EP1042132B1 - Diamond or gemstone marking by plurality of grooves - Google Patents

Diamond or gemstone marking by plurality of grooves Download PDF

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Publication number
EP1042132B1
EP1042132B1 EP98962614A EP98962614A EP1042132B1 EP 1042132 B1 EP1042132 B1 EP 1042132B1 EP 98962614 A EP98962614 A EP 98962614A EP 98962614 A EP98962614 A EP 98962614A EP 1042132 B1 EP1042132 B1 EP 1042132B1
Authority
EP
European Patent Office
Prior art keywords
mark
grooves
gemstone
diamond
ion beam
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98962614A
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German (de)
English (en)
French (fr)
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EP1042132A1 (en
Inventor
James Gordon Charters Smith
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gersan Ets
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Gersan Ets
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Application filed by Gersan Ets filed Critical Gersan Ets
Publication of EP1042132A1 publication Critical patent/EP1042132A1/en
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Publication of EP1042132B1 publication Critical patent/EP1042132B1/en
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Expired - Lifetime legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B44DECORATIVE ARTS
    • B44BMACHINES, APPARATUS OR TOOLS FOR ARTISTIC WORK, e.g. FOR SCULPTURING, GUILLOCHING, CARVING, BRANDING, INLAYING
    • B44B7/00Machines, apparatus or hand tools for branding, e.g. using radiant energy such as laser beams
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B44DECORATIVE ARTS
    • B44BMACHINES, APPARATUS OR TOOLS FOR ARTISTIC WORK, e.g. FOR SCULPTURING, GUILLOCHING, CARVING, BRANDING, INLAYING
    • B44B3/00Artist's machines or apparatus equipped with tools or work holders moving or able to be controlled substantially two- dimensionally for carving, engraving, or guilloching shallow ornamenting or markings
    • B44B3/04Artist's machines or apparatus equipped with tools or work holders moving or able to be controlled substantially two- dimensionally for carving, engraving, or guilloching shallow ornamenting or markings wherein non-plane surfaces are worked
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B44DECORATIVE ARTS
    • B44BMACHINES, APPARATUS OR TOOLS FOR ARTISTIC WORK, e.g. FOR SCULPTURING, GUILLOCHING, CARVING, BRANDING, INLAYING
    • B44B2700/00Machines, apparatus, tools or accessories for artistic work
    • B44B2700/08Machines, apparatus or hand tools for branding

