CN103710747B - Nitride single crystal film and method are prepared in the conveying of a kind of interval, N source - Google Patents
Nitride single crystal film and method are prepared in the conveying of a kind of interval, N source Download PDFInfo
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- CN103710747B CN103710747B CN201310629266.8A CN201310629266A CN103710747B CN 103710747 B CN103710747 B CN 103710747B CN 201310629266 A CN201310629266 A CN 201310629266A CN 103710747 B CN103710747 B CN 103710747B
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- 239000013078 crystal Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 150000004767 nitrides Chemical class 0.000 title abstract description 27
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical group [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910017083 AlN Inorganic materials 0.000 claims abstract description 55
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 52
- 229910021529 ammonia Inorganic materials 0.000 claims description 26
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 12
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 claims description 11
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 10
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 229910002601 GaN Inorganic materials 0.000 claims 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 15
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000012876 topography Methods 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 30
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 125000004429 atom Chemical group 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 238000001451 molecular beam epitaxy Methods 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910002704 AlGaN Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 time Chemical compound 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000038 ultrahigh vacuum chemical vapour deposition Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention is the nitride single crystal film prepared of interval, a kind of N source supply source and method, and its structure is aluminium nitride AlN buffer layer in single crystalline substrate; Being nitride single crystal film on aluminium nitride AlN buffer layer, its preparation method, comprises following processing step: 1) single crystalline substrate puts into reaction chamber, high bake; 2) in single crystalline substrate, Al soakage layer is prepared; 3) on soakage layer, prepare aluminium nitride AlN buffer layer; 4) on aluminium nitride AlN buffer layer, nitride single crystal film is prepared; 5) it is down to room temperature, takes out. Advantage: present method, because preparing on the basis of aluminium nitride advantage in interval supply source method, adds In atmosphere and the advantage of Al soakage layer, so further improving crystal and the surface quality of aluminum nitride buffer layer and nitride single crystal film, reduces membrane stress; Have that structure is simple, technique is controlled; Surface topography is good; The features such as low cost.
Description
Technical field
The present invention relates to one and utilize In tensio-active agent and Al soakage layer, in single crystalline substrate, aluminum nitride buffer layer is prepared in conveying N source in interval, thus nitride single crystal film and method are prepared in interval, the N source conveying improving nitride single crystal film quality. Belong to wide bandgap semiconductor epitaxial material technical field.
Background technology
At present, nitride film is because lacking high-quality homo-substrate, hetero epitaxy mode is mostly adopted to prepare the nitride epitaxial film of better quality, but there is bigger lattice and difference of thermal expansion coefficients between foreign substrate and epitaxial film, belong to big mismatch system, highdensity dislocation and defect will be produced in epitaxial film. How difference according to substrate kind, can adopt gan or aluminium nitride as buffer layer. Aluminum nitride buffer layer is because lattice parameter is less, and stable in properties, produces stress to the nitride film of growth on it, can reduce in epitaxial film because mismatch stress produces the probability of crackle, in addition, because its insulativity is better, in electronics and microwave device, more application is obtained.
Although aluminum nitride buffer layer can be prepared by conventional epitaxy method, but because the physics-chem characteristic of self is limited, higher preparation temperature will be conducive to improving crystalline perfection. The ceiling temperature of present epitaxial device is on the low side, except no special changes a social system heater block, otherwise, it is very difficult to obtain high-quality aluminium nitride material. Through exploring, the method for growing aluminum nitride has growth and interval supply source growth method continuously. Continuous growth method be aluminium nitride process of growth keeps Al source and N source unremitting continue to lead to into, prepare aluminium nitride by processing condition such as adjustment temperature, pressure, flows; Interval supply source growth method is that Al source and N source or one wherein are in a pulsed fashion apart from one another by leading to into reaction chamber, object avoids Al source and N source to mix too early, reduce pre-reaction, relatively add the surface transport length of Al atom simultaneously, so just can when not improving growth temperature, lead to the quality into improvement of terms aluminium nitride such as time, flow, interval times by adjustment Al source and N source, reduce the upper temperature limit requirement of epitaxial device.The obstacle of continuous growth method needs the growth temperature significantly improving epitaxial device, faces the transformation difficult problems such as power supply, well heater, pilot circuit, reaction chamber. It is utilize existing installation that interval leads to the advantage for method, does not need to improve preparation temperature, just can be improved the preparation of aluminium nitride by the input mode and order changing source. Although interval supply source method is better than the effect of continuous growth method, but the length surface of the just Al atom changed, the quality of aluminium nitride is not improved from change Al this basic reason of atomic surface travelling speed.
