CN110643980A - Preparation method of micrometer-thickness vanadium dioxide thin film fine pattern - Google Patents
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- CN110643980A CN110643980A CN201910904963.7A CN201910904963A CN110643980A CN 110643980 A CN110643980 A CN 110643980A CN 201910904963 A CN201910904963 A CN 201910904963A CN 110643980 A CN110643980 A CN 110643980A
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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Abstract
The invention belongs to the technical field of microelectronics and materials, and particularly relates to a preparation method of a micrometer-thickness vanadium dioxide film micro-fine pattern. The invention provides a preparation method of a micrometer-thickness vanadium dioxide film micro-pattern, which is simple in process and low in cost. The method comprises the following steps: a. sol preparation: preparing vanadyl acetylacetonate, polyvinylpyrrolidone and anhydrous methanol to obtain vanadium dioxide precursor sol, stirring at room temperature, and standing to obtain photosensitive vanadium dioxide precursor sol; b. preparing a gel film: coating the photosensitive vanadium dioxide precursor sol on a substrate to obtain a vanadium-containing gel film; c. micro-processing of the gel film: baking the vanadium-containing gel film, covering a mask plate, exposing under an ultraviolet lamp, and immersing into a mixed solution of anhydrous methanol and n-butyl alcohol for solution washing to obtain a vanadium-containing gel film micro-fine pattern; d. and carrying out heat treatment on the vanadium-containing gel film micro-fine pattern to obtain a micrometer-thickness vanadium dioxide film micro-fine pattern. The method has potential application prospect.
Description
Technical Field
The invention belongs to the technical field of microelectronics and materials, and particularly relates to a preparation method of a micrometer-thickness vanadium dioxide film micro-fine pattern.
Background
Vanadium dioxide is regarded as a revolutionary material for future electronic industry, and one key characteristic of vanadium dioxide is that the vanadium dioxide is an insulator at room temperature, and the atomic structure of the vanadium dioxide is changed into a metal structure (conductor) from a room-temperature crystal structure after the temperature is higher than 68 ℃. This unique characteristic, known as metal-insulator transition (MIT), makes it an ideal choice for replacing silicon materials for a new generation of low power consumption electronic devices.
At present, the photoelectric device of vanadium dioxide material is mainly applied in thin film state, and has been successfully applied in various fields such as electrochromic device, optical switch, micro battery, energy-saving coating, intelligent window and micrometering radiant heat device.
Thin film micro-patterning is one of the key technologies for the fabrication of various micro or integrated functional devices. The current methods for processing the micro-patterns of the film mainly comprise a high-energy beam etching method, a wet etching method, a nano-imprinting method and the like. However, these methods usually involve expensive equipment such as vacuum or ion beam, and the process is complicated and costly. In particular, the fine processing steps of the methods are carried out after the preparation of the thin film is finished, so that the structure, the appearance and the like of the thin film are greatly influenced, and the performance of a device is further influenced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a micron-thickness vanadium dioxide film micro-pattern, which has the advantages of simple process, low cost and complete structure and can realize clear outline of the vanadium dioxide film micro-pattern.
The technical scheme adopted by the invention for solving the technical problems is to provide a preparation method of a micrometer-thickness vanadium dioxide film micro-fine pattern. The method comprises the following steps:
a. sol preparation: preparing vanadyl acetylacetonate, polyvinylpyrrolidone and anhydrous methanol to obtain vanadium dioxide precursor sol, stirring at room temperature, and standing to obtain photosensitive vanadium dioxide precursor sol;
b. preparing a gel film: coating the photosensitive vanadium dioxide precursor sol on a substrate to obtain a vanadium-containing gel film;
c. micro-processing of the gel film: baking the vanadium-containing gel film, covering a mask plate, exposing under an ultraviolet lamp, and immersing into a mixed solution of anhydrous methanol and n-butyl alcohol for solution washing to obtain a vanadium-containing gel film micro-fine pattern;
d. and carrying out heat treatment on the vanadium-containing gel film micro-fine pattern to obtain a micrometer-thickness vanadium dioxide film micro-fine pattern.
In the preparation method of the micron-thickness vanadium dioxide film fine pattern, in the step a, the dosage of vanadyl acetylacetonate and polyvinylpyrrolidone is such that the molar ratio of vanadium ions in the vanadium dioxide precursor sol to polyvinylpyrrolidone is 2: 1-10: 1.
