CN104914211A - Preparation method of particle and short rod-like vanadium oxide film - Google Patents
Preparation method of particle and short rod-like vanadium oxide film Download PDFInfo
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Abstract
The invention discloses a preparation method of particle and short rod-like vanadium oxide film. The method comprises the steps of: (1) cleaning a ceramic sheet substrate; (2) conducting magnetron sputtering on the ceramic sheet substrate to prepare a Pt interdigital electrode; (3) conducting magnetron sputtering to prepare a metal vanadium film; (4) conducting magnetron sputtering to spray copper on a pure metal V film; and (5) rapidly annealing to prepare the vanadium oxide film. The method provided by the invention can quickly prepare particle and short rod-like vanadium oxide film, strictly control the process parameters and improve process repeatability and surface area of the vanadium oxide film. The vanadium oxide film has great potential in terms of improving the sensitivity of gas sensors, and can be better applied to reality.
Description
Technical field
The invention belongs to technical field of semiconductors, be specifically related to the preparation method of a kind of particle and corynebacterium vanadium oxide film.
Background technology
Vanadium oxide is as a kind of metal oxide semiconductor material, and the film formed by its preparation, owing to having different valence states and structure, causes the broad interest of researcher.Research finds, vanadium oxide film can be used as catalyzer in redox reaction, especially to hydrocarbon, oxysulfide, oxides of nitrogen, there is very large catalytic action, therefore, vanadium oxide film can be made gas sensor element, to certain gas, as ethanol, nitrogen dioxide, methane etc., detect.
As gas sensor, sensitivity, response/release time and working temperature are three key factors of a judge gas sensor.High sensitivity illustrates that gas sensor is high for the susceptibility of surveyed gas; Fast response/release time represents gas sensor and can make a response to surveyed gas fast, reinstatement state that also can be very fast after having responded; Working temperature determines the requirement of gas sensor for working environment.Generally speaking, as the metal-oxide semiconductor (MOS) of gas sensor, its working temperature is higher than room temperature.Therefore, low working temperature makes gas sensor better be applied in real life.Its medium sensitivity passes judgment on gas sensor to the physical quantity of surveyed gas sensitization degree as one, and its lifting is very important for gas sensor.At present, domestic and international researcher mainly through doping, prepare composite structure, optimize the serial of methods such as microscopic appearance to improve metal oxide thin films for the sensitivity of survey gas.The microscopic appearance wherein optimizing film has the meaning of reality for improving the sensitivity of film.In gas-sensitive reaction, survey gas and gas sensor contact area have impact on sensitivity.The contact area of gas and gas sensor is more abundant, then react more thorough, sensitivity is higher.Therefore, optimize the microscopic appearance of film, the contact area improving film and gas is very important for gas sensor.
Summary of the invention
In order to solve problems of the prior art, the invention provides the preparation method of a kind of particle and corynebacterium vanadium oxide film, overcoming the problem that the sensitivity of gas sensor in prior art is not high.
Technical scheme of the present invention is:
A preparation method for particle and corynebacterium vanadium oxide film, has following steps:
(1) cleaning ceramic sheet (alundum (Al2O3)) substrate:
Potsherd substrate used is of a size of 10mm × 25mm × 0.635mm.Potsherd substrate is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15-20min, removing surface organic matter impurity.Subsequently deionized water is put in potsherd substrate to clean, after having rinsed, put into absolute ethyl alcohol, therefrom take out dry for standby.
(2) magnetron sputtering prepares the interdigital electrode of Pt in potsherd substrate:
Adopt JCP-200 high vacuum magnetron sputtering coater in potsherd substrate, plate the interdigital electrode of Pt.Sputtering target material is the Pt metal target of purity 99.999%.Potsherd substrate cleaned in step (1) is added that the mask of interdigital electrode fixes, and puts into vacuum chamber.Mechanical pump and molecular pump is utilized to vacuumize, when high vacuum table is shown as 0.0E-5, pass into the argon gas that quality purity is 99.999% in vacuum chamber, argon gas flow velocity is 20-30sccm, adjustment sputtering power is 90-110W, sputters about the rotating speed of substrate is adjusted to half.Sputtering time is 2-3min, and base reservoir temperature during sputtering is room temperature.
