CN105696071A - Process method capable of effectively overcoming Kyropoulos-method crystal cracking - Google Patents
Process method capable of effectively overcoming Kyropoulos-method crystal cracking Download PDFInfo
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- CN105696071A CN105696071A CN201610173841.1A CN201610173841A CN105696071A CN 105696071 A CN105696071 A CN 105696071A CN 201610173841 A CN201610173841 A CN 201610173841A CN 105696071 A CN105696071 A CN 105696071A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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- Crystallography & Structural Chemistry (AREA)
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a process method capable of effectively overcoming Kyropoulos-method crystal cracking. The process method specifically comprises a process method for preventing the large area of the bottom of a crystal from being stuck to a crucible in a crystal growth process and releasing the crystal from the crucible after the growth is ended. By controlling a pulling speed and a cooling speed at the later period of equal-diameter growth, the growth speed of the crystal becomes slow; the crystal is released from a wall of the crucible through regulating a voltage value and manipulating a pulling rod. With the adoption of the process method disclosed by the invention, a condition that the large area of the bottom of the growing crystal is stuck to the crucible can be effectively prevented, and the diameter consistency of the crystal is good; in a cooling process, the crystal is separated from the wall of the crucible, so that the heat stress of the crystal is reduced, the probability of the crystal cracking is greatly reduced, and the yield and the sampling rate of the crystal are improved; the growth period can be easily shortened and the production cost is reduced.
Description
Technical field
The present invention relates to kyropoulos field of crystal growth, particularly relate to a kind of method that can effectively solve crystal cleavage in kyropoulos sapphire crystal growth process。
Background technology
Sapphire crystal (is commonly called as corundum), have high-melting-point, high rigidity, heat conductivity good, from vacuum, ultraviolet, visible, from near-infrared to mid-infrared, all have the excellent properties such as higher light transmission, in addition, sapphire crystal has the resistance to dissolubility of high temperature, good chemical stability, it it is excellent laser host material, it it is the window material of various optical element, infrared military installation and high intensity laser beam, it is widely used in blue-light semiconductor diode (LED) and the backing material of diode LD, almost throughout all substrate fields。
Current sapphire growing method mainly has czochralski method (CZ), EFG technique (EFG), kyropoulos (KY), heat-exchanging method (HEM) etc.。Wherein kyropoulos has the optimum temperature gradation of sapphire growth, is one of main stream approach being best suitable for growing large-size sapphire single-crystal of generally acknowledging in the world。Ideally, in growth course, crystal should not contact with crucible, but due to the solid-liquid interface shape of dimpling and the bigger thermograde of crucible bottom, cause isodiametric growth of crystal later stage excessive velocities to be difficult to control to, be prone to the viscous crucible of sidewall of crucible phase Adhesion formation large area bottom crystal, cause that in cooling procedure, crystal thermal stress is excessive, cause cracking, greatly reduce the yield rate of crystal and rate of drawing materials, and growth cycle can be extended, increase production cost。
Summary of the invention
For overcoming the problems referred to above, the present invention provides a kind of process that can effectively solve kyropoulos crystal cleavage, by controlling the speed of growth of crystal in the isodiametric growth later stage, prevent bottom crystal, occur that large area glues crucible, having yield rate height, growth cycle is short, the advantage that production cost is low。
The technical solution adopted for the present invention to solve the technical problems is: a kind of process that can effectively solve kyropoulos crystal cleavage, comprises the steps:
1. alumina raw material is loaded in Kyropoulos furnace crucible according to the inventory preset, lifting rod installs seed crystal, evacuation, start heating system and make melting sources；After raw material melts completely, find suitable seeding temperature and start seeding, seeding complete after according to the kyropoulos technique initialization rate of pulling and rate of temperature fall, make crystal enter shouldering, isodiametric growth stage。
