CN103334089B - The preparation method of ECR-PEMOCVD low temperature depositing InN film on Diamond wafer - Google Patents
The preparation method of ECR-PEMOCVD low temperature depositing InN film on Diamond wafer Download PDFInfo
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Abstract
The invention belongs to technical field of novel photoelectric material sediment preparation, a kind of preparation method preparing ECR-PEMOCVD low temperature depositing InN film on Diamond wafer of the InN optoelectronic film that electric property is good, heat dispersion is good is provided.The present invention includes following steps: after 1) Diamond wafer substrate being used acetone, ethanol, deionized water ultrasonic cleaning successively, dry up feeding reaction chamber with nitrogen; 2) ECR-PEMOCVD system is adopted, reaction chamber is vacuumized, substrate heating to 20 ~ 600 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed into again in reaction chamber, trimethyl indium and nitrogen flow are than being (1 ~ 2): (100 ~ 200), controlling gas total pressure is 0.8 ~ 2.0Pa, and electron cyclotron resonace reaction 30min ~ 3h, obtains the InN optoelectronic film at Diamond wafer substrate.
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 Diamond wafer.
Background technology
Indium nitride (InN) is the important member in III group-III nitride.As compared to GaN with AlN, 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, because nitrogenous source decomposition temperature is high and lack the problems such as suitable substrate material, particularly to weather resistance and the heat dissipation problem of the device of high power, high, limit the device application of InN.
Summary of the invention
The present invention is exactly for the problems referred to above, provides a kind of preparation method preparing ECR-PEMOCVD low temperature depositing InN film on Diamond wafer of the InN optoelectronic film that electric property is good, heat dispersion is good.
For achieving the above object, the present invention adopts following technical scheme, the present invention includes following steps.
1), after Diamond wafer substrate being used acetone, ethanol, deionized water ultrasonic cleaning successively, feeding reaction chamber is dried up with nitrogen.
2) ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition is adopted, China Patent No. can be adopted to be 01101424.5, name is called equipment disclosed in " electronically cyclic resonating, microwave plasma reinforcing and metal and organic chemically vapor-phase depositing epitaxial system and technology ") system, reaction chamber is vacuumized, substrate heating to 20 ~ 600 DEG C, the trimethyl indium that hydrogen carries is passed into again in reaction chamber, nitrogen, trimethyl indium and nitrogen flow are than being (1 ~ 2): (100 ~ 200), controlling gas total pressure is 0.8 ~ 2.0Pa, electron cyclotron resonace reaction 30min ~ 3h, obtain the InN optoelectronic film at Diamond wafer substrate.
As a kind of preferred version, Diamond wafer substrate of the present invention prepares under the reaction source condition of methane and hydrogen in HF CVD system, and free standing diamond thickness is 1mm.
As another kind of preferred version, the purity of trimethyl indium of the present invention and the purity of nitrogen are all 99.99%.
As another kind of preferred version, the ultrasonic cleaning time of the present invention is 5 minutes, and reaction chamber is evacuated to 9.0 × 10
-4pa.
As another kind of preferred version, trimethyl indium of the present invention and nitrogen flow are controlled by mass flowmeter, and electron cyclotron resonace power is 650W.
As another kind of preferred version, substrate heating to 200 DEG C of the present invention, trimethyl indium and nitrogen flow are respectively 1sccm(milliliter per minute) and 100sccm, controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 30min.
As another kind of preferred version, substrate heating to 500 DEG C of the present invention, trimethyl indium and nitrogen flow are respectively 1sccm and 150sccm, and controlling gas total pressure is 2.0Pa, electron cyclotron resonace reaction 50min.
As another kind of preferred version, substrate heating to 600 DEG C of the present invention, trimethyl indium and nitrogen flow are respectively 2sccm and 200sccm, and controlling gas total pressure is 1.5 Pa, electron cyclotron resonace reaction 120min.
Secondly, substrate heating to 400 DEG C of the present invention, trimethyl indium and nitrogen flow are respectively 1sccm and 200sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 100min.
In addition, substrate heating to 600 DEG C of the present invention, trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 120min.
Beneficial effect of the present invention.
The present invention utilizes the ECR-PEMOCVD technology that accurately can control low temperature depositing, and the correlation parameter in reaction process and material are selected, set, thus deposition prepares high-quality InN optoelectronic film in Diamond wafer base substrate, cost is very low.In addition, diamond has very high thermal conductivity and excellent thermotolerance, is well suited for the application such as the device of high power, high; Diamond wafer of the present invention on-chip InN optoelectronic film product 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 self-supporting diamond.
