CN103456603A - Method for preparing gallium oxide film on gallium series heterogeneous semiconductor substrate and gallium oxide film - Google Patents
Method for preparing gallium oxide film on gallium series heterogeneous semiconductor substrate and gallium oxide film Download PDFInfo
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Abstract
The invention provides a method for preparing a gallium oxide film on a gallium series heterogeneous semiconductor substrate and the gallium oxide film. The method for preparing the gallium oxide film on the gallium series heterogeneous semiconductor substrate comprises the following steps: selecting a gallium series semiconductor substrate, cleaning the surface of the gallium series semiconductor substrate, then in an atmosphere containing the oxygen partial pressure, adopting external energy to process the gallium series semiconductor substrate to open chemical bonds, formed by gallium atoms and other component atoms, on the surface area of the gallium series semiconductor substrate, enabling the gallium atoms and oxygen atoms in the atmosphere to be combined to form gallium-oxygen bonds, and finally growing the gallium oxide film on the processed gallium series heterogeneous semiconductor substrate through the gallium oxide film growing technology. The method for preparing the gallium oxide film on the gallium series heterogeneous semiconductor substrate is scientific and reasonable in step, the various problems in the prior art are solved, and the defect density of a heteroepitaxial growth gallium oxide film is effectively reduced.
Description
Technical field
The present invention relates to the semi-conducting material technology of preparing, relating in particular to a kind of is method and the gallium oxide film for preparing the gallium oxide film on the heterogeneous semiconductor substrate at gallium.
Background technology
The gallium oxide material has monoclinic form, has the direct band gap structure, and energy gap is 4.9eV, at aspects such as luminous, detection and electronic devices, important application is arranged, and is the study hotspot in current wide bandgap semiconductor materials field.Although can in laboratory, prepare gallium oxide single crystal at present, its crystal mass need to improve, and the gallium oxide single crystal volume that at present prepared by laboratory is often very little, and preparation cost is very high; Gallium oxide film prepared on gallium oxide homogeneity single crystalline substrate by what is more important is difficult to carry out combination collocation with other semi-conducting material, and this has just limited the application of gallium oxide film greatly.
In order to address the above problem, people attempt the gallium oxide film preparation on other heterogeneous semiconductor substrate, and the substrate often adopted at present comprises sapphire, magnesium oxide and silicon etc.But, these substrates are different from the crystal formation of gallium oxide material, and lattice mismatch is large, cause can producing larger stress at the gallium oxide film in epitaxial process, a large amount of defects is introduced in the release meeting of stress in the gallium oxide film of heteroepitaxial growth, causes the quality of gallium oxide film significantly to descend.So urgently a kind of can be to prepare the method for high-quality gallium oxide film on the heterogeneous semiconductor substrate at gallium.
Summary of the invention
The object of the invention is to, for above-mentioned having now at gallium, be to prepare the gallium oxide film on the heterogeneous semiconductor substrate to have second-rate problem, proposing a kind of is to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium, and the method can be reduced in the defect concentration caused by stress in the gallium oxide film effectively.
For achieving the above object, the technical solution used in the present invention is: a kind of is to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium, comprises the following steps:
1) choose gallium based semiconductor substrate, and cleaning gallium based semiconductor substrate surface;
2) in containing the atmosphere of partial pressure of oxygen, adopt external energy to be processed gallium based semiconductor substrate, the chemical bond of the gallium atom of gallium based semiconductor substrate surface area and the formation of other constituent atoms is opened, made the oxygen atom of gallium atom in atmosphere be combined and form gallium oxygen key.
3) adopt the gallium based semiconductor Grown gallium oxide film of gallium oxide film growing technology after processing.
Further, described cleaning gallium based semiconductor substrate surface is the organic and inorganic impurity of removing the absorption of gallium based semiconductor substrate surface, and the compound layer that covers because of reaction of substrate surface.
Further, described manner of cleaning up comprises chemical cleaning and/or physical cleaning.
Further, described energy is one or more in ion beam bombardment, high energy particle irradiation, electromagnetic field and thermal radiation.
Further, described step 2) temperature is that 50-1200 ℃, air pressure are 10
-2-10
3the intensity that torr, time are 1-120min, energy is equivalent to provides energy 10 for each gallium atom of substrate surface
-1-10
2eV.
Further, the gallium oxide film growing technology that described gallium oxide film growing technology is controlled extension speed.
