CN100424820C - A technique to generate mixed allotropic structure of VO2 film on Si base - Google Patents
A technique to generate mixed allotropic structure of VO2 film on Si base Download PDFInfo
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- CN100424820C CN100424820C CNB2006101510721A CN200610151072A CN100424820C CN 100424820 C CN100424820 C CN 100424820C CN B2006101510721 A CNB2006101510721 A CN B2006101510721A CN 200610151072 A CN200610151072 A CN 200610151072A CN 100424820 C CN100424820 C CN 100424820C
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Abstract
The related growing technology for mixed allotropic VO2 film comprises: 1. cleaning the substrate; 2. removing the impurity gas; 3. filling Ar gas, and starting up the RF sputtering system; 4. sputtering the VO2 film on Si substrate; 5. vacuum annealing and sintering to obtain the final product comprised only VO2(B) and VO2(M). The product has surface roughness as 6-15nm, TCR value up to -1.50%/K~-5.65%/K, and resistively as 0.06~10.44omega .cm, and can increase the sensitivity of Si-base room-temperature IR detector 5~10%.
Description
Technical field
The present invention relates to a kind of growth VO
2The technology of film.
Background technology
VO
2Film is that recent two decades comes the domestic and international research focus because its excellent photoelectric properties and sensitive characteristic more and more are subject to people's attention, and has been widely used in photoelectric switching device, thermistor and room temperature infrared detector.Aspect Infrared Detectors, adopt growth orientation VO in the Si substrate
2Film helps large-area VO
2Detector array and Si base signal reads that to carry out monolithic integrated with processing unit.VO
2Have four kinds of allotropy structure: VO
2(A), VO
2(B), VO
2(M) and VO
2(R), VO wherein
2(B) (monocline, lattice constant: a=1.203nm, b=0.369nm, c=0.642nm) and VO
2(M) (monocline, lattice constant: a=0.575nm, b=0.542nm, c=0.538nm) structure close, near room temperature, be semiconductor, have high heat resistance temperature coefficient (TCR) value (TCR
VO2 (B)≈-2%/K, TCR
VO2 (M)≈-4%/K) is the desirable thermo-sensitive material that is applied to Si substrate room temperature infrared detector; And VO
2(A) (tetragonal, lattice constant: a=0.844nm, b=0.844nm, c=0.768nm) and VO
2(R) (rutile structure, lattice constant: a=0.455nm, b=0.455nm, c=0.288nm) heat resistance temperature coefficient (TCR) value is low.Technologies such as the sol-gel process that adopts, pulsed laser deposition, chemical vapour deposition technique, magnetron sputtering method are at the VO of Si basal growth at present
2Film has VO
2(A) and/or VO
2(R), heat resistance temperature coefficient is lower, has had a strong impact on the detectivity of room temperature infrared detector.
