CN103966668A - Growth method for controlling diameter of rod-like sapphire crystal based on protective atmosphere - Google Patents
Growth method for controlling diameter of rod-like sapphire crystal based on protective atmosphere Download PDFInfo
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Abstract
The invention relates to a growth method for controlling the diameter of a rod-like sapphire crystal based on a protective atmosphere. An airflow introduction passage is distributed around the upper end of a mold within a thermal field when a crystal is grown, gas flowing in from the airflow introduction passage performs convection heat dissipation on the upper end of the mold, and the heat dissipation strength of the mold is controlled by adjusting the flow rate of the gas so as to adjust the thickness of a liquid film at the solid-liquid interface of the crystal and change the size and shape of a sapphire product; the purpose of changing the diameter of the crystal is fulfilled by controlling the flow rate of the gas scouring the surface of the mold based on the size and shape of the sapphire; when the diameter of the grown crystal needs to be increased, the velocity of the gas flowing into the airflow passage can be increased; when the diameter of the grown crystal needs to be reduced, the velocity of the gas flowing into the airflow passage can be reduced. The growth method disclosed by the invention has the advantages that the shape of the grown crystal is controlled by adopting the method of cooling the mold with gas flow, so that the influence of external disturbance on the shape of the crystal can be overcome in the growth process; in addition, the growth method can also be used for growing a crystal in a specific shape.
Description
Technical field
A kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control of the present invention belongs to crystal technique field, particularly a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control.
Background technology
Guided mode method, claims again EFG method, is a kind of growing method that by mould, liquation is frozen into crystal.When raw material is by after heater heats, raw material is melted into liquation in crucible, and liquation, by the mould lower end being placed in liquation, imports to mould upper end by wicking action, and forms liquid film (claiming again melt films) at mould upper end face.Under the control of suitable thermograde, seed crystal completes seeding after contacting with the liquid film of mould upper end, by the uniform velocity the lifting of seed crystal, makes liquid film constantly solidify formation monocrystalline.The shape of monocrystalline determines by the shape of mould upper surface, and the process of guided mode method growth rhabdolith can application reference number be 2012100179402 patent.Crystal growing process is divided into the steps such as seeding, shouldering, isometrical (or wide) growth, and the target that will control in crystal growing process is the crystal that grows specified shape.Be used to form the parts of environment of crystal growth, comprise that crucible, mould, well heater, lagging material etc. are referred to as thermal field (Hot Zone).
In current guided mode method is grown the process of bar-shaped sapphire crystal, the shape of crystal is difficult to control conventionally, if thermal field (Hot Zone) in the process of crystal growth all the time in stable insulation and heat-processed, can grow the uniform crystal of shape; If due to external disturbance (furnace pressure variation, heating current fluctuation, air-flow condition variation etc.), the shape of crystal also can change because of disturbance, make the size of crystal become large or diminish; Taking growth cylindrical crystal as example, without crystal growth control means in the situation that, the target shape growing is columniform sapphire crystal, but often becomes lageniform crystal under external disturbance.
In special sector application, need to there is the sapphire crystal of special shape, such as the sapphire crystal for ornament, therefore, in crystal growing process, can change in real time crystallographic dimension, just become a kind of demand, through retrieval related documents, do not find the technical scheme identical with the present invention.
Summary of the invention
The technical problem to be solved in the present invention is to provide one can overcome external environment impact, and the grow method of bar-shaped sapphire crystal of the guided mode method that can grow specified shape.
For solving the problems of the technologies described above; technical scheme of the present invention is: a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control; its innovative point is: around the upper end of mould when crystal growth in thermal field, be furnished with air-flow introduction passage; the gas flowing into from air-flow introduction passage carries out heat loss through convection to mould upper end; the specific heat load of controlling mould by the flow velocity of adjustments of gas regulates the thickness of crystal solid-liquid interface place liquid film, changes the size and dimension of sapphire product.
Further, the size and dimension of described sapphire product is to be determined by the diameter of sapphire crystal, the air-flow velocity that can wash away die surface by control is controlled the diameter of sapphire crystal, in the time the crystal diameter of growth need to being strengthened, can increase the gas velocity of inlet air flow stream passage; In the time the crystal diameter of growth need to being reduced, can reduce the gas velocity of inlet air flow stream passage.
