CN1599031A - Method of preparing high quality non-polar GaN self-support substrate - Google Patents
Method of preparing high quality non-polar GaN self-support substrate Download PDFInfo
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- CN1599031A CN1599031A CN200410041436.1A CN200410041436A CN1599031A CN 1599031 A CN1599031 A CN 1599031A CN 200410041436 A CN200410041436 A CN 200410041436A CN 1599031 A CN1599031 A CN 1599031A
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- 239000000758 substrate Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 28
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims abstract description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 13
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 13
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 13
- 229910052744 lithium Inorganic materials 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 3
- MNKMDLVKGZBOEW-UHFFFAOYSA-M lithium;3,4,5-trihydroxybenzoate Chemical compound [Li+].OC1=CC(C([O-])=O)=CC(O)=C1O MNKMDLVKGZBOEW-UHFFFAOYSA-M 0.000 abstract 3
- 238000005406 washing Methods 0.000 abstract 1
- 229910002601 GaN Inorganic materials 0.000 description 55
- 239000010408 film Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 11
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910010092 LiAlO2 Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
The invention discloses a method of high quality nonpolar GaN self-supporting substrate. We make the high quality nonpolar GaN self-supporting substrate from the lithium aluminate or lithium gallate acid substrate. After washing it, the lithium aluminate or lithium gallate acid substrate is put into the reactor, raise the temperature to the growth temperature of between 800deg.C and 950deg.C and choose the NH3 and HCl as the raw gases until the growth finishes. The features of the invention lie in the following aspects: because the lattice constant of the lithium aluminate (001) or lithium gallate acid is almost same with that of the GaN (11-20) and has no great structural mismatch, the dislocation density of the GaN film is relatively low and the film has high quality.
Description
One, technical field
The present invention relates to utilize hydride vapour phase epitaxy method at novel substrate lithium aluminate (LiAlO2) (perhaps lithium gallium oxide, LiGaO2) growing GaN film and obtain the method and the technology of self-supporting non-polar GaN backing material on the substrate.
Two, technical background
With GaN and InGaN, AlGaN alloy material is that the III group nitride material of representative is the novel semiconductor material of extremely paying attention in the world in recent years.The direct band gap of its 1.9-6.2eV continuous variable, excellent physics, chemical stability, high saturated electron drift velocity, superior functions such as high disruptive field intensity and high heat conductance make it become the most preferably material of short wavelength's semiconductor photoelectronic device and high frequency, high pressure, the preparation of high temperature microelectronic component.
The III group-III nitride has broad application prospects in field of optoelectronic devices such as light demonstration, optical storage, optical illumination.Aspect light demonstration and optical illumination, super large-screen and full color display with the making of high efficiency blue-green light LED, the multidate information that can be used for the various occasions in indoor and outdoor shows, makes ultra-large type, whole plane, high definition, radiationless, low-power consumption, true color large scale display field also account for quite great proportion.The high efficiency white light emitting diode is as the novel high-efficiency and energy-saving solid light source, useful life was above 100,000 hours, comparable incandescent lamp economize on electricity 5-10 doubly, reach the dual purpose that economizes on resources, reduces environmental pollution, will worldwide cause an epoch-making deep revolution of lighting electric light source surely.
Aspect optical storage and optical detection, the blue-light semiconductor laser is used to make DVD of future generation, can improve storage density more than 20 times than present CD CD.And the characteristics of gallium nitride material broad-band gap have also guaranteed its application prospect at semiconductor device such as high temperature, high-power and ultraviolet light detectors.It has advantages such as high reliability, high efficiency, response fast, long-life, total solidsization, volume are little, will bring into play significant role in fields such as spaceship, the detection of rocket plumage cigarette, Atmospheric Survey, fire.
In the end of the year 1994, Japanese Giat Ind SA takes the lead in releasing III group-III nitride brightness blue light Light-Emitting Diode (LED), and the said firm releases green light LED again subsequently, has now formed the large-scale production ability.In December nineteen ninety-five, the said firm develops first III group-III nitride Multiple Quantum Well laser diode (LD) in the world, and the device stream time surpasses 10,000 hours at present, has released be pilot.It is 100,000 hours GaN based high-power semiconductor laser that Sony has been released life expectancy in October, 2002.From the market angle, the market of GaN base LED constantly enlarges, and its market is with the speed increment in every year 30%.
