WO2022141356A1 - Microwave annealing and modification method for gallium oxide material - Google Patents

Microwave annealing and modification method for gallium oxide material Download PDF

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WO2022141356A1
WO2022141356A1 PCT/CN2020/141978 CN2020141978W WO2022141356A1 WO 2022141356 A1 WO2022141356 A1 WO 2022141356A1 CN 2020141978 W CN2020141978 W CN 2020141978W WO 2022141356 A1 WO2022141356 A1 WO 2022141356A1
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gallium oxide
microwave annealing
temperature
annealing
microwave
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PCT/CN2020/141978
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Chinese (zh)
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马宏平
侯欣蓝
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光华临港工程应用技术研发(上海)有限公司
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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
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
    • H01L21/46—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
    • H01L21/477—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
    • 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
    • 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
    • H01L21/02656—Special treatments
    • H01L21/02664—Aftertreatments

Definitions

  • the invention relates to the technical field of semiconductor manufacturing, in particular to a microwave annealing modification method for gallium oxide materials.
  • gallium oxide As a third-generation wide-bandgap semiconductor material, gallium oxide has the advantages of larger band gap and higher breakdown field strength.
  • the ultra-wide band gap characteristic of gallium oxide material makes it have broad application prospects in the field of high-power and high-frequency device manufacturing.
  • Annealing is an important step in semiconductor process engineering for modifying layers of materials.
  • Traditional annealing processes include tube furnace annealing, laser annealing and rapid thermal annealing (RTP).
  • the tube furnace annealing method and the rapid thermal annealing method require high temperature during the implementation of the annealing process, which easily induces the thermal diffusion effect, resulting in the diffusion between the gallium oxide thin film material and the substrate, which will cause serious diffusion. affect the performance of the final device.
  • the current laser annealing method mainly used in the industry has the disadvantages of high equipment cost and unfavorable mass production.
  • the invention provides a microwave annealing modification method for gallium oxide material, which is used to solve the problem that thermal diffusion is easy to occur in the process of annealing the gallium oxide material in the prior art, so as to improve the performance of the finally formed semiconductor device , and reduce the annealing cost of gallium oxide material.
  • the present invention provides a microwave annealing modification method for gallium oxide material, comprising the following steps:
  • the surface of the substrate has a layer of gallium oxide
  • the gallium oxide layer is subjected to microwave annealing treatment at a preset temperature, the preset temperature being lower than a diffusion temperature, and the diffusion temperature is the heat generated between the gallium oxide material in the gallium oxide layer and the substrate Minimum temperature for diffusion.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer at a preset temperature include:
  • a plurality of preset temperatures are set, and microwave annealing treatment is performed on the gallium oxide layer at each preset temperature in sequence.
  • the plurality of preset temperatures are arranged in order from low temperature to high temperature;
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer at each preset temperature in sequence include:
  • microwave annealing is performed on the gallium oxide layer at each preset temperature in sequence.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer at each preset temperature include:
  • the substrate with the gallium oxide layer is taken out from the microwave annealer cavity.
  • the following steps are further included:
  • the cavity of the microwave annealing furnace is purged with an inert gas to remove impurity gas in the cavity of the microwave annealing furnace.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature include:
  • Microwave annealing parameters are set and an annealing atmosphere is passed into the microwave annealing furnace cavity to perform annealing treatment, and the maximum annealing temperature in the microwave annealing parameters is the preset temperature.
  • the annealing atmosphere is an argon atmosphere or a nitrogen atmosphere.
  • the specific step of cooling the microwave annealed gallium oxide layer in the microwave annealing furnace cavity includes:
  • the cavity of the microwave annealing furnace is purged with an inert gas to reduce the temperature of the cavity of the microwave annealing furnace.
  • the preset temperature is 200°C-600°C.
  • the gallium oxide layer on the surface of the substrate is annealed by the microwave annealing treatment method, and the annealing temperature (ie the preset temperature) during the microwave annealing treatment process is controlled.
  • the diffusion temperature is the lowest temperature at which thermal diffusion occurs between the gallium oxide material in the gallium oxide layer and the substrate, so as to avoid the existing traditional annealing method due to the annealing temperature during the annealing process.
  • FIG. 2 is a schematic structural diagram of a substrate having a gallium oxide layer in an embodiment of the present invention.
  • FIG. 3 is the surface topography of the unannealed and microwave annealed gallium oxide films at different temperatures taken by atomic force microscopy (AFM).
  • AFM atomic force microscopy
  • FIG. 1 is a flow chart of the microwave annealing modification method for gallium oxide materials in the specific embodiment of the present invention
  • FIG. 2 is the present invention.
  • step S11 a substrate 20 is provided, and the surface of the substrate 20 has a gallium oxide layer 21 , as shown in FIG. 2 .
  • the material of the substrate 20 may be Si, SiC or GaN.
  • the gallium oxide layer 21 may be formed on the surface of the substrate 20 by a chemical vapor deposition process, a physical vapor deposition process or an atomic layer deposition process.
  • Step S12 microwave annealing is performed on the gallium oxide layer 21 at a preset temperature, where the preset temperature is lower than a diffusion temperature, and the diffusion temperature is the gallium oxide material in the gallium oxide layer 21 and the lining The lowest temperature at which thermal diffusion occurs between the bottoms 20 .
  • the essence of microwave annealing is to directly heat the stacked structure (ie, the stacked structure composed of the substrate 20 and the gallium oxide layer 21 ) with microwaves.
