CN103451729A - Growth method of square sapphire - Google Patents
Growth method of square sapphire Download PDFInfo
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- CN103451729A CN103451729A CN2013104244246A CN201310424424A CN103451729A CN 103451729 A CN103451729 A CN 103451729A CN 2013104244246 A CN2013104244246 A CN 2013104244246A CN 201310424424 A CN201310424424 A CN 201310424424A CN 103451729 A CN103451729 A CN 103451729A
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Abstract
The embodiment of the invention provides a growth method of a square sapphire, and relates to the field of gem manufacturing. According to the method, bubbles formed on the upper parts of crystals in a preparation process are reduced, and the utilization rate of the crystals is improved. The method comprises the following steps of heating a raw material in a square crucible until the raw material is melted, adjusting the voltage, keeping a stable convection form on the surface of the melt in the square crucible and deviating a cold core away from the geometrical center position of the square crucible; adjusting a seed crystal position to obtain the seed crystal position gradually close to the liquid surface of the melt, meanwhile, adjusting the voltage, preheating the seed crystal, rotating in a matching manner by using the conventional lift process, meanwhile, adjusting the temperature, adjusting the size of the crystallization end part, finally covering the crystallization end part with the cold core and starting to shoulder the crystal; after shouldering to a predetermined size, slightly boosting the voltage to promote the completion of the shouldering, then continuously and slowly cooling to gradually grow and form the crystal, and boosting the voltage again when the crystal is grown to the growth tail end so as to smoothly end the crystal growth; reducing the voltage until a power supply is turned off, and gradually cooling the crystal in a single crystal furnace to finish crystal growth.
Description
Technical field
The present invention relates to jewel and manufacture field, relate in particular to a kind of square sapphire method of growth.
Background technology
Sapphire crystal (being commonly called as corundum) has uniqueness, good physicochemical property, particularly in 0.2 ~ 5.0 mu m waveband, has good light transmission, can be widely used in the fields such as infrared military equipment, satellite and space technology; And, because sapphire crystal also has dielectric insulation, constant characteristics such as specific inductivity, become one of most widely used substrate material.
At present, sapphire growth method mainly contains crystal pulling method, reverse mould method, kyropoulos, heat-exchanging method etc.Wherein, the most frequently used method when kyropoulos is current industrial production sapphire crystal, be characterized in, the crystal diameter when expanding shoulder suddenly becomes large and occurs in the growth stage casing that waist returns and melts contraction, bottom seamlessly transits ending, and the sapphire crystal therefore grown presents pyriform usually.
In realizing process of the present invention, the contriver finds that there are the following problems: because kyropoulos growing sapphire crystal optimum orientation is that A is to growth, and crystal bar extract direction be generally C to, extract vertically downward crystal bar from pyriform crystal ingot circumference, limit by the crystal ingot profile and cause the crystal utilization ratio low; And the circular crucible thermal field of existing growth pyriform crystal easily forms the bubble enrichment region on crystal top, thereby reduce the use value of crystal ingot, raise long brilliant cost.
Summary of the invention
The purpose of this invention is to provide a kind of sapphire method of growth rectangle, reduced the bubble that crystal top forms, and improved the crystal utilization ratio.
The embodiment of the present invention provides a kind of growth rectangle sapphire method, comprising:
In described step 101, the described cold heart with depart from square crucible geometric centre position and be less than 20mm.
In described step 102, the seed crystal preheating is at its lower end of seed crystal and melt liquid level 2 ~ 10mm place's preheating 10～60 min.Eliminate stress.
In described step 102, utilize traditional czochralski process, coordinating the rotational speed rate of rotation is 0.2 ~ 15rpm.
In described step 104, crystal is cooled to gradually 200-300 ℃ in single crystal growing furnace.
The sapphire method of growth rectangle that the embodiment of the present invention provides, adopt square crucible, its thermal field is evenly distributed, and crystal top bubble population stable, that prepare is less, the crystal utilization ratio is high, and, the growth square crystal all significantly surpasses the pyriform crystal on crystal quality and utilization ratio, so the present invention has the potential of significantly promoting and impelling the more capable replacement of industry equipment.
The accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the square sapphire method flow diagram of a kind of growth that the embodiment of the present invention one provides;
The square sapphire crucible structure schematic diagram of a kind of growth that Fig. 2 provides for the embodiment of the present invention.