Definitions

  • the present invention relates to a method and apparatus for forming a mark on a surface of a diamond or gemstone, which mark comprises one or more unitary indicia.
  • the mark may be any mark, but the invention is particularly but not exclusively directed to applying an information mark to the diamond and the indicia can be alphanumeric characters or the like.
  • 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, and especially for applying a mark which is invisible to the naked eye or invisible to the eye using a x10 loupe (which is the loupe used by jewellers), when the mark can be applied to a polished facet of the gemstone without detracting from its clarity grade.
  • the marks can be used to uniquely identify the gemstone by a serial number or as a brand or quality mark, but it should not detract from the value or appearance of the stone, and should preferably not exhibit blackening.
  • EP 0 648 445 discloses a method of forming a mark on a surface of a diamond or gemstone, comprising the step of forming a plurality of grooves on said surface of the diamond or gemstone, which grooves define the mark, the grooves producing a visible diffraction effect under certain lighting and magnification conditions. Said grooves cover the whole of a facet and the intention is to increase the beauty of the material by producing an effect which is clearly visible to the naked eye. There is no suggestion of the grooves serving any other purpose.
  • US 4 425 769 discloses creating an identifying mark on a diamond or other gemstone, but there is no suggestion of forming grooves to create a diffraction effect.
  • US 4 467 172 and WO 97/03846 disclose putting an identifying mark on a diamond, but there is no suggestion of forming grooves to create a diffraction effect.
  • US 4 639 301 discloses a focussed ion beam machine for repairing optical and ion masks and X-ray lithography masks and reticules. There is no suggestion of applying marks to a diamond or gemstone and no suggestion of forming grooves to create a diffraction effect.
  • the present invention provides methods as set forth in claim 1, 2 or 19.
  • each groove is not less than about 10 nm deep and/or not more than about 50 nm deep with no evidence of blackening. A specific example would be around 30 nm.
  • the grooves may be in the form of parallel lines which can be elongate and substantially equally spaced a part, or even a plurality of intersecting grooves forming cross-hatched pattern, depending on the effect desired.
  • marking can be carried out using any suitable means, e.g. etching with an excimer laser or plasma etching, marking is preferably carried out using an ion beam, and most preferably by direct writing on the diamond surface with a focused ion beam.
  • etching with an excimer laser or plasma etching marking is preferably carried out using an ion beam, and most preferably by direct writing on the diamond surface with a focused ion beam.
  • ion beam By limiting the dose, sputtering of carbon atoms can be avoided, sputtering causing direct material removal; this enables a mark to be applied with a controlled depth and good resolution.
  • Gallium ions are used, but a beam of other suitable ions may alternatively be used.
  • the incident ions cause disordering that converts the diamond to a graphite-like or other non-diamond structure that can be cleaned using, for example, a powerful oxidizing agent, such as molten potassium nitrate, at a temperature of approximately 380-550 Centigrade for a period of between a few minutes and several hours.
  • a powerful oxidizing agent such as molten potassium nitrate
  • potassium nitrate has been found to be more effective in removing disordered diamond than other known processes, thus allowing a mark of a given depth to be produced with a relatively low dose of ions.
  • Suitable oxidising agents may be molten compounds such as alkali metal salts; compounds in the form XnYm where the group X may be Li + , Na + , K + , Rb + , Cs + or other cation, and the group Y may be OH - , NO 3 - , O 2 2- , O 2- , CO 3 2- or other anion, the integers n and m being used to maintain charge balance. Mixtures of such compounds may be used. Air or other oxygen-containing gases may also be present.
  • the disordered layer of the diamond can be removed using an acid or potassium nitrate dissolved in acid.
  • an acid or potassium nitrate dissolved in acid for example, molten potassium nitrate eliminates acid fumes.
  • the need to dispose of spent acid is eliminated, thereby offering safety, environmental and economic benefits.
  • the depth of disordering is determined by the range of ions. For 50 keV Gallium, this range is about 30 nm.
  • the minimum dose may be around 10 13 / cm 2 and is preferably about 10 14 /cm 2 to 10 15 /cm 2 , but good marks can be applied with a fairly modest dose, the preferred maximum dose being about 10 16 /cm 2 or even up to about 10 17 /cm 2 . However, the dose depends upon the ions being used and their energy (as measured in keV).
  • the ion beam dose is a total number of incident ions per unit area at the sample surface, during the marking.
  • the beam current may be about 0.5 nA, and the beam energy not less than about 10 keV or about 30 keV and/or not greater than about 100 keV or about 50 keV.
  • the region to be marked and/or the surrounding area may be coated with an electrically conducting layer, for instance gold, prior to forming the mark, so that an electrical connection can be provided before marking with an ion beam, to prevent charging.
  • the thickness of the gold, or other coating alters the variation of depth of the mark with beam energy and may thus be chosen to optimise the mark produced.
  • the accuracy of the method is such that no masking is required: the ion beam is applied directly to the surface of the diamond at the positions where the grooves are required to be formed.
  • the ion beam is applied directly to the surface of the diamond at the positions where the grooves are required to be formed.
  • the mark When the mark has been formed on the surface of the diamond or gemstone, it can be viewed as set forth in claim 19.
  • the mark is preferably viewed against a dark background, ie. it is preferred that the illuminating light is substantially prevented from reflecting through the stone and appearing directly behind or close to the mark. It will be apparent to a person skilled in the art that, in order to achieve this, the angle and direction from which the illuminating light is supplied (and hence the orientation and spacing of the lines) must be chosen so as to ensure that no light can follow the undesired path.
  • the typical range of magnification required to view the mark is x10 to x50.
  • d.sin ⁇ ⁇ n. ⁇
  • d is the distance between each groove
  • is the angle of the incident light
  • is the wavelength of the diffracted light
  • n is an integer.
  • n 1.
  • d and n are fixed, and the wavelength of diffracted light, i.e. the colour which the mark will appear when viewed, can be varied by varying the angle of incident light.
  • the angle of the incident light i.e. ⁇
  • is set so that ⁇ is around 450nm, using the above equation.
  • is set so that ⁇ is around 620nm.
  • a diamond gemstone is mounted in a suitable holder and placed in a vacuum chamber equipped with a focused ion beam source such as supplied by FEI or Micrion.
  • a focused ion beam source such as supplied by FEI or Micrion.
  • the region to be marked may be irradiated using an electron flood gun supplied by Micrion, providing a low energy, e.g. 1-100 eV, source of electrons, to prevent the diamond from becoming charged.
  • the sample is removed from the vacuum chamber, placed in a stainless steel crucible, and covered with a powerful oxidising agent, such as molten potassium nitrate, for a period of around one to two hours.
  • a powerful oxidising agent such as molten potassium nitrate
  • the sample is subsequently cooled and removed from the potassium nitrate before being cleaned using water and ethanol, thereby removing the portions of the diamond surface which have been disordered by the ion beam, and leaving a series of closely spaced grooves each around 30 - 35 nm deep, with no evidence of blackening.
  • the exposed region Upon examination before cleaning, the exposed region is identifiable by its graphite-like appearance when examined, for example, in a reflected light microscope. Such a mark would not be acceptable to a diamond grader, in that it would substantially reduce the clarity grade of the diamond. However, after cleaning using the powerful oxidising agent, the mark is not easily visible in a microscope, with no contrast between the mark and surrounding areas. The mark only becomes visible when illuminated by preferably two directional light sources at an angle which corresponds to the angle of diffracted light of a particular wavelength, for example blue light, at which time the mark appears blue. Such a mark is acceptable to a diamond grader in that it does not detrimentally affect the clarity grade of the diamond.
  • the closely spaced grooves are preferably formed within an 'invisible outline' of an alphanumeric character or the like, as shown in Figure 1 of the drawings.
  • the marked diamond 104 is placed on the viewing surface 100 of a conventional microscope 102.
  • the diamond 104 is illuminated by two directional light sources 106 having an angle ⁇ relative to the vertical axis Y.
  • is chosen so that the mark appears to be, for example, blue or red, as desired.
  • the directional light sources may be provided by a generally ring-shaped illuminator, all but two diametrically opposite portions thereof being masked off.
  • a conventional microscope may include illumination means comprising a circular ring-shaped source comprising optical fibres illuminated by a remote tungsten light bulb.
  • any suitable light source may be used to produce the same effect.
  • the directional sources may comprise a light source and an opaque screen located in the incident light path, the screen having two apertures formed therein, the apertures being formed on either side of a generally central position such that two angular directional light sources are produced.