  • the presence of the microwave field reduces the crystallization activation energy of the grain boundaries of the gallium oxide material, so that the amorphous gallium oxide layer 21 film can be annealed at a lower temperature (ie, under the preset temperature condition lower than the diffusion temperature).
  • the crystal nucleus can be formed and crystallized rapidly, and the interdiffusion effect of elements can be effectively controlled under lower temperature conditions, and a gallium oxide film with less interface diffusion can be finally prepared.
  • the microwave annealing technology can not only effectively reduce the thermal budget, avoid the thermal diffusion effect, and achieve the effect of low temperature annealing, but also its annealing efficiency is higher.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at a preset temperature include:
  • a plurality of preset temperatures are set, and microwave annealing treatment is performed on the gallium oxide layer 21 at each preset temperature in sequence.
  • a plurality of the preset temperatures that are different from each other can be preset, and the preset temperature is used as the highest temperature in the microwave annealing process.
  • the gallium oxide layer 21 is subjected to microwave annealing treatment under the condition of temperature.
  • the maximum temperature refers to the maximum temperature that the cavity of the microwave annealing furnace rises to during the microwave annealing process.
  • the plurality of preset temperatures are arranged in order from low temperature to high temperature;
  • a plurality of the preset temperatures may be set in an arithmetic progression from low to high.
  • the difference between adjacent preset temperatures may be 50° C., 100° C. or other values.
  • a plurality of the preset temperatures are arranged in order from low temperature to high temperature, and the higher the temperature of the preset temperature, the smaller the difference between adjacent preset temperatures.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at each preset temperature in sequence include:
  • microwave annealing is performed on the gallium oxide layer at each preset temperature in sequence.
  • microwave annealing is performed on the gallium oxide layer at each of the preset temperatures in turn.
  • the plural in this specific embodiment refers to two or more.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at each preset temperature include:
  • the substrate with the gallium oxide layer is taken out from the microwave annealer cavity.
  • the following steps are further included:
  • the cavity of the microwave annealing furnace is purged with an inert gas to remove impurity gas in the cavity of the microwave annealing furnace.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature include:
  • Microwave annealing parameters are set and an annealing atmosphere is passed into the microwave annealing furnace cavity to perform annealing treatment, and the maximum annealing temperature in the microwave annealing parameters is the preset temperature.
  • the preset temperature is used as the maximum temperature of the microwave annealing process, which means that in a single microwave annealing process During the treatment process, the maximum temperature that can be raised inside the microwave annealing furnace cavity. After the microwave annealing furnace cavity is raised to the preset temperature, the preset temperature is maintained for a preset time, so as to realize the microwave annealing treatment of the gallium oxide layer.
  • the preset time is a preset annealing duration.
  • the annealing atmosphere is an argon atmosphere or a nitrogen atmosphere.
  • the specific step of cooling the microwave annealed gallium oxide layer in the microwave annealing furnace cavity includes:
  • the cavity of the microwave annealing furnace is purged with an inert gas to reduce the temperature of the cavity of the microwave annealing furnace.
  • the preset temperature is 200°C-600°C.
  • the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at a preset temperature include: step a, placing a sample: placing the substrate 20 with the gallium oxide layer 21 in a microwave annealing furnace In the middle position of the cavity, close the cavity door, and then vacuumize the microwave annealing furnace cavity; step b, cavity purging: first use a sufficient amount of argon to purge the microwave annealing furnace cavity and cleaning to remove the residual oxygen in the cavity of the microwave annealing furnace and on the inner wall of the cavity, and keep the argon gas purged for a period of time.
  • step c set annealing parameters: set the annealing power, the highest temperature during the annealing process, the annealing temperature steps and other process parameters, and pass the annealing atmosphere to 1.
  • the preset temperature is taken as the highest temperature in the annealing process;
  • Step d start annealing: set the annealing time, and start annealing;
  • Step e take out the sample, after the microwave annealing is completed, keep a sufficient amount of argon gas for the microwave annealing
  • the furnace cavity continues to be purged, and after the temperature in the cavity cools down naturally, the microwave annealed substrate with the gallium oxide layer is taken out from the cavity.
  • Steps a to e are repeated to perform multiple annealing treatments on the gallium oxide layer at a plurality of different preset temperatures, thereby improving annealing efficiency and improving annealing quality.
  • gallium oxide material sample refers to a semiconductor sample having a substrate and a gallium oxide layer on the surface of the substrate.
  • the microwave annealing modification method for gallium oxide materials adopts the microwave annealing method to anneal the gallium oxide layer on the surface of the substrate, and controls the annealing temperature during the microwave annealing treatment (ie, preset temperature) is lower than the diffusion temperature, and the diffusion temperature is the lowest temperature at which thermal diffusion occurs between the gallium oxide material in the gallium oxide layer and the substrate, so as to avoid the traditional annealing method in the annealing process.
  • the problem of thermal diffusion between the gallium oxide layer and the substrate is easy to occur when the annealing temperature is too high, and the microwave annealing cost is low, thereby reducing the annealing treatment cost of the gallium oxide material and facilitating large-scale quantitative production.
  • FIG. 3 is the surface topography of the unannealed and microwave annealed gallium oxide films at different temperatures taken by atomic force microscopy (AFM).
