CN108447897A - A kind of self-supporting diamond substrate heterojunction structure and preparation method - Google Patents
A kind of self-supporting diamond substrate heterojunction structure and preparation method Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 80
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 38
- 239000010432 diamond Substances 0.000 title claims abstract description 38
- 239000000758 substrate Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 64
- 239000010410 layer Substances 0.000 claims abstract description 30
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000011241 protective layer Substances 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 84
- 239000007789 gas Substances 0.000 claims description 70
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 229910052786 argon Inorganic materials 0.000 claims description 42
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 41
- 239000001301 oxygen Substances 0.000 claims description 41
- 229910052760 oxygen Inorganic materials 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 238000005546 reactive sputtering Methods 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 21
- 239000011777 magnesium Substances 0.000 claims description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 16
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 claims description 15
- 239000004411 aluminium Substances 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 10
- 230000004224 protection Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 238000004062 sedimentation Methods 0.000 claims description 7
- 238000004544 sputter deposition Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 230000002441 reversible effect Effects 0.000 abstract description 4
- 230000007704 transition Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910002601 GaN Inorganic materials 0.000 description 32
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 15
- 239000010409 thin film Substances 0.000 description 13
- 239000010408 film Substances 0.000 description 12
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 235000019589 hardness Nutrition 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/26—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, elements provided for in two or more of the groups H01L29/16, H01L29/18, H01L29/20, H01L29/22, H01L29/24, e.g. alloys
- H01L29/267—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, elements provided for in two or more of the groups H01L29/16, H01L29/18, H01L29/20, H01L29/22, H01L29/24, e.g. alloys in different semiconductor regions, e.g. heterojunctions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02376—Carbon, e.g. diamond-like carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02483—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
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Abstract
The invention belongs to a kind of reversible semiconductors to the manufacturing technology field of metal (SMT) first order transition coating, more particularly to a kind of self-supporting diamond substrate heterojunction structure and preparation method are sequentially prepared AZO transparent conductive film, p GaN materials layer, VO in self-supporting diamond substrate2Material layer, AZO transparent conductive film and the anticorrosive protective layers of TiN.A kind of VO with industrialization potential of the present invention2/ p GaN heterojunction structure bonded diamond materials and its technology of preparing.Preparation process is simple, it can be achieved that large-scale production.
Description
Technical field
The invention belongs to a kind of reversible semiconductors to the manufacturing technology field of metal (SMT) first order transition coating, especially relate to
And a kind of self-supporting diamond substrate heterojunction structure and preparation method.
Background technology
Vanadium dioxide (VO2) the reversible semiconductor of temperature driving occurs under the critical-temperature (Tc) of 341K to metal
(SMT) first order transition, and along with the change of crystal symmetry.At a temperature of less than Tc, VO2In monocline crystalline phase (P21/
C) semiconductor form, the wherein energy gap of V atom pairs are 0.6eV.At a temperature of higher than Tc, VO2In tetragonal crystal system
(P42/mnm) metallic state, wherein the overlapping between fermi level and V3d bands eliminates above-mentioned band gap.This crystal symmetry
The suddenly change that transition with electron band structure is usually transmitted along with its resistivity and near-infrared.Therefore, VO2For a long time by
The critical material being considered in intellectual material relies on these unique performances, VO2Film has been widely studied.It is well known that lining
The electrical and optical properties of film of the selection at bottom to being grown have important influence.Due to its broad-band gap (3.39eV) and some
Other excellent performances, gallium nitride (GaN) may be the important semi-conducting material of a new generation from after silicon.Particularly, since it has
There is the advantages of higher reliability, longer service life and lower power consumption, currently based on the photoelectron and microelectronics device of GaN
Part is instead of some routinely applications of Si and GaAs materials.By VO2It will likely be solid-state to be used to prepare heterostructure device
Novel device structure in electronics and photoelectronics opens up new chance.Also to the emerging device based on photon chamber and having
Source material shows huge potentiality.
Invention content
In order to solve the deficiency in high power device technology of preparing, the invention reside in provide a kind of self-supporting diamond substrate
Heterojunction structure and preparation method.
