CN102758255A - Method for growing large-size high-temperature oxide crystal through for top-seeded temperature gradient technique - Google Patents
Method for growing large-size high-temperature oxide crystal through for top-seeded temperature gradient technique Download PDFInfo
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Abstract
The invention discloses a method for growing large-size high-temperature oxide crystal through a top-seeded temperature gradient technique. The method comprises steps of placing raw materials in a crucible of a multi-chamber crystal furnace, fixing seed crystal on a bottom end portion of a seed crystal rod of a seed crystal lifting rotary mechanism, and melting raw materials in the crucible to form a melting liquid; gradually reducing the heating power, enabling the melting liquid temperature to be a little higher than a melting point and trend to be stable, and observing the cold point position of the melting; washing the seed crystal; moving a cold point to the central position of the seed crystal; completely coinciding the central line of the seed crystal after being washed with the cold point of the melting liquid and keeping a constant temperature; seeding; necking down; shouldering; performing an equal-diameter process; and performing in situ annealing. Accordingly, a Kyropoulos method, a Czochralski method, a heat exchanging method, a temperature gradient technique and a Bridgman method are combined together, and the large-size high-temperature oxide crystal is produced.
Description
Technical field
The invention discloses a kind of high-temp oxide crystal growth method, the method for especially a kind of top seed temperature gradient method growing large-size high-temp oxide crystal.
Background technology
At present, existing high-temp oxide crystal growth method mainly contains four kinds: crystal pulling method, heat-exchanging method, falling crucible method and temperature gradient method.
One, crystal pulling method in invention in 1918, so claim " Czoncharlski method " again, is called for short the CZ method by Czochralski, is to utilize seed crystal pulling growth from melt to go out the crystalline method, and this method is the topmost method by the melt growth monocrystalline.Containing the fused material in the heated crucible; The seed rod band seed crystal and is from top to bottom inserted melt; Because near the melt the solid-liquid interface is kept certain condensate depression, melt along the seed crystal crystallization, and grows into bar-like single crystal with the rising gradually of seed crystal, crucible can be by high-frequency induction or resistive heating.
The advantage of this method is:
1, in process of growth, can observe the crystalline upgrowth situation easily;
2, crystal growth at the bath surface place does not contact with crucible, can reduce crystalline stress significantly, prevents the parasitic nucleation of sidewall of crucible;
3, can use oriented seed and " necking down " technology easily, the dislocation of " necking down " back seed crystal is significantly reduced, the dislocation desity of growing crystal after the reduction shouldering, thus improve perfection of crystal;
4, control crystalline growth velocity accurately.
The shortcoming of this method is:
1, under the equal crucible condition, crystal is less, and diameter is no more than crucible 50%;
2, because gradient is bigger, the undue convexity of growth interface, thermal stresses is big, the dislocation increment causes that dislocation desity is excessive, and monocrystalline property is bad;
3, thermograde is big, and energy consumption is high.
Two, heat-exchanging method (being called for short the HEM method) is a kind of crystal technique of inventing for the growing large-size crystal.Schmid in 1970 and Viechnicki at first use heat-exchanging method to grow the sapphire crystal of bulk.Its principle is to utilize heat exchanger to take away heat; Make the longitudinal temperature gradient that forms a cold lower part and hot upper part in the crystal growth district; Control this thermograde by the size of gas flow (He cooling source) in the control heat exchanger and the height of change heating power more simultaneously, reach the interior molten soup of crucible whereby by slowly upwards being frozen into the crystalline purpose down.
The advantage of this method is:
1, temperature gradient distribution and gravity field are opposite, and crucible, crystal and heat exchanger are neither to be moved, and mechanical disturbance is stablized, do not had to crystal growth interface, the buoyancy convection current is little, eliminated the lattice defect that causes owing to mechanical movement;
2, still remain on the hot-zone after the crystal growth, the control helium gas flow can make temperature slowly evenly reduced by Tc, realizes in-situ annealing, reduces crystalline thermal stresses and defectives such as consequent crystal cleavage and dislocation;
3, under the equal crucible condition, can obtain the macrocrystal of crucible diameter about 90%.