But, GaN base LED and LD product be dropped into the consumption market, must do to improve accordingly and improve to the brightness and the process yield of GaN light-emitting diode and laser diode.The key of blue light GaN base LED and LD production development is the GaN crystal substrates that will obtain the fabricating low-defect-density of reasonable price, to adapt to the oriented growth of film GaN crystal in LED and the LD, does not also have the GaN substrate of this low defective in the market.
Therefore, lacking the GaN epitaxial substrate is the most basic factor that hinders III group nitride material and device technology development, is the current forward position high-tech of attaching great importance in the world, has very important technology and Practical significance.
Because the fusing point high (～3000 ℃) of GaN, and about 1600 ℃, can decompose, be difficult to grow GaN monocrystalline more than 4 inches with traditional crystal technique, can only accomplish especially that at present several millimeters are square, can not reach the requirement of making microelectronic component and opto-electronic device far away.Thereby the GaN backing material technology of the suitable scale manufacturing of exploitation is most important to development GaN semiconductor device industry.
Solving the major technique of this difficult problem at present, is GaN horizontal extension technology.Horizontal extension is exactly deposit masking material on the GaN planar materials that has obtained (as SiO2, Si3N4, W etc.) and carves specific graphical window, carries out the secondary epitaxy of GaN more thereon." accurate free " growth conditions owing to meet, and the direction of growth is perpendicular to the direction of climbing of former GaN dislocation, thereby the Grown GaN film has very high quality.Employing horizontal extension technology can reduce the dislocation density in the epitaxial loayer significantly, typically can be from～10
10/ cm
2Be reduced to＜10
6/ cm
2After horizontal extension GaN substrate on carry out thick film growth, and be aided with film-substrate separation technology, with substrate and GaN divided thin film from, just can obtain the more GaN backing material of low-dislocation-density.
The GaN backing material that adopts horizontal extension technology and HVPE thick film growing technology and lift-off technology to obtain, can be directly used in the high-power III-N semiconductor short wavelength laser of development on the one hand, high temperature, high frequency, high power electronic device, multiple novel semi-conductor devices such as UV photodetector part.On the other hand, GaN substrate itself also has huge market value.Owing to may have bigger horizontal tension in the ELOG film, may limit its application aspect bluish violet light laser.But by on ELOG GaN substrate, carry out more higher-quality GaN HVPE growth of low-dislocation-density or epitaxial growth, can eliminate the effect of tension force.The GaN substrate also can be used for wide bandgap materials such as growing high-quality ZnO.Still there is not at present GaN substrate product in enormous quantities, large-size high-quality in the world.
This invention is to utilize novel substrate to come the growing nonpolar face GaN film, utilizes nature difference unique between substrate and the GaN to obtain the GaN backing material of self-supporting.This novel backing material is exactly LiAlO2 (or LiGaO2).。Because the Grown GaN film is (10-10) orientation (see figure 1) on lithium aluminate (100) substrate, the c axle of polarity is in GaN growth for Thin Film face, so can obtain nonpolar GaN film.
Three, technology contents
The present invention seeks to: utilize hydride vapour phase epitaxy method growing nonpolar face GaN film on novel substrate lithium aluminate (LiAlO2) and lithium gallium oxide (LiGaO2) substrate, and the difference of utilizing thermal coefficient of expansion between lithium aluminate and the GaN makes the lithium aluminate substrate peel off automatically, perhaps adopt corroding method to remove lithium aluminate or lithium gallium oxide substrate, obtain high-quality self-supporting GaN backing material.Because the Grown GaN film is (10-10) orientation (see figure 1) on lithium aluminate (100) substrate, the c axle of polarity is in GaN growth for Thin Film face, so can obtain nonpolar GaN film.
