WO2023087544A1 - Epitaxial structure of n-polar surface algan-based ultraviolet photoelectric detector, and preparation method for epitaxial structure - Google Patents
Epitaxial structure of n-polar surface algan-based ultraviolet photoelectric detector, and preparation method for epitaxial structure Download PDFInfo
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
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- H01L31/03046—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds including ternary or quaternary compounds, e.g. GaAlAs, InGaAs, InGaAsP
- H01L31/03048—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds including ternary or quaternary compounds, e.g. GaAlAs, InGaAs, InGaAsP comprising a nitride compounds, e.g. InGaN
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- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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Definitions
- the invention relates to the technical field of photoelectric device detectors, in particular to an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector and a preparation method thereof.
- Group III nitride materials represented by GaN are hot materials for new-generation optoelectronic devices. Due to their wide band gap, fast working speed, excellent electrical and thermal conductivity and extremely low loss, they are regarded It is an excellent alternative material to realize the miniaturization of high-performance optoelectronic devices.
- the epitaxial structure of the traditional metal-polar AlGaN photodetector is limited by defects such as weak high-temperature thermal stability and the influence of the internal polarization electric field of the material.
- Polar AlGaN materials are considered as alternative materials for traditional metallic polar AlGaN-based photodetectors. Since AlGaN on the N-polar surface has an opposite built-in electric field direction and a more active surface state than the traditional metal polar surface, the growth of AlGaN materials on the N-polar surface cannot effectively improve its surface quality at this stage.
- the present invention provides an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector and a preparation method thereof.
- the N-polar surface AlGaN ultraviolet photodetector has a large working responsivity and high sensitivity.
- the first object of the present invention is to provide an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector.
- the second object of the present invention is to provide a method for preparing an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector.
- the non-doped N-polar surface AlN buffer layer includes a low-temperature growth non-doped N-polar surface AlN buffer layer and a high-temperature growth non-doped N-polar surface AlN buffer layer, and the low-temperature growth non-doped N A polar AlN buffer layer is grown on the silicon substrate, and the high-temperature grown non-doped N-polar AlN buffer layer is grown on the low-temperature grown non-doped N-polar AlN buffer layer.
- the thickness of the low-temperature-grown non-doped N-polar AlN buffer layer is 100-150 nm, and the thickness of the high-temperature-grown non-doped N-polar AlN buffer layer is 250-380 nm.
- the thickness of the carbon-doped semi-insulating N-polar AlN buffer layer is 380-440 nm, and the doping concentration is 6.0 ⁇ 10 17 to 4.0 ⁇ 10 18 cm -3 .
- the thickness of the carbon-doped N polar surface graded AlyGa 1-y N buffer layer is 480-630 nm, and the doping concentration is 5.0 ⁇ 10 16 to 2.0 ⁇ 10 17 cm -3 .
- the thickness of the non-doped N polar surface AlxGa1 -xN layer is 300-450nm.
- the silicon substrate is a single crystal silicon substrate, the Si (111) close-packed plane is used as the epitaxial plane, and the AlN [0001] direction is used as the epitaxial growth direction of the material.
- a method for preparing an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector comprising:
- the silicon substrate is placed in a vacuum chamber, and a non-doped N-polar surface AlN buffer layer is epitaxially grown on the silicon substrate, thereby preparing an N-polar surface AlN sample;
- N-polar AlN sample into the growth chamber, and feed NH 3 , N 2 , H 2 , CH 4 and trimethylaluminum into the chamber.
- the temperature of the chamber is lowered, and trimethylgallium is introduced into the chamber at the same time, and the carbon-doped semi-insulating N-polar AlN buffer layer is In-situ growth of carbon-doped N polar surface composition graded AlGaN buffer layer on the layer;
- the gas path of CH4 is closed, and the temperature of the chamber is increased.
- the non-doped N-polar AlGaN layer is grown in situ on the surface composition graded AlGaN buffer layer, and the change of the Al composition of the film is regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
- the epitaxial growth of the non-doped N-polar surface AlN buffer layer on the silicon substrate, thereby preparing the N-polar surface AlN sample specifically includes:
- the silicon substrate is grown under N-rich conditions at a low temperature to grow an AlN buffer layer on a non-doped N polar surface, and the Al source is an AlN high-purity ceramic target;
- the temperature of the system is increased, and the vacuum degree, laser energy, laser frequency and nitrogen flow in the cavity are kept constant.
- a high-temperature non-doped N-polar surface AlN buffer layer is grown on the N-polar surface AlN buffer layer to prepare an N-polar surface AlN sample.
- the silicon substrate is a single crystal silicon substrate, the Si(111) close-packed plane is used as the epitaxial plane, and the AlN [0001] direction is used as the material epitaxial growth direction.
- the present invention has the following beneficial effects:
- the N-polar surface AlGaN ultraviolet photodetector epitaxial structure provided by the present invention grows a layer of carbon-doped step-type N-polar AlGaN film under the non-doped N-polar surface AlGaN layer, by enhancing the carrier The mobility can effectively increase the photocurrent generation of non-doped N-polar AlGaN thin films, and enhance the power and detectability of AlGaN-based ultraviolet detectors.
- the present invention uses N-polarity AlGaN as the basic material of the device. Compared with metal-polarity AlGaN materials, it can effectively improve the high-temperature stability of the device structure, reduce the influence of the internal polarization electric field of AlGaN, and effectively improve the ultraviolet photoelectric detection. The photoelectric responsivity of the device and effectively reduce the difficulty of subsequent device processing.
- the present invention adopts the two-step growth method of low-temperature pulsed laser deposition combined with high-temperature MOCVD to grow the materials required for the epitaxial structure of AlGaN ultraviolet photodetectors on the N-polar surface, and through the structural design of the step-by-step AlGaN epitaxial buffer layer, it can Effectively suppress the reflow etching reaction between the III-nitride and the silicon substrate at high temperature, and the large lattice mismatch between the heterostructures, thereby reducing the dislocation density of the N-polar AlGaN epitaxial layer grown by high-temperature MOCVD and surface roughness.
- FIG. 1 is a schematic diagram of an epitaxial structure of an AlGaN ultraviolet photodetector on an N-polar plane according to an embodiment of the present invention.
- Fig. 2 is an atomic force microscope image of the surface morphology of an N-polarity AlGaN epitaxial wafer according to an embodiment of the present invention.
- FIG. 3 is an X-ray rocking curve test chart of an N-polarity AlGaN (0002) thin film according to an embodiment of the present invention.
- 1-Silicon substrate 2-Low temperature growth of non-doped N-polar surface AlN buffer layer, 3-High temperature growth of non-doped N-polar surface AlN buffer layer, 4-Carbon doped semi-insulating N-polar AlN buffer layer , 5-carbon-doped N-polar surface composition graded AlGaN buffer layer, 6-non-doped N-polar surface AlGaN layer.
- This embodiment provides a method for preparing an epitaxial structure of an AlGaN ultraviolet photodetector with an N-polar surface, the method comprising:
- the silicon substrate is a single crystal silicon substrate, the Si(111) close-packed surface is used as the epitaxial surface, and the AlN [0001] direction is used as the epitaxial growth direction of the material;
- the silicon substrate is placed in a vacuum chamber, the temperature is raised to 420-500°C, the vacuum in the chamber is pumped to 2.0 ⁇ 10 -4 to 4.0 ⁇ 10 -4 torr, and the laser energy is 250 ⁇ 320mJ, laser frequency 15 ⁇ 30Hz, nitrogen flow rate 2 ⁇ 10sccm, grow N-polar AlN film under N-rich conditions, Al source is AlN high-purity ceramic target;
- the temperature is increased to 850°C, and the vacuum degree, laser energy, laser frequency and nitrogen flow in the cavity are kept constant, and the high-temperature N-polar AlN film is epitaxially grown on the N-polar AlN film.
- the prepared N-polar AlN sample is placed in the growth chamber, and the chamber is vacuumed to 2.0 ⁇ 10 -6 ⁇ 4.0 ⁇ 10 -6 torr, The temperature is raised to 1000-1100°C, and NH 3 , N 2 , H 2 , CH 4 and trimethylaluminum are introduced into the chamber to epitaxially grow on the epitaxial wafer of the high-temperature non-doped N-polar surface AlN buffer layer Carbon-doped semi-insulating N-polar AlN buffer layer; during vapor deposition, the pressure in the reaction chamber is 180-220torr, and the flow rates of NH 3 , H 2 , CH 4 , and trimethylaluminum are 30-50slm, 60-100slm, and 10 ⁇ 20slm and 350 ⁇ 440sccm;
- MOCVD technology metal organic compound chemical vapor deposition growth method
- the temperature of the chamber is lowered to 770-800°C, and at the same time, trimethylgallium is introduced into the chamber to in-situ grow carbon-doped Gradient AlGaN buffer layer on the N polar surface;
- the pressure of the reaction chamber in vapor deposition is 180-240torr, and the flow rates of NH 3 , H 2 , CH 4 , trimethylaluminum and trimethylgallium are 30-50slm and 60-100slm respectively , 15 ⁇ 24slm, 400 ⁇ 450sccm and 100 ⁇ 150sccm;
- the reaction chamber pressure is 180-240 torr
- the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 30-50slm, 60-100slm, 400-450sccm and 100-150sccm, respectively.
