CN103352208A - Preparation method for InN film low temperature sedimentation on diamond plated film by adopting ECR-PEMOCVD - Google Patents
Preparation method for InN film low temperature sedimentation on diamond plated film by adopting ECR-PEMOCVD Download PDFInfo
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Abstract
The invention belongs to the technical field of novel photoelectric material sediment preparation, and provides a preparation method for the InN film low temperature sedimentation on diamond plated film by adopting the ECR-PEMOCVD. The method can be used for preparing an InN photoelectric film which has excellent electric performance and is low in cost, and comprises the following steps: 1), a Si substrate is subjected to ultrasonic cleaning by acetone, ethanol, and deionized water sequentially, and then is blow-dried by nitrogen gas and sent to a reaction chamber; 2), the reaction chamber is vacuumized by adopting a hot wire CVD (chemical vapor deposition) system, the substrate is heated, hydrogen and methane gas are introduced into the reaction chamber, and the diamond film can be obtained on the Si substrate.
Description
Technical field
The invention belongs to novel photoelectric deposition of material preparing technical field, relate in particular to a kind of ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film.
Background technology
Indium nitride (InN) is the important member in the III group-III nitride, compares with AlN with GaN, and the mobility of InN and spike speed etc. all is the highest, in the application of the electron devices such as high-speed high frequency transistor unique advantage is arranged; Its room temperature band gap is positioned at the near-infrared region, also is suitable for preparing the photoelectric devices such as high efficiency solar cell, semiconductor light-emitting-diode and optical communication device.But because the InN decomposition temperature is low, require low growth temperature, and the nitrogenous source decomposition temperature is high, so general InN film all is grown on some substrates such as sapphire.As everyone knows, the price of sapphire substrate is higher, uses it as the substrate of InN material, makes the cost of the device of InN material base be difficult to lower, and has seriously hindered the development of InN material devices.
Summary of the invention
The present invention is exactly for the problems referred to above, and a kind of good InN optoelectronic film of electric property and low ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film of cost of preparing is provided.
For achieving the above object, the present invention adopts following technical scheme, the present invention includes following steps.
1) the Si substrate is used acetone, ethanol and deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into reaction chamber.
2) with heated filament CVD system, reaction chamber is vacuumized, with the Si substrate heating, in reaction chamber, pass into hydrogen and methane gas, obtain diamond thin at the Si substrate base.
3) adopt the ECR-PEMOCVD system, reaction chamber is vacuumized, with substrate heating to 300～700 ℃, pass into trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, its two throughput ratio is (2～4): (80～150); Control gas total pressure is 1.2～1.8Pa; Electron cyclotron resonace reaction 30min～3h, the on-chip InN optoelectronic film of the Si that obtains at gold-plated diamond thin film.
As a kind of preferred version, the purity of trimethyl indium of the present invention and the purity of nitrogen are 99.99%.
As another kind of preferred version, the thickness of diamond thin of the present invention is 300nm.
As another kind of preferred version, step 1) ultrasonic cleaning of the present invention 5 minutes; Step 2) is evacuated to 1.0 * 10
-2Pa; Substrate heating to 800 ℃; Hydrogen and methane gas flow are respectively 200sccm and 4sccm, are controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, reaction 30min.
As another kind of preferred version, step 3) of the present invention is evacuated to 8.0 * 10
-4Pa; The flow of trimethyl indium, nitrogen is controlled by mass flowmeter; Electron cyclotron resonace power is 650W.
As another kind of preferred version, step 3) substrate heating to 300 of the present invention ℃; The throughput ratio of trimethyl indium and nitrogen is 2:80; Control gas total pressure is 1.2Pa; Electron cyclotron resonace reaction 30min.
As another kind of preferred version, step 3) substrate heating to 400 of the present invention ℃; The throughput ratio of trimethyl indium and nitrogen is 3:100; Control gas total pressure is 1.5Pa; Electron cyclotron resonace reaction 50min.
