CN102758255B - 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
- Publication number
- CN102758255B CN102758255B CN201210272246.5A CN201210272246A CN102758255B CN 102758255 B CN102758255 B CN 102758255B CN 201210272246 A CN201210272246 A CN 201210272246A CN 102758255 B CN102758255 B CN 102758255B
- Authority
- CN
- China
- Prior art keywords
- crystal
- seed
- seed crystal
- crucible
- liquation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 186
- 238000000034 method Methods 0.000 title claims abstract description 111
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims description 10
- 239000000498 cooling water Substances 0.000 claims description 8
- 230000007423 decrease Effects 0.000 claims description 7
- 239000012809 cooling fluid Substances 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 abstract description 13
- 238000010899 nucleation Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 description 7
- 230000035882 stress Effects 0.000 description 7
- 230000006911 nucleation Effects 0.000 description 6
- 230000003071 parasitic effect Effects 0.000 description 6
- 230000008646 thermal stress Effects 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000005484 gravity Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 210000003934 vacuole Anatomy 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000002109 crystal growth method Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000009331 sowing Methods 0.000 description 2
- 238000002231 Czochralski process Methods 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
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 is invented in 1918 by Czochralski, therefore also known as " Czoncharlski method ", be called for short CZ method, be the method utilizing seed crystal pulling growth from melt to go out crystal, this method is by the topmost method of melt growth monocrystalline.The material of melting is contained by the crucible that heats, seed rod from top to bottom inserts melt with seed crystal, due to the melt near solid-liquid interface maintain certain condensate depression, melt along seed crystallization, and grows into bar-like single crystal with the rising gradually of seed crystal, crucible can by high-frequency induction or resistive heating.
The advantage of the method is:
1, in process of growth, the upgrowth situation of crystal can be observed easily;
2, crystal is in the growth of bath surface place, does not contact, can reduce the stress of crystal significantly, prevent the parasitic nucleation of sidewall of crucible with crucible;
3, oriented seed and " necking down " technique can be used easily, the dislocation of " necking down " seed crystal is afterwards greatly reduced, reduce the dislocation desity of growing crystal after shouldering, thus improve perfection of crystal;
4, crystalline growth velocity is controlled accurately.
The shortcoming of the method is:
1, under equal crucible condition, crystal is less, and diameter is no more than crucible 50%;
2, because gradient is comparatively large, the projection that growth interface is undue, thermal stresses is large, dislocation increment causes dislocation desity excessive, monocrystalline bad;
3, thermograde is large, and energy consumption is high.
Two, heat-exchanging method (being called for short HEM method) is a kind of crystal technique invented in order to growing large-size crystal.Within 1970, first Schmid and Viechnicki use heat-exchanging method to grow the sapphire crystal of bulk.Its principle utilizes heat exchanger to take away heat, make the longitudinal temperature gradient forming a cold lower part and hot upper part in crystal growth district, simultaneously control this thermograde by the size controlling gas flow (He cooling source) in heat exchanger and the height that changes heating power again, reach whereby molten soup in crucible by under be slowly upwards frozen into the object of crystal.
The advantage of the method is:
1, temperature gradient distribution is contrary with gravity field, and crucible, crystal and heat exchanger neither move, and crystal growth interface is stable, mechanical disturbance, Natural convection are little, eliminates the lattice defect caused due to mechanical movement;
2, still remain on hot-zone after crystal growth, control helium gas flow and temperature can be made slowly evenly to be reduced by Tc, realize in-situ annealing, reduce thermal stresses and the defect such as consequent crystal cleavage and dislocation of crystal;
3, under equal crucible condition, the macrocrystal of crucible diameter about 90% can be obtained.
The shortcoming of the method is:
1, appointed condition requires high, whole complex process, and crystal growth cycles is grown, needed a large amount of helium to make refrigerant, and cost is high.