  • ALD atomic force microscopy
  • the annealing temperature increased from 250 °C to 450 °C, the surface roughness of the gallium oxide film gradually increased, and the surface morphology gradually changed from a needle-like disordered amorphous structure to a condensed spherical granular crystalline structure, and the microcrystalline particles had The size increases gradually, indicating that the microwave annealing process indeed effectively changes the crystallization and microstructure of the gallium oxide films.

Abstract

The present invention relates to a microwave annealing and modification method for a gallium oxide material. The microwave annealing and modification method for a gallium oxide material comprises the following steps: providing a substrate, wherein there is a gallium oxide layer on a surface of the substrate; and performing, at a preset temperature, a microwave annealing treatment on the gallium oxide layer, wherein the preset temperature is lower than a diffusion temperature, and the diffusion temperature is the lowest temperature at which thermal diffusion occurs between a gallium oxide material in the gallium oxide layer and the substrate. By means of the present invention, the problem of thermal diffusion being prone to occurring between a gallium oxide layer and a substrate in an annealing process due to an over-high annealing temperature within an existing conventional annealing manner is prevented; and microwave annealing has low cost, thereby reducing the annealing treatment cost of a gallium oxide material and facilitating large-scale quantitative production.

Description

用于氧化镓材料的微波退火改性方法Microwave annealing modification method for gallium oxide materials 技术领域technical field
本发明涉及半导体制造技术领域，尤其涉及一种用于氧化镓材料的微波退火改性方法。The invention relates to the technical field of semiconductor manufacturing, in particular to a microwave annealing modification method for gallium oxide materials.
背景技术Background technique
氧化镓作为第三代宽带隙半导体材料，具有禁带宽度更大、击穿场强更高的优势。氧化镓材料的超宽禁带特点使其在大功率、高频器件的制造领域具有广泛的应用前景。As a third-generation wide-bandgap semiconductor material, gallium oxide has the advantages of larger band gap and higher breakdown field strength. The ultra-wide band gap characteristic of gallium oxide material makes it have broad application prospects in the field of high-power and high-frequency device manufacturing.
退火是半导体制程工程中用于对材料层进行改性的重要步骤。传统的退火工艺有管式炉退火、激光退火和快速热退火(RTP)等。其中，管式炉退火方式和快速热退火方式在退火工艺实施过程中，所需的温度较高，容易诱发热扩散效应，导致氧化镓薄膜材料与衬底之间发生扩散，这种扩散会严重影响最终器件的性能。而当前业界主要使用的激光退火方式则存在设备成本高、不利于大规模量产的缺点。Annealing is an important step in semiconductor process engineering for modifying layers of materials. Traditional annealing processes include tube furnace annealing, laser annealing and rapid thermal annealing (RTP). Among them, the tube furnace annealing method and the rapid thermal annealing method require high temperature during the implementation of the annealing process, which easily induces the thermal diffusion effect, resulting in the diffusion between the gallium oxide thin film material and the substrate, which will cause serious diffusion. affect the performance of the final device. However, the current laser annealing method mainly used in the industry has the disadvantages of high equipment cost and unfavorable mass production.
因此，如何避免氧化镓材料在退火过程中易发生热扩散的问题，提高最终形成的器件的性能，并且降低氧化镓材料的退火成本，是当前亟待解决的技术问题。Therefore, how to avoid the problem of thermal diffusion of gallium oxide materials during the annealing process, improve the performance of the final formed device, and reduce the annealing cost of gallium oxide materials is a technical problem that needs to be solved urgently.
发明内容SUMMARY OF THE INVENTION
本发明提供一种用于氧化镓材料的微波退火改性方法，用于解决现有技术在对氧化镓材料进行退火处理的过程中易发生热扩散的问题，以提高最终形成的半导体器件的性能，并降低氧化镓材料的退火成本。The invention provides a microwave annealing modification method for gallium oxide material, which is used to solve the problem that thermal diffusion is easy to occur in the process of annealing the gallium oxide material in the prior art, so as to improve the performance of the finally formed semiconductor device , and reduce the annealing cost of gallium oxide material.
为了解决上述问题，本发明提供了一种用于氧化镓材料的微波退火改性方法，包括如下步骤：In order to solve the above problems, the present invention provides a microwave annealing modification method for gallium oxide material, comprising the following steps:
提供一衬底，所述衬底表面具有由氧化镓层；providing a substrate, the surface of the substrate has a layer of gallium oxide;
在预设温度下对所述氧化镓层进行微波退火处理，所述预设温度低于扩散温度，所述扩散温度为所述氧化镓层中的氧化镓材料与所述衬底之间发生热扩散的最低温度。The gallium oxide layer is subjected to microwave annealing treatment at a preset temperature, the preset temperature being lower than a diffusion temperature, and the diffusion temperature is the heat generated between the gallium oxide material in the gallium oxide layer and the substrate Minimum temperature for diffusion.
可选的，在预设温度下对所述氧化镓层进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer at a preset temperature include:
设置多个预设温度，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理。A plurality of preset temperatures are set, and microwave annealing treatment is performed on the gallium oxide layer at each preset temperature in sequence.
可选的，多个所述预设温度按照从低温到高温的顺序排列；Optionally, the plurality of preset temperatures are arranged in order from low temperature to high temperature;
任意相邻两个所述预设温度之间的差值均相等；或者，The difference between any two adjacent preset temperatures is equal; or,
所述预设温度的温度越高，相邻所述预设温度之间的差值越小。The higher the temperature of the preset temperature, the smaller the difference between adjacent preset temperatures.
