CN1889276A - Porous silicon-base vanadium oxide thin film with excellent heat insulating performance and producing method - Google Patents
Porous silicon-base vanadium oxide thin film with excellent heat insulating performance and producing method Download PDFInfo
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- CN1889276A CN1889276A CNA2006100149030A CN200610014903A CN1889276A CN 1889276 A CN1889276 A CN 1889276A CN A2006100149030 A CNA2006100149030 A CN A2006100149030A CN 200610014903 A CN200610014903 A CN 200610014903A CN 1889276 A CN1889276 A CN 1889276A
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- 229910001935 vanadium oxide Inorganic materials 0.000 title claims abstract description 45
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000010409 thin film Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000010408 film Substances 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 238000004544 sputter deposition Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 4
- 229910021426 porous silicon Inorganic materials 0.000 claims description 37
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 235000019441 ethanol Nutrition 0.000 abstract description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 238000009413 insulation Methods 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 208000030208 low-grade fever Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The present invention discloses porous silica base vanadium oxide film with good heat-insulating property and preparation method, belonging to vanadium oxide thin film thermistor technology. Said porous silica base vanadium oxide film includes monocrystalline silicon substrate, porous silica layer, silicon dioxide layer and vanadium oxide film layer. Preparation process includes: cleaning monocrystalline silicon piece in turn in concentrated sulfuric acid, deionized water, acetone and ethanol; electro-chemical corrosion in hydrofluoric acid and absolute ethyl alcohol miscible liquids and washing-up by deionized water to make porous silica layer; generating silicon dioxide layer on porous silica layer surface in plasma chemistry vapour deposition equipment; sputtering to obtain good heat-insulating property porous silica base vanadium oxide thin layer by magnetron sputtering method. Said invention has advantages of easy controlled technological conditions, density film, fine adhesiveness with substrate, large and uniform area, and good heat-insulating property.
Description
Technical field
The present invention relates to a kind of porous silicon-base vanadium oxide thin film and preparation method of excellent heat insulating performance, belong to the vanadium oxide film thermistor technology.
Background technology
With VO
2For the vanadium oxide film VOx of base at room temperature has high temperature coefficient of resistance, can reach-2 * 10
-2K
-1More than, be 5～10 times of common metal film, be the ideal material that is used for making heat-sensitive sensor, Infrared Detectors and infrared imaging device at present.Realize the application of the thermo-responsive performance of vanadium oxide film in above-mentioned field, the heat-insulating property of substrate is most important, to guarantee the high sensitivity of micro element under low input power.The backing material that is used for vanadium oxide film at present mainly is a monocrystalline silicon, silicon is 156W/MK owing to have high thermal conductivity, and infrared radiation causes that the heat of film increases, be easy to lose, be unfavorable for the realization of vanadium oxide film excellent heat sensitive resistance performance by substrate; Also have on silicon the heat insulation layer of coating as polyimides as substrate, but its preparation technology and Si CMOS technology are incompatible, are difficult to the batch process and the low cost of realization device.Therefore for the thermo-sensitive property that makes vanadium oxide film finds full expression, and manufacture craft and Si CMOS process compatible, need have the silicon class backing material of lower thermal conductivity; Adopt micro-structurals such as outstanding platform, cantilever, major defect is that mechanical stability is bad.Porous silicon has low thermal conductivity, can reduce to below the 1W/MK, is good heat insulator, simultaneously the mechanical performance of structure is improved.Except good heat-insulating property and mechanical performance, the advantage that porous silicon is used as heat insulation layer in MEMS also is the compatibility of porous silicon and IC technology.The porous silicon surface of preparing is smooth, not only can the smooth film of deposit, can also form high-quality epitaxy single-crystal layer, and provide condition for further on the porous silicon heat insulation layer, being prepared as transducer.The employing porous silicon to substitute traditional heat insulation structure, can improve the sensitivity and the stability of low-grade fever dependent sensor as heat insulation layer greatly.
Summary of the invention
The porous silicon-base vanadium oxide thin film and the preparation method that the purpose of this invention is to provide a kind of excellent heat insulating performance, this porous base vanadium oxide thin film has good thermal insulation properties, and its preparation method is simple.
The present invention is realized by the following technical programs, a kind of porous silicon-base vanadium oxide thin film of excellent heat insulating performance, it is characterized in that, in monocrystalline silicon basic unit, be followed successively by porous silicon layer, silicon dioxide layer and vanadium oxide film layer, described porous silicon layer porosity is that 60-80%, thickness are that 20-110 μ m and aperture are the porous silicon of 10-50nm, described silicon dioxide layer thickness is 980-1020 's, and described vanadium oxide film layer thickness is 0.1 μ m-0.5 μ m.
