CN102465337A - Multi-piece multi-source horizontal hydride vapor phase epitaxy growth system - Google Patents
Multi-piece multi-source horizontal hydride vapor phase epitaxy growth system Download PDFInfo
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- CN102465337A CN102465337A CN2010105497544A CN201010549754A CN102465337A CN 102465337 A CN102465337 A CN 102465337A CN 2010105497544 A CN2010105497544 A CN 2010105497544A CN 201010549754 A CN201010549754 A CN 201010549754A CN 102465337 A CN102465337 A CN 102465337A
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- 230000012010 growth Effects 0.000 title claims abstract description 68
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 title abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 49
- 239000010439 graphite Substances 0.000 claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 239000007789 gas Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- 150000004678 hydrides Chemical class 0.000 claims description 16
- 229910052594 sapphire Inorganic materials 0.000 claims description 11
- 239000010980 sapphire Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 5
- 230000005674 electromagnetic induction Effects 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 24
- 238000000407 epitaxy Methods 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 239000010408 film Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 5
- 239000012159 carrier gas Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000003319 supportive effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to a multi-piece multi-source horizontal hydride vapor phase epitaxy growth system, wherein a reaction chamber is of a horizontal structure, a graphite support is arranged in a growth region, different reaction sources are respectively provided with independent input pipelines, and epitaxy growth substrates are arranged on the graphite support. The multi-piece multi-source horizontal hydride vapor phase epitaxy (HVPE) growth system provided by the invention realizes large-scale application of GaN-based material growth and has the capability of growing multiple pieces of large-area GaN-based materials in one step.
Description
Technical field
The present invention relates to multiple-piece hydride gas-phase epitaxy (HVPE) growing semiconductor material such as GaN sill method and apparatus, be the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source system.
Background technology
With GaN and InGaN, AlGaN alloy material is that master's III-V group nitride material (claiming the GaN sill again) is the novel semiconductor material of extremely paying attention in the world in recent years.The GaN sill is the direct band gap semiconductor material with wide forbidden band, has the direct band gap of continuous variable between the 1.9-6.2eV, excellent physics, chemicalstability; High saturated electron drift velocity; High-performances such as high breaking down field strength and high heat conductance have important use at aspects such as short wavelength's semiconductor photoelectronic device and high frequency, high pressure, the preparations of high temperature microelectronic device, are used for making such as indigo plant, purple, ultraviolet band luminescent device, sensitive detection parts; High temperature, high frequency, High-Field high power device; Feds, radioprotective device, piezoelectric device etc.
The growth of GaN sill has a variety of methods, like gas phase epitaxy of metal organic compound (MOCVD), HTHP compound body GaN monocrystalline, molecular beam epitaxy (MBE), subliming method and hydride gas-phase epitaxy (HVPE) etc.Because the restriction of the physical properties of GaN sill own, the growth of GaN body monocrystalline has very big difficulty, as yet practicability not.Hydride gas-phase epitaxy can be used for isoepitaxial growth self-supporting GaN substrate owing to have high growth rate and horizontal-vertically extension ratio, causes to pay attention to widely and study.Early stage people mainly adopt hydride gas-phase epitaxy (HVPE) method direct growth GaN sill on Sapphire Substrate, separate again, obtain the GaN substrate material.The outstanding shortcoming of this method is that dislocation desity is very high in the GaN epitaxial film, generally reaches 10
10Cm
-2About.Present main method is to adopt methods such as horizontal extension, suspension extension, is aided with HVPE two-forty epitaxy technology growth thick film, at last former substrate is removed, thereby is obtained the lower self-supporting GaN substrate material of dislocation desity.Up to now, the self-supporting GaN substrate that the HVPE growth obtains, dislocation desity is lower than 10
6Cm
-2, area has reached 2 inches.But still can not satisfy the demand of practical application far away.
Because the restriction that traditional HVPE internal system structure, air-flow transport etc., HVPE still is mainly used in monolithic or three growths, thereby has limited the application of HVPE GaN sill, can't effectively bring into play the advantage of HVPE system.The present invention has provided a kind of horizontal HVPE growing system of multi-source that can be used for GaN sill growth in enormous quantities.