The invention is realized in this way
A kind of self-supporting diamond substrate heterojunction structure is transparent including the anticorrosive protective layers of TiN, AZO successively from top to bottom
Conductive film, VO2Material layer, p-GaN material layers, AZO transparent conductive film layer, self-supporting diamond substrate.
A kind of preparation method of self-supporting diamond substrate heterojunction structure is sequentially prepared AZO in self-supporting diamond substrate
Transparent conductive film, p-GaN material layers, VO2Material layer, AZO transparent conductive film and the anticorrosive protective layers of TiN.
Further, the preparation of AZO transparent conductive film includes：Self-supporting diamond substrate is first used into ionized water ultrasonic wave
After ten minutes, magnetron sputtering reative cell is sent into drying, 1.0 × 10 for cleaning-3Under conditions of Pa vacuum, in its self-supporting diamond
Substrate deposition prepares AZO transparent conductive electrodes.Its technological parameter condition is：Argon gas and oxygen as mixed gas reaction source,
Argon gas and oxygen flow ratio 4:1-10:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, preparation temperature 200
DEG C~400 DEG C, preparation time is 60~100 minutes.
Further, preparing p-GaN material layers in AZO transparent conductive film includes：Using plasma enhances organic matter
Chemical gas-phase deposition system prepares p-type GaN material, and vacuum is evacuated to 1.0 × 10-4Under conditions of Pa vacuum, trimethyl gallium and nitrogen
Gas adulterates two luxuriant magnesium to realize that GaN material p-type is adulterated, wherein TMGa flows are 1.0~1.5sccm, Cp as reaction source2Mg
Flow is 0.5~1.0sccm, and nitrogen flow is 100~150sccm, and depositing temperature is 400 DEG C~600 DEG C, and sedimentation time is
180min。
Further, VO is prepared in p-GaN material layers2Material layer includes：It is deposited in magnetic control sputtering system and prepares VO2,
1.0×10-3Under conditions of Pa vacuum, VO is prepared2Material layer, technological parameter condition are：Argon gas and oxygen are as mixed gas
Reaction source, argon gas and oxygen flow ratio 3:1~8:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, preparation temperature
It it is 100 DEG C~300 DEG C, preparation time is 200~300 minutes.
Further, in VO2It is prepared by magnetron sputtering in material layer, vacuum is extracted into the item of 1.0 × 10-3Pa vacuum
Under part, AZO transparent conductive electrodes are prepared, technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas
With oxygen flow ratio 5:1~7:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, preparation temperature is 100 DEG C~
300 DEG C, preparation time is 30~60 minutes.
Further, TiN anti-corrosion protection coatings are prepared by magnetron sputtering apparatus in AZO transparent conductive electrodes,
Technological parameter condition is：Nitrogen is as gas reaction source, and nitrogen flow is 30~80sccm, reactive sputtering titanium nitride target
Purity is 99.99%, and underlayer temperature is 100 DEG C~400 DEG C, and preparation time is 20~50 minutes.
It is finally completed a kind of TiN/AZO/VO2It is prepared by the initial stage of/p-GaN/AZO/ self-supporting diamond substrate heterojunction structures.
The present invention provides a kind of VO with industrialization potential2/ p-GaN heterojunction structure bonded diamond materials and its system
Standby technology.The present invention relates to using self-supporting diamond material, as substrate base, diamond is that nature radiating rate is most fast
Material, VO2/ p-GaN heterojunction structure bonded diamond materials can prepare high-power device as substrate.Then adopt
It uses AZO as the conductive electrode of device, on the one hand can be used as and slow down layer, on the one hand the lattice mismatch between reduction can be made
It is used for transparent conductive electrode.Then its TiN material is finally deposited, TiN material hardnesses are big, corrosion-resistant, efficiently solve device
Etching problem, further improve the service life of device.The preparation process is simple, it can be achieved that large-scale production.
