CN104562182B - Synthesis method of sapphire crystal - Google Patents
Synthesis method of sapphire crystal Download PDFInfo
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- CN104562182B CN104562182B CN201510048188.1A CN201510048188A CN104562182B CN 104562182 B CN104562182 B CN 104562182B CN 201510048188 A CN201510048188 A CN 201510048188A CN 104562182 B CN104562182 B CN 104562182B
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Abstract
The invention discloses a synthesis method of sapphire crystal. The synthesis method mainly comprises the following steps: powder preparation and crystal growth, namely adding ammonium ferric sulfate, ammonium hexafluorotitanate and zinc salt to deionized water to prepare a coloring agent solution; adding the coloring agent solution to aluminum ammonium sulfate powder; dewatering, roasting and sieving to prepare gamma-Al2O3 powder; and melting and crystallizing the powder to gradually grow through a flame fusion method, so as to form the crystal. The synthetic gemstone is blue, uniform and attractive in color, and relatively large in size in comparison with the size of the gemstone synthesized by a similar synthesis method; the yield reaches over 80%; and the quality is stable.
Description
Technical field
The present invention relates to a kind of synthetic method of sapphire crystal, belongs to artificial synthesized gem crystal technical field.
Background technology
For a long time flame melt method growing sapphire there is a problem of one it is serious be that crystal radially colours uneven, center color
It is shallow, edge color depth, the product for processing is unsightly, it is impossible to meets user's needs, and is also easy to overflow in growing, bursts,
Cause stock utilization low, yield rate is low, above-mentioned deficiency limits the commercial Application of synthetic sapphire.
During sapphire crystal crystalline growth, coloring principle be in colouring agent active matter titanium and ferrous iron with Ti4++Fe2+=
2Al3+Same valency isomorph form replace aluminium, i.e., two neighboring [AlO6] octahedra respectively by [TiO6] and [Fe2+O6] two
Octahedron is replaced and causes blueness, and can above-mentioned replacement process be smoothed out and oxyhydrogen flame atmosphere, Ti4+And Fe2+Content and other
Addition species and content are closely related.
The colouring agent active component that patent CN1362384A is prepared removes the oxide and titanyl compound of iron, also comprising manganese
The mixing of one or two and the above in the oxide of oxide, the oxide of cobalt, the oxide of nickel, the oxide of vanadium and copper
Thing, makes powder after mixing with alum, and then prepares sapphire using flame melt method, the sapphire small volume for obtaining, circle
Head diameter 18mm, half boule crystal lengths 55mm.
In flame melt method synthetic gem crystallization process, the metallic element of doping enters lattice, makes lattice structure change,
The problems such as uneven dopant profiles, crystal clarity and integrity degree are reduced, light transmittance declines easily is produced in melt condensation process,
Considerable influence is produced to crystal mass, therefore doped metallic elements species is more more more is unfavorable for synthesizing the gem crystal of high-quality, compels
Being essential will be improved to sapphire synthetic method.
The content of the invention
To solve the deficiencies in the prior art, it is an object of the invention to provide a kind of uniform coloring is attractive in appearance, high yield rate, matter
The synthetic method of the stable sapphire crystal of amount.
In order to realize above-mentioned target, the present invention is adopted the following technical scheme that：
A kind of synthetic method of sapphire crystal, comprises the steps：
S1, ammonium ferric sulfate, ammonium titanium fluoride and zinc salt are added in deionized water and stirred to fully dissolving, be made into colouring agent
The content of solution, wherein ammonium ferric sulfate is 0.04-0.09g/mL, and the content of ammonium titanium fluoride is 0.03-0.06g/mL；
S2, colourant solution is well mixed with alum powder, then processed 30- under the conditions of 250-300 DEG C
60 minutes, colourant solution was 18-20mL/Kg with the volume mass ratio of alum powder；
S3, by the material after dehydration under the conditions of 1050-1100 DEG C roasting 2-3 hours, make powder, then sieve
γ-Al2O3；
S4, the γ-Al that will be prepared2O35-12 hours are sintered in jewel sintering machine using flame melt method, sapphire, hydrogen is obtained
Oxygen flame temperature control is at 2010-2030 DEG C.
Preferably, aforementioned zinc salt is zinc sulfate or zinc acetate.
Specifically, when zinc salt is zinc sulfate, content of the zinc sulfate in colourant solution is 0.02-0.06g/mL；When
When zinc salt is zinc acetate, content of the zinc acetate in colourant solution is 0.02-0.07g/mL.
Preferably, in step S3, the sieve number adopted when sieving is 100-120 mesh.
It is highly preferred that purity >=99.99% of aforementioned alum powder.
More preferably, in step S4, in oxyhydrogen flame unstripped gas, hydrogen purity >=99.5%, oxygen purity >=99.5%.
