CN103334088A - Method for low-temperature deposition of InN film on glass substrate - Google Patents
Method for low-temperature deposition of InN film on glass substrate Download PDFInfo
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- CN103334088A CN103334088A CN2013102983578A CN201310298357A CN103334088A CN 103334088 A CN103334088 A CN 103334088A CN 2013102983578 A CN2013102983578 A CN 2013102983578A CN 201310298357 A CN201310298357 A CN 201310298357A CN 103334088 A CN103334088 A CN 103334088A
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Abstract
The invention belongs to the technical field of novel photoelectric material deposition and preparation, and provides a method for the low-temperature deposition of an InN film on a glass substrate, from which the InN photoelectric film with favorable electrical properties can be prepared. The method comprises the following steps: 1), allowing the glass substrate to be subjected to acetone, ethanol, deionized water and ultrasonic cleaning, and then feeding to a reaction chamber after being dried by the nitrogen gas; 2), vacuumizing the reaction chamber by an ECR-PEMOCVD system, heating the glass substrate to 20-400 DEG C, pumping trimethylindium carried by hydrogen, and nitrogen gas into the reaction chamber at the flow ratio of (2-4):(100-200), wherein the overall gas pressure is controlled at 0.8-2.0 Pa, and the electronic convolution resonance vibration reaction is carried out for 30 min-3 h. Due to the adoption of the method, the InN photoelectric film on the glass substrate is prepared.
Description
Technical field
The invention belongs to novel photoelectric material deposition preparing technical field, relate in particular to a kind of on glass substrate the method for low temperature depositing InN 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 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 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 nitrogenous source decomposition temperature height, so general InN film all is grown on some substrates such as sapphire.As everyone knows, the price of sapphire substrate is higher, with its substrate as the InN material, makes the device cost 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 at the problems referred to above, and a kind of method of low temperature depositing InN film on glass substrate for preparing the good InN optoelectronic film of electric property is provided.
For achieving the above object, the present invention adopts following technical scheme, the present invention includes following steps.
1) glass substrate is used acetone, ethanol, deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into reaction chamber.
2) adopt ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition) system, reaction chamber is vacuumized, glass substrate is heated to 20～400 ℃, in reaction chamber, feed trimethyl indium, the nitrogen that hydrogen carries again, trimethyl indium is (2～4) with the nitrogen flow ratio: (100～200), control gas total pressure is 0.8～2.0Pa, electron cyclotron resonace reaction 30min～3h, the InN optoelectronic film that obtains at glass substrate.
As a kind of preferred version, described glass substrate of the present invention is the corning glass substrate, and thickness is 0.2mm～0.8mm.
As another kind of preferred version, the purity of trimethyl indium of the present invention and the purity of nitrogen all are 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 8.0 * 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, and the thickness of InN optoelectronic film is 200nm～1 μ m.
As another kind of preferred version, glass substrate of the present invention is heated to 20 ℃, and trimethyl indium and nitrogen flow are respectively 2sccm(milliliter per minute) and 100sccm, control gas total pressure is 0.8 Pa, electron cyclotron resonace reaction 30min.
As another kind of preferred version, glass substrate of the present invention is heated to 100 ℃, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and control gas total pressure is 2.0Pa, electron cyclotron resonace reaction 70min.
As another kind of preferred version, glass substrate of the present invention is heated to 200 ℃, and trimethyl indium and nitrogen flow are respectively 3sccm and 200sccm, and control gas total pressure is 1.5Pa, electron cyclotron resonace reaction 120min.
Secondly, glass substrate of the present invention is heated to 400 ℃, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and control gas total pressure is 2.0Pa, electron cyclotron resonace reaction 100min.
In addition, glass substrate of the present invention is heated to 400 ℃, and trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and control gas total pressure is 1.4Pa, electron cyclotron resonace reaction 180min.
Beneficial effect of the present invention.