VO provided by the invention2The heterojunction structure of/p-GaN combinations is the novel device in solidstate electronics and photoelectronics
Part structure opens up new chance.In addition, oxide and III-V semiconductors with switching characteristic it is integrated also to it is emerging based on
The device and active material of photon chamber show huge potentiality.Solving heat dissipation problem prepares high-power VO simultaneously2/p-
GaN heterostructure devices.
Using VO2/p-GaN structures, the reversible semiconductor that the driving of N-type VO2 temperature had both been utilized turns to metal (SMT) level-one
The characteristic of change, and p-GaN structural reliabilities are utilized, high-power, long-life, low power consumption and heat safe feature,
The device that the two combines has wide application in high-power optoelectronic switch, high-power light storage device, lasing safety etc.,
Solve that device lifetime is short, the low problem of power.
Description of the drawings
Fig. 1 is the schematic diagram of structure of the invention；
Fig. 2 is VO of the present invention2The surface FE-SEM patterns of/p-GaN heterojunction structures；
Fig. 3 is that the combination of 1 sample of present example can be in the XPS measuring spectrum within the scope of 0-1100eV；
Fig. 4 is that the combination of 3 sample of present example can be in the XPS measuring spectrum within the scope of 0-1100eV；
Fig. 5 is the high-resolution spectroscopy and sample VO2/p-GaN of the amplification of the combination energy within the scope of 510-535eV of the present invention
The fitting result of heterojunction structure.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
XPS uses Thermo Scientific ESCALAB 250XiX X-ray photoelectron spectroscopy X instrument in the present invention,
The equipment uses Aka 1486.8eV radiographic sources, can reach the vacuum chamber of 3x10-8Pa.
The model of laboratory sample test of the present invention SEM used is JSM-6360LV, is produced in Japan.Device parameter is
The accelerating potential of 0.5-30kV, the amplification factor that ten thousand times of 8-30, the secondary electron resolution ratio under conditions of high low vacuum are respectively
3nm and 4nm.
Referring to Fig. 1, the present invention provides a kind of self-supporting diamond substrate heterojunction structure, anti-including TiN successively from top to bottom
Corrosion protection layer 6, AZO transparent conductive film 5, VO2Material layer 4, AZO transparent conductive film layer 2, is propped up at p-GaN material layers 3 certainly
Support diamond substrate 1.
The present invention provides a kind of preparation method of self-supporting diamond substrate heterojunction structure, self-supporting diamond substrate according to
Secondary preparation AZO transparent conductive film, p-GaN material layers, VO2Material layer, AZO transparent conductive film and the anticorrosive protective layers of TiN.
Embodiment 1
1, self-supporting diamond substrate is first used into ionized water ultrasonic cleaning after ten minutes, magnetron sputtering reaction is sent into drying
Room, 1.0 × 10-3Under conditions of Pa vacuum, AZO transparent conductive electrodes are prepared in its self-supporting diamond substrate deposition.Its work
Skill Parameter Conditions are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reactive sputtering oxidation
The purity of zinc doping aluminium target is 99.9%, and preparation temperature is 200 DEG C, and preparation time is 60 minutes.
2 then using plasma enhancing organic chemical vapor deposition system prepare p-type GaN material, vacuum is evacuated to
1.0×10-4Under conditions of Pa vacuum, trimethyl gallium (TMGa) and nitrogen (N2) it is used as reaction source, the luxuriant magnesium (Cp of doping two2Mg) come
Realize the doping of GaN material p-type.Wherein TMGa flows are 1.0sccm, Cp2Mg flows are 0.5sccm, and nitrogen flow is
100sccm.Depositing temperature is 400 DEG C, sedimentation time 180min.
3, it is deposited using magnetic control sputtering system and prepares VO2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, prepare
VO2Thin-film material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
8:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 100 DEG C, and preparation time is 200 minutes.
4 then magnetron sputtering preparation in, under conditions of vacuum is extracted into 1.0 × 10-3Pa vacuum, continue prepare AZO
Transparent conductive electrode.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
5:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 100 DEG C, and preparation time is 30 minutes.
