CN116411338A - Material boiling process for producing sapphire single crystal - Google Patents
Material boiling process for producing sapphire single crystal Download PDFInfo
- Publication number
- CN116411338A CN116411338A CN202310684672.8A CN202310684672A CN116411338A CN 116411338 A CN116411338 A CN 116411338A CN 202310684672 A CN202310684672 A CN 202310684672A CN 116411338 A CN116411338 A CN 116411338A
- Authority
- CN
- China
- Prior art keywords
- heater
- power
- crucible
- water flow
- sapphire single
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 52
- 230000008569 process Effects 0.000 title claims abstract description 49
- 238000009835 boiling Methods 0.000 title claims abstract description 40
- 239000013078 crystal Substances 0.000 title claims abstract description 39
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 36
- 239000010980 sapphire Substances 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title abstract description 32
- 239000012535 impurity Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 239000011261 inert gas Substances 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 230000002829 reductive effect Effects 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a material boiling process for producing sapphire single crystals, which belongs to the technical field of sapphire single crystal material boiling, and comprises the steps of firstly filling inert gas into equipment, operating a heater, raising the power of the heater to P1 to melt raw materials, raising the water flow V1 of a crucible shaft, raising the power of the heater to P2 after the raw materials in a crucible are melted and collapsed, raising the water flow of the crucible shaft to V2, carrying out impurity removal treatment after the raw materials in the crucible are completely melted, maintaining the power of the heater to P3, maintaining the water flow of the crucible shaft to V3, reducing the power of the heater and maintaining the power to P4 to stabilize the temperature in the equipment after the impurity removal treatment, raising the water flow of the crucible shaft to V4, and reducing the water flow of the crucible shaft to V5 after a period of time, wherein P1 is less than or equal to P2 is less than P3, and P3 is more than P4; v1 is more than or equal to V2 is more than or equal to V3 is less than or equal to V4, V4 is more than V5, and V5 is more than or equal to V2. Through the operations of inflating and increasing water flow, the impurity removing operation is enhanced and accelerated.
Description
Technical Field
The invention relates to the technical field of sapphire single crystal boiling, in particular to a boiling process for producing sapphire single crystals.
Background
The adoption of the KY method for growing the oversized high-quality sapphire crystal represents the highest level of the current sapphire preparation process. The product is a key material of the LED substrate of the current semiconductor energy-saving lighting chip and the large-scale integrated circuit substrate. The growth of large-size sapphire crystals is a future development trend, so the technology for growing high-quality crystals has a great competitive advantage.
The growth process of the KY method sapphire single crystal mainly comprises material boiling, diameter guiding, necking, shouldering, constant diameter growth and ending. The material boiling process is the process with the greatest risk in the whole sapphire single crystal production process, and accidents mainly comprise crucible deformation, material leakage, material spraying, more impurities in the material melting process and the like, so that the material boiling process is one of the reasons for higher production cost.
In the prior art, the material boiling process specifically comprises the following steps:
1. and (3) filling inert gas with the flow of 0-5L/min before melting, so as to ensure stable furnace pressure in the growth stage of the sapphire single crystal.
2. The power of the heater is regulated to slowly raise the temperature for 120h to 60-80kw, the solid sapphire raw material is completely melted into liquid state, the temperature is continuously raised for 3h, the power is increased for 5-10kw, and the temperature is stabilized for 10h, so that the material boiling and impurity removing are carried out.
3. And after the boiling, reducing the power to the seeding power every 5 hours to stabilize the temperature.
Bubbles in the sapphire single crystal by the KY method react with impurities of tungsten and molybdenum materials to generate complex gas oxides after the molten aluminum oxide is decomposed, and the boiling stage is an impurity discharging process, but in the actual production process, when the sapphire single crystal is produced by using the boiling process, impurities generated by raw materials in different stages are relatively less discharged, so that the production quality of the crystal is affected.
Disclosure of Invention
In order to overcome the defects, the invention provides a boiling process for producing sapphire single crystals, which aims to solve the problem that impurities generated by raw materials at different stages are relatively less in discharge.