Technical solution of the present invention:
At first, in HVPE growing system or MOCVD system, at 850-950 ℃ of growing GaN film; Secondly, control suitable rate of temperature fall, cool the temperature to room temperature, lithium aluminate substrate or lithium gallium oxide substrate and GaN film natural separation can obtain the GaN substrate of self-supporting; Also can adopt corroding method to remove lithium aluminate or lithium gallium oxide substrate.
Mechanism of the present invention and technical characterstic are:
1, because the lattice constant basically identical of lithium aluminate (001) or lithium gallium oxide and GaN (11-20) does not have very big structural mismatch, the GaN thin film dislocation density that growth obtains is lower, and quality is higher.
2, owing to there is bigger Hot expansion coefficient difference between lithium aluminate or lithium gallium oxide and the GaN, suitable control rate of temperature fall, the lithium aluminate substrate can automatically and between the GaN film separate, contact-making surface polishes or corrodes between the two, can obtain the pure GaN self-supporting substrate of high-quality.This has simplified GaN self-supporting underlay producing technique.
3, adopt corroding method also can remove lithium aluminate or lithium gallium oxide substrate easily, obtain self-supporting non-polar GaN substrate.
Four, description of drawings
The interfacial structure graph of a relation of Fig. 1 GaN and lithium aluminate
Fig. 2 the inventive method is in the room temperature PL of 900 ℃ of Grown GaN films spectrum, LASER Light Source: He-Cd325nm.
Fig. 3 utilizes the Raman spectrum of the inventive method (800,900 ℃) Grown GaN film under different temperatures on the lithium aluminate substrate
Five, embodiment
The technology of the present invention implementation process comprises following a few step:
1, the cleaning of lithium aluminate substrate and processing.
2, after the lithium aluminate substrate is put into reactor, slowly be warming up to growth temperature, can begin growing GaN.800～950 ℃ of growth temperatures.Gas flow difference: NH
3Flow is 600sccm, NH
3Carrier gas flux is 600sccm, and the HCl flow is 10sccm, and the HCl carrier gas flux is 20sccm, and total nitrogen is 3000sccm.。
3, grow into the suitable time after.Slowly reduce to room temperature according to certain speed, take out sample.Rate of temperature fall remains on 5～15 ℃/minute for good.
4, utilize the difference of thermal coefficient of expansion between lithium aluminate and the GaN to make the lithium aluminate substrate peel off automatically, perhaps adopt corroding method to remove the lithium aluminate substrate.Utilize the automatic method of stripping of difference substrate of thermal coefficient of expansion to be: the control rate of temperature fall slowly is cooled to room temperature as 10 ℃/minute after growth is finished, and substrate can separate automatically with GaN.Rate of temperature fall is too fast slow excessively, and the lithium aluminate substrate can be cracked, causes that GaN is cracked.
5, residual part lithium aluminate is removed in a mirror polish or the corrosion that the GaN film is contacted with the lithium aluminate substrate.Can obtain high quality GaN self-supporting substrate.Corroding method is: remove the lithium aluminate substrate with inorganic acid.Hydrochloric acid, sulfuric acid, phosphoric acid all can.
6, the inventive method is used for the condition of lithium gallium oxide (LiGaO2) with above-mentioned.Same this method also is applicable to the substrate that has similarity with lithium aluminate.
Claims (4)
1, a kind of method for preparing high-quality non-polar GaN self-supporting substrate, it is characterized in that utilizing the method for lithium aluminate or lithium gallium oxide substrate preparation high-quality non-polar GaN self-supporting substrate, after the cleaning of lithium aluminate or lithium gallium oxide substrate and processing put into reactor, be warming up to growth temperature under 800～950 ℃ of conditions, with NH
3With HCl be unstripped gas growth, finish up to growth.
2, by the described method for preparing high-quality non-polar GaN self-supporting substrate of claim 1, the difference that it is characterized in that utilizing thermal coefficient of expansion is slowly reduced to room temperature with the substrate method of stripping after growth is finished, and rate of temperature fall remains on 5～15 ℃/minute.
3, by the described method of utilizing lithium aluminate or lithium gallium oxide substrate preparation high-quality non-polar GaN self-supporting substrate of claim 1, the control rate of temperature fall slowly was cooled to room temperature as 10 ℃/minute after its feature growth was finished, and substrate can separate automatically with GaN.