5, continue to prepare TiN anti-corrosion protection coatings in magnetron sputtering preparation, technological parameter condition is：Nitrogen conduct
The purity in gas reaction source, nitrogen flow 30sccm, reactive sputtering titanium nitride target is 99.99%, underlayer temperature 100
DEG C, preparation time is 20 minutes.
Using scanning electron microscope microscope (SEM) analytical equipment to VO after experiment2/ p-GaN heterojunction structures
Surface topography is tested analysis.The results are shown in Figure 2 for it, and the thin-film material pattern that can be prepared by Fig. 2 is very smooth, crystal grain
Distribution is very uniform, meets the requirement of device.Use XPS to VO later2/ p-GaN heterojunction structures are tested analysis, such as Fig. 3
It is shown, all elements that can well in recognition combination object in XPS measuring spectrum.We detect that there are p- in all samples
GaN and VO2Signal, show to have prepared two kinds of thin-film materials.
Embodiment 2
1, self-supporting diamond substrate is first used into ionized water ultrasonic cleaning after ten minutes, magnetron sputtering reaction is sent into drying
Room, 1.0 × 10-3Under conditions of Pa vacuum, AZO transparent conductive electrodes are prepared in its self-supporting diamond substrate deposition.Its work
Skill Parameter Conditions are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 4:1, reactive sputtering oxidation
The purity of zinc doping aluminium target is 99.9%, and preparation temperature is 250 DEG C, and preparation time is 60 minutes.
2 then using plasma enhancing organic chemical vapor deposition system prepare p-type GaN material, vacuum is evacuated to
1.0×10-4Under conditions of Pa vacuum, trimethyl gallium (TMGa) and nitrogen (N2) it is used as reaction source, the luxuriant magnesium (Cp of doping two2Mg) come
Realize the doping of GaN material p-type.Wherein TMGa flows are 1.2sccm, Cp2Mg flows are 0.7sccm, and nitrogen flow is
150sccm.Depositing temperature is 500 DEG C, sedimentation time 180min.
3, it is deposited using magnetic control sputtering system and prepares VO2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, prepare
VO2Thin-film material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
3:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 200 DEG C, and preparation time is 200 minutes.
4 then magnetron sputtering preparation in, vacuum is extracted into 1.0 × 10-3Under conditions of Pa vacuum, it is saturating to continue preparation AZO
Bright conductive electrode.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 7:
1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 60 minutes.
5, continue to prepare TiN anti-corrosion protection coatings in magnetron sputtering preparation, technological parameter condition is：Nitrogen conduct
The purity in gas reaction source, nitrogen flow 60sccm, reactive sputtering titanium nitride target is 99.99%, underlayer temperature 300
DEG C, preparation time is 20 minutes.
Embodiment 3
1, self-supporting diamond substrate is first used into ionized water ultrasonic cleaning after ten minutes, magnetron sputtering reaction is sent into drying
Room, 1.0 × 10-3Under conditions of Pa vacuum, AZO transparent conductive electrodes are prepared in its self-supporting diamond substrate deposition.Its work
Skill Parameter Conditions are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 10:1, reactive sputtering oxidation
The purity of zinc doping aluminium target is 99.9%, and preparation temperature is 400 DEG C, and preparation time is 100 minutes.
2 then using plasma enhancing organic chemical vapor deposition system prepare p-type GaN material, vacuum is evacuated to
1.0×10-4Under conditions of Pa vacuum, trimethyl gallium (TMGa) and nitrogen (N2) it is used as reaction source, the luxuriant magnesium (Cp of doping two2Mg) come
Realize the doping of GaN material p-type.Wherein TMGa flows are 1.5sccm, Cp2Mg flows are 1sccm, nitrogen flow 150sccm.
Depositing temperature is 450 DEG C, sedimentation time 180min.
3, it is deposited using magnetic control sputtering system and prepares VO2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, prepare
VO2Thin-film material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
5:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 200 DEG C, and preparation time is 200 minutes.
4 then magnetron sputtering preparation in, under conditions of vacuum is extracted into 1.0 × 10-3Pa vacuum, continue prepare AZO
Transparent conductive electrode.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
6:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 250 DEG C, and preparation time is 30 minutes.