Preferably, the molar ratio of vanadium ions to polyvinylpyrrolidone in the vanadium dioxide precursor sol is 3: 1.
Further, in the step a, the addition amount of the anhydrous methanol enables the concentration of the vanadium dioxide precursor sol to be 0.1-0.5 mol/L.
Further, in the step a, the stirring time is 6-10 h. The standing time is 36-72 h.
Preferably, the stirring time is 8 h. The standing time is 60 h.
In the step b, the photosensitive vanadium dioxide precursor sol is coated on the substrate, and a vanadium-containing gel film is obtained on a silicon substrate or a glass substrate by a dip-coating method or a spin-coating method.
Further, the pulling speed of the dipping pulling method is 1-3 mm/s. The spin coating method has a rotating speed of 2000-4000 rpm and a time of 10-30 s.
In the preparation method of the micron-thickness vanadium dioxide film fine pattern, in the step c, the baking condition is that the film is baked for 10-30 min at 90-150 ℃.
Preferably, the baking condition is baking at 100 ℃ for 20 min.
Further, in the step c, the wavelength of the ultraviolet lamp is 240-400 nm. The exposure time is 60-120 min.
Preferably, the exposure time is 90 min.
Further, in the step c, the volume ratio of the anhydrous methanol to the n-butanol in the mixed solution of the anhydrous methanol and the n-butanol is 1: 1-5: 1. The time of the solution washing is 10-30 s.
Preferably, the time of the elution is 15 s.
In the preparation method of the micron-thickness vanadium dioxide film fine pattern, in the step d, the heat treatment is to keep the temperature of the vanadium-containing gel film fine pattern at 550-750 ℃ for 60-150 min under the protection of nitrogen.
Preferably, the heat treatment is to preserve the vanadium-containing gel film fine pattern at 700 ℃ for 100min under the protection of nitrogen.
Further, in the step d, the temperature rise rate in the heat treatment process is 5-15 ℃/min.
Preferably, the rate of temperature rise during the heat treatment is 10 ℃/min.
The invention also provides a micro-pattern of the micron-thickness vanadium dioxide thin film prepared by the method.
The invention has the beneficial effects that:
according to the invention, vanadyl acetylacetonate is used as a raw material, PVP is added to prepare the vanadium dioxide precursor sol with excellent ultraviolet sensitization characteristics, the sol is stable, the viscosity is controllable, the film forming property is good, and the vanadium dioxide film with the thickness of 1-5 μm can be prepared at one time. The invention adopts the ultraviolet mask technology to carry out micro-processing on the gel film, and the obtained micro-pattern has clear outline and regular structure, and the line width can reach micron level. The method realizes the micro-processing before the vanadium dioxide film is formed, and avoids the deterioration of the structure and the performance of the film. The pure-phase vanadium dioxide material prepared by the method does not influence the phase and surface appearance of the film after micro-patterning, has good phase change characteristics and can effectively play a role in breaking a circuit. The method of the invention does not need expensive equipment and photoresist assistance, has simple process and low cost and has potential engineering application prospect.
Drawings
FIG. 1 is a flow chart of the method for preparing a vanadium dioxide film micro-pattern.
FIG. 2 shows a fine pattern of a vanadium dioxide thin film prepared by the method of the present invention.
FIG. 3 is a R-T curve diagram of a 50 μm line width vanadium dioxide thin line prepared in example 1 of the present invention.
Detailed Description
Specifically, the invention provides a preparation method of a micrometer-thickness vanadium dioxide film fine pattern. The method comprises the following steps:
a. sol preparation: taking vanadyl acetylacetonate as a raw material, polyvinylpyrrolidone (PVP, molecular weight 8000) as an additive and anhydrous methanol as a solvent to prepare vanadium dioxide precursor sol, enabling the molar ratio of vanadium ions in the vanadium dioxide precursor sol to the polyvinylpyrrolidone to be 2: 1-10: 1, adjusting the addition of the anhydrous methanol to enable the concentration of the vanadium dioxide precursor sol to be 0.1-0.5 mol/L, stirring at room temperature for 6-10 h, and standing for 36-72 h to obtain photosensitive vanadium dioxide precursor sol;
b. preparing a gel film: obtaining a vanadium-containing gel film on a silicon substrate by dipping and pulling method or spin coating method of the photosensitive vanadium dioxide precursor sol; the pulling speed of the dipping pulling method is 1-3 mm/s; the spin coating method has a rotation speed of 2000-4000 rpm for 10-30 s.