- the epitaxial structure of the N-polar surface AlGaN ultraviolet photodetector prepared in this embodiment is shown in FIG. 1 .
- a method for preparing an epitaxial structure of an AlGaN-based ultraviolet photodetector on an N-polar surface is specifically as follows:
- Substrate surface cleaning Put the silicon substrate into acetone, absolute ethanol, and deionized water in sequence, and ultrasonically clean it for 5 minutes in sequence. After taking it out, rinse it with deionized water and dry it with hot high-purity nitrogen;
- step (6) Epitaxial growth of carbon-doped N polar surface composition graded AlyGa 1-y N layer: After completing step (5) film growth in MOCVD, lower the chamber temperature to 780°C, Through trimethylgallium, the carbon-doped N polar surface composition graded AlGaN buffer layer is grown in situ on the epitaxial wafer.
- the pressure of the reaction chamber is 210torr
- step (6) Epitaxial growth of non-doped N-polar Al x Ga 1-x N layer: After the film growth in step (6) is completed in MOCVD, the gas path of CH 4 is closed, and the temperature of the chamber is raised to 830°C. The non-doped N-polar AlGaN layer is grown in situ on the epitaxial wafer. In the vapor phase deposition, the reaction chamber pressure is 210torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 40slm, 80slm, 430sccm, and 120sccm, respectively. At the same time, the change of the Al composition of the film layer was regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
- the N-polar surface AlGaN ultraviolet photodetector epitaxial structure obtained in this embodiment includes non-doped N-polar surface AlN buffer layers (including low-temperature growth of non-doped N-polar surface AlN buffer layers) grown sequentially on the silicon substrate 1.
- Layer 2 and high temperature growth non-doped N polar face AlN buffer layer 3 carbon doped N polar face AlN layer 4, carbon doped N polar face composition graded A y Ga 1-y N buffer layer 5 and Non-doped N polar surface AlxGa1 -xN layer 6; wherein, the buffer layer of the non-doped N polar surface AlN layer is 420nm, wherein the thickness of the low-temperature growth non-doped N polar surface AlN buffer layer is 120nm, The thickness of the non-doped N polar surface AlN buffer layer grown at high temperature is 300nm, the thickness of the carbon doped N polar surface AlN layer is 380nm, and the doping concentration is 2.0 ⁇ 10 18 cm -3 ; the carbon doped N polar surface component Gradient Al y Ga 1-y N (the value of y changes from 0.95 to 0.75 from bottom to top) buffer layer thickness is 500nm, doping concentration is 1.5 ⁇ 10 17 cm -3 ; non-doped N polar
- the epitaxial structure of the N polar surface AlGaN ultraviolet photodetector prepared in this example is shown in Figure 1.
- the AFM characterization of the surface of the AlGaN thin film is shown in Figure 2. It can be seen that the surface quality is good; the N pole See Figure 3 for the test results of the X-ray rocking curve of the AlGaN (0002) thin film. It can be seen that the crystal quality of the thin film is good.
- a method for preparing an epitaxial structure of an AlGaN-based ultraviolet photodetector on an N-polar surface is specifically as follows:
- Substrate surface cleaning Put the silicon substrate into acetone, absolute ethanol, and deionized water in sequence, and ultrasonically clean it for 5 minutes in sequence. After taking it out, rinse it with deionized water and dry it with hot high-purity nitrogen;
- step (6) Epitaxial growth of carbon-doped N polar surface composition graded AlyGa 1-y N layer: After completing step (5) film growth in MOCVD, lower the chamber temperature to 780°C, Through trimethylgallium, the carbon-doped N polar surface composition graded AlGaN buffer layer is grown in situ on the epitaxial wafer.
- the reaction chamber pressure is 210torr
- step (6) Epitaxial growth of non-doped N-polar Al x Ga 1-x N layer: After the film growth in step (6) is completed in MOCVD, the gas path of CH 4 is closed, and the temperature of the chamber is raised to 830°C. The non-doped N-polar AlGaN layer is grown in situ on the epitaxial wafer. In the vapor phase deposition, the reaction chamber pressure is 210torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 40slm, 80slm, 430sccm, and 120sccm, respectively. At the same time, the change of the Al composition of the film layer was regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
- a method for preparing an epitaxial structure of an AlGaN-based ultraviolet photodetector on an N-polar surface is specifically as follows:
- Substrate surface cleaning Put the silicon substrate into acetone, absolute ethanol, and deionized water in sequence, and ultrasonically clean it for 5 minutes in sequence. After taking it out, rinse it with deionized water and dry it with hot high-purity nitrogen;
- step (6) Epitaxial growth of carbon-doped N polar surface composition graded AlyGa 1-y N layer: After completing step (5) film growth in MOCVD, lower the chamber temperature to 780°C, Through trimethylgallium, the carbon-doped N polar surface composition graded AlGaN buffer layer is grown in situ on the epitaxial wafer.
- the pressure of the reaction chamber is 210torr
- step (6) Epitaxial growth of non-doped N-polar Al x Ga 1-x N layer: After completing step (6) film growth in MOCVD, close the gas path of CH 4 , raise the chamber temperature to 850°C, and The non-doped N-polar AlGaN layer is grown in situ on the epitaxial wafer.
- the pressure of the reaction chamber is 240torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 50slm, 100slm, 450sccm, and 120sccm, respectively.
- the change of the Al composition of the film layer was regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
- the N-polar surface AlGaN ultraviolet photodetector epitaxial structure obtained in this embodiment includes a non-doped N-polar surface AlN layer buffer layer, a carbon-doped N-polar surface AlN layer, a carbon-doped N-polar surface AlN layer, and a carbon-doped
- the hetero-N polar surface composition graded Al y Ga 1-y N buffer layer (from bottom to top y 0.95 ⁇ 0.75) and the non-doped N polar surface Al x Ga 1-x N layer; the non-doped
- the buffer layer of the AlN layer on the N polar surface is 500nm, and the thickness of the AlN buffer layer on the non-doped N polar surface grown at low temperature is 150nm, and the thickness of the AlN buffer layer on the high temperature grown non-doped N polar surface is 350nm;
- the thickness of the AlN layer on the surface is 400nm, and the doping concentration is 2.0 ⁇ 10 18 cm -3 ; the carbon-doped
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Abstract
Disclosed in the present invention are an epitaxial structure of an N-polar surface AlGaN-based ultraviolet photoelectric detector, and a preparation method for the epitaxial structure. The epitaxial structure of an N-polar surface AlGaN-based ultraviolet photoelectric detector comprises: a non-doped N-polar surface AlN buffer layer, a carbon-doped semi-insulated N-polar AlN buffer layer, a carbon-doped N-polar surface composition-gradient AlyGa1-yN buffer layer and a non-doped N-polar surface AlxGa1-xN layer, which are sequentially grown on a silicon substrate, wherein x = 0.5-0.8, and y = 0.75-0.95. By means of the epitaxial structure of an N-polar surface AlGaN-based ultraviolet photoelectric detector provided in the present invention, the power and detection rate of an AlGaN-based ultraviolet detector are enhanced, thereby increasing a photoelectric response degree of the ultraviolet photoelectric detector, and effectively reducing the subsequent machining difficulty in a device. By means of the preparation method provided in the present invention, the dislocation density and surface roughness of an N-polar AlGaN epitaxial layer, which is grown by means of high-temperature MOCVD, are reduced.
Description
本发明涉及光电器件探测器技术领域,特别涉及一种N极性面AlGaN紫外光电探测器外延结构及其制备方法。The invention relates to the technical field of photoelectric device detectors, in particular to an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector and a preparation method thereof.
