CN102212871A - Growth method for sapphire crystals and crystal growth furnace structure for growing sapphire crystals - Google Patents
Growth method for sapphire crystals and crystal growth furnace structure for growing sapphire crystals Download PDFInfo
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Abstract
The invention relates to a growth method for sapphire crystals and a crystal growth furnace structure for growing the sapphire crystals. The growth method comprises the following steps of: a, mixing 40 to 60 weight percent of aluminum oxide crystals, 20 to 30 weight percent of aluminum oxide crystal blocks and 10 to 30 weight percent of aluminum oxide crystal grains uniformly, and putting the mixture into a crucible; b, putting the crucible with the aluminum oxide crystals into the crystal growth furnace, vacuumizing, and heating the crystal growth furnace to 2,200 DEG C; c, heating the aluminum oxide crystals in the crucible until the aluminum oxide crystals are in a molten state, reducing the temperature of the crucible to between 2,150 and 2,200 DEG C, and starting to lead the crystals when a solid-liquid interface is formed in the crucible; d, reducing the temperature of the crucible to between 1,900 and 2,100 DEG C to grow the crystals; e, maintaining the temperature of the crystal growth furnace; f, annealing the crystal growth furnace; and h, breaking vacuum by argon in the crystal growth furnace, starting the crystal growth furnace and taking the sapphire crystals out. In the growth method, process steps are simple, the processing is convenient, and the method is energy-saving, environment-friendly, high in applicability, safe and reliable.
Description
Technical field
The present invention relates to a kind of growth method of sapphire crystal and the brilliant furnace structure of length that sapphire crystal growth has, the brilliant furnace structure of length of the growth method of monocrystalline sapphire (alumina single crystal) and growth usefulness specifically belongs to the technical field of sapphire crystal.
Background technology
At present, single crystal sapphire substrate is very important in the utilization of modern science and technology product, photodiode (LED) with opto-electronics is an example, the investigation of materials of gan (GaN) is above 20 years, but always because the substrate (Substrate) that does not have lattice parameter to cooperate, so crystal is long bad, and p type gan is difficult for making, so make slow progress, these problems are until 1 983 years, the loyal doctor's Shi human aluminium nitride (AlN) such as (S.Yoshida) in the field of Japan) on sapphire (Sapphire) substrate, does buffer layer with the high temperature growth earlier, again thereon during growing gallium nitride, crystallization is better, red rugged brave professor people such as (I.Akasaki) discovery of Nagoya University afterwards uniformly at the thin aluminium nitride of the long one deck of low temperature (about 600 ℃), can obtain the material of picture minute surface with organo-metallic vapour deposition process (MOCVD or OMVPE) thereon again with high temperature (about about 1000 ℃) gallium nitride growth.1991 Nian Riya companies (Nichia Co.) researcher's Shuji Nakamuras (S.Nakamura) are used noncrystal gan instead and are grown into buffer layer (Buffer Layer) earlier with low temperature, during again with the high temperature gallium nitride growth, also obtain smooth film as the minute surface.Another problem of how being p-GaN also obtains to break through, people such as red rugged brave professor at first were entrained in magnesium (Mg) and make its growth in the gan in 1989, carry out the electron beam irradiation after growing up to and obtain p type gan, the back future, the Shuji Nakamura of inferior company was found electron beam, but be that the temperature of gan is raise, hydrogen among the Ma-H is separated and the magnesium acceptor is produced low-impedance gan by sensitization, if he finds also a hydrogen to be driven away with about 700 ℃ thermal annealing, make the magnesium sensitization and finish the work of p type.Utilize above two discoveries, Ri Ya company announced successfully to develop the GaN blue light-emitting diode (LED) of luminosity one candle light (Cd) in 1993, and the life-span reaches tens thousand of hours.After this message is delivered, cause global attention at once, the existing a lot of groups in all parts of the world are in manufacturing, character and the application of this type of material of research at present.With the TaiWan, China patent is example, invents No. 1245440 name and is called photodiode patent (with reference to patent announcement on December 11st, 2005), and it includes: a substrate; One