CN102817072A - Preparation method of doping raw material used for growing gem single crystal through edge-defined film-fed growth method - Google Patents
Preparation method of doping raw material used for growing gem single crystal through edge-defined film-fed growth method Download PDFInfo
- Publication number
- CN102817072A CN102817072A CN2012102704503A CN201210270450A CN102817072A CN 102817072 A CN102817072 A CN 102817072A CN 2012102704503 A CN2012102704503 A CN 2012102704503A CN 201210270450 A CN201210270450 A CN 201210270450A CN 102817072 A CN102817072 A CN 102817072A
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- Prior art keywords
- preparation
- single crystal
- aluminium oxide
- high purity
- purity aluminium
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Links
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000013078 crystal Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002994 raw material Substances 0.000 title claims abstract description 15
- 238000005231 Edge Defined Film Fed Growth Methods 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000010437 gem Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002019 doping agent Substances 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 61
- 229910001751 gemstone Inorganic materials 0.000 claims description 22
- 239000011236 particulate material Substances 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 9
- 238000012216 screening Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 7
- 239000010979 ruby Substances 0.000 claims description 7
- 229910001750 ruby Inorganic materials 0.000 claims description 7
- 229910052594 sapphire Inorganic materials 0.000 claims description 7
- 239000010980 sapphire Substances 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 230000001788 irregular Effects 0.000 claims description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- FPFSGDXIBUDDKZ-UHFFFAOYSA-N 3-decyl-2-hydroxycyclopent-2-en-1-one Chemical compound CCCCCCCCCCC1=C(O)C(=O)CC1 FPFSGDXIBUDDKZ-UHFFFAOYSA-N 0.000 claims description 3
- JOSWYUNQBRPBDN-UHFFFAOYSA-P ammonium dichromate Chemical compound [NH4+].[NH4+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O JOSWYUNQBRPBDN-UHFFFAOYSA-P 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000009490 roller compaction Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000003086 colorant Substances 0.000 abstract description 7
- 239000008187 granular material Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 2
- 238000004040 coloring Methods 0.000 abstract 1
- 230000003628 erosive effect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of a doping raw material used for growing a gem single crystal through an edge-defined film-fed growth method. In the method, a quantitatively prepared doping agent is added into a porous high-purity aluminum oxide granular material, and then the mixture is used for growing the gem single crystal; and synthetic gems in different colors can be obtained by adjusting the formula and the volume of addition of the doping agent. The preparation method has the advantages of shortening the technical process, greatly reducing the cost, avoiding erosion of a colorant caused by a flame method production engineering and improving the coloring accuracy. With the adoption of the porous high-purity aluminum oxide granular material as a carrier of the colorant, the colorant can be sufficiently absorbed and adhered to opening gaps and surfaces of the particle material so that the error between the calculated volume of addition and the actual content of the colorant is greatly reduced.
Description
Technical field:
The present invention relates to colored gemstone single crystal growing field, relate in particular to a kind of preparation method who is used for the doped raw material of guided mode method growth jewel single crystal growing.
Background technology:
The corundum gem crystal has that intensity is hard, heat resistant and wear resistant is wiped; Corrosion resistance is strong, translucidus can, series of characteristics such as electrical insulation capability is good; Therefore as the important techniques crystalline material; Synthetic corundum class jewel has been widely used in a series of high-tech technical fields such as national defence, military affairs, scientific research, and number of applications is also arranged on civilian industry simultaneously.
And according to different performances and request for utilization, people add different tinting materials through various compound methods, to obtain the gem crystal of different colours, are applied to different fields.
The present invention relates to colored gemstone single crystal growing field, relate in particular to the method for preparing raw material of a kind of guided mode method growth red (or blue) jewel.The present invention is employed in to add the growth that doping agent carries out redness (or blue) jewel monocrystalline in the colourless white gem crystal growth raw material.
Summary of the invention:
The purpose of this invention is to provide a kind of preparation method who is used for the doped raw material of guided mode method growth jewel single crystal growing, cross the content of controlling various impurity and control crystal color.