2, temperature gradient distribution is contrary with gravity field, is unfavorable for impurities removal;
3, crystal contacts with crucible, and the stress of crystal is large, and easy parasitic nucleation causes polycrystalline;
4, crystal growth can not control in real time and observe;
5, growth interface excess convexity, thermal stresses and dislocation excessive.
Three, falling crucible method (Bridgman-stockbarger method) is declined gradually by the crucible that is vertically placed, and make it by a temperature gradient zone (in temperature, height bends down), melt solidifies from bottom to top.By the relative movement between crucible and melt, form certain temperature field, make crystal growth.The crystallization front that thermograde is formed is excessively cold is the motivating force maintaining crystal growth.Use point end crucible successfully can obtain monocrystalline, also can place seed crystal in crucible bottom.Close crucible will be used for volatile materials.
The advantage of the method is:
1, crucible is closed, and can produce the crystal of volatile matter;
2, composition is easy to control;
3, can growing large-size monocrystalline under equal crucible condition, can to 90% diameter;
4, crystal growth interface dimpling, ideal close to planar interface;
5, accurately crystalline growth velocity can be controlled.
The shortcoming of the method is:
1, the material of negative thermal expansion coefficient should not be used for, and fluid density is greater than the material of solid density;
2, due to crucible effect, easily stress is formed, parasitic nucleation and pollution;
3, be not easy to observe;
4, there is mechanical disturbance in descending mechanism.
Four, temperature gradient method (being called for short TGT method), also known as the warm terraced method of guiding, is with the melt single crystal method of oriented seed induction, is that China's Shanghai ray machine institute's Crystal study room is in a kind of method for monocrystal growth of the nineties invention in latter stage.Its device adopts molybdenum crucible, graphite heater, and there is a seed slot at crucible bottom center, avoids seed crystal to be melted when material.Temperature field is provided jointly by graphite heater and refrigerating unit.Heating element is the cylinder being slit into the wavy lath power circuit of rectangle by upper and lower groove, and whole cylinder is arranged on the graphite electrode plate that is connected with water cooled electrode.The lath first half punches according to certain rules, from top to bottom causes the near-linear temperature difference after making it be energized with regulation heating resistance.And the heating element Lower Half temperature difference is created by the conduction of graphite heater and water cooled electrode plate.
The advantage of the method:
1, during crystal growth, thermograde is contrary with gravity direction, and crucible, crystal and heating element do not move, and avoiding problems the melt eddy current of thermal convection and mechanical movement generation;
2, after crystal growth, surrounded by melt, be still in hot-zone.So just can control its speed of cooling, reduce thermal stresses;
3., during crystal growth, solid-liquid interface is among melt encirclement.The thermal perturbation of such bath surface and mechanical disturbance can be reduced by melt so that eliminate before arrival solid-liquid interface.
The shortcoming of the method:
1, temperature gradient distribution is contrary with gravity field, is unfavorable for impurities removal;
2, crystal contacts with crucible, and the stress of crystal is large, and easy parasitic nucleation causes polycrystalline;
3, crystal growth can not control in real time and observe;
4, growth interface excess convexity, thermal stresses and dislocation excessive.
The key of crystal technique is finally be reflected on the shape controlling of crystal growth solid-liquid interface, and the shape of solid-liquid interface directly has influence on the quality of crystal.The shape improving solid-liquid interface can avoid facet growth and kernel, can control the trend of the dislocation crossing with solid-liquid interface.The shape of solid-liquid interface is also closely related with the distribution of the formation of solute segregation, bubble in crystal, thermal stresses.
Existing growing method, does not have a kind of method can carry out real-time manual control according to the different steps of crystal growth to crystal growth interface.
