CN100398703C - Method for growing high-performance tube type sapphire - Google Patents
Method for growing high-performance tube type sapphire Download PDFInfo
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- CN100398703C CN100398703C CNB2006100138017A CN200610013801A CN100398703C CN 100398703 C CN100398703 C CN 100398703C CN B2006100138017 A CNB2006100138017 A CN B2006100138017A CN 200610013801 A CN200610013801 A CN 200610013801A CN 100398703 C CN100398703 C CN 100398703C
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Abstract
The present invention discloses a method for growing high-performance tubular sapphire. In the method, one-step molding wetting EFG technology is utilized, and tubular sapphire of the required inner diameter and outer diameter sizes and lengths is directly drawn from flux. The present invention is characterized in that the specification size of the tubular sapphire is firstly determined, and a matching long tubular mould is manufactured according to the specification size; high-purity sapphire particles manufactured with the flame fusion method are secondly selected as raw material, and high quality seed crystal grown with the Czochralski method in the (0001) direction is selected to grow the tubular sapphire. The temperature difference in the transverse direction is within 2 DEG C; the temperature gradient in the longitudinal direction within 10MM from the end face of the mould is 3 DEG C to 4 DEG C; the growth rate is 30MM /h to 40MM /h. The method has the advantages that the high-performance tubular sapphire of the required inner diameter and outer diameter sizes and lengths can be directly obtained, and the difficulty and the waste of post machining of rod-like crystal is avoided. The type products can be applied to the high technological field of a plurality of industry, such as semiconductor, chemical industry, aviation, spaceflight, national defense, etc.
Description
Technical field
The invention relates to the growth method of jewel, particularly a kind of method for growing high-performance tube type sapphire.
Background technology
The high-performance tube sapphire, it is regular to have outward appearance, smooth surface, transparency is better, the characteristics that perfection of crystal is good, because the high-melting-point that had of sapphire crystal itself, high rigidity, corrosion-resistant, good a series of premium propertiess such as infrared transmittivity, this series products can be applicable to the high-tech area of conglomeraties such as semi-conductor, chemical industry, Aeronautics and Astronautics, national defence again.Method about the jewel of directly growing from melt is according to U.S. H.E.LaBelle, and the method for Jr. is carried out, and is called moistened guide mould process, i.e. the EFG method.United States Patent (USP) 3591348 discloses the method for growth white stone, and Chinese patent 85103282.6 discloses the method and the device of growing bar shaped ruby, and Chinese patent 90109706.3 discloses the method for preparation of star-light gem.Adopt above-mentioned disclosed method adding man-hour, operation is complicated, and yield rate is low, the final product quality weak effect.
Summary of the invention
The objective of the invention is in order to overcome the problem that above technology exists, a kind of method for growing high-performance tube type sapphire is provided, utilize one-time formed guided mode law technology, directly draw the tubulose sapphire of required inside and outside footpath size and length from melt, it is simple to reach operation, the yield rate height, outward appearance is regular, smooth surface, transparency is better, the purpose that perfection of crystal is good.
To achieve these goals, the technical solution used in the present invention is: a kind of method for growing high-performance tube type sapphire, adopt one-time formed wetting edge-defined technology, directly from melt, draw required in, the tubulose sapphire of outside dimension and length, it is characterized in that, at first determine the sapphire specification of tubulose, make the mould that is complementary according to above-mentioned specification, then, select for use high purity flame melt method sapphire particle as raw material, select for use Czochralski grown＜0001〉direction high-quality seed crystal, use the long tube mould, carry out the sapphire growth of tubulose, the warm field condition of crystal growth is wanted rationally, and laterally want evenly the temperature field, and transverse temperature difference is in 2 ℃, longitudinal temperature gradient is 3-4 ℃ in distance die face 10mm, and growth velocity is 30-40mm/h.
The tubulose sapphire of above-mentioned specification comprises external diameter φ 4mm-φ 30mm, wall thickness 1.5mm-3mm, and maximum length is 250mm.
Above-mentioned mould is selected high-quality forging and pressing molybdenum materials for use, and Design and Machining becomes with required crystal face shaping and size and is complementary, and has the round piped high precision long tube mould of capillary seam.