The shortcoming of this method is:
1, appointed condition require high, whole complex process, the crystal growth cycle is long, need a large amount of helium make refrigerant, cost is high.
2, temperature gradient distribution and gravity field are opposite, are unfavorable for impurities removal;
3, crystal contacts with crucible, and crystalline stress is big, and easy parasitic nucleation causes polycrystalline;
4, crystal growth can not be controlled and observe in real time;
5, growth interface excess convexity, thermal stresses and dislocation are excessive.
Three, falling crucible method (Bridgman-stockbarger method) is that a vertical crucible of placing is descended gradually, makes it pass through a temperature gradient zone (relative superiority or inferiority is low on the temperature), and melt solidifies from bottom to top.Through relatively moving between crucible and the melt, form certain temperature field, make crystal growth.The crystallization forward position that thermograde forms is cold excessively to be the motivating force of keeping crystal growth.Use point end crucible can successfully obtain monocrystalline, also can place seed crystal in crucible bottom.To use close crucible for volatile materials.
The advantage of this method is:
1, crucible seals, and can produce the crystal of volatile matter;
2, composition is easy to control;
3, but growing large-size monocrystalline under the equal crucible condition can arrive 90% diameter;
4, crystal growth interface dimpling, comparatively desirable near planar interface;
5, can accurately control crystalline growth velocity.
The shortcoming of this method is:
The material that 1, should not be used for negative thermal expansion coefficient, and fluid density is greater than the material of solid density;
2, because the crucible effect forms stress, parasitic nucleation and pollution easily;
3, be not easy to observe;
4, there is mechanical disturbance in descending mechanism down.
Four, temperature gradient method (being called for short the TGT method) claims guiding warm terraced method again, is with oriented seed inductive melt single crystal method, is a kind of method for monocrystal growth of China Shanghai ray machine institute crystal research department in the nineties invention in latter stage.Its device adopts molybdenum crucible, graphite heater, and there is a seed slot at the crucible bottom center, avoids seed crystal when changing material, to be melted.The temperature field is provided by graphite heater and refrigerating unit jointly.Heating element is slit into the cylinder of the wavy lath power circuit of rectangle for groove about the quilt, on the graphite electrode plate that whole cylinder is installed in water cooled electrode links to each other.The lath first half punches according to certain rules, causes the intimate linear temperature difference to regulate from top to bottom after heating resistor makes its energising.And the heating element Lower Half temperature difference is created through the conduction of graphite heater and water cooled electrode plate.
The advantage of this method:
1, thermograde is opposite with gravity direction during crystal growth, and crucible, crystal and heating element do not move, and this has just been avoided the melt eddy current of thermal convection and mechanical movement generation;
2, after the crystal growth, surround, still be in the hot-zone by melt.So just can control its speed of cooling, reduce thermal stresses;
3. during crystal growth, solid-liquid interface is among melt surrounds.The thermal perturbation of bath surface and mechanical disturbance can be reduced so that elimination by melt before arriving solid-liquid interface like this.
The shortcoming of this method:
1, temperature gradient distribution and gravity field are opposite, are unfavorable for impurities removal;
2, crystal contacts with crucible, and crystalline stress is big, and easy parasitic nucleation causes polycrystalline;
3, crystal growth can not be controlled and observe in real time;
4, growth interface excess convexity, thermal stresses and dislocation are excessive.
The key of crystal technique finally is to be reflected in the shape control of crystal growth solid-liquid interface, and the shape of solid-liquid interface directly has influence on the crystalline quality.Improve the shape of solid-liquid interface and can avoid facet growth and kernel, can control the trend of the dislocation that intersects with solid-liquid interface.The shape of solid-liquid interface also with crystal in solute gather partially, the distribution of the formation of bubble, thermal stresses is closely related.
Existing growing method does not have a kind of method to carry out real-time artificial control to crystal growth interface according to the different steps of crystal growth.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in the prior art, the method for a kind of top seed temperature gradient method growing large-size high-temp oxide crystal is provided.
