CN111304735A - Cubic zirconium sapphire growth crystal furnace and cubic zirconium sapphire synthesis method - Google Patents
Cubic zirconium sapphire growth crystal furnace and cubic zirconium sapphire synthesis method Download PDFInfo
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- CN111304735A CN111304735A CN202010289411.2A CN202010289411A CN111304735A CN 111304735 A CN111304735 A CN 111304735A CN 202010289411 A CN202010289411 A CN 202010289411A CN 111304735 A CN111304735 A CN 111304735A
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- furnace body
- furnace
- sapphire
- cubic zirconium
- crystal
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- 239000013078 crystal Substances 0.000 title claims abstract description 49
- 239000010987 cubic zirconia Substances 0.000 title claims abstract description 26
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 25
- 239000010980 sapphire Substances 0.000 title claims abstract description 25
- 238000001308 synthesis method Methods 0.000 title description 4
- 230000006698 induction Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 15
- 239000010949 copper Substances 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000498 cooling water Substances 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- 239000003086 colorant Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000006872 improvement Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005674 electromagnetic induction Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000289 melt material Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- 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
Abstract
The invention discloses a cubic zirconium sapphire growth crystal furnace and a method for synthesizing cubic zirconium sapphire. The crystal furnace comprises a furnace body, wherein an induction copper pipe for heating is arranged outside the furnace body, and the ratio of the length to the width of the furnace body is greater than 1. By utilizing the induction frequency characteristic of the high-frequency current, the length of the furnace body is increased on the premise of not influencing the melting of the central crystal, and the volume of the furnace body is increased, so that the yield is increased.
Description
Technical Field
The invention relates to a growth crystal furnace for synthesizing cubic zirconium sapphire and a method for synthesizing sapphire by using the crystal furnace.
Background
The precious stone grade synthetic cubic zirconia is also called Sujiu diamond, homogeneous crystal, hardness up to 8.5, refractive index 2.17, temperature resistance of more than 2000 ℃, thus being widely applied to aerospace, optics, temperature resistant materials, jewelry and civil materials. In recent years, the market of domestic cubic zirconia crystal production is competitive, and the survival of the fittest is basically in a stable state. And the current production technology can be compared favorably with foreign production technologies, has competitiveness in both product yield and quality, and has considerable prospect.
At present, the main method for synthesizing the cubic zirconia crystal is a cold crucible method, and a circular high-frequency induction furnace is used all over the world. As shown in FIG. 1, the diameter of the induction furnace is generally 1m to 1.2m, then the raw material powder of the fused zirconium is fed, and the crystal growth is carried out by lifting the induction coil by a lifter by 3 mm to 12 mm. The reason why the diameter of the induction furnace in the prior art can only be 1.5m at most is that the larger the diameter is, the larger the center distance is, the more difficult the raw material positioned in the center is to melt, so that the crystal has poor transparency and quality and cannot meet the requirement.
The sapphire is produced by using the existing crystal furnace, the single furnace yield is low, single crystals are fewer, and the electricity cost is high. At present, the production process at home and abroad is almost the same, the bottleneck is basically reached, the center can not be melted and grown, and the method is also the main reason for limiting the development of enterprises for producing cubic zirconia crystals.
Disclosure of Invention
In view of the above, the invention provides a cubic zirconium sapphire growth crystal furnace and a cubic zirconium sapphire synthesis method, which utilize a flat furnace body to replace the existing round furnace body, thereby ensuring the melting of the central raw material of the furnace body, ensuring the crystal quality, and improving the yield on the premise of no change of heating power.
In order to solve the technical problems, the technical scheme of the invention is to adopt a cubic zirconium sapphire growth crystal furnace, which comprises a furnace body, wherein an induction copper pipe for heating is externally coated on the furnace body, and the ratio of the length to the width of the furnace body is more than 1. By utilizing the induction frequency characteristic of the high-frequency current, the length of the furnace body is increased on the premise of not influencing the melting of the central crystal, and the volume of the furnace body is increased, so that the yield is increased.
As an improvement, the ratio of the length to the width of the furnace body is 2.
As a further improvement, the width of the furnace body is 1-1.2 m, the length is 2-2.4 m, and the height is 0.8-1 m.
As another further improvement, the cross section of the furnace body is oblong.
As an improvement, the induction copper pipe is vertically arranged, and the bottom of the induction copper pipe is connected with a header chassis; and a cooling water inlet and a cooling water outlet are arranged on the header base plate. So that the pressure of the cooling water in each induction copper pipe is consistent, and the cooling effect is ensured.