Summary of the invention
The problem that the present invention will solve is: the restriction that existing HVPE system receives that internal structure, air-flow transport etc., can not satisfy the growing requirements of GaN base thick-film material in enormous quantities.
Technical scheme of the present invention is: the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source system, comprise reaction cavity and heating system, and be provided with the vitellarium in the reaction cavity; Be provided with the graphite rest in the vitellarium, reaction cavity is a horizontal type structure, and reflection cavity one end is the reaction source inlet; One end is the tail gas outlet, and different reaction sources is respectively equipped with independently input channel, and said input channel stretches into reaction cavity before the graphite rest by the reaction source inlet; The graphite rest is square, places the multi-disc epitaxial growth substrate on the graphite rest, the size of graphite rest by what of epitaxial growth substrate quantity from 60 * 60mm to 350 * 350mm; Epitaxial growth substrate is evenly distributed on the graphite rest; The vitellarium temperature is 1000～1100 ℃, and reaction cavity adopts silica tube, and reaction chamber pressure remains on the 0.1-1.1 normal atmosphere.
Further, the bearing surface relative wind direction of graphite rest tilts 1～45 °, is used for improving the homogeneity of GaN on the substrate that multi-disc arranges; The graphite rest also can be around the rotation of rest medullary ray, and rotating speed is in order to improve the homogeneity of GaN film from 0-1000 rev/min equally.
The heating system of reaction cavity adopts two warm areas, many warm areas or the control of single warm area temperature; Type of heating is resistance furnace or RF heating; RF heating is: reaction cavity is provided with graphite sleeve outward; Graphite sleeve is placed in the ruhmkorff coil of electromagnetic induction heater, and the graphite sleeve is outer to coat the non-inflammable insulation layer of heat conduction, and places inert gas environment.
As preferably, reaction source is sprayed on the surface of epitaxial growth substrate through quartzy spray header uniformly.
The disposable sheet number that is placed on the epitaxial growth substrate on the graphite rest of the present invention comprises 6,9,15,25 2 inches Sapphire Substrate, perhaps 3,54 inches Sapphire Substrate.
The present invention proposes a kind of horizontal hydride gas-phase epitaxy of multi-disc multi-source formula (HVPE) growing system; To realize the large-scale application of GaN sill growth; Can 6,9,15 25 of disposable growths even the big area GaN sill of multi-disc number more, realize the supply in enormous quantities of GaN thick-film material.
Description of drawings
Fig. 1 is the horizontal HVPE system schematic of multiple-piece multi-source of the present invention.HCl and source metal reaction, the gaseous product of generation gets into the vitellarium, reacts at substrate surface and NH3 mixing, forms GaN.Tail gas and reaction dust are extracted out through mechanical pump.The metal source temperature is from 300～1100 degrees centigrade, and the vitellarium temperature is from 400～1100 degrees centigrade.Metal source can increase corresponding gas transport system and source metal pipeline structure as required, realizes the growth of multi-source formula, obtains AlGaInN alloy growth or doping, is the bimetal source structure among the figure.
Fig. 2 is for flat-temperature zone 300 * 300mm of the present invention the time, and the graphite that can adopt sets off structure.Can place 9,25 2 inches Sapphire Substrate or 54 inches Sapphire Substrate.
Embodiment
HVPE of the present invention system comprises several sections: the multipath gas transport system, realize the growth of polynary semiconductor alloy material or mix; Specially designed multiple-piece graphite sets off and corresponding reaction source structure for conveying; The size of graphite rest by what of epitaxial growth substrate quantity from 60X60mm to 350X350mm; Independently inclination/the rotational structure of reaction source transport pipe, graphite rest, to the heating system and the quartzy spray header of big volume vitellarium; Realize the growth in enormous quantities of semiconductor material, also guarantee the quality of growth material when improving output; Novel quartz reaction cavity configuration, this cavity configuration is compact, also can realize the HVPE growth of nitride material when adopting single warm area, efficient energy-saving.Reaction cavity is a horizontal type structure; Reaction cavity one end is the reaction source inlet, and an end is the tail gas outlet, and the centre is the vitellarium; Be provided with the graphite rest in the vitellarium; Different reaction sources is respectively equipped with independently input channel, and said input channel stretches into reaction cavity before the graphite rest by the reaction source inlet, places epitaxial growth substrate on the graphite rest.