5, continue to prepare TiN anti-corrosion protection coatings in magnetron sputtering preparation, technological parameter condition is：Nitrogen conduct
The purity in gas reaction source, nitrogen flow 70sccm, reactive sputtering titanium nitride target is 99.99%, underlayer temperature 250
DEG C, preparation time is 20 minutes.
Using XPS to VO after experiment2/ p-GaN heterojunction structures are tested analysis, as shown in figure 4, being surveyed in XPS
All elements that can well in recognition combination object in amount spectrum.We detect that there are p-GaN and VO in all samples2Letter
Number, show to have prepared two kinds of thin-film materials.In addition, being calculated as 12.90eV from Fig. 5 in conjunction with energy span, it was demonstrated that
VO2The VO of/p-GaN/ heterojunction structures2The valence state of V in layer is mainly made of V4+.
Example 4
1, self-supporting diamond substrate is first used into ionized water ultrasonic cleaning after ten minutes, magnetron sputtering reaction is sent into drying
Room, 1.0 × 10-3Under conditions of Pa vacuum, AZO transparent conductive electrodes are prepared in its self-supporting diamond substrate deposition.Its work
Skill Parameter Conditions are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 4:1, reactive sputtering oxidation
The purity of zinc doping aluminium target is 99.9%, and preparation temperature is 350 DEG C, and preparation time is 60 minutes.
2 then using plasma enhancing organic chemical vapor deposition system prepare p-type GaN material, vacuum is evacuated to
1.0×10-4Under conditions of Pa vacuum, trimethyl gallium (TMGa) and nitrogen (N2) it is used as reaction source, the luxuriant magnesium (Cp of doping two2Mg) come
Realize the doping of GaN material p-type.Wherein TMGa flows are 1.4sccm, Cp2Mg flows are 0.5sccm, and nitrogen flow is
100sccm.Depositing temperature is 550 DEG C, sedimentation time 180min.
3, it is deposited using magnetic control sputtering system and prepares VO2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, prepare
VO2Thin-film material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
6:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 260 DEG C, and preparation time is 200 minutes.
4 then magnetron sputtering preparation in, vacuum is extracted into 1.0 × 10-3Under conditions of Pa vacuum, it is saturating to continue preparation AZO
Bright conductive electrode.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 5:
1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 200 DEG C, and preparation time is 30 minutes.
5, continue to prepare TiN anti-corrosion protection coatings in magnetron sputtering preparation, technological parameter condition is：Nitrogen conduct
The purity in gas reaction source, nitrogen flow 40sccm, reactive sputtering titanium nitride target is 99.99%, underlayer temperature 300
DEG C, preparation time is 20 minutes.
Embodiment 5
1, self-supporting diamond substrate is first used into ionized water ultrasonic cleaning after ten minutes, magnetron sputtering reaction is sent into drying
Room, 1.0 × 10-3Under conditions of Pa vacuum, AZO transparent conductive electrodes are prepared in its self-supporting diamond substrate deposition.Its work
Skill Parameter Conditions are：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 8:1, reactive sputtering oxidation
The purity of zinc doping aluminium target is 99.9%, and preparation temperature is 400 DEG C, and preparation time is 60 minutes.
2 then using plasma enhancing organic chemical vapor deposition system prepare p-type GaN material, vacuum is evacuated to
1.0×10-4Under conditions of Pa vacuum, trimethyl gallium (TMGa) and nitrogen (N2) it is used as reaction source, the luxuriant magnesium (Cp of doping two2Mg) come
Realize the doping of GaN material p-type.Wherein TMGa flows are 1sccm, Cp2Mg flows are 1.0sccm, nitrogen flow 150sccm.
Depositing temperature is 600 DEG C, sedimentation time 180min.
3, it is deposited using magnetic control sputtering system and prepares VO2Thin-film material, 1.0 × 10-3Under conditions of Pa vacuum, prepare
VO2Thin-film material.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
3:1, the purity of reactive sputtering vanadium dioxide target is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 200 minutes.