The ECR-PEMOCVD technology of low temperature depositing can be accurately controlled in utilization of the present invention, and the correlation parameter in the reaction process and material are selected, set, thereby prepares high-quality InN optoelectronic film in glass substrate substrate deposition, and cost is very low.In addition, the InN optoelectronic film product on the glass substrate of the present invention has good electric property 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 InN film on the embodiment of the invention 1 corning glass substrate.
Fig. 2 is the transmission collection of illustrative plates spectrum of InN film on the embodiment of the invention 1 corning glass substrate.
The InN/ corning glass substrate structure film synoptic diagram that Fig. 3 obtains for the inventive method.
Among Fig. 3,1 is the corning glass substrate, and 2 is the InN optoelectronic film.
Embodiment
The present invention includes following steps.
1) glass substrate is used acetone, ethanol, deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into reaction chamber.
2) adopt the ECR-PEMOCVD system, reaction chamber is vacuumized, glass substrate is heated to 20～400 ℃, in reaction chamber, feed trimethyl indium, the nitrogen that hydrogen carries again, trimethyl indium is (2～4) with the nitrogen flow ratio: (100～200), control gas total pressure is 0.8～2.0Pa, electron cyclotron resonace reaction 30min ~ 3h, the InN optoelectronic film that obtains at glass substrate.
Described glass substrate is the corning glass substrate, and thickness is 0.2mm～0.8mm.
The purity of described trimethyl indium (TMIn) and the purity of nitrogen all are 99.99%.
The described ultrasonic cleaning time is 5 minutes, and reaction chamber is evacuated to 8.0 * 10
-4Pa.
Described trimethyl indium and nitrogen flow are controlled by mass flowmeter, and electron cyclotron resonace power is 650W, and the thickness of InN optoelectronic film is 200nm～1 μ m.
Described glass substrate is heated to 20 ℃, and trimethyl indium and nitrogen flow are respectively 2sccm and 100sccm, and control gas total pressure is 0.8 Pa, electron cyclotron resonace reaction 30min.
Described glass substrate is heated to 100 ℃, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and control gas total pressure is 2.0Pa, electron cyclotron resonace reaction 70min.
Described glass substrate is heated to 200 ℃, and trimethyl indium and nitrogen flow are respectively 3sccm and 200sccm, and control gas total pressure is 1.5 Pa, electron cyclotron resonace reaction 120min.
Described glass substrate is heated to 400 ℃, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and control gas total pressure is 2.0Pa, electron cyclotron resonace reaction 100min.
Described glass substrate is heated to 400 ℃, and trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and control gas total pressure is 1.4Pa, electron cyclotron resonace reaction 180min.
After the corning glass substrate used acetone, ethanol, deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into reaction chamber.
Reaction chamber is evacuated to 8.0 * 10
-4Pa, when substrate is not heated to be 20 ℃ of room temperatures, feed trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 2:100, by quality flowmeter flow quantity control, flow parameter is respectively 2sccm and 100sccm; Control gas total pressure is 0.8Pa; Be 650W at electron cyclotron resonace power, reaction 30min obtains the optoelectronic film at the InN of corning glass substrate.
Experiment finishes the back and adopts the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 1, and on-chip its electric property of InN film of corning glass 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, and as shown in Figure 1, its result shows that ECR-PEMOCVD system low temperature depositing InN optoelectronic film on the corning glass substrate has good preferred orientation structure, shows that the InN film has crystalline quality preferably.Then sample thin film has been carried out the analysis of transmitted spectrum, as shown in Figure 2, its result shows that ECR-PEMOCVD system low temperature depositing InN optoelectronic film on the corning glass substrate has the good light transmittance energy, and in 800nm～1000nm wavelength region, the transmitance of InN film is about 85%.Test result shows, the on-chip InN film of corning glass satisfies high frequency, high power device to the requirement of film quality.