Further, in described air-flow introduction passage, the pass of the diameter of gas flow rate and die surface is:
①
②
③
Wherein
represent Nu Saier number, Tm represent die temperature, Tg represent gas flow temperature,
represent that the thermal conductivity of gas, characteristic length, the q that L represents mould are due to the heat flow rate per unit area that wash away increase of air-flow to mould; H represent melt films thickness, v represent seed crystal pull rate,
represent latent heat,
represent melt thermal conductivity,
represent that thermal conductivity, Tc and the Ti of crystal represents respectively the temperature of crystalline temp and solid-liquid interface;
represent crystal radius changing value,
for on the occasion of time crystal radius become large,
location variation, the Φ that during for negative value, the radius of crystal diminishes, v represents seed crystal lifting speed, dh is crystal structure interface represents crystal growth angle;
Wherein, Φ is according to the Infiltrating difference between crystal orientation and melt and mould, and it is worth between 65 degree to 75 degree, rc is crystal radius, and t represents the time, considers in long brilliant technological process, v does not adjust conventionally, and crystal to mold material determine after, Φ be also one determine constant value;
Therefore solvable equation formula group obtains:
increase,
> 0, otherwise
reduce,
< 0;
determined by the size of mould and the flow velocity of air-flow, thus the increase of the flow velocity of air-flow,
> 0, on the contrary the flow velocity of air-flow reduce,
< 0.
Further: described air-flow introduction passage is based on original thermal insulating material for being incubated, and forms by the mode of cutting processing.
Further, the mode of described cutting processing is boring.
Further, thermal insulating material is for solidifying graphite felt.
Further, described gas is one or more in rare gas element, CO or CO2.
Further, described gas is Ar.
Further, to be shaped as cross section be circular right cylinder to described rhabdolith.
Further, to be shaped as cross section be foursquare rectangular parallelepiped to described rhabdolith.
The invention has the advantages that: 1. the flow velocity that passes through to regulate the gas in the air-flow introduction passage of mould upper end in the process of growth of crystal, affect the specific heat load of mould upper end, regulate the thickness of crystal solid-liquid interface place liquid film, change in real time the size of crystal, make the shape of crystal controlled, thereby grow the crystal of specified shape; Gas channel, by original thermal insulating material for being incubated, forms by the mode of Drilling operation, has ensured the compactedness that thermal field internal heater and lagging material are arranged, and has reduced manufacturing cost; 2. thermal insulating material is to solidify graphite felt, and curing graphite felt is the material of a kind of easy boring and cutting, is again the lagging material that can bear the high temperature of 2500 degree left and right simultaneously, convenient manufacture and practical; 3. the gas in air-flow introduction passage is one or more in rare gas element, CO or CO2, and the requirement of chemical stability from high temperature, as the best selection of cooling effect gas; 4. rare gas element is preferably selected argon gas, and the cost performance of argon gas is high; 5. consider from the heat radiation symmetry of latent heat of solidification, it is circular right cylinder that the method is particularly useful for cross section, or the cross section rhabdolith that is foursquare rectangular parallelepiped.
Brief description of the drawings
Fig. 1 is the schematic diagram of a kind of sapphire crystal growth equipment of embodiments of the invention.
Fig. 2 is the schema of the inventive method.
Embodiment
Growth method of the present invention has adopted the method for air-flow cooling die, the shape of crystal growth is under control, as shown in Figure 2, the present invention has disclosed the growth method of the bar-shaped sapphire crystal of a kind of guided mode method, when it is grown at crystal, around the upper end of the mould in thermal field, be furnished with air-flow introduction passage, the gas flowing into from air-flow introduction passage carries out heat loss through convection to mould upper end, the specific heat load of controlling mould by the flow velocity of adjustments of gas regulates the thickness of crystal solid-liquid interface place liquid film, changes the size and dimension of sapphire product.
