CN107299315A - A kind of high insulaion resistance silica membrane material and preparation method thereof - Google Patents
A kind of high insulaion resistance silica membrane material and preparation method thereof Download PDFInfo
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- CN107299315A CN107299315A CN201710561828.8A CN201710561828A CN107299315A CN 107299315 A CN107299315 A CN 107299315A CN 201710561828 A CN201710561828 A CN 201710561828A CN 107299315 A CN107299315 A CN 107299315A
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- membrane material
- insulaion resistance
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- silica membrane
- silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The present invention relates to a kind of high insulaion resistance silica membrane material and preparation method thereof, belong to Surface Machining, coating, thin-film material technical field.The preparation method is：The silica membrane material with high insulaion resistance is obtained using the method for magnetron sputtering, during silicon dioxide film growth, substrate is being cooked periodicity straight reciprocating motion parallel to target surface direction, and movement velocity is 0.56 55.56cm/min, and the period of motion is 5 500.High insulaion resistance silica membrane material of the present invention has high insulaion resistance with existing silica membrane material ratio.
Description
Technical field
The present invention relates to a kind of high insulaion resistance silica membrane material and preparation method thereof, belong to Surface Machining, painting
Layer, thin-film material technical field.
Background technology
Silica (Silicon Dioxide, SiO2) thin-film material is the important high insulaion resistance material of a class, thin
There is important application in the fields such as film sensors, integrated circuit, for example：Between metallic substrates and thin-film thermocouple temperature sensor
Insulating barrier, insulating barrier between the thin film strain meter in metallic substrates etc..
At present, silica membrane uses thermal oxidation technique and prepared, and still, thermal oxidation technique is preparing silica membrane
When substrate need to be heated to more than 1000 DEG C, and can only be monocrystalline silicon to substrate, which limits thermal oxidation technique in gold
High-insulativity silica membrane is prepared in category substrate.Chemical vapour deposition technique is also the conventional side for preparing silica membrane
Method, still, contains substantial amounts of chemical bond Si-H, reduces dioxy in silica membrane prepared by chemical vapour deposition technique
The insulating properties of SiClx film, and base reservoir temperature is also more than 200 DEG C, which also limits chemical vapour deposition technique in Metal Substrate
High-insulativity silica membrane is prepared on bottom.Silica membrane can also be prepared by other method, for example：Ion beam sputtering is sunk
Product technology, technique for atomic layer deposition, chemical bath synthetic technology, sol-gel technique etc., still, above-mentioned technology is present
Weak point, for example：It is both needed to outwardly discharge in preparation process containing Cl, F, CO2、SO2、NO2Deng Tail Gas, environment is caused
Pollution；The silica membrane material compactness of preparation is low, poor insulativity, film and substrate caking power are poor；Preparing titanium dioxide
During silicon thin film material, high-temperature heat treatment need to be carried out, there is that time-consuming, the low problem of efficiency.
The content of the invention
The present invention effectively increases dioxy by controlling substrate in the straight reciprocating motion cycle parallel to target surface direction
The insulaion resistance of SiClx thin-film material.
The invention provides a kind of preparation method of high insulaion resistance silica membrane material, the preparation method is：
The silica membrane material with high insulaion resistance is obtained using the method for magnetron sputtering, in silicon dioxide film growth process
In, substrate is being cooked periodicity straight reciprocating motion parallel to target surface direction, and movement velocity is 0.56-55.56cm/min, fortune
The dynamic cycle is 5-500.
DC pulse shielding power supply working frequency of the present invention is preferably 5-350kHz.
Reversing time of the present invention is preferably 0.4-5.0 μ s.
Silicon target Sputtering power density of the present invention is preferably 0.83-11.11W/cm2。
Back end vacuum of the present invention is preferably 1-3 × 10-3Pa。
Sputtering vacuum of the present invention is preferably 0.2-0.9Pa.
Sedimentation time of the present invention is preferably 1-5h.
The temperature of magnetron sputtering of the present invention is preferably room temperature.
The target of magnetron sputtering of the present invention is preferably silicon target, and its purity is 99.99%.
The working gas of magnetron sputtering of the present invention is that flow-rate ratio is preferably 10-20：3-7 argon and oxygen, the purity of argon
For 99.99%, oxygen purity is 99.99%.
Another object of the present invention is provide high insulaion resistance silica membrane material prepared by a kind of above method.
The thickness of silica membrane material of the present invention is preferably 2-5 μm.
The insulaion resistance of silica membrane material of the present invention is preferably ＞ 108Ω/3μm。
The present invention has the beneficial effect that：
1. high insulaion resistance silica membrane material of the present invention has with existing silica membrane material ratio
There is high insulaion resistance；
2. the working gas of magnetron sputtering of the present invention is high-purity argon and high pure oxygen, to environment without any pollution；
3. preparation method of the present invention is simple, cost is low, yield is high, is easy to large-scale industrial production.