Summary of the invention
The objective of the invention is in order to solve the VO of present technology at the Si basal growth
2Film has VO
2(A) and/or VO
2(R), heat resistance temperature coefficient is low, has had a strong impact on the problem of the detectivity of room temperature infrared detector, and a kind of Si basal growth mixing allotropy structure of VO that provides
2The technology of film.Si basal growth mixing allotropy structure of VO
2The technology of film is carried out according to the following steps: (one) cleans the Si substrate and removes oxide-film; (2) Si substrate and simple substance V target are placed the settling chamber, in the settling chamber, feed Ar gas and vacuumize again, and repeatable operation 4～10 times, the Si base reservoir temperature remains 400 ℃; (3) feed Ar gas and open rf magnetron sputtering coating system power supply once more; (4) treat that the Ar pneumoelectric strengthens radio-frequency power voltage gradually to 300V after producing plasma, feed O immediately
2Gas, O
2The total gas flow rate of gas and Ar gas is 23～27sccm, and chamber pressure is controlled to be 0.30～0.35Pa, and it is 400 ℃ that the Si substrate keeps temperature, and the distance between simple substance V target and Si substrate is 58～62mm, and the Si substrate bias is 0V, Si primary surface VO
2Film stops radio frequency sputtering after reaching setting thickness, is cooled to 200 ℃ with the settling chamber, and then stops O
2The feeding of gas and Ar gas; (5) the sputter growth there is VO
2Quartz ampoule is enclosed in the Si substrate of film, vacuumizes, and vacuum degree reduces to 10 in the quartz ampoule
-3～10
-2Pa vacuumizes quartz ampoule and puts into resistance furnace annealing, and annealing temperature is 450 ℃～500 ℃, and annealing time is 8～15h, and the vitreosil pipe is cooled to room temperature with resistance furnace then, the Si base VO that promptly obtains growing and mix the allotropy structure
2Film; O in its step (four)
2Throughput accounts for 7.8% of total gas flow rate.The mixing allotropy structure of VO that the present invention grows on the Si base
2Film only contains the VO of high heat resistance temperature coefficient value
2(B) and VO
2(M) two kinds of allotropy structures.The mixing allotropy structure of VO that the present invention grows on the Si base
2Film surface is smooth, roughness is 6nm～15nm, VO
2Film heat resistance temperature coefficient (TCR) height in 25 ℃ of environment is-1.50%/K～-5.65%/K, VO
2Film resistivity in 25 ℃ of environment is moderate to be 0.06 Ω cm～10.44 Ω cm, has improved the detection performance of Si basal cell temperature Infrared Detectors, and especially the detectivity of Si basal cell temperature Infrared Detectors has improved 5～10%.
Embodiment
Embodiment one: present embodiment Si basal growth mixes with the abnormally-structured VO of rope
2The technology of film is carried out according to the following steps: (one) cleans the Si substrate and removes oxide-film; (2) Si substrate and simple substance V target are placed the settling chamber, in the settling chamber, feed Ar gas and vacuumize again, and repeatable operation 4～10 times, the Si base reservoir temperature remains 400 ℃; (3) feed Ar gas and open rf magnetron sputtering coating system power supply once more; (4) treat that the Ar pneumoelectric strengthens radio-frequency power voltage gradually to 300V after producing plasma, feed O immediately
2Gas, O
2The total gas flow rate of gas and Ar gas is 23～27sccm, and chamber pressure is controlled to be 0.30～0.35Pa, and it is 400 ℃ that the Si substrate keeps temperature, and the distance between simple substance V target and Si substrate is 58～62mm, and the Si substrate bias is 0V, Si primary surface VO
2Film stops radio frequency sputtering after reaching setting thickness, is cooled to 200 ℃ with the settling chamber, and then stops O
2The feeding of gas and Ar gas; (5) the sputter growth there is VO
2Quartz ampoule is enclosed in the Si substrate of film, vacuumizes, and vacuum degree reduces to 10 in the quartz ampoule
-3～10
-2Pa vacuumizes quartz ampoule and puts into resistance furnace annealing, and annealing temperature is 450 ℃～500 ℃, and annealing time is 8～15h, and the vitreosil pipe is cooled to room temperature with resistance furnace then, the Si base VO that promptly obtains growing and mix the allotropy structure
2Film; O in its step (four)
2Throughput accounts for 7.8% of total gas flow rate.
Set Si primary surface VO in the present embodiment
2Film thickness is 2.8 μ m, Si primary surface VO
2The thickness of film can be set according to actual needs.The Si base reservoir temperature remains 400 ℃ and can remove residual water of substrate surface and volatile impurity in the present embodiment step (two).