The invention is realized in the following way: the invention provides a boiling process for producing sapphire single crystals, which comprises the following steps:
filling inert gas into the equipment;
the heater works, the power of the heater is increased to P1 to melt raw materials, and the water flow V1 of the crucible shaft is increased;
after the raw materials in the crucible are melted and collapsed, the power of the heater is increased to P2, and the water flow of the crucible shaft is increased to V2;
carrying out impurity removal treatment after the raw materials in the crucible are completely melted, wherein the power of a heater is maintained at P3, and the water flow of a crucible shaft is maintained at V3;
after the discharging process, reducing the heater power and maintaining at P4 to stabilize the temperature in the apparatus, and increasing the water flow rate of the crucible shaft to V4, and after a period of time, decreasing the water flow rate of the crucible shaft to V5;
wherein P1 is less than or equal to P2 and less than P3, and P3 is more than P4; v1 is more than or equal to V2 is more than or equal to V3 is less than or equal to V4, V4 is more than V5, and V5 is more than or equal to V2.
In one embodiment of the invention, p1=40-60 kw, p2=50-75 kw, p3=55-85 kw, p4=40-80 kw.
In one embodiment of the present invention, p1=50±3kw, p2=60±3kw, p3=75±3kw, p4=60±10kw.
In one embodiment of the invention, p1=45 kw, p2=55 kw, p3=65 kw, p4=60 kw.
In one embodiment of the present invention, v1=0-30L/min, v2=20-70L/min, v3=20-70L/min, v4=40-70L/min, v5=0-30L/min.
In one embodiment of the present invention, v1=20±5L/min, v2=40±5L/min, v3=40±5L/min, v4=55±5L/min, v5=20±5L/min.
In one embodiment of the invention, in the impurity removal process, the power of the heater is increased with the impurity removal time, or the power of the heater is divided into at least two sections according to the impurity removal time, and the heater power of the first section is less than the heater power of the second section.
In one embodiment of the invention, the time for the impurity removal treatment is between 3 and 50 hours.
In one embodiment of the invention, the inert gas is flushed into the device at a flow rate of 0-5L/min before the heater is operated; after the heater works, the flow rate of inert gas injected into the equipment is increased to 10-20L/min; and after the boiling process is finished, reducing the flow of inert gas to 0-10L/min.
In one embodiment of the invention, the flow of inert gas is increased during the discharge process compared to the raw material melting stage.
The beneficial effects of the invention are as follows: the material boiling process for producing the sapphire single crystal, which is obtained through the design, has the following effects:
1. the flow rate of the inert gas is increased, the circulation rate of the air flow in the furnace is accelerated, and the impurity removal is accelerated.
2. The water flow of the crucible shaft is increased, the temperature difference value of the solution at the center of the crucible and the crucible wall is increased, and the convection impurity removal of the melt is enhanced.
3. And the process is reasonably arranged, the risk occurrence probability in the production process is reduced, and meanwhile, the boiling materials and the impurity discharging are more sufficient.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a boiling process for producing sapphire single crystals according to an embodiment of the present invention;
FIG. 2 is a table of sapphire product purity (99.9996%) and elemental measurements after the use of the table 1 frit process;
fig. 3 is a table of sapphire product purity (99.9988%) and elemental measurements under conventional frit manufacturing processes.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
Examples
Referring to fig. 1 and tables 1-4, the present invention provides a technical solution: a material boiling process for producing sapphire single crystal comprises the following steps.
And (3) filling inert gas from the beginning of melting to the end of boiling, wherein the flow rate of the inert gas is 0-5L/min before the heater works, the flow rate of the air inlet is increased to 10-20L/min after the heater works, and the flow rate of the inert gas needs to be reduced to 0-10L/min after the boiling process is completed. Specifically, under the high temperature condition, tungsten and molybdenum materials and solid raw materials are melted to burn out a large amount of impurities, wherein a part of impurities exist in a gaseous state, the sufficient inert gas flow can accelerate the gas flow circulation rate in the furnace, and the gaseous impurities can be discharged through the gas flow circulation to reduce the residual amount of the impurities, so that the production quality of crystals is improved.
