CN105543969B - A kind of growing method of improvement AlN film crystal quality - Google Patents

A kind of growing method of improvement AlN film crystal quality Download PDF

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CN105543969B
CN105543969B CN201610044801.7A CN201610044801A CN105543969B CN 105543969 B CN105543969 B CN 105543969B CN 201610044801 A CN201610044801 A CN 201610044801A CN 105543969 B CN105543969 B CN 105543969B
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aln
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crystal quality
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trimethyl
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CN105543969A (en
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吴真龙
曾颀尧
郑建钦
田宇
李鹏飞
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NANTONG TONGFANG SEMICONDUCTOR CO Ltd
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NANTONG TONGFANG SEMICONDUCTOR CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403—AIII-nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0209—Pretreatment of the material to be coated by heating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A kind of growing method of improvement AlN film crystal quality, is related to the metal-organic chemical vapor deposition equipment MOCVD growing technologies field of III group-III nitride.The present invention uses two-step method growing AIN film, comprises the following steps：1）Cleaning baking substrate；2）Nitridation or pre- logical trimethyl aluminium；3）Low-temperature epitaxy AlN cushions；4）Heating annealing；5）High growth temperature AlN films；Above-mentioned steps 3）With step 5）In at least one step need to be passed through trimethyl gallium as surfactant.Compared with the existing technology, the AlN films prepared with the method for the present invention, have the characteristics that dislocation density is small, surface smoothness is good.

Description

A kind of growing method of improvement AlN film crystal quality
Technical field
The present invention relates to the metal-organic chemical vapor deposition equipment MOCVD growing technologies field of III group-III nitride, is particularly Improve the growing method of AlN film crystal quality.
Background technology
The deep ultraviolet DUV luminescent devices and sensitive detection parts of high Al contents AlGaN epitaxial films based on high quality can be wide It is general to apply in the field such as disinfection, water and Food processing, biochemistry detection, information storage, radar detection and secure communication, market Potentiality and application prospect are very huge.And the AlN substrates and template of high-crystal quality are to prepare above-mentioned high-performance deep-UV light-emitting With the key foundation of sensitive detection parts.
The AlN single crystalline substrates of high quality are expensive at present, it is high to prepare difficulty.Therefore, in the prior art, international research person Selection prepares the AlN films of high quality using metal-organic chemical vapor deposition equipment on a sapphire substrate, often selects two steps Method or pulse law technology.
Al-N bond energys are 2.88eV (Ga-N bond energys are 1.93eV), are highest in group III-nitride, so Al atom keys It is difficult desorption after conjunction, migrating required activation in growing surface can be very high.Therefore, during prepared by above-mentioned two-step method, the life of AlN extensions Long to be mainly shown as three-dimensional island pattern, rough surface, island, which merges, easily produces dislocation and crystal boundary, causes dislocation density very big, Seriously affect the performance of the ultraviolet electrical part of AlGaN bases.Further, since also there is higher heat mistake between AlN and Sapphire Substrate Match somebody with somebody and lattice mismatch, exacerbate the deterioration of crystal quality.
The content of the invention
For above-mentioned the deficiencies in the prior art, the object of the present invention is to provide one kind to improve AlN film crystal matter The growing method of amount.The AlN films prepared with this method, have the characteristics that dislocation density is small, surface smoothness is good.
In order to reach foregoing invention purpose, technical scheme is realized as follows：
A kind of growing method of improvement AlN film crystal quality, using two-step method growing AIN film, it is characterised in that bag Include following steps：
1）Cleaning baking substrate；
2）Nitridation or pre- logical trimethyl aluminium；
3）Low-temperature epitaxy AlN cushions；
4）Heating annealing；
5）High growth temperature AlN films；
Above-mentioned steps 3）With step 5）In at least one step need to be passed through trimethyl gallium as surfactant.
In above-mentioned growing method, the step 1）Substrate use sapphire, silicon or carborundum in one kind.