Summary of the invention
The object of the invention is to overcome the deficiencies 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 described top seed temperature gradient method growing large-size high-temp oxide crystal comprises the steps:
A, raw material is loaded in the crucible of multi-chamber crystal furnace, seed crystal is fixed on the bottom of the seed rod of seed rod lifting rotation mechanism, seed rod lifting rotation mechanism is connected with Weighing mechanism, covers the lid of multi-chamber crystal furnace, is pumped into 1.0 × 10 by multi-chamber crystal furnace
-3~ 1.0 × 10
-4after Pa, heating element is energized, and heats, until the melting sources in crucible becomes liquation with the speed of 4500 ~ 5000W/h;
After b, melting sources, progressively reduce heating element power with the speed of 300 ~ 500W/h and make melt temperature a little more than more than fusing point 20 ~ 50 DEG C and tend towards stability, observe the cold spot position of melt simultaneously;
C, control seed rod lifting rotation mechanism, seed rod is rotated decline, the hypomere of seed crystal inserts in liquation washes seed crystal, rapid control seed rod lifting rotation mechanism, seed rod is rotated and rises and drive more than the disengaging of the seed crystal after washing liquation about 10 ~ 20mm place, and observe cold spot and whether overlap with seed crystal central position;
D, the position of departing from according to cold spot and seed crystal, regulate cold spot to depart from the cooling water flow of the rightabout furnace wall branch in seed crystal central position, guarantee that cold spot moves towards seed crystal central position; If cold spot position is positioned at the upper left corner at seed crystal center, then tune up the cooling water flow of furnace wall lower right position;
After e, the medullary ray of rear seed crystal to be washed overlap completely with the cold spot of liquation, constant temperature 4 ~ 6h;
F, control seed rod lifting rotation mechanism, seed rod is rotated decline, washing rear seed crystal inserts in liquation, wash after rear seed crystal inserts liquation and control seed rod lifting rotation mechanism, seed rod is made to rotate rising 2 ~ 3mm, the liquation being positioned at cold spot position is washed rear seed crystal and is mentioned and stick to and wash on rear seed crystal, and the bottom washing rear seed crystal is still in liquation, completes and sows;
G, sowed after, seed crystal lifts with the speed of 20 ~ 30mm/h, and guarantee that constriction diameters is at 15 ~ 20mm, necking down length completes necking down after 15 ~ 20mm;
H, necking down terminate rear beginning shouldering, rotating speed is 4 ~ 10rpm, pulling rate is 0.3 ~ 1.5mm/h, heating element power fall rate is 200 ~ 400W/h, in shouldering process, the flow of dynamic adjustments crystal furnace wall each chamber cooling fluid guarantees the cylindrical of shoulder state in a center of symmetry (identical with cold spot centering control principle), when crystal growth is to during from sidewall of crucible 5 ~ 10mm, complete shouldering;
I, seed rod lifting rotation mechanism stop the rotation, controlling seed rod lifting rotation mechanism makes seed rod at the uniform velocity rise with the speed of 0.1 ~ 0.5mm/h, with the rate reduction heating element power of 100 ~ 300W/h, the flow of heating element power, each chamber in crystal furnace wall and bell cooling fluid is controlled by the weighing data of Weighing mechanism, crystal is made to keep equal diameter growth, crystal mass evenly increases, and gathering way is 3 ~ 5Kg/h;
The growth of j, crystal equal diameter terminates laggard row in-situ annealing.
Tool of the present invention has the following advantages:
1, adopt the heating element of surrounding band bottom-heated, realize crucible bottom to lower and on temperature gradient distribution; Temperature gradient distribution is identical with gravity field, and crystal growth from top to down, is conducive to impurities removal;
2, in the process of growth, " sowing " and " shouldering " can observe the situation of crystal growth easily; " isometrical " stage adopts weighing technology accurately to control crystal growth;
3, after crystal growth enters isodiametric growth, crucible, crystal and heat exchanger neither move, and crystal growth interface is stable, mechanical disturbance, Natural convection are little, eliminates the lattice defect caused due to mechanical movement;
4, crystal is in the growth of bath surface place, does not contact, can reduce the stress of crystal significantly, prevent the parasitic nucleation of sidewall of crucible with crucible; Simultaneously can growing large-size monocrystalline under equal crucible condition, can to 90% diameter;
5, oriented seed and " necking down " technique can be used easily, the dislocation of " necking down " seed crystal is afterwards greatly reduced, reduce the dislocation desity expanding growing crystal after shoulder, thus improve perfection of crystal;
6, the amount of cooling water of the fluid of each decile of zonal control furnace wall (eight equal parts), can regulate the position of crucible temperature field cold spot, guarantees sowing and shouldering quality of crystal; After the isometrical beginning of crystal, the heat in crystals and the above region of crystal top can be cumulative, when crystal is grown up to a certain extent, solid-liquid interface can overturn, have a strong impact on crystal mass, the present invention can tune up the cooling water flow at bell place while crystal is grown up, and can take away the thermal value being collected at the above region of crystal top more, achieve crystal growth interface dimpling, close to planar interface.