According to technical scheme provided by the invention, the method for said top seed temperature gradient method growing large-size high-temp oxide crystal comprises the steps:
A, raw material is packed in the crucible of multi-cavity chamber crystal furnace; Seed crystal is fixed on the bottom of the seed rod of seed rod elevating and rotating machine structure; Seed rod elevating and rotating machine structure links to each other with Weighing mechanism, covers the lid of multi-cavity chamber crystal furnace, with being pumped into 1.0 * 10 in the crystal furnace of multi-cavity chamber
-3~ 1.0 * 10
-4Behind the Pa, the heating element energising, with the speed heating of 4500 ~ 5000W/h, the raw material in crucible is fused into liquation;
After the fusing of b, raw material, progressively reduce heating element power with the speed of 300 ~ 500W/h and make melt temperature, observe the cold spot position of melt simultaneously a little more than more than the fusing point 20 ~ 50 ℃ and tend towards stability;
C, control seed rod elevating and rotating machine structure; Make the seed rod rotation descend; The hypomere of seed crystal inserts in the liquation and washes seed crystal; Control seed rod elevating and rotating machine structure rapidly, make the seed crystal after seed rod rotation rising and drive are washed break away from about 10 ~ 20mm place more than the liquation, and whether the observation cold spot overlaps with the seed crystal central position;
D, according to the position that cold spot and seed crystal depart from, regulate the cooling water flow that cold spot departs from rightabout furnace wall, seed crystal central position branch, guarantee that cold spot moves towards the seed crystal central position; If the cold spot position is positioned at the upper left corner at seed crystal center, then transfer the cooling water flow of position, the lower right corner, big furnace wall;
The medullary ray of e, back to be washed seed crystal is with after the cold spot of liquation overlaps fully, constant temperature 4 ~ 6h;
F, control seed rod elevating and rotating machine structure; Make seed rod rotate and descend, wash the back seed crystal and insert in the liquation, control seed rod elevating and rotating machine structure behind the seed crystal insertion liquation after washing; Make seed rod rotate the 2 ~ 3mm that rises; The liquation that is positioned at the cold spot position is washed the back seed crystal and is mentioned and stick to and wash on the seed crystal of back, and the bottom of washing the back seed crystal still is in the liquation, and completion is sowed;
After g, the completion of sowing, seed crystal lifts with the speed of 20 ~ 30mm/h, guarantees constriction diameters at 15 ~ 20mm, and necking down length is accomplished necking down behind 15 ~ 20mm;
H, necking down begin shouldering after finishing; Rotating speed is 4 ~ 10rpm; Pulling rate is 0.3 ~ 1.5mm/h, and heating element power fall off rate is 200 ~ 400W/h, and the flow of each chamber cooling fluid of dynamic conditioning crystal furnace wall guarantees that the cylindrical of shoulder becomes centrosymmetry state (identical with cold spot centering control principle) in the shouldering process; When crystal growth is extremely left sidewall of crucible 5 ~ 10mm, accomplish shouldering;
I, seed rod elevating and rotating machine structure stop the rotation; Control seed rod elevating and rotating machine structure makes seed rod at the uniform velocity rise with the speed of 0.1 ~ 0.5mm/h; Reduce heating element power with the speed of 100 ~ 300W/h, the flow of weigh Data Control heating element power, each chamber of crystal furnace wall and bell cooling fluid through Weighing mechanism makes crystal keep the equal diameter growth; Crystal mass evenly increases, and gathering way is 3 ~ 5Kg/h;
Carry out in-situ annealing behind j, the crystal equal diameter growth ending.