Beneficial effect of the present invention: be directly from melt, to draw out the high-performance tube sapphire, guarantee that its outward appearance is regular, smooth surface, transparency is better, the characteristics that perfection of crystal is good, and it utilizes one-time formed guided mode law technology, the direct tubulose sapphire that draws required inside and outside footpath size and length from melt, exempted because sapphire has high-melting-point, high rigidity, performance such as corrosion-resistant, and be difficult to by rhabdolith difficulty that postmenstruation, mechanical workout formed again and waste.Therefore, present method is the Perfected process of these type of special-shaped sapphire goods of growth, and it is simple to reach technology, and is easy to process, improves the purpose of finished product rate and quality product.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail: a kind of method for growing high-performance tube type sapphire, adopt one-time formed wetting edge-defined technology, directly from melt, draw required in, the tubulose sapphire of outside dimension and length, at first determine the sapphire specification of tubulose, for guaranteeing to grow fine tubulose sapphire crystal, so long tube mould that needs Design and Machining and required crystalline face shaping and size to be complementary, then, select for use high purity flame melt method sapphire particle as raw material, select for use Czochralski grown＜0001〉direction high-quality seed crystal, use the long tube mould, carry out the sapphire growth of tubulose, set up the warm field condition of rational crystal growth, reach uniform transverse temperature field, transverse temperature difference is in 2 ℃, and longitudinal temperature gradient is 3-4 ℃ in distance die face 10mm, and growth velocity is 30-40mm/h.
The tubulose sapphire of above-mentioned specification comprises external diameter φ 4mm-φ 30mm, wall thickness 1.5mm-3mm, and maximum length is 250mm.
Above-mentioned mould is selected high-quality forging and pressing molybdenum materials for use, and Design and Machining becomes with required crystal face shaping and size and is complementary, and has the round piped high precision long tube mould of capillary seam.
The invention will be further described below in conjunction with example: the device that adopts Chinese patent 85103282 growing bar shaped rubies, adopt cylindric molybdenum induction heating element, molybdenum crucible and molybdenum mould, according to the sapphire Dimensions of needed tubulose, as external diameter Φ 30mm, wall thickness 3mm and length 250mm, determine the apparent size of needed long tube mould, make the long tube mould that is complementary according to above-mentioned specification, mould is installed in the crucible, the high purity flame melt method sapphire particle of packing into an amount of in the crucible, with Czochralski grown＜0001〉direction high-quality seed crystal is installed on the molybdenum system anchor clamps, adjusts the position of crucible, guarantees that die tip and seed end align, then the single crystal growing furnace working spaces is vacuumized, charge into pure argon.After aforesaid operations is finished, begin energising, regulating power gradually heats up, the temperature at mould top should be controlled at about 2070 ℃, makes the sapphire particle fusing in the crucible, in the heating and heat-insulating device system that required tubulose sapphire is complementary, set up rational crystal growth temperature field condition, reach uniform transverse temperature field, transverse temperature difference is in 2 ℃, and longitudinal temperature gradient guarantees 3-4 ℃ in distance die face 10mm.Select growth velocity 30mm/h, crystal growing process continuously carries out, and till the melt in crucible is all run out of, grows required tubulose sapphire crystal.With the good tubulose sapphire blank of growing, through simple cutting and grinding, cut unnecessary body, polish the end face of body, just obtained needed high-quality tubulose sapphire goods.
High-performance tube sapphire by the present invention's growth, it is regular to have outward appearance, smooth surface, transparency is better, the characteristics that perfection of crystal is good, because the high-melting-point that had of sapphire crystal itself, high rigidity, corrosion-resistant, good a series of premium propertiess such as infrared transmittivity, this series products can be applicable to the high-tech area of conglomeraties such as semi-conductor, chemical industry, Aeronautics and Astronautics, national defence again.
Claims (3)
1. method for growing high-performance tube type sapphire, adopt one-time formed wetting edge-defined technology, directly from melt, draw required in, the tubulose sapphire of outside dimension and length, it is characterized in that, at first determine the sapphire specification of tubulose, make the mould that is complementary according to above-mentioned specification, then, select for use high purity flame melt method sapphire particle as raw material, select for use Czochralski grown＜0001〉direction high-quality seed crystal, use the long tube mould, carry out the sapphire growth of tubulose, the warm field condition of crystal growth is wanted rationally, laterally want evenly the temperature field, transverse temperature difference is in 2 ℃, and longitudinal temperature gradient is 3-4 ℃ in distance die face 10mm, and growth velocity is 30-40mm/h.
