CN100558947C - The method of growing indium nitride monocrystal thin films - Google Patents

The method of growing indium nitride monocrystal thin films Download PDF

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CN100558947C
CN100558947C CNB2007100629795A CN200710062979A CN100558947C CN 100558947 C CN100558947 C CN 100558947C CN B2007100629795 A CNB2007100629795 A CN B2007100629795A CN 200710062979 A CN200710062979 A CN 200710062979A CN 100558947 C CN100558947 C CN 100558947C
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indium nitride
thin films
monocrystal thin
growing
nitride monocrystal
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CN101230487A (en
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王晓亮
肖红领
胡国新
杨翠柏
冉学军
王翠梅
张小宾
李建平
李晋闽
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Institute of Semiconductors of CAS
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Abstract

The method of a kind of growing indium nitride monocrystal thin films of the present invention is characterized in that, comprises the steps: step 1: select a substrate; Step 2: adopt metal-organic chemical vapor deposition equipment technology one deck nucleating layer of growing on substrate, this nucleating layer can increase the nucleation density of substrate surface; Step 3: adopt metal-organic chemical vapor deposition equipment technology one deck buffer layer of grow on nucleating layer, this buffer layer can reduce the defect concentration of epitaxial film, the raising crystal mass; Step 4: adopt metal-organic chemical vapor deposition equipment technology growing indium nitride monocrystal thin films on buffer layer, this indium nitride monocrystal thin films surfacing, crystal mass height.

