CN103695999A - Nitride single crystal membrane prepared by alternate source supply and method - Google Patents
Nitride single crystal membrane prepared by alternate source supply and method Download PDFInfo
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Abstract
The invention relates to a high-quality nitride single crystal membrane prepared by alternate source supply. According to the structure of the membrane, an aluminum nitride (AlN) buffer layer is on a single crystal substrate, and the nitride single crystal membrane is on the AlN buffer layer. The preparation method comprises the following steps of a) putting the single crystal substrate into a reaction chamber for roasting at a high temperature; b) preparing an aluminum infiltrating layer on the single crystal substrate; c) preparing the AlN buffer layer on the infiltrating layer; d) preparing the nitride single crystal membrane on the AlN buffer layer; and e) cooling down to room temperature and taking out. The nitride single crystal membrane has the advantages that on the basis of preparing the aluminum nitride buffer layer with high quality crystal by alternate source supply, the quality of the crystal and the surface of the nitride single crystal membrane can be further improved by combining In protective atmosphere and the Al infiltrating layer, the stress of the membrane is lowered; and the nitride single crystal membrane has the characteristics of simple structure, controllable preparation method, good surface appearance and low cost.
Description
Technical field
The present invention relates to be a kind of In that utilizes in single crystalline substrate as protective atmosphere, with Al soakage layer and alternately pass into Al source, aluminum nitride buffer layer is prepared in N source, thereby improve nitride single crystal film and method prepared by the alternately supply source of nitride single crystal film quality.Belong to wide bandgap semiconductor epitaxial material technical field.
Background technology
For want of high-quality monocrystal material is as homo-substrate, and nitride film is prepared in the hetero epitaxy mode of large mismatch substantially.Conventionally introduce two-step approach and overcome lattice mismatch and the coefficient of thermal expansion mismatch between substrate and epitaxial film, can obtain the nitride epitaxial film of better quality.According to the difference of substrate kind, how 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, reduces the probability cracking, in addition, better because of its insulativity, in multiple electronics and microwave device, obtains more application.
Conventional epitaxy method can be prepared aluminum nitride buffer layer, but because the restriction on the low side of conventional epitaxial device growth temperature, its crystal mass can't be satisfactory.The method of growing aluminum nitride has continuous growth and replaces TongYuan's growth method.Growth method is in aluminium nitride process of growth, to keep unremitting the continuing in Al source and N source to pass into continuously, by adjusting the processing condition such as temperature, pressure, flow, prepares aluminium nitride; Alternately TongYuan's growth method is that Al source and N source alternately pass into pulse mode respectively, mainly to avoid pre-reaction, during not having N source to pass into, relatively increased the surface transport length of Al atom, can not improve under the condition of growth temperature, by adjusting the quality of the improvement of terms aluminium nitride such as the time that passes into, flow, interval time in Al source and N source.The obstacle of growth method is the growth temperature that need to significantly improve epitaxial device continuously, faces the transformation difficult problems such as power supply, well heater, pilot circuit, reaction chamber.Alternately the advantage of TongYuan's method is not need to improve growth temperature, just can improve the preparation of aluminium nitride.Although alternately TongYuan's method is better than the effect of continuous growth method to a certain extent, the just length surface of Al atom changing, does not have the quality that improves aluminium nitride from changing this basic reason of Al atomic surface travelling speed.
Summary of the invention
What the present invention proposed is a kind of nitride single crystal film and method that alternately prepared by supply source, and its object is intended to overcome the existing above-mentioned defect of prior art.Replacing supply source method increase Al atomic surface migration length, prepare on the basis of high quality aluminum nitride buffer layer, introduce on the one hand the protection of In atmosphere, effectively improve Al atom in the travelling speed of substrate surface, and after AlN synthesis finishes, continue to pass into certain hour, impel the improvement of surface quality; While replacing TongYuan on the other hand, Al source is first passed into substrate surface, this step has two effects, be to replace the first step that aluminium nitride is prepared by TongYuan, also can form soakage layer at substrate surface simultaneously, the surface energy that reduces substrate, passes into subsequently N source and Al soakage layer and generates aluminium nitride, has improved the crystal mass of aluminium nitride.In addition, after AlN synthesis finishes, In source also will continue to pass into for some time and closes, has guaranteed surperficial planeness and slickness.In the situation that not improving growth temperature, can further improve crystal mass and the surface topography of nitride single crystal film, reduce stress, avoid continuous growing method and replaced supply source legal system for the deficiency of AlN buffer layer.The advantages such as it is simple that the present invention has method, and technology difficulty is little, easy realization.