The crucible bearing carries the crucible, and simultaneously, the crucible bearing is directly contacted with the bottom of the furnace to provide a channel for heat conduction, and the water flow is gradually increased from 0L/min to 70L/min. When the water flow of the crucible shaft is increased to 40-60L/min, the heat conduction of the lower part is increased after the water cooling effect is enhanced, and the solution temperature difference between the center of the crucible and the wall of the crucible is increased in the high-temperature melt boiling stage, so that the convection of the solution is enhanced, and the impurity removal rate is accelerated.
In order to ensure the normal speed pushing of the solid-liquid interface in the single crystal growth stage, the water flow of the crucible shaft is regulated back to the numerical value before modification after the material boiling process is finished, the water cooling effect of the crucible shaft is ensured to be normal, a relatively proper and stable cold center area is formed by melt in the pot, the formation of micro convex surfaces of the solid-liquid growth interface is facilitated in the shoulder-placing and constant diameter stage of the crystal, and the discharge of bubbles in the crystal growth stage is facilitated by the micro convex surface of the solid-liquid interface, so that high-quality crystals are facilitated.
Heating, namely, after heating is started, heating power P1 is regulated to be within the range of 40kw-60kw, and the temperature is quickly increased. Wherein, the power of P1 is preferably adjusted to 50+ -3 kw, and further, the power of P1 is preferably 45kw. The water flow V1 of the crucible shaft is regulated to 0-30L/min, and the optimal water flow V1 is 20+/-5L/min. Due to the characteristic of the heating hysteresis of the power of the heater of the large furnace platform, the temperature rise is slow in a short time and basically not influenced on the thermal field piece.
And when other parameters are unchanged, the raw materials in the crucible absorb heat and collapse, and the maintaining time is about 2-2.5 h. The alumina raw material in the middle and lower part of the crucible will melt first in the heated stage, and then the material in the upper part of the crucible will fall down, which requires attention to the collapse time and the corresponding heater power to be recorded.
After the raw materials in the crucible are melted and collapsed, the heating power P2 is kept to be 50-75kw, wherein the power of the P2 is preferably adjusted to be 60+/-3 kw, and further, the power of the P2 is preferably 55kw. The water flow rate of the crucible shaft is raised to v2=20-70L/min, and is optimally 40±5L/min. In the actual production process, the condition that part of raw materials are continuously adhered to the inner wall of the crucible can occur when the materials collapse, if the adhesive materials are adhered to the inner wall of the crucible for a long time and are not changed, the crystal and the adhesive materials are scratched or even blocked when the crystal growth is completed to separate from the solution, and the crystal liquid removal failure is caused. Meanwhile, the partial temperature drop is caused by the heat absorption of the collapsed material melting, and the melted raw material is likely to be recrystallized due to the temperature drop, so that the spraying is easy to occur. The heating of the power is carried out at the stage to accelerate the melting of the binder, prevent the local temperature of the liquid surface from being too low for crystallization, and reduce the risk of abnormal production process.
And (3) carrying out impurity removal treatment after the raw materials in the crucible are completely melted, and continuously raising the power P3 of the heater to 55-85kw and maintaining. Wherein, the power of P3 is preferably increased to 75+/-3 kw, preferably, the power of the heater is continuously increased to 65kw after the raw material is changed from solid state to liquid state by absorbing heat, the impurity discharging time is preferably controlled between 3 and 50h, and the 4h boiling time is prolonged. At the moment, the solution heat convection rate is strongest at the highest temperature, and the raw materials are fully melted under the environment, so that the boiling of the raw materials is more fully favorable for impurity removal. The impurity removal stage requires an increased inert gas introduction amount compared to the raw material melting stage. In this stage, the power of the heater increases with the time of the impurity removal, or the power of the heater is divided into at least two sections by the time of the impurity removal, the heater power of the first section < the heater power of the second section.
After the draining process, the heater power is reduced and maintained at P4 to stabilize the temperature within the apparatus, and the water flow rate of the crucible shaft is increased to V4, and after a period of time, the water flow rate of the crucible shaft is reduced to V5, specifically p4=40-80 kw, which may be 60±10kw, or more preferably, the power is 60kw. And v4=40-70L/min, more preferably 55±5L/min. After stabilizing for a period of time, the water flow V5 of the crucible shaft needs to be reduced to 20+/-5L/min. After the material is fully boiled, the power is slowly reduced to seeding power to stabilize the temperature, the lower shaft water flow is recovered and changed to a numerical value before the temperature is stabilized, and the inert gas argon flow is recovered to 2L/min optimally, so that the later seeding and shouldering operations are facilitated.
