CN1752270A - Opposite target reaction magnetocontrol sputtering method for preparing vanadium oxide film - Google Patents
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Abstract
A process for preparing the vanadium oxide film by magnetically controlled sputtering with the reaction between two opposite targets includes such steps as washing Si (or glass) substrate, depositing a silicon oxide film layer on the Si substrate by PECVD method, and magnetically controlled sputtering with two opposite targets to deposit vanadium oxide film. The technological condition for said sputtering is also disclosed. Said film features high electric resistance-temp coefficient and low electric resistance at ordinary temp.
Description
Technical field
The present invention relates to the method that a kind of subtend target reaction magnetocontrol sputtering prepares vanadium oxide film, belong to the vanadium oxide film technology of preparing.
Background technology
Since nineteen fifty-nine Morin finds the vanadium oxide film phase-change characteristic, the research of vanadium oxide film has constantly been carried out always.Vanadium dioxide film has the phase-change characteristic that is changed into the hot metal phase by cryogenic semiconductor mutually, and is accompanied by the sudden change of resistivity, susceptibility, optical transmittance and reflectivity, makes it have numerous application at microelectronics and optoelectronic areas.Because vanadium is polyvalent metal, can with oxygen in conjunction with forming multiple oxide compound, though particularly be that the vanadium oxide mixed phase polycrystal film of base does not have the phase transition temperature characteristic,, can reach-2 * 10 owing to it has high temperature coefficient of resistance near room temperature with VO2
-2K
-1More than, be 5～10 times of common metal film.Therefore with VO
2For the vanadium oxide mixed phase polycrystal film of base is the ideal material that is used for making infrared acquisition and infrared imaging device thermistor at present.
Sputter coating is the most frequently used method for preparing vanadium oxide film at present.Existing reactive sputtering process has high TCR value and low room temperature resistance in order to make sedimentary vanadium oxide film, not only need accurately to control the processing parameter of deposition film, to form the vanadium oxide film of proper composition, and need after deposition film, at high temperature carry out long thermal annealing, this has not only increased the difficulty of technology, has also reduced the repeatability of technology.The method that also has a kind of sputter to prepare vanadium oxide film is first metal refining vanadium film, form vanadium oxide film through oxide-diffused and after annealing again, CN 1392286A for example, though this method does not need strict control reaction gas flow in the sputter coating process, oxide-diffused and post growth annealing also need higher temperature.During single in addition target sputter coating, target utilization is low, the substrate temperature rise.
Summary of the invention
The purpose of this invention is to provide the method that a kind of subtend target reaction magnetocontrol sputtering prepares vanadium oxide film, the vanadium oxide film that utilizes this method to make has high temperature coefficient of resistance and low room temperature resistance value.
The present invention is realized that by the following technical programs a kind of method for preparing vanadium oxide film is characterized in that comprising following process:
1) glass substrate or silicon substrate surface are cleaned.Silicon chip adopts the standard semiconductor purging method to clean, then dry for standby.The glass substrate cleaning process is as follows: carries out ultrasonic cleaning with acetone,, uses the ethanol ultrasonic cleaning then through deionized water rinsing, and again through deionized water rinsing, dry for standby;
2), strengthen chemical vapour deposition (PECVD) method deposition one deck silicon oxide film at the silicon chip surface using plasma earlier if adopting silicon is substrate;
3) preparation vanadium oxide film: high purity vanadium metal target subtend is placed in the vacuum chamber, glass substrate or silicon substrate is placed on the substrate frame back of the body end vacuum＜3 * 10
-4Pa is that 100: 1～140: 1 argon gas and oxygen feed vacuum chamber to operating air pressure 1.5～2Pa with the flow volume ratio, and is 190～240W with sputtering power, and substrate temperature is 25～200 ℃, and sputtering time is 30～75 minutes spatter film formings.
Above-mentioned argon gas and oxygen flow volume ratio are 120: 1～130: 1.