The present invention has following advantage:
1, adopt around the heating element of band bottom heating, realize crucible bottom to down and on temperature gradient distribution; Temperature gradient distribution is identical with gravity field, and crystal growth helps impurities removal from top to down;
2, in the process of growth, " sowing " and " shouldering " can be observed the situation of crystal growth easily; " isometrical " stage adopts weighing technology that crystal growth is accurately controlled;
3, crucible, crystal and heat exchanger are neither mobile behind the crystal growth entering isodiametric growth, and mechanical disturbance is stablized, do not had to crystal growth interface, the buoyancy convection current is little, eliminated the lattice defect that causes owing to mechanical movement;
4, crystal growth at the bath surface place does not contact with crucible, can reduce crystalline stress significantly, prevents the parasitic nucleation of sidewall of crucible; But growing large-size monocrystalline under the simultaneously equal crucible condition can arrive 90% diameter;
5, can use oriented seed and " necking down " technology easily, the dislocation of " necking down " back seed crystal is significantly reduced, reduce the dislocation desity that expands shoulder back growing crystal, thereby improve perfection of crystal;
6, subregion is controlled the fluidic amount of cooling water of each five equilibrium of furnace wall (eight equal parts), can regulate the position of a crucible temperature cold spot, guarantees that crystalline is sowed and the shouldering quality; After the isometrical beginning of crystal; The heat in the above zone of crystals and crystal top can be cumulative, grows up after to a certain degree when crystal, and solid-liquid interface can be overturn; Have a strong impact on crystal mass; The present invention can transfer the cooling water flow at big bell place when crystal is grown up, can take away much more more thermal values that are collected at the above zone of crystal top, has realized the crystal growth interface dimpling, near planar interface.
The present invention is except the advantage that combines each technology, and outstanding feature is in whole crystal growing process, to control the gradient at temperature each position through regulating each piecemeal cooled region fluid amount of cooling water, reaches the purpose of control solid-liquid interface.
Method of the present invention is kyropoulos, crystal pulling method (CZ), heat-exchanging method (HEM), warm terraced method (TGT) and falling crucible method are combined; Create the special high-temperature vacuum crystal furnace at an adjustable thermograde and Wen Chang center; Through shove charge, pumping high vacuum, temperature increasing for melting materials, wash that seed crystal, real-time temperature field control, crystal pulling method are sowed, repeatedly " diameter reducing process ", crystal pulling method " shouldering technology ", crystal growth interface control (protruding interface regulate become dimpling or near planar interface), " isometrical technology " HEM heat exchange combines TGT technology isodiametric growth (the control diameter technology is weighed for CZ), CZ method to finish up and take off crucible, in-situ annealing, produces the large size high-temp oxide crystal.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
The method of a kind of top of the present invention seed temperature gradient method growing large-size high-temp oxide crystal comprises the steps:
A, raw material is packed in the crucible of multi-cavity chamber crystal furnace; Seed crystal is fixed on the bottom of the seed rod of seed rod elevating and rotating machine structure; Seed rod elevating and rotating machine structure links to each other with Weighing mechanism, covers the lid of multi-cavity chamber crystal furnace, with being pumped into 1.0 * 10 in the crystal furnace of multi-cavity chamber
-3~ 1.0 * 10
-4Behind the Pa, the heating element energising, with the speed heating of 4500 ~ 5000W/h, the raw material in crucible is fused into liquation;
After the fusing of b, raw material, progressively reduce heating element power with the speed of 300 ~ 500W/h and make the raw material melt temperature, observe the cold spot position of raw material liquation simultaneously a little more than more than the fusing point 20 ~ 50 ℃ and tend towards stability;
C, control seed rod elevating and rotating machine structure; Make the seed rod rotation descend; The hypomere of seed crystal inserts in the liquation and washes seed crystal; Control seed rod elevating and rotating machine structure rapidly, make the seed crystal after seed rod rotation rising and drive are washed break away from about 10 ~ 20mm place more than the liquation, and whether the observation cold spot overlaps with the seed crystal central position;
D, according to the position that cold spot and seed crystal depart from, regulate the cooling water flow that cold spot departs from seed crystal central position rightabout burner hearth branch, guarantee that cold spot moves towards the seed crystal central position; During actually operating,, then transfer the cooling water flow of position, the lower right corner, big furnace wall if the cold spot position is positioned at the upper left corner at seed crystal center;