Further, the control precision of the gallium oxide film growing technology of described controlled extension speed reaches the atomic layer rank.
Further, described gallium oxide film growing technology is a kind of in magnetron sputtering, atomic layer epitaxy, molecular beam epitaxy and metal-organic chemical vapor deposition equipment technology.
Further, the temperature of described step 3) is that 300-1200 ℃, reative cell air pressure are 10
-9-10
3torr, oxygen source are 10 with the molar flow ratio in gallium source
-1-10
5.
Another object of the present invention is also to disclose a kind of gallium oxide film, and this gallium oxide film has good crystalline quality.
For achieving the above object, the technical solution used in the present invention is: it is that the method for preparing the gallium oxide film on the heterogeneous semiconductor substrate is prepared from gallium that a kind of gallium oxide film adopts above-mentioned.
The present invention relates at gallium is to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate, before growth first to the modifying surface area of selected substrate again structure process, utilizing the gallium atom in substrate, is previously prepared skim gallium oxide film on the heterogeneous semiconductor substrate by pretreating process at gallium.Use surface-treated substrate to carry out subsequently epitaxial growing gallium oxide film, can reach the homogenous growth effect, can effectively reduce the defect concentration caused by stress in the gallium oxide film due to lattice mismatch in heteroepitaxy, this gallium oxide film prepared can be well and other semi-conducting material carry out combination collocation, make the gallium oxide film that more wide application can be arranged.
The accompanying drawing explanation
Fig. 1 utilizes oxygen ion beam to gallium nitride/sapphire compound substrate modifying surface schematic diagram of structure again in embodiment 1;
Fig. 2 adopts the metal-organic chemical vapor deposition equipment technology to carry out the schematic diagram of gallium oxide film extension on the transformed substrate in surface in embodiment 1;
The X-ray diffraction test collection of illustrative plates that Fig. 3 is the gallium oxide film of preparation in embodiment 1;
Fig. 4 utilizes heat radiation method to gallium nitride/sapphire compound substrate modifying surface schematic diagram of structure again in embodiment 2;
Fig. 5 adopts the metal-organic chemical vapor deposition equipment technology to transform the schematic diagram that carries out gallium oxide film extension on substrate on surface in embodiment 2;
The X-ray diffraction test collection of illustrative plates that Fig. 6 is the gallium oxide film of preparation in embodiment 2.
Embodiment
The invention discloses a kind of is to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium, and the method can be reduced in the defect concentration caused by stress in the gallium oxide film due to lattice mismatch in the heteroepitaxy process effectively.Particularly, the present invention is that the method for preparing the gallium oxide film on the heterogeneous semiconductor substrate comprises the following steps at gallium:
1) choose gallium based semiconductor substrate, and cleaning gallium based semiconductor substrate surface;
2) in containing the atmosphere of partial pressure of oxygen (atmosphere that contains oxygen atom), adopt external energy to be processed gallium based semiconductor substrate, the chemical bond of the gallium atom of gallium based semiconductor substrate surface area and the formation of other constituent atoms is opened, made the oxygen atom of gallium atom in atmosphere be combined and form gallium oxygen key.
3) adopt the gallium based semiconductor Grown gallium oxide film of gallium oxide film growing technology after processing.
Described cleaning gallium based semiconductor substrate surface is the organic and inorganic impurity of removing the absorption of gallium based semiconductor substrate surface.Manner of cleaning up of the present invention comprises chemical cleaning and/or physical cleaning.
Described energy is one or more in ion beam bombardment, high energy particle irradiation, electromagnetic field and thermal radiation.
Described step 2) temperature that regulation and control are processed is 50-1200 ℃, is preferably 650-950 ℃; Air pressure is 10
-2-10
3torr, be preferably 1-5torr or 760torr; Time is 1-120min, is preferably 5-30min; The intensity of energy flow energy is equivalent to provides energy 10 for each gallium atom of substrate surface
-1-10
2eV, be preferably 10-20eV.The intensity of the temperature that the present invention processes by regulation and control, air pressure, time and energy is controlled degree of crystallinity, stoichiometric proportion, surface topography and the thickness of gallium oxide thin layer.The gallium oxide film growing technology that described gallium oxide film growing technology is controlled extension speed.The control precision of the gallium oxide film growing technology of described controlled extension speed reaches the atomic layer rank.Described gallium oxide film growing technology is a kind of in magnetron sputtering, atomic layer epitaxy, molecular beam epitaxy and metal-organic chemical vapor deposition equipment technology.
