CN104439245A - Method for preparing single-orientation thermosensitive thin film through vacuum coating - Google Patents
Method for preparing single-orientation thermosensitive thin film through vacuum coating Download PDFInfo
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- CN104439245A CN104439245A CN201310429241.3A CN201310429241A CN104439245A CN 104439245 A CN104439245 A CN 104439245A CN 201310429241 A CN201310429241 A CN 201310429241A CN 104439245 A CN104439245 A CN 104439245A
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000010409 thin film Substances 0.000 title claims abstract description 13
- 238000001771 vacuum deposition Methods 0.000 title claims abstract description 6
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 10
- 239000011029 spinel Substances 0.000 claims abstract description 10
- 239000010408 film Substances 0.000 claims description 34
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 20
- 238000004544 sputter deposition Methods 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 229910018553 Ni—O Inorganic materials 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 6
- 239000004575 stone Substances 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 210000001161 mammalian embryo Anatomy 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 230000011218 segmentation Effects 0.000 claims description 5
- 238000010583 slow cooling Methods 0.000 claims description 5
- YQOXCVSNNFQMLM-UHFFFAOYSA-N [Mn].[Ni]=O.[Co] Chemical compound [Mn].[Ni]=O.[Co] YQOXCVSNNFQMLM-UHFFFAOYSA-N 0.000 claims 4
- 239000011572 manganese Substances 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Physical Vapour Deposition (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing a single-orientation thermosensitive thin film through vacuum coating. By using the method, the thin film large in area and good in compactness can be prepared. Compared with a thin film prepared by a sol-gel method, the method is more accurate in parameter control, and the prepared thin film is higher in compactness and of a single spinel structure. The thin film prepared through the method can be used for manufacturing linear array thermosensitive detection devices, area array thermosensitive detection devices, thermistor detecting devices of a microbridge structure and thermistor detecting devices of a top and bottom electrode structure.
Description
Technical field
The present invention relates to a kind of method that single-orientated thermosensitive film is prepared in vacuum coating.
Background technology
Mn-Co-Ni-O series material is a kind of thermo-sensitive material with very high negative temperature coefficient of resistance.Such oxide semiconductor material is because of its stable performance, and the feature that operating temperature is wide and obtain very large development, is widely used in thermometric, temperature control, compensation, voltage stabilizing, remote control, flow, flow-speed measurement and time delay equipment.In addition, this kind of material has the excellent specific property such as broad spectral response and performance long-term stability, in the detection of low temperature temperature-sensitive and civilian Uncooled infrared detection of space technology, have very important application.MCNO then has the minimum resistivity of this type of series material, therefore in Mn-Co-Ni-O thermo-sensitive material, occupies critical role.
The advantage that sol-gal process prepares thin-film material is that equipment is simple, cost is low, stoichiometric proportion is easy to control; Shortcoming is that the impact that quality of materials is subject to preparation process condition and external environment situation is comparatively large, and have very large empirical, preparation parameter is difficult to quantize.Pulsed laser deposition utilizes high-energy focusing laser pulse bundle to irradiate target material surface, the thin layer of target material surface is burnt, form twilight sunset, on substrate, gathers film forming, its advantage is that the ratio of component of the film prepared and the stoichiometric proportion of target are consistent, shortcoming is that the normal cohesion in film surface forms subparticle and makes surface quality undesirable, is unfavorable for preparing large area film.And utilize magnetically controlled sputter method to prepare film, then have that thin film composition dense uniform, film forming speed are fast, stable performance, film adhesive strength advantages of higher.
This patent prepares the method for the MCNO film of single spinel structure by providing magnetron sputtering method.Apply this method, the MCN film that large area, compactness are good can be prepared.Compare polycrystalline MCNO film prepared by sol-gal process, the film that this method is made is single spinel structure, and state modulator is more accurate, and the MCNO film density prepared is higher.
Summary of the invention
The object of this invention is to provide a kind of method that single-orientated thermosensitive film is prepared in vacuum coating, the technical problem that in the chemical solution method before solving, state modulator precision is not high, quality of forming film is easily affected by environment.
The object of the present invention is achieved like this:
(1) polycrystal target is prepared.Sol-gal process is adopted to prepare powder and the polycrystal target of Mn-Co-Ni-O.Take acetate powder according to the ratio of metal ion chemistry metering than Mn: Co: Ni=13: 8: 4, use sol-gal process to prepare MCNO powder.Get 60gMCNO powder, add PVA binding agent, granulation, be namely pressed into plain embryo down at 40MPa, segmentation dries burning 10 hours after coming unstuck under 1050 degrees Celsius, be cooled to 800 degrees Celsius and dry burnings 12 hours.Take out with after stove cooling.Polishing, polishing, obtained diameter 61 millimeters, thickness is about 4 millimeters, the MCNO polycrystal target of the good Emission in Cubic spinel structure of density.