2. according to the described method for growing high-performance tube type sapphire of claim 1, it is characterized in that the tubulose sapphire of above-mentioned specification comprises external diameter φ 4mm-φ 30mm, wall thickness 1.5mm-3mm, maximum length is 250mm.
3. according to the described method for growing high-performance tube type sapphire of claim 1, it is characterized in that, above-mentioned mould is selected high-quality forging and pressing molybdenum materials for use, and Design and Machining becomes with required crystal face shaping and size and is complementary, and has the round piped high precision long tube mould of capillary seam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100138017A CN100398703C (en) | 2006-05-22 | 2006-05-22 | Method for growing high-performance tube type sapphire |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100138017A CN100398703C (en) | 2006-05-22 | 2006-05-22 | Method for growing high-performance tube type sapphire |
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| CN1884634A CN1884634A (en) | 2006-12-27 |
| CN100398703C true CN100398703C (en) | 2008-07-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2006100138017A Expired - Fee Related CN100398703C (en) | 2006-05-22 | 2006-05-22 | Method for growing high-performance tube type sapphire |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100575566C (en) * | 2007-12-28 | 2009-12-30 | 中国科学院上海光学精密机械研究所 | The method of growing method of carbon-doped sapphire crystal by EFG |
| CN101328604B (en) * | 2008-08-01 | 2011-06-22 | 成都东骏激光股份有限公司 | Manufacturing method of large size special-shaped thin wall molybdenum crucible and special hot pressing furnace |
| CN101857970B (en) * | 2010-04-16 | 2012-11-21 | 镇江市丹徒区黄墟润蓝晶体制造厂 | Growing method of large-size flaky sapphire crystals |
| CN102432268B (en) * | 2011-09-04 | 2012-12-05 | 湖北菲利华石英玻璃股份有限公司 | Method for sintering alumina powder into alumina lump material used for sapphire crystal production through flame fusion technique |
| 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 |
| CN103696005A (en) * | 2014-01-07 | 2014-04-02 | 镇江和和蓝晶科技有限公司 | Mold for simultaneous growth of multiple sapphire tubes through edge-defined film-fed growth technique |
| CN103710752A (en) * | 2014-01-07 | 2014-04-09 | 镇江和和蓝晶科技有限公司 | Die for growing large-diameter tubular sapphire with edge-defined film-fed growth process |
| CN103710753A (en) * | 2014-01-07 | 2014-04-09 | 镇江和和蓝晶科技有限公司 | Die for synchronously growing multiple thick-rod sapphires with edge-defined film-fed growth process |
| CN103726101B (en) * | 2014-01-20 | 2016-04-13 | 江苏苏博瑞光电设备科技有限公司 | A kind of ending method reducing EFG technique growth tubulose sapphire crystal cracking |
| CN104088011B (en) * | 2014-07-15 | 2017-01-18 | 牛玥 | Preparation method of sapphire micro-capillary and die used in preparation method |
| CN104532341B (en) * | 2014-12-15 | 2017-04-05 | 江苏苏博瑞光电设备科技有限公司 | The growing method of crucible structure and sapphire test tube for sapphire tube growth |
| CN107059114A (en) * | 2017-03-08 | 2017-08-18 | 同济大学 | The mould and method of a kind of EFG technique growth crystal optical fibre |
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| US3591348A (en) * | 1968-01-24 | 1971-07-06 | Tyco Laboratories Inc | Method of growing crystalline materials |
| CN1015651B (en) * | 1990-12-08 | 1992-02-26 | 天津市硅酸盐研究所 | Process for preparation of star-light gem |
| CN1061812A (en) * | 1990-11-27 | 1992-06-10 | 俞鹤庆 | Massive saphire growing technology |
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2006
- 2006-05-22 CN CNB2006100138017A patent/CN100398703C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3591348A (en) * | 1968-01-24 | 1971-07-06 | Tyco Laboratories Inc | Method of growing crystalline materials |
| CN1061812A (en) * | 1990-11-27 | 1992-06-10 | 俞鹤庆 | Massive saphire growing technology |
| CN1015651B (en) * | 1990-12-08 | 1992-02-26 | 天津市硅酸盐研究所 | Process for preparation of star-light gem |
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| 导模法生长76mm片状蓝宝石晶体. 郭洪石等.人工晶体学报，第3-4期. 1997 |
| 导模法生长76mm片状蓝宝石晶体. 郭洪石等.人工晶体学报，第3-4期. 1997 * |
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| CN1884634A (en) | 2006-12-27 |
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