As a further improvement on the present invention, in above-mentioned material process, initially with higher heating rate up voltage, it is generally 500-2000mv/h, after 8-15h, namely when voltage is 8500-9000mv, then adopt less heating rate up voltage, be generally 100-600mv/h, until being finally reached material voltage, this material voltage is 9300mv ± 100mv, so controls to can ensure that raw material is heated evenly, can reduce the injury to crucible simultaneously。
Further, in seeding process, the diameter of brilliant knot is 0-40mm。
The rate of pulling that seeding sets after completing is less than 0.5mm/h, and rate of temperature fall is less than 15mv/h。
2. when after the 1/2-3/4 of crystal growth to step 1. middle inventory, the rate of pulling is raised 5-8 times by step basis 1., rate of temperature fall is decreased to original 1/4-3/4 so that the speed of growth of crystal is reduced to the 1/3-3/4 of isodiametric growth stage length speed, carries out isometrical ending growth。
3. when crystal weight reach step 1. in inventory after, on step basis 2., continue to raise rate of pulling 5-8 times, increase rate of temperature fall 5-7 times, until crystal weight exceedes the 10-30kg of inventory, it is ensured that after crystal growth, stopping lifts。
Further, when crystal weight exceedes more than the 30kg of inventory, lift need to be suspended, lift again until weight is down to inventory ± 20kg。
4. bring the voltage up to step 1. in seeding complete time magnitude of voltage ± 200mv, along with temperature raises, crystal weight can be gradually reduced, and meanwhile slowly lifts up lifting rod until crystal mass is stable at inventory ± 2kg, stop lift, check that crystal whether and has gap between sidewall of crucible。Preferably, the above-mentioned rate of pulling is 1-15mm/min, and the lift time is 5-30mm。
As a further improvement on the present invention, bring the voltage up to seeding complete time magnitude of voltage time less than 30min, crystal melting otherwise can be caused serious。
Further, check according to the situation of rocking of lifting rod, whether and to have the method in gap between sidewall of crucible be slightly stir lifting rod to crystal, judges that whether crystal is mutually bonding with sidewall of crucible, every 1-30min judgement once。
Magnitude of voltage when 5. voltage recovery to step 3. being terminated, observes 20-90min, it is determined that crystal does not occur that secondary glues crucible, and the de-crucible of crystal is successfully entered temperature-fall period。
As the further improvement of the present invention, if above-mentioned steps 4. with 5. in occur that crystal is mutually bonding with sidewall of crucible, then 4. and 5. need to repeat step, until the de-crucible success of crystal, namely between crystal and sidewall of crucible, have gap。
For preventing viscous crucible further, after step 5. de-crucible success, also include adjusting lifting rod position, make crystal be in the RC step of crucible。
Above-mentioned process is applicable not only to growing sapphire crystal, is also adaptable for growth YAG serial crystal, Ti∶Sapphire laser, the contour melting crystals of scintillation crystal, does not repeat them here。
Beneficial effects of the present invention: the present invention passes through the control in the isodiametric growth later stage to the rate of pulling, rate of temperature fall so that crystal length speed slows down, in addition by regulation voltage level and manipulation lifting rod so that crystal and sidewall of crucible are separated。The present invention can effectively prevent the generation of the viscous crucible of large area bottom growth crystal, and crystal diameter concordance is good, owing in cooling procedure, crystal separates with sidewall of crucible, thus reduce the thermal stress of crystal, greatly reduce the probability of crystal cleavage, improve the yield rate of crystal and rate of drawing materials, advantageously reduce growth cycle, reduce production cost。
Below with reference to embodiment, the present invention is described in detail。
Detailed description of the invention
Embodiment 1,
A kind of process solving 40kg level sapphire crystal kyropoulos cracking, comprises the steps:
1. 40kg alumina raw material is loaded in Kyropoulos furnace crucible, lifting rod installs seed crystal, evacuation, start heating system and make melting sources。In above-mentioned material process, initially with higher heating rate up voltage, it is generally 500-2000mv/h, after 12h when close to material voltage and 9000mv, adopt less heating rate up voltage again, be generally 100-600mv/h, until being finally reached material voltage 9300mv ± 100mv。