The invention has the advantages that, adopt the mode of facing targets sputtering, thus the target utilization height, the sputter rate height, sputter is even, and the sputter procedure substrate temperature is low, and the vanadium oxide film after the sputter need not carry out high-temperature heat treatment.The temperature coefficient of resistance of vanadium oxide film between 20～30 ℃ by the present invention's preparation can reach-3 * 10
-2K
-1More than, far above the plain metal thermistor, the room temperature square resistance can reach below 50K Ω/, can be used to make low noise low-grade fever sensitive detection parts to the susceptibility of temperature.
Description of drawings
X-ray photoelectron spectroscopic analysis (XPS) spectrogram of the vanadium oxide film that Fig. 1 makes for the present invention.1# curve correspondence among the figure+5 valency vanadium, its shared volume ratio in film is 35.03%; 2# curve correspondence+4 valency vanadium, its shared volume ratio in film is 51.46%; 3# curve correspondence+3 valency vanadium, its shared volume ratio in film is 13.51%; The 4# curve is 1#, 2#, the stack of 3# curve.
Atomic force microscope (AFM) the pattern picture of the vanadium oxide film that Fig. 2 makes for the present invention.
Scanning electronic microscope (SEM) photo of the vanadium oxide film that Fig. 3 makes for the present invention.The vanadium oxide film uniform crystal particles, the compactness that make of the present invention is good as can be seen from Figure.
The resistance temperature curve of the vanadium oxide film that Fig. 4 makes for the embodiment of the invention 1;
The resistance temperature curve of the vanadium oxide film that Fig. 5 makes for the embodiment of the invention 2.
Embodiment
Embodiment 1 prepares the vanadium oxide film of high temperature coefficient of resistance on glass substrate, concrete steps are as follows:
1) clean glass substrate, process is as follows: carry out ultrasonic cleaning with acetone, through deionized water rinsing, use the ethanol ultrasonic cleaning then, again through deionized water rinsing;
2) adopt subtend target reaction magnetocontrol sputtering method, prepare vanadium oxide film, open vacuum chamber, put into glass substrate, take out rough vacuum earlier, drive high valve then, pumping high vacuum to 3 * 10 at above-mentioned glass substrate
-4Below the Pa, be that 120: 1 argon gas and oxygen feed vacuum chamber to operating air pressure 2Pa with the flow volume ratio, and be 240W with the sputtering power that substrate temperature is 25 ℃, sputtering time is 30 minutes spatter film formings.；
3) above-mentioned vanadium oxide film is carried out the resistance-temperature characteristic test, record room temperature square resistance 28.5K Ω/, temperature coefficient of resistance is-3.3 * 10 between 20～30 ℃
-2K
-1, resistance temperature curve as shown in Figure 4.
Embodiment 2 prepares the vanadium oxide film of high temperature coefficient of resistance on silicon substrate, concrete steps are as follows:
1) silicon chip is carried out surface cleaning, to remove pollution organism, dust and the impurity metal ion of silicon chip surface, process is as follows: the vitriol oil (concentration is 98%) and hydrogen peroxide were hybridly prepared into scavenging solution in 3: 1 by volume, silicon chip was soaked 40 minutes in this scavenging solution, use the deionized water rinsing silicon chip, use ammoniacal liquor, hydrogen peroxide and deionized water to mix in 1: 40: 50 by volume then, soaked silicon chip 30 minutes, use deionized water rinsing again.Adopt the PECVD method to deposit one deck silicon oxide film earlier on silicon chip, back of the body end vacuum is 4.5 * 10
-1Pa, operating air pressure are 4.3Pa, and substrate temperature is 150 ℃, and working gas is N
2O and SiH
4, airshed is respectively 12ml/min and 38ml/min, and deposition time is 10 minutes, SiO
2Layer thickness is about 1000 ;
2) adopt subtend target reaction magnetocontrol sputtering method, prepare vanadium oxide film, open vacuum chamber, put into silicon substrate, take out rough vacuum earlier, drive high valve then, pumping high vacuum to 3 * 10 at above-mentioned silicon substrate
-4Below the Pa, be that 120: 1 argon gas and oxygen feed vacuum chamber to operating air pressure 2Pa with the flow volume ratio, and be 240W with the sputtering power that substrate temperature is 25 ℃, sputtering time is 45 minutes spatter film formings.；
3) above-mentioned vanadium oxide film is carried out the resistance-temperature characteristic test, record room temperature square resistance 45K Ω/, temperature coefficient of resistance between 20～30 ℃-3.5 * 10
-2K
-1, resistance temperature curve as shown in Figure 5.