可选的，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer at each preset temperature in sequence include:
按照多个所述预设温度的高低顺序，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理。According to the order of the plurality of preset temperatures, microwave annealing is performed on the gallium oxide layer at each preset temperature in sequence.
可选的，在每一所述预设温度下对所述氧化镓层进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer at each preset temperature include:
放置所述衬底至微波退火炉腔体内，并对所述微波退火炉腔体进行抽真空处理；placing the substrate in the cavity of the microwave annealing furnace, and vacuumizing the cavity of the microwave annealing furnace;
以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理；performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature;
于所述微波退火炉腔体内冷却经所述微波退火处理的所述氧化镓层；cooling the gallium oxide layer treated by the microwave annealing in the microwave annealing furnace cavity;
自所述微波退火炉腔体取出具有所述氧化镓层的衬底。The substrate with the gallium oxide layer is taken out from the microwave annealer cavity.
可选的，以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理之前，还包括如下步骤：Optionally, before the microwave annealing treatment is performed on the gallium oxide layer with the preset temperature as the maximum temperature, the following steps are further included:
采用惰性气体对所述微波退火炉腔体进行吹扫，排除所述微波退火炉腔体内的杂质气体。The cavity of the microwave annealing furnace is purged with an inert gas to remove impurity gas in the cavity of the microwave annealing furnace.
可选的，以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature include:
设定微波退火参数并向所述微波退火炉腔体通入退火气氛，进行退火处理，所述微波退火参数中的最高退火温度为所述预设温度。Microwave annealing parameters are set and an annealing atmosphere is passed into the microwave annealing furnace cavity to perform annealing treatment, and the maximum annealing temperature in the microwave annealing parameters is the preset temperature.
可选的，所述退火气氛为氩气气氛或者氮气气氛。Optionally, the annealing atmosphere is an argon atmosphere or a nitrogen atmosphere.
可选的，于所述微波退火炉腔体内冷却经所述微波退火处理的所述氧化镓层的具体步骤包括：Optionally, the specific step of cooling the microwave annealed gallium oxide layer in the microwave annealing furnace cavity includes:
采用惰性气体对所述微波退火炉腔体进行吹扫，降低所述微波退火炉腔体的温度。The cavity of the microwave annealing furnace is purged with an inert gas to reduce the temperature of the cavity of the microwave annealing furnace.
可选的，所述预设温度为200℃-600℃。Optionally, the preset temperature is 200°C-600°C.
本发明提供的用于氧化镓材料的微波退火改性方法，采用微波退火处理的方法对衬底表面的氧化镓层进行退火处理，且控制微波退火处理过程中的退火温度(即预设温度)低于扩散温度，所述扩散温度为所述氧化镓层中的氧化镓材料与所述衬底之间发生热扩散的最低温度，从而避免了现有传统的退火方式在退火过程中因退火温度过高而易发生氧化镓层与衬底之间热扩散的问题，且微波退火成本低廉，从而降低了氧化镓材料的退火处理成本，利于大规模量化生产。In the microwave annealing modification method for gallium oxide material provided by the present invention, the gallium oxide layer on the surface of the substrate is annealed by the microwave annealing treatment method, and the annealing temperature (ie the preset temperature) during the microwave annealing treatment process is controlled. Lower than the diffusion temperature, the diffusion temperature is the lowest temperature at which thermal diffusion occurs between the gallium oxide material in the gallium oxide layer and the substrate, so as to avoid the existing traditional annealing method due to the annealing temperature during the annealing process. If it is too high, the problem of thermal diffusion between the gallium oxide layer and the substrate is likely to occur, and the microwave annealing cost is low, thereby reducing the annealing treatment cost of the gallium oxide material, which is conducive to large-scale quantitative production.
附图说明Description of drawings
附图1是本发明具体实施方式中用于氧化镓材料的微波退火改性方法的流程图；Accompanying drawing 1 is the flow chart of the microwave annealing modification method for gallium oxide material in the specific embodiment of the present invention;
附图2是本发明具体实施方式中具有氧化镓层的衬底的结构示意图。FIG. 2 is a schematic structural diagram of a substrate having a gallium oxide layer in an embodiment of the present invention.
附图3是利用原子力显微镜(AFM)拍摄的未退火和不同温度微波退火后的氧化镓薄膜的表面形貌图。FIG. 3 is the surface topography of the unannealed and microwave annealed gallium oxide films at different temperatures taken by atomic force microscopy (AFM).
具体实施方式Detailed ways
下面结合附图对本发明提供的用于氧化镓材料的微波退火改性方法的具体实施方式做详细说明。The specific embodiments of the microwave annealing modification method for gallium oxide material provided by the present invention will be described in detail below with reference to the accompanying drawings.
本具体实施方式提供了一种用于氧化镓材料的微波退火改性方法，附图1是本发明具体实施方式中用于氧化镓材料的微波退火改性方法的流程图，附图2是本发明具体实施方式中具有氧化镓层的衬底的结构示意图。如图1所示，本具体实施方式所述的用于氧化镓材料的微波退火改性方法，包括如下步骤：This specific embodiment provides a microwave annealing modification method for gallium oxide materials. FIG. 1 is a flow chart of the microwave annealing modification method for gallium oxide materials in the specific embodiment of the present invention, and FIG. 2 is the present invention. A schematic diagram of the structure of a substrate with a gallium oxide layer in the specific embodiment of the invention. As shown in FIG. 1 , the microwave annealing modification method for gallium oxide material described in this specific embodiment includes the following steps:
步骤S11，提供一衬底20，所述衬底20表面具有由氧化镓层21，如图2所示。In step S11 , a substrate 20 is provided, and the surface of the substrate 20 has a gallium oxide layer 21 , as shown in FIG. 2 .