The preparation method of above-mentioned porous silicon-base vanadium oxide thin film is characterized in that comprising following process:
1) be that to put into mass concentration be that 98% sulfuric acid and mass concentration are 30% 3: 1 by volume cleaning fluid of hydrogen peroxide for the single-sided polishing monocrystalline silicon piece of p type 100 crystal faces of 380-500 μ m with thickness, soak at ambient temperature, till bubble not, remove the organic pollution on surface; Rinse well with deionized water again, put into mass concentration then and be 20% HF solution and soak the oxide layer of removing the surface in 30 seconds, rinse well with deionized water, with silicon slice placed ultrasonic cleaning 5 minutes in acetone soln, put into the absolute ethyl alcohol ultrasonic cleaning again 5 minutes, it is standby at last silicon chip to be put into absolute ethyl alcohol;
2) will put into through the cleaned monocrystalline silicon piece of step 1) is that 1: 1 mass concentration is 40% the HF and the corrosive liquid of absolute ethyl alcohol by volume, in corrosive liquid, be that 40-80mA carries out electrochemical corrosion with the current density, etching time is 30-50 minute, take out then and utilize deionized water wash, making porosity is that 60-80%, thickness are that 20-110 μ m, aperture are the porous silicon of 10-50nm;
3) with step 2) porous silicon that makes is 4.5 * 10 in back of the body end vacuum
-1Pa, operating air pressure are 4.3Pa, and substrate temperature is 150 ℃, and working gas is N
2O and SiH
4, flow is respectively 12ml/min and 38ml/min, and deposition time is 10 minutes, and generating thickness on the porous silicon substrate is 980-1020 silica membrane layer;
4) silicon dioxide that step 3) is made/porous silicon substrate places the vacuum chamber of DPS-III type ultra high vacuum facing-target magnetron sputtering system equipment, adopting quality purity is that 99.9% vanadium metal is as target, quality purity be 99.999% argon gas and quality purity be 99.995% oxygen as working gas, be (2-3) * 10 with the base vacuum degree
-4Pa, sputter operating air pressure are 1-2.0Pa, and sputtering power is 200-240W, sputtering time 0.5-1 hour, and Ar, O
2Gas flow is respectively 48ml/min and 0.4ml/min, for the process conditions sputter obtains the vanadium oxide film layer that thickness is 0.1-0.5 μ m, thereby obtains the porous silicon-base vanadium oxide thin film of excellent heat insulating performance.
The invention has the advantages that, the film densification of adopting the facing-target magnetron sputtering system method to obtain, good with the substrate adhesiveness, area is big and even, and easy control of process conditions, porous silicon/silicon dioxide/vanadium oxide the structure for preparing does not need to carry out the corrosion of porous silicon substrate, just can make vanadium oxide film have heat-insulating property preferably, within 0～100 μ W power bracket, the resistance of the thermistor that deposits on the silicon base only is 2.1K Ω/μ W with the speed that power descends, and the resistance fall off rate that deposits on porous silicon layer can reach 41.6K Ω/μ W, and fall off rate is the former nearly 20 times.
Description of drawings
Fig. 1 is the structural representation of porous silicon-base vanadium oxide thin film of the present invention.Among the figure: 1 is silicon base, and 2 is porous silicon layer, and 3 is silicon dioxide layer, and 4 is the vanadium oxide film layer;
Fig. 2 is the temperature variant curve chart of resistance of embodiment 1 prepared porous silicon-base vanadium oxide thin film;
Fig. 3 approaches the resistance of vanadium film with variable power curve comparison diagram for the present invention prepared porous silicon-base vanadium oxide thin film and existing silica-based oxidation.Among the figure: 1 is that the preparation Vanadium Oxide Thin Film Resistance is with the curve of variable power on the silicon, and 2 is to prepare the curve of Vanadium Oxide Thin Film Resistance with variable power on the porous silicon;
Fig. 4 is the resistance of the vanadium oxide film for preparing with the inventive method curve comparison diagram with variable power on the porous silicon of different porosities.Among the figure: 1 for porosity be the Vanadium Oxide Thin Film Resistance for preparing on 79% the porous silicon curve with variable power, 2 for porosity is the Vanadium Oxide Thin Film Resistance for preparing on 73% the porous silicon curve with variable power, 3 for porosity be the Vanadium Oxide Thin Film Resistance for preparing on 63% the porous silicon curve with variable power.