In above-mentioned growing method, the step 2）Nitridation or pre- logical trimethyl aluminium process temperature be 500-1100 DEG C, Chamber pressure is 20-200mbar, time 5-120s.
In above-mentioned growing method, the step 3）In AlN cushions epitaxial growth temperature be 500-1200 DEG C, reaction Chamber pressure is 20-200mbar, and buffer layer thickness 5-100nm, V/III ratio is 100-10000.
In above-mentioned growing method, the step 5）In AlN thin film epitaxial growths temperature be 1000-1400 DEG C, reaction Chamber pressure is 20-200mbar, and AlN film thicknesses are 1-5 μm, and V/III ratio is 10-1000.
In above-mentioned growing method, the trimethyl gallium that is passed through as surfactant, trimethyl gallium and trimethyl aluminium Flow molar ratio is 0.1-1, and the Ga components in actual AlN layers of incorporation are 0.01-0.1.
In above-mentioned growing method, the step 5）In in high growth temperature AlN films, surfactant trimethyl gallium The stage of being passed through is wherein certain part of flood or flood.
In above-mentioned growing method, the growing AIN method is metal-organic chemical vapor deposition equipment method.
The present invention compared with the existing technology has the following advantages that as a result of the above method：
The growing method of AlN epitaxial layers of the present invention uses two-step method, in low-temperature epitaxy AlN cushions or high growth temperature Trimethyl gallium is passed through during AlN films as surfactant, or in low-temperature epitaxy AlN cushions and high growth temperature AlN films When be all passed through trimethyl gallium as surfactant, can improve crystal quality and surface topography.Utilize surface migration ability phase The transfer ability of III race's metallic atom of growing surface is improved to preferable Ga atoms, promotes the growth of step stream, improves surfacing Degree so that relatively low growth temperature can be achieved with the two dimensional mode of AlN.In addition, the present invention AlN grow nucleation or into When core merges, the nucleation size of incorporation Ga atom increase AlN crystal grain, can effectively reduce what is brought when growth island merges Dislocation.
The present invention will be further described with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is the flow chart of growing method of the present invention；
Fig. 2 is to be passed through and be not passed through the XRD (102) for the AlN films that trimethyl gallium is grown in the embodiment of the present invention one The rocking curve in face compares figure；
Fig. 3 is to be passed through and be not passed through three axis ω -2 θ of the AlN films that trimethyl gallium is grown in the embodiment of the present invention one Scanning curve compares figure.
Embodiment
Referring to Fig. 1, the present invention improves the growing method of AlN film crystal quality, using two-step method growing AIN film, bag Include following steps：
1）Cleaning baking substrate；Substrate uses one kind in sapphire, silicon or carborundum.
2）Nitridation or pre- logical trimethyl aluminium；Nitridation or pre- logical trimethyl aluminium process temperature are 500-1100 DEG C, react chamber pressure Power is 20-200mbar, time 5-120s.
3）Using metal-organic chemical vapor deposition equipment method low-temperature epitaxy AlN cushions；AlN cushion epitaxial growth temperatures For 500-1200 DEG C, chamber pressure 20-200mbar, buffer layer thickness 5-100nm, V/III ratio is 100-10000.
4）Heating annealing；
5）Using metal-organic chemical vapor deposition equipment method high growth temperature AlN films；AlN thin film epitaxial growth temperature is 1000-1400 DEG C, chamber pressure 20-200mbar, AlN film thickness are 1-5 μm, and V/III ratio is 10-1000.
Above-mentioned steps 3）With step 5）In at least one step need to be passed through trimethyl gallium as surfactant.Trimethyl The flow molar ratio of gallium and trimethyl aluminium is 0.1-1, and the Ga components in actual AlN layers of incorporation are 0.01-0.1.In high growth temperature During AlN films, surfactant trimethyl gallium is passed through wherein certain part that the stage is flood or flood.