nucleating layer is arranged on this substrate, and is formed by AlxGal-xN, to solve the unmatched phenomenon of lattice, wherein 0≤x≤1; One buffer layer is arranged on this nucleating layer; One n type contact layer is arranged on this buffer layer, and is electrically connected at a n type electrode, and this n type contact layer is formed by n-AlxGal-xN, wherein 0≤x≤0.3; One n type coating is arranged on this n type contact layer, and is formed by n-AlxGal-xN, wherein 0≤x≤0.3; One luminescent layer is arranged on this n type coating layer; One p type barrier layer is formed on this luminescent layer, prevents the carrier overflow, and this p type barrier layer is formed by p-AlxGal-xN, wherein 0≤x≤0.4; One p type coating is formed on this p type barrier layer, and with the limitation carrier, this p type coating is formed by p-AlxGal-xN, wherein 0≤x≤0.3; And a p type contact layer, be to be positioned on this p type coating, and be electrically connected at a p type electrode that this p type contact layer is formed by p-AlxGal-xN, wherein 0≤x≤0.15; Wherein, when applying a suitable forward bias voltage drop in this n type electrode and this p type electrode, can excite this luminescent layer to produce wavelength and be the how light output of rice of 300-380. and wherein this substrate is to be selected from by sapphire substrate, silicon substrate, silicon carbide substrate, gallium nitride base board, aluminium nitride substrate, aluminium gallium nitride alloy substrate and zinc oxide substrate to be become one of to make up.And, be fit closely baseplate material, so also important with regard to especially of the technology that grows up to of sapphire substrate because lattice and the gan of sapphire substrate (alumina single crystal) is very approaching.
In addition, produces the main gordian technique of sapphire substrate and be in 2050 ℃ of high temperature alumina powder to be melted and growing crystal, and the long crystal method of sapphire includes following several substantially usually:
Flame melting method (Flame Fusion): the flame melting method is to utilize hydrogen, oxygen combustion pyritous torch, the aluminum oxide powder that drops is from top to down melted, liquid melts to drop on the kind that lower wall accepts and solidifies, and the change as growing up just like the stalagmite in the stalactite grotto is big.This kind alumina single crystal maximum can reach 3 centimetres of diameters, but bubble may be contained in its inside, and flaws such as aluminum oxide powder that does not melt and residual stress, so only be applicable to the purposes such as sapphire glass, sapphire gear (Gear) and ornament on wrist-watch surface.The sapphire factory of this kind of world production gains fame and fortune in Europe, and for example Fa Guo Bircon is well-known.
The method of fluxing (Flux Growth): the rule of fluxing is to utilize fusing assistant, as plumbous oxide, aluminum fluoride and Sodium Fluoride etc., aluminum oxide being lower than 2050 0C dissolving, is slowly cooled off via liquid again, and supersaturation is separated out.This kind method is the method that novel material is cultivated in the traditional experiment chamber, is not suitable for the volume production of industry member.Be the company that produces ornaments such as jewel with this at present, as U.S. JO Crystal and Chatham.
Czochralski method (Czochralski method): Czochralski method is to utilize graphite resistance or the heating of induced method, the aluminum oxide powder that is contained in crucible is melted under passivity gas or in the vacuum, again the sapphire kind is fallen at leisure from top to bottom, contact liquid level slightly, the rotation slowly of crystal seed this moment, and upwards drawing goes out sapphire crystal seed.The size of its diameter and quality then decide according to the speed and the liquid level temperature controlling that draw high, and this method is fit to industrial production, and there are companies such as the Union Carbide of the U.S. and Canadian Crystar in well-known in the world production firm.
Guided mode method (Edge-defined Film-fed Growth EFG): the brilliant equipment unit of length of EFG guided mode method, be similar to Czochralski method, but its crystal does not rotate in growth, and diameter of upwards drawing and shape, is controlled by a metal pattern (Die) that is suspended in the aluminum oxide liquid level.It has great pulling rate, can produce the circle crystal column or the flat chip of hollow.Good in economic efficiency, but crystal contains highdensity residual stress and difference row (dislocation), is suitable for optical applications but not semiconductor substrate.The Kyocera that main in the world production company is a Japan.
