CN101054723A - Method for growing R-surface sapphire crystal - Google Patents
Method for growing R-surface sapphire crystal Download PDFInfo
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- CN101054723A CN101054723A CN 200710073286 CN200710073286A CN101054723A CN 101054723 A CN101054723 A CN 101054723A CN 200710073286 CN200710073286 CN 200710073286 CN 200710073286 A CN200710073286 A CN 200710073286A CN 101054723 A CN101054723 A CN 101054723A
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Abstract
The present invention provides a process for upgrowth of R surface sapphire to develop crystal with synthetic fused mass method, wherein a czochralski method is adopted for seminationsowing, neck receiving and shoulder putting, and a kyropoulos method and/or temperature gradient technique is adopted during the equal-diameter growth. The equipments and the modes of heating used in the process are not restricted strictly, and a czochralski equipment is adopted usually, which can be used regardless induction heating or resistance heating. Said process possess the advantages of czochralski method, kyropoulos method and temperature gradient technique: it can develop crystal with large size without much pollution, wherein the liquid level and the instances of crystal growth can be observed; it can also adopt the existent czochralski method equipment. At the same time, the process overcomes the shortcomings (such as high color centre and location erroneous rate) of the czochralski method and the temperature gradient technique, can produce crystal with excellent quality, small stress, without slip band and twins defects, with low dislocation density, with excellent crystal perfection and optical homogeneity, easy to its industrialization.
Description
Technical field
The present invention relates to crystal growth, be specifically related to melt growth R surface sapphire crystal, particularly in conjunction with a kind of comprehensive melt growth method that lifts, steeps multiple growth patterns such as living and warm ladder.
Technical background
Gan (GaN) is after silicon single-crystal, and one of most important novel material that the mankind find at semiconductor applications is a revolution in fields such as light source, demonstration, illumination.The most widely used at present GaN substrate material is a sapphire crystal.
Usually the GaN epitaxial film for preparing on sapphire is grown along the C axle, and the C axle is the polar axis of GaN, cause occurring in the GaN base device active layer quantum well very strong built in field, therefore luminous efficiency can reduce, development non-polar plane extension, be expected to overcome this physical phenomenon, luminous efficiency is improved.
LED generally adopts the sapphire of (0001) face (being the C face).Along with the brightness of LED is more and more higher, also more and more stricter to the requirement of substrate manufacturer.Heavy caliberization also will be an important topic from now on.
Studies show that, adopt surface passivation and MOCVD low-temperature epitaxy to go up formation InGaN quantum dot, and constitute the multilayered structure of this quantum dot at sapphire (0001) face (being the C face) and sapphire (1102) face (being the R face).The InGaN quantum dot of growing on the InGaN quantum dot of growing on the R surface sapphire substrate and the C surface sapphire substrate is compared, and its photoluminescence (PL) is composed not only intensity height, and does not have multi-peaks structure.Be used in the InGaN quantum dot of growing on the R surface sapphire and be expected to avoid the influence of built in field, obtain the stable luminescent device of high-quantum efficiency and emission wavelength as active layer.
At present, from melt growing crystal be the preparation crystal the most frequently used with most important a kind of method.Needed monocrystal material during modern technologies such as electronics, optics are used, major part prepares with the melt growth method.For example: Si, Ge, CaAs, GaP, LiNbO
3, Nd:YAG, Nd:Cr:GSGG, LiAlO
2, Al
2O
3And Ti:Al
2O
3Crystal etc., and the halogen compound of some basic metal and alkaline-earth metal etc.Many crystal enter the suitability for industrialized production of different scales already.
The method of growing crystal is varied in the melt, for example crystal pulling method at first is to introduce seed crystal to form a monocrystalline nuclear in melt, then, constantly carry out rearranging of atom or molecule on the boundary of nucleus melt, the array of being piled up directly changes oldered array into and forms crystal.This is the most general the most frequently used method.Also have warm terraced method, that is the Bridgman method, utilize thermograde that melt in the crucible is solidified into crystal gradually, wherein can be with or without seed crystal, also can keep temperature-resistant and make degradation under the crucible.Kyropoulos (Kyropoul method) seed crystals that use are immersed in melt inner control temperature with it and grow, wherein slowly rotary pulling or not rotary pulling more.The top-seeded solution growth that also has flux method and improvement thereof, zone melting method, melting zone method (float-zone method), flame melt method or the like.