Embodiment
More in order to solve the crystal top bubble cluster that prior art prepares for the square sapphire method of growing, the problem that the crystal utilization ratio is low, the embodiment of the present invention provides a kind of growth square sapphire method.
As shown in Figure 1, a kind of square sapphire method of growth that the embodiment of the present invention provides, the method comprises:
In the present embodiment, similar with growth pyriform sapphire crystal, utilize kyropoulos to prepare sapphire crystal, difference is, adopts square crucible to be prepared.By boosted voltage, by after the fusing of the raw material in square crucible, regulating voltage, make bath surface convection current form stable in square crucible, and make the cold heart depart from square crucible geometric centre position.Preferably, make the cold heart and square crucible geometric centre position deviation be less than 20mm.
It should be noted that, the actual needs that the square crucible thermal field that adopts of growth square crystal can be drawn the bar gauge lattice according to crystal designs different length ratios to improve the square crystal utilization ratio.In an embodiment of the present invention, as shown in Figure 2, the technical essential of preparation rectangle sapphire crystal is the length ratio of reasonable disposition square crystal 2, can before growing crystal, preset to draw excellent scheme and extract the utilization ratio of 2,4,6 inches crystal bars with raising square crystal 2; Adopt square crucible 1 and square tungsten cage heating member to be enclosed in square crucible periphery with same length and width ratio.Further, coordinate square crucible to adopt square tungsten cage heating element to present evenly linear to guarantee the inner thermal field of crucible.Can adopt square zirconia brick side screen thermal insulation layer or circular tungsten, molybdenum side screen thermal insulation layer (adopting square tungsten, molybdenum thermal insulation layer can produce the excessive and uncontrollable side screen distortion of amplitude so that confuse the inner temperature of crucible) outside square crucible, tungsten cage heating element.If adopted zirconia brick side screen thermal insulation layer can be used in conjunction with square burner hearth, so can save the furnace volume utilization ratio..
In the seeding technological process, slowly regulate the seed crystal position and make it move closer to melt liquid level, regulating voltage, avoid the seed crystal melting simultaneously.Preferably, lower end and melt liquid level 2 ~ 10mm place's preheating 10～60 min, to eliminate stress.Further, utilize traditional czochralski process, coordinate rotation, preferably speed of rotation is 0.2 ~ 15rpm.Determine and lift height at every turn according to the spreading rate of crystallization end, regulate temperature simultaneously, the size of crystallization control end, final crystallization end covers the cold heart and starts shouldering;
The liquid of the thermal field of square crucible in crystal shouldering process flows back to Lu Yike and clearly flows along square crucible crest line, is conducive to get rid of crystal top bubble, improves the crystal growth quality.
In order to be applicable to feeding, preferably, crystal is cooled to gradually 200-300 ℃ in single crystal growing furnace.
After taking turns long crystalline substance through one, from square crystal ingot, extract the crystal bar that specification is suitable (2,4,6in).Crystal bar grinds by end surface grinding, cylindrical barreling, flat limit and substrate slice or the diaphragm of making dimension are afterwards cut, grind, thrown to back segment.
Therefore, the sapphire method of growth rectangle that the embodiment of the present invention provides, adopt square crucible, its thermal field is evenly distributed, and crystal top bubble population stable, that prepare is less, the crystal utilization ratio is high, and the growth square crystal all significantly surpasses the pyriform crystal on crystal quality and utilization ratio, so the present invention has the potential of significantly promoting and impelling the more capable replacement of industry equipment.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (5)
1. the sapphire method of growth rectangle, is characterized in that, comprising:
Step 101, the raw material heated in square crucible extremely melt, and regulating voltage, make bath surface convection current form stable in square crucible, and make the cold heart depart from square crucible geometric centre position;
Step 102, slowly regulate the seed crystal position and make it move closer to melt liquid level, the while regulating voltage, avoid the seed crystal melting, the seed crystal preheating, utilize traditional czochralski process, coordinates rotation, determine and lift height at every turn according to the spreading rate of crystallization end, regulate temperature simultaneously, the size of crystallization control end, final crystallization end covers the cold heart and starts shouldering;
Step 103, crystal shouldering are to predetermined size, and boosted voltage impels shouldering to complete slightly, continue thereafter, slow cooling makes crystal growth and shaping gradually, when growing end again boosted voltage so that crystal growth ending smoothly;
Step 104, reduce voltage until powered-down, crystal is cooling gradually in single crystal growing furnace, long brilliant the end;
The technical essential for preparing square sapphire crystal is that the length ratio of reasonable disposition square crystal can be preset before growing crystal and draws excellent scheme and extract the utilization ratio of 2,4,6 inches crystal bars to improve square crystal; The characteristics of side's crucible thermal field be its can adopt pros or to a certain degree within rectangular as the crucible planar profile, its tungsten cage heating member is enclosed in the crucible periphery with same length and width ratio.