4,, it is characterized in that utilizing at the bottom of polishing or the corroding method peeling liner: remove the lithium aluminate substrate with inorganic acid by the described method of utilizing lithium aluminate or lithium gallium oxide substrate preparation high-quality non-polar GaN self-supporting substrate of claim 1.
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| CNB2004100414361A CN1329955C (en) | 2004-07-21 | 2004-07-21 | Method of preparing high quality non-polar GaN self-support substrate |
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| CNB2004100414361A CN1329955C (en) | 2004-07-21 | 2004-07-21 | Method of preparing high quality non-polar GaN self-support substrate |
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| CN1599031A true CN1599031A (en) | 2005-03-23 |
| CN1329955C CN1329955C (en) | 2007-08-01 |
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Cited By (6)
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| CN100344006C (en) * | 2005-10-13 | 2007-10-17 | 南京大学 | Method for developing structure of LED device of InGaN/GaN quantum trap in M faces |
| CN101901758A (en) * | 2010-06-24 | 2010-12-01 | 西安电子科技大学 | MOCVD growth method of non-polar m-surface GaN film based on m-surface SiC substrate |
| CN101509145B (en) * | 2009-02-24 | 2011-03-30 | 上海蓝光科技有限公司 | Method for growing nonpolar a face GaN film on lithium aluminate substrate |
| CN102828251A (en) * | 2012-09-10 | 2012-12-19 | 中国科学院半导体研究所 | Method for preparing aluminum nitride single crystal material |
| WO2018165910A1 (en) * | 2017-03-13 | 2018-09-20 | 中国科学院福建物质结构研究所 | Porous gallium nitride single crystal material, preparation method therefor and use thereof |
| CN110670135A (en) * | 2018-07-03 | 2020-01-10 | 中国科学院福建物质结构研究所 | Gallium nitride single crystal material and preparation method thereof |
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| US6632725B2 (en) * | 2001-06-29 | 2003-10-14 | Centre National De La Recherche Scientifique (Cnrs) | Process for producing an epitaxial layer of gallium nitride by the HVPE method |
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| CN1227718C (en) * | 2003-02-18 | 2005-11-16 | 华南师范大学 | Method for making gallium nitride crystal |
| CN1450208A (en) * | 2003-05-09 | 2003-10-22 | 中国科学院上海光学精密机械研究所 | Method for growing lithium aluminate and lithium gallate crystals |
-
2004
- 2004-07-21 CN CNB2004100414361A patent/CN1329955C/en not_active Expired - Fee Related
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| CN101509145B (en) * | 2009-02-24 | 2011-03-30 | 上海蓝光科技有限公司 | Method for growing nonpolar a face GaN film on lithium aluminate substrate |
| CN101901758A (en) * | 2010-06-24 | 2010-12-01 | 西安电子科技大学 | MOCVD growth method of non-polar m-surface GaN film based on m-surface SiC substrate |
| CN101901758B (en) * | 2010-06-24 | 2012-05-23 | 西安电子科技大学 | MOCVD growth method of non-polar m-surface GaN film based on m-surface SiC substrate |
| CN102828251A (en) * | 2012-09-10 | 2012-12-19 | 中国科学院半导体研究所 | Method for preparing aluminum nitride single crystal material |
| CN102828251B (en) * | 2012-09-10 | 2015-02-18 | 中国科学院半导体研究所 | Method for preparing aluminum nitride single crystal material |
| WO2018165910A1 (en) * | 2017-03-13 | 2018-09-20 | 中国科学院福建物质结构研究所 | Porous gallium nitride single crystal material, preparation method therefor and use thereof |
| CN108570709A (en) * | 2017-03-13 | 2018-09-25 | 中国科学院福建物质结构研究所 | A kind of nitride porous algan single crystal material, preparation method and application |
| CN110670135A (en) * | 2018-07-03 | 2020-01-10 | 中国科学院福建物质结构研究所 | Gallium nitride single crystal material and preparation method thereof |
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