CN103334088B - The method of low temperature depositing InN film on a glass substrate - Google Patents
The method of low temperature depositing InN film on a glass substrate Download PDFInfo
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- CN103334088B CN103334088B CN201310298357.8A CN201310298357A CN103334088B CN 103334088 B CN103334088 B CN 103334088B CN 201310298357 A CN201310298357 A CN 201310298357A CN 103334088 B CN103334088 B CN 103334088B
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Abstract
<b> the invention belongs to technical field of novel photoelectric material sediment preparation, provides a kind of method preparing the </b><bGreatT.Gre of the low temperature depositing on a glass substrate aT.GTInN</b><bGr eatT.GreaT.GT film of the good </b><bGreatT.Gre aT.GTInN</b><bGr eatT.GreaT.GT optoelectronic film of electric property.The present invention includes following steps: </b><bGreatT.Gre aT.GT1</b><bGrea tT.GreaT.GT) glass substrate is used acetone, ethanol, deionized water ultrasonic cleaning successively after, dry up feeding reaction chamber with nitrogen; </b><bGreatT.Gre aT.GT2</b><bGrea tT.GreaT.GT) adopt </b><bGreatT.Gre aT.GTECR-PEMOCVD</b>LEssT.LTs sT.LTb> system, reaction chamber is vacuumized, glass substrate is heated to </b><bGreatT.Gre aT.GT20</b><bGre atT.GreaT.GT ~ </b><bGreatT.Gre aT.GT400</b><bGr eatT.GreaT.GT DEG C, the trimethyl indium that hydrogen carries is passed into again in reaction chamber, nitrogen, trimethyl indium and nitrogen flow are than being (</b><bGreatT.Gre aT.GT2</b><bGrea tT.GreaT.GT ~ </b><bGreatT.Gre aT.GT4</b><bGrea tT.GreaT.GT): (</b><bGreatT.Gre aT.GT100</b><bGr eatT.GreaT.GT ~ </b><bGreatT.Gre aT.GT200</b><bGr eatT.GreaT.GT), controlling gas total pressure is </b><bGreatT.Gre aT.GT0.8</b><bGr eatT.GreaT.GT ~ </b><bGreatT.Gre aT.GT2.0Pa</b><b >, electron cyclotron resonace reaction </b><bGreatT.Gre aT.GT30min</b><b > ~ </b><bGreatT.Gre aT.GT3h, </b><bGreatT.Gre aT.GT obtains the </b><bGreatT.Gre aT.GTInN</b><bGr eatT.GreaT.GT optoelectronic film at glass substrate.</b>
Description
Technical field
The invention belongs to technical field of novel photoelectric material sediment preparation, particularly relate to a kind of method of the InN of low temperature depositing on a glass substrate 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 method preparing the InN of the low temperature depositing on a glass substrate film of the good InN optoelectronic film of electric property.
For achieving the above object, the present invention adopts following technical scheme, the present invention includes following steps.
1), after glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, feeding reaction chamber is dried up with nitrogen.
2) ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition is adopted) system, reaction chamber is vacuumized, glass substrate is heated to 20 ~ 400 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed into again in reaction chamber, trimethyl indium and nitrogen flow are than being (2 ~ 4): (100 ~ 200), controlling gas total pressure is 0.8 ~ 2.0Pa, and electron cyclotron resonace reaction 30min ~ 3h, obtains the InN optoelectronic film at glass substrate.
As a kind of preferred version, described glass substrate of the present invention is 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 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 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 the thickness of 650W, InN optoelectronic film is 200nm ~ 1 μm.
As another kind of preferred version, glass substrate of the present invention is heated to 20 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm(milliliter per minute) and 100sccm, controlling gas total pressure is 0.8Pa, electron cyclotron resonace reaction 30min.
As another kind of preferred version, glass substrate of the present invention is heated to 100 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and controlling 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 DEG C, and trimethyl indium and nitrogen flow are respectively 3sccm and 200sccm, and controlling gas total pressure is 1.5Pa, electron cyclotron resonace reaction 120min.
Secondly, glass substrate of the present invention is heated to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and controlling gas total pressure is 2.0Pa, electron cyclotron resonace reaction 100min.
In addition, glass substrate of the present invention is heated to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and controlling gas total pressure is 1.4Pa, electron cyclotron resonace reaction 180min.
Beneficial effect of the present invention.
The present invention utilizes the ECR-PEMOCVD technology that accurately can control low temperature depositing, and selects the correlation parameter in reaction process and material, set, thus prepares high-quality InN optoelectronic film at glass substrate deposited on substrates, and cost is very low.In addition, the InN optoelectronic film product on glass substrate of the present invention has good electric property 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 InN film on the embodiment of the present invention 1 Corning glass substrate.
