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CN110517950B - A kind of method for preparing zinc blende GaN thin film on diamond substrate - Google Patents

A kind of method for preparing zinc blende GaN thin film on diamond substrate Download PDF

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CN110517950B
CN110517950B CN201910686402.4A CN201910686402A CN110517950B CN 110517950 B CN110517950 B CN 110517950B CN 201910686402 A CN201910686402 A CN 201910686402A CN 110517950 B CN110517950 B CN 110517950B
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diamond substrate
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nucleation layer
mbar
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李天保
于斌
张哲�
贾伟
余春燕
董海亮
贾志刚
许并社
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Taiyuan University of Technology
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Abstract

The invention belongs to the technical field of GaN film preparation, and provides a method for preparing a sphalerite GaN film on a diamond substrate. First, XeF is used for diamond substrate2Carrying out fluorination treatment on the plasma, and forming a C-F bond on the surface of the diamond after treatment, wherein the C-F bond is used as a nucleation site; then placing the diamond substrate in an MOCVD reaction chamber to grow a GaN nucleation layer, annealing the nucleation layer, and finally merging and growing to form the zincblende GaN film. The method for growing the sphalerite GaN film by taking the diamond as the heat sink substrate has important significance for realizing the GaN-based high-efficiency green light LED device and heat dissipation thereof.

