CN114717657A - Method for epitaxially growing nickel oxide single crystal film based on plasma-assisted laser molecular beam - Google Patents
Method for epitaxially growing nickel oxide single crystal film based on plasma-assisted laser molecular beam Download PDFInfo
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- CN114717657A CN114717657A CN202210272003.5A CN202210272003A CN114717657A CN 114717657 A CN114717657 A CN 114717657A CN 202210272003 A CN202210272003 A CN 202210272003A CN 114717657 A CN114717657 A CN 114717657A
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- 239000013078 crystal Substances 0.000 title claims abstract description 44
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 40
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 16
- 230000003746 surface roughness Effects 0.000 claims abstract description 11
- 238000001534 heteroepitaxy Methods 0.000 claims abstract description 7
- 239000010409 thin film Substances 0.000 claims description 13
- 239000010408 film Substances 0.000 claims description 11
- 229910052594 sapphire Inorganic materials 0.000 claims description 11
- 239000010980 sapphire Substances 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 8
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000013077 target material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 3
- 238000007872 degassing Methods 0.000 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 6
- 230000008021 deposition Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 125000004430 oxygen atom Chemical group O* 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 abstract 2
- 229910001195 gallium oxide Inorganic materials 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000000407 epitaxy Methods 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 6
- 238000000089 atomic force micrograph Methods 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002128 reflection high energy electron diffraction Methods 0.000 description 2
- 241001354791 Baliga Species 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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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
- C30B29/16—Oxides
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for epitaxially growing a nickel oxide single crystal film based on plasma-assisted laser molecular beams. Firstly, preprocessing an oxide substrate; and heteroepitaxially growing nickel oxide on the oxide substrate at normal temperature by using oxygen plasma assisted laser molecular beam epitaxy to obtain single crystal nickel oxide. The method combines substrate pretreatment and oxygen plasma auxiliary deposition, optimizes growth conditions through laser molecular beam epitaxy, obtains NiO single crystal at normal temperature, improves crystal quality, reduces surface roughness and enables device performance to be improved considerably. Due to the effective pretreatment of the substrate, a macro step flow structure is formed on the surface of the substrate, thereby being beneficial to the formation of NiO single crystal; in addition, oxygen atoms are activated by the aid of oxygen plasma, and single crystal NiO is heteroepitaxial at normal temperature. The high-quality heteroepitaxy of the natural p-type material on the gallium oxide substrate widens the realization way of the gallium oxide-based high-power device.
Description
Technical Field
The invention relates to a method for epitaxially growing a nickel oxide single crystal film based on plasma-assisted laser molecular beams, belonging to the technical field of preparation of wide bandgap semiconductor material devices.
Background
Ga as a super-wide bandgap semiconductor material2O3The high-breakdown-strength GaN-SiC semiconductor has a larger forbidden band width (4.5-4.9 eV) and a high breakdown field strength (8MV/cm), has a Baliga excellent value of over 3000 which is 5-10 times that of wide-band-gap semiconductors GaN and SiC, and has wide application prospects in the fields of power devices, radio frequency devices and the like. However, Ga2O3Many challenges still remain in research, and the lack of p-type doping capability remains based on Ga2O3Is limited by the power electronics of (a). Search for other p-type wide bandgap semiconductor materials and use of the materials in combination with Ga2O3Forming high quality heterogeneous integration is one possible solution.
NiO is a natural p-type oxide semiconductor and has attracted much attention due to its band gap of 3.2-3.8 eV, excellent chemical stability, and high visible light transmittance. In addition, the large exciton binding energy (110meV) makes it more widely used than GaN, ZnO, etc., and NiO and Ga2O3There is a well-matched epitaxial relationship and band structure between them. Common nickel oxide epitaxy methods include magnetron sputtering, laser molecular beam epitaxy, and the like. The nickel oxide obtained by magnetron sputtering is usually polycrystalline and amorphous, the surface roughness of the film obtained by the particle bombardment deposition mode is large, various defects exist in the crystal, the transportation of current carriers is hindered by the existence of a polycrystalline boundary, and the improvement of the device performance is still greatly limited.