Its theoretical foundation is:
Wash away the air-flow velocity of die surface by control, can reach the object that changes crystal diameter, in described air-flow introduction passage, the relation of the diameter of gas flow rate and die surface is represented by following three relational expressions, wash away the air-flow velocity of die surface by control, can reach the object that changes crystal diameter, in described air-flow introduction passage, the relation of the diameter of gas flow rate and die surface is represented by following three relational expressions:
(1) relational expression of gas flow rate and the gas heat flow rate per unit area that washes away increase to mould is:
Wherein
represent Nu Saier number, Tm represent die temperature, Tg represent gas flow temperature,
represent that the thermal conductivity of gas, characteristic length, the q that L represents mould are due to the heat flow rate per unit area that wash away increase of air-flow to mould,
size determined by the size of mould and the flow velocity of air-flow, air-flow velocity is more
quantity is larger;
(2) relational expression of die temperature and mould upper surface melt films thickness is:
Wherein h represent melt films thickness, v represent seed crystal pull rate,
represent latent heat,
represent melt thermal conductivity,
represent that thermal conductivity, Tm, Tc and the Ti of crystal represents the temperature at die temperature, crystalline temp and solid-liquid (crystallization) interface successively; Can find out from relational expression, if ignore the subtle change of Tc and Ti in long brilliant process, and get fixing seed crystal lifting speed v, the influence factor of h only depends on die temperature Tm, after solving differential relationship, can learn, in the time that die temperature Tm rises, melt films thickness h will become greatly, otherwise h diminishes;
(3) relational expression of crystal radius and melt films thickness:
Wherein
represent crystal radius changing value,
for on the occasion of time crystal radius become large,
during for negative value, the radius of crystal diminishes, v represents that seed crystal lifting speed, h represent that melt films thickness, dh are that location variation, the Φ at crystal structure interface represents crystal growth angle; Φ is according to the Infiltrating difference between crystal orientation and melt and mould, it is worth between 65 degree to 75 degree, and rc is crystal radius, and t represents the time, consider in long brilliant technological process, v does not adjust conventionally, and crystal to mold material determine after, Φ be also one determine constant value, analyze relationship formula can be learnt, in the time that h value increases, be negative value, crystal diameter reduces; In the time that h value reduces, be on the occasion of, crystal diameter increase;
Described in comprehensive above-mentioned relation formula (1)-(3):
Can learn, wash away the air-flow velocity of die surface by control, can reach the object that changes crystal diameter, in the time the crystal diameter of growth in real time need to being strengthened, can increase the gas velocity of inlet air flow stream passage, will be declined by the temperature of relational expression (1) mould, from relational expression (2), the melt films thickness of mould upper end face will reduce, and from relational expression (3), finally make the diameter of corresponding crystal increase; Otherwise, reduce the gas velocity of flow path gas channel, can reduce in real time the diameter of corresponding crystal; Therefore only need by the specific heat load of the flow rate effect mould of adjustments of gas, regulate the thickness of crystal solid-liquid interface place liquid film, thereby finally meet sapphire product in size and dimension requirement.
Above-mentioned guided mode method is grown sapphire crystal growth equipment that bar-shaped sapphire crystal method uses in the time realizing as shown in Figure 1:
Crucible 9 is positioned on crucible pedestal 6, in crucible 9, put into the high purity aluminium oxide starting material that purity is greater than 99.995%, in crucible 9, be also fixed with end face is circular mould 8 simultaneously, the central hairiness finedraw of mould 8, well heater is heat-generating pipe 3, and heat-generating pipe 3 is arranged on around crucible 9, and thermal field is formed the insulation of thermal field thermal insulation layer by insulated tank 1, upper insulation cover 4, lower insulation cover 2, the upper surface of mould 8 is aimed in the air outlet of gas port 10, and seed crystal is fixed on seed rod 12; Under the effect of radio-frequency induction coil 5, pass through induction heating, heat-generating pipe 3 heatings will be rapidly heated, and thermal field thermal insulation layer makes heat be not easy loss, under suitable heating power, mould 8 tip temperature can reach 2050 degree left and right like this, and high purity aluminium oxide raw material is melted liquid, liquation, along the capillary seam of mould 8, rises to capillary seam top.Seed rod 12 declines, and makes seed crystal contact the rear melt films 7 that forms with mould, continues to grow crystal 11 after lifting seed rod.
Described air-flow introduction passage is based on original thermal insulating material for being incubated, and forms by the mode of cutting processing
Preferably, here insulated tank 1, upper insulation cover 4 and lower insulation cover 2 all adopts curing graphite felt to process, heat-generating pipe 3 is processed by graphite material, gas port 10 forms by Drilling operation mode on insulated tank 1, gas in gas port is selected argon gas, the method of the present invention cross section that is particularly useful for growing is circular right cylinder, or the cross section sapphire crystal that is foursquare rectangular parallelepiped.