Technical solution of the present invention: a kind of utilization replaces the brilliant film of high quality nitride prepared by supply source, and its structure is to be aluminium nitride AlN buffer layer in single crystalline substrate; On aluminium nitride AlN buffer layer, it is nitride single crystal film.
Its preparation method, comprises following processing step:
A) single crystalline substrate is put into reaction chamber, high bake;
B) in single crystalline substrate, prepare Al soakage layer;
C) on soakage layer, prepare aluminium nitride AlN buffer layer;
D) on aluminium nitride AlN buffer layer, prepare nitride single crystal film;
E) be down to room temperature, take out.
Advantage of the present invention: 1) AlN buffer layer preparation process and preparation finish all to adopt In atmosphere protection in rear for some time, effectively increase the travelling speed of Al atom, improves the smooth of the crystal mass of aluminum nitride buffer layer and surface.2) adopt Al soakage layer to fall low surface energy, improve stress and the crystal mass of aluminum nitride buffer layer.3) the AlN buffer layer of alternating growth contributes to realize two-dimensional growth, and the stress of buffering nitride single crystal film, improves crystal and surface quality.4) simple in structure, preparation technology is controlled.5) cost is low, is widely used, can growing nitride series monocrystal film and multilayered structure.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of preparing nitride single crystal film.
Accompanying drawing 2 is the sequential schematic that pass in In source in aluminum nitride buffer layer preparation process, Al source and N source.
In figure 1 is single crystalline substrate, the 2nd, aluminium nitride (AlN) buffer layer, the 3rd, nitride single crystal film.
Embodiment
Contrast accompanying drawing 1,2, the brilliant film of high quality nitride, its structure is in single crystalline substrate 1, to be aluminium nitride AlN buffer layer 2; On aluminium nitride AlN buffer layer, it is nitride single crystal film 3.
Its preparation method, comprises following processing step:
A) single crystalline substrate is put into reaction chamber, high bake;
B) in single crystalline substrate, prepare Al soakage layer;
C) on soakage layer, prepare aluminium nitride AlN buffer layer;
D) on aluminium nitride AlN buffer layer, prepare nitride single crystal film;
E) be down to room temperature, take out.
Described single crystalline substrate is sapphire, silicon carbide (SiC), silicon (Si), gan, aluminium nitride, silicon-on-insulator (SOI) or lithium aluminate.
After finishing with preparation in described aluminium nitride AlN buffer layer preparation process, at the appointed time, pass into all the time In source.
The method preparation that described aluminium nitride AlN buffer layer adopts Al source and N source alternately to pass into, each is prepared unit and first passes into Al source and stop after 5 ~ 30 seconds, then passes into N source and stop after 5 ~ 30 seconds, until AlN buffer layer thickness meets the demands.
The preparation temperature T of described aluminium nitride AlN buffer layer
lbe 500 ℃≤T
l≤ 1300 ℃, thickness t is 10nm≤t≤1000nm.
Described nitride single crystal film comprises gan, aluminium nitride, indium nitride binary single-crystal film, or consisting of polynary monocrystal thin films, and multilayered structure.