Crystal pulling method has been realized industrialization at first, for example semiconductor crystal such as silicon single crystal; Also have oxide crystal such as garnet class, sapphire and ruby, niobium, tantalic acid salt and nonlinear optics borate family crystal.The patent documentation of this respect piece is unequal to poly-.But this method defectiveness at first is that crystal diameter is limited by crucible diameter, and both ratios generally are 1: 3, only about 1: 2 of elemental crystal such as silicon single-crystal maximum, and therefore many improvement flowers are at continuous charging (for example continuous growth of silicon single-crystal); Next is to have concentration gradient when the material that mixes than the heavy ion radius, has a strong impact on use.
The patent of crystal pulling method such as KR2001017991, RU2164267, JP11121855sls, JP10338594, US5866092 etc.The patent such as the CN 85100534 of the terraced method of temperature, RU 2049832 etc.Its shortcoming is to contain defectives such as bubble in the crystal, is difficult to obtain high quality crystal.Also have CN 97106255 and JP7010672 etc., vertical warm terraced method growing lithium aluminate and lithium gallate crystal.The patent of kyropoulos such as CS8801546 and CS264935.Its shortcoming is that the speed of growth is slow, is unfavorable for industrialization.Different methods has different separately relative merits.
ZL200310112171.5 has proposed a kind of comprehensive melting method, and it has inherited common crystal pulling method, and the advantage of kyropoulos and warm terraced method has overcome the main drawback of crystal pulling method and warm terraced method growing crystal simultaneously.
Summary of the invention
The growth method that the purpose of this invention is to provide a kind of R surface sapphire crystal with comprehensive melt method for growing crystal, wherein uses crystal pulling method to sow, receive neck, shouldering, adopts kyropoulos and/or warm terraced method when isodiametric growth.
About another patent of invention of comprehensive melt ratio juris and the visible the applicant of method, i.e. ZL200310112171.5, on July 22nd, 2005 authorized, and title is " a comprehensive melt method for growing crystal ", and its content this paper is in conjunction with quoting.
Other purposes of the present invention and advantage will be more clear hereinafter.
Purpose of the present invention is intended to overcome above-mentioned the deficiencies in the prior art, and a kind of comprehensive melting method is provided, can growing large-size high-quality R surface sapphire crystal.This method uses crystal pulling method to sow, receive neck, shouldering, adopts kyropoulos and/or warm terraced method when isodiametric growth.
At first introduce seed crystal in melt, carry out seeding and shouldering with general crystal pulling method, wherein seed crystal is fallen in the crucible in the raw-material melt, it is molten that seed crystal and melt are soaked mutually.Induce by seed crystal that molecule is rearranged for oldered array on solid-liquid body interface, form crystal.Utilize crystal growing and pulling device rotation, vertical operation to control crystalline growth velocity, until reaching the diameter that needs.The general technology parameter of crystal pulling method all is known, and certainly, different its parameters of raw material are different; But can obtain by conventional optimization test fully, need not to give unnecessary details.Generally speaking, rotating speed between 5～200rpm, preferred 10～50rpm.Between the general 0.1～5.0mm/hr of pulling rate, preferred 1.0～2.5mm/hr.
During isodiametric growth, can stop to lift or lifting with low speed, cooling simultaneously is so that all carry out the growth of crystalline major portion under melt liquid level.Can be that kyropoulos also can be warm terraced method or both combinations.So, growing environment is stable, is easy to obtain the crystal of good quality.Meanwhile, broken through the diameter restrictions of crystal pulling method, can growth diameter greater than the crystal of crystal pulling method.In other words, use the general technology parameter of kyropoulos and/or warm terraced method during isodiametric growth.Equally, these processing parameters are different and variant according to raw material, can obtain by conventional optimization test equally.The disclosed parameter of above-mentioned reference all can be used for reference.Cooling rate is generally between 0.1～5 ℃/hr when using warm terraced method; The big cooling rate of crystalline size is slow, otherwise fast slightly.When using kyropoulos, can lift also and can not lift, rotate or do not rotate.Cooling rate is faster a little than the terraced method of temperature.Rotating speed is generally 0～50, preferred 5～20rpm; Pulling rate is generally 0～5, between preferred 0.2～2.0mm/hr.