The Si base reservoir temperature is as the criterion with the temperature that thermocouple records among step in the present embodiment (two) and (four); The rf magnetron sputtering coating system is the rf magnetron sputtering coating machine in the step (three); Gas flow is controlled Si primary surface VO in the step (four) with mass flowmenter
2The thickness of film records with quartz crystal oscillator and is as the criterion; With KSW-12-11B type temperature control instrument temperature control, resistance furnace adopts SX in the step (five)
3/ 12-10 molding box formula resistance furnace.The present embodiment roughness of film utilizes atomic force microscope to carry software detection, present embodiment VO
2The film roughness is 6nm～15nm.The VO that present embodiment prepares with the X-ray detection
2Film is determined VO
2Film is an amorphous vanadium oxides, only contains VO
2(B) and VO
2(M) two kinds of allotropy structures, wherein VO
2(B) be the growth of (011) high preferred orientation, VO
2(M) be non-oriented growth mode.
Embodiment two: the difference of present embodiment and embodiment one is: with p-Si (100) as the Si substrate.Other is identical with execution mode one.
Be substrate with p-Si (100) in the present embodiment, p-Si (100) substrate resistivity is 8～12 Ω cm.
Embodiment three: the difference of present embodiment and embodiment one is: step () is removed the oxide-film of Si substrate according to the following steps: the Si substrate is cleaned 4～6min with the acetone sonic oscillation earlier, remove remaining acetone with deionized water rinsing again, clean 4～6min with the ethanol sonic oscillation then, remove remaining ethanol with deionized water rinsing again, clean 2～3min with hydrofluoric acid solution afterwards; Wherein hydrofluoric acid solution is made up of the hydrofluoric acid of 1 times of volume and the deionized water of 8 times of volumes by volume.Other step is identical with execution mode one.
Embodiment four: the difference of present embodiment and embodiment one is: vacuumize for the last time in the step (two), vacuum degree is 10 in the settling chamber
-6～10
-5Pa.Other step is identical with execution mode one.
Embodiment five: the difference of present embodiment and embodiment one is: repeatable operation is 5～9 times in the step (two).Other step is identical with execution mode one.
Embodiment six: the difference of present embodiment and embodiment one is: repeatable operation is 6～8 times in the step (two).Other step is identical with execution mode one.
Embodiment seven: the difference of present embodiment and embodiment one is: O in the step (four)
2The total gas flow rate of gas and Ar gas is 25sccm.Other step is identical with execution mode one.
Embodiment eight: the difference of present embodiment and embodiment one is: chamber pressure is controlled to be 0.33Pa in the step (four).Other step is identical with execution mode one.
Embodiment nine: the difference of present embodiment and embodiment one is: the distance in the step (four) between simple substance V target and Si substrate is 60mm.Other step is identical with execution mode one.
Embodiment ten: the difference of present embodiment and embodiment one is: step (five) sputter growth has VO
2The Si substrate of film is used alcohol and deionized water mixed solution clean surface before enclosing quartz ampoule, and wherein the volume ratio of alcohol and deionized water is 1～2: 1.Other step is identical with execution mode one.
Present embodiment can effectively be removed VO
2The impurity of film surface or oxide-film are especially removed owing to be exposed to the oxide-film that forms in the air for a long time.
Embodiment 11: the difference of present embodiment and embodiment one is: annealing temperature is 450 ℃ in the step (five), and annealing time is 14h.Other step is identical with execution mode one.
Embodiment 12: the difference of present embodiment and embodiment one is: annealing temperature is 500 ℃ in the step (five), and annealing time is 9h.Other step is identical with execution mode one.