Fig. 2 is the X ray diffracting spectrum of InN film on embodiment 1 self-supporting diamond substrate.
Fig. 3 is the InN/ free-standing diamond film structural membrane schematic diagram that the inventive method obtains.
In Fig. 3,1 is free-standing diamond film structure thick film substrate, and 2 is InN sample thin film.
Embodiment
The present invention includes following steps.
1), after Diamond wafer substrate being used acetone, ethanol, deionized water ultrasonic cleaning successively, feeding reaction chamber is dried up with nitrogen.
2) ECR-PEMOCVD system is adopted, reaction chamber is vacuumized, substrate heating to 20 ~ 600 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed into again in reaction chamber, trimethyl indium and nitrogen flow are than being (1 ~ 2): (100 ~ 200), controlling gas total pressure is 0.8 ~ 2.0Pa, and electron cyclotron resonace reaction 30min ~ 3h, obtains the InN optoelectronic film at Diamond wafer substrate.
Described Diamond wafer substrate prepares under the reaction source condition of methane and hydrogen in HF CVD system, and its diamond is stick-up substrate, and free standing diamond thickness is 1mm.
The purity of described trimethyl indium and the purity of nitrogen are all 99.99%.
The described ultrasonic cleaning time is 5 minutes, and reaction chamber is evacuated to 9.0 × 10
-4pa.
Described trimethyl indium and nitrogen flow are controlled by mass flowmeter, and electron cyclotron resonace power is 650W.
Described substrate heating to 200 DEG C, trimethyl indium and nitrogen flow are respectively 1sccm(milliliter per minute) and 100sccm, controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 30min.
Described substrate heating to 500 DEG C, trimethyl indium and nitrogen flow are respectively 1sccm and 150sccm, and controlling gas total pressure is 2.0Pa, electron cyclotron resonace reaction 50min.
Described substrate heating to 600 DEG C, trimethyl indium and nitrogen flow are respectively 2sccm and 200sccm, and controlling gas total pressure is 1.5 Pa, electron cyclotron resonace reaction 120min.
Described substrate heating to 400 DEG C, trimethyl indium and nitrogen flow are respectively 1sccm and 200sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 100min.
Described substrate heating to 600 DEG C, trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 120min.
Embodiment 1.
After free standing diamond substrate acetone, ethanol and deionized water ultrasonic wave being cleaned successively, dry up feeding reaction chamber with nitrogen; Reaction chamber is evacuated to 9.0 × 10
-4pa, by substrate heating to 200 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 1:100, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 1 sccm and 100sccm; Controlling gas total pressure is 1.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains the on-chip InN optoelectronic film of Diamond wafer.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Its result is as shown in table 1, and on-chip its electric property of InN film of free standing diamond 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 free standing diamond substrate has good preferred orientation structure, shows that InN film has good crystalline quality.Test result shows, the on-chip InN film of free standing diamond 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 Diamond wafer.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Diamond wafer substrate | 49.2 | 0.95×10 20 |
Embodiment 2.
After free standing diamond substrate acetone, ethanol and deionized water ultrasonic wave being cleaned successively, dry up feeding reaction chamber with nitrogen; Reaction chamber is evacuated to 9.0 × 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 1:150, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 1 sccm and 150sccm; Controlling gas total pressure is 2.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 50min, obtains the on-chip InN optoelectronic film of Diamond wafer.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Its result is as shown in table 2, and on-chip its electric property of InN film of free standing diamond is good as can be seen from Table 2, mobility and carrier concentration better.Test result shows, the on-chip InN film of free standing diamond meets high frequency, and high power device is to the requirement of Electrical performance.
The electric property of table 2 ECR-PEMOCVD low temperature depositing InN on Diamond wafer.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Diamond wafer substrate | 33.4 | 1.32×10 20 |
Embodiment 3.
After free standing diamond substrate acetone, ethanol and deionized water ultrasonic wave being cleaned successively, dry up feeding reaction chamber with nitrogen; Reaction chamber is evacuated to 9.0 × 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 2:200, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 2 sccm and 200sccm; Controlling gas total pressure is 1.5Pa; Be 650W in electron cyclotron resonance frequency, reaction 120min, obtains the on-chip InN optoelectronic film of Diamond wafer.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Its result is as shown in table 3, and on-chip its electric property of InN film of free standing diamond is good as can be seen from Table 3, mobility and carrier concentration better.Test result shows, the on-chip InN film of free standing diamond meets high frequency, and high power device is to the requirement of Electrical performance.