Brief description of the drawings
The width of accompanying drawing 3 of the present invention,
Fig. 1 is the test chart of high insulaion resistance silica membrane material of the present invention；
Fig. 2 is that substrate of the present invention is being cooked the schematic diagram of periodicity straight reciprocating motion parallel to target surface direction；
Fig. 3 is embodiment 1-5, the insulating resistance value of silica membrane material described in comparative example 1；
Wherein, 1, metallic substrates, 2, aluminium hearth electrode, 3, silica membrane layer, 4, aluminium top electrode, 5, megger test
Instrument, 6, stepper motor, 7, substrate, 8, silicon target.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Embodiment 1
A kind of preparation method of high insulaion resistance silica membrane material, the preparation method is：Utilize DC pulse
Reaction magnetocontrol sputtering method at ambient temperature, using slide as base material, using purity be 99.99% silicon as sputtering target
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carries out magnetron sputtering and prepares silica as sputter gas
Film, substrate is cooked periodicity straight reciprocating motion parallel to silicon target, and movement velocity is 0.56cm/min, and the period of motion is 5, is obtained
Silica-film thickness be 2.77 μm, its insulaion resistance be 1.53 ± 0.58 × 108Ω。
Wherein, DC pulse shielding power supply working frequency is 100kHz, and reversing time is 1 μ s, silicon target Sputtering power density
For 3.33W/cm2, argon flow is 20sccm, and oxygen flow is 5sccm, and back end vacuum is 3.0 × 10-3Pa, sputtering vacuum is
0.7Pa, sedimentation time is 3h.
Embodiment 2
A kind of preparation method of high insulaion resistance silica membrane material, the preparation method is：Utilize DC pulse
Reaction magnetocontrol sputtering method at ambient temperature, using slide as base material, using purity be 99.99% silicon as sputtering target
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carries out magnetron sputtering and prepares silica as sputter gas
Film, substrate is cooked periodicity straight reciprocating motion parallel to silicon target, and movement velocity is 2.22cm/min, and the period of motion is 20, is obtained
The silica-film thickness arrived is 3.13 μm, and its insulaion resistance is 4.19 ± 1.47 × 108Ω。
Wherein, DC pulse shielding power supply working frequency is 100kHz, and reversing time is 1 μ s, silicon target Sputtering power density
For 3.33W/cm2, argon flow is 20sccm, and oxygen flow is 5sccm, and back end vacuum is 3.0 × 10-3Pa, sputtering vacuum is
0.7Pa, sedimentation time is 3h.
Embodiment 3
A kind of preparation method of high insulaion resistance silica membrane material, the preparation method is：Utilize DC pulse
Reaction magnetocontrol sputtering method at ambient temperature, using slide as base material, using purity be 99.99% silicon as sputtering target
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carries out magnetron sputtering and prepares silica as sputter gas
Film, substrate is cooked periodicity straight reciprocating motion parallel to silicon target, and movement velocity is 5.55cm/min, and the period of motion is 50, is obtained
The silica-film thickness arrived is 3.01 μm, and its insulaion resistance is 7.49 ± 4.09 × 108Ω。
Wherein, DC pulse shielding power supply working frequency is 100kHz, and reversing time is 1 μ s, silicon target Sputtering power density
For 3.33W/cm2, argon flow is 20sccm, and oxygen flow is 5sccm, and back end vacuum is 3.0 × 10-3Pa, sputtering vacuum is
0.7Pa, sedimentation time is 3h.
Embodiment 4
A kind of preparation method of high insulaion resistance silica membrane material, the preparation method is：Utilize DC pulse
Reaction magnetocontrol sputtering method at ambient temperature, using slide as base material, using purity be 99.99% silicon as sputtering target
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carries out magnetron sputtering and prepares silica as sputter gas
Film, substrate is cooked periodicity straight reciprocating motion parallel to silicon target, and movement velocity is 10.8cm/min, and the period of motion is 100, is obtained
The silica-film thickness arrived is 3.11 μm, and its insulaion resistance is 8.69 ± 4.53 × 108Ω。
Wherein, DC pulse shielding power supply working frequency is 100kHz, and reversing time is 1 μ s, silicon target Sputtering power density
For 3.33W/cm2, argon flow is 20sccm, and oxygen flow is 5sccm, and back end vacuum is 3.0 × 10-3Pa, sputtering vacuum is
0.7Pa, sedimentation time is 3h.