Landscapes

  • Adornments (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Investigating Materials By The Use Of Optical Means Adapted For Particular Applications (AREA)
  • Welding Or Cutting Using Electron Beams (AREA)
EP98962614A 1997-12-24 1998-12-23 Diamond or gemstone marking by plurality of grooves Expired - Lifetime EP1042132B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB9727364 1997-12-24
GBGB9727364.3A GB9727364D0 (en) 1997-12-24 1997-12-24 Watermark
PCT/GB1998/003889 WO1999033671A1 (en) 1997-12-24 1998-12-23 Diamond or gemstone marking by plurality of grooves

Publications (2)

Publication Number Publication Date
EP1042132A1 EP1042132A1 (en) 2000-10-11
EP1042132B1 true EP1042132B1 (en) 2003-12-03

Family

ID=10824244

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98962614A Expired - Lifetime EP1042132B1 (en) 1997-12-24 1998-12-23 Diamond or gemstone marking by plurality of grooves

Country Status (15)

Country Link
EP (1) EP1042132B1 (ru)
JP (2) JP4497720B2 (ru)
KR (1) KR100501089B1 (ru)
CN (1) CN1146506C (ru)
AU (1) AU746557B2 (ru)
CA (1) CA2316957C (ru)
DE (1) DE69820295T2 (ru)
ES (1) ES2212385T3 (ru)
GB (2) GB9727364D0 (ru)
HK (1) HK1020032A1 (ru)
IL (1) IL136967A0 (ru)
RU (1) RU2215659C2 (ru)
TW (1) TW458836B (ru)
WO (1) WO1999033671A1 (ru)
ZA (1) ZA9811838B (ru)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3810548A4 (en) * 2018-06-25 2022-03-16 IIA Technologies Pte. Ltd. DIAMOND HAVING NANOSTRUCTURES ON ONE OF ITS SURFACES TO GENERATE STRUCTURAL COLORS AND ITS PRODUCTION METHOD