(2) magnetron sputtering deposition MCNO film: select MP-3S type high vacuum magnetron sputtering coating system, open chamber, be positioned on rotary table top by the white stone substrate slice cleaned up, covers vacuum chamber chamber lid, extracts background vacuum to 5 × 10
-4pa, logical argon gas stream, choose 45 degree of inclined target radio-frequency sputtering patterns, sputtering power is 60-80W, and operating voltage is 220V, sputters under straight argon atmosphere; Partial pressure of ar gas be 0.4Pa substrate and target distance be 25cm, in thin film growth process, underlayer temperature is 200 degrees Celsius, the thickness of prepared film is controlled between 120nm-230nm according to sputtering power and sputtering time, after having sputtered, close argon gas, closure molecule pump, be slow cooling to 150 degrees Celsius, close mechanical pump, open vent valve, be down to after room temperature until rotary table top temperature and sample is taken out.
Annealing in process: the film of acquisition and substrate slice to be placed in quick anneal oven in 750 degrees Celsius: anneal 30 minutes to 1 hour, be down to after room temperature until body of heater and take out sample strip.
Accompanying drawing explanation
Fig. 1 is the method flow diagram that magnetron sputtering prepares MCNO film.
Fig. 2 sputters the X-ray diffractogram that thickness is respectively the MCNO film of 120nm, 150nm and 230nm on white stone substrate slice.Respectively through 750 degrees Celsius, 30 minutes and 750 degrees Celsius, 30 minutes, the annealing in process of 750 degrees Celsius, 60 minutes, both diffraction patterns all met spinel structure, and have single spinel structure.
Detailed description of the invention
Examples of implementation 1
(1) polycrystal target is prepared.Sol-gal process is adopted to prepare powder and the polycrystal target of Mn-Co-Ni-O.Take acetate powder according to the ratio of metal ion chemistry metering than Mn: Co: Ni=13: 8: 4, use sol-gal process to prepare MCNO powder; Get 60gMCNO powder, add binding agent, granulation, under 40MPa, be pressed into plain embryo, segmentation dries burning 10 hours after coming unstuck under 1050 degrees Celsius, Temperature fall to 800 degree Celsius dries burning 12 hours; Take out with after stove cooling, polishing, polishing, obtained diameter 61 millimeters, thickness is about 4 millimeters, the MCNO polycrystal target of the good Emission in Cubic spinel structure of density.
(2) magnetron sputtering deposition MCNO film: select MP-3S type high vacuum magnetron sputtering coating system, open chamber, be positioned on rotary table top by the white stone substrate slice cleaned up, covers vacuum chamber chamber lid, extracts background vacuum to 5 × 10
-4pa, logical argon gas stream, choose 45 degree of inclined target radio-frequency sputtering patterns, sputtering power is 60W, and operating voltage is 220V, sputters under straight argon atmosphere; Partial pressure of ar gas be 0.4Pa substrate and target distance be 25cm, in thin film growth process, underlayer temperature is 200 degrees Celsius, sputtering time 2.5 hours, prepares the thickness of film at about 120nm, after having sputtered, close argon gas, closure molecule pump, is slow cooling to 150 degrees Celsius, closes mechanical pump, open vent valve, be down to after room temperature until rotary table top temperature and sample is taken out.
(3) annealing in process: the film of acquisition and substrate slice to be placed in quick anneal oven in 750 degrees Celsius: anneal 30 minutes.Be down to after room temperature until body of heater and take out sample strip.
Examples of implementation 2
(1) polycrystal target is prepared: adopt sol-gal process to prepare powder and the polycrystal target of Mn-Co-Ni-O.Take acetate powder according to the ratio of metal ion chemistry metering than Mn: Co: Ni=13: 8: 4, use sol-gal process to prepare MCNO powder; Get 60gMCNO powder, add binding agent, granulation, under 40MPa, be pressed into plain embryo, segmentation dries burning 10 hours after coming unstuck under 1050 degrees Celsius, Temperature fall to 800 degree Celsius dries burning 12 hours; Take out with after stove cooling, polishing, polishing, obtained diameter 61 millimeters, thickness is about 4 millimeters, the MCNO polycrystal target of the good Emission in Cubic spinel structure of density.
(2) magnetron sputtering deposition MCNO film: select MP-3S type high vacuum magnetron sputtering coating system, open chamber, be positioned on rotary table top by the white stone substrate slice cleaned up, covers vacuum chamber chamber lid, extracts background vacuum to 5 × 10
-4pa, logical argon gas stream, choose 45 degree of inclined target radio-frequency sputtering patterns, sputtering power is 80W, and operating voltage is 220V, sputters under straight argon atmosphere; Partial pressure of ar gas be 0.4Pa substrate and target distance be 25cm, in thin film growth process, underlayer temperature is 200 degrees Celsius, sputtering time 3 hours, prepares the thickness of film at about 150nm, after having sputtered, close argon gas, closure molecule pump, is slow cooling to 150 degrees Celsius, closes mechanical pump, open vent valve, be down to after room temperature until rotary table top temperature and sample is taken out;
(3) annealing in process: the film of acquisition and substrate slice to be placed in quick anneal oven in 750 degrees Celsius: anneal 30 minutes, be down to after room temperature until body of heater and take out sample strip.
