CN111085411B - High-insulation-resistance silicon dioxide thin film material and preparation method thereof - Google Patents
High-insulation-resistance silicon dioxide thin film material and preparation method thereof Download PDFInfo
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- CN111085411B CN111085411B CN202010012476.2A CN202010012476A CN111085411B CN 111085411 B CN111085411 B CN 111085411B CN 202010012476 A CN202010012476 A CN 202010012476A CN 111085411 B CN111085411 B CN 111085411B
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0486—Operating the coating or treatment in a controlled atmosphere
Abstract
The invention relates to a high-insulation-resistance silicon dioxide thin film material and a preparation method thereof, belonging to the technical field of surface processing, coatings and thin film materials. The preparation method comprises the following steps: the silicon dioxide film material with high insulation resistance is obtained by utilizing an atmospheric pressure discharge method, the atmospheric pressure discharge temperature is room temperature, in the growth process of the silicon dioxide film, a nozzle of an atmospheric pressure discharge device is always vertical to the surface of the substrate, the nozzle keeps a constant distance with the surface of the substrate, and the nozzle does periodic reciprocating motion relative to the surface of the substrate. Compared with the existing silicon dioxide film material, the silicon dioxide film material with high insulation resistance has high insulation resistance.
Description
Technical Field
The invention relates to a high-insulation-resistance silicon dioxide thin film material and a preparation method thereof, belonging to the technical field of surface processing, coatings and thin film materials.
Background
Silicon Dioxide (SiO)2) Thin film materials are an important high insulation resistance material, and have important applications in the fields of thin film sensors, integrated circuits and the like, for example: an insulating layer between the metal substrate and the thin film thermocouple temperature sensor, an insulating layer between the metal substrate and the thin film strain gauge, and the like.
At present, the silicon dioxide film is prepared by a thermal oxidation technology, but the thermal oxidation technology needs to heat the substrate to more than 1000 ℃ when preparing the silicon dioxide film, and the substrate can only be monocrystalline silicon, so that the preparation of the high-insulation silicon dioxide film on the metal substrate by the thermal oxidation technology is limited. The chemical vapor deposition technology is also a common method for preparing the silicon dioxide film, however, the silicon dioxide film prepared by the chemical vapor deposition technology contains a large amount of chemical bonds Si-H, the insulating property of the silicon dioxide film is reduced, and the substrate temperature is also above 200 ℃, which also limits the preparation of the high-insulating silicon dioxide film on the metal substrate by the chemical vapor deposition technology. However, when the magnetron sputtering technique is used for preparing the silicon dioxide film, the substrate is required to be of a planar structure, and the silicon dioxide film cannot be uniformly prepared on a complex curved surface, which also limits the magnetron sputtering technique to prepare the high-insulation silicon dioxide film on the surface of the metal substrate with the complex curved surface structure. Silica films can also be prepared by other methods, for example: ion beam sputtering deposition, atomic layer deposition, chemical water bath synthesis, sol-gel, etc., however, all have some disadvantages, such as: a high-insulation silicon dioxide film cannot be prepared on the surface of a metal substrate with a complex curved surface structure; the prepared silicon dioxide film material has low compactness, poor insulativity and poor binding force between the film and the substrate; in the process of preparing the silicon dioxide film material, high-temperature heat treatment is needed, and the problems of long time consumption, low efficiency and the like exist.
Disclosure of Invention
The invention effectively improves the insulation resistance of the silicon dioxide film material prepared on the surface of the substrate with the complex curved surface structure by controlling the reciprocating periodic motion of the nozzle of the atmospheric pressure discharge device in the direction parallel to the surface of the substrate.
The invention provides a preparation method of a high-insulation resistance silicon dioxide thin film material, which comprises the following steps: obtaining a silicon dioxide film material with high insulation resistance by using an atmospheric pressure discharge method, wherein the atmospheric pressure discharge temperature is room temperature, a nozzle of an atmospheric pressure discharge device is always vertical to the surface of a substrate in the growth process of the silicon dioxide film, the nozzle keeps a constant distance with the surface of the substrate, and the nozzle performs periodic reciprocating motion relative to the surface of the substrate; the moving speed is more than 0.5cm/min, the periodic reciprocating times are more than 1, the deposition time is more than 1min, and the thickness of the silicon dioxide film material is more than 1 mu m.
The atmospheric pressure discharge power supply is a direct current power supply or an alternating current power supply, and the power supply power is preferably more than 20W, and more preferably 20-500W.
It is further preferred according to the invention that the movement speed is 0.5-60 cm/min.
It is further preferred in the present invention that the number of the periodic reciprocating movements is 1 to 50.
It is further preferred according to the present invention that the deposition time is 1-20 min.
It is further preferred that the thickness of the silica thin film material is 1 to 10 μm.