The present invention is except in conjunction with except the advantage of each technique, and most outstanding feature is the gradient by regulating each piecemeal cooled region fluid amount of cooling water to control each position, warm field in whole crystal growing process, reaches the object controlling solid-liquid interface.
Method of the present invention is kyropoulos, crystal pulling method (CZ), heat-exchanging method (HEM), the terraced method of temperature (TGT) and falling crucible method combine, create the special high-temperature vacuum crystal furnace at a temperature-adjustable gradient and Wen Chang center, pass through shove charge, pumping high vacuum, temperature increasing for melting materials, wash seed crystal, real-time temperature field control, crystal pulling method is sowed, repeatedly " diameter reducing process ", crystal pulling method " shouldering technique ", crystal growth interface control (Raised key axis regulate become dimpling or close to planar interface), " isometrical technique " HEM heat exchange is in conjunction with TGT technology isodiametric growth (control diameter technology is that CZ weighs), CZ method ending & takes off crucible, in-situ annealing, produce large size high-temp oxide crystal.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
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 loaded in the crucible of multi-chamber crystal furnace, seed crystal is fixed on the bottom of the seed rod of seed rod lifting rotation mechanism, seed rod lifting rotation mechanism is connected with Weighing mechanism, covers the lid of multi-chamber crystal furnace, is pumped into 1.0 × 10 by multi-chamber crystal furnace
-3~ 1.0 × 10
-4after Pa, heating element is energized, and heats, until the melting sources in crucible becomes liquation with the speed of 4500 ~ 5000W/h;
After b, melting sources, progressively reduce heating element power with the speed of 300 ~ 500W/h and make raw material melt temperature a little more than more than fusing point 20 ~ 50 DEG C and tend towards stability, observe the cold spot position of raw material liquation simultaneously;
C, control seed rod lifting rotation mechanism, seed rod is rotated decline, the hypomere of seed crystal inserts in liquation washes seed crystal, rapid control seed rod lifting rotation mechanism, seed rod is rotated and rises and drive more than the disengaging of the seed crystal after washing liquation about 10 ~ 20mm place, and observe cold spot and whether overlap with seed crystal central position;
D, the position of departing from according to cold spot and seed crystal, regulate cold spot to depart from the cooling water flow of the rightabout burner hearth branch in seed crystal central position, guarantee that cold spot moves towards seed crystal central position; During actually operating, if cold spot position is positioned at the upper left corner at seed crystal center, then tune up the cooling water flow of furnace wall lower right position;
After e, the medullary ray of rear seed crystal to be washed overlap completely with the cold spot of liquation, constant temperature 4 ~ 6h;
F, control seed rod lifting rotation mechanism, seed rod is rotated decline, washing rear seed crystal inserts in liquation, wash after rear seed crystal inserts liquation and control seed rod lifting rotation mechanism, seed rod is made to rotate rising 2 ~ 3mm, the liquation being positioned at cold spot position is washed rear seed crystal and is mentioned and stick to and wash on rear seed crystal, and the bottom washing rear seed crystal is still in liquation, completes and sows;
G, sowed after, seed crystal lifts with the speed of 20 ~ 30mm/h, and guarantee that constriction diameters is at 15 ~ 20mm, necking down length completes necking down after 15 ~ 20mm;
H, necking down terminate rear beginning shouldering, rotating speed is 4 ~ 10rpm, pulling rate is 0.3 ~ 1.5mm/h, heating element power fall rate is 200 ~ 400W/h, in shouldering process, the flow of dynamic adjustments crystal furnace wall each chamber cooling fluid guarantees the cylindrical of shoulder state in a center of symmetry (identical with cold spot centering control principle), when crystal growth is to during from sidewall of crucible 5 ~ 10mm, complete shouldering;