After raw material melts completely, finding suitable seeding temperature and start seeding, the diameter of brilliant knot is 0-50mm。Seeding complete after according to the kyropoulos technique initialization rate of pulling and rate of temperature fall, make crystal enter shouldering, isodiametric growth stage。The rate of pulling set is as 0-0.5mm/h, and rate of temperature fall is 0-15mv/h。
2. when after crystal growth to 20-30kg, on step basis 1., the rate of pulling being raised 0.2-2mm/h, rate of temperature fall reduces 2-6mv/h so that the speed of growth of crystal is reduced to 200-700g/h, carries out isometrical ending growth。
3., after crystal growth reaches 40kg, step basis 2. is continued raise rate of pulling 0.2-2mm/h, and change rate of temperature fall into 8-20mv/h, until crystal weight reaches 50-65kg, it is ensured that after crystal growth, stop lift。
4. bring the voltage up to step 1. in seeding complete time magnitude of voltage 9000mv, manually slowly lift up lifting rod 5-30mm with the rate of pulling of 1-15mm/min, until crystal mass is stable at 38-42kg, stop lift。
Check that crystal whether and has gap between sidewall of crucible, concrete, slightly stir lifting rod, judge that whether crystal is mutually bonding with sidewall of crucible according to the situation of rocking of lifting rod, every 1-30min judgement once。
Further, bring the voltage up to seeding complete time magnitude of voltage time less than 30min, crystal melting otherwise can be caused serious。
Magnitude of voltage when 5. voltage recovery to step 3. being terminated, observes 20-90min, it is determined that crystal does not occur that secondary glues crucible, and the de-crucible of crystal is successfully entered temperature-fall period。
If above-mentioned steps 4. with 5. in occur that crystal is mutually bonding with sidewall of crucible, then 4. and 5. need to repeat step, until the de-crucible success of crystal, namely between crystal and sidewall of crucible, have gap。
Embodiment 2,
A kind of process solving 80kg level sapphire crystal kyropoulos cracking, comprises the steps:
1. 80kg alumina raw material is loaded in Kyropoulos furnace crucible, lifting rod installs seed crystal, evacuation, start heating system and make melting sources。In above-mentioned material process, initially with higher heating rate up voltage, being generally after 500-2000mv/h, 14h when close to material voltage, then adopt less heating rate up voltage, being generally 100-600mv/h, until being finally reached material voltage。
After raw material melts completely, finding suitable seeding temperature and start seeding, the diameter of brilliant knot is 0-50mm。Seeding complete after according to the kyropoulos technique initialization rate of pulling and rate of temperature fall, make crystal enter shouldering, isodiametric growth stage。The rate of pulling set is as 0-0.4mm/h, and rate of temperature fall is 0-8mv/h。
2. when after crystal growth to 40-60kg, on step basis 1., the rate of pulling being raised 0.2-2mm/h, rate of temperature fall reduces 2-6mv/h so that the speed of growth of crystal is reduced to 200-700g/h, carries out isometrical ending growth。
3., after crystal growth reaches 80kg, step basis 2. is continued raise rate of pulling 0.2-2mm/h, and change rate of temperature fall into 8-20mv/h, until crystal weight reaches 90-100kg, it is ensured that after crystal growth, stop lift。
Further, when crystal weight exceedes more than the 30kg of inventory, lift need to be suspended, lift again until weight is down to inventory ± 20kg。
4. bring the voltage up to step 1. in seeding complete time magnitude of voltage ± 200mv, meanwhile slowly lift up lifting rod 5-30mm, until crystal mass is stable at inventory 78-82kg, stop lift, check that crystal whether and has gap between sidewall of crucible。
Preferably, the rate of pulling of lifting rod is 1-15mm/min。Bring the voltage up to seeding complete time magnitude of voltage time less than 30min, crystal melting otherwise can be caused serious。
Further, check according to the situation of rocking of lifting rod, whether and to have the method in gap between sidewall of crucible be slightly stir lifting rod to crystal, judges that whether crystal is mutually bonding with sidewall of crucible, every 1-30min judgement once。
Magnitude of voltage when 5. voltage recovery to step 3. being terminated, observes 20-90min, it is determined that crystal does not occur that secondary glues crucible, after the de-crucible success of crystal, adjusts lifting rod position, makes crystal be in crucible center, subsequently enter temperature-fall period。
