CN103352204B - ECR-PEMOCVD system is to the preparation method of InN/GaN/ free-standing diamond film structure - Google Patents
ECR-PEMOCVD system is to the preparation method of InN/GaN/ free-standing diamond film structure Download PDFInfo
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Abstract
The invention belongs to technical field of novel photoelectric material sediment preparation, provide a kind of electric property is good, heat dispersion is good ECR-PEMOCVD system to the preparation method of InN/GaN/ free-standing diamond film structure.The present invention includes following steps: 1) free-standing diamond film substrate is used successively acetone, ethanol, deionized water successively after ultrasonic cleaning, dry up feeding reaction chamber with nitrogen; 2) ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition is adopted) system, reaction chamber is vacuumized, heated substrate to 400 ~ 600 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries; Control gas total pressure, electron cyclotron resonace is obtained by reacting the GaN buffer layer thin film at free-standing diamond film substrate.
Description
Technical field
the invention belongs to technical field of novel photoelectric material sediment preparation, particularly relate to a kind of ECR-PEMOCVD system to the preparation method of InN/GaN/ free-standing diamond film structure.
Background technology
in more than ten years in the past, the research about InN semiconductor material causes the great interest of people.InN is a kind of important direct band gap III hi-nitride semiconductor material, and compared with GaN, AlN of the same clan, InN has minimum virtual mass and the highest carrier mobility, saturation drift velocity, and its low field mobility can reach 3200 cm
2
/ Vs, peak shift speed can reach 4.3 × 10
7
cm/s, these characteristics make InN have unique advantage in high frequency centimetre is applied with millimetric wave device.Prepare the prerequisite that high-quality InN epitaxial film is InN semiconductor material research and apply, but the preparation of InN film there are two large difficulties, are that the decomposition temperature of InN is lower on the one hand, are about about 600 DEG C, and as the NH in N source
3
decomposition temperature then require very high, generally at about 1000 DEG C, therefore how the growth temperature of control InN just creates contradiction, and generally traditional MOCVD technical requirements temperature, more than 800 DEG C, limits the growth temperature problem of InN.
Summary of the invention
the present invention is exactly for the problems referred to above, provides a kind of electric property is good, heat dispersion is good ECR-PEMOCVD system to the preparation method of InN/GaN/ free-standing diamond film structure.
for achieving the above object, the present invention adopts following technical scheme, the present invention includes following steps.
1) free-standing diamond film substrate is used successively acetone, ethanol, deionized water successively after ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
2) ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition is adopted) system, reaction chamber is vacuumized, heated substrate to 400 ~ 600 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries; Control gas total pressure, electron cyclotron resonace is obtained by reacting the GaN buffer layer thin film at free-standing diamond film substrate.
3) continue to adopt ECR-PEMOCVD system, reaction chamber is vacuumized, by substrate heating to 200 DEG C ~ 400 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed 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 deposition is prepared into InN film, obtains at the structural InN optoelectronic film of GaN buffer layer thin film/free-standing diamond film.
as a kind of preferred version, free-standing diamond film substrate of the present invention prepares under the reaction source condition of methane and hydrogen in HF CVD system, and be stick-up substrate, free standing diamond thickness is 1mm.
as another kind of preferred version, the purity of trimethyl-gallium of the present invention, trimethyl indium and the purity of nitrogen are 99.99%.
as another kind of preferred version, the step 1) ultrasonic cleaning time of the present invention is 5 minutes.
step 2) reaction chamber is evacuated to 9.0 × 10
-4
pa, controls trimethyl-gallium by mass flowmeter and nitrogen flow is respectively 0.8sccm and 100sccm; Controlling gas total pressure is 1.2Pa; Electron cyclotron resonace power is 650W, reaction 30min.
as another kind of preferred version, step 3) reaction chamber of the present invention is evacuated to 8.0 × 10
-4
pa, controlled the flow of trimethyl indium and nitrogen by mass flowmeter, electron cyclotron resonace power is 650W.
as another kind of preferred version, step 2 of the present invention) by substrate heating to 400 DEG C.
step 3) is by substrate heating to 200 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 180min.
as another kind of preferred version, step 2 of the present invention) by substrate heating to 500 DEG C.
step 3) is by substrate heating to 300 DEG C, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 120min.
as another kind of preferred version, step 2 of the present invention) by substrate heating to 600 DEG C.
step 3) is by substrate heating to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 200sccm, and controlling gas total pressure is 1.2Pa, electron cyclotron resonace reaction 60min.
secondly, step 2 of the present invention) by substrate heating to 485 DEG C.
step 3) is by substrate heating to 360 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and controlling gas total pressure is 1.5Pa, electron cyclotron resonace reaction 90min.
in addition, step 2 of the present invention) by substrate heating to 500 DEG C.
step 3) is by substrate heating to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 1sccm and 150sccm, and controlling gas total pressure is 1.8Pa, electron cyclotron resonace reaction 50min.