Description

Method for preparing sphalerite GaN film on diamond substrate
Technical Field
The invention belongs to the technical field of GaN film preparation, and particularly relates to a method for preparing a sphalerite GaN film on a diamond substrate.
Background
The sphalerite GaN is a semiconductor material with a nonpolar structure, and spontaneous polarization does not exist, so that the epitaxial light-emitting structure prepared from the sphalerite GaN can avoid quantum confinement Stark effect. Secondly, compared with a wurtzite GaN structure, the band gap of the sphalerite GaN structure is narrow, green light emission can be realized only by doping a small amount of indium, and the problem of low green light effect, namely 'green gap' in the existing full-color LED is favorably solved.
As the photovoltaic power device made of GaN-based materials develops in the direction of smaller size, larger output power and higher frequency, the problem of "heat" becomes more and more prominent, and gradually becomes a bottleneck that restricts the device from being improved to higher performance. Diamond has excellent thermal properties with thermal conductivity values up to 2000W/m.K. The high-thermal conductivity diamond is used as a substrate or a heat sink of a high-frequency and high-power GaN-based device, so that the self-heating effect of the GaN-based high-power device can be reduced, and the problem of rapid reduction of power density along with increase of total power and increase of frequency is hopefully solved. In 2003, Felix Ejeckam realized diamond-based gallium nitride for the first time by transferring a GaN epitaxial layer grown on a silicon substrate onto a diamond substrate synthesized by chemical vapor deposition; but the preparation method is comparatively complicated and has high process cost. In 2009, songming et al proposed diamond-based LED structures in patents, but they did not propose a specific fabrication method. In 2013, zhang dong et al, Shenyang engineering college, proposed the use of an electron cyclotron resonance-plasma enhanced metal organic chemical vapor deposition (ECR-PEMOCVD) system to produce InN/GaN/diamond structures.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing a sphalerite GaN film on a diamond substrate.
The invention is realized by the following technical scheme: a method for preparing zinc blende GaN film on diamond substrate comprises applying XeF to diamond substrate2Carrying out fluorination treatment on the plasma, and forming a C-F bond on the surface of the diamond after treatment, wherein the C-F bond is used as a nucleation site; then placing the diamond substrate in an MOCVD reaction chamber to grow a GaN nucleation layer, annealing the nucleation layer, and finally merging and growing to form the zincblende GaN film.
The method comprises the following specific steps:
(1) fluoridation processing the diamond substrate: the pressure of the diamond substrate fluorination treatment is 20-100 mbar, the power is 100-2Plasma treatment for 150-; forming C-F bonds on the surface of the diamond after treatment, and using the C-F bonds as nucleation sites to nucleate GaN on the surface of the diamond;
(2) growing a GaN nucleation layer: placing the diamond substrate into an MOCVD reaction chamber, and performing reaction at 1200 ℃ and under the pressure of 120-2Cleaning for 10-15 min in atmosphere; after cleaning, the temperature is reduced to 500-650 ℃, and NH is introduced under 400-600 mbar3And trimethyl gallium (TMGa), the V/III ratio is 600-800, the growth time is 200-300 s, and a compact nucleation layer is obtained;
(3) annealing treatment: heating to 1100-1200 deg.C and 300-450 mbar, NH3Carrying out high-temperature annealing on the GaN nucleation layer for 2-6 min as an annealing atmosphere;
(4) growing a zinc blende GaN film: NH is introduced at 1050 ℃ and 1150 ℃ and under the pressure of 100 ℃ and 150mbar3And TMGa, the V/III ratio is 300-800, and the GaN film is grown in a combined mode for 2-3 h.
The invention has the following beneficial effects:
when the LED photoelectric device operates under high power and high frequency, the light efficiency of the device is reduced and the service life of the device is shortened due to insufficient heat dissipation. The diamond has high thermal conductivity, and when the diamond is selected as the heat sink substrate of the photoelectric device, the problem of insufficient heat dissipation can be effectively overcome. According to the invention, the diamond is used as the heat sink substrate to grow the zinc blende GaN film, so that on one hand, a foundation is laid for further preparing a photoelectric device made of the zinc blende GaN-based film material, and the problem of low green light efficiency in the existing full-color LED is solved; on the other hand, the heat dissipation problem of the photoelectric device under the high-power and high-frequency operation is also solved.
Drawings
FIG. 1 is a schematic diagram of the growth process of preparing a zincblende GaN film by using a diamond substrate according to the invention.
FIG. 2 AFM image of the surface of the sample of example 1.
Figure 3X-ray diffraction pattern (XRD) of the sample of example 1.
Detailed Description
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, which illustrate process flows of various embodiments, and which are not intended to be limiting of the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the invention to those skilled in the art. The present invention will be described more specifically with reference to the following embodiments with reference to the accompanying drawings.
Example 1: a method for preparing zinc blende GaN film on diamond substrate comprises applying XeF to diamond substrate2Carrying out fluorination treatment on the plasma, and forming a C-F bond on the surface of the diamond after treatment, wherein the C-F bond is used as a nucleation site; then placing the diamond substrate in an MOCVD reaction chamber to grow a GaN nucleation layer, annealing the nucleation layer, and finally merging and growing to form the zincblende GaN film. The method comprises the following specific steps:
1) fluoridation processing the diamond substrate: subjecting the diamond substrate to a fluorination treatment at a pressure of 50mbar and a power of 100 mW using XeF2Plasma treatment 150 s.
2) Growing a GaN nucleation layer: placing the diamond substrate in MOCVD reaction chamber, and heating at 1200 deg.C under 150mbar pressure H2The cleaning step was carried out in an atmosphere for 10 min. After the cleaning step, the temperature is reduced to 500 ℃, a GaN nucleation layer grows on the surface of the diamond substrate under the pressure of 400 mbar, and NH is introduced3And TMGa with flow rates of 20000 mu mol/min and 30 mu mol/min, respectively, a V/III ratio of 600, and a growth time of 200 s.
3) Annealing treatment: heating to 1100 deg.C, annealing GaN nucleation layer at 300mbar for 4 min while introducing NH3The flow rate was 360000. mu. mol/min.
4) Growing a zinc blende GaN film: controlling the temperature at 1050 deg.C, further growing GaN film under 100mbar, introducing NH3And TMGa flow rate of 10000 mol/min and 26 mu mol/min respectively, V/III ratio of 300, and growth time of 2 h.
The surface morphology and the structure of the samples of the zincblende GaN thin film grown on diamond in example 1 were analyzed, respectively. FIG. 2 is an Atomic Force Microscopy (AFM) image of the surface topography and flatness of a sample, from which it can be seen that the atomic level step laminar flow reflects a very flat surface with a root mean square Roughness (RMS) measurement of only 0.31 nm. FIG. 3 is an analysis pattern (XRD) of a sample X-ray diffractometer, and it can be seen from the pattern that the sample orientation is good, the sample grows mainly in the direction perpendicular to the zincblende (200) plane, and the maximum half-peak width of the (200) plane is narrow, indicating that the zincblende GaN thin film has high crystal quality.
Example 2: a method for preparing a sphalerite GaN film on a diamond substrate comprises the following specific steps:
1) fluoridation processing the diamond substrate: subjecting the diamond substrate to a fluorination treatment at a pressure of 100mbar and a power of 300mW using XeF2Plasma treatment is carried out for 250 s.
2) Growing a GaN nucleation layer: placing the diamond substrate in MOCVD reaction chamber, and heating at 1200 deg.C under 200 mbar pressure H2The cleaning step was carried out in an atmosphere for 15 min. After the cleaning step, the temperature is reduced to 650 ℃, a GaN nucleation layer grows on the surface of the diamond substrate under the pressure of 600 mbar, and NH is introduced3And TMGa flow rates were 26600. mu. mol/min, 36. mu. mol/min, V/III ratio was 800, and growth time was 300s, respectively.
3) Annealing treatment: heating to 1200 deg.C, annealing GaN nucleation layer at 450 mbar for 6 min while introducing NH3The flow rate was 630000. mu. mol/min.
4) Growing a zinc blende GaN film: controlling the temperature at 1150 deg.C, further growing GaN film at 150mbar, introducing NH3And TMGa flow rate of 20000 mu mol/min and 30 mu mol/min respectively, V/III ratio of 800, and growth time of 2.5 h.
Example 3: a method for preparing a sphalerite GaN film on a diamond substrate comprises the following specific steps:
1) fluoridation processing the diamond substrate: subjecting the diamond substrate to a fluorination treatment at a pressure of 20 mbar and a power of 200mW using XeF2Plasma treatment is carried out for 200 s.
2) Growing a GaN nucleation layer: placing the diamond substrate in MOCVD reaction chamber, and heating at 1200 deg.C under 120 mbar pressure H2The cleaning step was carried out in an atmosphere for 13 min. After the cleaning step, the temperature is reduced to 550 ℃, a GaN nucleation layer grows on the surface of the diamond substrate under the pressure of 500 mbar, and NH is introduced3And TMGa flow rates of 23000. mu. mol/min and 33. mu. mol/min, respectively, a V/III ratio of 700, and a growth time of 250 s.
3) Annealing treatment: heating to 1150 deg.C for 400 mHigh-temperature annealing the GaN nucleation layer for 2 min under bar, introducing NH during annealing3The flow rate was 450000. mu. mol/min.
4) Growing a zinc blende GaN film: controlling the temperature at 1100 deg.C, further growing GaN film under 130 mbar, introducing NH3And TMGa at 15000. mu. mol/min and 28. mu. mol/min, respectively, a V/III ratio of 500 and a growth time of 3 hours.