I, seed rod lifting rotation mechanism stop the rotation, controlling seed rod lifting rotation mechanism makes seed rod at the uniform velocity rise with the speed of 0.1 ~ 0.5mm/h, with the rate reduction heater power of 100-300W/h, the flow of heating element temperature, each chamber in crystal furnace wall and bell cooling fluid is controlled by the weighing data of Weighing mechanism, crystal is made to keep equal diameter growth, crystal mass evenly increases, and gathering way is 3 ~ 5Kg/h;
The growth of j, crystal equal diameter terminates laggard row in-situ annealing.
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 crystal pulling method (CZ) is compared result: thought of a way by concrement vacuole, heat-exchanging method (HEM), crucible decline and the warm field design advantage of TGT, successfully achieve " plane interface growth ", solve crystal pulling method " Raised key axis growth " stress large thus cause the problem of large dislocation desity; Thought of a way by concrement vacuole, the warm field design of heat-exchanging method (HEM), falling crucible method and temperature gradient method (TGT) and growth technique advantage, larger crystal diameter (crystal of such as 110 ~ 120mm only needs the crucible internal diameter of about 130mm) can be realized in less crucible; Grow with the crystal energy consumption of size well below crystal pulling method; The crystal growth middle and later periods, major part have employed the technical characterstic of kyropoulos, avoids the interference of mechanical vibration.For kyropoulos (Kyropoulos) comparative result: to be thought of a way by concrement vacuole, the warm field design advantage of crystal pulling method, heat-exchanging method (HEM) and temperature gradient method (TGT), in conjunction with crystal pulling method technological advantage, successfully solve traditional kyropoulos produces larger thermal shocking problem when crystal growth terminates to depart from remainder melt; Control there is very large novelty in signals collecting and temperature, achieve the real-time control of crystal growth.
Method of the present invention overcomes traditional kyropoulos crystal growing process and is subject to the shortcoming (as: water temperature changes, voltage fluctuation) that extraneous factor variable effect is larger; Adopt special Method and Technology, solve the shortcoming of kyropoulos to warm field symmetrical requirements harshness; In conjunction with crystal pulling method technological advantage, first carry out repeatedly " undergauge " technique and effectively reduce dislocation on seed crystal, take elder generation's " czochralski process " " the raw technique of bubble " afterwards.Temperature gradient method (TGT), heat-exchanging method (HEM) to be compared with falling crucible method result: the technological advantage taking crystal pulling method and kyropoulos, have employed the method for top seed crystal, the seed crystal being different from temperature gradient method (TGT), falling crucible method and heat-exchanging method (HEM) is completely placed on crucible bottom; Concrement vacuole is thought of a way and the warm field design advantage of crystal pulling method, successfully solves the main drawback of falling crucible method, temperature gradient method (TGT) and heat-exchanging method (HEM): crystal contacts with sidewall of crucible thus produces stress or parasitic nucleation.Simultaneously owing to not contacting with sidewall of crucible, substantially prolongs the work-ing life of crucible; Meanwhile, solve the problem that falling crucible method, temperature gradient method (TGT) and heat-exchanging method (HEM) process of growth can not directly be observed, achieve the real-time control of crystal growth.
The equipment adopted in the present invention is the conventional equipment used in prior art.