As another kind of preferred version, step 3) substrate heating to 500 of the present invention ℃; The throughput ratio of trimethyl indium and nitrogen is 3:90; Control gas total pressure is 1.6Pa; Electron cyclotron resonace reaction 70min.
Secondly, step 3) substrate heating to 600 of the present invention ℃; The throughput ratio of trimethyl indium and nitrogen is 2:150; Control gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 180min.
In addition, step 3) substrate heating to 700 of the present invention ℃; The throughput ratio of trimethyl indium and nitrogen is 4:150; Control gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 150min.
Beneficial effect of the present invention.
The present invention prepared diamond (diamond possesses very high thermal conductivity and good thermotolerance) thick film with heated filament CVD system in the Si deposition before this, recycling can accurately be controlled the ECR-PEMOCVD technology of low temperature depositing, and the correlation parameter in the reaction process and material selected, set, thereby low temperature depositing is prepared high-quality InN optoelectronic film on the Si of gold-plated diamond thin film substrate, and cost is very low.In addition, the on-chip InN optoelectronic film of the Si of the gold-plated diamond thin film of the present invention product has good electric property and heat dispersion after tested, is easy to prepare the powerful device of high frequency.
Description of drawings
The present invention will be further described below in conjunction with the drawings and specific embodiments.Protection domain of the present invention not only is confined to the statement of following content.
Fig. 1 is the X ray diffracting spectrum of gold-plated diamond thin film on the Si substrate.
Fig. 2 is the X ray diffracting spectrum of InN/diamond/Si structure.
Fig. 3 is the InN/diamond/Si structural membrane schematic diagram that the inventive method obtains.
1 is the Si substrate among Fig. 3, and 2 is diamond thin, and 3 is the InN sample thin film.
Embodiment
The present invention includes following steps.
1) the Si substrate is used acetone, ethanol and deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into reaction chamber.
2) with heated filament CVD system, reaction chamber is vacuumized, with the Si substrate heating, in reaction chamber, pass into hydrogen and methane gas, obtain diamond thin at the Si substrate base.
3) adopt the ECR-PEMOCVD system, reaction chamber is vacuumized, with substrate heating to 300～700 ℃, pass into trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, its two throughput ratio is (2～4): (80～150); Control gas total pressure is 1.2～1.8Pa; Electron cyclotron resonace reaction 30min～3h, the on-chip InN optoelectronic film of the Si that obtains at gold-plated diamond thin film.
The purity of described trimethyl indium and the purity of nitrogen are 99.99%.
The thickness of described diamond thin is 300nm.
Described step 1) ultrasonic cleaning 5 minutes; Step 2) is evacuated to 1.0 * 10
-2Pa; Substrate heating to 800 ℃; Hydrogen and methane gas flow are respectively 200sccm and 4sccm, are controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, reaction 30min.
Described step 3) is evacuated to 8.0 * 10
-4Pa; The flow of trimethyl indium, nitrogen is controlled by mass flowmeter; Electron cyclotron resonace power is 650W.
Described step 3) substrate heating to 300 ℃; The throughput ratio of trimethyl indium and nitrogen is 2:80; Control gas total pressure is 1.2Pa; Electron cyclotron resonace reaction 30min.
Described step 3) substrate heating to 400 ℃; The throughput ratio of trimethyl indium and nitrogen is 3:100; Control gas total pressure is 1.5Pa; Electron cyclotron resonace reaction 50min.
Described step 3) substrate heating to 500 ℃; The throughput ratio of trimethyl indium and nitrogen is 3:90; Control gas total pressure is 1.6Pa; Electron cyclotron resonace reaction 70min.
Described step 3) substrate heating to 600 ℃; The throughput ratio of trimethyl indium and nitrogen is 2:150; Control gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 180min.
Described step 3) substrate heating to 700 ℃; The throughput ratio of trimethyl indium and nitrogen is 4:150; Control gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 150min.
Embodiment 1.