It is further preferred that in step S4, sintering time is more than 8 hours.
The invention has benefit that：The present invention proposes a kind of synthetic method of sapphire crystal, and colouring agent is except containing master
Want coloring active matter iron oxide and titanyl compound, also containing a kind of oxide of zinc, Zn-ef ficiency be introduced for promote
Enter main coloring active matter uniform coloring.Doped metallic elements species of the present invention is less, to crystal perfection degree and crystal mass not
Profit affects less.Moreover, the strict control flame atmosphere of the present invention and colouring agent each component ratio, it is equal that synthesis obtains coloring
It is even it is attractive in appearance, burst less, high yield rate, stay-in-grade sapphire crystal.
Specific embodiment
Make specific introduction to the present invention below in conjunction with specific embodiment.
Embodiment 1
Ammonium ferric sulfate powder, ammonium titanium fluoride powder and sulfuric acid zinc powder are added in deionized water and stirred to fully dissolving, is made into
The content of colourant solution, wherein ammonium ferric sulfate is 0.05g/mL, and the content of ammonium titanium fluoride is 0.03g/mL, and zinc sulfate content is
0.03g/mL；Colourant solution is mixed with the alum powder of purity >=99.99% in ratio of the volume mass than 20mL/Kg
It is even, processed 30 minutes at 300 DEG C；Then, by the material after dehydration, roasting makes powder, mistake in 3 hours at 1050 DEG C
Sieve to obtain γ-Al2O3, sieve number is 120 mesh；Finally, the γ-Al that will be prepared2O3Sintered in jewel sintering machine using flame melt method
Sapphire is made within 8 hours, oxyhydrogen flame temperature control is at 2020 DEG C.The boule for obtaining does not ftracture, and stands intact, and entire body is in indigo plant
Color, melts impurity invariably, diameter 21mm, total length 79mm, and high yield rate is up to 81%.
Embodiment 2
Ammonium ferric sulfate powder, ammonium titanium fluoride powder and acetic acid zinc powder are added in deionized water and stirred to fully dissolving, is made into
The content of colourant solution, wherein ammonium ferric sulfate is 0.08g/mL, and the content of ammonium titanium fluoride is 0.04g/mL, and acetic acid Zn content is
0.03g/mL；Colourant solution is mixed with the alum powder of purity >=99.99% in ratio of the volume mass than 18mL/Kg
It is even, processed 30 minutes at 300 DEG C；Then, by the material after dehydration, roasting makes powder, mistake in 3 hours at 1050 DEG C
Sieve to obtain γ-Al2O3, sieve number is 120 mesh；Finally, the γ-Al that will be prepared2O3Sintered in jewel sintering machine using flame melt method
Sapphire is made within 10 hours, oxyhydrogen flame temperature control is at 2030 DEG C.The boule for obtaining does not ftracture, and stands intact, and entire body is in indigo plant
Color, melts impurity invariably, diameter 20mm, total length 78mm, and high yield rate is up to 80%.
Embodiment 3
Ammonium ferric sulfate powder, ammonium titanium fluoride powder and sulfuric acid zinc powder are added in deionized water and stirred to fully dissolving, is made into
The content of colourant solution, wherein ammonium ferric sulfate is 0.05g/mL, and the content of ammonium titanium fluoride is 0.06g/mL, and zinc sulfate content is
0.05g/mL；Colourant solution is mixed with the alum powder of purity >=99.99% in ratio of the volume mass than 19mL/Kg
It is even, processed 40 minutes at 250 DEG C；Then, by the material after dehydration, roasting makes powder, mistake in 2 hours at 1100 DEG C
Sieve to obtain γ-Al2O3, sieve number is 120 mesh；Finally, the γ-Al that will be prepared2O3Sintered in jewel sintering machine using flame melt method
Sapphire is made within 7 hours, oxyhydrogen flame temperature control is at 2020 DEG C.The boule for obtaining does not ftracture, and stands intact, and entire body is in indigo plant
Color, melts impurity invariably, diameter 21mm, total length 80mm, and high yield rate is up to 82%.
Embodiment 4
Ammonium ferric sulfate powder, ammonium titanium fluoride powder and acetic acid zinc powder are added in deionized water and stirred to fully dissolving, is made into
The content of colourant solution, wherein ammonium ferric sulfate is 0.07g/mL, and the content of ammonium titanium fluoride is 0.04g/mL, and acetic acid Zn content is
0.06g/mL；Colourant solution is mixed with the alum powder of purity >=99.99% in ratio of the volume mass than 18mL/Kg
It is even, processed 45 minutes at 250 DEG C；Then, by the material after dehydration, roasting makes powder, mistake in 3 hours at 1050 DEG C
Sieve to obtain γ-Al2O3, sieve number is 120 mesh；Finally, the γ-Al that will be prepared2O3Sintered in jewel sintering machine using flame melt method
Sapphire is made within 11 hours, oxyhydrogen flame temperature control is at 2020 DEG C.The boule for obtaining does not ftracture, and stands intact, and entire body is in indigo plant
Color, melts impurity invariably, diameter 21mm, total length 81mm, and high yield rate is up to 81%.