Claims (1)
1. a method for top seed temperature gradient method growing high-temp oxide crystal, is characterized in that the method comprises the steps:
A, raw material is loaded in the crucible of multi-chamber crystal furnace, seed crystal is fixed on the bottom of the seed rod of seed rod lifting rotation mechanism, seed rod lifting rotation mechanism is connected with Weighing mechanism, covers the lid of multi-chamber crystal furnace, is pumped into 1.0 × 10 by multi-chamber crystal furnace
-3~ 1.0 × 10
-4after Pa, the heating element energising on crucible outer wall, heats with the speed of 4500 ~ 5000W/h, until the melting sources in crucible becomes liquation;
After b, melting sources, progressively reduce heating element power with the speed of 300 ~ 500W/h and make raw material melt temperature higher than more than fusing point 20 ~ 50 DEG C and tend towards stability, observe the cold heart position of raw material liquation simultaneously;
C, control seed rod lifting rotation mechanism, seed rod is rotated decline, the hypomere of seed crystal inserts in raw material liquation washes seed crystal, rapid control seed rod lifting rotation mechanism, seed rod is rotated and rises and drive more than the disengaging of the seed crystal after washing liquation 10 ~ 20mm place, and observe the cold heart and whether overlap with seed crystal central position;
D, the position of departing from according to the cold heart and seed crystal, regulate the cold heart to depart from the cooling water flow of the rightabout burner hearth branch in seed crystal central position, guarantee that the cold heart moves towards seed crystal central position;
After e, the medullary ray of rear seed crystal to be washed overlap completely with the cold heart of liquation, constant temperature 4 ~ 6h;
F, control seed rod lifting rotation mechanism, seed rod is rotated decline, washing rear seed crystal inserts in liquation, wash after rear seed crystal inserts liquation and control seed rod lifting rotation mechanism, seed rod is made to rotate rising 2 ~ 3mm, the liquation being positioned at cold heart position is washed rear seed crystal and is mentioned and stick to and wash on rear seed crystal, and the bottom washing rear seed crystal is still in liquation, completes and sows;
G, sowed after, seed crystal lifts with the speed of 20 ~ 30mm/h, and guarantee that constriction diameters is at 15 ~ 20mm, necking down length completes necking down after 15 ~ 20mm;
H, necking down terminate rear beginning shouldering, rotating speed is 4 ~ 10rpm, pulling rate is 0.3 ~ 1.5mm/h, heating element power fall rate is 200 ~ 400W/h, in shouldering process, the flow of dynamic adjustments crystal furnace wall each chamber cooling fluid guarantees the cylindrical of shoulder state in a center of symmetry, when crystal growth is to during from sidewall of crucible 5 ~ 10mm, complete shouldering;
I, seed rod lifting rotation mechanism stop the rotation, controlling seed rod lifting rotation mechanism makes seed rod at the uniform velocity rise with the speed of 0.1 ~ 0.5mm/h, with the rate reduction heating member power of 100 ~ 300W/h, the flow of heating element temperature, each chamber in crystal furnace wall and bell cooling fluid is controlled by the weighing data of Weighing mechanism, crystal is made to keep equal diameter growth, crystal mass evenly increases, and gathering way is 3 ~ 5Kg/h;
The growth of j, crystal equal diameter terminates laggard row in-situ annealing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210272246.5A CN102758255B (en) | 2012-08-02 | 2012-08-02 | Method for growing large-size high-temperature oxide crystal through for top-seeded temperature gradient technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210272246.5A CN102758255B (en) | 2012-08-02 | 2012-08-02 | Method for growing large-size high-temperature oxide crystal through for top-seeded temperature gradient technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102758255A CN102758255A (en) | 2012-10-31 |
| CN102758255B true CN102758255B (en) | 2015-05-27 |
Family
ID=47052894
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210272246.5A Active CN102758255B (en) | 2012-08-02 | 2012-08-02 | Method for growing large-size high-temperature oxide crystal through for top-seeded temperature gradient technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102758255B (en) |