Embodiment one：
According to following steps growing AIN film, trimethyl gallium is passed through in high growth temperature AlN films：
1）Chamber pressure is set as 150mbar, reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen Baking 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) trimethyl aluminium, trimethyl gallium and ammonia are passed through while, trimethyl aluminium and TMGa flow rate be respectively 25 and The flow molar ratio of 300sccm, trimethyl gallium and trimethyl aluminium is that 1, V/III ratios are 100, keeps chamber pressure 50mbar, Reaction chamber temperature is 1150 DEG C, high temperature epitaxy growing AIN, and thickness is 0.5 μm.Trimethyl gallium is then shut off, continues epitaxial growth AlN, thickness are 1.5 μm.Growth gained AlN overall film thickness is 2 μm.
From figure 2 it can be seen that XRD (102) face halfwidth for being passed through the AlN films of trimethyl gallium growth is 650, hence it is evident that Less than XRD (102) face halfwidth 980 for the AlN films for not being passed through trimethyl gallium growth.Illustrate to be passed through trimethyl gallium growth AlN films can be obviously improved crystal quality.From figure 3, it can be seen that it is passed through three axis ω -2 of the AlN films of trimethyl gallium growth It is low at AlN (002) peak compared with three axis ω -2 θ scanning curves of AlN films of the θ scanning curves with not being passed through trimethyl gallium growth Substantially there are the relatively low small peak of a intensity, the corresponding AlN films for mixing a small amount of Ga in angle side, and Ga calculations are 0.05.
Embodiment two：
According to following steps growing AIN film, trimethyl gallium is passed through in high growth temperature AlN films：
1）Chamber pressure is set as 150mbar, reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen In, toast 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) trimethyl aluminium, trimethyl gallium and ammonia are passed through while, trimethyl aluminium and TMGa flow rate be respectively 2.5 and The flow molar ratio of 300sccm, trimethyl gallium and trimethyl aluminium is that 0.1, V/III ratios are 100, keeps chamber pressure 50mbar, reaction chamber temperature are 1150 DEG C, and high temperature epitaxy growing AIN, thickness is 0.3 μm.Trimethyl gallium is then shut off, is continued outer Epitaxial growth AlN, thickness are 1.7 μm.Growth gained AlN overall film thickness is 2 μm.
Embodiment three：
According to following steps growing AIN film, trimethyl gallium is passed through in high growth temperature AlN films：
1）Chamber pressure is set as 150mbar, reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen In, toast 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) trimethyl aluminium, trimethyl gallium and ammonia are passed through while, trimethyl aluminium and TMGa flow rate be respectively 12.5 and The flow molar ratio of 300sccm, trimethyl gallium and trimethyl aluminium is that 0.5, V/III ratios are 100, keeps chamber pressure 50mbar, reaction chamber temperature are 1150 DEG C, and high temperature epitaxy growing AIN, thickness is 0.7 μm.Trimethyl gallium is then shut off, is continued outer Epitaxial growth AlN, thickness are 1.3 μm.Growth gained AlN overall film thickness is 2 μm.
Example IV：
According to following steps growing AIN film, trimethyl gallium is passed through in high growth temperature AlN films：
1）Chamber pressure is set as 150mbar, reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen In, toast 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) chamber pressure 50mbar is kept, reaction chamber temperature is 1150 DEG C, and V/III ratios are 100, high temperature epitaxy growth AlN, thickness are 1 μm.Then trimethyl aluminium, trimethyl gallium and ammonia are passed through at the same time, and trimethyl aluminium is distinguished with TMGa flow rate For 12.5 and 300sccm, the flow molar ratio of trimethyl gallium and trimethyl aluminium is 0.5, continues epitaxial growth AlN, thickness is 1 μ m.Growth gained AlN overall film thickness is 2 μm.