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, greatly reduce epitaxial temperature, growth temperature is made to control below 500 DEG C, in GaN/ free-standing diamond film base substrate, deposition prepares high-quality InN optoelectronic film, and cost is very low.In addition, diamond has excellent heat dispersion, and the InN optoelectronic film product of the present invention on GaN/ free-standing diamond film substrate structure has good electric property and heat dispersion after tested, is easy to prepare the powerful device of high frequency.Secondly, GaN and InN has similar crystalline structure, their stable phase is hexagonal wurtzite structure, as the buffer layer between InN and free-standing diamond film, well solves the lattice mismatch issue existed between InN epitaxial film and free-standing diamond film substrate.
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 GaN/ Diamond wafer structure X ray diffracting spectrum.
fig. 2 is that InN thin film deposition is prepared in the structural X ray diffracting spectrum of GaN/ Diamond wafer.
fig. 3 is the surface topography of InN film sample.
fig. 4 is the InN/GaN/ free-standing diamond film structural membrane schematic diagram that the inventive method obtains.
in Fig. 4,1 is free-standing diamond film substrate, and 2 is GaN film buffer layer, and 3 is InN sample thin film.
Embodiment
the present invention includes following steps.
1) free-standing diamond film substrate is used successively acetone, ethanol, deionized water successively after ultrasonic cleaning, dry up feeding reaction chamber with nitrogen.
2) ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition is adopted) system, reaction chamber is vacuumized, heated substrate to 400 ~ 600 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries; Control gas total pressure, electron cyclotron resonace is obtained by reacting the GaN buffer layer thin film at free-standing diamond film substrate.
3) continue to adopt ECR-PEMOCVD system, reaction chamber is vacuumized, by substrate heating to 200 DEG C ~ 400 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed 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 deposition is prepared into InN film, obtains at the structural InN optoelectronic film of GaN buffer layer thin film/free-standing diamond film.
described free-standing diamond film substrate prepares under the reaction source condition of methane and hydrogen in HF CVD system, and be stick-up substrate, free standing diamond thickness is 1mm.
the purity of described trimethyl-gallium, trimethyl indium and the purity of nitrogen are 99.99%.
the described step 1) ultrasonic cleaning time is 5 minutes.
step 2) reaction chamber is evacuated to 9.0 × 10
-4
pa, controls trimethyl-gallium by mass flowmeter and nitrogen flow is respectively 0.8sccm and 100sccm; Controlling gas total pressure is 1.2Pa; Electron cyclotron resonace power is 650W, reaction 30min.
described step 3) reaction chamber is evacuated to 8.0 × 10
-4
pa, controlled the flow of trimethyl indium and nitrogen by mass flowmeter, electron cyclotron resonace power is 650W.
described step 2) by substrate heating to 400 DEG C.
step 3) is by substrate heating to 200 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 180min.
described step 2) by substrate heating to 500 DEG C.
step 3) is by substrate heating to 300 DEG C, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 120min.
described step 2) by substrate heating to 600 DEG C.
step 3) is by substrate heating to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 200sccm, and controlling gas total pressure is 1.2Pa, electron cyclotron resonace reaction 60min.
described step 2) by substrate heating to 485 DEG C.
step 3) is by substrate heating to 360 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and controlling gas total pressure is 1.5Pa, electron cyclotron resonace reaction 90min.
described step 2) by substrate heating to 500 DEG C.
step 3) is by substrate heating to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 1sccm and 150sccm, and controlling gas total pressure is 1.8Pa, electron cyclotron resonace reaction 50min.
embodiment 1.
used by free-standing diamond film substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up feeding reaction chamber with nitrogen; Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 × 10
-4
pa, by substrate heating to 400 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries, flow both it is 0.8sccm and 100sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains the GaN buffer layer thin film at free-standing diamond film substrate.Then adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 × 10
-4
pa, by substrate heating to 200 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is 2:100, and its flow is 2sccm and 100sccm, is controlled by mass flowmeter; Controlling gas total pressure is 0.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 180min, obtains at the structural InN optoelectronic film of GaN/ free-standing diamond film.