The method is specific as follows:
Step 1: put into high-purity oxidized still starting material that purity is greater than 99.995% in crucible 9, mould 8 is fixed in crucible simultaneously;
Step 2: crucible 9 is placed on the crucible pedestal 6 in thermal field;
Step 3: crystal growing thermal field is vacuumized, and vacuum tightness is 103Pa left and right;
Step 4: by radio-frequency induction coil 5 induction heating, make well heater 3 heating make the temperature in thermal field be warming up to 2050 degree left and right, high-purity mangesium oxide aluminum feedstock is melted;
Step 5: in the time that solution rises to capillary seam top along the capillary seam of mould 8, seed rod 12 is declined and carry out seeding, crystal is with the speed growth of 10～100mm/h;
Step 6: in process of growth,, to one or more in the interior logical rare gas element of gas port 10, CO or CO2 in thermal field, preferably, the gas here adopts argon gas;
Step 7: when being subject to external disturbance, when crystal 11 diameters are greater than design load, suitably reduce the interior gas velocity of gas port 10, make crystal 11 diameters get back to design load;
Step 8: when being subject to external disturbance, in the time that crystal 11 diameters are less than design load, suitably increase the gas velocity in gas port 10, make crystal 11 diameters get back to design load;
Step 9: when the diameter of crystal 11 and mould 7 sizes are when basically identical, keep melt films 7 thickness constant, realize isodiametric growth until crystal 11 growths finish;
Step 10: lift seed rod 12 and make crystal 11 break away from moulds, make subsequently thermal field be cooled to 1900 degree, keep for some time to carry out anneal;
Step 11: heating power is slowly fallen to zero, take out crystal 11 after waiting crystal 11 temperature to approach room temperature.
Taking growth cross section as circular cylindrical sapphire crystal is as example, the diameter of required growing sapphire crystal is 50mm,
Embodiment mono-: when the diameter of sapphire crystal is 47MM, need to increase gas flow rate and make its diameter increase to 50MM time, data are as shown in the table:
| The diameter (MM) of current crystal | Gas flow rate L/S | Aeration time (S) | The diameter (MM) of gas after ventilation |
| 47 | 1 | 30 | 50 |
| 47 | 5 | 10 | 50 |
| 47 | 10 | - | Liquid membrane declines, h≤0, and now liquid film solidifies |
Above-mentioned data show, in the time that needs increase sapphire crystal diameter, its gas flow rate is controlled between 5-8S as good.
Embodiment bis-: when the diameter of sapphire crystal is 54MM, need to reduce gas flow rate and make its diameter be reduced to 50MM time, data are as shown in the table
| The diameter (MM) of current crystal | Raw-gas flow velocity L/S | Existing gas flow rate L/S | Aeration time (MIN) | The diameter (MM) of gas after ventilation |
| 54 | 5 | 2 | 120 | 50 |
| 54 | 5 | 1 | 60 | 50 |
| 54 | 5 | 0 | 37 | 50 |
Above-mentioned data show, in the time that needs reduce sapphire crystal diameter, its aeration time is longer.
Claims (10)
1. the growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control; it is characterized in that: around the upper end of mould when crystal growth in thermal field, be furnished with air-flow introduction passage; the gas flowing into from air-flow introduction passage carries out heat loss through convection to mould upper end; the specific heat load of controlling mould by the flow velocity of adjustments of gas regulates the thickness of crystal solid-liquid interface place liquid film, changes the size and dimension of sapphire product.
2. a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to claim 1, it is characterized in that: the size and dimension of described sapphire product is to be determined by the diameter of sapphire crystal, the air-flow velocity that can wash away die surface by control is controlled the diameter of sapphire crystal, in the time the crystal diameter of growth need to being strengthened, can increase the gas velocity of inlet air flow stream passage; In the time the crystal diameter of growth need to being reduced, can reduce the gas velocity of inlet air flow stream passage.