The Kyropoulos:Kyropoulos method utmost point is similar to Czochralski method, but its crystal does not utilize rotation, unfavorable using to regard it as the control diameter in growth, and solidifies cooling and contraction in crucible.The crystalline size that grows up at last is slightly less than crucible, so must be through numerous and diverse post-treatment to reach final diameter.
Thermal gradient method (Thermal Gradient Technique): thermal gradient is to be formed in research and development in 1978 by U.S. Crystal systems company, and has applied for patented technology.It is with directional crystal inductive melt single crystal method, comprise the crucible, heating element and the shielding unit that are placed in the simple bell-jar vacuum resistance furnace, still, there is molybdenum polution in this law crystal growing process, other impurity is mainly introduced by raw material, the essential high-purity raw that adopts.
The monocrystalline sapphire that the above long crystal method of sapphire is grown, have contaminating impurity or its crystal mass and size and all be restricted, be difficult to satisfy the long long disappearance of brilliant needs time of high performance requirements, cost height and high temperature of assemblies such as optics, semi-conductor, communication.More than be the disappearance of existing technology maximum, in fact the technical barrier of demanding urgently overcoming for industry.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of growth method of sapphire crystal and the brilliant furnace structure of length that sapphire crystal growth is used are provided, its processing step is simple, and is easy to process, energy-conserving and environment-protective, and suitability is good, and is safe and reliable.
According to technical scheme provided by the invention, a kind of growth method of sapphire crystal, described growth method comprises the steps:
A, provide the alpha-alumina crystals material, described alpha-alumina crystals material comprises alpha-alumina crystals, aluminum oxide crystal block and alumina grain, and the alpha-alumina crystals with 40% ~ 60%, 20% ~ 30% aluminum oxide crystal block and 10% ~ 30% alumina grain are put into crucible after according to the weight percent uniform mixing;
B, the crucible that will place the alpha-alumina crystals material are put into long brilliant stove and are vacuumized, and the temperature of long brilliant stove are heated to 2200 ℃, to the alpha-alumina crystals material material in the crucible;
When the alpha-alumina crystals in c, the crucible is heated to molten state, long brilliant stove is lowered the temperature, the temperature of crucible is reduced between 2150 ℃ ~ 2200 ℃; And when solid-liquid interface occurring in the crucible, begin the alpha-alumina crystals seeding in the crucible;
After alpha-alumina crystals seeding in d, the crucible is finished, long brilliant stove is lowered the temperature, make the temperature of crucible reduce to 1900 ℃ ~ 2100 ℃, so that long brilliant in crucible;
E, treat in the crucible that long brilliant operation finishes the back long brilliant stove is incubated;
F, long brilliant stove is annealed, make the temperature in the long brilliant stove reduce to 1000 ℃ gradually by 2000 ℃;
H, long brilliant stove is carried out making the temperature of long brilliant stove reduce to normal temperature gradually after annealing operation finishes;
I, after reducing to normal temperature in the long brilliant stove, in the long brilliant stove with the argon gas vacuum breaker, open long brilliant stove and also take out sapphire crystal.
Among the described step c, the seeding post by crucible top and be positioned at the seed crystal seeding of seeding column end; During seeding, the end of seed crystal and seeding post is extended the solid-liquid interface place of crucible, the moving seed crystal of seeding cornice rotates in crucible.
Among the described step e, when length is brilliant in the crucible, rotate the crucible that is positioned at long brilliant stove.
The brilliant furnace structure of the length that a kind of sapphire crystal growth is used comprises body of heater, and the bottom of described body of heater is provided with the rotation brace table that is used to place crucible, and described rotation brace table is positioned at the centre of body of heater; Be provided with the thermal field that is used for the crucible heating in the body of heater, described thermal field is positioned at the outer ring of rotation brace table; Outer ring corresponding to thermal field in the body of heater is provided with thermal insulation layer; The bottom of body of heater is provided with water-in and water outlet, and described water-in is connected with body of heater with water outlet; The top of body of heater is provided with tracheae, and described tracheae is connected with body of heater.