c. Micro-processing of the gel film: drying the vanadium-containing gel film at 90-150 ℃ for 10-30 min, covering the mask plate, exposing the mask plate for 60-120 min under an ultraviolet lamp with the wavelength of 240-400 nm, and immersing the mask plate into a mixed solution of anhydrous methanol and n-butyl alcohol in a volume ratio of 1: 1-5: 1 for washing for 10-30 s to obtain a vanadium-containing gel film fine pattern;
d. and (3) carrying out heat treatment on the vanadium-containing gel film fine pattern, raising the temperature from room temperature to 550-750 ℃ at the speed of 5-15 ℃/min in the heat treatment process, and preserving the heat for 60-150 min under the protection of nitrogen, so as to obtain the micron-thickness vanadium dioxide film fine pattern.
In the step a, after vanadyl acetylacetonate is dissolved, carbonyl provides electrons in the standing process to enable oxygen ions and vanadium ions to react to generate a cyclic chelate, and the cyclic chelate has an ultraviolet photosensitive characteristic. The invention adopts PVP as an additive to prepare the vanadium dioxide precursor sol, can obviously improve the viscosity of the sol, promotes the formation of V-O chelate rings to a certain extent, can improve the photosensitivity of the sol, and can realize the preparation of the vanadium dioxide film with the micron thickness by one-time film preparation.
The vanadium dioxide precursor sol is endowed with the ultraviolet photosensitive characteristic by a method of combining sol-gel and chemical modification, and the vanadium dioxide precursor sol can be directly processed by photoetching by utilizing the characteristic. According to the method, the vanadium dioxide film micro-pattern can be obtained without the assistance of photoresist and expensive equipment, so that the cost is greatly saved.
The concentration of the vanadium dioxide precursor sol in the step a of the invention refers to the ratio of the mole number of vanadium in the sol to the total volume of the sol.
In step c, the vanadium-containing gel film is further reacted under the irradiation of ultraviolet light to generate an-O-V-O-network structure which is insoluble in an organic solvent, and a fine pattern can be obtained through organic solution washing. And c, performing micro-processing on the vanadium-containing gel film by adopting an ultraviolet mask technology, so that the obtained vanadium-containing gel film has clear figure and complete structure, and the line width can reach micron level.
The mask plate in the step c can be selected into a specific shape according to the requirement.
In the step d of the invention, the vanadium-containing gel film micro-fine pattern is subjected to heat treatment to decompose organic matters in the gel film, so that a micron-thickness vanadium dioxide film micro-fine pattern is obtained.
The invention also provides a micro-pattern of the micron-thickness vanadium dioxide thin film prepared by the method.
The present invention will be further illustrated by the following specific examples.
Example 1
Adding vanadyl acetylacetonate powder and polyvinylpyrrolidone (PVP, molecular weight 8000) into anhydrous methanol to prepare vanadium dioxide precursor sol, wherein the molar ratio of vanadium ions to PVP in the sol is 3:1, and the sol concentration is 0.1 mol/L. Stirring for 8h at room temperature, and standing for 60h to obtain the photosensitive vanadium dioxide precursor sol. Taking a single crystal silicon substrate as a substrate, and obtaining the vanadium-containing gel film by adopting a dip-coating method, wherein the coating speed is 2 mm/s. Baking the vanadium-containing gel film at 100 ℃ for 20min, covering the vanadium-containing gel film with a mask plate with a specific shape, exposing the vanadium-containing gel film for 90min under an ultraviolet lamp, and then soaking the vanadium-containing gel film into a mixed solution of anhydrous methanol and n-butyl alcohol (the volume ratio of the anhydrous methanol to the n-butyl alcohol is 3:1) for washing for 15s to obtain the vanadium-containing gel film micro-fine pattern. And (3) carrying out heat treatment on the vanadium-containing gel film micro-fine pattern at 700 ℃ for 100min under the protection of nitrogen, so that organic matters in the gel film are decomposed, and a crystalline vanadium dioxide film micro-fine pattern with the micron thickness of 2 microns is obtained. The obtained vanadium dioxide film micro-pattern sample is a single vanadium dioxide phase, the micro-pattern has clear outline and regular structure, and the minimum line width is about 10 mu m. The phase transition temperature of vanadium dioxide is about 70 ℃, and the resistance change amplitude before and after phase transition is about two orders of magnitude.