Its structure is in single crystalline substrate 1, to be aluminium nitride (AlN) buffer layer 2; On aluminium nitride (AlN) buffer layer 2, it is nitride single crystal film 3.
embodiment 1
1) select single crystalline Si substrate, put into MOCVD reaction chamber;
2) be warming up to 1080 ℃, hydrogen atmosphere baking 10 minutes;
3) be cooled to 600 ℃, 150torr, trimethyl indium and trimethyl aluminium passed into after 30 seconds, stopped passing into trimethyl aluminium, formed Al soakage layer, and ammonia stops after passing into 30 seconds;
4) pass into trimethyl aluminium and stop after 30 seconds, ammonia stops after passing into 30 seconds, keeps alternately passing into trimethyl aluminium and ammonia, until aluminium nitride thickness reaches 100nm, closes trimethyl aluminium;
5) pass into ammonia, after 30 seconds, stop passing into trimethyl indium;
6) be warming up to 1060 ℃, 100Torr, passes into the trimethyl-gallium thick GaN monocrystal thin films of 2 μ m of growing;
7) close trimethyl-gallium, in protection of ammonia, drop to room temperature.
embodiment 2
1) select monocrystalline SOI substrate, put into MOCVD reaction chamber;
2) be warming up to 1060 ℃, hydrogen atmosphere baking 10 minutes;
3) be cooled to 1000 ℃, 100torr, trimethyl indium and trimethyl aluminium passed into after 20 seconds, stopped passing into trimethyl aluminium, formed Al soakage layer, and ammonia stops after passing into 20 seconds;
4) pass into trimethyl aluminium and stop after 20 seconds, ammonia stops after passing into 20 seconds, keeps alternately passing into trimethyl aluminium and ammonia, until aluminium nitride thickness reaches 500nm, closes trimethyl aluminium;
5) pass into ammonia, after 20 seconds, stop passing into trimethyl indium;
6) close trimethyl aluminium, be warming up to 1060 ℃, 100Torr, passes into trimethyl-gallium and the silane thick N-shaped GaN of the 3 μ m monocrystal thin films of growing;
7) close trimethyl-gallium and silane, in protection of ammonia, drop to room temperature.
Embodiment 3
1) select monocrystalline sapphire substrate, put into MOCVD reaction chamber;
2) be warming up to 1100 ℃, hydrogen atmosphere baking 10 minutes;
3) be cooled to 1080 ℃, 80torr, trimethyl indium and trimethyl aluminium passed into after 10 seconds, stopped passing into trimethyl aluminium, formed Al soakage layer, and ammonia stops after passing into 10 seconds;
4) pass into trimethyl aluminium and stop after 10 seconds, ammonia stops after passing into 10 seconds, keeps alternately passing into trimethyl aluminium and ammonia, until aluminium nitride thickness reaches 1000nm, closes trimethyl aluminium;
5) pass into ammonia, after 10 seconds, stop passing into trimethyl indium;
6) be warming up to 1060 ℃, 100Torr, passes into trimethyl-gallium and the trimethyl aluminium thick AlGaN monocrystal thin films of 1 μ m of growing;
7) close trimethyl-gallium and trimethyl aluminium, in protection of ammonia, drop to room temperature.
Embodiment 4
1) select monocrystal SiC substrate, put into MOCVD reaction chamber;
2) be warming up to 1100 ℃, hydrogen atmosphere baking 10 minutes;
3) be warming up to 1200 ℃, 50torr, trimethyl indium and trimethyl aluminium passed into after 10 seconds, stopped passing into trimethyl aluminium, formed Al soakage layer, and ammonia stops after passing into 20 seconds;
4) pass into trimethyl aluminium and stop after 10 seconds, ammonia stops after passing into 20 seconds, keeps alternately passing into trimethyl aluminium and ammonia, until aluminium nitride thickness reaches 200nm, closes trimethyl aluminium;
5) pass into ammonia, after 15 seconds, stop passing into trimethyl indium;
6) be cooled to 1060 ℃, 100Torr, passes into trimethyl-gallium and the trimethyl aluminium thick AlGaN monocrystal thin films of 1 μ m of growing;
7) close trimethyl-gallium and trimethyl aluminium, in protection of ammonia, drop to room temperature.