Table 1: based on speculation, experiments are carried out under a boiling process with fixed power and fixed water flow, and the purity of the product is obviously improved
Experimental data: in the project of improving the boiling process, the purity of the sapphire product under the condition is found to be 99.9996% (refer to figure 2 of the specification) which is higher than the purity of 99.9988% of the sapphire product obtained under the traditional boiling process (refer to figure 3 of the specification); specifically, the content of Ga element was significantly reduced from conventional 10 PPM.WT to 0.1 PPM.WT or less.
Conclusion of experiment: under the conditions of the power and the water flow, the purity of the product is obviously improved; and obtaining the optimal process condition by experience and experiment.
Table 2: setting power and adjusting water flow to prove the effect of water flow on purity
Experimental data: the content of Ga element is reduced by slightly fluctuation of other elements, and the content of Ga element is fluctuated between 10.6 and 7.9 PPM.WT by the conventional 10 PPM.WT.
Summary of the experiment: under the power condition, the water flow has an upper limit on the effect of purity, the optimal range of the water flow is v1=20±5L/min, v2=40±5L/min, v3=40±5L/min, v4=55±5L/min, and v5=20±5L/min; the purity of the sapphire product is favorably controlled to be near 99.9990 percent.
Table 3: setting water flow and adjusting power to demonstrate the effect of power on purity
Experimental data: the contents of three elements of Na, si and Cl are increased; the content of Ga element is obviously reduced and fluctuates between 9.1 PPM.WT and 0.1 PPM.WT.
Summary of the experiment: the power has great influence on the purity, and particularly plays a key role in the impurity removal of Ga element; however, the impurity removing effect of a part of the elements is rather reduced while the Ga element is being removed. In the experiment, the optimal power group is p1=45kw, p2=55kw, p3=65kw, p4=60 kw, and the sapphire product purity is stabilized around 99.9996%, even 99.9997%.
Referring to fig. 2 and 3, according to the change of the total purity, the purity can be improved by a material boiling process, the tungsten-molybdenum thermal field element and partial impurities burnt by the raw materials at high temperature are volatilized in a gaseous state in a heating and temperature raising stage, and the gas circulation in the furnace is quickened by increasing the flow of inert gas filled in the material boiling stage, so that the impurities are discharged and the residual quantity is reduced.
The heater is used as a heating source to provide heat through radiation to act on the crucible and the heat preservation layer, and the heat preservation layer reduces heat loss and provides a proper temperature gradient to be beneficial to normal growth of crystals. The crucible then applies heat to the feedstock by thermal conduction. Because the bottom and the side of the crucible are heated at the same time, the temperature of the lower part rises relatively fast, the solid raw material at the lower part of the crucible is melted preferentially, so that the phenomenon of material collapse occurs, and the final solid raw material absorbs heat and is melted into liquid state completely through process temperature rising control.
One end of the crucible shaft supports the crucible, and the other end of the crucible shaft contacts with the furnace bottom.
Specifically, the working principle of the boiling process for producing the sapphire single crystal is as follows: inert gas is introduced in the process from the beginning of dissolving material to the boiling of material, and the water flow of a crucible shaft is increased in the boiling process, so that the crucible shaft is rapidly subjected to impurity discharging treatment, and meanwhile, the crucible shaft is continuously heated in the dissolving material and boiling process, so that raw materials are melted, the materials adhered to the inner wall can be melted, the solution heat convection rate is enhanced under the high temperature condition, the raw materials are further fully melted, the boiling is more sufficient, and the impurity discharging is facilitated.
It should be noted that, specific model specifications of the heater need to be determined by selecting a model according to actual specifications of the device, and a specific model selection calculation method adopts the prior art in the field, so detailed description is omitted.