The temperature of described step 3) is 300-1200 ℃, is preferably 650-900 ℃; Reative cell air pressure is 10
-9-10
3torr, be preferably 10
-9-10
-7torr or 1-5torr oxygen source are 10 with the molar flow ratio in gallium source
-1-10
5, be preferably 1-100 or 5.0 * 10
3-5.0 * 10
4.The present invention realizes the preparation of high-quality gallium oxide film by optimizing temperature, reative cell air pressure, source supply mode and quantity delivered.
The invention also discloses a kind of gallium oxide film, it is that the method for preparing the gallium oxide film on the heterogeneous semiconductor substrate is prepared from gallium that this gallium oxide film adopts above-mentioned.This gallium oxide film has good crystalline quality (because this method first generates one deck gallium oxide on gallium based semiconductor surface, then carry out again epitaxial growth and belong to homoepitaxy, the stress that basic elimination lattice mismatch causes, and then the defect caused is just few), can be well and other semi-conducting material carry out combination collocation, make the gallium oxide film that more wide application can be arranged.
Below further illustrate the present invention by specific embodiment.
Embodiment 1
Fig. 1 utilizes oxygen ion beam to gallium nitride/sapphire compound substrate modifying surface schematic diagram of structure again in embodiment 1; Fig. 2 adopts the metal-organic chemical vapor deposition equipment technology to carry out the schematic diagram of gallium oxide film extension on the transformed substrate in surface in embodiment 1; The X-ray diffraction test collection of illustrative plates that Fig. 3 is the gallium oxide film of preparation in embodiment 1.
Referring to Fig. 1 and Fig. 2, the present embodiment discloses a kind of metal-organic chemical vapor deposition equipment that utilizes and prepared the method for gallium oxide film on sapphire 3/ gallium nitride 2 compound substrate, and it is oxygen plasma that the method adopts energy, specifically comprises following steps:
Step 1: on choice for use sapphire 3 substrates extension the compound substrate of 2 layers of gallium nitride, substrate surface is cleared up, mainly for the organic and inorganic impurity of adsorption, and the non-component composition layer that covers because of reaction of substrate surface; Manner of cleaning up comprises chemistry and two kinds of physics.
Step 2: at room temperature, under oxygen plasma 1 environment, compound substrate is bombarded, oxygen flow 20sccm wherein, power is 50W, and reative cell pressure is 0.5Pa, and be 300s action time.Make the gallium nitrogen bond fission on gallium nitride top layer, nitrogen-atoms breaks away from away, and the gallium atom can be combined with oxygen atom, forms gallium oxygen key, thereby at gallium nitride substrate surface preparation skim gallium oxide film 5.Control degree of crystallinity, stoichiometric proportion, surface topography and the thickness of gallium oxide thin layer by reative cell pressure, oxygen plasma action time and bombardment power.
Step 3: pass into gallium source and oxygen source 4, utilize metal-organic chemical vapor deposition equipment, continue epitaxial growth gallium oxide film on the compound substrate of preparing through above-mentioned two steps.Regulating the trimethyl gallium source temperature is 800torr and carrier gas (high-purity argon gas) flow 20sccm for-10 ℃, source bottle pressure, and auxiliary gas (high-purity argon gas) flow is 500sccm; The adjusting oxygen flow is 900sccm; Controlling growth temperature is 700 ℃, and the speed of growth is 0.4 μ m/h, grows 1 hour, and sheet is got in then shutdown system cooling, obtains the gallium oxide film prepared.
The gallium oxide film that the present embodiment is prepared is characterized, and the X-ray diffraction test result of sample as shown in Figure 3, can tentatively see that from figure the gallium oxide film has (202) orientation.
Fig. 4 utilizes heat radiation method to gallium nitride/sapphire compound substrate modifying surface schematic diagram of structure again in embodiment 2; Fig. 5 adopts the metal-organic chemical vapor deposition equipment technology to transform the schematic diagram that carries out gallium oxide film extension on substrate on surface in embodiment 2; The X-ray diffraction test collection of illustrative plates that Fig. 6 is the gallium oxide film of preparation in embodiment 2.