Embodiment 3
Present embodiment is similar to embodiment 2, difference is that the processing parameter of step 2 is: with the flow volume ratio is that 130: 1 argon gas and oxygen feed vacuum chamber to operating air pressure 1.5Pa, sputtering power is 195W, sputtering time 75 minutes, substrate temperature is 200 ℃, vanadium oxide film is carried out the resistance-temperature characteristic test, record room temperature square resistance 1.4K Ω/, near temperature coefficient of resistance-2.4 * 10 between 20～30 ℃
-2K
-1
Claims (2)
1. a subtend target reaction magnetocontrol sputtering prepares the method for vanadium oxide film, it is characterized in that comprising following process:
1) glass substrate or silicon substrate surface are cleaned: silicon chip adopts the standard semiconductor purging method to clean, then dry for standby; The glass substrate cleaning process is carried out ultrasonic cleaning with acetone, through deionized water rinsing, uses the ethanol ultrasonic cleaning then, again through deionized water rinsing, and dry for standby;
2), strengthen chemical gaseous phase depositing process deposition one deck silicon oxide film at the silicon chip surface using plasma earlier if adopting silicon is substrate;
3) preparation vanadium oxide film: high purity vanadium metal target subtend is placed in the vacuum chamber, glass substrate or silicon substrate is placed on the substrate frame back of the body end vacuum＜3 * 10
-4Pa is that 100: 1～140: 1 argon gas and oxygen feed vacuum chamber to operating air pressure 1.5～2Pa with the flow volume ratio, and is 190～240W with sputtering power, and substrate temperature is 25～200 ℃, and sputtering time is 30～75 minutes spatter film formings.
2. the method for preparing vanadium oxide film by the described subtend target reaction magnetocontrol sputtering of claim 1 is characterized in that argon gas and oxygen flow volume ratio are 120: 1～130: 1.
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| CN100424820C (en) * | 2006-11-27 | 2008-10-08 | 哈尔滨工业大学 | A technique to generate mixed allotropic structure of VO2 film on Si base |
| CN100424819C (en) * | 2006-11-24 | 2008-10-08 | 哈尔滨工业大学 | A method for orientation growth of VO2 film of pulse laser deposition Si base |
| CN101812666A (en) * | 2010-04-09 | 2010-08-25 | 南京理工大学 | Preparation method of vanadium oxide thin film material for non-refrigerated infrared focal plane array |
| CN101950092A (en) * | 2010-09-08 | 2011-01-19 | 天津大学 | Terahertz wave band vanadium oxide optical switch and preparation method thereof |
| CN102002667A (en) * | 2010-11-22 | 2011-04-06 | 烟台睿创微纳技术有限公司 | Method and equipment for preparing high-repeatability vanadium oxide film |
| CN102251216A (en) * | 2011-07-19 | 2011-11-23 | 电子科技大学 | Method for preparing tungsten-doped vanadium oxide film |
| CN102952540A (en) * | 2011-08-25 | 2013-03-06 | 海洋王照明科技股份有限公司 | Samarium-doped strontium sulfate luminescent film, preparation method and organic electroluminescent device |
| CN103361614A (en) * | 2013-06-29 | 2013-10-23 | 天津大学 | Method for preparing Terahertz modulator film material based on flexible substrate |
| CN103540903A (en) * | 2013-10-21 | 2014-01-29 | 中国科学院上海硅酸盐研究所 | Low-temperature high-resistance temperature coefficient non-heat stagnation thin-film material and preparation method thereof |
| CN103882399A (en) * | 2014-03-18 | 2014-06-25 | 天津大学 | Preparation method of flexible substrate based nano vanadium oxide functional film with phase transition characteristic |