The power supply of the heater and its principle will be clear to a person skilled in the art and will not be described in detail here.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A boiling process for producing sapphire single crystals, which is characterized by comprising the following steps:
filling inert gas into the equipment;
the heater works, the power of the heater is increased to P1 to melt raw materials, and the water flow V1 of the crucible shaft is increased;
after the raw materials in the crucible are melted and collapsed, the power of the heater is increased to P2, and the water flow of the crucible shaft is increased to V2;
carrying out impurity removal treatment after the raw materials in the crucible are completely melted, wherein the power of a heater is maintained at P3, and the water flow of a crucible shaft is maintained at V3;
after the discharging process, reducing the heater power and maintaining at P4 to stabilize the temperature in the apparatus, and increasing the water flow rate of the crucible shaft to V4, and after a period of time, decreasing the water flow rate of the crucible shaft to V5;
wherein P1 is less than or equal to P2 and less than P3, and P3 is more than P4; v1 is more than or equal to V2 is more than or equal to V3 is less than or equal to V4, V4 is more than V5, and V5 is more than or equal to V2.
2. The process for producing a sapphire single crystal according to claim 1, wherein p1=40-60 kw, p2=50-75 kw, p3=55-85 kw, p4=40-80 kw.
3. A process for producing a sapphire single crystal according to claim 2, wherein p1=50±3kw, p2=60±3kw, p3=75±3kw, p4=60±10kw.
4. A process for producing a sapphire single crystal according to claim 2, wherein p1=45 kw, p2=55 kw, p3=65 kw and p4=60 kw.
5. The process for producing a sapphire single crystal according to claim 1, wherein v1=0-30L/min, v2=20-70L/min, v3=20-70L/min, v4=40-70L/min, v5=0-30L/min.
6. The process of claim 5, wherein v1=20±5L/min, v2=40±5L/min, v3=40±5L/min, v4=55±5L/min, v5=20±5L/min.
7. The process for producing a sapphire single crystal according to claim 1, wherein the power of the heater is increased with the impurity removal time or the power of the heater is divided into at least two sections by the impurity removal time in the impurity removal process, and the heater power of the first section is less than the heater power of the second section.
8. The process for producing a sapphire single crystal according to claim 7, wherein the time for the impurity removal treatment is 3-50 hours.
9. The process for producing a sapphire single crystal according to claim 1, wherein the flow rate of inert gas introduced into the apparatus before the operation of the heater is 0-5L/min; after the heater works, the flow rate of inert gas injected into the equipment is increased to 10-20L/min; and after the boiling process is finished, reducing the flow of inert gas to 0-10L/min.
10. The boiling process for sapphire single crystal according to claim 9, wherein the flow rate of inert gas is increased in the impurity removal process stage as compared to the raw material melting stage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310684672.8A CN116411338A (en) | 2023-06-12 | 2023-06-12 | Material boiling process for producing sapphire single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310684672.8A CN116411338A (en) | 2023-06-12 | 2023-06-12 | Material boiling process for producing sapphire single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116411338A true CN116411338A (en) | 2023-07-11 |
Family
ID=87053011
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310684672.8A Pending CN116411338A (en) | 2023-06-12 | 2023-06-12 | Material boiling process for producing sapphire single crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116411338A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162130A (en) * | 2011-05-26 | 2011-08-24 | 浙江昀丰新能源科技有限公司 | Preparation method of sapphire monocrystalline |
| CN103173855A (en) * | 2013-03-12 | 2013-06-26 | 贵阳嘉瑜光电科技咨询中心 | Method for growing HEM crystal under protection of inert gas |
| CN103614765A (en) * | 2013-10-31 | 2014-03-05 | 中国科学院上海光学精密机械研究所 | Method of heating graphite to grow sapphire crystal |
| CN103741206A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Polycrystalline silicon ingot casting molten material and impurity removing process |
| CN104109904A (en) * | 2014-05-27 | 2014-10-22 | 上海佳宇信息技术有限公司 | Seeding method of sapphire crystal growth kyropoulos method |