Fig. 2 is the transmission collection of illustrative plates spectrum of InN film on the embodiment of the present invention 1 Corning glass substrate.
Fig. 3 is the InN/ Corning glass substrate structural membrane schematic diagram that the inventive method obtains.
In Fig. 3,1 is Corning glass substrate, and 2 is InN optoelectronic film.
Embodiment
The present invention includes following steps.
1), after glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, feeding reaction chamber is dried up with nitrogen.
2) ECR-PEMOCVD system is adopted, reaction chamber is vacuumized, glass substrate is heated to 20 ~ 400 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed into again in reaction chamber, trimethyl indium and nitrogen flow are than being (2 ~ 4): (100 ~ 200), controlling gas total pressure is 0.8 ~ 2.0Pa, and electron cyclotron resonace reaction 30min ~ 3h, obtains the InN optoelectronic film at glass substrate.
Described glass substrate is Corning glass substrate, and thickness is 0.2mm ~ 0.8mm.
The purity of described trimethyl indium (TMIn) and the purity of nitrogen are all 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 the thickness of 650W, InN optoelectronic film is 200nm ~ 1 μm.
Described glass substrate is heated to 20 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 100sccm, and controlling gas total pressure is 0.8Pa, electron cyclotron resonace reaction 30min.
Described glass substrate is heated to 100 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and controlling gas total pressure is 2.0Pa, electron cyclotron resonace reaction 70min.
Described glass substrate is heated to 200 DEG C, and trimethyl indium and nitrogen flow are respectively 3sccm and 200sccm, and controlling gas total pressure is 1.5Pa, electron cyclotron resonace reaction 120min.
Described glass substrate is heated to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and controlling gas total pressure is 2.0Pa, electron cyclotron resonace reaction 100min.
Described glass substrate is heated to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 1.5sccm and 180sccm, and controlling gas total pressure is 1.4Pa, electron cyclotron resonace reaction 180min.
Embodiment 1.
After Corning glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
Reaction chamber is evacuated to 8.0 × 10
-4pa, when substrate not being heated to be room temperature 20 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 2:100, controlled by quality flowmeter flow quantity, flow parameter is respectively 2sccm and 100sccm; Controlling gas total pressure is 0.8Pa; Be 650W at electron cyclotron resonace power, reaction 30min, obtains the InN optoelectronic film at Corning glass substrate.
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 its electric property of InN film as can be seen from Table 1 on Corning glass substrate is good, mobility and carrier concentration better.Carried out the analysis of X-ray diffraction to sample thin film, as shown in Figure 1, its result shows that ECR-PEMOCVD system low temperature depositing InN optoelectronic film on Corning glass substrate has good preferred orientation structure, shows that InN film has good crystalline quality.Then the analysis of transmitted spectrum 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 Corning glass substrate has good light transmission, and in 800nm ~ 1000nm wavelength region, the transmitance of InN film is about 85%.Test result shows, the InN film on Corning glass substrate meets high frequency, high power device to the requirement of film quality.
The electric property of table 1ECR-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 Corning glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
Reaction chamber is evacuated to 8.0 × 10
-4pa, by substrate heating to 100 DEG C, passes into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 2:150, and controlled by quality flowmeter flow quantity, flow parameter is respectively 2sccm and 150sccm; Controlling gas total pressure is 2.0Pa; Be 650W at electron cyclotron resonace power, reaction 70min, obtains the InN optoelectronic film on Corning glass substrate.
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 its electric property of InN film as can be seen from Table 2 on Corning glass substrate is good, mobility and carrier concentration better.Test result shows, the InN film on Corning glass substrate meets high frequency, and high power device is to the requirement of Electrical performance.
The electric property of table 2ECR-PEMOCVD low temperature depositing InN on Corning glass substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Corning glass substrate | 74.8 | 9.2×10 18 |
Embodiment 3.
After Corning glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
Reaction chamber is evacuated to 8.0 × 10
-4pa, by substrate heating to 200 DEG C, passes into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 3:200, and controlled by quality flowmeter flow quantity, flow parameter is respectively 3sccm and 200sccm; Controlling gas total pressure is 1.5Pa; Be 650W at electron cyclotron resonace power, reaction 120min, obtains the InN optoelectronic film on Corning glass substrate.
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 its electric property of InN film as can be seen from Table 3 on Corning glass substrate is good, mobility and carrier concentration better.Test result shows, the InN film on Corning glass substrate meets high frequency, and high power device is to the requirement of Electrical performance.
The electric property of table 3ECR-PEMOCVD low temperature depositing InN on Corning glass substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Corning glass substrate | 53.9 | 4.2.×10 18 |
Embodiment 4.