At present, high-temperature epitaxy is often required to obtain a high-quality oxide heteroepitaxial film, and the epitaxy cost is high and the process is complex. In addition, the commonly used growth means such as magnetron sputtering is usually particle bombardment deposition rather than epitaxial growth, and usually polycrystalline and amorphous nickel oxide is obtained, which has large surface roughness and poor crystal quality, so that the improvement of the device performance still has a bottleneck.
Disclosure of Invention
The invention aims to: aiming at improving the quality of nickel oxide crystals and breaking through the bottleneck of device performance, the method for obtaining the nickel oxide single crystals with low surface roughness by Laser Molecular Beam Epitaxy (LMBE) at normal temperature in combination with substrate pretreatment and oxygen plasma assisted deposition is provided. According to the invention, the oxygen plasma assisted NiO growth does not need high temperature, the growth steps are simplified, the pretreatment of the substrate and the optimization of the growth conditions optimize common polycrystalline and amorphous products into single crystal NiO, the crystal quality is improved, the surface roughness is reduced, and the improvement of the device performance is considerable.
The invention adopts the following technical scheme for solving the technical problems:
the method for growing the nickel oxide single crystal film based on plasma-assisted laser molecular beam epitaxy combines substrate pretreatment and oxygen plasma assistance, and obtains the nickel oxide single crystal through laser molecular beam epitaxy at normal temperature, and specifically comprises the following steps:
(1) pretreating the oxide substrate;
(2) and carrying out heteroepitaxy on nickel oxide on an oxide substrate at normal temperature by using oxygen plasma-assisted laser molecular beam epitaxy to obtain single crystal nickel oxide.
Further, the oxide substrate in the step (1) is c-plane sapphire, ZnO or Ga2O3。
Further, the pretreatment in the step (1) comprises the following specific steps: and corroding the oxide substrate in hot concentrated sulfuric acid for 0.5-1 h, and then annealing at high temperature for 12-24 h.
Further, the temperature of the concentrated sulfuric acid is 120-180 ℃.
Further, the annealing temperature is 1000-1500 ℃.
Further, in the step (2), the laser wavelength is λ 248nm, and the laser power density is 135-225 mJ; the laser frequency is 1-10 Hz.
Further, in the step (2), the power of the oxygen plasma is 150-300W, the flow of the oxygen is 1.5-3 sccm, and the growth pressure is 1 multiplied by 10-5～9×10-5Torr。
Further, the step (2) of heteroepitaxially growing nickel oxide on the oxide substrate specifically comprises the following steps:
putting the cleaned substrate dried by nitrogen into a pre-pumping chamber of laser molecular beam epitaxy equipment, and sending the substrate into a growth chamber after being baked and degassed in the pre-pumping chamber; the target material is nickel oxide, and the growth atmosphere is O2。
Furthermore, the vacuum degree of the pre-pumping chamber is 6 multiplied by 10-7Below Torr, the background vacuum of the growth chamber is 6X 10-8Torr below; the distance d between the substrate and the target materialS-T40-50 cm; said O is2The purity of the nickel oxide target is more than 99.99 percent, and the purity of the nickel oxide target is more than 99.99 percent.
According to the nickel oxide single crystal thin film prepared by the method, the surface roughness of the nickel oxide single crystal thin film is reduced to 0.20 nm.
Advantageous effects
(1) By combining substrate pretreatment, oxygen plasma assistance and optimization of growth conditions, NiO single crystal is obtained at normal temperature through laser molecular beam epitaxy, and the surface roughness can be reduced to 0.20 nm.
(2) The effective pretreatment of the substrate is benefited, the substrate surface is formed, and the formation of NiO single crystal is facilitated; oxygen plasma assisted deposition activates oxygen atoms, so that the NiO single crystal can be heteroepitaxially grown at normal temperature.
In a word, NiO obtained by heteroepitaxy is single crystal, and the surface roughness is greatly reduced.
