CN109338467A - A kind of preparation method of coloring uniform color jewel - Google Patents
A kind of preparation method of coloring uniform color jewel Download PDFInfo
- Publication number
- CN109338467A CN109338467A CN201811283666.7A CN201811283666A CN109338467A CN 109338467 A CN109338467 A CN 109338467A CN 201811283666 A CN201811283666 A CN 201811283666A CN 109338467 A CN109338467 A CN 109338467A
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- CN
- China
- Prior art keywords
- seed crystal
- mold
- preparation
- molybdenum
- uniform color
- 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.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
Abstract
A kind of preparation method of coloring uniform color jewel, comprising steps of annular molybdenum, which is covered interior close packed, expires molybdenum filament or tungsten wire, with molybdenum ring top in same plane at the top of molybdenum filament or tungsten wire, it grinds and polishes the die top after assembling, mold and empty burning mold are cleaned, the mold after empty burn is placed in crucible center later；Select M to or C to seed crystal, seed crystal is fixed on seedholder, by colour jewel raw material be packed into molybdenum crucible, mold mouth blowing grain；Fire door is closed, vacuumizes, fills protection gas；Vacuumize and applying argon gas: heating melts mold mouth material grain；Seeding；Shouldering；Isodiametric growth；Room temperature is dropped to come out of the stove.A kind of preparation method of coloring uniform color jewel of the invention, the colour jewel chromogenic ion of preparation are evenly distributed on the inside of entire crystal, solve the problems, such as that the long color gem coloring of EFG technique is uneven.
Description
Technical field
The present invention relates to jewel production methods, and in particular to a kind of preparation method of coloring uniform color jewel.
Background technique
Sapphire (Al2O3) it is also known as white stone, it is the crystalline material that hardness is only second to diamond in the world, there is broadband
The better opticals such as permeability, high intensity, wear-resistant, corrosion-resistant, high temperature resistant, mechanics and thermal property, have been widely used in state
Anti-, science and technology and civil field.Artificial synthesized ethereal blue gem crystal is in the unglazed absorption of visible light wave segment limit, therefore crystal color
It is colourless, transparent.Sapphire crystal is adulterated, red, blue, yellow, green etc. can be showed according to the difference of doping colouring ions
Multiple color obtains colour jewel crystal, can be applied to the fields such as jewelry, detector, laser.Since sapphire hardness is high,
It is difficult to or processing cost is high, EFG technique growth colour jewel is generallyd use at present, because of the crystalline substance that EFG technique is grown
Shape significantly reduces the difficulty of processing close to the shape of target product, reduces the processing loss of precious materials, former material
Expect that utilization rate is high, but the artificial synthesized generally existing uneven color of colour jewel crystal, color are dim at present, color difference is big etc.
Problem, it is difficult to meet the requirement of application.As shown in Figure 1, the colour jewel surface staining of EFG technique growth, internal color is close to nothing
Color, this is because the chromogenic ion about 90% of doping is distributed in gem crystal surface, it is internal few.There is the reason of this phenomenon
It is that doping chromogenic ion concentration distribution is related in the feed mode of die surface with melt, for example pore or capillary are sewn on mould
The chromogenic ion at tool center, doping is mainly distributed on crystal edge, stitches and is fed if it is annular capillary, and the chromogenic ion of doping removes
Being distributed in crystal edge can also be distributed in germ nucleus.Furthermore the distribution for adulterating chromogenic ion is also related with pulling rate, works as pulling rate
When very fast, the chromogenic ion of 100mm/h or more, doping can be covered with entire crystals.
Summary of the invention
The purpose of the present invention is to provide a kind of uniform colour jewel preparation methods of coloring, to overcome the above-mentioned prior art
Existing defect.
