CN107299315B - A kind of high insulation resistance silica membrane material and preparation method thereof - Google Patents
A kind of high insulation resistance silica membrane material and preparation method thereof Download PDFInfo
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- CN107299315B CN107299315B CN201710561828.8A CN201710561828A CN107299315B CN 107299315 B CN107299315 B CN 107299315B CN 201710561828 A CN201710561828 A CN 201710561828A CN 107299315 B CN107299315 B CN 107299315B
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- insulation resistance
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- silica membrane
- membrane material
- high insulation
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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 insulation resistance silica membrane materials and preparation method thereof, belong to surface processing, coating, thin-film material technical field.The preparation method is that: the silica membrane material with high insulation resistance is obtained using the method for magnetron sputtering, during silicon dioxide film growth, substrate is cooked periodical straight reciprocating motion being parallel to target surface direction, movement velocity is 0.56-55.56cm/min, period of motion 5-500.High insulation resistance silica membrane material of the present invention and existing silica membrane material ratio have high insulation resistance.
Description
Technical field
The present invention relates to a kind of high insulation resistance silica membrane materials and preparation method thereof, belong to surface processing, apply
Layer, thin-film material technical field.
Background technique
Silica (Silicon Dioxide, SiO2) thin-film material is a kind of important high insulation resistance material, thin
The fields such as film sensors, integrated circuit have important application, such as: between metallic substrates and thin-film thermocouple temperature sensor
Insulating layer, the insulating layer between the thin film strain meter in metallic substrates etc..
Currently, silica membrane is mostly used thermal oxidation technique preparation, still, thermal oxidation technique is preparing silica membrane
When substrate need to be heated to 1000 DEG C or more, and can only be monocrystalline silicon to substrate, which limits thermal oxidation techniques in gold
Belong to and prepares high-insulativity silica membrane in substrate.Chemical vapour deposition technique is also the common side for preparing silica membrane
Method still contains a large amount of chemical bond Si-H in the silica membrane of chemical vapour deposition technique preparation, reduces dioxy
The insulation performance of SiClx film, and base reservoir temperature, also at 200 DEG C or more, which also limits chemical vapour deposition techniques in Metal Substrate
High-insulativity silica membrane is prepared on bottom.Silica membrane can also be prepared by other methods, such as: ion beam sputtering is heavy
Product technology, technique for atomic layer deposition, chemical bath synthetic technology, sol-gel technique etc., still, above-mentioned technology exists
Shortcoming, such as: it is both needed to outwardly discharge in preparation process containing Cl, F, CO2、SO2、NO2Equal Tail Gas, cause environment
Pollution；The silica membrane material compactness of preparation is low, poor insulativity, film and substrate caking power are poor；In preparation titanium dioxide
During silicon thin film material, high-temperature heat treatment need to be carried out, there is the problems such as time-consuming, low efficiency.
Summary of the invention
The present invention, in the straight reciprocating motion period for being parallel to target surface direction, effectively increases dioxy by control substrate
The insulation resistance of SiClx thin-film material.
The present invention provides a kind of preparation methods of high insulation resistance silica membrane material, the preparation method is that:
The silica membrane material with high insulation resistance is obtained using the method for magnetron sputtering, in silicon dioxide film growth process
In, substrate is cooked periodical straight reciprocating motion being parallel to target surface direction, movement velocity 0.56-55.56cm/min, fortune
The dynamic period 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 degree of the present invention is preferably 1-3 × 10-3Pa。
Sputtering vacuum degree 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, purity 99.99%.
The working gas of magnetron sputtering of the present invention is the argon and oxygen that flow-rate ratio is preferably 10-20:3-7, the purity of argon
It is 99.99%, oxygen purity 99.99%.
Another object of the present invention is provide a kind of high insulation resistance silica membrane material of above method preparation.
The thickness of silica membrane material of the present invention is preferably 2-5 μm.
The insulation resistance of silica membrane material of the present invention is preferably > 108Ω/3μm。
The invention has the following beneficial effects:
1. high insulation resistance silica membrane material of the present invention and existing silica membrane material are than having
There is high insulation 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, at low cost, yield is high, it is convenient for large-scale industrial production.
