CN103474331B - The growing epitaxial method of AlN template on a sapphire substrate - Google Patents
The growing epitaxial method of AlN template on a sapphire substrate Download PDFInfo
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- CN103474331B CN103474331B CN201310461033.1A CN201310461033A CN103474331B CN 103474331 B CN103474331 B CN 103474331B CN 201310461033 A CN201310461033 A CN 201310461033A CN 103474331 B CN103474331 B CN 103474331B
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- aln
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- trimethyl aluminium
- sapphire
- aln template
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- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 35
- 239000010980 sapphire Substances 0.000 title claims abstract description 35
- 239000000758 substrate Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 20
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 4
- 230000004907 flux Effects 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 229910002704 AlGaN Inorganic materials 0.000 description 3
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Abstract
A method for growing epitaxial AlN template on a sapphire substrate, its scheme is: take trimethyl aluminium as MO source, NH
3for gaseous source, metalorganic chemical vapor depositing operation is adopted to grow AlN template at sapphire surface; When growing AIN template, trimethyl aluminium is prior to NH
3pass in reative cell, postpone 1-5 after passing into trimethyl aluminium and pass into NH again second
3, NH
3generate AlN after reacting with the Al atom being attached to sapphire surface, finally grow AlN template at sapphire surface; NH
3with V/III of trimethyl aluminium than being 51 ~ 256, reative cell internal gas pressure is 20 ~ 50mbar, and temperature is 1200 DEG C.Advantageous Effects of the present invention is: method simple practical, does not need resilient coating, can under relatively low underlayer temperature (1200 DEG C), and grow the AlN template that surface atom level is smooth, AlN template mean roughness is about 0.5nm.
Description
Technical field
The present invention relates to a kind of Organic Chemical Vapor deposition (MOCVD) technique, particularly relate to a kind of method of the AlN of growing epitaxial on a sapphire substrate template.
Background technology
At present, be both at home and abroad that the nitride epitaxial growth technology of substrate is very ripe with sapphire/GaN, but for deep UV (ultraviolet light) electronic device, because GaN material will cause the serious reduction of device light emitting efficiency to the strong absorption effect of ultraviolet light, nearly all incident light all can be absorbed by GaN layer and cannot be with source region generation photoelectric current, and the nitride template being therefore substrate with sapphire/GaN is not suitable for for making deep UV (ultraviolet light) electronic device; In order to solve foregoing problems, a kind of comparatively feasible technology path is: discard GaN template, is directly having deep UV (ultraviolet light) well through the AlGaN epitaxial loayer of the Grown on Sapphire Substrates high Al contents of characteristic.
The AlGaN epitaxial loayer of growth high Al contents, optimal substrate should be the ultraviolet light that AlN, AlN crystal is greater than 200nm to wavelength is all transparent, and AlN and AlGaN can form good Lattice Matching, and AlN also has good thermal conductance (thermal conductivity 3Wcm
-1k
-1), be conducive to the high-power performance improving device. in addition, owing to there is the maximum velocity of sound (6200m/s), higher piezoelectric coupling coefficient in all known SAW filter materials, AlN or a kind of desirable radio frequency SAW filter materials; But the technology of preparing of AlN single crystalline substrate is also immature, expensive both at home and abroad at present, and supply of material difficulty (especially large-sized substrate).
2006, the people such as SoukhoveevV report and adopt HVPE(hydride gas-phase epitaxy) method successfully grows high-quality AlN template on a sapphire substrate, but the AlN template obtained by HVPE method cannot make follow-up device epitaxial structure in growth in situ mode, therefore technical process relative complex, from the viewpoint of reducing process complexity, be necessary the technology of exploration MOCVD method direct growth AlN template on a sapphire substrate.
Summary of the invention
For the problem in background technology, the present invention proposes a kind of method of the AlN of growing epitaxial on a sapphire substrate template, its innovation is: take trimethyl aluminium as MO source, NH
3for gaseous source, metalorganic chemical vapor depositing operation is adopted to grow AlN template at sapphire surface; When growing AIN template, trimethyl aluminium is prior to NH
3pass in reative cell, postpone 1-5 after passing into trimethyl aluminium and pass into NH again second
3, NH
3generate AlN after reacting with the Al atom being attached to sapphire surface, finally grow AlN template at sapphire surface; NH
3with V/III of trimethyl aluminium than being 51 ~ 256, reative cell internal gas pressure is 20 ~ 50mbar, and temperature is 1200 DEG C.