以GaN为代表的III族氮化物材料是新一代光电器件的热点材料,由于其较宽的禁带宽度、较快的工作速度、优异的导电导热性能和损耗极低等优良特性,被视为是实现高性能光电器件小型化的优异替代材料。然而传统的金属极性的AlGaN光电探测器外延结构由于高温热稳定性弱、材料内部极化电场影响等缺陷的限制,同时随着N极性面III族氮化物材料制备工艺的日渐成熟,N极性AlGaN材料被视为传统金属极性AlGaN基光电探测器的替代材料。由于N极性面AlGaN相比于传统金属极性面具有相反的内建电场方向、更活泼的表面状态,因此现阶段通过传统方法进行N极性面AlGaN材料的生长不能有效提高其表面质量。Group III nitride materials represented by GaN are hot materials for new-generation optoelectronic devices. Due to their wide band gap, fast working speed, excellent electrical and thermal conductivity and extremely low loss, they are regarded It is an excellent alternative material to realize the miniaturization of high-performance optoelectronic devices. However, the epitaxial structure of the traditional metal-polar AlGaN photodetector is limited by defects such as weak high-temperature thermal stability and the influence of the internal polarization electric field of the material. Polar AlGaN materials are considered as alternative materials for traditional metallic polar AlGaN-based photodetectors. Since AlGaN on the N-polar surface has an opposite built-in electric field direction and a more active surface state than the traditional metal polar surface, the growth of AlGaN materials on the N-polar surface cannot effectively improve its surface quality at this stage.
发明内容Contents of the invention
为了解决上述现有技术的不足,本发明提供了一种N极性面AlGaN紫外光电探测器外延结构及其制备方法,该N极性面AlGaN紫外光电探测器工作响应度大,灵敏度高。In order to solve the above-mentioned deficiencies in the prior art, the present invention provides an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector and a preparation method thereof. The N-polar surface AlGaN ultraviolet photodetector has a large working responsivity and high sensitivity.
本发明的第一个目的在于提供一种N极性面AlGaN紫外光电探测器外延结构。The first object of the present invention is to provide an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector.
本发明的第二个目的在于提供一种N极性面AlGaN紫外光电探测器外延结构的制备方法。The second object of the present invention is to provide a method for preparing an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector.
本发明的第一个目的可以通过采取如下技术方案达到:First purpose of the present invention can be achieved by taking the following technical solutions:
一种N极性面AlGaN紫外光电探测器外延结构,包括在硅衬底上依次生长的非掺杂N极性面AlN缓冲层、碳掺杂半绝缘化N极性AlN缓冲层、碳掺杂N极性面组分渐变Al
yGa
1-yN缓冲层和非掺杂N极性面Al
xGa
1-xN层;其中,x=0.5~0.8,y=0.75~0.95。
An N-polar surface AlGaN ultraviolet photodetector epitaxial structure, including a non-doped N-polar surface AlN buffer layer, a carbon-doped semi-insulating N-polar AlN buffer layer, a carbon-doped A graded composition AlyGa1 -yN buffer layer on the N-polar surface and an AlxGa1 -xN layer on the non-doped N-polar surface; wherein, x=0.5-0.8, y=0.75-0.95.
进一步的,所述非掺杂N极性面AlN缓冲层包括低温生长非掺杂N极性面AlN缓冲层和高温生长非掺杂N极性面AlN缓冲层,所述低温生长非掺杂N极性AlN缓冲层生长在所述硅衬底上,所述高温生长非掺杂N极性AlN缓冲层生长在所述低温生长非掺杂N极性AlN缓冲层上。Further, the non-doped N-polar surface AlN buffer layer includes a low-temperature growth non-doped N-polar surface AlN buffer layer and a high-temperature growth non-doped N-polar surface AlN buffer layer, and the low-temperature growth non-doped N A polar AlN buffer layer is grown on the silicon substrate, and the high-temperature grown non-doped N-polar AlN buffer layer is grown on the low-temperature grown non-doped N-polar AlN buffer layer.
进一步的,所述低温生长非掺杂N极性AlN缓冲层的厚度为100~150nm,所述高 温生长非掺杂N极性AlN缓冲层的厚度为250~380nm。Further, the thickness of the low-temperature-grown non-doped N-polar AlN buffer layer is 100-150 nm, and the thickness of the high-temperature-grown non-doped N-polar AlN buffer layer is 250-380 nm.
进一步的,所述碳掺杂半绝缘化N极性AlN缓冲层的厚度为380~440nm,掺杂浓度为6.0×10
17~4.0×10
18cm
-3。
Further, the thickness of the carbon-doped semi-insulating N-polar AlN buffer layer is 380-440 nm, and the doping concentration is 6.0×10 17 to 4.0×10 18 cm -3 .
进一步的,所述碳掺杂N极性面组分渐变Al
yGa
1-yN缓冲层的厚度为480~630nm,掺杂浓度为5.0×10
16~2.0×10
17cm
-3。
Further, the thickness of the carbon-doped N polar surface graded AlyGa 1-y N buffer layer is 480-630 nm, and the doping concentration is 5.0×10 16 to 2.0×10 17 cm -3 .
进一步的,所述非掺杂N极性面Al
xGa
1-xN层的厚度为300~450nm。
Further, the thickness of the non-doped N polar surface AlxGa1 -xN layer is 300-450nm.
进一步的,所述硅衬底采用单晶硅衬底,以Si(111)密排面为外延面,以AlN[0001]方向作为材料外延生长方向。Further, the silicon substrate is a single crystal silicon substrate, the Si (111) close-packed plane is used as the epitaxial plane, and the AlN [0001] direction is used as the epitaxial growth direction of the material.
本发明的第二个目的可以通过采取如下技术方案达到:The second purpose of the present invention can be achieved by taking the following technical solutions:
一种N极性面AlGaN紫外光电探测器外延结构的制备方法,所述方法包括:A method for preparing an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector, the method comprising:
将所述硅衬底进行超声清洗后吹干;Blow dry the silicon substrate after ultrasonic cleaning;
采用脉冲激光沉积工艺,将所述硅衬底放入真空室中,在所述硅衬底上外延生长非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品;Using a pulsed laser deposition process, the silicon substrate is placed in a vacuum chamber, and a non-doped N-polar surface AlN buffer layer is epitaxially grown on the silicon substrate, thereby preparing an N-polar surface AlN sample;
采用金属有机物化学气相沉积设备生长法,将所述N极性AlN样品放入生长腔室内,并向腔室内通入NH
3、N
2、H
2、CH
4和三甲基铝,在所述非掺杂N极性面AlN缓冲层上外延生长碳掺杂半绝缘化N极性AlN缓冲层;
Using metal-organic chemical vapor deposition equipment growth method, put the N-polar AlN sample into the growth chamber, and feed NH 3 , N 2 , H 2 , CH 4 and trimethylaluminum into the chamber. Epitaxial growth of carbon-doped semi-insulating N-polar AlN buffer layer on the non-doped N-polar surface AlN buffer layer;
在完成所述碳掺杂半绝缘化N极性AlN缓冲层生长后,将腔体温度降低,同时向腔室内通入三甲基镓,在所述碳掺杂半绝缘化N极性AlN缓冲层上原位生长碳掺杂N极性面组分渐变AlGaN缓冲层;After the growth of the carbon-doped semi-insulating N-polar AlN buffer layer is completed, the temperature of the chamber is lowered, and trimethylgallium is introduced into the chamber at the same time, and the carbon-doped semi-insulating N-polar AlN buffer layer is In-situ growth of carbon-doped N polar surface composition graded AlGaN buffer layer on the layer;
在金属有机化合物化学气相沉积设备中完成所述碳掺杂N极性面组分渐变AlGaN缓冲层生长后,关闭CH4的气路,将腔体温度升高,在所述碳掺杂N极性面组分渐变AlGaN缓冲层上原位生长非掺杂N极性AlGaN层,同时通过调整三甲基铝流量与生长温度,调控膜层Al组分变化。After completing the growth of the carbon-doped N polar surface composition graded AlGaN buffer layer in the metal organic compound chemical vapor deposition equipment, the gas path of CH4 is closed, and the temperature of the chamber is increased. The non-doped N-polar AlGaN layer is grown in situ on the surface composition graded AlGaN buffer layer, and the change of the Al composition of the film is regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
进一步的,所述在所述硅衬底外延生长非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品,具体包括:Further, the epitaxial growth of the non-doped N-polar surface AlN buffer layer on the silicon substrate, thereby preparing the N-polar surface AlN sample, specifically includes:
所述硅衬底在富N条件下生长低温生长非掺杂N极性面AlN缓冲层,Al源为AlN高纯陶瓷靶材;The silicon substrate is grown under N-rich conditions at a low temperature to grow an AlN buffer layer on a non-doped N polar surface, and the Al source is an AlN high-purity ceramic target;
在完成所述低温生长非掺杂N极性面AlN缓冲层生长后,将***温度升高,腔体内真空度、激光能量、激光频率和氮气流量保持不变,在所述低温生长非掺杂N极性面AlN缓冲层上生长高温非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品。After the growth of the AlN buffer layer on the non-doped N polar surface of the low-temperature growth is completed, the temperature of the system is increased, and the vacuum degree, laser energy, laser frequency and nitrogen flow in the cavity are kept constant. A high-temperature non-doped N-polar surface AlN buffer layer is grown on the N-polar surface AlN buffer layer to prepare an N-polar surface AlN sample.