Embodiment five：
According to following steps growing AIN film, trimethyl gallium is passed through in high growth temperature AlN films：
1）Chamber pressure is set as 150mbar, reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen In, toast 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) trimethyl aluminium, trimethyl gallium and ammonia are passed through while, trimethyl aluminium and TMGa flow rate be respectively 12.5 and The flow molar ratio of 300sccm, trimethyl gallium and trimethyl aluminium is that 0.5, V/III ratios are 100, keeps chamber pressure 50mbar, reaction chamber temperature are 1150 DEG C, and high temperature epitaxy growing AIN, thickness is 2 μm.
Embodiment six：
According to following steps growing AIN film, trimethyl gallium is passed through in low-temperature epitaxy AlN cushions：
1) chamber pressure is set as 150mbar, and reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen In, toast 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, It is passed through trimethyl aluminium, trimethyl gallium and ammonia at the same time, TMGa flow rate is respectively 10sccm, trimethyl gallium and trimethyl aluminium Flow molar ratio is that 0.1, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) while trimethyl aluminium and ammonia are passed through, V/III molar ratios are 200, keep chamber pressure 50mbar, reaction Room temperature is 1150 DEG C, high temperature epitaxy growing AIN, and thickness is 2 μm.
Embodiment seven：
According to following steps growing AIN film, three are all passed through in low-temperature epitaxy AlN cushions and high growth temperature AlN films Methyl gallium：
1) chamber pressure is set as 150mbar, and reaction chamber temperature is 1100 DEG C, by Sapphire Substrate in atmosphere of hydrogen In, toast 10 minutes.
2) 950 DEG C are cooled to, pre- logical trimethyl aluminium 10s.
3) chamber pressure is down to 100mbar, is warming up to 1000 DEG C of growing AIN cushions, growth thickness 20nm, It is passed through trimethyl aluminium, trimethyl gallium and ammonia at the same time, TMGa flow rate is respectively 10sccm, trimethyl gallium and trimethyl aluminium Flow molar ratio is that 0.1, V/III ratios are 1000.
4) chamber pressure is down to 50mbar, stops logical trimethyl aluminium, continue to be passed through ammonia, with 400 second time temperature Degree rises to 1150 DEG C, stablizes 60s.
5) trimethyl aluminium, trimethyl gallium and ammonia are passed through while, trimethyl aluminium and TMGa flow rate be respectively 25 and The flow molar ratio of 300sccm, trimethyl gallium and trimethyl aluminium is that 1, V/III ratios are 100, keeps chamber pressure 50mbar, Reaction chamber temperature is 1150 DEG C, high temperature epitaxy growing AIN, and thickness is 0.5 μm.Trimethyl gallium is then shut off, continues epitaxial growth AlN, thickness are 1.5 μm.Growth gained AlN overall film thickness is 2 μm.
The crystal quality of AlN epitaxial films is characterized using X-ray diffraction rocking curve halfwidth, utilizes atomic force microscopy Mirror characterizes the surface roughness of AlN epitaxial films.It turns out that the AlN extensions of growing method growth using the present invention are thin Film is compared with the sample that usual conditions are grown, and crystal quality significantly improves, and surface roughness is obviously reduced.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.Although with reference to the foregoing embodiments The present invention is described in detail, those of ordinary skill in the art still can be to the skill described in foregoing embodiments Art scheme is modified, or carries out equivalent substitution to which part technical characteristic；It is all belong to shown according to the technical program And the modification or replacement being clear to, the essence of appropriate technical solution is departed from various embodiments of the present invention technical solution, belong to In protection scope of the present invention.

Claims (7)

  1. A kind of 1. growing method of improvement AlN film crystal quality, using two-step method growing AIN film, it is characterised in that including Following steps：
    1）Cleaning baking substrate；
    2）Nitridation or pre- logical trimethyl aluminium；
    3）Low-temperature epitaxy AlN cushions；
    4）Heating annealing；
    5）High growth temperature AlN films；
    Above-mentioned steps 3）With step 5）In at least one step need to be passed through trimethyl gallium as surfactant, it is described to be passed through three For methyl gallium as surfactant, the flow molar ratio of trimethyl gallium and trimethyl aluminium is 0.1-1, in actual AlN layers of incorporation Ga components are 0.01-0.1.