Use successively acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes the Si substrate, dry up with nitrogen and send into heated filament CVD reaction chamber; Heated filament CVD reaction chamber is evacuated to 1.0 * 10
-2Pa with substrate heating to 800 ℃, passes into hydrogen and methane gas in reaction chamber, its two flow is that hydrogen is that 200sccm and methane are 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min obtains diamond thin at the Si substrate base.And then with the upper gold-plated diamond thin film substrate of Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response chamber is evacuated to 8.0 * 10
-4Pa with substrate heating to 300 ℃, passes into trimethyl indium (TMIn), the nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2The reaction source flow-ratio control is 2:80, and by quality flowmeter flow quantity control, flow parameter is respectively 2 sccm and 80sccm; Control gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min obtains the on-chip InN optoelectronic film at gold-plated diamond thin film Si.
After finishing, experiment adopt the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Because diamond is non-conductive, its electric property all comes from the InN film.Its result is as shown in table 1, and on-chip its electric property of InN film of gold-plated diamond thin film Si is good as can be seen from Table 1, and mobility and carrier concentration are better.Sample thin film has been carried out the analysis of X-ray diffraction, as shown in Figure 2, its result shows that ECR-PEMOCVD system low temperature depositing InN optoelectronic film on gold-plated diamond thin film Si substrate has good preferred orientation structure, shows that the InN film has preferably crystalline quality.Test result shows, the InN film of gold-plated diamond thin film Si substrate satisfies high frequency, and high power device is to the requirement of film quality.
The electric property of table 1 ECR-PEMOCVD low temperature depositing InN on gold-plated diamond thin film Si substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on the gold-plated diamond thin film Si substrate | 43.8 | 0.93×10 20 |
Use successively acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes the Si substrate, dry up with nitrogen and send into heated filament CVD reaction chamber; Heated filament CVD reaction chamber is evacuated to 1.0 * 10
-2Pa with substrate heating to 800 ℃, passes into hydrogen and methane gas in reaction chamber, its two flow is that hydrogen is that 200sccm and methane are 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min obtains diamond thin at the Si substrate base.And then with the upper gold-plated diamond thin film substrate of Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response chamber is evacuated to 8.0 * 10
-4Pa with substrate heating to 400 ℃, passes into trimethyl indium (TMIn), the nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2The reaction source flow-ratio control is 3:100, and by quality flowmeter flow quantity control, flow parameter is respectively 3sccm and 100sccm; Control gas total pressure is 1.5Pa; Be 650W in electron cyclotron resonance frequency, reaction 50min obtains the on-chip InN optoelectronic film at gold-plated diamond thin film Si.
After finishing, experiment adopt the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Because diamond is non-conductive, its electric property all comes from the InN film.Its result is as shown in table 2, and on-chip its electric property of InN film of gold-plated diamond thin film Si is good as can be seen from Table 2, and mobility and carrier concentration are better.Test result shows, the InN film of gold-plated diamond thin film Si substrate satisfies high frequency, and high power device is to the requirement of film quality.
The electric property of table 2 ECR-PEMOCVD low temperature depositing InN on gold-plated diamond thin film Si substrate.
Use successively acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes the Si substrate, dry up with nitrogen and send into heated filament CVD reaction chamber; Heated filament CVD reaction chamber is evacuated to 1.0 * 10
-2Pa with substrate heating to 800 ℃, passes into hydrogen and methane gas in reaction chamber, its two flow is that hydrogen is that 200sccm and methane are 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min obtains diamond thin at the Si substrate base.And then with the upper gold-plated diamond thin film substrate of Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response chamber is evacuated to 8.0 * 10
-4Pa with substrate heating to 500 ℃, passes into trimethyl indium (TMIn), the nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2The reaction source flow-ratio control is 3:90, and by quality flowmeter flow quantity control, flow parameter is respectively 3sccm and 90sccm; Control gas total pressure is 1.6Pa; Be 650W in electron cyclotron resonance frequency, reaction 70min obtains the on-chip InN optoelectronic film at gold-plated diamond thin film Si.
