CN103352208B - The preparation method of ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film - Google Patents
The preparation method of ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film Download PDFInfo
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Abstract
The invention belongs to technical field of novel photoelectric material sediment preparation, provide a kind of and prepare the good InN optoelectronic film of electric property and the preparation method of the low ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film of cost.The present invention includes following steps: after 1) Si substrate being used acetone, ethanol and deionized water ultrasonic cleaning successively, dry up feeding reaction chamber with nitrogen; 2) use HF CVD system, reaction chamber is vacuumized, by Si substrate heating, in reaction chamber, pass into hydrogen and methane gas, Si substrate base obtains diamond thin.
Description
Technical field
The invention belongs to technical field of novel photoelectric material sediment preparation, particularly relate to the preparation method of a kind of ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film.
Background technology
Indium nitride (InN) is the important member in III group-III nitride, compares with GaN with AlN, and the mobility of InN and spike speed etc. are all the highest, and the application of the electron devices such as high-speed high frequency transistor has unique advantage; Its band gap at room temperature is positioned at near-infrared region, is also suitable for preparing the photoelectric devices such as high efficiency solar cell, semiconductor light-emitting-diode and optical communication device.But because InN decomposition temperature is low, require low growth temperature, and nitrogenous source decomposition temperature is high, so general InN film all grows 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, seriously hinders the development of InN material devices.
Summary of the invention
The present invention is exactly for the problems referred to above, provides a kind of and prepares the good InN optoelectronic film of electric property and the preparation method of the low ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film of cost.
For achieving the above object, the present invention adopts following technical scheme, the present invention includes following steps.
1), after Si substrate being used acetone, ethanol and deionized water ultrasonic cleaning successively, feeding reaction chamber is dried up with nitrogen.
2) use HF CVD system, reaction chamber is vacuumized, by Si substrate heating, in reaction chamber, pass into hydrogen and methane gas, Si substrate base obtains diamond thin.
3) adopt ECR-PEMOCVD system, vacuumized by reaction chamber, by substrate heating to 300 ~ 700 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is (2 ~ 4): (80 ~ 150); Controlling gas total pressure is 1.2 ~ 1.8Pa; Electron cyclotron resonace reaction 30min ~ 3h, obtains at the on-chip InN optoelectronic film of the Si of 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) be evacuated to 1.0 × 10
-2pa; Substrate heating to 800 DEG C; 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 DEG C of the present invention; The throughput ratio of trimethyl indium and nitrogen is 2:80; Controlling gas total pressure is 1.2Pa; Electron cyclotron resonace reaction 30min.
As another kind of preferred version, step 3) substrate heating to 400 DEG C of the present invention; The throughput ratio of trimethyl indium and nitrogen is 3:100; Controlling gas total pressure is 1.5Pa; Electron cyclotron resonace reaction 50min.
As another kind of preferred version, step 3) substrate heating to 500 DEG C of the present invention; The throughput ratio of trimethyl indium and nitrogen is 3:90; Controlling gas total pressure is 1.6Pa; Electron cyclotron resonace reaction 70min.
Secondly, step 3) substrate heating to 600 DEG C of the present invention; The throughput ratio of trimethyl indium and nitrogen is 2:150; Controlling gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 180min.
In addition, step 3) substrate heating to 700 DEG C of the present invention; The throughput ratio of trimethyl indium and nitrogen is 4:150; Controlling gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 150min.
Beneficial effect of the present invention.
The present invention deposited by HF CVD system before this and prepared diamond (diamond possesses very high thermal conductivity and excellent thermotolerance) thick film on Si, recycling accurately can control the ECR-PEMOCVD technology of low temperature depositing, and the correlation parameter in reaction process and material are selected, set, thus low temperature depositing prepares high-quality InN optoelectronic film on the Si substrate of gold-plated diamond thin film, cost is very low.In addition, the Si on-chip InN optoelectronic film product of the gold-plated diamond thin film of the present invention has good electric property and heat dispersion after tested, is easy to prepare the powerful device of high frequency.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.Scope is not only confined to the statement of following content.
Fig. 1 is the X ray diffracting spectrum of gold-plated diamond thin film on 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.
In Fig. 3,1 is Si substrate, and 2 is diamond thin, and 3 is InN sample thin film.
Embodiment
The present invention includes following steps.