Embodiment 5
1) select monocrystal SiC substrate, put into MBE reaction chamber;
2) be warming up to 890 ℃, toast 10 minutes;
3) be warming up to 910 ℃, He Lv source, indium source passed into after 10 seconds, stopped logical aluminium, formed Al soakage layer, and nitrogenous source stops after passing into 15 seconds;
4) pass into aluminium and stop after 5 seconds, N source stops after passing into 5 seconds, keeps alternately passing into aluminium source and nitrogenous source, until aluminium nitride thickness reaches 10nm, closes aluminium source;
5) pass into nitrogenous source, after 10 seconds, stop passing into indium source;
6) be cooled to 800 ℃, pass into the Ga source thick GaN monocrystal thin films of 2 μ m of growing;
7) close Ga and N source, be down to room temperature.
According to not only can the grow nitride single crystal film of low-dislocation-density of aforesaid method, the various device architectures of continued growth thereon.
Preparation broad stopband monocrystal thin films structure involved in the present invention and method can be utilized common 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 technical characterstic, realization of the present invention includes but not limited to aforesaid method.
Claims (7)
1. utilize the brilliant film of high quality nitride that alternately prepared by supply source, it is characterized in that in single crystalline substrate it being aluminium nitride AlN buffer layer; On aluminium nitride AlN buffer layer, it is nitride single crystal film.
2. a kind of utilization as claimed in claim 1 replaces the method that supply source is prepared the brilliant film of high quality nitride, it is characterized in that the method, comprises following processing step:
A) single crystalline substrate is put into reaction chamber, high bake;
B) in single crystalline substrate, prepare Al soakage layer;
C) on soakage layer, prepare aluminium nitride AlN buffer layer;
D) on aluminium nitride AlN buffer layer, prepare nitride single crystal film;
E) be down to room temperature, take out.
3. a kind of utilization according to claim 1 replaces the brilliant film of high quality nitride prepared by supply source, it is characterized in that described single crystalline substrate is sapphire, silicon carbide SiC, silicon Si, gan, aluminium nitride, silicon-on-insulator SOI or lithium aluminate.
4. a kind of utilization according to claim 1 replaces the brilliant film of high quality nitride prepared by supply source, it is characterized in that in described aluminium nitride AlN buffer layer preparation process and preparation finish after at the appointed time, pass into all the time In source.
5. a kind of utilization according to claim 1 replaces the brilliant film of high quality nitride prepared by supply source, it is characterized in that the method preparation that described aluminium nitride AlN buffer layer adopts Al source and N source alternately to pass into, be that each is prepared unit and first passes into Al source and stop after 5 ~ 30 seconds, pass into again N source and stop after 5 ~ 30 seconds, until AlN buffer layer thickness meets the demands.
6. a kind of utilization according to claim 1 replaces the brilliant film of high quality nitride prepared by supply source, it is characterized in that the preparation temperature T of described aluminium nitride AlN buffer layer
lbe 500 ℃≤T
l≤ 1300 ℃, thickness t is 10nm≤t≤1000nm.
7. a kind of utilization according to claim 1 replaces the brilliant film of high quality nitride prepared by supply source, it is characterized in that described nitride single crystal film comprises gan, aluminium nitride, indium nitride binary single-crystal film, or consisting of polynary monocrystal thin films, and multilayered structure.
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| CN105543969A (en) * | 2016-01-25 | 2016-05-04 | 南通同方半导体有限公司 | Growth method for improving quality of AlN thin film crystal |
| CN110224020A (en) * | 2019-05-28 | 2019-09-10 | 苏州汉骅半导体有限公司 | The method for manufacturing high quality and high uniformity group III-nitride epitaxial structure |
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| CN111739791A (en) * | 2020-08-25 | 2020-10-02 | 中电化合物半导体有限公司 | Epitaxial structure of gallium nitride material and preparation method |
| CN111739791B (en) * | 2020-08-25 | 2020-12-18 | 中电化合物半导体有限公司 | Epitaxial structure of gallium nitride material and preparation method |
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| CN113284986A (en) * | 2021-03-29 | 2021-08-20 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer |
| CN113284986B (en) * | 2021-03-29 | 2023-03-24 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer |
| CN113481593A (en) * | 2021-05-14 | 2021-10-08 | 华灿光电（浙江）有限公司 | Preparation method of light-emitting diode epitaxial wafer with AlN |
| CN114277443A (en) * | 2021-12-28 | 2022-04-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitride single crystal film, and preparation method and application thereof |
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