(3) magnetron sputtering prepares the film of vanadium metal:
DPS-III type ultrahigh vacuum DC facing targets magnetron sputtering instrument is adopted to deposit pure vanadium metal film in the potsherd substrate being coated with Pt interdigital electrode.Deposition targets select purity be 99.999% vanadium metal target.First need to vacuumize, namely utilize mechanical pump and molecular pump to take out body vacuum to (3.0-4.0) × 10
-4pa.Air inlet after reaching required vacuum tightness in cavity.Using quality purity be the argon gas of 99.999% as working gas, controlling argon gas flow velocity is 45-50sccm, and the operating pressure of adjustment sputtering is 1.0-2.0pa.Finally sputter, the power in sputter procedure is 70-90W, and sputtering time is 20-40min, and base reservoir temperature during adjustment sputtering is that room temperature is to 500 DEG C.
(4) magnetron sputtering sprays copper on pure metal V film:
Adopt the copper facing on metal V film of DPS-III type ultrahigh vacuum DC facing targets magnetron sputtering instrument.Deposition targets is metallic copper.First mechanical pump and molecular pump is utilized to take out body vacuum to (3.0-4.0) × 10
-4pa.After having vacuumized, be that the argon gas of 99.999% passes in vacuum chamber by quality purity, controlling argon gas flow velocity is 40-50sccm, and the operating pressure of adjustment sputtering is 1.0-2.0pa.Sputter after above parameter adjustment is good, the power in sputter procedure is 70-90W, and sputtering time is 0-10s, and base reservoir temperature during sputtering is room temperature.
(5) vanadium oxide film is prepared in short annealing
The film that step (4) is obtained is put into quick anneal oven anneal, object is that vanadium film is oxidized to vanadium oxide film.The oxygen that purity is greater than 99.999% is passed in annealing process.The parameter arranged in annealing process is as follows: annealing temperature is 450-500 DEG C, and the heating-up time is 8-12s, and temperature retention time is 200-300s, and temperature fall time is 80-100s.Oxygen gas flow rate when heating up and be incubated is 3-8slpm, and oxygen gas flow rate during cooling is 10slpm.
Compared with the prior art, beneficial effect of the present invention is:
1) the vanadium oxide film particle size prepared is at Nano grade.Preparation technology is simple, and parameter is less and controllability is high, greatly shortens preparation time, improves repeatability.
2) a kind of method preparing particle and corynebacterium vanadium oxide film is fast provided.By base reservoir temperature during adjustment splash-proofing sputtering metal V and the operation carrying out spray copper on pure metal V film, the microscopic appearance of film is made to there occurs very large change, particle and corynebacterium has been become from sheet and stratiform, improve the surface area of film, improve significant for gas sensor sensitivity.
The inventive method can prepare particle and corynebacterium vanadium oxide film fast, can strict Controlling Technology parameter, improves the surface area of process repeatability and vanadium oxide film.Make vanadium oxide film have very large potentiality in the sensitivity raising of gas sensor, better can be applied to reality.
Accompanying drawing explanation
Fig. 1 (a) is the scanning electron microscope diagram shape of simple metal V in embodiment 1;
Fig. 1 (b) is the scanning electron microscope diagram shape of simple metal V in comparative example 1;
Fig. 2 (a) is the scanning electron microscope diagram shape of vanadium oxide film in embodiment 1;
Fig. 2 (b) is the scanning electron microscope diagram shape of vanadium oxide film in embodiment 2;
Fig. 2 (c) is the scanning electron microscope diagram shape of vanadium oxide film in embodiment 3;
Fig. 2 (d) is the scanning electron microscope diagram shape of vanadium oxide film in comparative example 1;
Fig. 2 (e) is the scanning electron microscope diagram shape of vanadium oxide film in comparative example 2.
Embodiment
Below in conjunction with accompanying drawing, the present invention is elaborated.
Embodiment 1
1) cleaning ceramic sheet substrate:
The potsherd substrate being of a size of 10mm × 25mm × 0.635mm is put into successively acetone solvent, absolute ethyl alcohol sonic oscillation 15min.Put it in deionized water subsequently and clean, after having rinsed, put into absolute ethyl alcohol, therefrom take out dry for standby.
2) magnetron sputtering prepares the interdigital electrode of Pt in potsherd substrate:
Adopt small-sized magnetic control sputtering device in potsherd substrate, plate the interdigital electrode of Pt.Potsherd substrate cleaned in step (1) is added that the mask of interdigital electrode fixes, and puts into vacuum chamber.Utilize mechanical pump and molecular pump to vacuumize, when high vacuum table is shown as 0.0E-5, pass into the argon gas that quality purity is 99.999% in vacuum chamber, argon gas flow velocity is 24sccm, and adjustment sputtering power is 100W, the rotating speed of substrate is adjusted to half and sputters.Sputtering time is 2min, and base reservoir temperature during sputtering is room temperature.