Technical scheme of the present invention is following:
Be used for the preparation method of the doped raw material of guided mode method growth jewel single crystal growing, may further comprise the steps:
(1), the moulding of porous high purity aluminium oxide particulate material:
At first α phase high purity aluminium oxide powder and sticker A are mixed, said α phase high purity aluminium oxide powder consumption is the 0.5%-10% of sticker A; Adopt dry method rolling shaper roller-compaction then, obtain particulate material; Remove less than 1mm, greater than the particle of 5mm through vibratory screening apparatus at last, obtain the irregular particle shape blank of 1-5mm;
(2), the sintering of porous high purity aluminium oxide particulate material:
A: low temperature binder removal: irregular particle shape blank in the step (1) is packed in the corundum saggar, put into the binder removal stove, slowly rise to 800 ℃, constant temperature 2-5 hour;
B: high temperature sintering: the blank behind the binder removal is packed in the high temperature kiln, be warming up to 1450-1700 ℃, constant temperature 5-10 hour;
C: screening: disperse, screen through vibratory screening apparatus, obtain being of a size of 1-5mm, loose density 1.5-2.0g/cm
3Porous high purity aluminium oxide particulate material;
(3), the interpolation of doping agent:
A: the selection of tinting material: according to needed color of gemstones, select the tinting material kind, ruby is Cr
2O
3, sapphire is Fe
2O
3And TiO
2, addition is 0.01%-1%, adds in the elements such as Ca, Mg, V, Co, Mn one or more according to needed color category (redness, red-purple, orange red etc.) and shade again, addition is 0.01%-0.1%;
B: the configuration of tinting material: according to the tinting material proportioning of selecting, Cr
2O
3With the ammonium dichromate is preparation, Fe
2O
3And TiO
2With ferric ammonium sulfate and ammonium titanium fluoride is preparation, and load weighted preparation and tinting material are added stirring in the pure water, dissolving successively;
C: soak: the porous high purity aluminium oxide particulate material that the takes by weighing 1-3kg crucible of packing into, add the tinting material that configures of 1-5 L, covered particulate material, soak more than 24 hours at 30-50 ℃ of constant temperature;
D: calcining: in the warm kiln, rise to 500-1000 ℃ during crucible packed into, constant temperature 2-8 hour, promptly obtain being used for the doped raw material of guided mode method growth redness or blue gem single crystal growing according to the heating curve of setting.
Described sticker A is a type or several kinds in the materials such as paraffin, Vilaterm, Vestolen PP 7052, Z 150PH, o-phthalic acid dibutyl ester (DOP), dibutylester, Triple Pressed Stearic Acid.
Beneficial effect of the present invention:
1, compares with the complicated technology of traditional " it is raw material production guided mode method ruby sapphire that alumina powder doping → flame method is produced ruby sapphire → with the flame method jewel "; Aluminium oxide granule pellet after the doping directly is used for the guided mode method and produces ruby sapphire; Technical process is shortened, and cost reduces significantly, simultaneously; The tinting material of having avoided causing in the flame method production engineering is ablated, and has improved painted accuracy rate;
2, be the tinting material carrier with porous high purity aluminium oxide particulate material, be convenient to tinting material and fully adsorb and be attached to particulate material clearance gap and surface, significantly reduced the error that tinting material calculates addition and actual content;
3, adulterating method is simple, helps satisfying the tinting material configuration of different colours requirement, helps producing the ruby sapphire of many kinds.
Embodiment
Execute example 1: be used for the preparation method of the doped raw material of guided mode method growth jewel single crystal growing, may further comprise the steps:
(1), the moulding of porous high purity aluminium oxide particulate material:
At first α phase high purity aluminium oxide powder and sticker A are mixed, said α phase high purity aluminium oxide powder consumption is the 0.5%-10% of sticker A; Adopt dry method rolling shaper roller-compaction then, obtain particulate material; Remove less than 1mm, greater than the particle of 5mm through vibratory screening apparatus at last, obtain the irregular particle shape blank of 1-5mm;
(2), the sintering of porous high purity aluminium oxide particulate material:
A: low temperature binder removal: irregular particle shape blank in the step (1) is packed in the corundum saggar, put into the binder removal stove, slowly rise to 800 ℃, constant temperature 2-5 hour;
B: high temperature sintering: the blank behind the binder removal is packed in the high temperature kiln, be warming up to 1450-1700 ℃, constant temperature 5-10 hour;
C: screening: disperse, screen through vibratory screening apparatus, obtain being of a size of 1-5mm, loose density 1.5-2.0g/cm
3Porous high purity aluminium oxide particulate material;
(3), the interpolation of doping agent:
A: the selection of tinting material: according to needed color of gemstones, select the tinting material kind, ruby is Cr
2O
3, sapphire is Fe
2O
3And TiO
2, addition is 0.01%-1%, adds in the elements such as Ca, Mg, V, Co, Mn one or more according to needed color category (redness, red-purple, orange red etc.) and shade again, addition is 0.01%-0.1%;
B: the configuration of tinting material: according to the tinting material proportioning of selecting, Cr
2O
3With the ammonium dichromate is preparation, Fe
2O
3And TiO
2With ferric ammonium sulfate and ammonium titanium fluoride is preparation, and load weighted preparation and tinting material are added stirring in the pure water, dissolving successively;
C: soak: the porous high purity aluminium oxide particulate material that the takes by weighing 1-3kg crucible of packing into, add the tinting material that configures of 1-5 L, covered particulate material, soak more than 24 hours at 30-50 ℃ of constant temperature;
D: calcining: in the warm kiln, rise to 500-1000 ℃ during crucible packed into, constant temperature 2-8 hour, promptly obtain being used for the doped raw material of guided mode method growth redness or blue gem single crystal growing according to the heating curve of setting.