When crystal growth finishes, crystal is proposed the liquid level of melt.If have the rotation and lift, can stop in good time, controlled temperature is slowly reduced to room temperature then.This moment, cooling rate can be used for reference the cooling rate of kyropoulos, generally between 10～100 ℃/hr.Or between 1～100 ℃/hr of warm terraced method.Certainly, the later stage can be strengthened cooling rate, and not ftractureing with crystal is as the criterion.
Equipment that present method is used and type of heating do not have strict restriction, use the general equipment that lifts usually; No matter induction heating still is a resistive heating can both be used.In conjunction with sophisticated equipment and computer control present method is attained a yet higher goal.And use a computer control and going up or LOAD CELLS and optics or infrared sensor etc. down of the crystal growth equipment of China at present finishes that employed equipment is exactly computer control and last LOAD CELLS when of the present invention more.In other words, although the temperature field of kyropoulos and/or warm terraced method and crystal pulling method is slightly variant, there is no particular requirement in the method.In general, the lower limit of the common temperature of a use crystal pulling method scope gets final product or is lower.Because in melt growth, the temperature field of the whole bag of tricks is similar.When thermograde is excessive,, easily produce defective though can make fast growth crystal thermal stresses big.Temperature is terraced when too small, though it is slow to make crystal mass improve the speed of growth, is unfavorable for industrialization.The warm ladder of crystal pulling method can be bigger, and bubble is living relative less with the warm ladder of warm terraced method.From the crystal growth principle, guaranteeing that warm ladder is the bigger the better under the crystalline quality situation, the big output height of temperature ladder.During the good crystal growth of thermal conductivity, warm ladder can be greatly; The crystal temperature ladder of poor heat conductivity is then smaller.As long as by simple optimization test, be not difficult to obtain suitable temperature field.In addition, need be aspect insulation need suitably to strengthen, because present method crystalline size big than simple crystal pulling method sometimes.
Equally, crucible is not had strict restriction yet, only otherwise with fusant reaction and can be just in the operation of crystal pulling temperature.For example precious metal crucible, oxide compound crucible or quartz crucible etc., different crystal different heating mode is used different crucibles, and this is well known to those skilled in the art.During the growth high temperature crystal, resistive heating can be used graphite, tungsten or molybdenum or the heating of its alloy.In this case, generally adopt inert atmosphere or reducing atmosphere; Use tungsten, molybdenum or its alloy radiation shield and crucible simultaneously.
Description of drawings
Fig. 1 is the warm field device structural representation of the inventive method growth R surface sapphire crystal;
Fig. 2 is the synoptic diagram of the inventive method growth R surface sapphire crystal.
Wherein 1 is the Medium frequency induction coil, the 2nd, and die casting mica base, the 3rd, zirconium white collet, the 4th, zirconium white insulation sand, the 5th, zirconium white insulation base, the 6th, zirconium white ring, the 7th, stay-warm case on the zirconium white, the 8th, refractory brick cover (1), the 9th, refractory brick cover (2), the 10th, quartz socket tube, the 11st, miramint crucible cover, the 12nd, miramint crucible, the 13rd, ceramic lifting rod, the 14th, miramint seed chuck, the 15th, seed crystal, the 16th, liquid level, the 17th, melt, the 18th, crystal.
Hereinafter with reference to accompanying drawing in detail the present invention is described in detail in conjunction with specific embodiments, same numbers is represented same parts in the accompanying drawing.Certainly, embodiment is only for explanation restriction absolutely not.
Embodiment
Embodiment 1
Use homemade single crystal growing furnace (for example factory of Xi'an University of Technology makes, and has computer control, last LOAD CELLS), the miramint crucible, Frequency Induction Heating, the zirconium white lagging material, specific configuration is as shown in Figure 1.
The direction of growth of R surface sapphire be [1120] to, therefore use [1120] to seed crystal.