Described thermal field comprises electromagnetism or resistance heating coil.
Described rotation brace table be used to drive the following drive-motor that the rotation brace table rotates and link to each other; The central section of rotation brace table is provided with the rotation back shaft, and described rotation back shaft links to each other with the output shaft of lower rotating electrical machine.
The intravital bottom of described stove is provided with and is used for thermometric thermopair; Described thermopair is a rhenium thorium alloy thermopair.The intravital top of described stove is provided with the CCD video sensor.
The top of described body of heater is provided with rotating machine, and the described output shaft of going up rotating machine is provided with the seeding post, and described seeding post stretches in the body of heater corresponding to the other end that links to each other with the output shaft of last rotating machine; The seeding post is equipped with seed crystal corresponding to stretching into the intravital end of stove.
The described rotating machine of going up links to each other with the output terminal of controller, described controller respectively be used to observe the intravital CCD video sensor of stove, the thermopair that is used to measure working temperature in the body of heater and lower rotating electrical machine and link to each other; The output shaft of described lower rotating electrical machine links to each other with the rotation brace table.
Advantage of the present invention: the crucible that will have alpha-alumina crystals is earlier put into body of heater, and body of heater vacuumizes by tracheae; The intravital thermal field of stove heats the alpha-alumina crystals in the crucible, after detecting by rhenium thorium alloy thermopair, the temperature of thermal field heating is transferred in the controller, the CCD video sensor arrives controller with the intravital work transmission of video images of stove simultaneously, by doing the rotating speed that image comparison back is in time controlled temperature of thermal field and gone up rotating machine, lower rotating electrical machine, controller can accurately be controlled the working order of rotating machine in the controller; Last rotating machine is finished seeding and long brilliant process by rotation, the lifting of seeding post and seed crystal, measures and the working accuracy height, can keep required processing temperature in the body of heater, and Working Procedure Controlling is easy to operate; When treating that the long crystalline substance of sapphire crystal finishes, controller makes the rotation of lower rotating electrical machine, and lower rotating electrical machine drives the rotation of crucible, is convenient to take out sapphire crystal; Controller and CCD video sensor and thermopair corresponding matching can accurately be controlled the whole course of processing, and the working accuracy height improves working (machining) efficiency, cuts down finished cost, and technological operation is simple, and energy-conserving and environment-protective are safe and reliable.
Description of drawings
Fig. 1 is the structural representation of the long brilliant stove of the present invention.
Embodiment
The invention will be further described below in conjunction with concrete drawings and Examples.
As shown in Figure 1: the present invention is used for the brilliant furnace structure of length that sapphire crystal growth uses and comprises rotating machine 1, CCD video sensor 2, tracheae 3, seed crystal 4, the first alpha-alumina crystals piece 5, the second alpha-alumina crystals piece 6, thermal insulation layer 7, rotation brace table 8, water-in 9, water outlet 10, lower rotating electrical machine 11, thermopair 12, thermal field 13, seeding post 14, rotation back shaft 15, body of heater 16, controller 17 and crucible 18.