Described sticker A is a type or several kinds in the materials such as paraffin, Vilaterm, Vestolen PP 7052, Z 150PH, o-phthalic acid dibutyl ester (DOP), dibutylester, Triple Pressed Stearic Acid.
(4) product performance index
Claims (2)
1. preparation method who is used for the doped raw material of guided mode method growth jewel single crystal growing is characterized in that may further comprise the steps:
(1), the moulding of porous high purity aluminium oxide particulate material:
At first α phase high purity aluminium oxide powder and sticker A are mixed, said α phase high purity aluminium oxide powder consumption is the 0.5%-10% of sticker A; Adopt dry method rolling shaper roller-compaction then, obtain particulate material; Remove less than 1mm, greater than the particle of 5mm through vibratory screening apparatus at last, obtain the irregular particle shape blank of 1-5mm;
(2), the sintering of porous high purity aluminium oxide particulate material:
A: low temperature binder removal: irregular particle shape blank in the step (1) is packed in the corundum saggar, put into the binder removal stove, slowly rise to 800 ℃, constant temperature 2-5 hour;
B: high temperature sintering: the blank behind the binder removal is packed in the high temperature kiln, be warming up to 1450-1700 ℃, constant temperature 5-10 hour;
C: screening: disperse, screen through vibratory screening apparatus, obtain being of a size of 1-5mm, loose density 1.5-2.0g/cm
3Porous high purity aluminium oxide particulate material;
(3), the interpolation of doping agent:
A: the selection of tinting material: according to needed color of gemstones, select the tinting material kind, ruby is Cr
2O
3, sapphire is Fe
2O
3And TiO
2, addition is 0.01%-1%, adds in the elements such as Ca, Mg, V, Co, Mn one or more according to needed color category (redness, red-purple, orange red etc.) and shade again, addition is 0.01%-0.1%;
B: the configuration of tinting material: according to the tinting material proportioning of selecting, Cr
2O
3With the ammonium dichromate is preparation, Fe
2O
3And TiO
2With ferric ammonium sulfate and ammonium titanium fluoride is preparation, and load weighted preparation and tinting material are added stirring in the pure water, dissolving successively;
C: soak: the porous high purity aluminium oxide particulate material that the takes by weighing 1-3kg crucible of packing into, add the tinting material that configures of 1-5 L, covered particulate material, soak more than 24 hours at 30-50 ℃ of constant temperature;
D: calcining: in the warm kiln, rise to 500-1000 ℃ during crucible packed into, constant temperature 2-8 hour, promptly obtain being used for the doped raw material of guided mode method growth redness or blue gem single crystal growing according to the heating curve of setting.