Principle of the present invention is: the present invention passes into NH after adopting and first passing into trimethyl aluminium
3mode carry out growing AIN template, pass into trimethyl aluminium in advance, can make sapphire surface to adhere in advance last layer Al atom, avoid NH
3directly contact with sapphire surface and cause sapphire surface by nitrogenize, effectively to suppress the AlN film with mixing polar crystal domain to produce, improving the homogeneity of the AlN speed of growth.The present invention adopts low V/III than carrying out growing AIN template, growth technique of the prior art generally adopts 700 ~ 800 high V/III than carrying out, high V/III reduces in substrate surface animal migration than causing Al atom, be unfavorable for the foundation of two dimensional mode, be also just unfavorable for the formation of smooth epitaxial surface.The reative cell air pressure of present invention process is lower, and low reaction room air pressure effectively can reduce NH
3with trimethyl aluminium reactivity in the gas phase, thus reduce because of NH
3react in the gas phase with trimethyl aluminium and generate dust granules and be deposited on substrate, meanwhile, under the acting in conjunction of low reaction room air pressure and low V/III ratio, the animal migration of Al atom on substrate can be improved further.
Preferably, trimethyl aluminium flow is 40 ~ 80sccm, NH3 flow is 80 ~ 200sccm.
Preferably, before growing AIN template, be 1200 ~ 1250 DEG C in temperature, under pressure is 90 ~ 110mbar, carrier gas flux is the condition of 5000 ~ 7000sccm, removal of impurities carried out to sapphire surface.
Preferably, described AlN template thickness is 1 μm.AlN template thickness regulates by controlling the reaction time, if AlN template thickness is comparatively large, easily occurs crackle.
Advantageous Effects of the present invention is: method simple practical, does not need resilient coating, can under relatively low underlayer temperature (1200 DEG C), and grow the AlN template that surface atom level is smooth, AlN template mean roughness is about 0.5nm.
Embodiment
A method for growing epitaxial AlN template on a sapphire substrate, its innovation is: take trimethyl aluminium as MO source, NH
3for gaseous source, metalorganic chemical vapor depositing operation is adopted to grow AlN template at sapphire surface; When growing AIN template, trimethyl aluminium is prior to NH
3pass in reative cell, postpone 1-5 after passing into trimethyl aluminium and pass into NH again second
3, NH
3generate AlN after reacting with the Al atom being attached to sapphire surface, finally grow AlN template at sapphire surface; NH
3with V/III of trimethyl aluminium than being 51 ~ 256, reative cell internal gas pressure is 20 ~ 50mbar, and temperature is 1200 DEG C.
Further, trimethyl aluminium flow is 40 ~ 80sccm, NH3 flow is 80 ~ 200sccm.
Further, before growing AIN template, be 1200 ~ 1250 DEG C in temperature, under pressure is 90 ~ 110mbar, carrier gas flux is the condition of 5000 ~ 7000sccm, removal of impurities carried out to sapphire surface.
Further, described AlN template thickness is 1 μm.
Embodiment:
Sapphire Substrate is loaded in the reative cell of MOCVD device, in the environment of 1200 DEG C of underlayer temperatures, 100mbar Hydrogen Vapor Pressure, 6000sccm carrier gas flux, toasts 10 minutes, eliminate surface impurity; Reative cell internal gas pressure is adjusted to 40mbar, underlayer temperature is adjusted to 1200 DEG C, in reative cell, pass into trimethyl aluminium, trimethyl aluminium flow is 60sccm, postpones after 3 seconds, in reative cell, passes into NH
3, by controlling the reaction time, sapphire surface is grown AlN template that thickness is 1 μm.
Claims (4)
1. a growing epitaxial method for AlN template on a sapphire substrate, is characterized in that: take trimethyl aluminium as MO source, NH
3for gaseous source, metalorganic chemical vapor depositing operation is adopted to grow AlN template at sapphire surface; When growing AIN template, trimethyl aluminium is prior to NH
3pass in reative cell, postpone 1-5 after passing into trimethyl aluminium and pass into NH again second
3, NH
3generate AlN after reacting with the Al atom being attached to sapphire surface, finally grow AlN template at sapphire surface; NH
3with V/III of trimethyl aluminium than being 51 ~ 256, reative cell internal gas pressure is 20 ~ 50mbar, and temperature is 1200 DEG C.