After finishing, experiment adopt the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Because diamond is non-conductive, its electric property all comes from the InN film.Its result is as shown in table 3, and on-chip its electric property of InN film of gold-plated diamond thin film Si is good as can be seen from Table 3, and mobility and carrier concentration are better.Test result shows, the InN film of gold-plated diamond thin film Si substrate satisfies high frequency, and high power device is to the requirement of film quality.
The electric property of table 3 ECR-PEMOCVD low temperature depositing InN on gold-plated diamond thin film Si substrate.
Embodiment 4.
Use successively acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes the Si substrate, dry up with nitrogen and send into heated filament CVD reaction chamber; Heated filament CVD reaction chamber is evacuated to 1.0 * 10
-2Pa with substrate heating to 800 ℃, passes into hydrogen and methane gas in reaction chamber, its two flow is that hydrogen is that 200sccm and methane are 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min obtains diamond thin at the Si substrate base.And then with the upper gold-plated diamond thin film substrate of Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response chamber is evacuated to 8.0 * 10
-4Pa with substrate heating to 600 ℃, passes into trimethyl indium (TMIn), the nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2The reaction source flow-ratio control is 2:150, and by quality flowmeter flow quantity control, flow parameter is respectively 2sccm and 150sccm; Control gas total pressure is 1.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 180min obtains the on-chip InN optoelectronic film at gold-plated diamond thin film Si.
After finishing, experiment adopt the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Because diamond is non-conductive, its electric property all comes from the InN film.Its result is as shown in table 4, and on-chip its electric property of InN film of gold-plated diamond thin film Si is good as can be seen from Table 4, and mobility and carrier concentration are better.Test result shows, the InN film of gold-plated diamond thin film Si substrate satisfies high frequency, and high power device is to the requirement of film quality.
The electric property of table 4 ECR-PEMOCVD low temperature depositing InN on gold-plated diamond thin film Si substrate.
Embodiment 5.
Use successively acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes the Si substrate, dry up with nitrogen and send into heated filament CVD reaction chamber; Heated filament CVD reaction chamber is evacuated to 1.0 * 10
-2Pa with substrate heating to 800 ℃, passes into hydrogen and methane gas in reaction chamber, its two flow is that hydrogen is that 200sccm and methane are 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min obtains diamond thin at the Si substrate base.And then with the upper gold-plated diamond thin film substrate of Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response chamber is evacuated to 8.0 * 10
-4Pa with substrate heating to 700 ℃, passes into trimethyl indium (TMIn), the nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2The reaction source flow-ratio control is 4:150, and by quality flowmeter flow quantity control, flow parameter is respectively 4sccm and 150sccm; Control gas total pressure is 1.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 150min obtains the on-chip InN optoelectronic film at gold-plated diamond thin film Si.
After finishing, experiment adopt the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Because diamond is non-conductive, its electric property all comes from the InN film.Its result is as shown in table 5, and on-chip its electric property of InN film of gold-plated diamond thin film Si is good as can be seen from Table 5, and mobility and carrier concentration are better.Test result shows, the InN film of gold-plated diamond thin film Si substrate satisfies high frequency, and high power device is to the requirement of film quality.
The electric property of table 5 ECR-PEMOCVD low temperature depositing InN on gold-plated diamond thin film Si substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on the gold-plated diamond thin film Si substrate | 26.5 | 1.72×10 20 |
As shown in Figure 1, vertical diamond thin is polycrystalline, has preferred orientation, and quality is good, satisfies the requirement to the diamond thin thermal diffusivity of InN film.
The electrical performance testing of sample of the present invention Hall testing apparatus, the model of Hall system is HL5500PC, range is 0.1 Ohm/square-100 GOhm/square).
The model of X-ray diffraction analysis instrument is: the model of XRD test is Bruker AXS D8.
Be understandable that, above about specific descriptions of the present invention, only for the present invention being described and being not to be subject to the described technical scheme of the embodiment of the invention, those of ordinary skill in the art is to be understood that, still can make amendment or be equal to replacement the present invention, to reach identical technique effect; Use needs as long as satisfy, all within protection scope of the present invention.