4 then magnetron sputtering preparation in, under conditions of vacuum is extracted into 1.0 × 10-3Pa vacuum, continue prepare AZO
Transparent conductive electrode.Its technological parameter condition is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio
7:1, the purity of the Zinc oxide doped aluminium target of reactive sputtering is 99.9%, and preparation temperature is 300 DEG C, and preparation time is 30 minutes.
5, continue to prepare TiN anti-corrosion protection coatings in magnetron sputtering preparation, technological parameter condition is：Nitrogen conduct
The purity in gas reaction source, nitrogen flow 80sccm, reactive sputtering titanium nitride target is 99.99%, underlayer temperature 400
DEG C, preparation time is 20 minutes.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (7)
1. a kind of self-supporting diamond substrate heterojunction structure, which is characterized in that include the anticorrosive protections of TiN successively from top to bottom
Layer, AZO transparent conductive film, VO2Material layer, p-GaN material layers, AZO transparent conductive film layer, self-supporting diamond substrate.
2. a kind of preparation method of self-supporting diamond substrate heterojunction structure, which is characterized in that self-supporting diamond substrate according to
Secondary preparation AZO transparent conductive film, p-GaN material layers, VO2Material layer, AZO transparent conductive film and the anticorrosive protective layers of TiN.
3. preparation method according to claim 2, which is characterized in that the preparation of AZO transparent conductive film includes：It will be from branch
It supports diamond substrate and first uses ionized water ultrasonic cleaning after ten minutes, magnetron sputtering reative cell is sent into drying, 1.0 × 10-3Pa
Under conditions of vacuum, AZO transparent conductive electrodes are prepared in its self-supporting diamond substrate deposition.Its technological parameter condition is：Argon
Gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 4:1-10:1, the Zinc oxide doped aluminium target of reactive sputtering
The purity of material is 99.9%, and preparation temperature is 200 DEG C~400 DEG C, and preparation time is 60~100 minutes.
4. preparation method according to claim 2, which is characterized in that prepare p-GaN material layers in AZO transparent conductive film
Including：Using plasma enhances organic chemical vapor deposition system and prepares p-type GaN material, and vacuum is evacuated to 1.0 × 10- 4Under conditions of Pa vacuum, trimethyl gallium and nitrogen adulterate two luxuriant magnesium to realize that GaN material p-type is adulterated as reaction source, wherein
TMGa flows are 1.0~1.5sccm, Cp2Mg flows are 0.5~1.0sccm, and nitrogen flow is 100~150sccm, deposition temperature
Degree is 400 DEG C~600 DEG C, sedimentation time 180min.
5. preparation method according to claim 2, which is characterized in that prepare VO in p-GaN material layers2Material layer includes：
Magnetic control sputtering system deposition prepares VO2, under conditions of 1.0 × 10-3Pa vacuum, prepare VO2Material layer, technological parameter condition
It is：Argon gas and oxygen are as mixed gas reaction source, argon gas and oxygen flow ratio 3:1~8:1, reactive sputtering vanadium dioxide target
The purity of material is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, and preparation time is 200~300 minutes.
6. preparation method according to claim 2, which is characterized in that in VO2It is prepared by magnetron sputtering in material layer, it will
Vacuum is extracted under conditions of 1.0 × 10-3Pa vacuum, prepares AZO transparent conductive electrodes, and technological parameter condition is：Argon gas and oxygen
Gas is as mixed gas reaction source, argon gas and oxygen flow ratio 5:1~7:1, the Zinc oxide doped aluminium target of reactive sputtering it is pure
Degree is 99.9%, and preparation temperature is 100 DEG C~300 DEG C, and preparation time is 30~60 minutes.
7. preparation method according to claim 2, which is characterized in that pass through magnetron sputtering in AZO transparent conductive electrodes
Equipment prepares TiN anti-corrosion protection coatings, and technological parameter condition is：Nitrogen is as gas reaction source, nitrogen flow 30
The purity of~80sccm, reactive sputtering titanium nitride target are 99.99%, and underlayer temperature is 100 DEG C~400 DEG C, and preparation time is
20~50 minutes.
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