The present invention adopt resistance furnace or RF heating all can, key is to guarantee that vitellarium (flat-temperature zone) has suitable length and higher temperature homogeneity, the general temperature in vitellarium is 1000～1100 ℃; Length is according to the size adjustment of graphite rest; In the control of the temperature of heating system, be not limited to two traditional warm area structures, can two warm areas, many warm areas or the control of single warm area all can; Also can realize the HVPE growth of nitride material when adopting single warm area, efficient energy-saving.Can adopt single warm area or two warm area according to the demand of material growth.Under the larger-size situation of graphite rest; The also corresponding increase of reaction cavity volume; Preferred employing this moment RF heating: reaction cavity is provided with graphite sleeve outward; Graphite sleeve is placed in the ruhmkorff coil of electromagnetic induction heater, and the graphite sleeve is outer to coat the non-inflammable insulation layer of heat conduction, and places inert gas environment.This mode can guarantee that the temperature in large-sized reaction cavity internal heating district is even, and can be heated to 1000～1100 ℃ rapidly, when adopting RF heating, can adopt two warm areas also can only single warm area mode.
Many reaction sources multichannel transport structure: the present invention is used for the growth of GaN sill, and reaction source can adopt the different metallic source, gallium, indium, aluminium, magnesium etc., and each source metal all has independently gas transport system.System of the present invention can also adopt source metal to make doping agent when using, and prepares novel nitride semi-conductor material, prepares magnetic semiconductor material as adopting manganese, iron, cobalt, chromium etc. as doping metals.
Vitellarium multi-disc graphite supportive structure: the graphite rest can carry 6 (2 * 3); 9 (3 * 3); 15 (3 * 5) even 25 (5 * 5) 2 inches sapphires, perhaps 3,54 inches sapphire epitaxial growth substrate, epitaxial growth substrate is evenly distributed on the graphite rest; Corresponding graphite rest area shows like Fig. 2 from 120 * 180mm to 350 * 350mm spatial dimension.The graphite rest can be with respect to air flow line certain angle I that tilts; Like I=0～45 degree; Be used for improving the growth homogeneity of GaN sill on the epitaxial growth substrate that multi-disc arranges; The graphite rest also can be around the rotation of rest longitudinal cenlerline, and rotating speed is in order to improve the homogeneity of GaN sill film from 0～1000 rev/min equally.Also can keep tilting under the situation of rest rotation, angle is from 0～45 °.
Reaction cavity adopts the silica tube design, and reaction chamber pressure remains on the 0.1-1.1 normal atmosphere.GaCl or NH
3Gas can adopt another patented technology " improving the method and apparatus of the hydride vapour phase epitaxy growth GaN material homogeneity " patent No.: ZL200810019104.1 of applicant to transporting of substrate surface; Be sprayed at uniformly through quartzy spray header on the surface of epitaxial growth substrate, also can adopt the mode of reaction source as shown in Figure 1 direct gaseous diffusion under the conveying of carrier gas.
Nitrogen or argon gas or hydrogen and hydrogen and nitrogen mixture body are adopted in carrier gas.
One of technology implementation mode of the present invention, preparation GaN material comprises following a few step:
1, the cleaning of Sapphire Substrate and processing.
2, after Sapphire Substrate is put into the vitellarium of reaction cavity, slowly be warming up to growth temperature, can begin growing GaN.1000～1100 ℃ of growth temperatures.Gas flow difference: NH
3Flow is 1000sccm, NH
3Carrier gas flux is 2000sccm, and the HCl flow is 100sccm, and the HCl carrier gas flux is 200sccm, and total nitrogen is 8000sccm.Sample is 2 inches Sapphire Substrate, is 2 (row) X3 (OK)=6 distribution.Reaction cavity pressure 0.9 normal atmosphere.
3, grow into the suitable time after, slowly reduce to room temperature according to certain speed, take out sample.Those skilled in the art such as growth time here and rate of temperature fall can grasp according to existing GaN growth knowledge, and growth time is 10 minutes in the present embodiment, and growth velocity is 60 microns/hour, and the thickness difference is about the 0.5-1 micron between every capable sample.