The aluminum oxide 2500 that sintering is crossed restrains the crucible of putting into diameter 100mm, vacuumizes to reach 10
-2Charge into hydrogen behind the Pa to 0.8atm.Heat up and melt, reduce seed rod preheating seed crystal, seed crystal rotating speed 30rpm allows seed crystal contact melt liquid level, lifts with 2.5mm/hr after the thermal equilibrium; Receive neck and shouldering.Gradual slow reduces pulling rate and rotating speed behind the about 15mm of crystal diameter, branch is clipped to 1.5mm/hr and 15rpm is 30mm until crystal diameter, reduce pulling rate and rotating speed according to the further gradual slow of the amplification of crystal diameter, when diameter is 60mm left and right sides Shi Tingla, rotating speed is 8rpm.Thermal equilibrium 40 minutes, this moment, diameter still can strengthen a little.With the speed cooling of 0.2 ℃/hr, the cooling rate gradual slow is until 0.5 ℃/hr two days later.What of clout the reduction of observing melt liquid level judge, slowly pulling crystal leaves melt then, and beginning is accelerated cooling rate gradually with the cooling of 20 ℃/hr speed, and until reducing to room temperature, blank is taken out in blow-on.
Cut blank end to end, directed R face (1102) is cut the 2mm thin slice, and polishing both surfaces is carried out optical detection, and the result is as follows:
Dislocation desity D＜3 * 10
3/ cm
2,
Optical transmittance: ultraviolet 0.3 mu m waveband T＞80%; 0.4～4 mu m waveband T＞87%;
Optical homogeneity Δ n=2 * 10
-5
Do not have bubble, be mingled with in the crystal of growth, macroscopic defects such as cracking.
Embodiment 2
With step and the equipment of embodiment 1, seeding shouldering speed that different is is 1.5 to change to 1.0mm/hr gradually, and rotating speed remains on 10rpm always.Obtain the R surface sapphire of good quality.
Embodiment 3
With step and the equipment of embodiment 1, different tungsten crucible and the tungsten crucibles lids of being to use, the gas that charges into is nitrogen, and seeding shouldering speed is 1.5 to change to 1.0mm/hr gradually, and rotating speed remains on 10rpm always.Obtain the R surface sapphire of good quality equally, low-dislocation-density, low scattering, structural integrity height, optical homogeneity Δ n=9 * 10
-7
Embodiment 4
Substantially according to embodiment 1 same step and equipment, different be to use Iridium Crucible and iraurite crucibles cover, and the gas that charges into is nitrogen; Pull rate during the seeding shouldering is 1mm/h, rotating speed 15rpm; Stop during isodiametric growth lifting, rotating speed 5rpm, cooling rate is 0.5 ℃/hr.Obtain the extraordinary crystal of optical homogeneity.Also use the graphite resistance heating in addition under same parameter condition, grow in molybdenum crucible and radiation shield and the argon gas, the crystal optics homogeneity is better than induction heating, but light extraction efficiency is poor slightly, and annealing time is longer.
This method many crystal of can growing. From growing principle, the advantage of this method is self-evident. It continues Held common czochralski method, the advantage of kyropoulos and warm terraced method: but the growing large-size crystal, and pollution is few, in growth Liquid level and crystal growing state can be observed in the process, establishing of original Czochralski grown crystal can also be used Standby, reduced investment. This technology has overcome colour center and the dislocation of czochralski method and warm terraced method grown crystal simultaneously The problem that rate is high can grow the large-size crystals of high-quality, and crystal stress is little, no glide band and Twin Defects, Dislocation density is low, and crystal perfection and optical homogeneity are good; Be easy to industrialization.
Those skilled in the art can do many improvement and conversion after reading specification, but all do not exceed this Bright spiritual scope.
Claims (5)
1. the growth method of a R surface sapphire is characterized in that with comprehensive melt method for growing crystal, uses crystal pulling method to sow, receive neck, shouldering, adopts kyropoulos and/or warm terraced method when isodiametric growth.
2. according to the process of claim 1 wherein that the speed range when lifting is 5～200rpm, the pulling rate scope is 0.1～5.0mm/hr; Cooling rate scope during isodiametric growth is 0.1～5 ℃/hr; During isodiametric growth, speed range is 0～50rpm, and the pulling rate scope is 0～5mm/hr.
3. use induction heating to grow according to the process of claim 1 wherein.
4. use the graphite resistance heating to grow according to the process of claim 1 wherein.
According to the process of claim 1 wherein pulling growth during the stage pulling rate and rotating speed change.