Drawings
Fig. 1 is a reflection high-energy electron diffraction pattern of NiO obtained by normal temperature epitaxy on a c-plane sapphire substrate.
Fig. 2 is an X-ray 2 θ - ω scan of NiO obtained by normal temperature epitaxy on a c-plane sapphire substrate.
FIG. 3 is a rocking graph of the X-ray diffraction (111) plane of the NiO film prepared.
Fig. 4(a) is an atomic force microscope image of a pretreated c-plane sapphire substrate, and (b) is an atomic force microscope image of the prepared NiO single crystal thin film.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The oxide substrate used for NiO heteroepitaxy is c-plane sapphire, ZnO, Ga2O3。
Example 1
In this embodiment, an oxygen plasma is used to perform epitaxy of a nickel oxide single crystal on a sapphire substrate at room temperature, and the specific steps are as follows:
(1) preprocessing a c-plane sapphire substrate: corroding in hot concentrated sulfuric acid (150 ℃) for 30min, and annealing at high temperature (1200 ℃) in an annealing furnace for 12 h;
(2) heteroepitaxy NiO at room temperature using laser molecular beam epitaxy (λ 248 nm): the substrate after being cleaned and dried by nitrogen is put into a pre-pumping chamber of laser molecular beam epitaxy equipment, and the vacuum degree of the pre-pumping chamber is 6 multiplied by 10-7Torr, baking and degassing in a pre-pumping chamber, and sending into a growth chamber with background vacuum degree of 6 × 10-8Torr; NiO (purity of 99.99%) is used as a target material, and the growth atmosphere is O2(purity over 99.99%); substrate target spacing dS-T45cm, the laser power density is 135mJ, and the laser frequency is 2 Hz;
(3) by oxygen plasma assisted deposition, the oxygen plasma power is 200W, the oxygen flow is 2sccm, and the growth pressure is 6X 10-5Torr, NiO was epitaxially grown at room temperature for 3 hours.
As shown in fig. 1, which is a reflection high-energy electron diffraction pattern of NiO obtained by normal temperature epitaxy on a c-plane sapphire substrate, it can be seen from the diffraction fringes in the figure that the prepared NiO is single crystal, and the surface of the sample is very flat.
As shown in fig. 2, which is an X-ray 2 θ - ω scan of NiO obtained by normal temperature epitaxy on a c-plane sapphire substrate, it was confirmed that the diffraction peak of NiO was cubic NiO, and that heteroepitaxy yielded cubic NiO single crystal.
FIG. 3 is a rocking curve diagram of the X-ray diffraction (111) plane of the prepared NiO film, the full width at half maximum of the rocking curve is an important index for representing the quality of the single crystal, and the full width at half maximum of the rocking curve of the (111) plane of the prepared NiO film is 0.77 degrees, which shows that the crystal quality of the prepared NiO single crystal film is good.
As shown in fig. 4(a), which is an atomic force microscope image of a pretreated c-plane sapphire substrate, ravines can be seen, and the surface roughness is 0.23 nm; (b) the surface roughness was 0.20nm for atomic force microscopy images of the prepared NiO film.
Claims (10)
1. The method for growing the nickel oxide single crystal film based on plasma-assisted laser molecular beam epitaxy is characterized in that the single crystal nickel oxide is obtained by laser molecular beam epitaxy at normal temperature by combining substrate pretreatment and oxygen plasma assistance, and specifically comprises the following steps:
(1) pretreating the oxide substrate;
(2) and carrying out heteroepitaxy on nickel oxide on an oxide substrate at normal temperature by using oxygen plasma-assisted laser molecular beam epitaxy to obtain single crystal nickel oxide.
2. The method for growing a nickel oxide single crystal thin film based on plasma-assisted laser molecular beam epitaxy as claimed in claim 1, wherein the oxide substrate in step (1) is c-plane sapphire, ZnO or Ga2O3。
3. The method for epitaxially growing a nickel oxide single crystal thin film based on the plasma-assisted laser molecular beam according to claim 1, wherein the pretreatment in the step (1) comprises the following specific steps: and corroding the oxide substrate in hot concentrated sulfuric acid for 0.5-1 h, and then annealing at high temperature for 12-24 h.