The medullary ray of e, back to be washed seed crystal is with after the cold spot of liquation overlaps fully, constant temperature 4 ~ 6h;
F, control seed rod elevating and rotating machine structure; Make seed rod rotate and descend, wash the back seed crystal and insert in the liquation, control seed rod elevating and rotating machine structure behind the seed crystal insertion liquation after washing; Make seed rod rotate the 2 ~ 3mm that rises; The liquation that is positioned at the cold spot position is washed the back seed crystal and is mentioned and stick to and wash on the seed crystal of back, and the bottom of washing the back seed crystal still is in the liquation, and completion is sowed;
After g, the completion of sowing, seed crystal lifts with the speed of 20 ~ 30mm/h, guarantees constriction diameters at 15 ~ 20mm, and necking down length is accomplished necking down behind 15 ~ 20mm;
H, necking down begin shouldering after finishing; Rotating speed is 4 ~ 10rpm; Pulling rate is 0.3 ~ 1.5mm/h, and heating element power fall off rate is 200 ~ 400W/h, and the flow of each chamber cooling fluid of dynamic conditioning crystal furnace wall guarantees that the cylindrical of shoulder becomes centrosymmetry state (identical with cold spot centering control principle) in the shouldering process; When crystal growth is extremely left sidewall of crucible 5 ~ 10mm, accomplish shouldering;
I, seed rod elevating and rotating machine structure stop the rotation; Control seed rod elevating and rotating machine structure makes seed rod at the uniform velocity rise with the speed of 0.1 ~ 0.5mm/h; Reduce heater power with the speed of 100-300W/h, the flow of weigh Data Control heating element temperature, each chamber of crystal furnace wall and bell cooling fluid through Weighing mechanism makes crystal keep the equal diameter growth; Crystal mass evenly increases, and gathering way is 3 ~ 5Kg/h;
Carry out in-situ annealing behind j, the crystal equal diameter growth ending.
The invention has the beneficial effects as follows and utilize minimum energy consumption and minimum cost to produce multiple high-quality high-temp oxide crystal material product.And for crystal pulling method (CZ) result that compares: through concrement vacuole think of a way, heat-exchanging method (HEM), crucible descends and the temperature design advantage of TGT; Successfully realized " plane interface growth ", solved crystal pulling method " protruding interface growth " thereby the big problem that causes big dislocation desity of stress; Through concrement vacuole think of a way, temperature the design and the growth technique advantage of heat-exchanging method (HEM), falling crucible method and temperature gradient method (TGT), can in less crucible, realize bigger crystal diameter (for example the crystal of 110 ~ 120mm only needs the crucible internal diameter about 130mm); Grow unidimensional crystal energy consumption well below crystal pulling method; The crystal growth middle and later periods, major part has adopted the technical characterstic of kyropoulos, has avoided the interference of mechanical vibration.For kyropoulos (Kyropoulos) comparative result: through concrement vacuole think of a way, the temperature design advantage of crystal pulling method, heat-exchanging method (HEM) and temperature gradient method (TGT); In conjunction with the crystal pulling method technological advantage, successfully solved traditional kyropoulos and when crystal growth end and remainder melt disengaging, produced the problem of big thermal shocking; In signals collecting and temperature control, very big novelty is arranged, realized the real-time control of crystal growth.
Method of the present invention has overcome traditional kyropoulos crystal growing process and has received the bigger shortcoming of extraneous factor variable effect (as: water temperature changes, voltage fluctuation); Adopt special method and technology, solved kyropoulos a temperature symmetry is required harsh shortcoming; In conjunction with the crystal pulling method technological advantage, carry out repeatedly " undergauge " technology earlier and effectively reduce the dislocation on the seed crystal, take elder generation's " czochralski process " back " bubble is given birth to technology ".For temperature gradient method (TGT), heat-exchanging method (HEM) and the falling crucible method result that compares: the technological advantage of having taked crystal pulling method and kyropoulos; Adopted the method for top seed crystal, the seed crystal that is different from temperature gradient method (TGT), falling crucible method and heat-exchanging method (HEM) fully is placed on crucible bottom; Concrement vacuole temperature the design advantage with crystal pulling method of thinking of a way has successfully solved the main drawback of falling crucible method, temperature gradient method (TGT) and heat-exchanging method (HEM): thus crystal contacts generation stress or parasitic nucleation with sidewall of crucible.Owing to do not contact, prolonged the work-ing life of crucible greatly simultaneously with sidewall of crucible; Simultaneously, solve the problem that falling crucible method, temperature gradient method (TGT) and heat-exchanging method (HEM) process of growth can not direct viewing, realized the real-time control of crystal growth.