The electric property of table 3 ECR-PEMOCVD low temperature depositing InN on Diamond wafer.
| Sample | Mobility (cm2/VS) | Carrier concentration (cm-3) |
| InN film on Diamond wafer substrate | 22.8 | 2.16×10 20 |
Embodiment 4.
After free standing diamond substrate acetone, ethanol and deionized water ultrasonic wave being cleaned successively, dry up feeding reaction chamber with nitrogen; Reaction chamber is evacuated to 9.0 × 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 1:200, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 1sccm and 200sccm; Controlling gas total pressure is 1.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 100min, obtains the on-chip InN optoelectronic film of Diamond wafer.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Its result is as shown in table 4, and on-chip its electric property of InN film of free standing diamond is good as can be seen from Table 4, mobility and carrier concentration better.Test result shows, the on-chip InN film of free standing diamond meets high frequency, and high power device is to the requirement of Electrical performance.
The electric property of table 4ECR-PEMOCVD low temperature depositing InN on Diamond wafer.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Diamond wafer substrate | 38.6 | 1.36×10 20 |
Embodiment 5.
After free standing diamond substrate acetone, ethanol and deionized water ultrasonic wave being cleaned successively, dry up feeding reaction chamber with nitrogen; Reaction chamber is evacuated to 9.0 × 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 1.5:180, is controlled by quality flowmeter flow quantity, and flow parameter is respectively 1.5sccm and 180sccm; Controlling gas total pressure is 1.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 120min, obtains the on-chip InN optoelectronic film of Diamond wafer.
Experiment terminates rear employing Hall test equipment and has carried out test analysis to the mobility of film and carrier concentration.Its result is as shown in table 5, and on-chip its electric property of InN film of free standing diamond is good as can be seen from Table 5, mobility and carrier concentration better.Test result shows, the on-chip InN film of free standing diamond meets high frequency, and high power device is to the requirement of Electrical performance.
The electric property of table 5ECR-PEMOCVD low temperature depositing InN on Diamond wafer.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm- 3) |
| InN film on Diamond wafer substrate | 23.5 | 1.69×10 20 |
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 x instrument is: Bruker AXS D8.
As shown in Figure 1, free standing diamond substrate is polycrystalline, has preferred orientation, and quality is good, meets the requirement of high power device to thermal diffusivity.
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 (7)
- The preparation method of 1.ECR-PEMOCVD low temperature depositing InN film on Diamond wafer, is characterized in that comprising the following steps:1), after Diamond wafer substrate being used acetone, ethanol, deionized water ultrasonic cleaning successively, feeding reaction chamber is dried up with nitrogen;2) ECR-PEMOCVD system is adopted, reaction chamber is vacuumized, substrate heating to 20 ~ 600 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed into again in reaction chamber, trimethyl indium and nitrogen flow are than being (1 ~ 2): (100 ~ 200), controlling gas total pressure is 0.8 ~ 2.0Pa, and electron cyclotron resonace reaction 30min ~ 3h, obtains the InN optoelectronic film at Diamond wafer substrate;Described Diamond wafer substrate prepares under the reaction source condition of methane and hydrogen in HF CVD system, and free standing diamond thickness is 1mm;The described ultrasonic cleaning time is 5 minutes, and reaction chamber is evacuated to 9.0 × 10-4 Pa;Described trimethyl indium and nitrogen flow are controlled by mass flowmeter, and electron cyclotron resonace power is 650W;Described ECR-PEMOCVD system comprises gas distributing system, ultra-high vacuum system, computer data acquiring and Controlling System, well heater and sample table is provided with in epitaxial chamber in ultra-high vacuum system, sample table is connected with sample table rotating mechanism and sample table riser, gas distributing system high vacuum valve A is connected with quartz discharge room with epitaxial chamber respectively with high vacuum valve B, epitaxial chamber side is provided with viewing window, also comprises:A) by microwave power source, microwave transmission system, variable-length antenna and stop up with extension the quartz discharge room be communicated with and form coupled mode electron cyclotron resonance microwave plasmas source, chamber:B) multicell structure ultra-high vacuum system; epitaxial chamber in multicell structure ultra-high vacuum system vacuum gate valve is connected with dress specimen chamber; dress specimen chamber is connected with pretreatment chamber; epitaxial chamber's vacuum gate valve is connected with turbomolecular pump and sputter ion pump respectively, epitaxial chamber is arranged mechanical manipulator and magnetictransmission bar;C) the examination and analysb system be made up of the opticmeasurement arranged above the refletcion high-energy electron diffraction instrument arranged in epitaxial chamber side, fluorescent screen and CCD imaging system and quadrupole mass spectrometer and epitaxial chamber and electromagnetic measurement, refletcion high-energy electron diffraction instrument and quadrupole mass spectrometer share a differential extraction pump.