在本具体实施方式中，所述衬底20的材料可以为Si、SiC或者GaN。所述氧化镓层21可以采用化学气相沉积工艺、物理气相沉积工艺或者原子层沉积工艺形成于所述衬底20表面。In this specific embodiment, the material of the substrate 20 may be Si, SiC or GaN. The gallium oxide layer 21 may be formed on the surface of the substrate 20 by a chemical vapor deposition process, a physical vapor deposition process or an atomic layer deposition process.
步骤S12，在预设温度下对所述氧化镓层21进行微波退火处理，所述预设温度低于扩散温度，所述扩散温度为所述氧化镓层21中的氧化镓材料与所述衬底20之间发生热扩散的最低温度。Step S12, microwave annealing is performed on the gallium oxide layer 21 at a preset temperature, where the preset temperature is lower than a diffusion temperature, and the diffusion temperature is the gallium oxide material in the gallium oxide layer 21 and the lining The lowest temperature at which thermal diffusion occurs between the bottoms 20 .
具体来说，微波退火的本质是直接以微波对叠层结构(即由所述衬底20与所述氧化镓层21构成的叠层结构)进行加热。微波场的存在降低了氧化镓材料晶粒间界的结晶活化能，使得无定形氧化镓层21薄膜在较低温条件下(即低于所述扩散温度的所述预设温度条件下)退火就能形成晶核并快速结晶，同时较低温条件有效控制了元素的相互扩散效应，最终制备得到界面扩散少的氧化镓薄膜。相比于传统退火技术，采用微波退火技术不仅可以有效降低热预算，避免热扩散效应，达到低温退火的效果，而且其退火效率也更高。Specifically, the essence of microwave annealing is to directly heat the stacked structure (ie, the stacked structure composed of the substrate 20 and the gallium oxide layer 21 ) with microwaves. The presence of the microwave field reduces the crystallization activation energy of the grain boundaries of the gallium oxide material, so that the amorphous gallium oxide layer 21 film can be annealed at a lower temperature (ie, under the preset temperature condition lower than the diffusion temperature). The crystal nucleus can be formed and crystallized rapidly, and the interdiffusion effect of elements can be effectively controlled under lower temperature conditions, and a gallium oxide film with less interface diffusion can be finally prepared. Compared with the traditional annealing technology, the microwave annealing technology can not only effectively reduce the thermal budget, avoid the thermal diffusion effect, and achieve the effect of low temperature annealing, but also its annealing efficiency is higher.
可选的，在预设温度下对所述氧化镓层21进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at a preset temperature include:
设置多个预设温度，依次在每一所述预设温度下对所述氧化镓层21进行微波退火处理。A plurality of preset temperatures are set, and microwave annealing treatment is performed on the gallium oxide layer 21 at each preset temperature in sequence.
具体来说，为了进一步提高微波退火处理的效果，可以预先设置多个互不相同的所述预设温度，以所述预设温度作为微波退火过程中的最高温度，依次在每一所述预设温度条件下对所述氧化镓层21进行微波退火处理。所述最高温度是指，在微波退火处理的过程中，微波退火炉腔体所升到的最高温度。Specifically, in order to further improve the effect of the microwave annealing treatment, a plurality of the preset temperatures that are different from each other can be preset, and the preset temperature is used as the highest temperature in the microwave annealing process. The gallium oxide layer 21 is subjected to microwave annealing treatment under the condition of temperature. The maximum temperature refers to the maximum temperature that the cavity of the microwave annealing furnace rises to during the microwave annealing process.
可选的，多个所述预设温度按照从低温到高温的顺序排列；Optionally, the plurality of preset temperatures are arranged in order from low temperature to high temperature;
任意相邻两个所述预设温度之间的差值均相等；或者，The difference between any two adjacent preset temperatures is equal; or,
所述预设温度的温度越高，相邻所述预设温度之间的差值越小。The higher the temperature of the preset temperature, the smaller the difference between adjacent preset temperatures.
具体来说，多个所述预设温度的具体数值，本领域技术人员可以根据实际需要进行设置，例如根据所需要的退火后所述氧化镓层21的物理性质要求进行设置。为了简化预设温度的设定步骤，可以设置多个按照从低到高呈等差数列排布的所述预设温度。相邻所述预设温度之间的差值可以为50℃、100℃或者其他数值。Specifically, those skilled in the art can set the specific values of the plurality of preset temperatures according to actual needs, for example, according to the required physical property requirements of the gallium oxide layer 21 after annealing. In order to simplify the step of setting the preset temperature, a plurality of the preset temperatures may be set in an arithmetic progression from low to high. The difference between adjacent preset temperatures may be 50° C., 100° C. or other values.
为了进一步提高微波退火的效率，多个所述预设温度按照从低温到高温的顺序排列，且所述预设温度的温度越高，相邻所述预设温度之间的差值越小。In order to further improve the efficiency of microwave annealing, a plurality of the preset temperatures are arranged in order from low temperature to high temperature, and the higher the temperature of the preset temperature, the smaller the difference between adjacent preset temperatures.