| CN104213087A (en) * | 2013-10-17 | 2014-12-17 | 常州博锐恒电子科技有限公司 | Magnetron sputtering preparation method of vanadium oxide |
| CN113774348A (en) * | 2021-09-22 | 2021-12-10 | 季华实验室 | High-temperature superconductor with amorphous vanadium oxide film, preparation method thereof and high-temperature superconducting coil |
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| EP2610230A2 (en) * | 1998-08-31 | 2013-07-03 | Idemitsu Kosan Co., Ltd. | Target for transparent electroconductive film, transparent electroconductive material, transparent electroconductive glass, and transparent electroconductive film |
| CN1195097C (en) * | 2002-07-13 | 2005-03-30 | 华中科技大学 | Process for prapring vanadium oxide film |
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| CN100424819C (en) * | 2006-11-24 | 2008-10-08 | 哈尔滨工业大学 | A method for orientation growth of VO2 film of pulse laser deposition Si base |
| CN100424820C (en) * | 2006-11-27 | 2008-10-08 | 哈尔滨工业大学 | A technique to generate mixed allotropic structure of VO2 film on Si base |
| CN101812666A (en) * | 2010-04-09 | 2010-08-25 | 南京理工大学 | Preparation method of vanadium oxide thin film material for non-refrigerated infrared focal plane array |
| CN101950092A (en) * | 2010-09-08 | 2011-01-19 | 天津大学 | Terahertz wave band vanadium oxide optical switch and preparation method thereof |
| CN102002667A (en) * | 2010-11-22 | 2011-04-06 | 烟台睿创微纳技术有限公司 | Method and equipment for preparing high-repeatability vanadium oxide film |
| CN102251216A (en) * | 2011-07-19 | 2011-11-23 | 电子科技大学 | Method for preparing tungsten-doped vanadium oxide film |
| CN102952540B (en) * | 2011-08-25 | 2014-07-23 | 海洋王照明科技股份有限公司 | Samarium-doped strontium sulfate luminescent film, preparation method and organic electroluminescent device |
| CN102952540A (en) * | 2011-08-25 | 2013-03-06 | 海洋王照明科技股份有限公司 | Samarium-doped strontium sulfate luminescent film, preparation method and organic electroluminescent device |
| CN103361614A (en) * | 2013-06-29 | 2013-10-23 | 天津大学 | Method for preparing Terahertz modulator film material based on flexible substrate |
| CN104213087A (en) * | 2013-10-17 | 2014-12-17 | 常州博锐恒电子科技有限公司 | Magnetron sputtering preparation method of vanadium oxide |
| CN103540903A (en) * | 2013-10-21 | 2014-01-29 | 中国科学院上海硅酸盐研究所 | Low-temperature high-resistance temperature coefficient non-heat stagnation thin-film material and preparation method thereof |
| CN103540903B (en) * | 2013-10-21 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | A kind of Low-temperature high-resistance temperature coefficient non-heat stagnation thin-film material and preparation method thereof |
| CN103882399A (en) * | 2014-03-18 | 2014-06-25 | 天津大学 | Preparation method of flexible substrate based nano vanadium oxide functional film with phase transition characteristic |
| CN113774348A (en) * | 2021-09-22 | 2021-12-10 | 季华实验室 | High-temperature superconductor with amorphous vanadium oxide film, preparation method thereof and high-temperature superconducting coil |
| CN114250444A (en) * | 2021-12-01 | 2022-03-29 | 安徽光智科技有限公司 | Method for plasma-assisted chemical vapor deposition of high-purity tungsten sputtering target material |
| CN114049983A (en) * | 2021-12-27 | 2022-02-15 | 西安宏星电子浆料科技股份有限公司 | Chip resistor paste with high resistance concentration and preparation method thereof |
| CN114049983B (en) * | 2021-12-27 | 2022-04-08 | 西安宏星电子浆料科技股份有限公司 | Chip resistor paste with high resistance concentration and preparation method thereof |
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