3) magnetron sputtering prepares the film of vanadium metal:
DPS-III type ultrahigh vacuum DC facing targets magnetron sputtering instrument is adopted to deposit pure vanadium metal film in the potsherd substrate being coated with Pt interdigital electrode.Deposition targets select purity be 99.999% vanadium metal target.First need to vacuumize, namely utilize mechanical pump and molecular pump to take out body vacuum to 4.0 × 10
-4pa.Air inlet after reaching required vacuum tightness in cavity.Using quality purity be the argon gas of 99.999% as working gas, controlling argon gas flow velocity is 48sccm, and the operating pressure of adjustment sputtering is 2.0pa.Finally sputter, the power in sputter procedure is 72.5W, and sputtering time is 35min, the base reservoir temperature 400 DEG C during adjustment sputtering.The scanning electron microscope image of the metal V film that gained is pure is as shown in Fig. 1 (a).
4) magnetron sputtering sprays copper on pure metal V film:
Adopt the copper facing on metal V film of DPS-III type ultrahigh vacuum DC facing targets magnetron sputtering instrument.Deposition targets is metallic copper.First mechanical pump and molecular pump is utilized to take out body vacuum to 4.0 × 10
-4pa.After having vacuumized, be that the argon gas of 99.999% passes in vacuum chamber by quality purity, controlling argon gas flow velocity is 45sccm, and the operating pressure of adjustment sputtering is 2.0pa.Sputter after above parameter adjustment is good, the power in sputter procedure is 85W, and sputtering time is 5s, and base reservoir temperature during sputtering is room temperature.
5) vanadium oxide film is prepared in short annealing
The film that step (4) is obtained is put into quick anneal oven anneal, pass into the oxygen that purity is greater than 99.999%.The parameter arranged in annealing process is as follows: annealing temperature is 480 DEG C, and the heating-up time is 9.6s, and temperature retention time is 270s, and temperature fall time is 120s.Oxygen gas flow rate when heating up and be incubated is 5slpm, and oxygen gas flow rate during cooling is 10slpm.Utilize the surround and watch pattern of scanning electron microscope to the vanadium oxide film after annealing to observe, gained image is as shown in Fig. 2 (a).
Embodiment 2
The present embodiment is similar to embodiment 1, and difference is: step 3) in preparation pure metal V film time base reservoir temperature be room temperature.Sem observation is utilized to anneal rear oxidation vanadium film microscopic appearance as shown in Fig. 2 (b).
Embodiment 3
The present embodiment is similar to embodiment 1, and difference is: step 3) in preparation pure metal V film time base reservoir temperature be 350 DEG C.Sem observation is utilized to anneal rear oxidation vanadium film microscopic appearance as shown in Fig. 2 (c).
Comparative example 1
The present embodiment is similar to embodiment 1, and difference is: step 3) in preparation pure metal V film time base reservoir temperature be room temperature.And copper is not sprayed in V film surface, namely carry out step 4).The metal V film utilizing sem observation pure and the surface topography after annealing, metal V film image is as shown in Fig. 1 (b), and annealing rear oxidation vanadium film microscopic appearance is as shown in Fig. 2 (d).
Comparative example 2
The present embodiment is similar to embodiment 1, and difference is: copper is not sprayed in magnetron sputtering gained V film surface, namely carry out step 4).Utilize the surface topography of sem observation annealing rear oxidation vanadium as shown in Fig. 2 (e).
From the example of 4 above, base reservoir temperature during sputtering simple metal V film greatly have impact on the surface topography of V film, can be found out by the contrast of Fig. 1 (a) and Fig. 1 (b), base reservoir temperature is heated, cohesion is there occurs between granule, shape is by triangularity in order to spherical, and size is irregular.Base reservoir temperature when sputtering pure V film and whether spray the microscopic appearance that copper also greatly have impact on annealing rear oxidation vanadium film on V film.By relatively finding out of Fig. 2 (d) and (e), the lifting of base reservoir temperature, the pattern for vanadium oxide film does not have the change of matter; Found out by the contrast of Fig. 2 (b) and (d), base reservoir temperature is room temperature, and at V film surface spray copper after annealing, partial particulate and club shaped structure appear in gained vanadium oxide film surface, but still have mass part to be sheet; Found out by the contrast of Fig. 2 (a), (b) and (c), base reservoir temperature heated, and spray copper annealing, the surface of vanadium oxide film is graininess and bar-shaped, is evenly distributed.As can be seen here, copper is the key factor changing film morphology, and the heating of base reservoir temperature, this particle and club shaped structure can be made to distribute more fine and close and even.Therefore, by increasing base reservoir temperature, and to V film surface spray copper, the microscopic appearance of vanadium oxide film can be made to change a lot, make that it has sheet, layer structure becomes particle and club shaped structure, increase the surface area of film, can effectively increase gas absorption area, improve the air-sensitive performance of vanadium oxide film.