As shown in Figure 1: the bottom in the described body of heater 16 is provided with the rotation brace table 8 that is used to place crucible 18, and described rotation brace table 8 has table top portion, and crucible 18 is positioned in the table top portion; Rotation brace table 8 convexes with rotation back shaft 15 corresponding to the opposite side that table top portion is set, rotation back shaft 15 is positioned at the central section of rotation brace table 8, rotation brace table 8 is installed on bottom in the body of heater 16 by rotation back shaft 15, and rotation brace table 8 can rotate in body of heater 16.Be provided with thermal field 13 in the body of heater 16, described thermal field 13 is positioned at the outer ring of rotation brace table 8, and thermal field 13 adopts electromagnetism or resistance heating coil, also can adopt other heat form.Outer ring corresponding to thermal field 13 in the body of heater 16 is provided with thermal insulation layer 7, and after the crucible 18 on 13 pairs of rotations of thermal field brace table 8 was heated to the temperature of setting, thermal insulation layer 7 can carry out corresponding maintenance with the temperature in the body of heater 16, is suitable for the requirement of complete processing.Body of heater 16 is provided with and drives the driving mechanism that rotation brace table 8 rotates, described driving mechanism is a lower rotating electrical machine 11, described lower rotating electrical machine 11 is positioned at the below of body of heater 16 bottoms, and the output shaft of lower rotating electrical machine 11 links to each other with rotation back shaft 15, rotates thereby can drive rotation brace table 8.The top of body of heater 16 is provided with tracheae 3, and the cavity in described tracheae 3 and the body of heater 16 is connected, can vacuumize the cavitys in the body of heater 16 by tracheae 3, and can be to vacuum breakers in the body of heater 16.Bottoms in the body of heater 16 are provided with water-in 9 and water outlet 10, and described water-in 9, water outlet 10 all are connected with the interior cavity of body of heater 16.
In order to know the working temperature of body of heater 16, be provided with temperature sensor in the body of heater 16, described temperature sensor adopts thermopair 12, and described thermopair 12 is positioned at 7 of thermal field 13 and thermal insulation layers; Thermopair 12 adopts rhenium thorium alloy thermopairs, can accurately measure the working temperature of body of heater 16 by rhenium thorium alloy thermopair, can not cause the uncertainty of the technological temperature in the body of heater 16 because of the difference of thermal field 13 characteristics.In order to observe the working order in the body of heater 16, top in the body of heater 16 is provided with CCD(Charge-coupled Device) video sensor 2, described CCD video sensor 2 links to each other with controller 17, CCD video sensor 2 can be transferred to the working order in the body of heater 16 in the controller 17, controller 17 is done the image comparison with the video image and the controller 17 interior default images that receive, controller 17 can accurately carry out the corresponding working procedures operation after comparing by corresponding image, and is safe and reliable.Simultaneously, controller 17 links to each other with the output terminal of thermopair 12, and controller 17 receives the temperature value that thermopair 12 detects.Controller 17 links to each other with lower rotating electrical machine 11, the working order of controller 17 control lower rotating electrical machine 11.Controller 17 can adopt computer commonly used.
The top of body of heater 16 is provided with rotating machine 1, described upward rotating machine 1 is fixed in the top of body of heater 16, the output shaft of last rotating machine 1 is provided with seeding post 14, described seeding post 14 is vertical distribution in body of heater 16, seeding post 14 stretches in the body of heater 16 corresponding to the other end that links to each other with last rotating machine 1 output shaft; And seeding post 14 is provided with seed crystal 4 corresponding to the end of going deep in the body of heater 16, and described seed crystal 4 is used for the orientation of sapphire crystal growth.The described rotating machine 1 of going up links to each other with controller 17, and controller 17 is used to control the rotary state of rotating machine 1.
During use, place alpha-alumina crystals in the crucible 18 now, described alpha-alumina crystals comprises alpha-alumina crystals, aluminum oxide crystal block and alumina grain, the size difference of alpha-alumina crystals, aluminum oxide crystal block and alumina grain, thereby in crucible 18, form the size of the physical dimension of the first alpha-alumina crystals piece 5 and the second alpha-alumina crystals piece, 6, the first alpha-alumina crystals pieces 5 greater than the second alpha-alumina crystals piece 6.After placing alpha-alumina crystals in the crucible 18, crucible 18 is put into the cavity of body of heater 16, be about to crucible 18 and place in the table top portion of rotation bearing surfaces 8, then body of heater 16 is vacuumized by tracheae 3, thereby be convenient to follow-up sapphire crystal growth technology.