The electric property of table 1 ECR-PEMOCVD low temperature depositing InN on corning glass.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| Corning glass substrate InN film | 32.5 | 1.8×10 19 |
Embodiment 2.
After the corning glass substrate used acetone, ethanol, deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into reaction chamber.
Reaction chamber is evacuated to 8.0 * 10
-4Pa is heated to 100 ℃ with substrate, feeds trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 2:150, and by quality flowmeter flow quantity control, flow parameter is respectively 2sccm and 150sccm; Control gas total pressure is 2.0Pa; Be 650W at electron cyclotron resonace power, reaction 70min obtains the on-chip InN optoelectronic film of corning glass.
Experiment finishes the back and adopts the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 2, and on-chip its electric property of InN film of corning glass is good as can be seen from Table 2, and mobility and carrier concentration are better.Test result shows that the on-chip InN film of corning glass satisfies high frequency, and high power device is to film electricity performance demands.
The electric property of table 2 ECR-PEMOCVD low temperature depositing InN on the corning glass substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on the corning glass substrate | 74.8 | 9.2×10 18 |
Embodiment 3.
After the corning glass substrate used acetone, ethanol, deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into reaction chamber.
Reaction chamber is evacuated to 8.0 * 10
-4Pa is heated to 200 ℃ with substrate, feeds trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 3:200, and by quality flowmeter flow quantity control, flow parameter is respectively 3 sccm and 200sccm; Control gas total pressure is 1.5Pa; Be 650W at electron cyclotron resonace power, reaction 120min obtains the on-chip InN optoelectronic film of corning glass.
Experiment finishes the back and adopts the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 3, and on-chip its electric property of InN film of corning glass is good as can be seen from Table 3, and mobility and carrier concentration are better.Test result shows that the on-chip InN film of corning glass satisfies high frequency, and high power device is to film electricity performance demands.
The electric property of table 3 ECR-PEMOCVD low temperature depositing InN on the corning glass substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on the corning glass substrate | 53.9 | 4.2.×10 18 |
Embodiment 4.
After the corning glass substrate used acetone, ethanol, deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into reaction chamber.
Reaction chamber is evacuated to 8.0 * 10
-4Pa is heated to 400 ℃ with substrate, feeds trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 4:200, and by quality flowmeter flow quantity control, flow parameter is respectively 4sccm and 200sccm; Control gas total pressure is 2.0Pa; Be 650W at electron cyclotron resonace power, reaction 100min obtains the on-chip InN optoelectronic film of corning glass.
Experiment finishes the back and adopts the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 4, and on-chip its electric property of InN film of corning glass is good as can be seen from Table 4, and mobility and carrier concentration are better.Test result shows that the on-chip InN film of corning glass satisfies high frequency, and high power device is to film electricity performance demands.
The electric property of table 4ECR-PEMOCVD low temperature depositing InN on the corning glass substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on the corning glass substrate | 102.6 | 2.5×10 18 |
Embodiment 5.
After the corning glass substrate used acetone, ethanol, deionized water ultrasonic cleaning successively, dry up with nitrogen and to send into reaction chamber.
Reaction chamber is evacuated to 8.0 * 10
-4Pa is heated to 400 ℃ with substrate, feeds trimethyl indium, the nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 1.5:180, and by quality flowmeter flow quantity control, flow parameter is respectively 1.5sccm and 180sccm; Control gas total pressure is 1.4Pa; Be 650W at electron cyclotron resonace power, reaction 180min obtains the on-chip InN optoelectronic film of corning glass.
Experiment finishes the back and adopts the Hall testing apparatus that mobility and the carrier concentration of film have been carried out test analysis.Its result is as shown in table 5, and on-chip its electric property of InN film of corning glass is good as can be seen from Table 5, and mobility and carrier concentration are better.Test result shows that the on-chip InN film of corning glass satisfies high frequency, and high power device is to film electricity performance demands.