Description

The method of growing indium nitride monocrystal thin films
Technical field
The invention belongs to technical field of semiconductors, relate to a kind of method that adopts metal-organic chemical vapor deposition equipment technology growth indium nitride monocrystal thin films.
Background technology
In recent years, III-V compound semiconductor indium nitride is because the broad prospect of application on photoelectron and microelectronic device has caused the great interest of people.Indium nitride is considered to the preferred material of low-loss high-efficiency battery, optical mask and multiple sensors.Nearest studies show that indium nitride has good application prospects in Terahertz (THz) radiation, then can be used as plasma body filter material etc. in hot photovoltaic system.Theoretical Calculation shows, with respect to gallium arsenide, aluminium nitride and gan, indium nitride has superior stable state and transient state electrons transport property, its mobility, peak rate, saturation drift velocity and spike (overshoot) speed is high, a wherein low mobility can reach 3200cm2/Vs, peak shift speed can reach 4.3 * 107cm/s, and these electrons transport properties are not subjected to the influence of temperature change, the limiting frequency that can estimate the indium nitride field-effect transistor can be up to 400GHz, and these characteristics make indium nitride use at high frequency centimetre and millimetric wave device to have special advantages.In addition, it can also be as the raceway groove in the field-effect transistor of gallium nitride/aluminum gallium base, with improve current carrier in raceway groove mobility and reduce its transition time (transit time) by raceway groove.
But up to the present, indium nitride does not but obtain so superior electrology characteristic experimentally.This is that its body material is difficult to preparation because there is certain difficulty in the indium nitride material in growth, and growth for Thin Film faces and lacks the substrate material that lattice parameter and thermal expansivity all mate, and problem such as decomposition temperature is lower.
Summary of the invention
The objective of the invention is to, a kind of method of growing indium nitride monocrystal thin films is provided, this method is to adopt the method for metal-organic chemical vapor deposition equipment technology growth indium nitride monocrystal thin films, it can solve the lower problem of mobility ratio in the metal-organic chemical vapor deposition equipment technology growth indium nitride film process, growth conditions is controlled easily, makes that the epitaxy of indium nitride monocrystal is simple.
The method of a kind of growing indium nitride monocrystal thin films of the present invention is characterized in that, comprises the steps:
Step 1: select a substrate;
Step 2: adopt metal-organic chemical vapor deposition equipment technology one deck nucleating layer of growing on substrate, this nucleating layer can increase the nucleation density of substrate surface;
Step 3: adopt metal-organic chemical vapor deposition equipment technology one deck buffer layer of grow on nucleating layer, this buffer layer can reduce the defect concentration of epitaxial film, the raising crystal mass;
Step 4: adopt metal-organic chemical vapor deposition equipment technology growing indium nitride monocrystal thin films on buffer layer, this indium nitride monocrystal thin films surfacing, crystal mass height.
Wherein said substrate is sapphire or silicon carbide or silicon substrate.
The material of wherein said nucleating layer is Al xIn yGa 1-x-yN, wherein, x+y=1,0≤x<1,0≤y<1.
The material of wherein said buffer layer is a gan.
When wherein growing into stratum nucleare, growth temperature is 450-1150 ℃, and growth pressure is 5.33-26.67kPa, and thickness is 0.01-0.05 μ m, and preferable range is 850-1150 ℃, 0.01-0.03 μ m.
Wherein during the growing gallium nitride buffer layer, growth temperature is 900-1100 ℃, and growth pressure is 13.33-26.67kPa, and thickness is 1.00-2.00 μ m, and preferable range is 1000-1100 ℃, 1.50-2.00 μ m.
Wherein during growing indium nitride monocrystal thin films, growth temperature is 400-650 ℃, and growth pressure is 13.33-26.67kPa, and growth thickness is 0.15-0.65 μ m, and preferable range is 450-600 ℃.
The present invention adopts unique Al xIn yGa 1-x-yThe N buffer layer by accurate control growing condition, as temperature, pressure, V/III ratio, has effectively been alleviated the stress that lattice mismatch and thermal expansion bring; Simultaneously,, reduced the defect concentration of indium nitride epitaxial film, improved the crystal mass of indium nitride epitaxial film, obtained the indium nitride monocrystal thin films of room temperature mobility above 1100cm2/Vs by the growth conditions of control adjustment indium nitride epitaxial film.
Description of drawings
For further specifying content of the present invention, below in conjunction with embodiment and accompanying drawing the present invention is done a detailed description, wherein:
Fig. 1 is an indium nitride monocrystal thin films growth structure synoptic diagram of the present invention;
Fig. 2 is the twin crystal X ray θ-2 θ sweep test result of indium nitride monocrystal thin films of the present invention;
Fig. 3 is the twin crystal X ray peak width at half height test result of indium nitride monocrystal thin films of the present invention;
Fig. 4 is the surfaceness test result of indium nitride monocrystal thin films of the present invention;
Fig. 5 is the mobility test result of indium nitride monocrystal thin films of the present invention.
Embodiment
Key of the present invention is to adopt unique Al xIn yGa 1-x-yThe N buffer layer, wherein, x+y=1,0≤x<1,0≤y<1.When x=y=0, the Al that is adopted xIn yGa 1-x-yThe N buffer layer is the gan buffer layer.In process of growth,,, effectively alleviated the stress that lattice mismatch and thermal expansion bring as growth temperature, growth pressure, V/III ratio by accurate control growing condition; Simultaneously,, reduced the defect concentration of indium nitride epitaxial film, improved the crystal mass of indium nitride epitaxial film, obtained the indium nitride monocrystal thin films of room temperature mobility above 1100cm2/Vs by the growth conditions of control adjustment indium nitride epitaxial film.
The nucleating layer that forms under differing temps, buffer layer can be grown under cost-effective condition, and the defective between substrate and the extension indium nitride film is obviously reduced.By the crystalline texture of nucleating layer, buffer layer, the defective between substrate and the extension indium nitride film is relaxed.
See also shown in Figure 1ly, the present invention is a kind of method that adopts metal-organic chemical vapor deposition equipment technology growth indium nitride monocrystal thin films, it is characterized in that, comprises the steps:
Step 1: select a substrate 10, this substrate 10 comprises sapphire, silicon carbide and silicon substrate, also comprises other substrates that are fit to the indium nitride monocrystal thin films extension;
Step 2: on substrate 10, adopt metal-organic chemical vapor deposition equipment technology growth one deck Al xIn yGa 1-x-y N nucleating layer 20, wherein, x+y=1,0≤x<1,0≤y<1.Growth temperature is 450-115 ℃, and growth pressure is 5.33-26.67kPa, and thickness is 0.01-0.05 μ m, and preferable range is 850-1150 ℃, 0.01-0.03 μ m.This nucleating layer can increase the nucleation density of substrate surface.
Step 3: at Al xIn yGa 1-x-yAdopt metal-organic chemical vapor deposition equipment technology growth one deck gan buffer layer 30 on the N nucleating layer 20, growth temperature is 900-1100 ℃, and growth pressure is 13.33-26.67kPa, and thickness is 1.00-2.00 μ m, preferable range is 1000-1100 ℃, 1.50-2.00 μ m.This buffer layer can reduce the defect concentration of epitaxial film, improves crystal mass.
Step 4: reduce growth temperature at last, on gan buffer layer 30, adopt metal-organic chemical vapor deposition equipment technology growth one deck indium nitride monocrystal thin films 40, growth temperature is 400-650 ℃, growth pressure is 13.33-26.67kPa, growth thickness is 0.15-0.65 μ m, and preferable range is 450-600 ℃.
In the method for employing metal-organic chemical vapor deposition equipment technology growth indium nitride monocrystal thin films provided by the invention, the concrete growth temperature of each grown layer, growth pressure and growth thickness are as shown in table 1:
Table 1
Title Growth temperature Growth pressure Growth thickness Remarks
Al xIn yG a 1-x-y N nucleating layer 20 450-1150 ℃, preferable range is 850-1150 ℃ 5.33 -267 kPa 0.01-0.05 μ m, preferable range is 0.01-0.03 μ m x+y=1, 0≤x< 1,0≤y <1
Gan buffer layer 30 900-1100 ℃, preferable range is 1000-1100 ℃ 13.3 3-26 .67k Pa 1.00-2.00 μ m, preferable range is 1.50-2.00 μ m -
Indium nitride monocrystal thin films 40 400-650 ℃, preferable range is 450-600 ℃ 13.3 3-26 .67k Pa 0.15-0.65 μm -
The sample that is obtained by above growth step is carried out test analysis, and the indium nitride material with this technology growth is a monocrystalline as can be known, crystal structure quality height, and the surface is comparatively smooth.Use twin crystal X-ray diffraction method to confirm to have only indium nitride (0002) and gan (0002) to have (omitting corresponding substrate peak) in the θ-2 θ diffracting spectrum of (0002) face of this material, and the diffraction peak intensity height, peak position is clear; Do not find the diffraction peak (Fig. 2) of simple substance indium.Twin crystal X diffraction method confirms that also the rocking curve peak width at half height of this monocrystal material (0002) face is less than 7.1arcmin (Fig. 3).The atomic force microscope testing method confirms that this material surface roughness is less than 7.2nm (Fig. 4).The Hall testing method has confirmed that the room temperature mobility of this material has reached 1100cm2/Vs (Fig. 5).This explanation the present invention can improve the surfacing of indium nitride epitaxial film, the indium nitride monocrystal thin films that the room temperature mobility surpasses 1100cm2/Vs.
The present invention has reduced technology difficulty, has reduced processing step, has obtained to have more fabricating low-defect-density and more the indium nitride film material of high mobility, has improved the crystal mass and the surface finish of material simultaneously.Therefore, the present invention can significantly improve the epitaxy quality of indium nitride film.