Particularly, the growth method of sapphire crystal comprises the steps:
A, provide the alpha-alumina crystals material, described alpha-alumina crystals material comprises alpha-alumina crystals, aluminum oxide crystal block and alumina grain, and the alpha-alumina crystals with 40% ~ 60%, 20% ~ 30% aluminum oxide crystal block and 10% ~ 30% alumina grain are put into crucible 18 after according to the weight percent uniform mixing;
The weight of alumina single crystal adapts according to the size and the relevant processing request of crucible 18, and the weight of general alumina single crystal can be divided into 30kg, 60kg, 90kg or 250kg, and the alumina single crystal of Different Weight adds man-hour, has different requirements process period; Alpha-alumina crystals, aluminum oxide crystal block and stress manager's size dimension difference, the alpha-alumina crystals material also can adopt the material of pie; The difference of alpha-alumina crystals material is provided, can obtains the sapphire crystal of different qualities;
B, the crucible 18 that will have an alumina single crystal are put into the body of heater 16 of long brilliant stove and are vacuumized, and the temperature of long brilliant stove are heated to 2200 ℃, to the alumina single crystal material in the crucible 18;
When vacuumizing, the tracheae 3 by body of heater 16 tops carries out; After vacuumizing, the cavity in the whole body of heater 16 all is in vacuum state; Vacuumize finish after, heat by 13 pairs of bodies of heater 16 of thermal field, make the alumina single crystals in the crucible 18 rise to 2200 degree, can make the alumina single crystal in the crucible 18 be heated to liquid state to the alumina single crystal material; After the heating, be incubated by the thermal insulation layer 7 in the body of heater 16, thus the power loss that can save thermal field 13, the exchange of minimizing and outside heat, energy-conserving and environment-protective, safe and reliable; The temperature-rise period of body of heater 16 when thermal field 13 heating all detects by thermopair 12, and thermopair 12 outputs to the temperature that detects in the controller 17, thereby controller 17 can accurately be controlled the heat-processed of thermal field 13, improves the precision of processing;
When the alpha-alumina crystals in c, the crucible 18 is heated to molten state, long brilliant stove is lowered the temperature, the temperature of crucible 18 is reduced between 2150 ℃ ~ 2200 ℃; And when solid-liquid interface occurring in the crucible 18, begin the alumina single crystal seeding in the crucible 18;
When the temperature of crucible 18 after thermal field 13 is heated to 2200 degree, liquid state can appear melting in the alumina single crystals in the crucible 18, then to lowering the temperature in the body of heater 16, so that can carry out seeding to alumina single crystal; During seeding, seeding post 14 stretches in the crucible 18 corresponding to the end that seed crystal 4 is set, and at the solid-liquid interface of crucible 18, last rotating machine 1 drives seeding post 14 and rotates, thereby seed crystal 4 rotates in crucible 18, and the kind of seed crystal 4 can be selected according to the sapphire crystal of the needed different crystal faces of growth;
The Heating temperature of crucible 18 is detected by thermopair 12, alumina single crystal state in the crucible 18 is transferred in the controller 17 by CCD video sensor 2, controller 17 is according to the working temperature and the interior video situation that detect, can appropriately control the rotary state of rotating machine 1, can accurately control the seeding time point of the solid-liquid interface of crucible 18, can improve the success ratio of seeding, cut down finished cost;
After alumina single crystal seeding in d, the crucible is finished, long brilliant stove is lowered the temperature, make the temperature of crucible 18 reduce to 1900 ℃ ~ 2100 ℃, so that long brilliant in crucible 18;
After seeding is finished, need then grow brilliant process; When long brilliant, need to reduce the temperature value of crucibles 18 in the body of heater 16, the temperature value of crucible 18 need be spent between 2100 degree 1900, and long when brilliant, the alumina single crystals in the crucible 18 are finished long brilliant process under the effect of seed crystal 4;
E, treat in the crucible 18 that long brilliant operation finishes the back long brilliant stove is incubated;
When treating that promptly long crystalline substance is finished in the crucible 18, controller 17 rotates lower rotating electrical machine 11, and the output shaft of lower rotating electrical machine 11 rotates by rotation back shaft 15 driven rotary brace tables 8, thereby the crucible 18 that will rotate on the brace table 8 rotates; Crucible 18 can prevent contacting of growth obtains in the crucible 18 sapphire crystal and crucible 18 inwalls after rotating under the driving of lower rotating electrical machine 11, thereby can take out the sapphire crystal in the crucible 18 easily; The velocity of rotation of lower rotating electrical machine 11 is carried out arrange accordingly by controller 17 according to the weight of the alumina single crystal of placing in the crucible 18;