For achieving the above object, technical scheme is as follows:
A kind of preparation method of coloring uniform color jewel, comprising steps of
S1: annular molybdenum, which is covered interior close packed, expires molybdenum filament or tungsten wire, and molybdenum filament or tungsten wire top and molybdenum ring top are same flat
Face is ground and is polished the die top after assembling, cleaning mold and empty burning mold, the mold after empty burn is placed in crucible later
The heart；
S2: select M to or C to seed crystal, seed crystal is fixed on seedholder, by colour jewel raw material be packed into molybdenum crucible,
Mold mouth blowing grain；
S3: closing fire door, opens mechanical pump and is vacuumized, vacuum degree closes vaccum-pumping equipment after reaching predetermined value, fills
Protect gas to standard atmospheric pressure；
S4: opening heating power supply, which is warming up to predetermined temperature, melts mold mouth material grain；
S5: turning down seed crystal after the material grain fusing of mold mouth, to seed crystal carry out it is roasting it is brilliant after carry out seeding, make seed crystal blocks with
Melt welding, and seed crystal is lifted upwards；
S6: the seed rod rate of pulling is adjusted to shouldering and limits speed, makes crystal along seed crystal among mold by shouldering
To outgrowth；
S7: after shouldering, carrying out isodiametric growth, improves pulling rate to predetermined speed；
S8: it pulls crystal break away from moulds and cools down, come out of the stove after dropping to room temperature.
Technical solution as a further improvement of that present invention, select M to or C to seed crystal, seed crystal is fixed on seedholder
On, 5kg~7kg colour jewel raw material is packed into molybdenum crucible, mold mouth blowing grain.
Technical solution as a further improvement of that present invention, the step S3 are specifically included: being closed fire door, opened mechanical pump
It is vacuumized, vacuum degree closes vaccum-pumping equipment when reaching 3Pa~10Pa, later applying argon gas to standard atmospheric pressure.
Technical solution as a further improvement of that present invention, the step S4 are specifically included: being opened heating power supply and be warming up to
2100 DEG C~2300 DEG C, melt mold mouth material grain.
Technical solution as a further improvement of that present invention, the step S5 are specifically included: when the material grain of mold mouth melts
Seed crystal is turned down afterwards, seeding is carried out after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt welding, and upwards with 5mm/h~20mm/
The speed of h lifts seed crystal.
Technical solution as a further improvement of that present invention, the speed that limits is 20mm/h~300mm/h.
Technical solution as a further improvement of that present invention, the step S7 are specifically included: after shouldering, being carried out isometrical
Growth improves pulling rate to 100mm/h~400mm/h.
Technical solution as a further improvement of that present invention, the step S8 are specifically included: being pulled crystal break away from moulds, opened
Begin to cool down, drops to room temperature after 10h and come out of the stove.
Compared with prior art, a kind of beneficial effects of the present invention: the preparation side of coloring uniform color jewel of the invention
Method, the colour jewel chromogenic ion of preparation are evenly distributed on the inside of entire crystal, solve the long color gem coloring of EFG technique not
Equal problem.
Detailed description of the invention
Fig. 1 is the color jewel doping chromogenic ion radial distribution figure of existing EFG technique growth；
Fig. 2 is the mold assembling schematic diagram in the embodiment of the present invention.
Specific embodiment:
Following embodiment further illustrates the contents of the present invention, but should not be construed as limiting the invention.Without departing substantially from
In the case where spirit of that invention and essence, to modifications or substitutions made by the method for the present invention, step, model of the invention is belonged to
It encloses.Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.
Embodiment
Fig. 2 show the mold of growth crystal, is the molybdenum set of molybdenum filament mold, molybdenum filament or tungsten wire close packed into annular.
The shape of annular molybdenum set is rectangle or square or circle, and the wall thickness of annular molybdenum set is 1~10mm.Molybdenum filament or tungsten wire are
The cylinder of strip, the material of the cylinder of strip are molybdenum, tungsten or tungsten-molybdenum alloy, preferably the diameter molybdenum that is 1~2mm
Stick.