The electric property of table 5ECR-PEMOCVD low temperature depositing InN on corning glass.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on the corning glass substrate | 47.5 | 2.3×10 18 |
The electrical performance testing of sample of the present invention Hall testing apparatus, the model of Hall system is: HL5500PC, range are 0.1 Ohm/square～100 GOhm/square.
The model of the used instrument of x ray diffraction analysis x is: Bruker AXS D8.
The model that transmission spectrum is analyzed equipment used is: finish on the MAYA2000PRO fiber spectrometer of Ocean company, light source is DH-2000-BAL, and spectral range is 190 nm～1100nm.
Be understandable that, more than 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. the method for low temperature depositing InN film on glass substrate is characterized in that may further comprise the steps:
1) glass substrate is used acetone, ethanol, deionized water ultrasonic cleaning successively after, dry up with nitrogen and to send into reaction chamber;
2) adopt the ECR-PEMOCVD system, reaction chamber is vacuumized, glass substrate is heated to 20～400 ℃, in reaction chamber, feed trimethyl indium, the nitrogen that hydrogen carries again, trimethyl indium is (2～4) with the nitrogen flow ratio: (100～200), control gas total pressure is 0.8～2.0Pa, electron cyclotron resonace reaction 30min～3h, the InN optoelectronic film that obtains at glass substrate.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described glass substrate is the corning glass substrate, thickness is 0.2mm～0.8mm.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that the purity of described trimethyl indium and the purity of nitrogen all are 99.99%.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that the described ultrasonic cleaning time is 5 minutes, reaction chamber is evacuated to 8.0 * 10
-4Pa.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described trimethyl indium and nitrogen flow controlled by mass flowmeter, electron cyclotron resonace power is 650W, the thickness of InN optoelectronic film is 200nm～1 μ m.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described glass substrate is heated to 20 ℃, trimethyl indium and nitrogen flow are respectively 2sccm and 100sccm, and control gas total pressure is 0.8 Pa, electron cyclotron resonace reaction 30min.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described glass substrate is heated to 100 ℃, trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and control gas total pressure is 2.0Pa, electron cyclotron resonace reaction 70min.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described glass substrate is heated to 200 ℃, trimethyl indium and nitrogen flow are respectively 3sccm and 200sccm, and control gas total pressure is 1.5Pa, electron cyclotron resonace reaction 120min.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described glass substrate is heated to 400 ℃, trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and control gas total pressure is 2.0Pa, electron cyclotron resonace reaction 100min.
According to claim 1 described on glass substrate the method for low temperature depositing InN film, it is characterized in that described glass substrate is heated to 400 ℃, trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and control gas total pressure is 1.4Pa, electron cyclotron resonace reaction 180min.
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Cited By (3)
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| CN110431250A (en) * | 2017-02-14 | 2019-11-08 | 法国爱奥尼亚公司 | The sapphire method of the high-transmission rate antireflection of scratch-resistant is generated with Ion Beam Treatment |
| CN113897677A (en) * | 2021-09-30 | 2022-01-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Indium nitride crystal and method for growing same |
| CN114517288A (en) * | 2021-12-06 | 2022-05-20 | 浙江富芯微电子科技有限公司 | Method for forming InN film on SiC substrate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110431250A (en) * | 2017-02-14 | 2019-11-08 | 法国爱奥尼亚公司 | The sapphire method of the high-transmission rate antireflection of scratch-resistant is generated with Ion Beam Treatment |
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| CN113897677A (en) * | 2021-09-30 | 2022-01-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | Indium nitride crystal and method for growing same |
| CN114517288A (en) * | 2021-12-06 | 2022-05-20 | 浙江富芯微电子科技有限公司 | Method for forming InN film on SiC substrate |
| CN114517288B (en) * | 2021-12-06 | 2023-10-20 | 浙江富芯微电子科技有限公司 | Method for forming InN film on SiC substrate |
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