Embodiment 13: present embodiment Si basal growth mixing allotropy structure of VO
2The technology of film is carried out according to the following steps: (one) cleans the Si substrate and removes oxide-film; (2) Si substrate and simple substance V target are placed the settling chamber, in the settling chamber, feed Ar gas and vacuumize again, and repeatable operation 4～10 times, the Si base reservoir temperature remains 400 ℃; (3) feed Ar gas and open rf magnetron sputtering coating system power supply once more; (4) treat that the Ar pneumoelectric strengthens radio-frequency power voltage gradually to 300V after producing plasma, feed O immediately
2Gas, O
2The total gas flow rate of gas and Ar gas is 25sccm, and chamber pressure is controlled to be 0.33Pa, and it is 400 ℃ that the Si substrate keeps temperature, and the distance between simple substance V target and Si substrate is 60mm, and the Si substrate bias is 0V, Si primary surface VO
2Film stops radio frequency sputtering after reaching setting thickness, is cooled to 200 ℃ with the settling chamber, and then stops O
2The feeding of gas and Ar gas; (5) the sputter growth there is VO
2Quartz ampoule is enclosed in the Si substrate of film, vacuumizes, and vacuum degree reduces to 10 in the quartz ampoule
-3～10
-2Pa vacuumizes quartz ampoule and puts into resistance furnace annealing, and annealing temperature is 500 ℃, and annealing time is 8h, and the vitreosil pipe is cooled to room temperature with resistance furnace then, the Si base VO that promptly obtains growing and mix the allotropy structure
2Film; O in its step (four)
2Throughput accounts for 7.8% of total gas flow rate.
Set Si primary surface VO in the present embodiment
2Film thickness is 2.8 μ m.The mixing allotropy structure of VO that the present invention grows on the Si base
2The film surface r.m.s. roughness is 14.92nm, and room temperature (25 ℃) TCR is-2.98%/K that room temperature resistivity is 6.29 Ω cm.
Embodiment 14: present embodiment Si basal growth mixing allotropy structure of VO
2The technology of film is carried out according to the following steps: (one) cleans the Si substrate and removes oxide-film; (2) Si substrate and simple substance V target are placed the settling chamber, in the settling chamber, feed Ar gas and vacuumize again, and repeatable operation 4～10 times, the Si base reservoir temperature remains 400 ℃; (3) feed Ar gas and open rf magnetron sputtering coating system power supply once more; (4) treat that the Ar pneumoelectric strengthens radio-frequency power voltage gradually to 300V after producing plasma, feed O immediately
2Gas, O
2The total gas flow rate of gas and Ar gas is 25sccm, and chamber pressure is controlled to be 0.33Pa, and it is 400 ℃ that the Si substrate keeps temperature, and the distance between simple substance V target and Si substrate is 60mm, and the Si substrate bias is 0V, Si primary surface VO
2Film stops radio frequency sputtering after reaching setting thickness, is cooled to 200 ℃ with the settling chamber, and then stops O
2The feeding of gas and Ar gas; (5) the sputter growth there is VO
2Quartz ampoule is enclosed in the Si substrate of film, vacuumizes, and vacuum degree reduces to 10 in the quartz ampoule
-3～10
-2Pa vacuumizes quartz ampoule and puts into resistance furnace annealing, and annealing temperature is 450 ℃, and annealing time is 10h, and the vitreosil pipe is cooled to room temperature with resistance furnace then, the Si base VO that promptly obtains growing and mix the allotropy structure
2Film; O in its step (four)
2Throughput accounts for 7.8% of total gas flow rate.
Set Si primary surface VO in the present embodiment
2Film thickness is 3.0 μ m.The mixing allotropy structure of VO that the present invention grows on the Si base
2The film surface r.m.s. roughness is 6.22nm, and room temperature (25 ℃) TCR is-5.65%/K that room temperature resistivity is 1.42 Ω cm.