Summary of the invention
The present invention proposes the conveying of a kind of interval, N source and prepare nitride single crystal film and method; its object is intended to the above-mentioned defect overcome existing for prior art; adopting In atmosphere protection and Al layer to infiltrate, in single crystalline substrate, the method for aluminum nitride buffer layer and nitride single crystal film is prepared in input N source in interval. Interval supply source method can increase Al atomic surface migration length, prepare high quality aluminum nitride buffer layer, on this basis, introduce In on the one hand as tensio-active agent, fundamentally improve the travelling speed of Al atom at substrate surface, and continue to lead to into certain time after AlN synthesis terminates, impel the improvement of surface quality; On the other hand Al source is led to into substrate surface prior to N source, it is possible to form soakage layer at substrate surface, reduce the surface energy of substrate, lead to into N source and Al soakage layer generation aluminium nitride subsequently, it is to increase the crystal mass of aluminium nitride. In addition, after AlN synthesis terminates, In source also to be continued to lead to and closes into for some time again, ensure that the planeness on surface and slickness. Present method is not when improving growth temperature, it is possible to improve crystal mass and the surface topography of nitride single crystal film further, reduces stress, avoids continuous growing method and interval supply source method prepares the deficiency of AlN buffer layer. Having method simple, technology difficulty is little, it is easy to the advantages such as realization.
The technical solution of the present invention: nitride single crystal film and method are prepared in the conveying of a kind of interval, N source, and its structure is aluminium nitride AlN buffer layer in single crystalline substrate; Aluminium nitride AlN buffer layer is nitride single crystal film.
Its preparation method, comprises following processing step:
1) single crystalline substrate puts into reaction chamber, high bake;
2) in single crystalline substrate, Al soakage layer is prepared;
3) on soakage layer, prepare aluminium nitride AlN buffer layer;
4) on aluminium nitride AlN buffer layer, nitride single crystal film is prepared;
5) it is down to room temperature, takes out.
The advantage of the present invention: 1) AlN buffer layer preparation process and preparation terminate all to adopt in rear for some time In atmosphere protection, effectively increases the travelling speed of Al atom, it is to increase the crystal mass of aluminum nitride buffer layer is smooth with surface. 2) adopt Al soakage layer to reduce surface energy, improve stress and the crystal mass of aluminum nitride buffer layer. 3) the AlN buffer layer of interval, N source input preparation contributes to realizing two-dimensional growth, the stress of buffering nitride single crystal film, it is to increase crystal and surface quality. 4) structure is simple, and preparation technology is controlled. 5) cost is low, is widely used, it is possible to growing nitride series monocrystal film and multilayered structure.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of nitride single crystal film.
Accompanying drawing 2 is the leading to into sequential schematic of In source in aluminum nitride buffer layer preparation process, Al source and N source.
In figure, 1 be single crystalline substrate, 2 be aluminium nitride (AlN) buffer layer, 3 is nitride single crystal film.
Embodiment
Comparison accompanying drawing 1, nitride single crystal film, its structure is aluminium nitride AlN buffer layer 2 in single crystalline substrate 1; Aluminium nitride AlN buffer layer 2 is nitride single crystal film 3.
A method for the brilliant film of nitride is prepared in the conveying of interval, N source, comprises following processing step:
1) single crystalline substrate puts into reaction chamber, high bake;
2) in single crystalline substrate, Al soakage layer is prepared;
3) on soakage layer, prepare aluminium nitride AlN buffer layer;
4) on aluminium nitride AlN buffer layer, nitride single crystal film is prepared;
5) it is down to room temperature, takes out.