The equipment that is adopted among the present invention is the conventional equipment that uses in the prior art.
Claims (1)
1. the method for a top seed temperature gradient method growing large-size high-temp oxide crystal is characterized in that this method comprises the steps:
A, raw material is packed in the crucible of multi-cavity chamber crystal furnace; Seed crystal is fixed on the bottom of the seed rod of seed rod elevating and rotating machine structure; Seed rod elevating and rotating machine structure links to each other with Weighing mechanism, covers the lid of multi-cavity chamber crystal furnace, with being pumped into 1.0 * 10 in the crystal furnace of multi-cavity chamber
-3~ 1.0 * 10
-4Behind the Pa, the heating element energising on the crucible outer wall, with the speed heating of 4500 ~ 5000W/h, the raw material in crucible is fused into liquation;
After the fusing of b, raw material, progressively reduce heating element power with the speed of 300 ~ 500W/h and make the raw material melt temperature be higher than above 20 ~ 50 ℃ and tend towards stability of fusing point, observe the cold spot position of raw material liquation simultaneously;
C, control seed rod elevating and rotating machine structure; Make the seed rod rotation descend; The hypomere of seed crystal inserts in the raw material liquation and washes seed crystal; Rapid control seed rod elevating and rotating machine structure rises the seed rod rotation and the seed crystal that drives after washing breaks away from the above 10 ~ 20mm place of liquation, and whether the observation cold spot overlaps with the seed crystal central position;
D, according to the position that cold spot and seed crystal depart from, regulate the cooling water flow that cold spot departs from seed crystal central position rightabout burner hearth branch, guarantee that cold spot moves towards the seed crystal central position;
The medullary ray of e, back to be washed seed crystal is with after the cold spot of liquation overlaps fully, constant temperature 4 ~ 6h;
F, control seed rod elevating and rotating machine structure; Make seed rod rotate and descend, wash the back seed crystal and insert in the liquation, control seed rod elevating and rotating machine structure behind the seed crystal insertion liquation after washing; Make seed rod rotate the 2 ~ 3mm that rises; The liquation that is positioned at the cold spot position is washed the back seed crystal and is mentioned and stick to and wash on the seed crystal of back, and the bottom of washing the back seed crystal still is in the liquation, and completion is sowed;
After g, the completion of sowing, seed crystal lifts with the speed of 20 ~ 30mm/h, guarantees constriction diameters at 15 ~ 20mm, and necking down length is accomplished necking down behind 15 ~ 20mm;
H, necking down begin shouldering after finishing; Rotating speed is 4 ~ 10rpm; Pulling rate is 0.3 ~ 1.5mm/h, and heating element power fall off rate is 200 ~ 400W/h, and the flow of each chamber cooling fluid of dynamic conditioning crystal furnace wall guarantees that the cylindrical of shoulder becomes the centrosymmetry state in the shouldering process; When crystal growth is extremely left sidewall of crucible 5 ~ 10mm, accomplish shouldering;
I, seed rod elevating and rotating machine structure stop the rotation; Control seed rod elevating and rotating machine structure makes seed rod at the uniform velocity rise with the speed of 0.1 ~ 0.5mm/h; Reduce heating member power with the speed of 100 ~ 300W/h, the flow of weigh Data Control heating element temperature, each chamber of crystal furnace wall and bell cooling fluid through Weighing mechanism makes crystal keep the equal diameter growth; Crystal mass evenly increases, and gathering way is 3 ~ 5Kg/h;