After Corning glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
Reaction chamber is evacuated to 8.0 × 10
-4pa, by substrate heating to 400 DEG C, passes into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, and wherein trimethyl indium and the flow-ratio control of nitrogen reaction source are 4:200, and controlled by quality flowmeter flow quantity, flow parameter is respectively 4sccm and 200sccm; Controlling gas total pressure is 2.0Pa; Be 650W at electron cyclotron resonace power, reaction 100min, obtains the InN optoelectronic film on Corning glass substrate.
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 its electric property of InN film as can be seen from Table 4 on Corning glass substrate is good, mobility and carrier concentration better.Test result shows, the InN film on Corning glass substrate 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 Corning glass substrate.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Corning glass substrate | 102.6 | 2.5×10 18 |
Embodiment 5.
After Corning glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
Reaction chamber is evacuated to 8.0 × 10
-4pa, by substrate heating to 400 DEG C, passes into trimethyl indium, 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 controlled by quality flowmeter flow quantity, flow parameter is respectively 1.5sccm and 180sccm; Controlling gas total pressure is 1.4Pa; Be 650W at electron cyclotron resonace power, reaction 180min, obtains the InN optoelectronic film on Corning glass substrate.
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 its electric property of InN film as can be seen from Table 5 on Corning glass substrate is good, mobility and carrier concentration better.Test result shows, the InN film on Corning glass substrate 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 corning glass.
| Sample | Mobility (cm 2/V·S) | Carrier concentration (cm -3) |
| InN film on Corning glass substrate | 47.5 | 2.3×10 18 |
The electrical performance testing Hall test equipment of inventive samples, the model of Hall system is: HL5500PC, and range is 0.1Ohm/square ~ 100GOhm/square.
The model of x ray diffraction analysis x instrument is: BrukerAXSD8.
The model that transmission spectrum analyzes equipment used is: the MAYA2000PRO fiber spectrometer of Ocean company completes, and light source is DH-2000-BAL, and spectral range is 190nm ~ 1100nm.
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 (1)
1. the method for low temperature depositing InN film on a glass substrate, is characterized in that comprising the following steps:
1), after glass substrate being used successively acetone, ethanol, deionized water ultrasonic cleaning, feeding reaction chamber is dried up with nitrogen;
2) ECR-PEMOCVD system is adopted, reaction chamber is vacuumized, glass substrate is heated to 100 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed into again in reaction chamber, trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, controlling gas total pressure is 2.0Pa, and electron cyclotron resonace reaction 70min, obtains the InN optoelectronic film at glass substrate;
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 the thickness of 650W, InN optoelectronic film is 200nm ~ 1 μm;
Described glass substrate is Corning glass substrate, and thickness is 0.2mm ~ 0.8mm;
The purity of described trimethyl indium and the purity of nitrogen are all 99.99%.
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| FR3062855B1 (en) * | 2017-02-14 | 2019-04-19 | Sa Quertech | METHOD OF TREATING WITH A BEAM OF IONS TO PRODUCE A HIGH SCRATCH RESISTANT HIGH SCRATCH ANTIREFLECTION SAPHIR. |
| CN113897677B (en) * | 2021-09-30 | 2023-04-28 | 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1364946A (en) * | 2001-01-11 | 2002-08-21 | 大连理工大学 | Electronically cyclic resonating, microwave plasma reinforcing and metal and organic chemically vapor-phase depositing epitaxial system and technology |
| CN1563481A (en) * | 2004-03-16 | 2005-01-12 | 南京大学 | Method for growth of InN film through In deposition in advance |
| CN102560675A (en) * | 2012-03-06 | 2012-07-11 | 华南理工大学 | Nonpolar InN film growing on LiGao2 substrate and preparation method of nonpolar InN film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1364946A (en) * | 2001-01-11 | 2002-08-21 | 大连理工大学 | Electronically cyclic resonating, microwave plasma reinforcing and metal and organic chemically vapor-phase depositing epitaxial system and technology |
| CN1563481A (en) * | 2004-03-16 | 2005-01-12 | 南京大学 | Method for growth of InN film through In deposition in advance |
| CN102560675A (en) * | 2012-03-06 | 2012-07-11 | 华南理工大学 | Nonpolar InN film growing on LiGao2 substrate and preparation method of nonpolar InN film |
Non-Patent Citations (1)
| Title |
|---|
| 玻璃衬底上GaN和InN制备的研究;陈伟绩;《中国优秀硕士学位论文全文数据库 信息科技辑》;20110615(第6期);第6页第9-10行，第9页第4行至最后一行，第14页最后一行，第23页第4-6行，第27页第1-9行，第30页第4-5行，第33页1-8行，第36页第1-9行 * |
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