Claims (5)

1, a kind of method of growing indium nitride monocrystal thin films is characterized in that, comprises the steps:
Step 1: select a substrate;
Step 2: adopt metal-organic chemical vapor deposition equipment technology one deck nucleating layer of growing on substrate, the growth temperature of nucleating layer is 450-1150 ℃, and growth pressure is 5.33-26.67kPa, and thickness is 0.01-0.05 μ m, and the material of this nucleating layer is Al xIn yGa 1-x-yN, wherein, x+y=1,0<x<1,0<y<1, this nucleating layer can increase the nucleation density of substrate surface;
Step 3: adopt metal-organic chemical vapor deposition equipment technology one deck buffer layer of grow on nucleating layer, this buffer layer can reduce the defect concentration of epitaxial film, the raising crystal mass;
Step 4: adopt metal-organic chemical vapor deposition equipment technology growing indium nitride monocrystal thin films on buffer layer, this indium nitride monocrystal thin films surfacing, crystal mass height.
2, the method for growing indium nitride monocrystal thin films according to claim 1 is characterized in that, wherein said substrate is sapphire or silicon carbide or silicon substrate.
3, the method for growing indium nitride monocrystal thin films according to claim 1 is characterized in that, the material of wherein said buffer layer is a gan.
4, the method for growing indium nitride monocrystal thin films according to claim 1 is characterized in that, wherein during the growing gallium nitride buffer layer, growth temperature is 900-1100 ℃, and growth pressure is 13.33-26.67kPa, and thickness is 1.00-2.00 μ m.
5, the method for growing indium nitride monocrystal thin films according to claim 1 is characterized in that, wherein during growing indium nitride monocrystal thin films, growth temperature is 400-650 ℃, and growth pressure is 13.33-26.67kPa, and growth thickness is 0.15-0.65 μ m.
CNB2007100629795A 2007-01-24 2007-01-24 The method of growing indium nitride monocrystal thin films Expired - Fee Related CN100558947C (en)

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CN101397693B (en) * 2008-10-28 2011-09-28 厦门乾照光电股份有限公司 Method for high quality single crystal indium nitride film growth
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CN108977887B (en) * 2018-07-20 2023-11-17 深圳市科创数字显示技术有限公司 Method for growing single crystal indium nitride

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563481A (en) * 2004-03-16 2005-01-12 南京大学 Method for growth of InN film through In deposition in advance
CN1704505A (en) * 2004-06-02 2005-12-07 中国科学院半导体研究所 Method for growing high-resistance gallium nitride epitaxial film
CN1704507A (en) * 2004-06-02 2005-12-07 中国科学院半导体研究所 Method for growing high crystal quality indium nitride single-crystal epitaxial film
CN1811018A (en) * 2005-12-15 2006-08-02 南京大学 Epitaxial growth process of high-crystallinity monocrystal indium nitride film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1563481A (en) * 2004-03-16 2005-01-12 南京大学 Method for growth of InN film through In deposition in advance
CN1704505A (en) * 2004-06-02 2005-12-07 中国科学院半导体研究所 Method for growing high-resistance gallium nitride epitaxial film
CN1704507A (en) * 2004-06-02 2005-12-07 中国科学院半导体研究所 Method for growing high crystal quality indium nitride single-crystal epitaxial film
CN1811018A (en) * 2005-12-15 2006-08-02 南京大学 Epitaxial growth process of high-crystallinity monocrystal indium nitride film

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