Carry out in-situ annealing behind j, the crystal equal diameter growth ending.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110344108A (en) * | 2019-08-21 | 2019-10-18 | 眉山博雅新材料有限公司 | Upper lifting vacuum drying oven |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5938184B2 (en) * | 1977-11-11 | 1984-09-14 | 東芝セラミツクス株式会社 | Manufacturing method of saphia single crystal |
| JPS6259590A (en) * | 1985-09-10 | 1987-03-16 | Sumitomo Electric Ind Ltd | Production of compound semiconductor single crystal |
| JPH0812496A (en) * | 1994-06-30 | 1996-01-16 | Sony Corp | Production of ferrite single crystal |
| JPH08319195A (en) * | 1995-05-25 | 1996-12-03 | Japan Energy Corp | Production of lithium borate single crystal |
| JPH09328394A (en) * | 1996-06-07 | 1997-12-22 | Shin Etsu Chem Co Ltd | Production of oxide single crystal |
| JP2005001934A (en) * | 2003-06-11 | 2005-01-06 | Daiichi Kiden:Kk | Apparatus for pulling and growing sapphire single crystal |
| WO2005053003A2 (en) * | 2003-11-25 | 2005-06-09 | Toyota Jidosha Kabushiki Kaisha | Method of production of silicon carbide single crystal |
| CN1724722A (en) * | 2005-06-24 | 2006-01-25 | 哈尔滨工业大学 | Cold core shouldering micropulling proparation method of large size sapphire single crystal |
| CN101580963A (en) * | 2009-06-26 | 2009-11-18 | 哈尔滨工大奥瑞德光电技术有限公司 | SAPMAC method for preparing sapphire single-crystal with size above 300mm |
| CN101705516A (en) * | 2009-09-25 | 2010-05-12 | 上海元亮光电科技有限公司 | Method for growing large-size high-temperature oxide crystals by using top-seeded temperature gradient method |
| CN102051672A (en) * | 2009-10-29 | 2011-05-11 | 上海元亮光电科技有限公司 | Vertical temperature grade kyropoulos method for growing large-size high-temperature oxide crystals |
| CN102140675A (en) * | 2011-03-24 | 2011-08-03 | 哈尔滨奥瑞德光电技术股份有限公司 | Kyropoulos method for quickly growing large-size sapphire single crystal |
-
2012
- 2012-08-02 CN CN201210272246.5A patent/CN102758255B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5938184B2 (en) * | 1977-11-11 | 1984-09-14 | 東芝セラミツクス株式会社 | Manufacturing method of saphia single crystal |
| JPS6259590A (en) * | 1985-09-10 | 1987-03-16 | Sumitomo Electric Ind Ltd | Production of compound semiconductor single crystal |
| JPH0812496A (en) * | 1994-06-30 | 1996-01-16 | Sony Corp | Production of ferrite single crystal |
| JPH08319195A (en) * | 1995-05-25 | 1996-12-03 | Japan Energy Corp | Production of lithium borate single crystal |
| JPH09328394A (en) * | 1996-06-07 | 1997-12-22 | Shin Etsu Chem Co Ltd | Production of oxide single crystal |
| JP2005001934A (en) * | 2003-06-11 | 2005-01-06 | Daiichi Kiden:Kk | Apparatus for pulling and growing sapphire single crystal |
| WO2005053003A2 (en) * | 2003-11-25 | 2005-06-09 | Toyota Jidosha Kabushiki Kaisha | Method of production of silicon carbide single crystal |
| WO2005053003A3 (en) * | 2003-11-25 | 2008-02-14 | Toyota Motor Co Ltd | Method of production of silicon carbide single crystal |
| CN1724722A (en) * | 2005-06-24 | 2006-01-25 | 哈尔滨工业大学 | Cold core shouldering micropulling proparation method of large size sapphire single crystal |
| CN101580963A (en) * | 2009-06-26 | 2009-11-18 | 哈尔滨工大奥瑞德光电技术有限公司 | SAPMAC method for preparing sapphire single-crystal with size above 300mm |
| CN101705516A (en) * | 2009-09-25 | 2010-05-12 | 上海元亮光电科技有限公司 | Method for growing large-size high-temperature oxide crystals by using top-seeded temperature gradient method |
| CN102051672A (en) * | 2009-10-29 | 2011-05-11 | 上海元亮光电科技有限公司 | Vertical temperature grade kyropoulos method for growing large-size high-temperature oxide crystals |
| CN102140675A (en) * | 2011-03-24 | 2011-08-03 | 哈尔滨奥瑞德光电技术股份有限公司 | Kyropoulos method for quickly growing large-size sapphire single crystal |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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