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| CN 200710073286 CN101054723A (en) | 2007-02-07 | 2007-02-07 | Method for growing R-surface sapphire crystal |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102115911A (en) * | 2011-03-22 | 2011-07-06 | 北京工业大学 | Crucibleless growth method of sapphire crystals in different atmospheres |
| CN102127803A (en) * | 2011-03-08 | 2011-07-20 | 中国科学院上海硅酸盐研究所 | Growth method of rectangular specially-shaped sapphire crystal |
| CN102140675A (en) * | 2011-03-24 | 2011-08-03 | 哈尔滨奥瑞德光电技术股份有限公司 | Kyropoulos method for quickly growing large-size sapphire single crystal |
| CN102598317A (en) * | 2009-10-16 | 2012-07-18 | 首尔Opto仪器股份有限公司 | High-quality nonpolar or semipolar semiconductor device on porous nitride semiconductor and fabrication method thereof |
| CN102703970A (en) * | 2012-07-11 | 2012-10-03 | 浙江特锐新能源有限公司 | Kyropous method growth of titanium doped sapphire crystals |
| CN102978694A (en) * | 2012-11-05 | 2013-03-20 | 浙江东海蓝玉光电科技有限公司 | Improved kyropoulos method for sapphire crystal growth |
| CN103266356A (en) * | 2013-04-02 | 2013-08-28 | 苏州海铂晶体有限公司 | Method to prolong tungsten crucible cover |
| CN105135883A (en) * | 2015-08-27 | 2015-12-09 | 北京矿冶研究总院 | Intermediate frequency furnace high temperature sintering is with thermal-insulated frock |
| CN113308738A (en) * | 2021-06-01 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | Method for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
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2007
- 2007-02-07 CN CN 200710073286 patent/CN101054723A/en active Pending
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| US9153737B2 (en) | 2009-10-16 | 2015-10-06 | Seoul Viosys Co., Ltd. | High-quality non-polar/semi-polar semiconductor device on porous nitride semiconductor and manufacturing method thereof |
| CN102598317A (en) * | 2009-10-16 | 2012-07-18 | 首尔Opto仪器股份有限公司 | High-quality nonpolar or semipolar semiconductor device on porous nitride semiconductor and fabrication method thereof |
| CN102011184A (en) * | 2010-12-29 | 2011-04-13 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102011184B (en) * | 2010-12-29 | 2013-04-10 | 四川鑫通新材料有限责任公司 | Production method of alpha-aluminum oxide single crystal |
| CN102127803B (en) * | 2011-03-08 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Growth method of rectangular specially-shaped sapphire crystal |
| CN102127803A (en) * | 2011-03-08 | 2011-07-20 | 中国科学院上海硅酸盐研究所 | Growth method of rectangular specially-shaped sapphire crystal |
| CN102115911B (en) * | 2011-03-22 | 2012-08-15 | 北京工业大学 | Crucibleless growth method of sapphire crystals in different atmospheres |
| CN102115911A (en) * | 2011-03-22 | 2011-07-06 | 北京工业大学 | Crucibleless growth method of sapphire crystals in different atmospheres |
| CN102140675A (en) * | 2011-03-24 | 2011-08-03 | 哈尔滨奥瑞德光电技术股份有限公司 | Kyropoulos method for quickly growing large-size sapphire single crystal |
| CN102140675B (en) * | 2011-03-24 | 2012-11-21 | 哈尔滨奥瑞德光电技术股份有限公司 | Kyropoulos method for quickly growing large-size sapphire single crystal |
| CN102703970A (en) * | 2012-07-11 | 2012-10-03 | 浙江特锐新能源有限公司 | Kyropous method growth of titanium doped sapphire crystals |
| CN102978694A (en) * | 2012-11-05 | 2013-03-20 | 浙江东海蓝玉光电科技有限公司 | Improved kyropoulos method for sapphire crystal growth |
| CN103266356A (en) * | 2013-04-02 | 2013-08-28 | 苏州海铂晶体有限公司 | Method to prolong tungsten crucible cover |
| CN105135883A (en) * | 2015-08-27 | 2015-12-09 | 北京矿冶研究总院 | Intermediate frequency furnace high temperature sintering is with thermal-insulated frock |
| CN113308738A (en) * | 2021-06-01 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | Method for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
| WO2022252544A1 (en) * | 2021-06-01 | 2022-12-08 | 中国电子科技集团公司第十三研究所 | Method for preparing compound semiconductor crystal by combining continuous lec and vgf after injection synthesis |
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