| CN104695010A (en) * | 2014-12-26 | 2015-06-10 | 浙江东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
| CN107130289A (en) * | 2017-06-13 | 2017-09-05 | 江苏吉星新材料有限公司 | A kind of growing method for improving heat exchange large size sapphire crystal |
| CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
| CN108588832A (en) * | 2018-04-28 | 2018-09-28 | 内蒙古恒嘉晶体材料有限公司 | Prepare the improved kyropoulos and crystal growing furnace of sapphire crystal |
-
2023
- 2023-06-12 CN CN202310684672.8A patent/CN116411338A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102162130A (en) * | 2011-05-26 | 2011-08-24 | 浙江昀丰新能源科技有限公司 | Preparation method of sapphire monocrystalline |
| CN103173855A (en) * | 2013-03-12 | 2013-06-26 | 贵阳嘉瑜光电科技咨询中心 | Method for growing HEM crystal under protection of inert gas |
| CN103614765A (en) * | 2013-10-31 | 2014-03-05 | 中国科学院上海光学精密机械研究所 | Method of heating graphite to grow sapphire crystal |
| CN103741206A (en) * | 2014-01-28 | 2014-04-23 | 西安华晶电子技术股份有限公司 | Polycrystalline silicon ingot casting molten material and impurity removing process |
| CN104109904A (en) * | 2014-05-27 | 2014-10-22 | 上海佳宇信息技术有限公司 | Seeding method of sapphire crystal growth kyropoulos method |
| CN104695010A (en) * | 2014-12-26 | 2015-06-10 | 浙江东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
| CN107130289A (en) * | 2017-06-13 | 2017-09-05 | 江苏吉星新材料有限公司 | A kind of growing method for improving heat exchange large size sapphire crystal |
| CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
| CN108588832A (en) * | 2018-04-28 | 2018-09-28 | 内蒙古恒嘉晶体材料有限公司 | Prepare the improved kyropoulos and crystal growing furnace of sapphire crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2016041242A1 (en) | Quartz crucible used for repeatedly pulling monocrystalline silicon for multiple times and manufacturing method therefor | |
| CN102220633B (en) | Production technology of semiconductor grade silicon single crystal | |
| CN105019017A (en) | Method used for reducing oxygen content of czochralski silicon | |
| CN102220634B (en) | Method to raise production efficiency of czochralski silicon mono-crystal | |
| KR20010101045A (en) | Production method for silicon single crystal and production device for single crystal ingot, and heat treating method for silicon single crystal wafer | |
| JP4781020B2 (en) | Silica glass crucible for pulling silicon single crystal and method for producing quartz glass crucible for pulling silicon single crystal | |
| TWI774174B (en) | Seeding method for crystal growth | |
| JP2008019125A (en) | Method of melting semiconductor wafer base material and method of growing semiconductor wafer crystal | |
| CN117364225B (en) | Crystal growing method by co-rotating crystal and crucible | |
| JP2007326780A (en) | Method for producing quartz glass crucible for pulling up silicon single crystal | |
| CN104674339A (en) | Method for reducing crystal boundary in process of growing large sapphire by virtue of kyropoulos method | |
| JP6855358B2 (en) | Quartz glass crucible for pulling silicon single crystal | |
| CN116411338A (en) | Material boiling process for producing sapphire single crystal | |
| KR102038960B1 (en) | Silicon single crystal manufacturing method | |
| CN102719883B (en) | Semiconductor monocrystal silicon production process | |
| JP2008266090A (en) | Silicon crystal material and method for manufacturing fz (floating-zone) silicon single crystal using the material | |
| JP2016183071A (en) | Manufacturing method of silicon single crystal | |
| CN105483818B (en) | A kind of M2 types monocrystalline silicon shouldering method | |
| KR101105547B1 (en) | Heater used for manufacturing single crystal, Apparatus and Method of manufacturing single crystal using the same | |
| JP5685894B2 (en) | Quartz glass crucible, method for producing the same, and method for producing silicon single crystal | |
| JP2009242237A (en) | Apparatus and method for producing single crystal ingot | |
| CN115074827A (en) | Method for reducing oxygen content of single crystal head | |
| KR101855814B1 (en) | Process for producing single-crystal silicon | |
| CN115557521B (en) | Method for controlling impurity migration in fused magnesium melting preparation process and electrode angle adjusting device | |
| JP7150250B2 (en) | Quartz glass crucible and method for manufacturing quartz glass crucible |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20230711 |
|
| RJ01 | Rejection of invention patent application after publication |