As an improvement, the top surface of the header base plate is provided with a boss. The traditional furnace body chassis is designed in a plane, and during production, powder with the thickness of about 15-20 cm is used for bottoming so as to prevent pollutants from burning out the chassis and the chassis by a molten material at a high temperature; the base plate of the novel long circular furnace is convex in the middle and concave at the periphery, the convex base plate part increases the area of cooling water and enhances the cooling property, so that the technical procedure of powder material bottoming is not needed, and pollutants on the base plate can flow to the peripheral concave base plate along with the molten liquid, so that the internal quality of the upper crystals cannot be influenced.
The invention also provides a method for synthesizing cubic zirconium sapphire by using the crystal furnace, which comprises the following steps:
A. proportioning powder materials; uniformly mixing and stirring zirconium dioxide powder, yttrium oxide and a rare element colorant according to a proportion;
B. adding materials; filling the prepared powder and lump materials into the furnace body according to a proportion;
C. igniting; placing a plurality of carbon rods in the furnace body, wherein the carbon rods are placed into a shape consistent with the furnace body; starting up and igniting;
D. melting; increasing the heating power to 500-1200 KW;
E. pulling crystal; pulling crystal by adopting a pulling method;
F. taking crystals; and taking out the crystal after the temperature in the furnace body is reduced to the normal temperature.
Preferably, in step B, the ratio of powder to lump material is 1: 2.
Preferably, in the step C, the distance between the carbon rod and the furnace edge is 15-25 cm.
Preferably, in the step D, the melting time is 24-30 hours.
Preferably, in the step E, the lifting speed of the induction copper pipe is 5-15 mm/h.
The invention has the advantages that: the crystal furnace with the structure and the sapphire synthesis method with the steps utilize the flat furnace body to replace the existing round furnace body, and under the condition of constant power, the central melting of raw materials can be ensured, the crystal growth is good, and the capacity of the furnace body can be improved, so that the yield can be improved by about 2 times. The energy-saving effect is obvious, the power cost is greatly reduced, and the competitive advantage is obvious.
Drawings
FIG. 1 is a schematic structural view of a conventional crystal furnace.
FIG. 2 is a schematic view of the structure of a crystal growing furnace according to the present invention.
Fig. 3 is a cross-sectional view of the present invention.
The labels in the figure are: 1 furnace body, 2 induction copper pipes, 3 cooling water inlets, 4 cooling water outlets, 5 header base plates and 6 bosses.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following embodiments.
As shown in fig. 2 and 3, the invention provides a cubic zirconium sapphire growth crystal furnace, which comprises a furnace body 1, wherein an induction copper pipe 2 for heating is arranged outside the furnace body 1, the induction copper pipe 2 is vertically arranged, and the bottom of the induction copper pipe is connected with a header base plate 5; and a cooling water inlet 3 and a cooling water outlet 4 are arranged on the header base plate 5. The ratio of the length to the width of the furnace body 1 is greater than 1. Preferably, the ratio of the length to the width of the furnace body 1 is 2. Specifically, the width of the furnace body 1 is 1-1.2 m, the length is 2-2.4 m, and the height is 0.8-1 m.
The cross section of the furnace body 1 is oblong. The shape is an oval shape, and a shape formed by joining two semicircles and a rectangle. The diameter of the two semi-circles is equal to the short side of the rectangle.
The top surface of the header base plate 5 is provided with a boss 6. The shape of the boss 6 is consistent with that of the furnace body.
The invention also provides a method for synthesizing cubic zirconium sapphire by using the crystal furnace, which comprises the following steps:
A. proportioning powder materials; uniformly mixing and stirring zirconium dioxide powder, yttrium oxide and a rare element colorant according to a proportion;
B. adding materials; filling the prepared powder and the lump material into the furnace body according to the ratio of 1: 2;
C. igniting; placing a plurality of carbon rods in the furnace body, wherein the carbon rods are placed in a shape consistent with that of the furnace body, and the distance between the carbon rods and the furnace edge is 15-25 cm, namely the carbon rods are placed in a small long round shape; after the placement is finished, starting up and igniting;
D. melting; according to the size of the crystal furnace, the heating power is increased to 500-1200 KW; the melting time is 24-30 hours.
E. Pulling crystal; pulling crystal by adopting a pulling method; the lifting speed of the induction copper pipe is 5-15 mm/h.
F. Taking crystals; and taking out the crystal after the temperature in the furnace body is reduced to the normal temperature.