2. the preparation method who is used for the doped raw material of guided mode method growth jewel single crystal growing according to claim 1, it is characterized in that: described sticker A is a type or several kinds in the materials such as paraffin, Vilaterm, Vestolen PP 7052, Z 150PH, o-phthalic acid dibutyl ester (DOP), dibutylester, Triple Pressed Stearic Acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210270450.3A CN102817072B (en) | 2012-07-30 | 2012-07-30 | A kind of preparation method of the doped raw material for the single crystal growing of EFG technique growth jewel |
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|---|---|---|---|
| CN201210270450.3A CN102817072B (en) | 2012-07-30 | 2012-07-30 | A kind of preparation method of the doped raw material for the single crystal growing of EFG technique growth jewel |
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| Publication Number | Publication Date |
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| CN102817072A true CN102817072A (en) | 2012-12-12 |
| CN102817072B CN102817072B (en) | 2015-09-09 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014856A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Ferric-titanium-doped sapphire wafer and preparation method thereof |
| CN103359763A (en) * | 2013-07-04 | 2013-10-23 | 鸿福晶体科技(安徽)有限公司 | Chemical preparation method for spherical hollow alumina powder for producing gemstone by using flame fusion method |
| CN104775155A (en) * | 2015-05-05 | 2015-07-15 | 山东天岳先进材料科技有限公司 | Growing method for colored alumina gem mono-crystal |
| CN104775157A (en) * | 2015-05-05 | 2015-07-15 | 山东天岳先进材料科技有限公司 | Alumina sapphire single crystal growth method |
| CN104790035A (en) * | 2015-05-05 | 2015-07-22 | 山东天岳先进材料科技有限公司 | Method for growing red aluminum oxide gemstone single crystal |
| CN106149053A (en) * | 2015-04-13 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal |
| CN107034514A (en) * | 2017-02-28 | 2017-08-11 | 梧州市东麟宝石机械有限公司 | A kind of excellent ruby preparation method of permeability |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362384A (en) * | 2002-01-11 | 2002-08-07 | 烟台北极星华晶宝石有限责任公司 | Synthetic saphire and its production process |
-
2012
- 2012-07-30 CN CN201210270450.3A patent/CN102817072B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362384A (en) * | 2002-01-11 | 2002-08-07 | 烟台北极星华晶宝石有限责任公司 | Synthetic saphire and its production process |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014856A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Ferric-titanium-doped sapphire wafer and preparation method thereof |
| CN103014856B (en) * | 2013-01-10 | 2015-11-04 | 苏州巍迩光电科技有限公司 | Mix ferrotitanium sapphire wafer and preparation method thereof |
| CN103359763A (en) * | 2013-07-04 | 2013-10-23 | 鸿福晶体科技(安徽)有限公司 | Chemical preparation method for spherical hollow alumina powder for producing gemstone by using flame fusion method |
| CN106149053A (en) * | 2015-04-13 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | A kind of method of EFG technique growth high sensitivity thermoluminescence carbon-doped sapphire crystal |
| CN104775155A (en) * | 2015-05-05 | 2015-07-15 | 山东天岳先进材料科技有限公司 | Growing method for colored alumina gem mono-crystal |
| CN104775157A (en) * | 2015-05-05 | 2015-07-15 | 山东天岳先进材料科技有限公司 | Alumina sapphire single crystal growth method |
| CN104790035A (en) * | 2015-05-05 | 2015-07-22 | 山东天岳先进材料科技有限公司 | Method for growing red aluminum oxide gemstone single crystal |
| CN104775157B (en) * | 2015-05-05 | 2017-11-14 | 山东天岳先进材料科技有限公司 | A kind of growing method of blue alumina jewel monocrystalline |
| CN107034514A (en) * | 2017-02-28 | 2017-08-11 | 梧州市东麟宝石机械有限公司 | A kind of excellent ruby preparation method of permeability |
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| Publication number | Publication date |
|---|---|
| CN102817072B (en) | 2015-09-09 |
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Inventor after: Wang Nan Inventor after: Zhao Qing Inventor after: Jia Jianguo Inventor before: Jia Jianguo Inventor before: Hu Gaohua Inventor before: Shi An |
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Free format text: CORRECT: INVENTOR; FROM: JIA JIANGUO HU GAOHUA SHI AN TO: WANG NAN ZHAO QING JIA JIANGUO |
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Effective date of registration: 20170717 Address after: Figure 028000 Town Industrial Park Tongliao city the Inner Mongolia Autonomous Region Muli Horqin district Patentee after: Bourne smile sapphire Co., Ltd. Address before: 237321 Jinzhai Economic Development Zone, Anhui, Lu'an Patentee before: Homford Crystal Technology (Anhui) Co., Ltd. |
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| CP01 | Change in the name or title of a patent holder |
Address after: Figure 028000 Town Industrial Park Tongliao city the Inner Mongolia Autonomous Region Muli Horqin district Patentee after: Tongliao Seiko Sapphire Co., Ltd. Address before: Figure 028000 Town Industrial Park Tongliao city the Inner Mongolia Autonomous Region Muli Horqin district Patentee before: Bourne smile sapphire Co., Ltd. |