可选的，依次在每一所述预设温度下对所述氧化镓层21进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at each preset temperature in sequence include:
按照多个所述预设温度的高低顺序，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理。According to the order of the plurality of preset temperatures, microwave annealing is performed on the gallium oxide layer at each preset temperature in sequence.
举例来说，按照多个所述预设温度从低温到高温的顺序，依次在每一个所述预设温度下对所述氧化镓层进行微波退火处理。本具体实施方式中的多个是指两个及两个以上。For example, according to the sequence of the plurality of preset temperatures from low temperature to high temperature, microwave annealing is performed on the gallium oxide layer at each of the preset temperatures in turn. The plural in this specific embodiment refers to two or more.
可选的，在每一所述预设温度下对所述氧化镓层21进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at each preset temperature include:
放置所述衬底至微波退火炉腔体内，并对所述微波退火炉腔体进行抽真空处理；placing the substrate in the cavity of the microwave annealing furnace, and vacuumizing the cavity of the microwave annealing furnace;
以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理；performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature;
于所述微波退火炉腔体内冷却经所述微波退火处理的所述氧化镓层；cooling the gallium oxide layer treated by the microwave annealing in the microwave annealing furnace cavity;
自所述微波退火炉腔体取出具有所述氧化镓层的衬底。The substrate with the gallium oxide layer is taken out from the microwave annealer cavity.
可选的，以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理之前，还包括如下步骤：Optionally, before the microwave annealing treatment is performed on the gallium oxide layer with the preset temperature as the maximum temperature, the following steps are further included:
采用惰性气体对所述微波退火炉腔体进行吹扫，排除所述微波退火炉腔体内的杂质气体。The cavity of the microwave annealing furnace is purged with an inert gas to remove impurity gas in the cavity of the microwave annealing furnace.
可选的，以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理的具体步骤包括：Optionally, the specific steps of performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature include:
设定微波退火参数并向所述微波退火炉腔体通入退火气氛，进行退火处理，所述微波退火参数中的最高退火温度为所述预设温度。Microwave annealing parameters are set and an annealing atmosphere is passed into the microwave annealing furnace cavity to perform annealing treatment, and the maximum annealing temperature in the microwave annealing parameters is the preset temperature.
具体来说，在微波退火处理的过程中，微波退火炉腔体内的温度是逐渐升高的，本具体实施方式以所述预设温度作为微波退火处理的最高温度是指，在单次微波退火处理的过程中，所述微波退火炉腔体内部所能升到的最高温度。在所述微波退火炉腔体升到所述预设温度之后，保持所述预设温度一预设时间，实现对所述氧化镓层的微波退火处理。所述预设时间为预先设置的退火时长。Specifically, during the microwave annealing process, the temperature in the cavity of the microwave annealing furnace is gradually increased. In this specific embodiment, the preset temperature is used as the maximum temperature of the microwave annealing process, which means that in a single microwave annealing process During the treatment process, the maximum temperature that can be raised inside the microwave annealing furnace cavity. After the microwave annealing furnace cavity is raised to the preset temperature, the preset temperature is maintained for a preset time, so as to realize the microwave annealing treatment of the gallium oxide layer. The preset time is a preset annealing duration.
可选的，所述退火气氛为氩气气氛或者氮气气氛。Optionally, the annealing atmosphere is an argon atmosphere or a nitrogen atmosphere.
可选的，于所述微波退火炉腔体内冷却经所述微波退火处理的所述氧化镓层的具体步骤包括：Optionally, the specific step of cooling the microwave annealed gallium oxide layer in the microwave annealing furnace cavity includes:
采用惰性气体对所述微波退火炉腔体进行吹扫，降低所述微波退火炉腔体的温度。The cavity of the microwave annealing furnace is purged with an inert gas to reduce the temperature of the cavity of the microwave annealing furnace.
可选的，所述预设温度为200℃-600℃。Optionally, the preset temperature is 200°C-600°C.
举例来说，在预设温度下对所述氧化镓层21进行微波退火处理的具体步骤包括：步骤a，放置样品：将具有所述氧化镓层21的所述衬底20放入微波退火炉腔体的中间位置，关闭腔门，然后对所述微波退火炉腔体进行抽真空处理；步骤b，腔体吹扫：先利用足量的氩气对所述微波退火炉腔体进行吹扫和清理，以排除所述微波退火炉腔体内部和腔体内壁上残留的氧气，并保持氩气吹扫状态一段时间，本步骤中足量的氩气是指能够将微波退火炉腔体内部和腔体内壁上残留的氧气彻底排尽的氩气的量；步骤c，设定退火参数：设定退火功率、退火过程中最高温度、退火温度台阶等工艺参数，并通入退火气氛，以一所述预设温度作为退火过程中的最高温度；步骤d，开始退火：设定退火时长，开始退火；步骤e：取出样品，微波退火结束后，保持足量的氩气对所述微波退火炉腔体继续进行吹扫，待腔内温度自然冷却，然后从腔体内拿出经微波退火处理的具有氧化镓层的所述衬底。重复步骤a-步骤e，从而在多个不同的所述预设温度下对所述氧化镓层进行多次退火处理，从而提高退火效率，改善退火质量。For example, the specific steps of performing microwave annealing treatment on the gallium oxide layer 21 at a preset temperature include: step a, placing a sample: placing the substrate 20 with the gallium oxide layer 21 in a microwave annealing furnace In the middle position of the cavity, close the cavity door, and then vacuumize the microwave annealing furnace cavity; step b, cavity purging: first use a sufficient amount of argon to purge the microwave annealing furnace cavity and cleaning to remove the residual oxygen in the cavity of the microwave annealing furnace and on the inner wall of the cavity, and keep the argon gas purged for a period of time. and the amount of argon that is completely exhausted from the residual oxygen on the inner wall of the cavity; step c, set annealing parameters: set the annealing power, the highest temperature during the annealing process, the annealing temperature steps and other process parameters, and pass the annealing atmosphere to 1. The preset temperature is taken as the highest temperature in the annealing process; Step d, start annealing: set the annealing time, and start annealing; Step e: take out the sample, after the microwave annealing is completed, keep a sufficient amount of argon gas for the microwave annealing The furnace cavity continues to be purged, and after the temperature in the cavity cools down naturally, the microwave annealed substrate with the gallium oxide layer is taken out from the cavity. Steps a to e are repeated to perform multiple annealing treatments on the gallium oxide layer at a plurality of different preset temperatures, thereby improving annealing efficiency and improving annealing quality.