1), after Si substrate being used acetone, ethanol and deionized water ultrasonic cleaning successively, feeding reaction chamber is dried up with nitrogen.
2) use HF CVD system, reaction chamber is vacuumized, by Si substrate heating, in reaction chamber, pass into hydrogen and methane gas, Si substrate base obtains diamond thin.
3) adopt ECR-PEMOCVD system, vacuumized by reaction chamber, by substrate heating to 300 ~ 700 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is (2 ~ 4): (80 ~ 150); Controlling gas total pressure is 1.2 ~ 1.8Pa; Electron cyclotron resonace reaction 30min ~ 3h, obtains at the on-chip InN optoelectronic film of the Si of 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) be evacuated to 1.0 × 10
-2pa; Substrate heating to 800 DEG C; 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 DEG C; The throughput ratio of trimethyl indium and nitrogen is 2:80; Controlling gas total pressure is 1.2Pa; Electron cyclotron resonace reaction 30min.
Described step 3) substrate heating to 400 DEG C; The throughput ratio of trimethyl indium and nitrogen is 3:100; Controlling gas total pressure is 1.5Pa; Electron cyclotron resonace reaction 50min.
Described step 3) substrate heating to 500 DEG C; The throughput ratio of trimethyl indium and nitrogen is 3:90; Controlling gas total pressure is 1.6Pa; Electron cyclotron resonace reaction 70min.
Described step 3) substrate heating to 600 DEG C; The throughput ratio of trimethyl indium and nitrogen is 2:150; Controlling gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 180min.
Described step 3) substrate heating to 700 DEG C; The throughput ratio of trimethyl indium and nitrogen is 4:150; Controlling gas total pressure is 1.8Pa; Electron cyclotron resonace reaction 150min.
Embodiment 1.
Used by Si substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up with nitrogen and send into HF CVD reaction chamber; HF CVD reaction chamber is evacuated to 1.0 × 10
-2pa, by substrate heating to 800 DEG C, passes into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min, Si substrate base obtains diamond thin.And then by diamond thin film substrate gold-plated on Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response room is evacuated to 8.0 × 10
-4pa, by substrate heating to 300 DEG C, passes into trimethyl indium (TMIn), nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2reaction source flow-ratio control is 2:80, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 2 sccm and 80sccm; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains at the on-chip InN optoelectronic film of gold-plated diamond thin film Si.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Because diamond is non-conductive, its electric property all comes from 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, mobility and carrier concentration better.The analysis of X-ray diffraction has been carried out to sample thin film, 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 InN film has good crystalline quality.Test result shows, the InN film of gold-plated diamond thin film Si substrate meets 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 gold-plated diamond thin film Si substrate | 43.8 | 0.93×10 20 |
Embodiment 2.
Used by Si substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up with nitrogen and send into HF CVD reaction chamber; HF CVD reaction chamber is evacuated to 1.0 × 10
-2pa, by substrate heating to 800 DEG C, passes into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min, Si substrate base obtains diamond thin.And then by diamond thin film substrate gold-plated on Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response room is evacuated to 8.0 × 10
-4pa, by substrate heating to 400 DEG C, passes into trimethyl indium (TMIn), nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2reaction source flow-ratio control is 3:100, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 3sccm and 100sccm; Controlling gas total pressure is 1.5Pa; Be 650W in electron cyclotron resonance frequency, reaction 50min, obtains at the on-chip InN optoelectronic film of gold-plated diamond thin film Si.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Because diamond is non-conductive, its electric property all comes from 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, mobility and carrier concentration better.Test result shows, the InN film of gold-plated diamond thin film Si substrate meets 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.
Embodiment 3.
Used by Si substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up with nitrogen and send into HF CVD reaction chamber; HF CVD reaction chamber is evacuated to 1.0 × 10
-2pa, by substrate heating to 800 DEG C, passes into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min, Si substrate base obtains diamond thin.And then by diamond thin film substrate gold-plated on Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response room is evacuated to 8.0 × 10
-4pa, by substrate heating to 500 DEG C, passes into trimethyl indium (TMIn), nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2reaction source flow-ratio control is 3:90, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 3sccm and 90sccm; Controlling gas total pressure is 1.6Pa; Be 650W in electron cyclotron resonance frequency, reaction 70min, obtains at the on-chip InN optoelectronic film of gold-plated diamond thin film Si.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Because diamond is non-conductive, its electric property all comes from 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, mobility and carrier concentration better.Test result shows, the InN film of gold-plated diamond thin film Si substrate meets 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.