experiment terminates rear employing X-ray diffraction analysis equipment and has carried out test analysis to the crystal property of film and preferred orientation.As shown in Figure 2, the InN film of GaN/ free-standing diamond film structure has single preferred orientation to its result as seen from Figure 2, and InN thin film crystallization performance is good.The analysis of atomic force microscope about pattern is carried out to sample thin film, as shown in Figure 3, has shown that InN film has good surface topography.Test result shows, the structural InN film of GaN/ free-standing diamond film meets high frequency, and high power device is to the requirement of film quality.
embodiment 2.
used by free-standing diamond film substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up feeding reaction chamber with nitrogen; Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 × 10
-4
pa, by substrate heating to 500 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries, flow both it is 0.8sccm and 100sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains the GaN buffer layer thin film at free-standing diamond film substrate.Then adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 × 10
-4
pa, by substrate heating to 300 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is 4:200, and its flow is 4sccm and 200sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.0Pa; Be 650W in electron cyclotron resonance frequency, reaction 120min, obtains at the structural InN optoelectronic film of GaN/ free-standing diamond film.Experiment terminates to have carried out test analysis to InN film sample afterwards, and its test result shows, the structural InN film of GaN/ free-standing diamond film meets high frequency, and high power device is to the requirement of film quality.
embodiment 3.
used by free-standing diamond film substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up feeding reaction chamber with nitrogen; Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 × 10
-4
pa, by substrate heating to 600 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries, flow both it is 0.8sccm and 100sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains the GaN buffer layer thin film at free-standing diamond film substrate.Then adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 × 10
-4
pa, by substrate heating to 400 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is 2:200, and its flow is 2sccm and 200sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 60min, obtains at the structural InN optoelectronic film of GaN/ free-standing diamond film.Experiment terminates to have carried out test analysis to InN film sample afterwards, and its test result shows, the structural InN film of GaN/ free-standing diamond film meets high frequency, and high power device is to the requirement of film quality.
embodiment 4.
used by free-standing diamond film substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up feeding reaction chamber with nitrogen; Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 × 10
-4
pa, by substrate heating to 485 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries, flow both it is 0.8sccm and 100sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains the GaN buffer layer thin film at free-standing diamond film substrate.Then adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 × 10
-4
pa, by substrate heating to 360 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is 2:150, and its flow is 2sccm and 150sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.5Pa; Be 650W in electron cyclotron resonance frequency, reaction 90min, obtains at the structural InN optoelectronic film of GaN/ free-standing diamond film.Experiment terminates to have carried out test analysis to InN film sample afterwards, and its test result shows, the structural InN film of GaN/ free-standing diamond film meets high frequency, and high power device is to the requirement of film quality.
embodiment 5.
used by free-standing diamond film substrate acetone, ethanol and deionized water ultrasonic cleaning after 5 minutes successively, dry up feeding reaction chamber with nitrogen; Adopt ECR-PEMOCVD system, reaction chamber is evacuated to 9.0 × 10
-4
pa, by substrate heating to 500 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries, flow both it is 0.8sccm and 100sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.2Pa; Be 650W in electron cyclotron resonance frequency, reaction 30min, obtains the GaN buffer layer thin film at free-standing diamond film substrate.Then adopt ECR-PEMOCVD system, reaction chamber is evacuated to 8.0 × 10
-4
pa, by substrate heating to 400 DEG C, pass into trimethyl indium, nitrogen that hydrogen carries in reaction chamber, throughput ratio both it is 1:150, and its flow is 1sccm and 150sccm, is controlled by mass flowmeter; Controlling gas total pressure is 1.8Pa; Be 650W in electron cyclotron resonance frequency, reaction 50min, obtains at the structural InN optoelectronic film of GaN/ free-standing diamond film.Experiment terminates to have carried out test analysis to InN film sample afterwards, and its test result shows, the structural InN film of GaN/ free-standing diamond film meets high frequency, and high power device is to the requirement of film quality.
the crystal property test of inventive samples is X-ray diffraction analysis, and wherein the model of X-ray diffraction analysis instrument is: the model of XRD test is Bruker AXS D8.
the model of the atomic force microscope (AFM) that the present invention utilizes is Picoscan 2500, originates in Agilent company.Under the test condition of normal room temperature, testing and analyzing is carried out to the pattern of film sample.The test analysis region of sample is.
as shown in Figure 1, free standing diamond substrate is polycrystalline, has preferred orientation, and quality is good, and GaN is as buffer layer, and its crystalline quality is good, meets the requirement to substrate of InN film.