进一步的,所述硅衬底采用单晶硅衬底,以Si(111)密排面为外延面,以AlN[0001] 方向作为材料外延生长方向。Further, the silicon substrate is a single crystal silicon substrate, the Si(111) close-packed plane is used as the epitaxial plane, and the AlN [0001] direction is used as the material epitaxial growth direction.
本发明相对于现有技术具有如下的有益效果:Compared with the prior art, the present invention has the following beneficial effects:
1、本发明提供的N极性面AlGaN紫外光电探测器外延结构,在非掺杂N极性面AlGaN层下面生长一层碳掺杂的步进式N极性AlGaN薄膜,通过增强载流子的迁移率,能够有效增加非掺杂N极性AlGaN薄膜的光电流的产生,增强AlGaN基紫外探测器的功率和探测率。1. The N-polar surface AlGaN ultraviolet photodetector epitaxial structure provided by the present invention grows a layer of carbon-doped step-type N-polar AlGaN film under the non-doped N-polar surface AlGaN layer, by enhancing the carrier The mobility can effectively increase the photocurrent generation of non-doped N-polar AlGaN thin films, and enhance the power and detectability of AlGaN-based ultraviolet detectors.
2、本发明使用N极性AlGaN作为器件的基础材料,相比于金属极性的AlGaN材料,能够有效提高器件结构的高温稳定性,并减少AlGaN内部极化电场的影响,有效提高紫外光电探测器的光电响应度并有效降低后续器件加工难度。2. The present invention uses N-polarity AlGaN as the basic material of the device. Compared with metal-polarity AlGaN materials, it can effectively improve the high-temperature stability of the device structure, reduce the influence of the internal polarization electric field of AlGaN, and effectively improve the ultraviolet photoelectric detection. The photoelectric responsivity of the device and effectively reduce the difficulty of subsequent device processing.
3、本发明采用低温脉冲激光沉积结合高温MOCVD的两步生长法,生长N极性面AlGaN紫外光电探测器外延结构所需要的材料,并通过步进式的AlGaN外延缓冲层的结构设计,可以有效抑制III族氮化物与硅衬底间在高温下存在的回炉刻蚀反应、以及异质结构间较大的晶格失配,从而降低高温MOCVD生长的N极性AlGaN外延层的位错密度和表面粗糙度。3. The present invention adopts the two-step growth method of low-temperature pulsed laser deposition combined with high-temperature MOCVD to grow the materials required for the epitaxial structure of AlGaN ultraviolet photodetectors on the N-polar surface, and through the structural design of the step-by-step AlGaN epitaxial buffer layer, it can Effectively suppress the reflow etching reaction between the III-nitride and the silicon substrate at high temperature, and the large lattice mismatch between the heterostructures, thereby reducing the dislocation density of the N-polar AlGaN epitaxial layer grown by high-temperature MOCVD and surface roughness.
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图示出的结构获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. For those skilled in the art, other drawings can also be obtained according to the structures shown in these drawings without creative effort.
图1为本发明实施例的在N极性面AlGaN紫外光电探测器外延结构示意图。FIG. 1 is a schematic diagram of an epitaxial structure of an AlGaN ultraviolet photodetector on an N-polar plane according to an embodiment of the present invention.
图2为本发明实施例的N极性AlGaN外延片表面形貌原子力显微镜图。Fig. 2 is an atomic force microscope image of the surface morphology of an N-polarity AlGaN epitaxial wafer according to an embodiment of the present invention.
图3为本发明实施例的N极性AlGaN(0002)薄膜X射线摇摆曲线测试图。FIG. 3 is an X-ray rocking curve test chart of an N-polarity AlGaN (0002) thin film according to an embodiment of the present invention.
图1中:In Figure 1:
1-硅衬底、2-低温生长非掺杂N极性面AlN缓冲层、3-高温生长非掺杂N极性面AlN缓冲层、4-碳掺杂半绝缘化N极性AlN缓冲层、5-碳掺杂N极性面组分渐变AlGaN缓冲层、6-非掺杂N极性面AlGaN层。1-Silicon substrate, 2-Low temperature growth of non-doped N-polar surface AlN buffer layer, 3-High temperature growth of non-doped N-polar surface AlN buffer layer, 4-Carbon doped semi-insulating N-polar AlN buffer layer , 5-carbon-doped N-polar surface composition graded AlGaN buffer layer, 6-non-doped N-polar surface AlGaN layer.
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明的一部分实施例,而不是全部的实施例,基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发 明保护的范围。应当理解,描述的具体实施例仅仅用以解释本申请,并不用于限定本申请。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments It is a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work all belong to the protection scope of the present invention . It should be understood that the specific embodiments described are only used to explain the present application and are not intended to limit the present application.
实施例:Example:
本实施例提供了一种N极性面AlGaN紫外光电探测器外延结构的制备方法,所述方法包括:This embodiment provides a method for preparing an epitaxial structure of an AlGaN ultraviolet photodetector with an N-polar surface, the method comprising:
所述硅衬底采用单晶硅衬底,以Si(111)密排面为外延面,以AlN[0001]方向作为材料外延生长方向;The silicon substrate is a single crystal silicon substrate, the Si(111) close-packed surface is used as the epitaxial surface, and the AlN [0001] direction is used as the epitaxial growth direction of the material;
将所述硅衬底依次放入丙酮、无水乙醇、去离子水三种介质中,依次超声清洗,取出后用去离子水冲洗并使用热高纯氮气吹干;Put the silicon substrate into the three mediums of acetone, absolute ethanol, and deionized water in sequence, ultrasonically clean it in turn, rinse it with deionized water after taking it out, and dry it with hot high-purity nitrogen;
采用脉冲激光沉积工艺,将所述硅衬底放入真空室中,将温度升高至420~500℃、腔体内真空度抽至2.0×10
-4~4.0×10
-4torr、激光能量为250~320mJ、激光频率为15~30Hz、氮气流量为2~10sccm,在富N条件下生长N极性AlN薄膜,Al源为AlN高纯陶瓷靶材;
Using a pulsed laser deposition process, the silicon substrate is placed in a vacuum chamber, the temperature is raised to 420-500°C, the vacuum in the chamber is pumped to 2.0×10 -4 to 4.0×10 -4 torr, and the laser energy is 250~320mJ, laser frequency 15~30Hz, nitrogen flow rate 2~10sccm, grow N-polar AlN film under N-rich conditions, Al source is AlN high-purity ceramic target;
在完成所述N极性AlN薄膜生长后,将温度升高至850℃,腔体内真空度、激光能量、激光频率和氮气流量保持不变,在所述N极性AlN薄膜上外延生长高温非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品;After the growth of the N-polar AlN film is completed, the temperature is increased to 850°C, and the vacuum degree, laser energy, laser frequency and nitrogen flow in the cavity are kept constant, and the high-temperature N-polar AlN film is epitaxially grown on the N-polar AlN film. Doping the AlN buffer layer on the N polar surface to prepare an AlN sample on the N polar surface;
采用金属有机化合物化学气相沉积生长法(MOCVD技术),将制备的所述N极性AlN样品放入生长腔室内,将腔室真空度抽至2.0×10
-6~4.0×10
-6torr,温度升至1000~1100℃,并向腔室内通入NH
3、N
2、H
2、CH
4和三甲基铝,在所述高温非掺杂N极性面AlN缓冲层的外延片上外延生长碳掺杂半绝缘化N极性AlN缓冲层;气相沉积中,反应室气压为180~220torr,NH
3、H
2、CH
4、三甲基铝流量分别为30~50slm、60~100slm、10~20slm和350~440sccm;
Using metal organic compound chemical vapor deposition growth method (MOCVD technology), the prepared N-polar AlN sample is placed in the growth chamber, and the chamber is vacuumed to 2.0×10 -6 ~ 4.0×10 -6 torr, The temperature is raised to 1000-1100°C, and NH 3 , N 2 , H 2 , CH 4 and trimethylaluminum are introduced into the chamber to epitaxially grow on the epitaxial wafer of the high-temperature non-doped N-polar surface AlN buffer layer Carbon-doped semi-insulating N-polar AlN buffer layer; during vapor deposition, the pressure in the reaction chamber is 180-220torr, and the flow rates of NH 3 , H 2 , CH 4 , and trimethylaluminum are 30-50slm, 60-100slm, and 10 ~20slm and 350~440sccm;
在完成所述碳掺杂半绝缘化N极性AlN缓冲层生长后,将腔体温度降至770~800℃,同时向腔室内通入三甲基镓,在外延片上原位生长碳掺杂N极性面组分渐变AlGaN缓冲层;气相沉积中反应室气压为180~240torr,NH
3、H
2、CH
4、三甲基铝和三甲基镓流量分别为30~50slm、60~100slm、15~24slm、400~450sccm和100~150sccm;
After the growth of the carbon-doped semi-insulating N-polar AlN buffer layer is completed, the temperature of the chamber is lowered to 770-800°C, and at the same time, trimethylgallium is introduced into the chamber to in-situ grow carbon-doped Gradient AlGaN buffer layer on the N polar surface; the pressure of the reaction chamber in vapor deposition is 180-240torr, and the flow rates of NH 3 , H 2 , CH 4 , trimethylaluminum and trimethylgallium are 30-50slm and 60-100slm respectively , 15~24slm, 400~450sccm and 100~150sccm;
在MOCVD中完成所述碳掺杂N极性面组分渐变AlGaN缓冲层生长后,关闭CH4的气路,将腔体温度升至820~850℃,在外延片上原位生长非掺杂N极性AlGaN层;气相沉积中反应室气压为180~240torr,NH
3、H
2、三甲基铝和三甲基镓流量分别为30~50slm、60~100slm、400~450sccm和100~150sccm,同时,通过调整三甲基铝流量与生长温度,调控膜层Al组分变化。
After completing the growth of the carbon-doped N polar surface composition graded AlGaN buffer layer in MOCVD, close the gas path of CH4, raise the chamber temperature to 820-850°C, and grow non-doped N poles on the epitaxial wafer in situ AlGaN layer; during vapor deposition, the reaction chamber pressure is 180-240 torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 30-50slm, 60-100slm, 400-450sccm and 100-150sccm, respectively. , by adjusting the flow rate of trimethylaluminum and the growth temperature, the change of the Al composition of the film layer is regulated.