If above-mentioned steps 4. with 5. in occur that crystal is mutually bonding with sidewall of crucible, then need to repeat step 4. and 5. repeatedly, until the de-crucible success of crystal, namely between crystal and sidewall of crucible, have gap。
The above is only to presently preferred embodiments of the present invention; not the scope of the present invention is defined; therefore under the premise designing spirit without departing from the present invention; the equivalence that structure of the present invention, feature and principle are done by those of ordinary skill in the art changes or decoration, all should fall within the scope of protection of the present invention。
Claims (9)
1. the process that can effectively solve kyropoulos crystal cleavage, it is characterised in that comprise the steps:
1. alumina raw material is loaded in Kyropoulos furnace crucible according to the inventory preset, lifting rod installs seed crystal, evacuation, start heating system and make melting sources；After raw material melts completely, find suitable seeding temperature and start seeding, seeding complete after according to the kyropoulos technique initialization rate of pulling and rate of temperature fall, make crystal enter shouldering, isodiametric growth stage；
2. when after the 1/2-3/4 of crystal growth to step 1. middle inventory, the rate of pulling is raised 5-8 times by step basis 1., rate of temperature fall is decreased to original 1/4-3/4 so that the speed of growth of crystal is reduced to the 1/3-3/4 of isodiametric growth stage length speed, carries out isometrical ending growth；
3. when crystal weight reach step 1. in inventory after, on step basis 2., continue to raise rate of pulling 5-8 times, increase rate of temperature fall 5-7 times, until crystal weight exceedes the 10-30kg of inventory, it is ensured that after crystal growth, stopping lifts；
4. bring the voltage up to step 1. in seeding complete time magnitude of voltage ± 200mv, meanwhile slowly lift up lifting rod until crystal mass is stable at inventory ± 2kg, stop lift, check that crystal whether and has gap between sidewall of crucible；
Magnitude of voltage when 5. voltage recovery to step 3. being terminated, observes 20-90min, it is determined that crystal does not occur that secondary glues crucible, and the de-crucible of crystal is successfully entered temperature-fall period。
2. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 1, it is characterized in that, step 1. in the material stage, initially with higher heating rate up voltage, its heating rate is after 500-2000mv/h, 8-15h, namely when voltage is 8500-9000mv, adopting less heating rate up voltage again, this heating rate is 100-600mv/h, until being finally reached material voltage。
3. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 1, it is characterised in that in the step rate of pulling that 1. middle seeding sets after completing less than 0.5mm/h, rate of temperature fall is less than 15mv/h。
4. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 1, it is characterised in that step 3. in, if crystal weight exceedes more than the 30kg of inventory, lift need to be suspended, lift again until weight is down to inventory ± 20kg。
5. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 1, it is characterised in that step 4. described in the rate of pulling of lifting rod be 1-15mm/min, the lift time is 5-30mm。
6. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 1, it is characterised in that step 4. in bring the voltage up complete to seeding time magnitude of voltage time less than 30min。
7. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 1, it is characterized in that, step 4. described in check that crystal whether and has the method in gap and is between sidewall of crucible, slightly stir lifting rod, the situation of rocking according to lifting rod judges that whether crystal is mutually bonding with sidewall of crucible, judges once every 1-30min。
8. can effectively solve the process of kyropoulos crystal cleavage as described in any one of claim 1 to 7, it is characterized in that, described step 4. or 5. in if there is the crystal situation mutually bonding with sidewall of crucible, then 4. and 5. need to repeat step, until the de-crucible success of crystal。
9. can effectively solve the process of kyropoulos crystal cleavage as claimed in claim 8, it is characterised in that after step 5. de-crucible success, also include adjusting lifting rod position, make crystal be in the RC step of crucible。
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Application publication date: 20160622 |