在其他具体实施方式中，本领域技术人员还可根据实际需要，通过更换氧化镓材料样品，并重复步骤a-步骤e，达到对氧化镓材料样品批量退火处理的效果。所述氧化镓材料样品是指具有衬底以及位于衬底表面的氧化镓层的半导体样品。In other specific embodiments, those skilled in the art can also achieve the effect of batch annealing treatment of gallium oxide material samples by replacing gallium oxide material samples and repeating steps a to e according to actual needs. The gallium oxide material sample refers to a semiconductor sample having a substrate and a gallium oxide layer on the surface of the substrate.
本具体实施方式提供的用于氧化镓材料的微波退火改性方法，采用微波退火处理的方法对衬底表面的氧化镓层进行退火处理，且控制微波退火处理过程中的退火温度(即预设温度)低于扩散温度，所述扩散温度为所述氧化镓层中的氧化镓材料与所述衬底之间发生热扩散的最低温度，从而避免了现有传统的退火方式在退火过程中因退火温度过高而易发生氧化镓层与衬底之间热扩散的问题，且微波退火成本低廉，从而降低了氧化镓材料的退火处理成本，利于大规模量化生产。The microwave annealing modification method for gallium oxide materials provided by this specific embodiment adopts the microwave annealing method to anneal the gallium oxide layer on the surface of the substrate, and controls the annealing temperature during the microwave annealing treatment (ie, preset temperature) is lower than the diffusion temperature, and the diffusion temperature is the lowest temperature at which thermal diffusion occurs between the gallium oxide material in the gallium oxide layer and the substrate, so as to avoid the traditional annealing method in the annealing process. The problem of thermal diffusion between the gallium oxide layer and the substrate is easy to occur when the annealing temperature is too high, and the microwave annealing cost is low, thereby reducing the annealing treatment cost of the gallium oxide material and facilitating large-scale quantitative production.
附图3是利用原子力显微镜(AFM)拍摄的未退火和不同温度微波退火后的氧化镓薄膜的表面形貌图。对氧化镓样品退火前后进行形貌表征，对未退火的氧化镓薄膜以及分别经过250、350和450℃的微波退火后的氧化镓薄膜， 利用原子力显微镜对经不同处理的薄膜的表面微结构形貌进行了测试，如图3所示。可以看出，ALD生长的氧化镓薄膜为非晶的无序结构，如图3中a所示，表面粗糙度小。随着退火温度由250℃增加到450℃，氧化镓薄膜表面粗糙度逐渐增加，表面形貌由针尖状无序的非晶结构逐渐变为凝结的小球颗粒状结晶结构，且微结晶颗粒的尺寸逐步增加，说明微波退火过程确实有效地改变了氧化镓薄膜的结晶和微结构。FIG. 3 is the surface topography of the unannealed and microwave annealed gallium oxide films at different temperatures taken by atomic force microscopy (AFM). The morphology of the gallium oxide samples before and after annealing was characterized. For the unannealed gallium oxide thin films and the gallium oxide thin films after microwave annealing at 250, 350 and 450 °C, respectively, the surface microstructures of the films treated with different treatments were analyzed by atomic force microscopy. The appearance was tested, as shown in Figure 3. It can be seen that the gallium oxide film grown by ALD has an amorphous disordered structure, as shown in a in Figure 3, with small surface roughness. As the annealing temperature increased from 250 °C to 450 °C, the surface roughness of the gallium oxide film gradually increased, and the surface morphology gradually changed from a needle-like disordered amorphous structure to a condensed spherical granular crystalline structure, and the microcrystalline particles had The size increases gradually, indicating that the microwave annealing process indeed effectively changes the crystallization and microstructure of the gallium oxide films.
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above are only the preferred embodiments of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications can also be made, and these improvements and modifications should also be regarded as It is the protection scope of the present invention.

Claims (10)

  1. 一种用于氧化镓材料的微波退火改性方法，其特征在于，包括如下步骤：A kind of microwave annealing modification method for gallium oxide material, is characterized in that, comprises the following steps:
    提供一衬底，所述衬底表面具有由氧化镓层；providing a substrate, the surface of the substrate has a layer of gallium oxide;
    在预设温度下对所述氧化镓层进行微波退火处理，所述预设温度低于扩散温度，所述扩散温度为所述氧化镓层中的氧化镓材料与所述衬底之间发生热扩散的最低温度。The gallium oxide layer is subjected to microwave annealing treatment at a preset temperature, the preset temperature being lower than a diffusion temperature, and the diffusion temperature is the heat generated between the gallium oxide material in the gallium oxide layer and the substrate Minimum temperature for diffusion.