本实施例制备得到的N极性面AlGaN紫外光电探测器外延结构参见图1。The epitaxial structure of the N-polar surface AlGaN ultraviolet photodetector prepared in this embodiment is shown in FIG. 1 .
在一个实施例中,一种N极性面AlGaN基紫外光电探测器外延结构的制备方法,具体如下:In one embodiment, a method for preparing an epitaxial structure of an AlGaN-based ultraviolet photodetector on an N-polar surface is specifically as follows:
(1)衬底及其晶向的选取:采用单晶硅衬底,以Si(111)密排面作为外延面,以AlN[0001]方向作为材料外延生长方向;(1) Selection of the substrate and its crystal orientation: a single crystal silicon substrate is used, the Si(111) close-packed surface is used as the epitaxial surface, and the AlN [0001] direction is used as the epitaxial growth direction of the material;
(2)衬底表面清洗:将硅衬底依次放入丙酮、无水乙醇、去离子水三种介质中,依次超声清洗5min,取出后用去离子水冲洗并使用热高纯氮气吹干;(2) Substrate surface cleaning: Put the silicon substrate into acetone, absolute ethanol, and deionized water in sequence, and ultrasonically clean it for 5 minutes in sequence. After taking it out, rinse it with deionized water and dry it with hot high-purity nitrogen;
(3)非掺杂N极性面AlN缓冲层低温外延生长:采用脉冲激光沉积工艺,将洁净衬底放入真空室中,将衬底温度升高至450℃,腔内真空度抽至2.0×10
-4torr,激光能量为300mJ,激光频率为15Hz,氮气流量为4sccm,富N条件下生长N极性AlN薄膜,Al源为AlN高纯陶瓷靶材;
(3) Low-temperature epitaxial growth of the AlN buffer layer on the non-doped N polar surface: using a pulsed laser deposition process, put the clean substrate into a vacuum chamber, raise the substrate temperature to 450°C, and pump the vacuum to 2.0 ×10 -4 torr, the laser energy is 300mJ, the laser frequency is 15Hz, the nitrogen flow rate is 4sccm, the N-polar AlN film is grown under N-rich conditions, and the Al source is AlN high-purity ceramic target;
(4)非掺杂N极性面AlN缓冲层高温外延生长:将温度升高至850℃,其他参数保持与步骤(3)相同;(4) High-temperature epitaxial growth of the AlN buffer layer on the non-doped N polar surface: raise the temperature to 850° C., and keep other parameters the same as in step (3);
(5)碳掺杂N极性AlN层外延生长:采用MOCVD技术,将已制备的N极性AlN样品放入生长腔室内,将腔室真空度抽至3.0×10
-6,温度升至1050℃,并向腔室内通入NH
3、N
2、H
2、CH
4、三甲基铝,在步骤(4)得到的外延片上外延生长碳掺杂N极性面AlN层;所述气相沉积中,反应室气压为200torr,NH
3、H
2、CH
4、三甲基铝流量分别为40slm、75slm、17slm、400sccm;
(5) Epitaxial growth of carbon-doped N-polar AlN layer: Using MOCVD technology, put the prepared N-polar AlN sample into the growth chamber, pump the chamber vacuum to 3.0×10 -6 , and raise the temperature to 1050 ℃, and NH 3 , N 2 , H 2 , CH 4 , and trimethylaluminum are introduced into the chamber, and a carbon-doped N polar surface AlN layer is epitaxially grown on the epitaxial wafer obtained in step (4); the vapor deposition , the pressure in the reaction chamber is 200torr, and the flow rates of NH 3 , H 2 , CH 4 , and trimethylaluminum are 40slm, 75slm, 17slm, and 400sccm, respectively;
(6)碳掺杂N极性面组分渐变Al
yGa
1-yN层外延生长:在MOCVD中完成步骤(5)膜层生长后,将腔体温度降至780℃,同时向腔室内通入三甲基镓,在外延片上原位生长碳掺杂N极性面组分渐变AlGaN缓冲层。所述气相沉积中反应室气压为210torr,NH
3、H
2、CH
4、三甲基铝和三甲基镓流量分别为40slm、80slm、20slm、400sccm、20/100sccm(y=0.95时,流量为20sccm;当y=0.75,流量为100sccm);
(6) Epitaxial growth of carbon-doped N polar surface composition graded AlyGa 1-y N layer: After completing step (5) film growth in MOCVD, lower the chamber temperature to 780°C, Through trimethylgallium, the carbon-doped N polar surface composition graded AlGaN buffer layer is grown in situ on the epitaxial wafer. In the gas phase deposition, the pressure of the reaction chamber is 210torr, and the flow rates of NH 3 , H 2 , CH 4 , trimethylaluminum and trimethylgallium are 40slm, 80slm, 20slm, 400sccm, 20/100sccm (when y=0.95, the flow is 20sccm; when y=0.75, the flow rate is 100sccm);
(7)非掺杂N极性Al
xGa
1-xN层外延生长:在MOCVD中完成步骤(6)膜层生长后,关闭CH
4的气路,将腔体温度升至830℃,在外延片上原位生长非掺杂N极性AlGaN层。所述气相沉积中反应室气压为210torr,NH
3、H
2、三甲基铝和三甲基镓流量分别为40slm、80slm、430sccm、120sccm。同时,通过调整三甲基铝流量与生长温度调控膜层Al组分变化。
(7) Epitaxial growth of non-doped N-polar Al x Ga 1-x N layer: After the film growth in step (6) is completed in MOCVD, the gas path of CH 4 is closed, and the temperature of the chamber is raised to 830°C. The non-doped N-polar AlGaN layer is grown in situ on the epitaxial wafer. In the vapor phase deposition, the reaction chamber pressure is 210torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 40slm, 80slm, 430sccm, and 120sccm, respectively. At the same time, the change of the Al composition of the film layer was regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
本实施例得到的N极性面AlGaN紫外光电探测器外延结构,包括在硅衬底1上依次生长的非掺杂N极性面AlN缓冲层(包括低温生长非掺杂N极性面AlN缓冲层2和高温生长非掺杂N极性面AlN缓冲层3)、碳掺杂N极性面AlN层4、碳掺杂N极性面组分渐变Al
yGa
1-yN缓冲层5和非掺杂N极性面Al
xGa
1-xN层6;其中,非掺杂N极性面AlN层缓冲层为420nm,其中低温生长非掺杂N极性面AlN缓冲层厚度为120nm,高温生长非掺杂N极性面AlN缓冲层厚度为300nm,碳掺杂N极性面AlN层厚度为 380nm,掺杂浓度为2.0×10
18cm
-3;碳掺杂N极性面组分渐变Al
yGa
1-yN(由下往上y的取值从0.95变化到0.75)缓冲层厚度为500nm,掺杂浓度为1.5×10
17cm
-3;非掺杂N极性面Al
xGa
1-xN层厚度为300nm。
The N-polar surface AlGaN ultraviolet photodetector epitaxial structure obtained in this embodiment includes non-doped N-polar surface AlN buffer layers (including low-temperature growth of non-doped N-polar surface AlN buffer layers) grown sequentially on the silicon substrate 1. Layer 2 and high temperature growth non-doped N polar face AlN buffer layer 3), carbon doped N polar face AlN layer 4, carbon doped N polar face composition graded A y Ga 1-y N buffer layer 5 and Non-doped N polar surface AlxGa1 -xN layer 6; wherein, the buffer layer of the non-doped N polar surface AlN layer is 420nm, wherein the thickness of the low-temperature growth non-doped N polar surface AlN buffer layer is 120nm, The thickness of the non-doped N polar surface AlN buffer layer grown at high temperature is 300nm, the thickness of the carbon doped N polar surface AlN layer is 380nm, and the doping concentration is 2.0×10 18 cm -3 ; the carbon doped N polar surface component Gradient Al y Ga 1-y N (the value of y changes from 0.95 to 0.75 from bottom to top) buffer layer thickness is 500nm, doping concentration is 1.5×10 17 cm -3 ; non-doped N polar surface Al x The thickness of the Ga 1-x N layer is 300 nm.