The invention preferably has the surface of the substrate as a plane or a curved surface.
The curved surface can be a complex curved surface with any shape.
In the invention, the substrate material is preferably a dense material.
In the invention, the material of the compact material is preferably metal, circuit board, ceramic or semiconductor.
The invention preferably selects argon as the working gas of the atmospheric discharge, and the purity of the argon is 99.99 percent; the silicon source of the silicon dioxide film is silicon tetrachloride, and the purity of the silicon tetrachloride is more than 98 percent; the auxiliary oxygen source of the silicon dioxide film is oxygen, and the purity of the oxygen is 99.99%.
Preferably, the argon flow is > 1 slm; the oxygen flow is more than 5 sccm; the carrier gas of the silicon tetrachloride is argon or oxygen, and the flow of the carrier gas is more than 10 sccm.
It is further preferred that the argon flow is 1 to 10 slm.
It is further preferred according to the present invention that the oxygen flow rate is 5 to 50 sccm.
It is further preferred in the present invention that the carrier gas flow rate is 10 to 50 sccm.
The invention also aims to provide the high-insulation-resistance silicon dioxide thin film material prepared by the method.
The invention preferably selects the insulation resistance of the silicon dioxide film material to be more than 108Ω/μm。
The invention has the beneficial effects that:
compared with the existing silicon dioxide film material, the silicon dioxide film material with high insulation resistance has high insulation resistance;
the preparation method does not need vacuum conditions, and can work in any environment and any atmospheric conditions;
the preparation method can prepare the high-insulation resistance silicon dioxide film material on the surface of the substrate with any curved surface structure, and is not limited to the surface of the substrate with a planar structure;
the preparation method provided by the invention is simple, low in cost, high in yield and convenient for large-scale industrial production.
Drawings
In the figure 2 of the attached drawings of the invention,
FIG. 1 is a schematic view of a nozzle of the present invention in periodic reciprocating motion on a substrate surface;
FIG. 2 is a graph showing insulation resistance values of the silica thin film materials according to examples 1 to 5 and comparative example 1;
wherein: 1. and the nozzle 2, the base body 3 and the nozzle do reciprocating motion tracks on the surface of the base body.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
A preparation method of a high insulation resistance silicon dioxide thin film material comprises the following steps: under the condition of room temperature, an atmospheric pressure discharge device is utilized, a metal matrix in any shape is taken as a substrate material, argon with the purity of 99.99 percent is taken as a discharge gas and a carrier gas, oxygen with the purity of 99.99 percent is taken as a reaction gas, silicon tetrachloride with the purity of 99.99 percent is taken as a reaction liquid, the atmospheric pressure discharge is carried out to prepare a silicon dioxide film, a nozzle of the atmospheric pressure discharge device keeps a constant distance with the surface of the matrix, the thickness of the obtained silicon dioxide film is 1.31 mu m, and the insulation resistance of the silicon dioxide film is 1.55 +/-0.53 multiplied by 108Omega, the insulation resistance of the silicon dioxide film material is 1.19 plus or minus 0.48 multiplied by 10 according to the linear relation calculation of the insulation resistance of the silicon dioxide film material and the thickness thereof8Ω/μm。
Wherein: the power of the direct current power supply is 100W; the argon flow was 1 slm; the oxygen flow rate is 5 sccm; the carrier gas of the silicon tetrachloride is oxygen, and the flow rate is 10 sccm; the deposition time was 20 min. The matrix is fixed, the nozzle of the atmospheric pressure discharge device is always vertical to the surface of the matrix and reciprocates on the surface of the matrix, the distance between the nozzle and the surface of the matrix is constant to be 3mm, the movement speed of the nozzle relative to the matrix is 0.5cm/min, and the reciprocating movement frequency of the nozzle relative to the matrix is 1 time.
Example 2
A preparation method of a high insulation resistance silicon dioxide thin film material comprises the following steps: the method comprises the steps of utilizing an atmospheric pressure discharge device to discharge at the room temperature by taking a metal matrix in any shape as a substrate material, argon with the purity of 99.99 percent as a discharge gas and a carrier gas, oxygen with the purity of 99.99 percent as a reaction gas and silicon tetrachloride with the purity of 99.99 percent as a reaction liquid, preparing a silicon dioxide film, and keeping a constant distance between a nozzle of the atmospheric pressure discharge device and the surface of the matrix to obtain the silicon dioxide filmThe obtained silicon dioxide film has a thickness of 4.86 μm and an insulation resistance of 1.25 + -0.14 × 109Omega, the insulation resistance of the silicon dioxide film material is 2.57 +/-0.17 multiplied by 10 according to the linear relation between the insulation resistance of the silicon dioxide film material and the thickness of the silicon dioxide film material8Ω/μm。
Wherein: the working frequency of the alternating current power supply is 10kHz, and the power is 50W; the argon flow was 3 slcm; the carrier gas of the silicon tetrachloride is argon, and the flow rate is 20 sccm; the oxygen flow rate is 15 sccm; the deposition time was 15 min. The nozzle of the atmospheric pressure discharge device is fixed, the surface of the base body is always vertical to the nozzle of the atmospheric pressure discharge device, the base body reciprocates, the distance between the nozzle and the surface of the base body is constant to be 4mm, the movement speed of the base body relative to the nozzle is 5cm/min, and the reciprocating movement times of the base body relative to the nozzle is 10 times.