To sum up, the present invention on the basis of affecting crystal mass, passes through being added without the doped metallic elements of multiple types
Strict control flame atmosphere and colouring agent each component ratio, synthesis obtained uniform coloring it is attractive in appearance, without bursting, steady quality, body
The big sapphire crystal of product, and yield rate can reach more than 80%.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way for above-described embodiment, it is all to be obtained by the way of equivalent or equivalent transformation
Technical scheme, all falls within protection scope of the present invention.
Claims (7)
1. a kind of synthetic method of sapphire crystal, it is characterised in that comprise the steps：
S1, ammonium ferric sulfate, ammonium titanium fluoride and zinc salt are added in deionized water and stirred to fully dissolving, be made into colouring agent molten
The content of liquid, wherein ammonium ferric sulfate is 0.04-0.09g/mL, and the content of ammonium titanium fluoride is 0.03-0.06g/mL；
S2, colourant solution is well mixed with alum powder, then processed 30-60 point under the conditions of 250-300 DEG C
Clock, colourant solution is 18-20mL/Kg with the volume mass ratio of alum powder；
S3, by the material after dehydration under the conditions of 1050-1100 DEG C roasting 2-3 hours, make powder, then sieve γ-
Al2O3；
S4, the γ-Al that will be prepared2O35-12 hours are sintered in jewel sintering machine using flame melt method, sapphire, oxyhydrogen flame is obtained
Temperature control is at 2010-2030 DEG C.
2. the synthetic method of a kind of sapphire crystal according to claim 1, it is characterised in that the zinc salt is zinc sulfate
Or zinc acetate.
3. the synthetic method of a kind of sapphire crystal according to claim 2, it is characterised in that when zinc salt is zinc sulfate
When, content of the zinc sulfate in colourant solution is 0.02-0.06g/mL；When zinc salt is zinc acetate, zinc acetate is in colouring agent
Content in solution is 0.02-0.07g/mL.
4. the synthetic method of a kind of sapphire crystal according to claim 1, it is characterised in that in step S3, when sieving
The sieve number for adopting is 100-120 mesh.
5. the synthetic method of a kind of sapphire crystal according to claim 1, it is characterised in that the alum powder
Purity >=99.99%.
6. the synthetic method of a kind of sapphire crystal according to claim 1, it is characterised in that in step S4, oxyhydrogen flame
In unstripped gas, hydrogen purity >=99.5%, oxygen purity >=99.5%.
7. a kind of synthetic method of the sapphire crystal according to any one of claim 1-6, it is characterised in that step S4
In, sintering time is more than 8 hours.
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| CN106968011A (en) * | 2017-05-19 | 2017-07-21 | 四川晶蓝宝石科技发展有限公司 | Flame melt method polychrome jewel crystal growing furnace blanking device |
| CN107495561A (en) * | 2017-06-30 | 2017-12-22 | 秦斌 | One kind synthesis blue light noctilucence diamond and method |
Citations (5)
| 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 |
| CN101775661A (en) * | 2009-12-30 | 2010-07-14 | 鸿福晶体科技(安徽)有限公司 | Preparation method of sapphire doping agent |
| CN101941727A (en) * | 2010-09-14 | 2011-01-12 | 李振亚 | Method for producing aluminum oxide powder used as a raw material for producing sapphire crystals by flame melt process |
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61146794A (en) * | 1984-12-20 | 1986-07-04 | Toshiba Ceramics Co Ltd | Manufacture of single crystal alumina |
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Patent Citations (5)
| 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 |
| CN101775661A (en) * | 2009-12-30 | 2010-07-14 | 鸿福晶体科技(安徽)有限公司 | Preparation method of sapphire doping agent |
| CN101941727A (en) * | 2010-09-14 | 2011-01-12 | 李振亚 | Method for producing aluminum oxide powder used as a raw material for producing sapphire crystals by flame melt process |
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| 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 |
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Effective date of registration: 20180801 Address after: Room 1802, 1 floor, Torch Hotel, Changdi Torch Hotel, 259 Xihu District Wensanlu Road, Hangzhou, Zhejiang Patentee after: HANGZHOU ZHONGYI TECHNOLOGY CO., LTD. Address before: No. 85, river sea middle road, Xinbei District, Changzhou, Jiangsu Patentee before: CHANGZHOU YANJING TECHNOLOGY CO., LTD. |
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