Example 2
Adding vanadyl acetylacetonate powder and polyvinylpyrrolidone (PVP, molecular weight 8000) into anhydrous methanol to prepare vanadium dioxide precursor sol, wherein the molar ratio of vanadium ions to PVP in the sol is 2:1, and the sol concentration is 0.1 mol/L. Stirring for 6h at room temperature, and standing for 72h to obtain the photosensitive vanadium dioxide precursor sol. Taking a single crystal silicon substrate as a substrate, and obtaining the vanadium-containing gel film by adopting a dip-coating method, wherein the coating speed is 1 mm/s. Baking the vanadium-containing gel film at 90 ℃ for 30min, covering the vanadium-containing gel film with a mask plate with a specific shape, exposing the vanadium-containing gel film for 100min under an ultraviolet lamp, and then soaking the vanadium-containing gel film into a mixed solution of anhydrous methanol and n-butyl alcohol (the volume ratio of the anhydrous methanol to the n-butyl alcohol is 5:1) for washing for 20s to obtain the vanadium-containing gel film micro-fine pattern. And (3) carrying out heat treatment on the vanadium-containing gel film micro-fine pattern at 750 ℃ for 120min under the protection of nitrogen, so as to decompose organic matters in the gel film and obtain a crystalline vanadium dioxide film micro-fine pattern with the micron thickness of 3 microns. The obtained vanadium dioxide film micro-pattern sample is a single vanadium dioxide phase, the micro-pattern has clear outline and regular structure, and the minimum line width is about 15 mu m. The phase transition temperature of vanadium dioxide is about 72 ℃, and the resistance change amplitude before and after phase transition is about two orders of magnitude.
Example 3
Adding vanadyl acetylacetonate powder and polyvinylpyrrolidone (PVP, molecular weight 8000) into anhydrous methanol to prepare vanadium dioxide precursor sol, wherein the molar ratio of vanadium ions to PVP in the sol is 5:1, and the sol concentration is 0.2 mol/L. Stirring at room temperature for 10h, and aging for 36h to obtain the photosensitive vanadium dioxide precursor sol. Taking a single crystal silicon substrate as a substrate, and obtaining the vanadium-containing gel film by adopting a dip-coating method, wherein the coating speed is 2 mm/s. Baking the vanadium-containing gel film at 150 ℃ for 10min, covering the vanadium-containing gel film with a mask plate with a specific shape, exposing the vanadium-containing gel film for 120min under an ultraviolet lamp, and then soaking the vanadium-containing gel film into a mixed solution of anhydrous methanol and n-butyl alcohol (the volume ratio of the anhydrous methanol to the n-butyl alcohol is 2:1) for washing for 30s to obtain the vanadium-containing gel film micro-fine pattern. And (3) carrying out heat treatment on the vanadium-containing gel film micro-fine pattern at 650 ℃ under the protection of nitrogen for 150min to decompose organic matters in the gel film, so as to obtain a crystalline vanadium dioxide film micro-fine pattern with the micron thickness of 1 micron. The obtained vanadium dioxide film micro-pattern sample is a single vanadium dioxide phase, the micro-pattern has clear outline and regular structure, and the minimum line width is about 20 mu m. The phase transition temperature of vanadium dioxide is about 71 ℃, and the resistance change amplitude before and after phase transition is about two orders of magnitude.
As can be seen from the graphs in FIGS. 2 and 3, the vanadium dioxide thin film prepared by the method of the present invention has clear fine pattern profile, regular structure and good phase transition characteristics. From the examples 1 to 3, the method can be used for preparing the vanadium dioxide film with the micron thickness at one time, the prepared fine pattern has clear outline and regular structure, and the line width can reach the micron level.
Claims (10)
1. The preparation method of the micron-thickness vanadium dioxide film fine pattern is characterized by comprising the following steps of:
a. sol preparation: preparing vanadyl acetylacetonate, polyvinylpyrrolidone and anhydrous methanol to obtain vanadium dioxide precursor sol, stirring at room temperature, and standing to obtain photosensitive vanadium dioxide precursor sol;
b. preparing a gel film: coating the photosensitive vanadium dioxide precursor sol on a substrate to obtain a vanadium-containing gel film;
c. micro-processing of the gel film: baking the vanadium-containing gel film, covering a mask plate, exposing under an ultraviolet lamp, and immersing into a mixed solution of anhydrous methanol and n-butyl alcohol for solution washing to obtain a vanadium-containing gel film micro-fine pattern;
d. and carrying out heat treatment on the vanadium-containing gel film micro-fine pattern to obtain a micrometer-thickness vanadium dioxide film micro-fine pattern.