Examples of implementation 3
(1) polycrystal target is prepared: adopt sol-gal process to prepare powder and the polycrystal target of Mn-Co-Ni-O.Take acetate powder according to the ratio of metal ion chemistry metering than Mn: Co: Ni=13: 8: 4, use sol-gal process to prepare MCNO powder; Get 60gMCNO powder, add binding agent, granulation, under 40MPa, be pressed into plain embryo, segmentation dries burning 10 hours after coming unstuck under 1050 degrees Celsius, Temperature fall to 800 degree Celsius dries burning 12 hours; Take out with after stove cooling, polishing, polishing, obtained diameter 61 millimeters, thickness is about 4 millimeters, the MCNO polycrystal target of the good Emission in Cubic spinel structure of density.。
(2) magnetron sputtering deposition MCNO film: select MP-3S type high vacuum magnetron sputtering coating system, open chamber, be positioned on rotary table top by the white stone substrate slice cleaned up, covers vacuum chamber chamber lid, extracts background vacuum to 5 × 10
-4pa, logical argon gas stream, choose 45 degree of inclined target radio-frequency sputtering patterns, sputtering power is 80W, and operating voltage is 220V, sputters under straight argon atmosphere; Partial pressure of ar gas be 0.4Pa substrate and target distance be 25cm, in thin film growth process, underlayer temperature is 200 degrees Celsius, sputtering time 3 hours, prepares the thickness of film at about 230nm, after having sputtered, close argon gas, closure molecule pump, is slow cooling to 150 degrees Celsius, closes mechanical pump, open vent valve, be down to after room temperature until rotary table top temperature and sample is taken out.
(3) annealing in process: the film of acquisition and substrate slice to be placed in quick anneal oven in 750 degrees Celsius: anneal 30 minutes, be down to after room temperature until body of heater and take out sample strip.
Claims (1)
1. a method for single-orientated thermosensitive film is prepared in vacuum coating, it is characterized in that concrete steps are as follows:
Steps A prepares polycrystal target: adopt sol-gal process to prepare powder and the polycrystal target of Mn-Co-Ni-O.Take acetate powder according to the ratio of metal ion chemistry metering than Mn: Co: Ni=13: 8: 4, use sol-gal process to prepare manganese cobalt nickel oxygen powder; Get 60g manganese cobalt nickel oxygen powder, add binding agent, granulation, under 40MPa, be pressed into plain embryo, segmentation dries burning 10 hours after coming unstuck under 1050 degrees Celsius, Temperature fall to 800 degree Celsius dries burning 12 hours; Take out with after stove cooling, polishing, polishing, obtained diameter 61 millimeters, thickness is about 4 millimeters, the manganese cobalt nickel oxygen polycrystal target of the good Emission in Cubic spinel structure of density;
Step B magnetron sputtering deposition manganese cobalt nickel oxygen film: select MP-3S type high vacuum magnetron sputtering coating system, open chamber, be positioned on rotary table top by the white stone substrate slice cleaned up, covers vacuum chamber chamber lid, extracts background vacuum to 5 × 10
-4pa, logical argon gas stream, choose 45 degree of inclined target radio-frequency sputtering patterns, sputtering power is 60-80W, and operating voltage is 220V, sputters under straight argon atmosphere; Partial pressure of ar gas be 0.4Pa substrate and target distance be 25cm, in thin film growth process, underlayer temperature is 200 degrees Celsius, the thickness of prepared film is controlled between 120nm-230nm according to sputtering power and sputtering time, after having sputtered, close argon gas, closure molecule pump, be slow cooling to 150 degrees Celsius, close mechanical pump, open vent valve, be down to after room temperature until rotary table top temperature and sample is taken out;
Step C annealing in process: the film of acquisition and substrate slice to be placed in quick anneal oven in 750 degrees Celsius: anneal 30 minutes to 1 hour, be down to after room temperature until body of heater and take out sample strip.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310429241.3A CN104439245A (en) | 2013-09-17 | 2013-09-17 | Method for preparing single-orientation thermosensitive thin film through vacuum coating |
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| CN201310429241.3A CN104439245A (en) | 2013-09-17 | 2013-09-17 | Method for preparing single-orientation thermosensitive thin film through vacuum coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011747A (en) * | 2016-06-08 | 2016-10-12 | 中国科学院新疆理化技术研究所 | Preparation method of flexible thermosensitive films |
| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient thermal film |
-
2013
- 2013-09-17 CN CN201310429241.3A patent/CN104439245A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011747A (en) * | 2016-06-08 | 2016-10-12 | 中国科学院新疆理化技术研究所 | Preparation method of flexible thermosensitive films |
| CN109735807A (en) * | 2019-02-27 | 2019-05-10 | 华中科技大学 | A kind of preparation method of negative temperature coefficient thermal film |
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