Claims (10)
1.ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film is characterized in that may further comprise the steps:
1) the Si substrate is used acetone, ethanol and deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into reaction chamber;
2) with heated filament CVD system, reaction chamber is vacuumized, with the Si substrate heating, in reaction chamber, pass into hydrogen and methane gas, obtain diamond thin at the Si substrate base;
3) adopt the ECR-PEMOCVD system, reaction chamber is vacuumized, with substrate heating to 300～700 ℃, pass into trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, its two throughput ratio is (2～4): (80～150); Control gas total pressure is 1.2～1.8Pa; Electron cyclotron resonace reaction 30min～3h, the on-chip InN optoelectronic film of the Si that obtains at gold-plated diamond thin film.
2. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that the purity of described trimethyl indium and the purity of nitrogen are 99.99%.
3. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1, the thickness that it is characterized in that described diamond thin is 300nm.
4. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 1) ultrasonic cleaning 5 minutes; Step 2) is evacuated to 1.0 * 10
-2Pa; Substrate heating to 800 ℃; Hydrogen and methane gas flow are respectively 200sccm and 4sccm, are controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, reaction 30min.
5. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 3) is evacuated to 8.0 * 10
-4Pa; The flow of trimethyl indium, nitrogen is controlled by mass flowmeter; Electron cyclotron resonace power is 650W.
6. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 3) substrate heating to 300 ℃; The throughput ratio of trimethyl indium and nitrogen is 2:80; Control gas total pressure is 1.2Pa; Electron cyclotron resonace reaction 30min.
7. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 3) substrate heating to 400 ℃; The throughput ratio of trimethyl indium and nitrogen is 3:100; Control gas total pressure is 1.5Pa; Electron cyclotron resonace reaction 50min.
8. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 3) substrate heating to 500 ℃; The throughput ratio of trimethyl indium and nitrogen is 3:90; Control gas total pressure is 1.6Pa; Electron cyclotron resonace reaction 70min.
9. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 3) substrate heating to 600 ℃; The throughput ratio of trimethyl indium and nitrogen is 2:150; Control gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 180min.
10. described ECR-PEMOCVD low temperature depositing InN thin film technology method on the Si of gold-plated diamond thin film according to claim 1 is characterized in that described step 3) substrate heating to 700 ℃; The throughput ratio of trimethyl indium and nitrogen is 4:150; Control gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 150min.
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| US20080206569A1 (en) * | 2005-03-21 | 2008-08-28 | Andrew John Whitehead | Diamond Based Substrate for Electronic Device |
| CN102185583A (en) * | 2011-03-16 | 2011-09-14 | 大连理工大学 | AlN/GaN/freestanding diamond structured surface acoustic wave (SAW) device and preparation method thereof |
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| CN103014654A (en) * | 2012-12-27 | 2013-04-03 | 沈阳工程学院 | Preparation method of AlN/ZnO/InGaN/diamond/Si multilayer-structure surface acoustic wave filter |
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| US20080206569A1 (en) * | 2005-03-21 | 2008-08-28 | Andrew John Whitehead | Diamond Based Substrate for Electronic Device |
| CN102185583A (en) * | 2011-03-16 | 2011-09-14 | 大连理工大学 | AlN/GaN/freestanding diamond structured surface acoustic wave (SAW) device and preparation method thereof |
| CN103014655A (en) * | 2012-12-27 | 2013-04-03 | 沈阳工程学院 | Preparation method of Ga/Al-codoped ZnO film by ECR-PEMOCVD (electron cyclotron resonance-plasma-enhanced metal-organic chemical vapor deposition) low-temperature deposition |
| CN103014654A (en) * | 2012-12-27 | 2013-04-03 | 沈阳工程学院 | Preparation method of AlN/ZnO/InGaN/diamond/Si multilayer-structure surface acoustic wave filter |
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