Used by Si substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up with nitrogen and send into HF CVD reaction chamber; HF CVD reaction chamber is evacuated to 1.0 × 10
-2pa, by substrate heating to 800 DEG C, passes into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min, Si substrate base obtains diamond thin.And then by diamond thin film substrate gold-plated on Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response room is evacuated to 8.0 × 10
-4pa, by substrate heating to 600 DEG C, passes into trimethyl indium (TMIn), nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2reaction source flow-ratio control is 2:150, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 2sccm and 150sccm; Controlling gas total pressure is 1.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 180min, obtains at the on-chip InN optoelectronic film of gold-plated diamond thin film Si.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Because diamond is non-conductive, its electric property all comes from 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, mobility and carrier concentration better.Test result shows, the InN film of gold-plated diamond thin film Si substrate meets 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.
Used by Si substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up with nitrogen and send into HF CVD reaction chamber; HF CVD reaction chamber is evacuated to 1.0 × 10
-2pa, by substrate heating to 800 DEG C, passes into hydrogen and methane gas in reaction chamber, and flow both it is hydrogen be 200sccm and methane is 4sccm, is controlled by mass flowmeter; Heater voltage is 10V, and heater current is 50A, and reaction 30min, Si substrate base obtains diamond thin.And then by diamond thin film substrate gold-plated on Si, put into ECR-PEMOCVD system sediment chamber, ECR-PEMOCVD system response room is evacuated to 8.0 × 10
-4pa, by substrate heating to 700 DEG C, passes into trimethyl indium (TMIn), nitrogen (N that hydrogen carries in reaction chamber
2), wherein TMIn and N
2reaction source flow-ratio control is 4:150, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 4sccm and 150sccm; Controlling gas total pressure is 1.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 150min, obtains at the on-chip InN optoelectronic film of gold-plated diamond thin film Si.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Because diamond is non-conductive, its electric property all comes from 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, mobility and carrier concentration better.Test result shows, the InN film of gold-plated diamond thin film Si substrate meets 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 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, meets the requirement to diamond thin thermal diffusivity of InN film.
The electrical performance testing Hall test equipment of inventive samples, the model of Hall system is HL5500PC, and 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, the technical scheme described by the embodiment of the present invention is only not limited to for illustration of the present invention, those of ordinary skill in the art is to be understood that, still can modify to the present invention or equivalent replacement, to reach identical technique effect; Needs are used, all within protection scope of the present invention as long as meet.
Claims (4)
- The preparation method of 1.ECR-PEMOCVD low temperature depositing InN film on the Si of gold-plated diamond thin film, is characterized in that comprising the following steps:1) used by Si substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up feeding reaction chamber with nitrogen;2) use HF CVD system, reaction chamber is evacuated to 1.0 × 10 -2pa, by Si substrate heating to 800 DEG C, passes into hydrogen and methane gas in reaction chamber, and 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; Si substrate base obtains diamond thin;3) adopt ECR-PEMOCVD system, vacuumized by reaction chamber, by substrate heating to 300 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is 2:80; Controlling gas total pressure is 1.2Pa; Electron cyclotron resonace reaction 30min, obtains at the on-chip InN optoelectronic film of the Si of gold-plated diamond thin film.
- 2., according to the preparation method of the low temperature depositing InN film on the Si of gold-plated diamond thin film of ECR-PEMOCVD described in claim 1, it is characterized in that the purity of described trimethyl indium and the purity of nitrogen are 99.99%.
- 3., according to the preparation method of the low temperature depositing InN film on the Si of gold-plated diamond thin film of ECR-PEMOCVD described in claim 1, it is characterized in that the thickness of described diamond thin is 300nm.
- 4., according to the preparation method of the low temperature depositing InN film on the Si of gold-plated diamond thin film of ECR-PEMOCVD described in claim 1, it is characterized in that described step 3) vacuumizes 8.0 × 10 -4pa; The flow of trimethyl indium, nitrogen is controlled by mass flowmeter; Electron cyclotron resonace power is 650W.
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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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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 |
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 |
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 |
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