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2357737A (en) * 1999-12-27 2001-07-04 Yasuhira Mori Digitally marking a gemstone using a laser
CN1258734C (zh) * 2001-04-26 2006-06-07 维灵马可公司 产生和可视化视觉不可见的标记的方法
GB2424903B (en) * 2003-12-12 2008-06-25 Element Six Ltd Method of incorporating a mark in cvd diamond
WO2007067696A1 (en) 2005-12-06 2007-06-14 California Institute Of Technology Enhancing the optical characteristics of a gemstone
US8069688B2 (en) 2006-12-06 2011-12-06 California Institute Of Technology Gemstones and methods for controlling the appearance thereof
RU2427041C2 (ru) * 2009-05-08 2011-08-20 Юрий Константинович Низиенко Способ формирования идентификационной метки для маркировки ценных изделий и ценное изделие с ее использованием
RU2426487C2 (ru) * 2009-05-08 2011-08-20 Юрий Константинович Низиенко Идентификационная метка для маркировки ценных изделий и ценное изделие с ее использованием
RU2427908C1 (ru) 2010-03-29 2011-08-27 Юрий Константинович Низиенко Способ детектирования визуально невидимой идентификационной метки на поверхности ценного изделия, способ его позиционирования в процессе детектирования и детектор для реализации процесса
US20140312017A1 (en) 2011-07-27 2014-10-23 Alexander Potemkin Method For Applying a Data Marking to the Surface of a Diamond or Brilliant and For Determining the Authenticity Thereof
WO2013152155A1 (en) * 2012-04-04 2013-10-10 Merenfeld Miriam Reflective surface having a computer readable code
WO2014190801A1 (en) * 2013-05-30 2014-12-04 Goldway Technology Limited Method of marking material and system therefore, and material marked according to same method
MY175647A (en) * 2013-10-11 2020-07-03 Chow Tai Fook Jewellery Co Ltd Method of providing markings to precious stones including gemstones and diamonds, and markings and marked precious stones marked according to such a method
HK1198858A2 (en) 2014-04-16 2015-06-12 Master Dynamic Ltd Method of marking a solid state material, and solid state materials marked according to such a method
CH713538B1 (de) * 2017-03-02 2020-12-30 Guebelin Gem Lab Ltd Verfahren zum Rückverfolgbarmachen eines Schmucksteins.
US20210146716A1 (en) * 2018-02-23 2021-05-20 Master Dynamic Limited Method of marking a solid-state material, markings formed from such methods and solid-state materials marked according to such a method
EP3712717A1 (fr) * 2019-03-19 2020-09-23 Comadur S.A. Methode pour marquer une glace de montre en saphir
RU2720100C1 (ru) * 2019-03-26 2020-04-24 Акционерная Компания "АЛРОСА" (публичное акционерное общество) (АК "АЛРОСА" (ПАО)) Способ создания и детектирования оптически проницаемого изображения внутри алмаза и системы для детектирования (варианты)
CN111983804A (zh) * 2020-08-27 2020-11-24 蔡汉荣 一种金属表面及利用金属表面加工形成反射式投影成像的方法

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JPS56108712U (ru) * 1980-01-24 1981-08-24
EP0064780A1 (fr) * 1981-05-07 1982-11-17 Maurice Hakoune Procédé de traitement d'une pierre précieuse et pierre précieuse ainsi traitée
US4467172A (en) * 1983-01-03 1984-08-21 Jerry Ehrenwald Method and apparatus for laser engraving diamonds with permanent identification markings
US4639301B2 (en) * 1985-04-24 1999-05-04 Micrion Corp Focused ion beam processing
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3810548A4 (en) * 2018-06-25 2022-03-16 IIA Technologies Pte. Ltd. DIAMOND HAVING NANOSTRUCTURES ON ONE OF ITS SURFACES TO GENERATE STRUCTURAL COLORS AND ITS PRODUCTION METHOD

Also Published As

Publication number Publication date
GB2332651A (en) 1999-06-30
GB9727364D0 (en) 1998-02-25
AU1774399A (en) 1999-07-19
TW458836B (en) 2001-10-11
GB9828393D0 (en) 1999-02-17
RU2215659C2 (ru) 2003-11-10
JP2001526996A (ja) 2001-12-25
DE69820295T2 (de) 2004-10-21
KR100501089B1 (ko) 2005-07-18
KR20010040311A (ko) 2001-05-15
CN1284916A (zh) 2001-02-21
JP4497720B2 (ja) 2010-07-07
CA2316957A1 (en) 1999-07-08
DE69820295D1 (de) 2004-01-15
JP2009285733A (ja) 2009-12-10
CA2316957C (en) 2004-04-27
EP1042132A1 (en) 2000-10-11
GB2332651B (en) 2001-11-07
CN1146506C (zh) 2004-04-21
IL136967A0 (en) 2001-06-14
ZA9811838B (en) 2000-06-23
HK1020032A1 (en) 2000-03-10
AU746557B2 (en) 2002-05-02
WO1999033671A1 (en) 1999-07-08
ES2212385T3 (es) 2004-07-16

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