Described single crystalline substrate is sapphire, silicon carbide (SiC), silicon (Si), gan, aluminium nitride, silicon-on-insulator (SOI) or lithium aluminate.
After described aluminium nitride AlN buffer layer preparation process terminates with preparation at the appointed time, lead to all the time into In source.
Described aluminium nitride AlN buffer layer adopts and first leads to continually and steadily into Al source, then stops the interval carrying method preparation of 5-30 second after leading to the N source 5-30 second, until AlN buffer layer thickness meets requirement.
The preparation temperature TL of described aluminium nitride AlN buffer layer is 500 DEG C��TL��1300 DEG C, and thickness t is 10nm��t��1000nm.
Described nitride single crystal film comprises gan, aluminium nitride, nitrogenize indium binary single-crystal film, or consisting of many units monocrystal thin films, and multilayered structure.
Embodiment 1
1) select single crystalline Si substrate, put into MOCVD reaction chamber;
2) being warming up to 1080 DEG C, hydrogen atmosphere toasts 10 minutes;
3) it is cooled to 600 DEG C, 150torr, leads to into trimethyl indium and trimethyl aluminium 30 seconds;
4) lead to ammonia and stop 30 seconds after 30 seconds, then lead to ammonia and stop 30 seconds after 30 seconds, keep leading to into ammonia by this regular intervals, until aluminium nitride thickness reaches 100nm, close trimethyl aluminium;
5) lead to into ammonia, stop after 30 seconds leading to into trimethyl indium;
6) it is warming up to 1060 DEG C, 100Torr, leads to and grow 2 �� m-thick GaN single crystal films into trimethyl-gallium;
7) close trimethyl-gallium, drop to room temperature in protection of ammonia.
Embodiment 2
1) select monocrystalline SOI substrate, put into MOCVD reaction chamber;
2) being warming up to 1060 DEG C, hydrogen atmosphere toasts 10 minutes;
3) it is cooled to 1000 DEG C, 100torr, leads to into trimethyl indium and trimethyl aluminium 20 seconds;
4) lead to ammonia and stop 20 seconds after 20 seconds, then lead to ammonia and stop 20 seconds after 20 seconds, keep leading to into ammonia by this regular intervals, until aluminium nitride thickness reaches 500nm, close trimethyl aluminium;
5) lead to into ammonia, stop after 20 seconds leading to into trimethyl indium;
6) close trimethyl aluminium, it is warming up to 1060 DEG C, 100Torr, leads to and grow 3 �� m-thick n type GaN single crystal films into trimethyl-gallium and silane;
7) close trimethyl-gallium and silane, drop to room temperature in protection of ammonia.
Embodiment 3
1) select monocrystalline sapphire substrate, put into MOCVD reaction chamber;
2) being warming up to 1100 DEG C, hydrogen atmosphere toasts 10 minutes;
3) it is cooled to 1080 DEG C, 80torr, leads to into trimethyl indium and trimethyl aluminium 30 seconds;
4) lead to ammonia and stop 15 seconds after 10 seconds, then lead to ammonia and stop 15 seconds after 10 seconds, keep leading to into ammonia by this regular intervals, until aluminium nitride thickness reaches 1000nm, close trimethyl aluminium;
5) lead to into ammonia, stop after 30 seconds leading to into trimethyl indium;
6) it is warming up to 1060 DEG C, 100Torr, leads to and grow 1 �� m-thick into trimethyl-gallium and trimethyl aluminium
7) AlGaN monocrystal thin films;
8) close trimethyl-gallium and trimethyl aluminium, drop to room temperature in protection of ammonia.