4, graphite rest area is 120 * 180mm in the present embodiment, and growth flat-temperature zone length is 180mm.
On the basis of the foregoing description, change the diameter of reaction cavity and the area of stone mill rest, change the GaN substrate material number that is provided with, can realize raised growth GaN thin-film material.The homogeneity that reaction source had the multi-disc epitaxial growth substrate when system architecture of the present invention had guaranteed the multi-disc growth material; The special RF heating that adopts of the present invention can guarantee the major diameter reaction cavity heating all even fast; Integrate the growth that has realized a large amount of semiconductor film materials, and can guarantee the homogeneity of material growth thickness.
Claims (8)
1. the horizontal hydride gas phase epitaxial growth of a multi-disc multi-source system comprises reaction cavity and heating system, is provided with the vitellarium in the reaction cavity; Be provided with the graphite rest in the vitellarium, it is characterized in that reaction cavity is a horizontal type structure, reflection cavity one end is the reaction source inlet; One end is the tail gas outlet, and different reaction sources is respectively equipped with independently input channel, and said input channel stretches into reaction cavity before the graphite rest by the reaction source inlet; The graphite rest is square, places the multi-disc epitaxial growth substrate on the graphite rest, the surface size of graphite rest by what of epitaxial growth substrate quantity from 60 * 60mm to 350 * 350mm; Epitaxial growth substrate is evenly distributed on the graphite rest; The vitellarium temperature is 1000～1100 ℃, and reaction cavity adopts silica tube, and reaction chamber pressure remains on the 0.1-1.1 normal atmosphere.
2. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 1 system is characterized in that the bearing surface relative wind direction of graphite rest tilts 0～45 °.
3. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 1 and 2 system is characterized in that the longitudinal cenlerline rotation of graphite rest around the graphite rest, and speed range is 0～1000 rev/min.
4. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 1 and 2 system; It is characterized in that heating system adopts two warm areas, many warm areas or the control of single warm area temperature; Type of heating is resistance furnace or RF heating, and RF heating is: reaction cavity is provided with graphite sleeve outward, and graphite sleeve is placed in the ruhmkorff coil of electromagnetic induction heater; The graphite sleeve is outer to coat the non-inflammable insulation layer of heat conduction, and places inert gas environment.
5. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 3 system; It is characterized in that heating system adopts two warm areas, many warm areas or the control of single warm area temperature; Type of heating is resistance furnace or RF heating, and RF heating is: reaction cavity is provided with graphite sleeve outward, and graphite sleeve is placed in the ruhmkorff coil of electromagnetic induction heater; The graphite sleeve is outer to coat the non-inflammable insulation layer of heat conduction, and places inert gas environment.
6. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 1 and 2 system is characterized in that reaction source is sprayed on the surface of epitaxial growth substrate through quartzy spray header uniformly.
7. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 3 system is characterized in that reaction source is sprayed on the surface of epitaxial growth substrate through quartzy spray header uniformly.
8. the horizontal hydride gas phase epitaxial growth of a kind of multi-disc multi-source according to claim 1 system; It is characterized in that the disposable sheet number that is placed on the epitaxial growth substrate on the graphite rest comprises 6,9,15,25 2 inches Sapphire Substrate, perhaps 3,54 inches Sapphire Substrate.
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Cited By (5)
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| CN103276444A (en) * | 2013-05-15 | 2013-09-04 | 中国科学院半导体研究所 | Dual heating vapor phase epitaxial growth system |
| CN107740183A (en) * | 2017-10-12 | 2018-02-27 | 北京大学 | A kind of high temperature clean chamber system and method suitable for AlN crystal growths |
| CN111349970A (en) * | 2020-03-20 | 2020-06-30 | 山东科恒晶体材料科技有限公司 | Horizontal gallium nitride growth furnace |
| CN113355744A (en) * | 2020-03-05 | 2021-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Vapor phase epitaxial growth device and substrate bearing table thereof |
| CN114277360A (en) * | 2021-12-29 | 2022-04-05 | 季华实验室 | Chemical vapor deposition device |
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| CN102465337B (en) | 2014-07-16 |
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