3. a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to claim 2, is characterized in that: in described air-flow introduction passage, the pass of the diameter of gas flow rate and die surface is:
①
②
③
Wherein
represent Nu Saier number, Tm represent die temperature, Tg represent gas flow temperature,
represent that the thermal conductivity of gas, characteristic length, the q that L represents mould are due to the heat flow rate per unit area that wash away increase of air-flow to mould; H represent melt films thickness, v represent seed crystal pull rate,
represent latent heat,
represent melt thermal conductivity,
represent that thermal conductivity, Tc and the Ti of crystal represents respectively the temperature of crystalline temp and solid-liquid interface;
represent crystal radius changing value,
for on the occasion of time crystal radius become large,
location variation, the Φ that during for negative value, the radius of crystal diminishes, v represents seed crystal lifting speed, dh is crystal structure interface represents crystal growth angle;
Wherein, Φ is according to the Infiltrating difference between crystal orientation and melt and mould, and it is worth between 65 degree to 75 degree, rc is crystal radius, and t represents the time, considers in long brilliant technological process, v does not adjust conventionally, and crystal to mold material determine after, Φ be also one determine constant value;
Therefore solvable equation formula group obtains:
increase,
> 0, otherwise
reduce,
< 0;
determined by the size of mould and the flow velocity of air-flow, thus the increase of the flow velocity of air-flow,
> 0, on the contrary the flow velocity of air-flow reduce,
< 0.
4. a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to claim 1, is characterized in that: described air-flow introduction passage is based on original thermal insulating material for being incubated, and forms by the mode of cutting processing.
5. the growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to one kind of claim 4, is characterized in that: the mode of described cutting processing is boring.
6. the growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to one kind of claim 4, is characterized in that: thermal insulating material is for solidifying graphite felt.
7. a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to claim 1, is characterized in that: described gas is one or more in rare gas element, CO or CO2.
8. the growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to one kind of claim 7, is characterized in that: described gas is Ar.
9. a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to claim 1, is characterized in that: it is circular right cylinder that described rhabdolith is shaped as cross section.
10. a kind of growth method based on the bar-shaped sapphire crystal diameter of protective atmosphere control according to claim 1, is characterized in that: it is foursquare rectangular parallelepiped that described rhabdolith is shaped as cross section.
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Cited By (7)
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| CN104264215A (en) * | 2014-10-15 | 2015-01-07 | 江苏中电振华晶体技术有限公司 | Sapphire crystal growing device adopting edge defined film-fed growth techniques and growing method |
| CN104862775A (en) * | 2015-06-09 | 2015-08-26 | 江苏中电振华晶体技术有限公司 | Growth device for sapphire crystal hemisphere cover and growth method for sapphire crystal hemisphere cover |
| CN106676625A (en) * | 2017-02-21 | 2017-05-17 | 洛阳金诺机械工程有限公司 | Blowing device for drawing silicon cores |
| CN107352559A (en) * | 2017-08-30 | 2017-11-17 | 重庆博张机电设备有限公司 | A kind of rod alkali production equipment |
| CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
| CN112501690A (en) * | 2020-12-02 | 2021-03-16 | 通辽精工蓝宝石有限公司 | Growth method of sapphire single crystal |
| CN114150371A (en) * | 2021-12-06 | 2022-03-08 | 徐州鑫晶半导体科技有限公司 | Cooling assembly, control method thereof and crystal growing device |
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Cited By (9)
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|---|---|---|---|---|
| CN104264215A (en) * | 2014-10-15 | 2015-01-07 | 江苏中电振华晶体技术有限公司 | Sapphire crystal growing device adopting edge defined film-fed growth techniques and growing method |
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| CN104862775A (en) * | 2015-06-09 | 2015-08-26 | 江苏中电振华晶体技术有限公司 | Growth device for sapphire crystal hemisphere cover and growth method for sapphire crystal hemisphere cover |
| CN106676625A (en) * | 2017-02-21 | 2017-05-17 | 洛阳金诺机械工程有限公司 | Blowing device for drawing silicon cores |
| CN106676625B (en) * | 2017-02-21 | 2023-05-26 | 洛阳金诺机械工程有限公司 | Air blowing device for drawing silicon core |
| CN107352559A (en) * | 2017-08-30 | 2017-11-17 | 重庆博张机电设备有限公司 | A kind of rod alkali production equipment |
| CN108411367A (en) * | 2018-03-06 | 2018-08-17 | 同济大学 | Flow atmosphere EFG technique multi-disc sapphire crystallization device and method |
| CN112501690A (en) * | 2020-12-02 | 2021-03-16 | 通辽精工蓝宝石有限公司 | Growth method of sapphire single crystal |
| CN114150371A (en) * | 2021-12-06 | 2022-03-08 | 徐州鑫晶半导体科技有限公司 | Cooling assembly, control method thereof and crystal growing device |
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Application publication date: 20140806 |