本实施例制备得到的N极性面AlGaN紫外光电探测器外延结构参见图1,该生长条件下生长的外延结构中,AlGaN薄膜表面原子力显微镜表征图参见图2,可见表面质量较好;N极性AlGaN(0002)薄膜X射线摇摆曲线测试结果参见图3,可见薄膜晶体质量良好。The epitaxial structure of the N polar surface AlGaN ultraviolet photodetector prepared in this example is shown in Figure 1. In the epitaxial structure grown under this growth condition, the AFM characterization of the surface of the AlGaN thin film is shown in Figure 2. It can be seen that the surface quality is good; the N pole See Figure 3 for the test results of the X-ray rocking curve of the AlGaN (0002) thin film. It can be seen that the crystal quality of the thin film is good.
在一个实施例中,一种N极性面AlGaN基紫外光电探测器外延结构的制备方法,具体如下:In one embodiment, a method for preparing an epitaxial structure of an AlGaN-based ultraviolet photodetector on an N-polar surface is specifically as follows:
(1)衬底及其晶向的选取:采用单晶硅衬底,以Si(111)密排面作为外延面,以AlN[0001]方向作为材料外延生长方向;(1) Selection of the substrate and its crystal orientation: a single crystal silicon substrate is used, the Si(111) close-packed surface is used as the epitaxial surface, and the AlN [0001] direction is used as the epitaxial growth direction of the material;
(2)衬底表面清洗:将硅衬底依次放入丙酮、无水乙醇、去离子水三种介质中,依次超声清洗5min,取出后用去离子水冲洗并使用热高纯氮气吹干;(2) Substrate surface cleaning: Put the silicon substrate into acetone, absolute ethanol, and deionized water in sequence, and ultrasonically clean it for 5 minutes in sequence. After taking it out, rinse it with deionized water and dry it with hot high-purity nitrogen;
(3)非掺杂N极性面AlN缓冲层低温外延生长:采用脉冲激光沉积工艺,将洁净衬底放入真空室中,将衬底温度升高至420℃,腔内真空度抽至2.0×10
-4torr,激光能量为250mJ,激光频率为15Hz,氮气流量为2sccm,富N条件下生长N极性AlN薄膜,Al源为AlN高纯陶瓷靶材;
(3) Low-temperature epitaxial growth of the AlN buffer layer on the non-doped N polar surface: using a pulsed laser deposition process, put the clean substrate into the vacuum chamber, raise the substrate temperature to 420°C, and pump the vacuum to 2.0 ×10 -4 torr, the laser energy is 250mJ, the laser frequency is 15Hz, the nitrogen flow rate is 2sccm, the N-polar AlN film is grown under N-rich conditions, and the Al source is AlN high-purity ceramic target;
(4)非掺杂N极性面AlN缓冲层高温外延生长:将温度升高至950℃,其他参数保持与步骤(3)相同;(4) High-temperature epitaxial growth of the AlN buffer layer on the non-doped N polar surface: raise the temperature to 950° C., and keep other parameters the same as step (3);
(5)碳掺杂N极性AlN层外延生长:采用MOCVD技术,将已制备的N极性AlN样品放入生长腔室内,将腔室真空度抽至2.0×10
-6torr,温度升至1000℃,并向腔室内通入NH
3、N
2、H
2、CH
4、三甲基铝,在步骤(4)得到的外延片上外延生长碳掺杂N极性面AlN层;所述气相沉积中,反应室气压为180torr,NH
3、H
2、CH
4、三甲基铝流量分别为30slm、65slm、13slm、380sccm;
(5) Epitaxial growth of carbon-doped N-polar AlN layer: Using MOCVD technology, put the prepared N-polar AlN sample into the growth chamber, pump the chamber vacuum to 2.0×10 -6 torr, and raise the temperature to 1000°C, and NH 3 , N 2 , H 2 , CH 4 , and trimethylaluminum are introduced into the chamber, and a carbon-doped N polar surface AlN layer is epitaxially grown on the epitaxial wafer obtained in step (4); the gas phase During deposition, the pressure in the reaction chamber is 180torr, and the flow rates of NH 3 , H 2 , CH 4 , and trimethylaluminum are 30slm, 65slm, 13slm, and 380sccm, respectively;
(6)碳掺杂N极性面组分渐变Al
yGa
1-yN层外延生长:在MOCVD中完成步骤(5)膜层生长后,将腔体温度降至780℃,同时向腔室内通入三甲基镓,在外延片上原位生长碳掺杂N极性面组分渐变AlGaN缓冲层。所述气相沉积中反应室气压为210torr,NH
3、H
2、CH
4、三甲基铝和三甲基镓流量分别为30slm、60slm、15slm、420sccm、20/100sccm(y=0.95时,流量为20sccm;当y=0.75,流量为100sccm);
(6) Epitaxial growth of carbon-doped N polar surface composition graded AlyGa 1-y N layer: After completing step (5) film growth in MOCVD, lower the chamber temperature to 780°C, Through trimethylgallium, the carbon-doped N polar surface composition graded AlGaN buffer layer is grown in situ on the epitaxial wafer. In the gas phase deposition, the reaction chamber pressure is 210torr, and the flow rates of NH 3 , H 2 , CH 4 , trimethylaluminum and trimethylgallium are 30slm, 60slm, 15slm, 420sccm, 20/100sccm (when y=0.95, the flow is 20sccm; when y=0.75, the flow rate is 100sccm);
(7)非掺杂N极性Al
xGa
1-xN层外延生长:在MOCVD中完成步骤(6)膜层生长后,关闭CH
4的气路,将腔体温度升至830℃,在外延片上原位生长非掺杂N极性AlGaN层。所述气相沉积中反应室气压为210torr,NH
3、H
2、三甲基铝和三甲基镓流量分别 为40slm、80slm、430sccm、120sccm。同时,通过调整三甲基铝流量与生长温度调控膜层Al组分变化。
(7) Epitaxial growth of non-doped N-polar Al x Ga 1-x N layer: After the film growth in step (6) is completed in MOCVD, the gas path of CH 4 is closed, and the temperature of the chamber is raised to 830°C. The non-doped N-polar AlGaN layer is grown in situ on the epitaxial wafer. In the vapor phase deposition, the reaction chamber pressure is 210torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 40slm, 80slm, 430sccm, and 120sccm, respectively. At the same time, the change of the Al composition of the film layer was regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
本实施例得到的N极性面AlGaN紫外光电探测器外延结构,包括在硅衬底上依次生长的非掺杂N极性面AlN层缓冲层、碳掺杂N极性面AlN层、碳掺杂N极性面组分渐变Al
yGa
1-yN缓冲层(由下往上y=0.95~0.75)、非掺杂N极性面Al
xGa
1-xN层;所述非掺杂N极性面AlN层缓冲层为420nm,其中低温生长非掺杂N极性面AlN缓冲层厚度为120nm,高温生长非掺杂N极性面AlN缓冲层厚度为300nm;碳掺杂N极性面AlN层厚度为380nm,掺杂浓度为6.0×10
17~4.0×10
18cm
-3;碳掺杂N极性面组分渐变Al
yGa
1-yN(由下往上y=0.95~0.75)缓冲层厚度为500nm,掺杂浓度为5.0×10
16~2.0×10
17cm
-3;非掺杂N极性面Al
xGa
1-xN层厚度为300nm。
The N-polar surface AlGaN ultraviolet photodetector epitaxial structure obtained in this embodiment includes a non-doped N-polar surface AlN layer buffer layer, a carbon-doped N-polar surface AlN layer, a carbon-doped N-polar surface AlN layer, and a carbon-doped Gradient Al y Ga 1-y N buffer layer (from bottom to top y = 0.95 ~ 0.75), non-doped N polar surface Al x Ga 1-x N layer; the non-doped The buffer layer of the AlN layer on the N polar surface is 420nm, and the thickness of the AlN buffer layer on the non-doped N polar surface grown at low temperature is 120nm, and the thickness of the AlN buffer layer on the high temperature grown non-doped N polar surface is 300nm; The thickness of the AlN layer on the surface is 380nm, and the doping concentration is 6.0×10 17 ~ 4.0×10 18 cm -3 ; the composition of the carbon-doped N polar surface is gradually changed to Aly Ga 1-y N (from bottom to top y=0.95~ 0.75) The thickness of the buffer layer is 500nm, the doping concentration is 5.0×10 16 ~ 2.0×10 17 cm -3 ; the thickness of the Al x Ga 1-x N layer on the non-doped N polar surface is 300nm.