F, long brilliant stove is annealed, make the temperature in the long brilliant stove reduce to 1000 ℃ gradually by 2000 ℃;
After long brilliant operation is finished, also need the temperature in the body of heater 16 is carried out annealing operation, the temperature in the body of heater 16 is in annealing operation, and the temperature value in the body of heater 16 is reduced to 1000 degree gradually by 2000 degree, satisfy the processing temperature requirement of sapphire crystal, the performance behind the assurance sapphire crystal growth;
H, long brilliant stove is carried out making the temperature of long brilliant stove reduce to normal temperature gradually after annealing operation finishes;
After annealing operation, the temperature in the body of heater 16 is reduced to the normal temperature state gradually, this process need continues the corresponding time, and the temperature in body of heater 16 is in the normal temperature state;
I, after reducing to normal temperature in the long brilliant stove, in the long brilliant stove with the argon gas vacuum breaker, open long brilliant stove and also take out sapphire crystal.
After placing in the body of heater 16, crucible 18 vacuumizes, when body of heater 16 is reduced to the normal temperature process once more, remain vacuum state in the body of heater 16, feed argon gas by the cavity of tracheae 3 in body of heater 16 this moment, the pressure that feeds argon gas is standard pressure, thereby make the air pressure in the body of heater 16 identical, can take out the sapphire crystal that processing obtains in the body of heater 16 safely, so far finish the course of processing of a sapphire crystal with external pressure.
The present invention will have the crucible 18 of alumina single crystal earlier and put into body of heater 16, and body of heater 16 vacuumizes by tracheae 3; Alpha-alumina crystals in 13 pairs of crucibles of thermal field 18 in the body of heater 16 heats, after detecting by rhenium thorium alloy thermopair, the temperature of thermal field 13 heating is transferred in the controller 17, CCD video sensor 2 arrives controller 17 with the work transmission of video images in the body of heater 16 simultaneously, controller 17 is by doing the rotating speed that image comparison back is in time controlled thermal field 13 temperature and gone up rotating machine 1, lower rotating electrical machine 11, and controller 17 can accurately be controlled the working order of rotating machine 1; Last rotating machine 1 is finished seeding and long brilliant process by rotation, the lifting of seeding post 14 and seed crystal 4, measures and the working accuracy height, can keep required processing temperature in the body of heater 16, and Working Procedure Controlling is easy to operate; When treating that the long crystalline substance of sapphire crystal finishes, controller 17 makes the rotation of lower rotating electrical machine 11, and lower rotating electrical machine 11 drives the rotation of crucibles 18, is convenient to take out sapphire crystal; Controller 17 and CCD video sensor 2 and thermopair 12 corresponding matching can accurately be controlled the whole course of processing, and the working accuracy height improves working (machining) efficiency, cuts down finished cost, and technological operation is simple, and energy-conserving and environment-protective are safe and reliable.
Claims (10)
1. the growth method of a sapphire crystal is characterized in that, described growth method comprises the steps:
(a), provide the alpha-alumina crystals material, described alpha-alumina crystals material comprises alpha-alumina crystals, aluminum oxide crystal block and alumina grain, and the alpha-alumina crystals with 40% ~ 60%, 20% ~ 30% aluminum oxide crystal block and 10% ~ 30% alumina grain are put into crucible after according to the weight percent uniform mixing;
(b), the crucible that will place the alpha-alumina crystals material puts into long brilliant stove and vacuumizes, and the temperature of long brilliant stove is heated to 2200 ℃, to the alpha-alumina crystals material material in the crucible;
(c), when the alpha-alumina crystals in the crucible is heated to molten state, long brilliant stove is lowered the temperature, the temperature of crucible is reduced between 2150 ℃ ~ 2200 ℃; And when solid-liquid interface occurring in the crucible, begin the alpha-alumina crystals seeding in the crucible;
(d), after the alpha-alumina crystals seeding in the crucible finishes, long brilliant stove is lowered the temperature, make the temperature of crucible reduce to 1900 ℃ ~ 2100 ℃, so that long brilliant in crucible;
(e), treat after long brilliant operation is finished in the crucible long brilliant stove to be incubated;
(f), long brilliant stove is annealed, make the temperature in the long brilliant stove reduce to 1000 ℃ gradually by 2000 ℃;
(h), long brilliant stove is carried out making the temperature of long brilliant stove reduce to normal temperature gradually after annealing operation finishes;
(i), after reducing to normal temperature in the long brilliant stove, in the long brilliant stove with the argon gas vacuum breaker, open long brilliant stove and also take out sapphire crystal.