Example 3
A preparation method of a high insulation resistance silicon dioxide thin film material comprises the following steps: under the condition of room temperature, an atmospheric pressure discharge device is utilized, a metal matrix in any shape is taken as a substrate material, argon with the purity of 99.99 percent is taken as a discharge gas and a carrier gas, oxygen with the purity of 99.99 percent is taken as a reaction gas, silicon tetrachloride with the purity of 99.99 percent is taken as a reaction liquid, the atmospheric pressure discharge is carried out to prepare a silicon dioxide film, a nozzle of the atmospheric pressure discharge device keeps a constant distance with the surface of the matrix, the thickness of the obtained silicon dioxide film is 5.38 mu m, and the insulation resistance of the silicon dioxide film is 2.67 +/-0.32 multiplied by 109Omega, the insulation resistance of the silicon dioxide film material is 4.96 plus or minus 0.14 multiplied by 10 according to the linear relation calculation of the insulation resistance of the silicon dioxide film material and the thickness thereof8Ω/μm。
Wherein: the working frequency of the alternating current power supply is 20kHz, and the power is 70W; the argon flow was 5 slm; the carrier gas of the silicon tetrachloride is argon, and the flow rate is 30 sccm; the oxygen flow rate is 25 sccm; the deposition time was 10 min. The matrix is fixed, a nozzle of the atmospheric pressure discharge device is always vertical to the surface of the matrix and reciprocates on the surface of the matrix, the distance between the nozzle and the surface of the matrix is constant to be 3mm, the movement speed of the nozzle relative to the matrix is 10cm/min, and the reciprocating movement times of the nozzle relative to the matrix are 20 times.
Example 4
A preparation method of a high insulation resistance silicon dioxide thin film material comprises the following steps: under the condition of room temperature, an atmospheric pressure discharge device is utilized, a metal matrix in any shape is taken as a substrate material, argon with the purity of 99.99 percent is taken as a discharge gas and a carrier gas, oxygen with the purity of 99.99 percent is taken as a reaction gas, silicon tetrachloride with the purity of 99.99 percent is taken as a reaction liquid, the atmospheric pressure discharge is carried out to prepare a silicon dioxide film, a nozzle of the atmospheric pressure discharge device keeps a constant distance with the surface of the matrix, the thickness of the obtained silicon dioxide film is 6.47 mu m, and the insulation resistance of the silicon dioxide film is 3.49 +/-0.38 multiplied by 109Omega, the insulation resistance of the silicon dioxide film material is 5.39 plus or minus 0.18 multiplied by 10 according to the linear relation between the insulation resistance of the silicon dioxide film material and the thickness of the silicon dioxide film material8Ω/μm。
Wherein: the working frequency of the alternating current power supply is 50kHz, and the power is 90W; the argon flow was 7 slm; the carrier gas of the silicon tetrachloride is argon, and the flow rate is 40 sccm; the oxygen flow rate is 35 sccm; the deposition time was 7 min. The matrix is fixed, a nozzle of the atmospheric pressure discharge device is always vertical to the surface of the matrix and reciprocates on the surface of the matrix, the distance between the nozzle and the surface of the matrix is constant to be 4mm, the movement speed of the nozzle relative to the matrix is 30cm/min, and the reciprocating movement times of the nozzle relative to the matrix are 30 times.