本实施例制备的N极性面AlGaN紫外光电探测器外延结构测试结果参见图3。Refer to FIG. 3 for the test results of the epitaxial structure of the N-polar surface AlGaN ultraviolet photodetector prepared in this embodiment.
在一个实施例中,一种N极性面AlGaN基紫外光电探测器外延结构的制备方法,具体如下:In one embodiment, a method for preparing an epitaxial structure of an AlGaN-based ultraviolet photodetector on an N-polar surface is specifically as follows:
(1)衬底及其晶向的选取:采用单晶硅衬底,以Si(111)密排面作为外延面,以AlN[0001]方向作为材料外延生长方向;(1) Selection of the substrate and its crystal orientation: a single crystal silicon substrate is used, the Si(111) close-packed surface is used as the epitaxial surface, and the AlN [0001] direction is used as the epitaxial growth direction of the material;
(2)衬底表面清洗:将硅衬底依次放入丙酮、无水乙醇、去离子水三种介质中,依次超声清洗5min,取出后用去离子水冲洗并使用热高纯氮气吹干;(2) Substrate surface cleaning: Put the silicon substrate into acetone, absolute ethanol, and deionized water in sequence, and ultrasonically clean it for 5 minutes in sequence. After taking it out, rinse it with deionized water and dry it with hot high-purity nitrogen;
(3)非掺杂N极性面AlN缓冲层低温外延生长:采用脉冲激光沉积工艺,将洁净衬底放入真空室中,将衬底温度升高至500℃,腔内真空度抽至2.0×10
-4torr,激光能量为320mJ,激光频率为25Hz,氮气流量为10sccm,富N条件下生长N极性AlN薄膜,Al源为AlN高纯陶瓷靶材;
(3) Low-temperature epitaxial growth of the AlN buffer layer on the non-doped N polar surface: using a pulsed laser deposition process, put the clean substrate into the vacuum chamber, raise the substrate temperature to 500°C, and pump the vacuum to 2.0 ×10 -4 torr, the laser energy is 320mJ, the laser frequency is 25Hz, the nitrogen flow rate is 10sccm, and the N-polar AlN film is grown under N-rich conditions, and the Al source is AlN high-purity ceramic target;
(4)非掺杂N极性面AlN缓冲层高温外延生长:将温度升高至1000℃,其他参数保持与步骤(3)相同;(4) High-temperature epitaxial growth of the AlN buffer layer on the non-doped N polar surface: raise the temperature to 1000° C., and keep other parameters the same as step (3);
(5)碳掺杂N极性AlN层外延生长:采用MOCVD技术,将已制备的N极性AlN样品放入生长腔室内,将腔室真空度抽至4.0×10
-6,温度升至1100℃,并向腔室内通入NH
3、N
2、H
2、CH
4、三甲基铝,在步骤(4)得到的外延片上外延生长碳掺杂N极性面AlN层;所述气相沉积中,反应室气压为200torr(180~220),NH
3、H
2、CH
4、三甲基铝流量分别为50slm、85slm、20slm、440sccm;
(5) Epitaxial growth of carbon-doped N-polar AlN layer: Using MOCVD technology, put the prepared N-polar AlN sample into the growth chamber, pump the chamber vacuum to 4.0×10 -6 , and raise the temperature to 1100 ℃, and NH 3 , N 2 , H 2 , CH 4 , and trimethylaluminum are introduced into the chamber, and a carbon-doped N polar surface AlN layer is epitaxially grown on the epitaxial wafer obtained in step (4); the vapor deposition , the pressure in the reaction chamber is 200torr (180-220), and the flow rates of NH 3 , H 2 , CH 4 , and trimethylaluminum are 50slm, 85slm, 20slm, and 440sccm, respectively;
(6)碳掺杂N极性面组分渐变Al
yGa
1-yN层外延生长:在MOCVD中完成步骤(5)膜层生长后,将腔体温度降至780℃,同时向腔室内通入三甲基镓,在外延片上原位生长碳掺杂N极性面组分渐变AlGaN缓冲层。所述气相沉积中反应室气压为210torr,NH
3、H
2、CH
4、三甲基铝和三甲基镓流量分别为50slm、100slm、24slm、450sccm、20/100sccm (y=0.95时,流量为20sccm;当y=0.75,流量为100sccm);
(6) Epitaxial growth of carbon-doped N polar surface composition graded AlyGa 1-y N layer: After completing step (5) film growth in MOCVD, lower the chamber temperature to 780°C, Through trimethylgallium, the carbon-doped N polar surface composition graded AlGaN buffer layer is grown in situ on the epitaxial wafer. In the gas phase deposition, the pressure of the reaction chamber is 210torr, and the flow rates of NH 3 , H 2 , CH 4 , trimethylaluminum and trimethylgallium are 50slm, 100slm, 24slm, 450sccm, 20/100sccm (when y=0.95, the flow is 20sccm; when y=0.75, the flow rate is 100sccm);
(7)非掺杂N极性Al
xGa
1-xN层外延生长:在MOCVD中完成步骤(6)膜层生长后,关闭CH
4的气路,将腔体温度升至850℃,在外延片上原位生长非掺杂N极性AlGaN层。所述气相沉积中反应室气压为240torr,NH
3、H
2、三甲基铝和三甲基镓流量分别为50slm、100slm、450sccm、120sccm。同时,通过调整三甲基铝流量与生长温度调控膜层Al组分变化。
(7) Epitaxial growth of non-doped N-polar Al x Ga 1-x N layer: After completing step (6) film growth in MOCVD, close the gas path of CH 4 , raise the chamber temperature to 850°C, and The non-doped N-polar AlGaN layer is grown in situ on the epitaxial wafer. In the vapor phase deposition, the pressure of the reaction chamber is 240torr, and the flow rates of NH 3 , H 2 , trimethylaluminum and trimethylgallium are 50slm, 100slm, 450sccm, and 120sccm, respectively. At the same time, the change of the Al composition of the film layer was regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
本实施例得到的N极性面AlGaN紫外光电探测器外延结构,包括在硅衬底上依次生长的非掺杂N极性面AlN层缓冲层、碳掺杂N极性面AlN层、碳掺杂N极性面组分渐变Al
yGa
1-yN缓冲层(由下往上y=0.95~0.75)和非掺杂N极性面Al
xGa
1-xN层;所述非掺杂N极性面AlN层缓冲层为500nm,其中低温生长非掺杂N极性面AlN缓冲层厚度为150nm,高温生长非掺杂N极性面AlN缓冲层厚度为350nm;碳掺杂N极性面AlN层厚度为400nm,掺杂浓度为2.0×10
18cm
-3;碳掺杂N极性面组分渐变Al
yGa
1-yN(由下往上y=0.95,0.75)缓冲层厚度为550nm,掺杂浓度为1.5×10
17cm
-3;非掺杂N极性面Al
xGa
1-xN层厚度为350nm。
The N-polar surface AlGaN ultraviolet photodetector epitaxial structure obtained in this embodiment includes a non-doped N-polar surface AlN layer buffer layer, a carbon-doped N-polar surface AlN layer, a carbon-doped N-polar surface AlN layer, and a carbon-doped The hetero-N polar surface composition graded Al y Ga 1-y N buffer layer (from bottom to top y=0.95~0.75) and the non-doped N polar surface Al x Ga 1-x N layer; the non-doped The buffer layer of the AlN layer on the N polar surface is 500nm, and the thickness of the AlN buffer layer on the non-doped N polar surface grown at low temperature is 150nm, and the thickness of the AlN buffer layer on the high temperature grown non-doped N polar surface is 350nm; The thickness of the AlN layer on the surface is 400nm, and the doping concentration is 2.0×10 18 cm -3 ; the carbon-doped N polar surface composition gradually changes to AlyGa 1-y N (from bottom to top y=0.95,0.75) buffer layer thickness The thickness of the Al x Ga 1-x N layer on the non-doped N polar surface is 350 nm.
本实施例制备的N极性面AlGaN紫外光电探测器外延结构测试结果参见图3。Refer to FIG. 3 for the test results of the epitaxial structure of the N-polar surface AlGaN ultraviolet photodetector prepared in this embodiment.
以上所述,仅为本发明专利较佳的实施例,但本发明专利的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明专利所公开的范围内,根据本发明专利的技术方案及其发明构思加以等同替换或改变,都属于本发明专利的保护范围。The above is only a preferred embodiment of the patent of the present invention, but the scope of protection of the patent of the present invention is not limited thereto. Equivalent replacements or changes to the technical solutions and their inventive concepts all fall within the scope of protection of the invention patent.