- 2., according to the preparation method of the low temperature depositing InN film on Diamond wafer of ECR-PEMOCVD described in claim 1, it is characterized in that the purity of described trimethyl indium and the purity of nitrogen are all 99.99%.
- 3. according to the preparation method of the low temperature depositing InN film on Diamond wafer of ECR-PEMOCVD described in claim 1, it is characterized in that described substrate heating to 200 DEG C, trimethyl indium and nitrogen flow are respectively 1sccm and 100sccm, controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 30min.
- 4. according to the preparation method of the low temperature depositing InN film on Diamond wafer of ECR-PEMOCVD described in claim 1, it is characterized in that described substrate heating to 500 DEG C, trimethyl indium and nitrogen flow are respectively 1sccm and 150sccm, controlling gas total pressure is 2.0Pa, electron cyclotron resonace reaction 50min.
- 5. according to the preparation method of the low temperature depositing InN film on Diamond wafer of ECR-PEMOCVD described in claim 1, it is characterized in that described substrate heating to 600 DEG C, trimethyl indium and nitrogen flow are respectively 2sccm and 200sccm, controlling gas total pressure is 1.5 Pa, electron cyclotron resonace reaction 120min.
- 6. according to the preparation method of the low temperature depositing InN film on Diamond wafer of ECR-PEMOCVD described in claim 1, it is characterized in that described substrate heating to 400 DEG C, trimethyl indium and nitrogen flow are respectively 1sccm and 200sccm, controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 100min.
- 7. according to the preparation method of the low temperature depositing InN film on Diamond wafer of ECR-PEMOCVD described in claim 1, it is characterized in that described substrate heating to 600 DEG C, trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 120min.
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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 |
Non-Patent Citations (3)
| Title |
|---|
| Deposition and properties of highly c-oriented of InN films on sapphire substrates with ECR-plasma-enhanced MOCVD;Qin Fuwen;《RARE METALS》;20120430;第31卷(第2期);第1页左栏第1段至第2页右栏第1段 * |
| TMGa 流量对玻璃衬底上低温沉积GaN 的影响;陈伟绩;《真空科学与技术学报》;20120831;第30卷(第4期);参见第2页左栏第1段至第5页左栏第1段 * |
| 氮气流量对玻璃衬底上低温沉积GaN 薄膜结晶性的影响;王文彦;《半导体学报》;20081231;第29卷(第12期);全文 * |
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Inventor after: Gao Ning Inventor after: Li Dongyang Inventor after: Zhao Haiyan Inventor after: Lv Zhonghua Inventor after: Shu Xinlei Inventor after: Leng Xuemin Inventor after: Yu Geng Inventor after: Mao Wuping Inventor after: Liu Yangyi Inventor after: Zhong Hongyu Inventor before: Zhang Dong Inventor before: Du Shipeng Inventor before: Zhao Yan Inventor before: Wang Baoshi Inventor before: Yi Yunlong Inventor before: Jin Yuexin Inventor before: Zhang Xiangming Inventor before: Wang Jian Inventor before: Liu Liying Inventor before: Wang Gang Inventor before: Guo Rui Inventor before: Zhang Tieyan Inventor before: Wang Shuaijie Inventor before: Ju Zhenhe Inventor before: Wang Xiaowen Inventor before: Cao Fuyi Inventor before: Zhang Xiaohui Inventor before: Zhang Hongli Inventor before: Sun Yong Inventor before: Li Yucai |
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Effective date of registration: 20160519 Address after: 110136 Shenbei New Area, Liaoning, Shenyang North Road, No. 49, No. Patentee after: SHENYANG JIAYUE POWER TECHNOLOGY CO., LTD. Address before: Shenbei New Area Puchang road Shenyang City, Liaoning province 110136 No. 18 Patentee before: Shenyang Engineering College |