The distance between the ignition melting magnetic field of the traditional circular furnace and the peripheral electromagnetic induction coil is equal and far, so that in the melting process, the electric power and the process time can only be increased to slowly melt materials, the melting time is too long, the non-uniform melting temperature of powder in the furnace body can be influenced, the central melting material in the furnace cannot be well crystallized, polycrystal or broken crystal is generated, and the polycrystal or the broken crystal cannot be well crystallized into monocrystal; the distance between the ignition melting magnetic field of the novel long circular furnace and the peripheral electromagnetic induction coil is equal and short, so that the process time required by melting powder in the furnace body can be accelerated and shortened under the condition of equal power in the melting process, the time is saved, and the redundant energy consumption is reduced.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. The utility model provides a cubic zirconium sapphire growth crystal stove, includes the furnace body, the furnace body is enclosed by a plurality of response copper pipes that are used for the heating, its characterized in that: the ratio of the length to the width of the furnace body is greater than 1.
2. The cubic zirconium sapphire growth crystal furnace of claim 1, wherein: the ratio of the length to the width of the furnace body is 2.
3. The cubic zirconium sapphire growth crystal furnace of claim 1, wherein: the width of the furnace body is 1-1.2 m, the length is 2-2.4 m, and the height is 0.8-1 m.
4. The cubic zirconium sapphire growth crystal furnace of claim 1, wherein: the cross section of the furnace body is oblong.
5. The cubic zirconium sapphire growth crystal furnace of claim 1, wherein: the induction copper pipe is vertically arranged, and the bottom of the induction copper pipe is connected with the header chassis; and a cooling water inlet and a cooling water outlet are arranged on the header base plate.
6. The cubic zirconium sapphire growth crystal furnace of claim 5, wherein: the top surface of the header base plate is provided with a boss.
7. A method for synthesizing cubic zirconium sapphire by using the crystal furnace of any one of claims 1 to 5, characterized by comprising the steps of:
A. proportioning powder materials; uniformly mixing and stirring zirconium dioxide powder, yttrium oxide and a rare element colorant according to a proportion;
B. adding materials; filling the prepared powder and lump materials into the furnace body according to a proportion;
C. igniting; placing a plurality of carbon rods in the furnace body, wherein the carbon rods are placed into a shape consistent with the furnace body; starting up and igniting;
D. melting; increasing the heating power to 500-1200 KW;
E. pulling crystal; pulling crystal by adopting a pulling method;
F. taking crystals; and taking out the crystal after the temperature in the furnace body is reduced to the normal temperature.
8. The method of claim 7, wherein in step B, the ratio of powder to bulk is 1: 2.
9. The method for synthesizing cubic zirconium sapphire according to claim 7, wherein in the step C, the distance between the carbon rod and the furnace edge is 15-25 cm.
10. The method for synthesizing cubic zirconium sapphire according to claim 7, wherein in the step E, the lifting speed of the induction copper tube is 5-15 mm/h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010289411.2A CN111304735A (en) | 2020-04-14 | 2020-04-14 | Cubic zirconium sapphire growth crystal furnace and cubic zirconium sapphire synthesis method |
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| CN202010289411.2A CN111304735A (en) | 2020-04-14 | 2020-04-14 | Cubic zirconium sapphire growth crystal furnace and cubic zirconium sapphire synthesis method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517630A (en) * | 2004-04-08 | 2012-06-27 | 圣戈本陶瓷及塑料股份有限公司 | Single crystals and methods for fabricating same |
| CN203393260U (en) * | 2013-08-05 | 2014-01-15 | 劳云标 | Water cooling device |
| KR101358971B1 (en) * | 2012-09-06 | 2014-02-06 | (주)티피에스 | Sapphire single crystal growth furnace with zirconia powder typed heat |
| CN103806101A (en) * | 2012-11-15 | 2014-05-21 | 上海中电振华晶体技术有限公司 | Growth method and equipment of square sapphire crystal |
| CN212560511U (en) * | 2020-04-14 | 2021-02-19 | 四川省久宝晶体科技有限公司 | Cubic zirconium sapphire growth crystal furnace |
-
2020
- 2020-04-14 CN CN202010289411.2A patent/CN111304735A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517630A (en) * | 2004-04-08 | 2012-06-27 | 圣戈本陶瓷及塑料股份有限公司 | Single crystals and methods for fabricating same |
| KR101358971B1 (en) * | 2012-09-06 | 2014-02-06 | (주)티피에스 | Sapphire single crystal growth furnace with zirconia powder typed heat |
| CN103806101A (en) * | 2012-11-15 | 2014-05-21 | 上海中电振华晶体技术有限公司 | Growth method and equipment of square sapphire crystal |
| CN203393260U (en) * | 2013-08-05 | 2014-01-15 | 劳云标 | Water cooling device |
| CN212560511U (en) * | 2020-04-14 | 2021-02-19 | 四川省久宝晶体科技有限公司 | Cubic zirconium sapphire growth crystal furnace |
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