  2. 根据权利要求1所述的用于氧化镓材料的微波退火改性方法，其特征在于，在预设温度下对所述氧化镓层进行微波退火处理的具体步骤包括：The microwave annealing modification method for gallium oxide material according to claim 1, wherein the specific step of performing microwave annealing treatment on the gallium oxide layer at a preset temperature comprises:
    设置多个预设温度，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理。A plurality of preset temperatures are set, and microwave annealing treatment is performed on the gallium oxide layer at each preset temperature in sequence.
  3. 根据权利要求2所述的用于氧化镓材料的微波退火改性方法，其特征在于，多个所述预设温度按照从低温到高温的顺序排列；The microwave annealing modification method for gallium oxide material according to claim 2, wherein the plurality of preset temperatures are arranged in order from low temperature to high temperature;
    任意相邻两个所述预设温度之间的差值均相等；或者，The difference between any two adjacent preset temperatures is equal; or,
    所述预设温度的温度越高，相邻所述预设温度之间的差值越小。The higher the temperature of the preset temperature, the smaller the difference between adjacent preset temperatures.
  4. 根据权利要求2所述的用于氧化镓材料的微波退火改性方法，其特征在于，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理的具体步骤包括：The microwave annealing modification method for gallium oxide material according to claim 2, wherein the specific step of performing microwave annealing treatment on the gallium oxide layer at each preset temperature in sequence comprises:
    按照多个所述预设温度的高低顺序，依次在每一所述预设温度下对所述氧化镓层进行微波退火处理。According to the order of the plurality of preset temperatures, microwave annealing is performed on the gallium oxide layer at each preset temperature in sequence.
  5. 根据权利要求2所述的用于氧化镓材料的微波退火改性方法，其特征在于，在每一所述预设温度下对所述氧化镓层进行微波退火处理的具体步骤包括：The microwave annealing modification method for gallium oxide material according to claim 2, wherein the specific step of performing microwave annealing treatment on the gallium oxide layer at each preset temperature comprises:
    放置所述衬底至微波退火炉腔体内，并对所述微波退火炉腔体进行抽真空处理；placing the substrate in the cavity of the microwave annealing furnace, and vacuumizing the cavity of the microwave annealing furnace;
    以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理；performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature;
    于所述微波退火炉腔体内冷却经所述微波退火处理的所述氧化镓层；cooling the gallium oxide layer treated by the microwave annealing in the microwave annealing furnace cavity;
    自所述微波退火炉腔体取出具有所述氧化镓层的衬底。The substrate with the gallium oxide layer is taken out from the microwave annealer cavity.
  6. 根据权利要求5所述的用于氧化镓材料的微波退火改性方法，其特征在于， 以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理之前，还包括如下步骤：The microwave annealing modification method for gallium oxide material according to claim 5, wherein before the microwave annealing treatment is performed on the gallium oxide layer with the preset temperature as the maximum temperature, the method further comprises the following steps:
    采用惰性气体对所述微波退火炉腔体进行吹扫，排除所述微波退火炉腔体内的杂质气体。The cavity of the microwave annealing furnace is purged with an inert gas to remove impurity gas in the cavity of the microwave annealing furnace.
  7. 根据权利要求5所述的用于氧化镓材料的微波退火改性方法，其特征在于，以所述预设温度作为最高温度对所述氧化镓层进行微波退火处理的具体步骤包括：The microwave annealing modification method for gallium oxide material according to claim 5, wherein the specific step of performing microwave annealing treatment on the gallium oxide layer with the preset temperature as the maximum temperature comprises:
    设定微波退火参数并向所述微波退火炉腔体通入退火气氛，进行退火处理，所述微波退火参数中的最高退火温度为所述预设温度。Microwave annealing parameters are set and an annealing atmosphere is passed into the microwave annealing furnace cavity to perform annealing treatment, and the maximum annealing temperature in the microwave annealing parameters is the preset temperature.
  8. 根据权利要求5所述的用于氧化镓材料的微波退火改性方法，其特征在于，所述退火气氛为氩气气氛或者氮气气氛。The microwave annealing modification method for gallium oxide material according to claim 5, wherein the annealing atmosphere is an argon atmosphere or a nitrogen atmosphere.
  9. 根据权利要求5所述的用于氧化镓材料的微波退火改性方法，其特征在于，于所述微波退火炉腔体内冷却经所述微波退火处理的所述氧化镓层的具体步骤包括：The microwave annealing modification method for gallium oxide material according to claim 5, wherein the specific step of cooling the gallium oxide layer after the microwave annealing treatment in the microwave annealing furnace cavity comprises:
    采用惰性气体对所述微波退火炉腔体进行吹扫，降低所述微波退火炉腔体的温度。The cavity of the microwave annealing furnace is purged with an inert gas to reduce the temperature of the cavity of the microwave annealing furnace.
  10. 根据权利要求1所述的用于氧化镓材料的微波退火改性方法，其特征在于，所述预设温度为200℃-600℃。The microwave annealing modification method for gallium oxide material according to claim 1, wherein the preset temperature is 200°C-600°C.
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