Families Citing this family (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 | Method for producing lithium borate single crystal |
| JPH09328394A (en) * | 1996-06-07 | 1997-12-22 | Shin Etsu Chem Co Ltd | Method for producing oxide single crystal |
| JP2005001934A (en) * | 2003-06-11 | 2005-01-06 | Daiichi Kiden:Kk | Sapphire single crystal pulling growth equipment |
| CN1724722A (en) * | 2005-06-24 | 2006-01-25 | 哈尔滨工业大学 | Cold-heart shoulder micro-pulling method for large-size sapphire single crystals |
| WO2005053003A3 (en) * | 2003-11-25 | 2008-02-14 | Toyota Motor Co Ltd | Method of production of silicon carbide 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 (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 | Method for producing lithium borate single crystal |
| JPH09328394A (en) * | 1996-06-07 | 1997-12-22 | Shin Etsu Chem Co Ltd | Method for producing oxide single crystal |
| JP2005001934A (en) * | 2003-06-11 | 2005-01-06 | Daiichi Kiden:Kk | Sapphire single crystal pulling growth equipment |
| 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-heart shoulder micro-pulling method for large-size sapphire single crystals |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102758255A (en) | 2012-10-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102766901B (en) | The device and method of real-time, tunable Growth by Temperature Gradient Technique large size high temperature crystal | |
| CN102051674B (en) | Monocrystal ingot manufacturing device | |
| CN102162123B (en) | Dual-heater mobile-heat-shield type Czochralski crystal growing furnace | |
| CN102732947B (en) | Ingot thermal field for growing pure quasi-monocrystalline | |
| CN104651935B (en) | A kind of method that crucible rise method prepares high-quality sapphire crystal | |
| CN202558970U (en) | Single crystal like silicon ingot furnace | |
| CN102758249B (en) | A kind of preparation method of colourless boule monocrystal | |
| CN103103604B (en) | Large size C is to sapphire crystal manufacture method | |
| CN104651934B (en) | A kind of energy-saving sapphire crystal growing furnace | |
| CN102330148A (en) | Polysilicon ingot casting method with low defect and high output and thermal field structure thereof | |
| US5394825A (en) | Method and apparatus for growing shaped crystals | |
| CN209702906U (en) | A kind of single crystal growing furnace | |
| CN115216831B (en) | Crystal growth device and method capable of controlling temperature gradient | |
| CN102392293A (en) | Crystal silicon ingot furnace thermal field thermal gate control device and control method thereof | |
| CN202030860U (en) | Single crystal ingot manufacturing device | |
| CN104313680A (en) | Vertical pipe furnace apparatus for crystal growth and application method thereof | |
| CN104073875A (en) | Preparation method of large-size sapphire crystal dynamic temperature field | |
| CN202323097U (en) | Heat field and heat door control device of crystal silicon ingot furnace adopting centrosymmetric opening and closing | |
| CN102912430B (en) | Sapphire crystal growth equipment and method | |
| CN102433585B (en) | Thermal field structure of quasi-monocrystal ingot furnace | |
| CN102758255B (en) | Method for growing large-size high-temperature oxide crystal through for top-seeded temperature gradient technique | |
| CN103469305A (en) | Sapphire crystal nucleation method and special nucleation equipment therefor | |
| CN114150383A (en) | Device and method for growing high-temperature oxide crystal by seed crystal overhead improved heat exchange method | |
| CN201942779U (en) | Heat shield device applied to single crystal furnace | |
| CN105696072A (en) | Sapphire crystal growth furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20121031 Assignee: SHIHEZI XINLEI ELECTROMECHANICAL TECHNOLOGY CO., LTD. Assignor: Unionlight Technology Co., Ltd. Contract record no.: 2015320000558 Denomination of invention: Method for growing large-size high-temperature oxide crystals by using top-seeded temperature gradient method Granted publication date: 20150527 License type: Exclusive License Record date: 20150728 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model |