Claims (9)
1. a preparation method for particle and corynebacterium vanadium oxide film, is characterized in that, comprises the following steps:
(1) cleaning ceramic sheet substrate;
(2) magnetron sputtering prepares the interdigital electrode of Pt in potsherd substrate;
(3) magnetron sputtering prepares the film of vanadium metal;
(4) magnetron sputtering sprays copper on pure metal V film;
(5) vanadium oxide film is prepared in short annealing.
2. the preparation method of particle and corynebacterium vanadium oxide film according to claim 1, it is characterized in that, described step (1) refers to puts into acetone solvent, absolute ethyl alcohol sonic oscillation 15-20min successively by potsherd substrate, removing surface organic matter impurity; Subsequently deionized water is put in potsherd substrate to clean, after having rinsed, put into absolute ethyl alcohol, therefrom take out dry for standby.
3. the preparation method of particle and corynebacterium vanadium oxide film according to claim 1, it is characterized in that, described step (2) adopts JCP-200 high vacuum magnetron sputtering coater in potsherd substrate, plate the interdigital electrode of Pt, and sputtering target material is the Pt metal target of purity 99.999%.
4. the preparation method of particle and corynebacterium vanadium oxide film according to claim 3, it is characterized in that, described step (2) is specially and potsherd substrate cleaned in step (1) is added that the mask of interdigital electrode fixes, and puts into vacuum chamber; Mechanical pump and molecular pump is utilized to vacuumize, when high vacuum table is shown as 0.0E-5, pass into the argon gas that quality purity is 99.999% in vacuum chamber, argon gas flow velocity is 20-30sccm, adjustment sputtering power is 90-110W, sputters about the rotating speed of substrate is adjusted to half; Sputtering time is 2-3min, and base reservoir temperature during sputtering is room temperature.
5. the preparation method of particle and corynebacterium vanadium oxide film according to claim 1, it is characterized in that, described step (3) adopts DPS-III type ultrahigh vacuum DC facing targets magnetron sputtering instrument to deposit pure vanadium metal film in the potsherd substrate being coated with Pt interdigital electrode, deposition targets select purity be 99.999% vanadium metal target.
6. the preparation method of particle and corynebacterium vanadium oxide film according to claim 5, it is characterized in that, described step (3) is specially and first needs to vacuumize, and namely utilizes mechanical pump and molecular pump to take out body vacuum to (3.0-4.0) × 10
-4pa, air inlet after reaching required vacuum tightness in cavity; Using quality purity be the argon gas of 99.999% as working gas, controlling argon gas flow velocity is 45-50sccm, and the operating pressure of adjustment sputtering is 1.0-2.0pa; Finally sputter, the power in sputter procedure is 70-90W, and sputtering time is 20-40min, and base reservoir temperature during adjustment sputtering is that room temperature is to 600 DEG C.
7. the preparation method of particle and corynebacterium vanadium oxide film according to claim 1, is characterized in that, described step (4) adopts the copper facing on metal V film of DPS-III type ultrahigh vacuum DC facing targets magnetron sputtering instrument, and deposition targets is metallic copper.
8. the preparation method of particle and corynebacterium vanadium oxide film according to claim 7, it is characterized in that, described step (4) is specially and first utilizes mechanical pump and molecular pump to take out body vacuum to (3.0-4.0) × 10
-4quality purity, after having vacuumized, is that the argon gas of 99.999% passes in vacuum chamber by Pa, and controlling argon gas flow velocity is 40-50sccm, and the operating pressure of adjustment sputtering is 1.0-2.0pa; Sputter after above parameter adjustment is good, the power in sputter procedure is 70-90W, and sputtering time is 0-10s, and base reservoir temperature during sputtering is room temperature.
9. the preparation method of particle and corynebacterium vanadium oxide film according to claim 1, is characterized in that, pass into the oxygen that purity is greater than 99.999% in described step (5) annealing process; The parameter arranged in annealing process is as follows: annealing temperature is 450-500 DEG C, and the heating-up time is 8-12s, and temperature retention time is 200-300s, and temperature fall time is 80-100s; Oxygen gas flow rate when heating up and be incubated is 3-8slpm, and oxygen gas flow rate during cooling is 10slpm.
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| CN112683961A (en) * | 2020-12-02 | 2021-04-20 | 赛莱克斯微系统科技（北京）有限公司 | Gas sensor and method for manufacturing gas-sensitive film thereof |
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