2. method according to claim 1, is characterized in that, in described step 101, the described cold heart with depart from square crucible geometric centre position and be less than 20mm.
3. method according to claim 1 and 2, in described step 102, the seed crystal preheating is at its lower end of seed crystal and melt liquid level 2 ~ 10mm place's preheating 10～60 min, eliminates stress.
4. method according to claim 3, is characterized in that, in described step 102, utilizes traditional czochralski process, and coordinating the rotational speed rate of rotation is 0.2 ~ 15rpm.
5. method according to claim 4, is characterized in that, in described step 104, crystal is cooled to gradually 200-300 ℃ in single crystal growing furnace.
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| CN2013104244246A CN103451729A (en) | 2013-09-17 | 2013-09-17 | Growth method of square sapphire |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264224A (en) * | 2014-09-19 | 2015-01-07 | 天通控股股份有限公司 | Growth method of large-size square sapphire crystal |
| CN104911708A (en) * | 2015-06-15 | 2015-09-16 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing square sapphire crystal by Kyropoulos process |
| CN106435717A (en) * | 2016-08-24 | 2017-02-22 | 天通银厦新材料有限公司 | Growth equipment and growth technology for 200-kg sapphire crystals |
| CN107881550A (en) * | 2017-11-08 | 2018-04-06 | 中国科学院合肥物质科学研究院 | A kind of crystal growth method by melt method of large-size crystals |
| CN109338460A (en) * | 2018-09-30 | 2019-02-15 | 中国科学院合肥物质科学研究院 | A method of control garnet crystal nucleus growth |
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| CN102127803A (en) * | 2011-03-08 | 2011-07-20 | 中国科学院上海硅酸盐研究所 | Growth method of rectangular specially-shaped sapphire crystal |
| CN102162130A (en) * | 2011-05-26 | 2011-08-24 | 浙江昀丰新能源科技有限公司 | Preparation method of sapphire monocrystalline |
| US20120186513A1 (en) * | 2011-01-26 | 2012-07-26 | DK AZTEC Co., Ltd | Kyropoulos sapphire single crystal growing apparatus using elliptic crucible |
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| US20120186513A1 (en) * | 2011-01-26 | 2012-07-26 | DK AZTEC Co., Ltd | Kyropoulos sapphire single crystal growing apparatus using elliptic crucible |
| CN102127803A (en) * | 2011-03-08 | 2011-07-20 | 中国科学院上海硅酸盐研究所 | Growth method of rectangular specially-shaped sapphire crystal |
| CN102162130A (en) * | 2011-05-26 | 2011-08-24 | 浙江昀丰新能源科技有限公司 | Preparation method of sapphire monocrystalline |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264224A (en) * | 2014-09-19 | 2015-01-07 | 天通控股股份有限公司 | Growth method of large-size square sapphire crystal |
| CN104911708A (en) * | 2015-06-15 | 2015-09-16 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing square sapphire crystal by Kyropoulos process |
| CN104911708B (en) * | 2015-06-15 | 2017-10-27 | 哈尔滨奥瑞德光电技术有限公司 | Kyropoulos prepare the growing method of square sapphire crystal |
| CN106435717A (en) * | 2016-08-24 | 2017-02-22 | 天通银厦新材料有限公司 | Growth equipment and growth technology for 200-kg sapphire crystals |
| CN107881550A (en) * | 2017-11-08 | 2018-04-06 | 中国科学院合肥物质科学研究院 | A kind of crystal growth method by melt method of large-size crystals |
| CN109338460A (en) * | 2018-09-30 | 2019-02-15 | 中国科学院合肥物质科学研究院 | A method of control garnet crystal nucleus growth |
| CN109338460B (en) * | 2018-09-30 | 2021-03-30 | 中国科学院合肥物质科学研究院 | Method for controlling growth of garnet crystal nucleus |
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Application publication date: 20131218 |