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)
1.ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that comprising the following steps:
1) free-standing diamond film substrate is used successively acetone, ethanol, deionized water successively after ultrasonic cleaning, dry up feeding reaction chamber with nitrogen;
2) ECR-PEMOCVD(electron cyclotron resonace-plasma reinforcing and metal organic chemical vapor deposition is adopted) system, reaction chamber is vacuumized, heated substrate to 400 ~ 600 DEG C, in reaction chamber, pass into trimethyl-gallium, nitrogen that hydrogen carries; Control gas total pressure, electron cyclotron resonace is obtained by reacting the GaN buffer layer thin film at free-standing diamond film substrate;
3) continue to adopt ECR-PEMOCVD system, reaction chamber is vacuumized, by substrate heating to 200 DEG C ~ 400 DEG C, trimethyl indium, nitrogen that hydrogen carries is passed 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 deposition is prepared into InN film, obtains
The structural InN optoelectronic film of GaN buffer layer thin film/free-standing diamond film;
Described free-standing diamond film substrate prepares under the reaction source condition of methane and hydrogen in HF CVD system, and be stick-up substrate, free standing diamond thickness is 1mm;
The described step 1) ultrasonic cleaning time is 5 minutes; Step 2) reaction chamber is evacuated to 9.0 × 10
-4pa, controls trimethyl-gallium by mass flowmeter and nitrogen flow is respectively 0.8sccm and 100sccm; Controlling gas total pressure is 1.2Pa; Electron cyclotron resonace power is 650W, reaction 30min;
Described step 3) reaction chamber is evacuated to 8.0 × 10
-4pa, controlled the flow of trimethyl indium and nitrogen by mass flowmeter, electron cyclotron resonace power is 650W.
2. ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that the purity of described trimethyl-gallium, trimethyl indium and the purity of nitrogen are 99.99% according to claim 1.
3. ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that described step 2 according to claim 1) by substrate heating to 400 DEG C; Step 3) is by substrate heating to 200 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 180min.
4. ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that described step 2 according to claim 1) by substrate heating to 500 DEG C; Step 3) is by substrate heating to 300 DEG C, and trimethyl indium and nitrogen flow are respectively 4sccm and 200sccm, and controlling gas total pressure is 1.0Pa, electron cyclotron resonace reaction 120min.
5. ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that described step 2 according to claim 1) by substrate heating to 600 DEG C; Step 3) is by substrate heating to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 200sccm, and controlling gas total pressure is 1.2Pa, electron cyclotron resonace reaction 60min.
6. ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that described step 2 according to claim 1) by substrate heating to 485 DEG C; Step 3) is by substrate heating to 360 DEG C, and trimethyl indium and nitrogen flow are respectively 2sccm and 150sccm, and controlling gas total pressure is 1.5Pa, electron cyclotron resonace reaction 90min.
7. ECR-PEMOCVD system, to the preparation method of InN/GaN/ free-standing diamond film structure, is characterized in that described step 2 according to claim 1) by substrate heating to 500 DEG C; Step 3) is by substrate heating to 400 DEG C, and trimethyl indium and nitrogen flow are respectively 1sccm and 150sccm, and controlling gas total pressure is 1.8Pa, electron cyclotron resonace reaction 50min.
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| "基于ECR-PEMOCVD技术在蓝宝石衬底上高c轴择优的InN薄膜的制备及表征";周志峰;《中国优秀硕士学位论文全文数据库 信息科技辑》;20121231(第7期);正文第1、8、9、22、23、30页 * |
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Inventor after: Gao Yang Inventor after: Li Wenwen Inventor after: Wang Dalu Inventor after: Zhao Haiyan Inventor after: Zhang Lin Inventor after: Yu Geng Inventor after: Xu Aoran Inventor after: Han Xuerong Inventor after: Wang Zhen Inventor after: Wu Jiakuo Inventor before: Zhang Dong Inventor before: Wang Gang Inventor before: Wang Jian Inventor before: Liu Liying Inventor before: Guo Rui Inventor before: Wang Shuaijie Inventor before: Guan Xin Inventor before: Gao Wei Inventor before: Wang Baoshi Inventor before: Yi Yunlong Inventor before: Jin Yuexin Inventor before: Ju Zhenhe Inventor before: Zhang Yuyan Inventor before: Sun Xiaoyu Inventor before: Zheng Hong Inventor before: Li Yucai Inventor before: Du Shipeng Inventor before: Wang Lijie Inventor before: Zhang Xiaohui Inventor before: Li Shuangmei |
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Effective date of registration: 20160616 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 |