Example 5
A preparation method of a high insulation resistance silicon dioxide thin film material comprises the following steps: under the condition of room temperature, an atmospheric pressure discharge device is utilized, a metal matrix in any shape is taken as a substrate material, argon with the purity of 99.99 percent is taken as a discharge gas and a carrier gas, oxygen with the purity of 99.99 percent is taken as a reaction gas, silicon tetrachloride with the purity of 99.99 percent is taken as a reaction liquid, the atmospheric pressure discharge is carried out to prepare a silicon dioxide film, a nozzle of the atmospheric pressure discharge device keeps a constant distance with the surface of the matrix, the thickness of the obtained silicon dioxide film is 5.29 mu m, and the insulation resistance of the silicon dioxide film is 8.78 +/-0.53 multiplied by 109Omega, the insulation resistance of the silicon dioxide film material is 1.66 plus or minus 0.89 multiplied by 10 according to the linear relation calculation of the insulation resistance of the silicon dioxide film material and the thickness thereof9Ω/μm。
Wherein: the working frequency of the alternating current power supply is 13.56MHz, and the power is 200W; the argon flow was 10 slcm; the carrier gas of the silicon tetrachloride is argon, and the flow rate is 50 sccm; the oxygen flow rate is 50 sccm; the deposition time was 5 min. The matrix is fixed, the nozzle of the atmospheric pressure discharge device is always vertical to the surface of the matrix and reciprocates on the surface of the matrix, the distance between the nozzle and the surface of the matrix is constant to 5mm, the movement speed of the nozzle relative to the matrix is 60cm/min, and the reciprocating movement times of the nozzle relative to the matrix are 50 times.
Comparative example 1
A preparation method of a silicon dioxide film material comprises the following steps: under the condition of room temperature, an atmospheric pressure discharge device is utilized, a metal matrix in any shape is taken as a substrate material, argon with the purity of 99.99 percent is taken as a discharge gas and a carrier gas, oxygen with the purity of 99.99 percent is taken as a reaction gas, silicon tetrachloride with the purity of 99.99 percent is taken as a reaction liquid, the atmospheric pressure discharge is carried out to prepare a silicon dioxide film, a nozzle of the atmospheric pressure discharge device keeps a constant distance with the surface of the matrix, the thickness of the obtained silicon dioxide film is 5.05 mu m, and the insulation resistance of the silicon dioxide film is 1.48 +/-0.95 multiplied by 105Omega, the insulation resistance of the silicon dioxide film material is 2.9 plus or minus 1.9 multiplied by 10 according to the linear relation between the insulation resistance of the silicon dioxide film material and the thickness of the silicon dioxide film material4Ω/μm。
Wherein: the working frequency of the alternating current power supply is 5kHz, and the power is 30W; the argon flow was 3 slcm; the carrier gas of the silicon tetrachloride is argon, and the flow rate is 10 sccm; the deposition time was 20 min. The nozzle of the atmospheric pressure discharge device is fixed on the surface of the substrate, the distance between the nozzle and the surface of the substrate is constant and 5mm, and the nozzle does not move relative to the substrate.
Claims (7)
1. A preparation method of a high insulation resistance silicon dioxide film material is characterized by comprising the following steps: the preparation method comprises the following steps: obtaining a silicon dioxide film material with high insulation resistance by using an atmospheric pressure discharge method, wherein the atmospheric pressure discharge temperature is room temperature, a nozzle of an atmospheric pressure discharge device is always vertical to the surface of a substrate in the growth process of the silicon dioxide film, the nozzle keeps a constant distance with the surface of the substrate, and the nozzle performs periodic reciprocating motion relative to the surface of the substrate;
the movement speed is more than 0.5cm/min, the periodic reciprocating times are more than 1, the deposition time is more than 1min, and the thickness of the silicon dioxide film material is more than 1 mu m;
the surface of the substrate is a curved surface;
the silicon source of the silicon dioxide film is silicon tetrachloride.
2. The method of claim 1, wherein: the substrate material is a material made of compact materials.
3. The method of claim 2, wherein: the compact material is made of metal, circuit board, ceramic or semiconductor.
4. The production method according to claim 3, characterized in that: the working gas of the atmospheric pressure discharge is argon, and the purity of the argon is 99.99 percent;
the purity of the silicon tetrachloride is more than 98 percent;
the auxiliary oxygen source of the silicon dioxide film is oxygen, and the purity of the oxygen is 99.99%.
5. The method of claim 4, wherein: the argon flow is greater than 1 slm;
the oxygen flow is more than 5 sccm;
the carrier gas of the silicon tetrachloride is argon or oxygen, and the flow of the carrier gas is more than 10 sccm.
6. A high insulation resistance silicon dioxide thin film material prepared by the method of claim 1, 2, 3, 4 or 5.
7. The high insulation resistance silica thin film material according to claim 6, wherein: the insulation resistance of the silicon dioxide film material is more than 108Ω/μm。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1845797A (en) * | 2003-09-09 | 2006-10-11 | 陶氏环球技术公司 | Glow discharge-generated chemical vapor deposition |
| CN107299315A (en) * | 2017-07-11 | 2017-10-27 | 大连交通大学 | A kind of high insulaion resistance silica membrane material and preparation method thereof |
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| CN1845797A (en) * | 2003-09-09 | 2006-10-11 | 陶氏环球技术公司 | Glow discharge-generated chemical vapor deposition |
| CN107299315A (en) * | 2017-07-11 | 2017-10-27 | 大连交通大学 | A kind of high insulaion resistance silica membrane material and preparation method thereof |
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