Claims (1)

1.一种在金刚石衬底上制备闪锌矿GaN薄膜的方法，其特征在于：先对金刚石衬底用XeF2等离子体进行氟化处理，处理后的金刚石表面形成C-F键，C-F键作为形核位点；然后将金刚石衬底置于MOCVD反应室内生长GaN形核层，再对形核层退火处理，最后合并生长形成闪锌矿GaN薄膜；1. a method for preparing zinc blende GaN thin film on diamond substrate, it is characterized in that: first to diamond substrate with XeF plasma is carried out fluorination treatment, the diamond surface after treatment forms CF bond, and CF bond is used as shape. Nucleation site; then place the diamond substrate in the MOCVD reaction chamber to grow the GaN nucleation layer, then anneal the nucleation layer, and finally merge and grow to form a sphalerite GaN film; 具体步骤如下：Specific steps are as follows: （1）氟化处理金刚石衬底：金刚石衬底氟化处理的压力为20-100 mbar，功率为100-300mW，用XeF2等离子体处理150-250s；处理后金刚石表面形成C-F键，作为形核位点，使GaN在金刚石表面形核；(1) Fluorination treatment of diamond substrate: The pressure of the fluorination treatment of the diamond substrate is 20-100 mbar, the power is 100-300 mW, and the XeF 2 plasma is used for 150-250 s; Nucleation sites, allowing GaN to nucleate on the diamond surface; （2）生长GaN形核层：金刚石衬底放入MOCVD反应室中，在1200℃的温度，120-200 mbar压力下， H2气氛中进行清洗步骤10-15 min；清洗后，降温至 500-650℃，400-600 mbar下在金刚石衬底表面生长GaN形核层，通入NH3和TMGa的流量分别为20000-26600 μmol/min和30-36 μmol/min， V/III比为600-800，生长时间为200-300 s，获得致密形核层；(2) Growth of GaN nucleation layer: The diamond substrate is placed in the MOCVD reaction chamber, and the cleaning step is carried out at a temperature of 1200 °C, a pressure of 120-200 mbar, and a H 2 atmosphere for 10-15 min; after cleaning, the temperature is lowered to 500 -650℃, GaN nucleation layer was grown on the surface of diamond substrate at 400-600 mbar, the flow rates of NH 3 and TMGa were 20000-26600 μmol/min and 30-36 μmol/min, respectively, and the V/III ratio was 600 -800, the growth time is 200-300 s, and a dense nucleation layer is obtained; （3）退火处理：升温至1100-1200℃，300-450 mbar下对GaN形核层进行高温退火2-6min，退火时通入的NH3流量为360000-630000 μmol/min；(3) Annealing treatment: the temperature is raised to 1100-1200 °C, and the GaN nucleation layer is annealed at a high temperature of 300-450 mbar for 2-6 min. The NH 3 flow rate during annealing is 360000-630000 μmol/min; （4）生长闪锌矿GaN薄膜：温度控制在1050-1150℃，100-150 mbar下合并生长GaN薄膜，通入NH3和TMGa的流量分别10000-20000 mol/min、26-30 μmol/min，V/III比为300-800，生长时间为2-3 h。(4) Growth of sphalerite GaN film: the temperature is controlled at 1050-1150°C, and the GaN film is grown in combination at 100-150 mbar, and the flow rates of NH 3 and TMGa are 10000-20000 mol/min and 26-30 μmol/min, respectively. , the V/III ratio was 300-800, and the growth time was 2-3 h.
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