2. the method for the AlN of growing epitaxial on a sapphire substrate template according to claim 1, is characterized in that: trimethyl aluminium flow is 40 ~ 80sccm, NH3 flow is 80 ~ 200sccm.
3. the method for the AlN of growing epitaxial on a sapphire substrate template according to claim 1, it is characterized in that: before growing AIN template, be 1200 ~ 1250 DEG C in temperature, under pressure is 90 ~ 110mbar, carrier gas flux is the condition of 5000 ~ 7000sccm, removal of impurities carried out to sapphire surface.
4. the method for the AlN of growing epitaxial on a sapphire substrate template according to claim 1, is characterized in that: described AlN template thickness is 1 μm.
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| CN108085745A (en) * | 2017-12-28 | 2018-05-29 | 北京华进创威电子有限公司 | A kind of aluminum nitride crystal growth is prepared with homo-substrate and expanding growing method |
| CN110129765B (en) * | 2019-05-23 | 2021-04-02 | 广东省半导体产业技术研究院 | Nitride semiconductor material and preparation method thereof |
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|---|---|---|---|---|
| US6984841B2 (en) * | 2001-02-15 | 2006-01-10 | Sharp Kabushiki Kaisha | Nitride semiconductor light emitting element and production thereof |
| TW200733383A (en) * | 2006-02-23 | 2007-09-01 | Arima Optoelectronics Corp | Method of converting N face into Ga face for HEMT nitride buffer layer structure |
| CN101302648A (en) * | 2008-01-28 | 2008-11-12 | 中国电子科技集团公司第五十五研究所 | Gallium nitride thin film epitaxial growth structure and method |
| CN102394240A (en) * | 2011-11-18 | 2012-03-28 | 贵州大学 | TFT (thin film transistor)-LED (light-emitting diode) color array display base plate and manufacturing method thereof |
| CN102650074A (en) * | 2012-04-09 | 2012-08-29 | 中国电子科技集团公司第五十五研究所 | Structure and method for preparing large-sized wide-bandgap monocrystal film |
| CN102651310A (en) * | 2012-04-09 | 2012-08-29 | 中国电子科技集团公司第五十五研究所 | Wide bandgap monocrystal film prepared from multiple buffer layers and method |
| CN103117209A (en) * | 2013-02-01 | 2013-05-22 | 中山大学 | Gradient AlGaN layer preparation method and device prepared by same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6881981B2 (en) * | 2001-01-04 | 2005-04-19 | Sharp Kabushiki Kaisha | Nitride semiconductor light emitting device chip |
| JP4201725B2 (en) * | 2004-02-20 | 2008-12-24 | シャープ株式会社 | Manufacturing method of nitride semiconductor light emitting device |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6984841B2 (en) * | 2001-02-15 | 2006-01-10 | Sharp Kabushiki Kaisha | Nitride semiconductor light emitting element and production thereof |
| TW200733383A (en) * | 2006-02-23 | 2007-09-01 | Arima Optoelectronics Corp | Method of converting N face into Ga face for HEMT nitride buffer layer structure |
| CN101302648A (en) * | 2008-01-28 | 2008-11-12 | 中国电子科技集团公司第五十五研究所 | Gallium nitride thin film epitaxial growth structure and method |
| CN102394240A (en) * | 2011-11-18 | 2012-03-28 | 贵州大学 | TFT (thin film transistor)-LED (light-emitting diode) color array display base plate and manufacturing method thereof |
| CN102650074A (en) * | 2012-04-09 | 2012-08-29 | 中国电子科技集团公司第五十五研究所 | Structure and method for preparing large-sized wide-bandgap monocrystal film |
| CN102651310A (en) * | 2012-04-09 | 2012-08-29 | 中国电子科技集团公司第五十五研究所 | Wide bandgap monocrystal film prepared from multiple buffer layers and method |
| CN103117209A (en) * | 2013-02-01 | 2013-05-22 | 中山大学 | Gradient AlGaN layer preparation method and device prepared by same |
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