The method for preparing colour jewel using above-mentioned molybdenum filament mold is as follows, comprising steps of
1) assembly mold:
As shown in Fig. 2, annular molybdenum, which is covered interior close packed, expires molybdenum filament or tungsten wire, exist at the top of molybdenum filament or tungsten wire at the top of molybdenum ring
Same plane grinds and polishes the die top after assembling, cleaning mold and empty burning mold；Mold after empty burn is placed in crucible
Center；
2) shove charge:
Select M to or C to seed crystal, seed crystal is fixed on seedholder, by 5kg~7kg colour jewel raw material be packed into molybdenum
Crucible, mold mouth blowing grain；
3) it vacuumizes and applying argon gas:
Fire door is closed, mechanical pump is opened and is vacuumized, vacuum degree closes vacuum equipment, argon filling when reaching 3Pa~10Pa
Gas is to standard atmospheric pressure；
4) it heats up:
It opens heating power supply and is warming up to 2100 DEG C~2300 DEG C, melt mold mouth material grain；
5) seeding:
Seed crystal is turned down after the fusing of the material grain of mold mouth, carries out seeding after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melts
Body welding, and seed crystal is lifted with 5mm/h~20mm/h upwards；
6) shouldering:
The seed rod rate of pulling is adjusted to shouldering and limits speed 20mm/h~300mm/h, makes crystal along seed by shouldering
Crystalline substance is among mold to outgrowth；
7) isodiametric growth:
After shouldering, isodiametric growth is carried out, improves pulling rate to 100mm/h~400mm/h；
8) cool down:
Crystal break away from moulds is pulled, makes its cooling, drops to room temperature after 10h and come out of the stove.
After measured, the colour jewel of above-mentioned preparation method production, chromogenic ion are evenly distributed on the inside of entire crystal, gram
The problem of the long color gem coloring unevenness of EFG technique is taken.
Claims (8)
1. a kind of preparation method of coloring uniform color jewel, which is characterized in that comprising steps of
S1: annular molybdenum, which is covered interior close packed, expires molybdenum filament or tungsten wire, and molybdenum filament or tungsten wire top and molybdenum ring top are ground in same plane
The die top after assembling, cleaning mold and empty burning mold are ground and polished, the mold after empty burn is placed in crucible center later；
S2: select M to or C to seed crystal, seed crystal is fixed on seedholder, by colour jewel raw material be packed into molybdenum crucible, mold
Mouth blowing grain；
S3: closing fire door, opens mechanical pump and is vacuumized, vacuum degree closes vaccum-pumping equipment after reaching predetermined value, fills protection
Gas is to standard atmospheric pressure；
S4: opening heating power supply, which is warming up to predetermined temperature, melts mold mouth material grain；
S5: seed crystal is turned down after the material grain fusing of mold mouth, seeding is carried out after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt
Welding, and seed crystal is lifted upwards；
S6: being adjusted to shouldering for the seed rod rate of pulling and limit speed, keeps crystal outside among mold along seed crystal by shouldering
Growth；
S7: after shouldering, carrying out isodiametric growth, improves pulling rate to predetermined speed；
S8: it pulls crystal break away from moulds and cools down, come out of the stove after dropping to room temperature.
2. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the step S2
Specifically include: select M to or C to seed crystal, seed crystal is fixed on seedholder, by 5kg~7kg colour jewel raw material be packed into molybdenum
Crucible, mold mouth blowing grain.
3. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the step S3
It specifically including: closing fire door, open mechanical pump and vacuumized, vacuum degree closes vaccum-pumping equipment when reaching 3Pa~10Pa, it
Applying argon gas is to standard atmospheric pressure afterwards.
4. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the step S4
It specifically includes: opening heating power supply and be warming up to 2100 DEG C~2300 DEG C, melt mold mouth material grain.
5. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the step S5
It specifically includes: seed crystal being turned down after the material grain fusing of mold mouth, seeding is carried out after carrying out roasting crystalline substance to seed crystal, makes seed crystal blocks and melt
Body welding, and seed crystal is lifted with the speed of 5mm/h~20mm/h upwards.
6. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the restriction speed
Degree is 20mm/h~300mm/h.
7. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the step S7
It specifically includes: after shouldering, carrying out isodiametric growth, improve pulling rate to 100mm/h~400mm/h.