2. according to the growth method of the described sapphire crystal of claim 1, it is characterized in that: in the described step (c), the seeding post by crucible top and be positioned at the seed crystal seeding of seeding column end; During seeding, the end of seed crystal and seeding post is extended the solid-liquid interface place of crucible, the moving seed crystal of seeding cornice rotates in crucible.
3. according to the growth method of the described sapphire crystal of claim 1, it is characterized in that: in the described step (e), when length is brilliant in the crucible, rotate the crucible that is positioned at long brilliant stove.
4. brilliant furnace structure of length that sapphire crystal growth is used, it is characterized in that: comprise body of heater (16), the bottom of described body of heater (16) is provided with the rotation brace table (8) that is used to place crucible (18), and described rotation brace table (8) is positioned at the centre of body of heater (16); Be provided with the thermal field (13) that is used for crucible (18) heating in the body of heater (16), described thermal field (13) is positioned at the outer ring of rotation brace table (8); Outer ring corresponding to thermal field (13) in the body of heater (16) is provided with thermal insulation layer (7); The bottom of body of heater (16) is provided with water-in (9) and water outlet (10), and described water-in (9) is connected with body of heater (16) with water outlet (10); The top of body of heater (16) is provided with tracheae (3), and described tracheae (3) is connected with body of heater (16).
5. the brilliant furnace structure of using according to the sapphire crystal growth of claim 4 of length, it is characterized in that: described thermal field (13) comprises electromagnetism or resistance heating coil.
6. the brilliant furnace structure of using according to the sapphire crystal growth of claim 4 of length is characterized in that: described rotation brace table (8) be used for driving the following drive-motor (11) that rotation brace table (8) rotates and link to each other; The central section of rotation brace table (8) is provided with rotation back shaft (15), and described rotation back shaft (15) links to each other with the output shaft of lower rotating electrical machine (11).
7. the brilliant furnace structure of using according to the sapphire crystal growth of claim 4 of length is characterized in that: the bottom in the described body of heater (16) is provided with and is used for thermometric thermopair (12); Described thermopair (12) is a rhenium thorium alloy thermopair.
8. the brilliant furnace structure of using according to the sapphire crystal growth of claim 4 of length is characterized in that: the top in the described body of heater (16) is provided with CCD video sensor (2).
9. the brilliant furnace structure of using according to the sapphire crystal growth of claim 4 of length, it is characterized in that: the top of described body of heater (16) is provided with rotating machine (1), the described output shaft of going up rotating machine (1) is provided with seeding post (14), and the other end that described seeding post (14) links to each other corresponding to the output shaft with last rotating machine (1) stretches in the body of heater (16); Seeding post (14) is equipped with seed crystal (4) corresponding to the end of stretching in the body of heater (16).
10. the brilliant furnace structure of using according to the sapphire crystal growth of claim 9 of length, it is characterized in that: the described rotating machine (1) of going up links to each other with the output terminal of controller (17), and described controller (17) links to each other with the thermopair (12) and the lower rotating electrical machine (11) that are used to observe the interior CCD video sensor (2) of body of heater (16), be used to measure the interior working temperature of body of heater (16) respectively; The output shaft of described lower rotating electrical machine (11) links to each other with rotation brace table (8).
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