Embodiment
1) adopting thickness is 420 μ m, long 2.5cm, and wide 1cm, p type 100 single-sided polishing monocrystalline silicon pieces carry out following processing as substrate to the silicon chip surface: get mass concentration and be 98% H
2SO
430 milliliters and mass concentration are 30% H
2O
210 milliliters are made into cleaning fluid, and silicon chip is put into cleaning fluid, soak at ambient temperature, place 40 minutes, have removed surperficial organic pollution; Silicon chip is taken out the back with deionized water rinsing 3 times from mixed acid, put into volume again and be 30 milliliters, mass concentration and be 20% HF solution and soak the oxide layer of removing the surface in 30 seconds; Rinse well with deionized water again; Is ultrasonic cleaning 5 minutes in 20 milliliters the acetone soln with silicon slice placed at volume; Silicon chip is taken out, put into volume again and be 20 milliliters absolute ethyl alcohol ultrasonic cleaning 5 minutes; It is standby that the taking-up silicon chip is put into absolute ethyl alcohol; Adopt the method for double flute electrochemical corrosion, corrosive liquid is that mass concentration is 35 milliliters of 40% HF and the mixed liquor of 35 milliliters of 99.7% absolute ethyl alcohols, at 80mA/cm
2Corrosion is 50 minutes under the current density, and the porosity of preparing is 77%, thickness is that 100 μ m, corrosion window area are 0.946cm
2The porous silicon sample; Using plasma chemical vapour deposition technique (PECVD) method deposits one deck silicon oxide film earlier on porous silicon chip, specific practice is: earlier the porous silicon of handling well is placed vacuum chamber, take out back of the body end vacuum to 4.5 * 10
-1Pa, working gas pressure is 4.3Pa, and substrate temperature is 150 ℃, and working gas is N
2O and SiH
4, throughput is respectively 12ml/min and 38ml/min, and deposition time is 10 minutes, the SiO that obtains
2Layer thickness is 1000 ; Employing is to the target reaction magnetocontrol sputtering method, prepare vanadium oxide film at above-mentioned porous silicon substrate with silica, quality purity is that 99.9% vanadium metal is as target, the quality purity of argon gas and oxygen is respectively 99.999% and 99.995%, to the concrete steps of target reaction magnetocontrol sputtering is: take out back of the body end vacuum to 2 * 10
-4Pa, oxygen and argon flow amount be respectively than being 48ml/min:0.4ml/min,, sputtering pressure 2Pa, sputtering power are 210W, sputtering time 60 minutes, substrate temperature is a room temperature, and obtaining length is 2cm, and width is 0.2cm, and thickness is the vanadium oxide film layer of 0.3 μ m; Above-mentioned vanadium oxide film is carried out the resistance-power characteristic test, and power bracket is: 0-100 μ W, the resistor power curve as shown in Figure 3.The resistance fall off rate that deposits on porous silicon layer can reach 41.6 K Ω/μ W, heat insulating construction better performances of the present invention.
Present embodiment is similar to embodiment 1, and difference is: in the step 1 preparation porous silicon technological parameter in etching time be 30 minutes, the porosity of the film that obtains is 73%, thickness is 42 μ m; The sputtering power of step 4 is 210W, and the time is 45 minutes, and sputtering pressure is 1.5Pa, and the resistor power curve as shown in Figure 4.The thermal conductivity of porous silicon and its porosity, thickness is inversely proportional to, and porosity reduces, and the vanadium oxide resistance is 85.7K Ω/μ W with the Mean Speed that power descends.
Present embodiment is similar to embodiment 1, and difference is: in the step 1 preparation porous silicon technological parameter in current density become 40mA.cm
-2, etching time is 50 minutes still, and the porosity of the film that obtains is 63%, and thickness is 21 μ m; The sputtering power of step 4 becomes 240W, and the time is 30 minutes, and sputtering pressure is 1Pa, and the resistor power curve as shown in Figure 4.The vanadium oxide resistance is 57.1K Ω/μ W with the Mean Speed that power descends.
Claims (2)
1. the porous silicon-base vanadium oxide thin film of an excellent heat insulating performance, it is characterized in that, in monocrystalline silicon basic unit, be followed successively by porous silicon layer, silicon dioxide layer and vanadium oxide film layer, described porous silicon layer porosity is that 20-110 μ m and aperture are the porous silicon of 10-50nm for 60-80% thickness, and described silicon dioxide layer thickness is 980-1020 , and described vanadium oxide film layer thickness is 0.1-0.5um.