Embodiment 15: present embodiment Si basal growth mixing allotropy structure of VO
2The technology of film is carried out according to the following steps: (one) cleans the Si substrate and removes oxide-film; (2) Si substrate and simple substance V target are placed the settling chamber, in the settling chamber, feed Ar gas and vacuumize again, and repeatable operation 4～10 times, the Si base reservoir temperature remains 400 ℃; (3) feed Ar gas and open rf magnetron sputtering coating system power supply once more; (4) treat that the Ar pneumoelectric strengthens radio-frequency power voltage gradually to 300V after producing plasma, feed O immediately
2Gas, O
2The total gas flow rate of gas and Ar gas is 25sccm, and chamber pressure is controlled to be 0.33Pa, and it is 400 ℃ that the Si substrate keeps temperature, and the distance between simple substance V target and Si substrate is 60mm, and the Si substrate bias is 0V, Si primary surface VO
2Film stops radio frequency sputtering after reaching setting thickness, is cooled to 200 ℃ with the settling chamber, and then stops O
2The feeding of gas and Ar gas; (5) the sputter growth there is VO
2Quartz ampoule is enclosed in the Si substrate of film, vacuumizes, and vacuum degree reduces to 10 in the quartz ampoule
-3～10
-2Pa vacuumizes quartz ampoule and puts into resistance furnace annealing, and annealing temperature is 450 ℃, and annealing time is 15h, and the vitreosil pipe is cooled to room temperature with resistance furnace then, the Si base VO that promptly obtains growing and mix the allotropy structure
2Film; O in its step (four)
2Throughput accounts for 7.8% of total gas flow rate.
Set Si primary surface VO in the present embodiment
2Film thickness is 2.8 μ m.The mixing allotropy structure of VO that the present invention grows on the Si base
2The film surface r.m.s. roughness is 9.341nm, and room temperature (25 ℃) TCR is-4.62%/K that room temperature resistivity is 0.06 Ω cm.
Claims (9)
1. Si basal growth mixing allotropy structure of VO
2The technology of film is characterized in that Si basal growth mixing allotropy structure of VO
2The technology of film is carried out according to the following steps: one, clean the Si substrate and remove oxide-film; Two, Si substrate and simple substance V target are placed the settling chamber, in the settling chamber, feed Ar gas and vacuumize again, and repeatable operation 4～10 times, the Si base reservoir temperature remains 400 ℃; Three, feed Ar gas and open rf magnetron sputtering coating system power supply once more; Four, treat that the Ar pneumoelectric strengthens radio-frequency power voltage gradually to 300V after producing plasma, feed O immediately
2Gas, O
2The total gas flow rate of gas and Ar gas is 23～27sccm, and chamber pressure is controlled to be 0.30～0.35Pa, and it is 400 ℃ that the Si substrate keeps temperature, and the distance between simple substance V target and Si substrate is 58～62mm, and the Si substrate bias is 0V, Si primary surface VO
2Film stops radio frequency sputtering after reaching setting thickness, is cooled to 200 ℃ with the settling chamber, and then stops O
2The feeding of gas and Ar gas; Five, the sputter growth there is VO
2Quartz ampoule is enclosed in the Si substrate of film, vacuumizes, and vacuum degree reduces to 10 in the quartz ampoule
-3～10
-2Pa vacuumizes quartz ampoule and puts into resistance furnace annealing, and annealing temperature is 450 ℃～500 ℃, and annealing time is 8～15h, and the vitreosil pipe is cooled to room temperature with resistance furnace then, the Si base VO that promptly obtains growing and mix the allotropy structure
2Film; O in its step 4
2Throughput accounts for 7.8% of total gas flow rate.
2. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film, it is characterized in that step 1 removes the oxide-film of Si substrate according to the following steps: the Si substrate is cleaned 4～6min with the acetone sonic oscillation earlier, remove remaining acetone with deionized water rinsing again, clean 4～6min with the ethanol sonic oscillation then, remove remaining ethanol with deionized water rinsing again, clean 2～3min with hydrofluoric acid solution afterwards; Wherein hydrofluoric acid solution is made up of the hydrofluoric acid of 1 times of volume and the deionized water of 8 times of volumes by volume.
3. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that vacuumizing for the last time in the step 2, and vacuum degree is 10 in the settling chamber
-6～10
-5Pa.
4. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that O in the step 4
2The total gas flow rate of gas and Ar gas is 25sccm.
5. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that chamber pressure is controlled to be 0.33Pa in the step 4.
6. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that the distance between simple substance V target and Si substrate is 60mm in the step 4.
7. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that step 5 sputter growth has VO
2The Si substrate of film is used alcohol and deionized water mixed solution clean surface before enclosing quartz ampoule, and wherein the volume ratio of alcohol and deionized water is 1～2: 1.
8. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that annealing temperature is 450 ℃ in the step 5, and annealing time is 14h.
9. Si basal growth mixing allotropy structure of VO according to claim 1
2The technology of film is characterized in that annealing temperature is 500 ℃ in the step 5, and annealing time is 9h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101510721A CN100424820C (en) | 2006-11-27 | 2006-11-27 | A technique to generate mixed allotropic structure of VO2 film on Si base |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101510721A CN100424820C (en) | 2006-11-27 | 2006-11-27 | A technique to generate mixed allotropic structure of VO2 film on Si base |
Publications (2)
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|---|---|
| CN1963997A CN1963997A (en) | 2007-05-16 |
| CN100424820C true CN100424820C (en) | 2008-10-08 |
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| CNB2006101510721A Expired - Fee Related CN100424820C (en) | 2006-11-27 | 2006-11-27 | A technique to generate mixed allotropic structure of VO2 film on Si base |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140101610A (en) * | 2013-02-12 | 2014-08-20 | 삼성디스플레이 주식회사 | Deposition apparatus and manufacturing method of organic light emitting display using the same |
| CN103556201B (en) * | 2013-10-25 | 2016-09-07 | 上海师范大学 | A kind of Flaky vanadium dioxide film material and preparation method thereof |
| CN103572209B (en) * | 2013-11-05 | 2015-10-21 | 无锡英普林纳米科技有限公司 | A kind of preparation method of metastable-state vanadium dioxide thin film |
| CN115125488B (en) * | 2022-07-08 | 2023-11-03 | 成都市精鹰光电技术有限责任公司 | Thermosensitive film prepared based on mixed pulse reaction magnetron sputtering |
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| JP2003002791A (en) * | 2001-06-15 | 2003-01-08 | Zenji Hiroi | Member controlled in transition temperature |
| CN1529451A (en) * | 2003-10-05 | 2004-09-15 | 华中科技大学 | Miniature vanadium dioxide photoswitch and preparing method thereof |
| CN1598040A (en) * | 2004-08-25 | 2005-03-23 | 华中科技大学 | Process for preparing vanadium oxide film capable of regulating phase change temp. |
| CN1195097C (en) * | 2002-07-13 | 2005-03-30 | 华中科技大学 | Process for prapring vanadium oxide film |
| US6933553B2 (en) * | 2003-06-03 | 2005-08-23 | Electronics And Telecommunications Research Institute | Field effect transistor using vanadium dioxide layer as channel material and method of manufacturing the field effect transistor |
| CN1752270A (en) * | 2005-07-12 | 2006-03-29 | 天津大学 | Opposite target reaction magnetocontrol sputtering method for preparing vanadium oxide film |
-
2006
- 2006-11-27 CN CNB2006101510721A patent/CN100424820C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003002791A (en) * | 2001-06-15 | 2003-01-08 | Zenji Hiroi | Member controlled in transition temperature |
| CN1195097C (en) * | 2002-07-13 | 2005-03-30 | 华中科技大学 | Process for prapring vanadium oxide film |
| US6933553B2 (en) * | 2003-06-03 | 2005-08-23 | Electronics And Telecommunications Research Institute | Field effect transistor using vanadium dioxide layer as channel material and method of manufacturing the field effect transistor |
| CN1529451A (en) * | 2003-10-05 | 2004-09-15 | 华中科技大学 | Miniature vanadium dioxide photoswitch and preparing method thereof |
| CN1598040A (en) * | 2004-08-25 | 2005-03-23 | 华中科技大学 | Process for preparing vanadium oxide film capable of regulating phase change temp. |
| CN1752270A (en) * | 2005-07-12 | 2006-03-29 | 天津大学 | Opposite target reaction magnetocontrol sputtering method for preparing vanadium oxide film |
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