Claims (10)
- 一种N极性面AlGaN紫外光电探测器外延结构,其特征在于,包括在硅衬底上依次生长的非掺杂N极性面AlN缓冲层、碳掺杂半绝缘化N极性AlN缓冲层、碳掺杂N极性面组分渐变Al yGa 1-yN缓冲层和非掺杂N极性面Al xGa 1-xN层;其中,x=0.5~0.8,y=0.75~0.95。 An N-polar surface AlGaN ultraviolet photodetector epitaxial structure, characterized in that it includes a non-doped N-polar surface AlN buffer layer and a carbon-doped semi-insulating N-polar AlN buffer layer grown sequentially on a silicon substrate , carbon-doped N polar face composition graded A y Ga 1-y N buffer layer and non-doped N polar face Al x Ga 1-x N layer; wherein, x=0.5~0.8, y=0.75~0.95 .
- 根据权利要求1所述的N极性面AlGaN紫外光电探测器外延结构,其特征在于,所述非掺杂N极性面AlN缓冲层包括低温生长非掺杂N极性面AlN缓冲层和高温生长非掺杂N极性面AlN缓冲层,所述低温生长非掺杂N极性AlN缓冲层生长在所述硅衬底上,所述高温生长非掺杂N极性AlN缓冲层生长在所述低温生长非掺杂N极性AlN缓冲层上。The N-polar surface AlGaN ultraviolet photodetector epitaxial structure according to claim 1, wherein the non-doped N-polar surface AlN buffer layer comprises a low-temperature grown non-doped N-polar surface AlN buffer layer and a high-temperature growing a non-doped N-polar surface AlN buffer layer, the low-temperature grown non-doped N-polar AlN buffer layer is grown on the silicon substrate, and the high-temperature grown non-doped N-polar AlN buffer layer is grown on the The low-temperature growth of non-doped N-polar AlN buffer layer.
- 根据权利要求2所述的N极性面AlGaN紫外光电探测器外延结构,其特征在于,所述低温生长非掺杂N极性AlN缓冲层的厚度为100~150nm,所述高温生长非掺杂N极性AlN缓冲层的厚度为250~380nm。The N-polar surface AlGaN ultraviolet photodetector epitaxial structure according to claim 2, wherein the thickness of the low-temperature grown non-doped N-polar AlN buffer layer is 100-150 nm, and the high-temperature grown non-doped The thickness of the N-polar AlN buffer layer is 250-380 nm.
- 根据权利要求1所述的N极性面AlGaN紫外光电探测器外延结构,其特征在于,所述碳掺杂半绝缘化N极性AlN缓冲层的厚度为380~440nm,掺杂浓度为6.0×10 17~4.0×10 18cm -3。 The epitaxial structure of the N-polar surface AlGaN ultraviolet photodetector according to claim 1, wherein the thickness of the carbon-doped semi-insulating N-polar AlN buffer layer is 380-440 nm, and the doping concentration is 6.0× 10 17 ~ 4.0×10 18 cm -3 .
- 根据权利要求1所述的N极性面AlGaN紫外光电探测器外延结构,其特征在于,所述碳掺杂N极性面组分渐变Al yGa 1-yN缓冲层的厚度为480~630nm,掺杂浓度为5.0×10 16~2.0×10 17cm -3。 The N-polar surface AlGaN ultraviolet photodetector epitaxial structure according to claim 1, characterized in that the thickness of the carbon-doped N-polar surface composition gradient AlyGa1 -yN buffer layer is 480-630nm , and the doping concentration is 5.0×10 16 to 2.0×10 17 cm -3 .
- 根据权利要求1所述的N极性面AlGaN紫外光电探测器外延结构,其特征在于,所述非掺杂N极性面Al xGa 1-xN层的厚度为300~450nm。 The epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector according to claim 1, wherein the thickness of the non-doped N-polar surface AlxGa1 -xN layer is 300-450nm.
- 根据权利要求1~6任一项所述的N极性面AlGaN紫外光电探测器外延结构,其特征在于,所述硅衬底采用单晶硅衬底,以Si(111)密排面为外延面,以AlN[0001]方向作为材料外延生长方向。The epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector according to any one of claims 1 to 6, wherein the silicon substrate is a single crystal silicon substrate, and the Si (111) close-packed surface is used as the epitaxial structure. On the surface, the AlN [0001] direction is used as the epitaxial growth direction of the material.
- 一种如权利要求1~7任一项所述N极性面AlGaN紫外光电探测器外延结构的制备方法,其特征在于,所述方法包括:A method for preparing an epitaxial structure of an N-polar surface AlGaN ultraviolet photodetector according to any one of claims 1 to 7, wherein the method comprises:将所述硅衬底进行超声清洗后吹干;Blow dry the silicon substrate after ultrasonic cleaning;采用脉冲激光沉积工艺,将所述硅衬底放入真空室中,在所述硅衬底上外延生长非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品;Using a pulsed laser deposition process, the silicon substrate is placed in a vacuum chamber, and a non-doped N-polar surface AlN buffer layer is epitaxially grown on the silicon substrate, thereby preparing an N-polar surface AlN sample;采用金属有机物化学气相沉积设备生长法,将所述N极性AlN样品放入生长腔室内,并向腔室内通入NH 3、N 2、H 2、CH 4和三甲基铝,在所述非掺杂N极性面AlN缓 冲层上外延生长碳掺杂半绝缘化N极性AlN缓冲层; Using metal-organic chemical vapor deposition equipment growth method, put the N-polar AlN sample into the growth chamber, and feed NH 3 , N 2 , H 2 , CH 4 and trimethylaluminum into the chamber. Epitaxial growth of carbon-doped semi-insulating N-polar AlN buffer layer on the non-doped N-polar surface AlN buffer layer;在完成所述碳掺杂半绝缘化N极性AlN缓冲层生长后,将腔体温度降低,同时向腔室内通入三甲基镓,在所述碳掺杂半绝缘化N极性AlN缓冲层上原位生长碳掺杂N极性面组分渐变AlGaN缓冲层;After the growth of the carbon-doped semi-insulating N-polar AlN buffer layer is completed, the temperature of the chamber is lowered, and trimethylgallium is introduced into the chamber at the same time, and the carbon-doped semi-insulating N-polar AlN buffer layer is In-situ growth of carbon-doped N polar surface composition graded AlGaN buffer layer on the layer;在金属有机化合物化学气相沉积设备中完成所述碳掺杂N极性面组分渐变AlGaN缓冲层生长后,关闭CH4的气路,将腔体温度升高,在所述碳掺杂N极性面组分渐变AlGaN缓冲层上原位生长非掺杂N极性AlGaN层,同时通过调整三甲基铝流量与生长温度,调控膜层Al组分变化。After completing the growth of the carbon-doped N polar surface composition graded AlGaN buffer layer in the metal organic compound chemical vapor deposition equipment, the gas path of CH4 is closed, and the temperature of the chamber is increased. The non-doped N-polar AlGaN layer is grown in situ on the surface composition graded AlGaN buffer layer, and the change of the Al composition of the film is regulated by adjusting the flow rate of trimethylaluminum and the growth temperature.
- 根据权利要求8所述的制备方法,其特征在于,所述在所述硅衬底外延生长非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品,具体包括:The preparation method according to claim 8, wherein the non-doped N-polar surface AlN buffer layer is epitaxially grown on the silicon substrate, thereby preparing an N-polar surface AlN sample, specifically comprising:所述硅衬底在富N条件下生长低温生长非掺杂N极性面AlN缓冲层,Al源为AlN高纯陶瓷靶材;The silicon substrate is grown under N-rich conditions at a low temperature to grow an AlN buffer layer on a non-doped N polar surface, and the Al source is an AlN high-purity ceramic target;在完成所述低温生长非掺杂N极性面AlN缓冲层生长后,将***温度升高,腔体内真空度、激光能量、激光频率和氮气流量保持不变,在所述低温生长非掺杂N极性面AlN缓冲层上生长高温非掺杂N极性面AlN缓冲层,从而制得N极性面AlN样品。After the growth of the AlN buffer layer on the non-doped N polar surface of the low-temperature growth is completed, the temperature of the system is increased, and the vacuum degree, laser energy, laser frequency and nitrogen flow in the cavity are kept constant. A high-temperature non-doped N-polar surface AlN buffer layer is grown on the N-polar surface AlN buffer layer to prepare an N-polar surface AlN sample.
- 根据权利要求8所述的制备方法,其特征在于,所述硅衬底采用单晶硅衬底,以Si(111)密排面为外延面,以AlN[0001]方向作为材料外延生长方向。The preparation method according to claim 8, wherein the silicon substrate is a single crystal silicon substrate, the Si (111) close-packed plane is used as the epitaxial plane, and the AlN [0001] direction is used as the epitaxial growth direction of the material.
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