2. preparation method by the porous silicon-base vanadium oxide thin film of the described excellent heat insulating performance of claim 1 is characterized in that comprising following process:
1) be that to put into mass concentration be that 98% sulfuric acid and mass concentration are 30% 3: 1 by volume cleaning fluid of hydrogen peroxide for the single-sided polishing monocrystalline silicon piece of p type 100 crystal faces of 380-500 μ m with thickness, soak at ambient temperature, till bubble not, remove the organic pollution on surface; Rinse well with deionized water again, put into mass concentration then and be 20% HF solution and soak the oxide layer of removing the surface in 30 seconds, rinse well with deionized water, with silicon slice placed ultrasonic cleaning 5 minutes in acetone soln, put into the absolute ethyl alcohol ultrasonic cleaning again 5 minutes, it is standby at last silicon chip to be put into absolute ethyl alcohol;
2) will put into through the cleaned monocrystalline silicon piece of step 1) is that 1: 1 mass concentration is 40% the HF and the corrosive liquid of absolute ethyl alcohol by volume, in corrosive liquid, be that 40-80mA carries out electrochemical corrosion with the current density, etching time is 30-50 minute, take out then and utilize deionized water wash, making porosity is that 20-110 μ m aperture is the porous silicon of 10-50nm for 60-80% thickness;
3) with step 2) porous silicon that makes is 4.5 * 10 in back of the body end vacuum
-1Pa, operating air pressure are 4.3Pa, and substrate temperature is 150 ℃, and working gas is N
2O and SiH
4, flow is respectively 12ml/min and 38ml/min, and deposition time is 10 minutes, and generating thickness on the porous silicon substrate is 980-1020 silica membrane layer;
4) silicon dioxide that step 3) is made/porous silicon substrate places the vacuum chamber of ultra high vacuum facing-target magnetron sputtering system equipment, adopting quality purity is that 99.9% vanadium metal is as target, quality purity be 99.999% argon gas and quality purity be 99.995% oxygen as working gas, be (2-3) * 10 with the base vacuum degree
-4Pa, the sputter operating air pressure is 1-2.0Pa, sputtering power is 200-240W, sputtering time 0.5-1 hour, argon and carrier of oxygen flow are respectively 48ml/min and 0.4ml/min, for the process conditions sputter obtains the vanadium oxide film layer that thickness is 0.1-0.5 μ m, thereby obtain the porous silicon-base vanadium oxide thin film of excellent heat insulating performance.
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| CN100546049C CN100546049C (en) | 2009-09-30 |
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| CN101964367A (en) * | 2010-08-23 | 2011-02-02 | 中国科学院微电子研究所 | Substrate with porous structure and preparation method thereof |
| CN102649625A (en) * | 2012-05-03 | 2012-08-29 | 北京鼎臣超导科技有限公司 | Method for cleaning glass substrate for coating |
| CN103245696A (en) * | 2013-05-11 | 2013-08-14 | 天津大学 | Method for preparing porous silicon-based one-dimensional nanowire gas sensitive element |
| CN104142359A (en) * | 2014-07-18 | 2014-11-12 | 苏州能斯达电子科技有限公司 | MEMS gas sensor and machining method thereof |
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| CN105388191A (en) * | 2015-11-19 | 2016-03-09 | 天津大学 | Preparation method of ceramic-based vanadium oxide nano rod structured room temperature CH4 sensor |
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| CN101964367A (en) * | 2010-08-23 | 2011-02-02 | 中国科学院微电子研究所 | Substrate with porous structure and preparation method thereof |
| CN102649625A (en) * | 2012-05-03 | 2012-08-29 | 北京鼎臣超导科技有限公司 | Method for cleaning glass substrate for coating |
| CN102649625B (en) * | 2012-05-03 | 2014-06-18 | 北京鼎臣超导科技有限公司 | Method for cleaning glass substrate for coating |
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| CN104142359B (en) * | 2014-07-18 | 2016-08-31 | 苏州能斯达电子科技有限公司 | A kind of MEMS gas sensor and processing method thereof |
| CN104181203B (en) * | 2014-08-13 | 2017-12-22 | 苏州能斯达电子科技有限公司 | A kind of MEMS gas sensors and preparation method thereof |
| CN104181203A (en) * | 2014-08-13 | 2014-12-03 | 苏州能斯达电子科技有限公司 | MEMS gas sensor and manufacturing method thereof |
| CN105388191A (en) * | 2015-11-19 | 2016-03-09 | 天津大学 | Preparation method of ceramic-based vanadium oxide nano rod structured room temperature CH4 sensor |
| CN108550450A (en) * | 2018-04-19 | 2018-09-18 | 中国科学院新疆理化技术研究所 | A kind of thermosensitive film preparation method with adiabatic buffer layer structure |
| CN110386585A (en) * | 2018-04-20 | 2019-10-29 | 上海新微技术研发中心有限公司 | Preparation method of porous silicon substrate and porous silicon substrate |
| CN110911351A (en) * | 2019-11-25 | 2020-03-24 | 上海交通大学 | Method for preparing silicon oxide on surface of silicon wafer |
| CN110911269A (en) * | 2019-12-02 | 2020-03-24 | 上海交通大学 | Silicon wafer with silicon oxide film on surface and preparation method |
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