Embodiment 5
A kind of preparation method of high insulaion resistance silica membrane material, the preparation method is：Utilize DC pulse
Reaction magnetocontrol sputtering method at ambient temperature, using slide as base material, using purity be 99.99% silicon as sputtering target
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carries out magnetron sputtering and prepares silica as sputter gas
Film, substrate is cooked periodicity straight reciprocating motion parallel to silicon target, and movement velocity is 55.56cm/min, and the period of motion is 500,
Obtained silica-film thickness is 3.38 μm, and its insulaion resistance is 3.16 ± 0.69 × 109Ω。
Wherein, DC pulse shielding power supply working frequency is 100kHz, and reversing time is 1 μ s, silicon target Sputtering power density
For 3.33W/cm2, argon flow is 20sccm, and oxygen flow is 5sccm, and back end vacuum is 3.0 × 10-3Pa, sputtering vacuum is
0.7Pa, sedimentation time is 3h.
Comparative example 1
A kind of preparation method of silica membrane material, the preparation method is：Splashed using DC pulse reaction magnetic control
Shooting method at ambient temperature, using slide as base material, using purity be 99.99% silicon as sputtering target material, using purity as
The oxygen that 99.99% argon and purity is 99.99% is sputter gas, carries out magnetron sputtering and prepares silica membrane, substrate is put down
Row is in silicon target transfixion, and obtained silica-film thickness is 2.64 μm, and its insulaion resistance is 8.70 ± 0.76 × 106
Ω。
Wherein, DC pulse shielding power supply working frequency is 100kHz, and reversing time is 1 μ s, silicon target Sputtering power density
For 3.33W/cm2, argon flow is 20sccm, and oxygen flow is 5sccm, and back end vacuum is 3.0 × 10-3Pa, sputtering vacuum is
0.7Pa, sedimentation time is 3h.
Claims (7)
1. a kind of preparation method of high insulaion resistance silica membrane material, it is characterised in that：The preparation method is：Utilize
The method of magnetron sputtering obtains the silica membrane material with high insulaion resistance, during silicon dioxide film growth,
Substrate is being cooked periodicity straight reciprocating motion parallel to target surface direction, and movement velocity is 0.56-55.56cm/min, motion week
Phase is 5-500.
2. preparation method according to claim 1, it is characterised in that：The temperature of the magnetron sputtering is room temperature.
3. preparation method according to claim 1, it is characterised in that：The target of the magnetron sputtering is silicon target, its purity
For 99.99%.
4. preparation method according to claim 1, it is characterised in that：The working gas of the magnetron sputtering is flow-rate ratio
10-20：3-7 argon and oxygen, the purity of argon is 99.99%, and oxygen purity is 99.99%.
5. high insulaion resistance silica membrane material prepared by claim 1,2,3 or 4 methods describeds.
6. high insulaion resistance silica membrane material according to claim 5, it is characterised in that：The silica is thin
The thickness of membrane material is 2-5 μm.
7. high insulaion resistance silica membrane material according to claim 5, it is characterised in that：The silica is thin
The insulaion resistance ＞ 10 of membrane material8Ω/3μm。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111085411A (en) * | 2020-01-07 | 2020-05-01 | 大连交通大学 | High-insulation-resistance silicon dioxide thin film material and preparation method thereof |
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| JPH06264223A (en) * | 1993-03-16 | 1994-09-20 | Hitachi Ltd | Formation of silicon dioxide film |
| CN101724821A (en) * | 2009-12-25 | 2010-06-09 | 南开大学 | Magnetic control sputtering system capable of adjusting and controlling growth of light trapping structure film of silicon film battery |
| CN102096136A (en) * | 2010-12-17 | 2011-06-15 | 北京控制工程研究所 | Radiation resistant and ultraviolet filtering film for space optic quartz glass and manufacturing method thereof |
| CN104404466A (en) * | 2014-12-26 | 2015-03-11 | 合肥京东方光电科技有限公司 | Magnetron sputtering coating method and system |
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2017
- 2017-07-11 CN CN201710561828.8A patent/CN107299315B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06264223A (en) * | 1993-03-16 | 1994-09-20 | Hitachi Ltd | Formation of silicon dioxide film |
| CN101724821A (en) * | 2009-12-25 | 2010-06-09 | 南开大学 | Magnetic control sputtering system capable of adjusting and controlling growth of light trapping structure film of silicon film battery |
| CN102096136A (en) * | 2010-12-17 | 2011-06-15 | 北京控制工程研究所 | Radiation resistant and ultraviolet filtering film for space optic quartz glass and manufacturing method thereof |
| CN104404466A (en) * | 2014-12-26 | 2015-03-11 | 合肥京东方光电科技有限公司 | Magnetron sputtering coating method and system |
Non-Patent Citations (1)
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| 熊斌等: "基片温度对磁控溅射沉积二氧化硅的影响", 《真空》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111085411A (en) * | 2020-01-07 | 2020-05-01 | 大连交通大学 | High-insulation-resistance silicon dioxide thin film material and preparation method thereof |
| CN111085411B (en) * | 2020-01-07 | 2022-05-13 | 大连交通大学 | High-insulation-resistance silicon dioxide thin film material and preparation method thereof |
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| CN107299315B (en) | 2019-09-20 |
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