  2. 2. improve the growing method of AlN film crystal quality according to claim 1, it is characterised in that the step 1）'s Substrate uses one kind in sapphire, silicon or carborundum.
  3. 3. the growing method of improvement AlN film crystal quality according to claim 1 or claim 2, it is characterised in that the step 2） Nitridation or pre- logical trimethyl aluminium process temperature be 500-1100 DEG C, chamber pressure 20-200mbar, time 5-120s.
  4. 4. improve the growing method of AlN film crystal quality according to claim 3, it is characterised in that the step 3）In AlN cushions epitaxial growth temperature be 500-1200 DEG C, chamber pressure 20-200mbar, buffer layer thickness 5- 100nm, V/III ratio is 100-10000.
  5. 5. improve the growing method of AlN film crystal quality according to claim 4, it is characterised in that the step 5）In AlN thin film epitaxial growths temperature be 1000-1400 DEG C, chamber pressure 20-200mbar, AlN film thickness be 1-5 μm, V/III ratio is 10-1000.
  6. 6. improve the growing method of AlN film crystal quality according to claim 5, it is characterised in that the step 5）In In high growth temperature AlN films, surfactant trimethyl gallium is passed through wherein certain part that the stage is flood or flood.
  7. 7. improve the growing method of AlN film crystal quality according to claim 6, it is characterised in that the growing AIN side Method is metal-organic chemical vapor deposition equipment method.
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CN112725896B (en) * 2019-10-28 2022-04-22 宁波安芯美半导体有限公司 Preparation method of aluminum nitride single crystal film, aluminum nitride single crystal film and light-emitting diode
CN111341889B (en) * 2020-03-07 2021-04-13 孙蕾蕾 Semiconductor lighting epitaxial structure forming method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008153382A (en) * 2006-12-15 2008-07-03 Hitachi Cable Ltd Method of manufacturing nitride semiconductor
CN101603172A (en) * 2008-06-10 2009-12-16 北京大学 The method of a kind of growing AIN or AlGaN film
CN101777488A (en) * 2010-01-26 2010-07-14 南京大学 Growth method for obtaining high aluminium component Al-Ga-N alloys by improving aluminium doping efficiency
WO2012120497A4 (en) * 2011-03-04 2012-11-01 Mosaic Crystals Ltd. Method for surfactant crystal growth of a metal-nonmetal compound
CN103695999A (en) * 2013-12-02 2014-04-02 中国电子科技集团公司第五十五研究所 Nitride single crystal membrane prepared by alternate source supply and method
CN104319234A (en) * 2014-10-14 2015-01-28 北京大学 Method for growing high-crystal quality AlN epitaxial layer
CN104392909A (en) * 2014-10-14 2015-03-04 北京大学 AlN epitaxial film growing method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008153382A (en) * 2006-12-15 2008-07-03 Hitachi Cable Ltd Method of manufacturing nitride semiconductor
CN101603172A (en) * 2008-06-10 2009-12-16 北京大学 The method of a kind of growing AIN or AlGaN film
CN101777488A (en) * 2010-01-26 2010-07-14 南京大学 Growth method for obtaining high aluminium component Al-Ga-N alloys by improving aluminium doping efficiency
WO2012120497A4 (en) * 2011-03-04 2012-11-01 Mosaic Crystals Ltd. Method for surfactant crystal growth of a metal-nonmetal compound
CN103695999A (en) * 2013-12-02 2014-04-02 中国电子科技集团公司第五十五研究所 Nitride single crystal membrane prepared by alternate source supply and method
CN104319234A (en) * 2014-10-14 2015-01-28 北京大学 Method for growing high-crystal quality AlN epitaxial layer
CN104392909A (en) * 2014-10-14 2015-03-04 北京大学 AlN epitaxial film growing method

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