8. a kind of preparation method of coloring uniform color jewel according to claim 1, which is characterized in that the step S8
It specifically includes: pulling crystal break away from moulds, start to cool down, drop to room temperature after 10h and come out of the stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811283666.7A CN109338467A (en) | 2018-10-31 | 2018-10-31 | A kind of preparation method of coloring uniform color jewel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811283666.7A CN109338467A (en) | 2018-10-31 | 2018-10-31 | A kind of preparation method of coloring uniform color jewel |
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| Publication Number | Publication Date |
|---|---|
| CN109338467A true CN109338467A (en) | 2019-02-15 |
Family
ID=65312656
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|---|---|---|---|
| CN201811283666.7A Pending CN109338467A (en) | 2018-10-31 | 2018-10-31 | A kind of preparation method of coloring uniform color jewel |
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Citations (9)
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|---|---|---|---|---|
| CN85103282A (en) * | 1985-04-29 | 1986-10-29 | 天津市硅酸盐研究所 | The method of growing bar shaped ruby and device thereof |
| US20090081456A1 (en) * | 2007-09-26 | 2009-03-26 | Amit Goyal | Faceted ceramic fibers, tapes or ribbons and epitaxial devices therefrom |
| CN101857970A (en) * | 2010-04-16 | 2010-10-13 | 镇江市丹徒区黄墟润蓝晶体制造厂 | Growing method of large-size flaky sapphire crystals |
| US20100282160A1 (en) * | 2004-04-08 | 2010-11-11 | Saint-Gobain Ceramics & Plastics, Inc. | Single crystals and methods for fabricating same |
| CN102534758A (en) * | 2012-01-20 | 2012-07-04 | 上海中电振华晶体技术有限公司 | Growth method and growth device for bar-shaped sapphire crystals |
| CN102560631A (en) * | 2012-01-20 | 2012-07-11 | 上海中电振华晶体技术有限公司 | Growth method and equipment of sapphire crystal |
| US20140017479A1 (en) * | 2007-11-21 | 2014-01-16 | Guilford L. Mack, III | Method of forming an r-plane sapphire crystal |
| CN104532342A (en) * | 2014-12-15 | 2015-04-22 | 江苏苏博瑞光电设备科技有限公司 | Growth method for growing micropore sapphire crystal through guided mode method |
| CN105568382A (en) * | 2015-12-31 | 2016-05-11 | 同济大学 | Uniformly colored sapphire crystal and preparation method thereof |
-
2018
- 2018-10-31 CN CN201811283666.7A patent/CN109338467A/en active Pending
Patent Citations (9)
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|---|---|---|---|---|
| CN85103282A (en) * | 1985-04-29 | 1986-10-29 | 天津市硅酸盐研究所 | The method of growing bar shaped ruby and device thereof |
| US20100282160A1 (en) * | 2004-04-08 | 2010-11-11 | Saint-Gobain Ceramics & Plastics, Inc. | Single crystals and methods for fabricating same |
| US20090081456A1 (en) * | 2007-09-26 | 2009-03-26 | Amit Goyal | Faceted ceramic fibers, tapes or ribbons and epitaxial devices therefrom |
| US20140017479A1 (en) * | 2007-11-21 | 2014-01-16 | Guilford L. Mack, III | Method of forming an r-plane sapphire crystal |
| CN101857970A (en) * | 2010-04-16 | 2010-10-13 | 镇江市丹徒区黄墟润蓝晶体制造厂 | Growing method of large-size flaky sapphire crystals |
| CN102534758A (en) * | 2012-01-20 | 2012-07-04 | 上海中电振华晶体技术有限公司 | Growth method and growth device for bar-shaped sapphire crystals |
| CN102560631A (en) * | 2012-01-20 | 2012-07-11 | 上海中电振华晶体技术有限公司 | Growth method and equipment of sapphire crystal |
| CN104532342A (en) * | 2014-12-15 | 2015-04-22 | 江苏苏博瑞光电设备科技有限公司 | Growth method for growing micropore sapphire crystal through guided mode method |
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Application publication date: 20190215 |