2. The method for preparing the fine pattern of the micrometer-thickness vanadium dioxide thin film according to claim 1, characterized in that: in the step a, the dosage of the vanadyl acetylacetonate and the polyvinylpyrrolidone is such that the molar ratio of the vanadium ions in the vanadium dioxide precursor sol to the polyvinylpyrrolidone is 2: 1-10: 1.
3. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to claim 1 or 2, characterized in that: in the step a, the addition amount of the anhydrous methanol enables the concentration of the vanadium dioxide precursor sol to be 0.1-0.5 mol/L.
4. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to any one of claims 1 to 3, characterized in that: in the step a, the stirring time is 6-10 h; the standing time is 36-72 h.
5. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to any one of claims 1 to 4, characterized in that: in the step b, the photosensitive vanadium dioxide precursor sol is coated on the substrate, and a vanadium-containing gel film is obtained on a silicon substrate or a glass substrate by a dip-coating method or a spin-coating method; the pulling speed of the dipping pulling method is 1-3 mm/s; the spin coating method has a rotating speed of 2000-4000 rpm and a time of 10-30 s.
6. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to any one of claims 1 to 5, wherein the method comprises the following steps: in the step c, the wavelength of the ultraviolet lamp is 240-400 nm; the exposure time is 60-120 min.
7. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to any one of claims 1 to 6, characterized in that: in the step c, in the mixed solution of the anhydrous methanol and the n-butyl alcohol, the volume ratio of the anhydrous methanol to the n-butyl alcohol is 1: 1-5: 1; the time of the solution washing is 10-30 s.
8. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to any one of claims 1 to 7, characterized in that: in the step d, the heat treatment is to keep the vanadium-containing gel film micro-fine pattern at 550-750 ℃ for 60-150 min under the protection of nitrogen.
9. The method for preparing the micro-pattern of the micrometer-thickness vanadium dioxide thin film according to any one of claims 1 to 8, wherein the method comprises the following steps: in the step d, the temperature rising rate in the heat treatment process is 5-15 ℃/min.
10. The method for preparing the vanadium dioxide film with the micron thickness comprises the following steps of 1 to 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436606A (en) * | 2003-03-04 | 2003-08-20 | 中国科学院上海技术物理研究所 | Prepn process of vanadium oxide film material |
| CN1457504A (en) * | 2000-06-06 | 2003-11-19 | Ekc技术公司 | Method of making electronic materials |
| US20120040192A1 (en) * | 2008-10-20 | 2012-02-16 | The University Of Western Ontario | Method for inhibiting the oxidation of vo(acac)2 in solution |
| CN106048570A (en) * | 2016-07-26 | 2016-10-26 | 西安理工大学 | Preparation methods for ultraviolet light-sensitive lithium niobate sol and film fine-pattern thereof |
| CN108149228A (en) * | 2017-12-20 | 2018-06-12 | 西安理工大学 | A kind of CoFe2O4The preparation method and CoFe of photosensitive colloidal sol2O4The preparation method of Micropicture film |
-
2019
- 2019-09-24 CN CN201910904963.7A patent/CN110643980A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1457504A (en) * | 2000-06-06 | 2003-11-19 | Ekc技术公司 | Method of making electronic materials |
| CN1436606A (en) * | 2003-03-04 | 2003-08-20 | 中国科学院上海技术物理研究所 | Prepn process of vanadium oxide film material |
| US20120040192A1 (en) * | 2008-10-20 | 2012-02-16 | The University Of Western Ontario | Method for inhibiting the oxidation of vo(acac)2 in solution |
| CN106048570A (en) * | 2016-07-26 | 2016-10-26 | 西安理工大学 | Preparation methods for ultraviolet light-sensitive lithium niobate sol and film fine-pattern thereof |
| CN108149228A (en) * | 2017-12-20 | 2018-06-12 | 西安理工大学 | A kind of CoFe2O4The preparation method and CoFe of photosensitive colloidal sol2O4The preparation method of Micropicture film |
Non-Patent Citations (1)
| Title |
|---|
| 王超: "增强红外调节性能的聚硅氧院／二氧化钒复合薄膜的制备及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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