4. The method for epitaxially growing a nickel oxide single crystal thin film based on a plasma-assisted laser molecular beam according to claim 3, wherein the temperature of the concentrated sulfuric acid is 120-180 ℃.
5. The method for epitaxially growing a nickel oxide single crystal thin film based on a plasma-assisted laser molecular beam according to claim 3, wherein the annealing temperature is 1000 to 1500 ℃.
6. The method for epitaxially growing a nickel oxide single crystal thin film based on a plasma-assisted laser molecular beam according to claim 1, wherein in the step (2), the laser wavelength is λ 248nm or 193nm, and the laser power density is 135-225 mJ; the laser frequency is 1-10 Hz.
7. The method for epitaxial growth of nickel oxide single crystal thin film based on plasma assisted laser molecular beam according to claim 1, wherein the oxygen plasma power in step (2) is 150-300W, the oxygen flow rate is 1.5-3 sccm, and the growth pressure is 1 x 10-5～9×10-5Torr。
8. The method for epitaxially growing a nickel oxide single crystal thin film based on a plasma-assisted laser molecular beam according to claim 1, wherein the step (2) of heteroepitaxially growing nickel oxide on an oxide substrate comprises the following specific steps:
putting the cleaned substrate dried by nitrogen into a pre-pumping chamber of laser molecular beam epitaxy equipment, baking and degassing in the pre-pumping chamber, and then sending the substrate into a growth chamber; the target material is nickel oxide, and the growth atmosphere is O2。
9. The method for epitaxially growing a nickel oxide single crystal thin film based on plasma-assisted laser molecular beam according to claim 8, wherein the degree of vacuum of the pre-chamber is 6X 10-7Below Torr, the background vacuum of the growth chamber is 6X 10- 8Torr below; the distance d between the substrate and the target materialS-T40-50 cm; said O is2The purity of the nickel oxide target is more than 99.99 percent, and the purity of the nickel oxide target is more than 99.99 percent.
10. The nickel oxide single crystal thin film produced by the method according to any one of claims 1 to 9, wherein the surface roughness of the nickel oxide single crystal thin film is reduced to 0.20 nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115838971A (en) * | 2023-02-14 | 2023-03-24 | 楚赟精工科技(上海)有限公司 | Gallium oxide film and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN102534767A (en) * | 2011-12-29 | 2012-07-04 | 浙江大学 | Na-mixing method for growing p-type ZnO single crystal film |
| CN111334856A (en) * | 2020-02-18 | 2020-06-26 | 浙江大学 | Method for growing high-quality ZnO single crystal film by quasi van der waals epitaxy using plasma-assisted molecular beam epitaxy |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534767A (en) * | 2011-12-29 | 2012-07-04 | 浙江大学 | Na-mixing method for growing p-type ZnO single crystal film |
| CN111334856A (en) * | 2020-02-18 | 2020-06-26 | 浙江大学 | Method for growing high-quality ZnO single crystal film by quasi van der waals epitaxy using plasma-assisted molecular beam epitaxy |
Non-Patent Citations (3)
| Title |
|---|
| MELANIE BUDDE 等: "Structural, optical, and electrical properties of unintentionally doped NiO layers grown on MgO by plasma-assisted molecular beam epitaxy", 《JOURNAL OF APPLIED PHYSICS》 * |
| 倪曼曼: "基于ZnO的异质结的组建及其光电性能研究", 《中国优秀硕士学位论文数据库 信息科技辑》 * |
| 贝力等: "脉冲激光沉积制备NiO(111)外延薄膜及其结构研究", 《电子元件与材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115838971A (en) * | 2023-02-14 | 2023-03-24 | 楚赟精工科技(上海)有限公司 | Gallium oxide film and preparation method thereof |
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