Referring to Fig. 4 and Fig. 5, the present embodiment discloses a kind of metal-organic chemical vapor deposition equipment that utilizes and prepared the method for gallium oxide film on sapphire 3/ gallium nitride 2 compound substrate, and it is thermal radiation that the method adopts energy, specifically comprises following steps:
Step 1: on choice for use sapphire 3 substrates extension the compound substrate of 2 layers of gallium nitride, substrate surface is cleared up, mainly for the organic and inorganic impurity of adsorption, and the non-component composition layer that covers because of reaction of substrate surface; Manner of cleaning up comprises chemistry and two kinds of physics.
Step 2: sapphire 3/ gallium nitride 2 compound substrate are put into to the thermal annealing stove, under 750 ℃ of high purity oxygen gas atmosphere, carry out 30min heat treatment 6, the gallium nitrogen bond fission on gallium nitride 2 top layers, nitrogen-atoms breaks away from away, the gallium atom can be combined with oxygen atom, forms gallium oxygen key, thereby at gallium nitride substrate surface preparation skim gallium oxide film 5.Control degree of crystallinity, stoichiometric proportion, surface topography and the thickness of gallium oxide thin layer by pressure, oxygen flow, heat treatment temperature and time.
Step 3: pass into gallium source and oxygen source 4, utilize metal-organic chemical vapor deposition equipment, continue epitaxial growth gallium oxide film on the compound substrate of preparing through above-mentioned two steps.Regulating the trimethyl gallium source temperature is 800torr and carrier gas (high-purity argon gas) flow 20sccm for-10 ℃, source bottle pressure, and auxiliary gas (high-purity argon gas) flow is 500sccm; The adjusting oxygen flow is 900sccm; Controlling growth temperature is 700 ℃, and the speed of growth is 0.4 μ m/h, grows 1 hour, and sheet is got in then shutdown system cooling, obtains the gallium oxide film prepared.
The gallium oxide film that the present embodiment is prepared is characterized, and as shown in Figure 6, the gallium oxide film has (402) orientation to the X-ray diffraction test result of sample as we can see from the figure.
What the present invention was not limited to that above-described embodiment puts down in writing is method and the gallium oxide film for preparing the gallium oxide film on the heterogeneous semiconductor substrate at gallium, the change of the change of substrate cleaning way, energy kind, prepares the change of gallium oxide film method or reaction condition all within protection scope of the present invention.
Finally it should be noted that: above each embodiment, only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to aforementioned each embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: its technical scheme that still can put down in writing aforementioned each embodiment is modified, or some or all of technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the scope of various embodiments of the present invention technical scheme.
Claims (10)
1. one kind is to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium, it is characterized in that, comprises the following steps:
Choose gallium based semiconductor substrate, and cleaning gallium based semiconductor substrate surface;
In containing the atmosphere of partial pressure of oxygen, adopt external energy to be processed gallium based semiconductor substrate, the chemical bond of the gallium atom of gallium based semiconductor substrate surface area and the formation of other constituent atoms is opened, made the oxygen atom of gallium atom in atmosphere be combined and form gallium oxygen key;
Adopt the gallium based semiconductor Grown gallium oxide film of gallium oxide film growing technology after processing.
2. at gallium, be to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate according to claim 1, it is characterized in that, described cleaning gallium based semiconductor substrate surface is the organic and inorganic impurity of removing the absorption of gallium based semiconductor substrate surface, and the compound layer that covers because of reaction of substrate surface.
3. be to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium according to claim 1, it is characterized in that, described manner of cleaning up comprises chemical cleaning and/or physical cleaning.
4. be to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium according to claim 1, it is characterized in that, described energy is one or more in ion beam bombardment, high energy particle irradiation, electromagnetic field and thermal radiation.
5. being to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium according to claim 1, it is characterized in that described step 2) temperature 50-1200 ℃ of processing of regulation and control, air pressure be 10
-2-10
3the intensity that torr, time are 1-120min, energy is equivalent to provides energy 10 for each gallium atom of substrate surface
-1-10
2eV.
6. be to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium according to claim 1, it is characterized in that the gallium oxide film growing technology that described gallium oxide film growing technology is controlled extension speed.
7. be to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium according to claim 6, it is characterized in that, the control precision of the gallium oxide film growing technology of described controlled extension speed reaches the atomic layer rank.
8. according to claim 1 or 6 is to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium, it is characterized in that, described gallium oxide film growing technology is a kind of in magnetron sputtering, atomic layer epitaxy, molecular beam epitaxy and metal-organic chemical vapor deposition equipment technology.