Embodiment 4
1) select monocrystal SiC substrate, put into MOCVD reaction chamber;
2) being warming up to 1100 DEG C, hydrogen atmosphere toasts 10 minutes;
3) it is warming up to 1200 DEG C, 50torr, leads to into trimethyl indium and trimethyl aluminium 10 seconds;
4) lead to ammonia and stop 10 seconds after 15 seconds, then lead to ammonia and stop 10 seconds after 15 seconds, keep leading to into ammonia by this regular intervals, until aluminium nitride thickness reaches 200nm, close trimethyl aluminium;
5) lead to into ammonia, stop after 15 seconds leading to into trimethyl indium;
6) it is cooled to 1060 DEG C, 100Torr, leads to and grow 1 �� m-thick AlGaN monocrystal thin films into trimethyl-gallium and trimethyl aluminium;
7) close trimethyl-gallium and trimethyl aluminium, drop to room temperature in protection of ammonia.
Embodiment 5
1) select monocrystal SiC substrate, put into MBE reaction chamber;
2) it is warming up to 890 DEG C, toasts 10 minutes;
3) it is warming up to 910 DEG C, leads to into indium source and aluminium source 10 seconds;
4) nitrogenous source stops 5 seconds after leading to 5 seconds, then leads to nitrogenous source and stops 5 seconds after 5 seconds, keeps leading to into ammonia by this regular intervals, until aluminium nitride thickness reaches 10nm, and closedown aluminium source;
5) lead to into nitrogenous source, stop after 10 seconds leading to into indium source;
6) it is cooled to 800 DEG C, leads to the GaN single crystal film growing 2 �� m-thick into Ga source;
7) close Ga and N source, it is down to room temperature.
The nitride single crystal film growing low-dislocation-density it is possible not only to, it is also possible to continue the various device architecture of growth thereon according to aforesaid method.
Preparation broad stopband monocrystal thin films structure involved in the present invention and method can utilize common such as MOCVD(metal organic-matter chemical gas deposition), CVD(chemical vapor deposition), MBE(molecular beam epitaxy), UHVCVD(high vacuum chemical gas deposition) etc. film preparing technology realize, according to technology feature, the realization of the present invention includes but not limited to aforesaid method.
Claims (1)
1. a method for gallium nitride single crystal film is prepared in the conveying of interval, N source, it is characterized in that comprising following processing step:
1) select single crystalline Si substrate, put into MOCVD reaction chamber;
2) being warming up to 1080 DEG C, hydrogen atmosphere toasts 10 minutes;
3) it is cooled to 600 DEG C, 150Torr, leads to trimethyl indium and trimethyl aluminium after 30 seconds; Start step 4), still continue to lead to into trimethyl indium and trimethyl aluminium in aluminium nitride process of growth;
4) lead to ammonia and stop 30 seconds after 30 seconds, then lead to ammonia and stop 30 seconds after 30 seconds, keep leading to into ammonia by this regular intervals, until aluminium nitride thickness reaches 100nm, close trimethyl aluminium;
5) lead to into ammonia, stop after 30 seconds leading to into trimethyl indium;
6) it is warming up to 1060 DEG C, 100Torr, leads to and grow 2 �� m-thick GaN single crystal films into trimethyl-gallium;
7) close trimethyl-gallium, drop to room temperature in protection of ammonia.
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| CN103695999B (en) * | 2013-12-02 | 2016-04-27 | 中国电子科技集团公司第五十五研究所 | Nitride single crystal film prepared by a kind of alternately supply source and method |
| CN113539786B (en) * | 2020-04-17 | 2024-05-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Silicon-based gallium nitride epitaxial structure and preparation method thereof |
| CN111739791B (en) * | 2020-08-25 | 2020-12-18 | 中电化合物半导体有限公司 | Epitaxial structure and preparation method of gallium nitride material |
| CN112242463B (en) * | 2020-09-29 | 2022-05-20 | 苏州紫灿科技有限公司 | Deep ultraviolet LED with pulse doped electron blocking layer and preparation method thereof |
| CN112735943B (en) * | 2020-12-31 | 2023-08-15 | 广东省科学院半导体研究所 | Preparation method for growing nitrogen-polar group III nitride semiconductor film on silicon substrate |
| CN113802178A (en) * | 2021-08-06 | 2021-12-17 | 中国电子科技集团公司第五十五研究所 | Epitaxial method for improving interface morphology between gallium nitride heteroepitaxy and substrate |
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