The bilayer mask can provide greatly improved resolution (particularly in relation to the laser etching

technique disclosed in WO97/03846), and, in comparison with WO97/03846, requires a reduced pulse count if laser ablation is employed, for instance using about 20 pulses or fewer, say 10 pulses, rather than 500 pulses, making it practical to produce serial numbers with a sequence of masks, one for each number. The ablation could be performed using a mask projection technique, but can be performed by direct beam writing.
The resist can be any suitable resist, for instance a plastics (polymer) resist. The thickness of the resist layer may for instance be not less than about 0.5 micron and/or not more than about 1 micron
In general, it is preferred that the plasma etching should be to a depth of not less than labout 10 nm and/or not greater than about 70 nm, more preferably not less than about 20 nm and/or not greater than about 50 nm, a suitable value being about 30 nm.
As an alternative to plasma etching, the diamond exposed by the mask can be etched using a broad ion beam to convert it to graphite or other non-diamond carbon which may then be removed by, for example, acid cleaning.
A ijjjamond gemstone is mounted on a holder (or a plurality of diamond gemstones can be so mounted) A layer of non-conducting polymer plasma etch resist is applied to the exposed surface of the diamond, for instance by spin coating using e.g. a Novalac photoresist or by evaporation. The resist layer is 0.5 to 1 microns thick.
A layer of gold about 0 1 microns thick is deposited on the resist layer on at least part of the facet to be marked.

The resist and gold layers are patterned by laser ablation with about 10 pulses to leave a clean diamond surface. The laser wavelength is selected to give the best results with the chosen resist, shorter wavelengths permitting greater resolution than longer ones, 248 nm or other wavelengths may be used, but the preferred wavelength is 193 nm.
Using the holder, an electrical connection is made to the metal layer and the diamond is plasma etched in a standard manner, preferably under a partial pressure of oxygen. Zones of the facet not protected by the resist are etched to a depth of about 30 nm,
providing a clean etch with no evidence of blackening. The electrical connection to the
metal layer prevents charging.
The stone or stones is/are removed from the holder- The mask is removed by wet cleaning.
The apparatus used for the laser ablation can be similar to that shown in Figure 2 of WO 97/0.3846.
The present invention has been described above purely by way of example, and modifications can be made within the spirit of the invention. The invention also consists in any individual features described or implicit herein or any combination of any such features or any generalisation of any such features or combination.


1096-mas-1998- abstract.pdf

1096-mas-1998- claims duplicate.pdf

1096-mas-1998- claims original.pdf

1096-mas-1998- correspondence others.pdf

1096-mas-1998- correspondence po.pdf

1096-mas-1998- description complete duplicate.pdf

1096-mas-1998- description complete original.pdf

1096-mas-1998- form 1.pdf

1096-mas-1998- form 26.pdf

1096-mas-1998- form 3.pdf

1096-mas-1998- form 4.pdf

Patent Number 207791
Indian Patent Application Number 1096/MAS/1998
PG Journal Number 26/2007
Publication Date 29-Jun-2007
Grant Date 27-Jun-2007
Date of Filing 22-May-1998
Applicant Address AEULESTRASSE 5, 9490 VADUZ.
# Inventor's Name Inventor's Address
PCT International Classification Number B44C1/22
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 9710736.1 1997-05-23 U.K.