9. be to prepare the method for gallium oxide film on the heterogeneous semiconductor substrate at gallium according to claim 1, it is characterized in that, the temperature of described step 3) is that 300-1200 ℃, reative cell air pressure are 10
-9-10
3torr, oxygen source are 10 with the molar flow ratio in gallium source
-1-10
5.
10. a gallium oxide film, is characterized in that, adopting claim 1-9 any one described is that the method for preparing the gallium oxide film on the heterogeneous semiconductor substrate is prepared from gallium.
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Cited By (9)
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| CN106711020A (en) * | 2015-11-18 | 2017-05-24 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Nitriding method of substrate and production method of gallium nitride buffer layer |
| CN107785241A (en) * | 2017-10-09 | 2018-03-09 | 哈尔滨工业大学 | A kind of method for preparing beta-oxidation gallium film on a silicon substrate |
| CN109346400A (en) * | 2018-10-17 | 2019-02-15 | 吉林大学 | A kind of high quality Ga2O3Film and its hetero-epitaxy preparation method |
| CN110504343A (en) * | 2018-05-18 | 2019-11-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gallium oxide film and its growing method and application based on Sapphire Substrate |
| CN110752158A (en) * | 2019-10-28 | 2020-02-04 | 中国科学技术大学 | Method for repairing surface defects of gallium oxide material |
| CN111128687A (en) * | 2019-12-30 | 2020-05-08 | 镓特半导体科技（上海）有限公司 | Preparation method of self-supporting gallium nitride layer |
| WO2022115064A1 (en) * | 2020-11-25 | 2022-06-02 | Yildiz Teknik Universitesi | A method for growing high-quality heteroepitaxial monoclinic gallium oxide crystal |
| CN115821378A (en) * | 2022-11-29 | 2023-03-21 | 厦门大学 | Method for preparing gallium oxide film by plasma thermal oxidation |
| CN115863149A (en) * | 2022-12-12 | 2023-03-28 | 中国科学院上海微系统与信息技术研究所 | Preparation method of gallium oxide structure |
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| CN106711020A (en) * | 2015-11-18 | 2017-05-24 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Nitriding method of substrate and production method of gallium nitride buffer layer |
| CN107785241A (en) * | 2017-10-09 | 2018-03-09 | 哈尔滨工业大学 | A kind of method for preparing beta-oxidation gallium film on a silicon substrate |
| CN110504343A (en) * | 2018-05-18 | 2019-11-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gallium oxide film and its growing method and application based on Sapphire Substrate |
| CN109346400B (en) * | 2018-10-17 | 2021-09-10 | 吉林大学 | High-quality Ga2O3Film and heteroepitaxial preparation method thereof |
| CN109346400A (en) * | 2018-10-17 | 2019-02-15 | 吉林大学 | A kind of high quality Ga2O3Film and its hetero-epitaxy preparation method |
| CN110752158A (en) * | 2019-10-28 | 2020-02-04 | 中国科学技术大学 | Method for repairing surface defects of gallium oxide material |
| CN111128687A (en) * | 2019-12-30 | 2020-05-08 | 镓特半导体科技（上海）有限公司 | Preparation method of self-supporting gallium nitride layer |
| CN111128687B (en) * | 2019-12-30 | 2022-05-06 | 镓特半导体科技（上海）有限公司 | Preparation method of self-supporting gallium nitride layer |
| WO2022115064A1 (en) * | 2020-11-25 | 2022-06-02 | Yildiz Teknik Universitesi | A method for growing high-quality heteroepitaxial monoclinic gallium oxide crystal |
| CN114761627A (en) * | 2020-11-25 | 2022-07-15 | 伊尔德兹技术大学 | Method for growing high-quality heteroepitaxial monoclinic gallium oxide crystal |
| CN114761627B (en) * | 2020-11-25 | 2024-01-26 | 伊尔德兹技术大学 | Method for growing high-quality heteroepitaxial monoclinic gallium oxide crystal |
| CN115821378A (en) * | 2022-11-29 | 2023-03-21 | 厦门大学 | Method for preparing gallium oxide film by plasma thermal oxidation |
| CN115863149A (en) * | 2022-12-12 | 2023-03-28 | 中国科学院上海微系统与信息技术研究所 | Preparation method of gallium oxide structure |
| CN115863149B (en) * | 2022-12-12 | 2023-07-21 | 中国科学院上海微系统与信息技术研究所 | Preparation method of gallium oxide structure |
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