Detailed description of the invention
3 width of attached drawing of the present invention,
Fig. 1 is the test chart of high insulation resistance silica membrane material of the present invention；
Fig. 2 is substrate of the present invention in the schematic diagram for being parallel to target surface direction and doing periodical straight reciprocating motion；
Fig. 3 is the insulating resistance value of embodiment 1-5, 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.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Embodiment 1
A kind of preparation method of high insulation resistance silica membrane material, the preparation method is that: utilize DC pulse
At room temperature, using glass slide as base material, the silicon for being 99.99% using purity is sputtering target to reaction magnetocontrol sputtering method
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carry out magnetron sputtering and prepare silica as sputter gas
Film, substrate are parallel to silicon target and do periodical straight reciprocating motion, and movement velocity 0.56cm/min, is obtained the period of motion 5
Silica-film thickness be 2.77 μm, insulation 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 5sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 3h.
Embodiment 2
A kind of preparation method of high insulation resistance silica membrane material, the preparation method is that: utilize DC pulse
At room temperature, using glass slide as base material, the silicon for being 99.99% using purity is sputtering target to reaction magnetocontrol sputtering method
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carry out magnetron sputtering and prepare silica as sputter gas
Film, substrate are parallel to silicon target and do periodical straight reciprocating motion, and movement velocity 2.22cm/min, is obtained the period of motion 20
The silica-film thickness arrived is 3.13 μm, and insulation 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 5sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 3h.
Embodiment 3
A kind of preparation method of high insulation resistance silica membrane material, the preparation method is that: utilize DC pulse
At room temperature, using glass slide as base material, the silicon for being 99.99% using purity is sputtering target to reaction magnetocontrol sputtering method
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carry out magnetron sputtering and prepare silica as sputter gas
Film, substrate are parallel to silicon target and do periodical straight reciprocating motion, and movement velocity 5.55cm/min, is obtained the period of motion 50
The silica-film thickness arrived is 3.01 μm, and insulation 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 5sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 3h.
Embodiment 4
A kind of preparation method of high insulation resistance silica membrane material, the preparation method is that: utilize DC pulse
At room temperature, using glass slide as base material, the silicon for being 99.99% using purity is sputtering target to reaction magnetocontrol sputtering method
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carry out magnetron sputtering and prepare silica as sputter gas
Film, substrate are parallel to silicon target and do periodical straight reciprocating motion, and movement velocity 10.8cm/min, is obtained the period of motion 100
The silica-film thickness arrived is 3.11 μm, and insulation 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 5sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 3h.
Embodiment 5
A kind of preparation method of high insulation resistance silica membrane material, the preparation method is that: utilize DC pulse
At room temperature, using glass slide as base material, the silicon for being 99.99% using purity is sputtering target to reaction magnetocontrol sputtering method
Material, the oxygen that the argon and purity for being 99.99% using purity are 99.99% carry out magnetron sputtering and prepare silica as sputter gas
Film, substrate are parallel to silicon target and do periodical straight reciprocating motion, movement velocity 55.56cm/min, the period of motion 500,
Obtained silica-film thickness is 3.38 μm, and insulation 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 5sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 3h.
Comparative example 1
A kind of preparation method of silica membrane material, the preparation method is that: it is splashed using DC pulse reaction magnetic control
At room temperature, using glass slide as base material, the silicon for being 99.99% using purity is shooting method with purity as sputtering target material
The oxygen that 99.99% argon and purity is 99.99% is sputter gas, carries out magnetron sputtering and prepares silica membrane, substrate is flat
Row is stationary in silicon target, and obtained silica-film thickness is 2.64 μm, and insulation 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 5sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 3h.
Claims (5)
1. a kind of preparation method of high insulation resistance silica membrane material, it is characterised in that: the preparation method is that: it utilizes
The method of magnetron sputtering obtains the silica membrane material with high insulation resistance, and the temperature of magnetron sputtering is room temperature, two
During silicon oxide film growth, substrate is cooked periodical straight reciprocating motion being parallel to target surface direction, and movement velocity is
0.56-55.56cm/min, period of motion 5-500, silica membrane material with a thickness of 2-5 μm.
2. preparation method according to claim 1, it is characterised in that: the target of the magnetron sputtering is silicon target, purity
It is 99.99%.
3. preparation method according to claim 1, it is characterised in that: the working gas of the magnetron sputtering is flow-rate ratio
The argon and oxygen of 10-20:3-7, the purity of argon are 99.99%, oxygen purity 99.99%.
4. claim 1,2 or the high insulation resistance silica membrane material of 3 the methods preparation.
5. high insulation resistance silica membrane material according to claim 4, it is characterised in that: the silica is thin
The insulation resistance > 10 of membrane material8Ω。
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| 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 |
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| JPH06264223A (en) * | 1993-03-16 | 1994-09-20 | Hitachi Ltd | Formation of silicon dioxide film |
| 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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| 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 |
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