CN107587121A - The preparation method of DLC film and eyeglass - Google Patents
The preparation method of DLC film and eyeglass Download PDFInfo
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- CN107587121A CN107587121A CN201710657916.8A CN201710657916A CN107587121A CN 107587121 A CN107587121 A CN 107587121A CN 201710657916 A CN201710657916 A CN 201710657916A CN 107587121 A CN107587121 A CN 107587121A
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Abstract
The present invention relates to new material technology field, especially a kind of eyeglass, its preparation process includes：One transparent substrates are provided；Utilize microwave plasma CVD method, the mixed gas of methane, hydrogen and oxygen is passed through in the reactor chamber, to control temperature be 400 DEG C, microwave power is 1.5kw~2.5kw, 20~30mbar of air pressure, and hydrophily DLC film is formed in the transparent substrates lower surface；Utilize microwave plasma CVD method, the mixed gas of methane, hydrogen and oxygen is passed through in the reactor chamber, to control temperature be 400 DEG C, microwave power is 3kw~4kw, 35~45mbar of air pressure, and hydrophobicity DLC film is formed in the transparent substrates upper surface.The present invention obtains hydrophilic/hydrophobic DLC film, and two kinds of DLC films are had into application well applied in eyeglass preparation by controlling reaction condition.
Description
Technical field
The present invention relates to new material technology field, especially a kind of preparation method of DLC film.
Background technology
DLC film (DLC, DIAMOND-LIKE CARBON) is a kind of to be made up of carbon, in nature and bore
Stone is similar, while has the material of graphite atom composition structure again.DLC is a kind of noncrystalline membrane, due to high rigidity and
High elastic modulus, it is widely studied and applied.
The method for preparing DLC film at present is a lot, the carbon source and arrival matrix surface used in different preparation methods
Ion energy is different, and the structure and performance of the DLC film of deposition have very big difference.
Limited by current DLC production technologies, existing DLC film is usually therefore its visible light transmission from colored
Rate is very low, causes application also to limit.
The content of the invention
To solve the above problems, the present invention provides a kind of preparation method of eyeglass, comprise the following steps：
One transparent substrates are provided；
Using microwave plasma CVD method, the mixing of methane, hydrogen and oxygen is passed through in the reactor chamber
Gas, solid state microwave sources that selected frequency is 915MHz, temperature are 400 DEG C, microwave power is 1.5kw~2.5kw, air pressure 20~
30mbar, hydrophily DLC film is formed in the transparent substrates lower surface；
Using microwave plasma CVD method, the mixing of methane, hydrogen and oxygen is passed through in the reactor chamber
Gas, solid state microwave sources that selected frequency is 915MHz, temperature are 400 DEG C, microwave power is 3kw~4kw, air pressure 35~
45mbar, hydrophobicity DLC film is formed in the transparent substrates upper surface.
In addition, the present invention also provides the preparation method of this hydrophily DLC film, comprise the following steps：
Using microwave plasma CVD method, the mixing of methane, hydrogen and oxygen is passed through in the reactor chamber
Gas, selected frequency are 915MHz 400 DEG C of solid state microwave sources, temperature, power 1.5kw~2.5kw, 20~30mbar of air pressure,
Hydrophily DLC film is formed in the transparent substrates lower surface.
The present invention also provides the preparation method of this hydrophobicity DLC film, comprises the following steps：
Using microwave plasma CVD method, the mixing of methane, hydrogen and oxygen is passed through in the reactor chamber
Gas, selected frequency is 915MHz 400 DEG C of solid state microwave sources, temperature, power 3kw~4kw, 35~45mbar of air pressure, in institute
State transparent substrates upper surface and form hydrophobicity DLC film.
Beneficial effect：
The present invention uses microwave plasma CVD method, on the basis of it need not adjust reactant, leads to
Cross control reaction condition and obtain the different hydrophily DLC film of performance, hydrophobicity DLC film.The present invention also profit
Eyeglass is prepared with the hydrophily DLC film of acquisition, hydrophobicity DLC film so that eyeglass can obtain hydrophilic simultaneously
Property and hydrophobicity, available for fields such as swimming glasses, luntttes, have a good application prospect.
Brief description of the drawings
Fig. 1 a are ESEM (SEM) figure of hydrophily DLC film in the lens monomer of the embodiment of the present invention 1；Fig. 1 b
For ESEM (SEM) figure of hydrophobicity DLC film in the lens monomer of the embodiment of the present invention 2.
Fig. 2 is the light transmittance test result figure of hydrophily DLC film in the lens monomer of the embodiment of the present invention 2.
Fig. 3 is the light transmittance test result figure of hydrophobicity DLC film in the lens monomer of the embodiment of the present invention 2.
Fig. 4 is the structural representation of the eyeglass of the embodiment of the present invention 3.
Fig. 5 a are the PVvalue testing result figure of hydrophobicity DLC film in the lens monomer of the embodiment of the present invention 2；
Fig. 5 b are the wear rate test result figure of hydrophobicity DLC film in the lens monomer of the embodiment of the present invention 2.
Specific embodiment mode
Embodiment 1
The present embodiment provides a kind of preparation method of hydrophily DLC film, comprises the following steps：
The ready transparent substrates are placed in reaction chamber, are in the reactor chamber 3 according to volume flow ratio：100：1
It is passed through the mixed gas of methane, hydrogen and oxygen.Preferably, the Standard Gases of methane, hydrogen and oxygen are controlled in the present embodiment
Body flow is respectively：Methane 12sccm and hydrogen 400sccm, oxygen 4sccm.Further, reaction condition is controlled：From microwave
Frequency is 915MHZ high-power microwave solid source, 400 DEG C of temperature, microwave power 1.5kw~2.5kw, 20~30mbar of air pressure,
Hydrophily DLC film is formed on the surface of the transparent substrates.Specifically, coating speed is preferably 45~60min depositions
1 μm, thickness is formed close to the hydrophily DLC film of 5 μm (maximum gauge is no more than 10 μm).It is this with reference to shown in Fig. 1 a
The crystal particle diameter size of hydrophily DLC film is 50~100nm, shows good hydrophily.
In addition, the present embodiment additionally provides the light transmittance test of this hydrophily DLC film.Existing diamond-like
Stone film, it is coloured by being limited by production technology.And the DLC film that the present embodiment is produced is transparent nothing
Color.With reference to shown in Fig. 2, its visible region light transmittance in 400~700nm reaches more than 90%, illustrates hydrophily class
Diamond thin has very high light transmittance.Further, hydrophily DLC film has very high hardness, uses《GB/
T 6739-1996 hardness of film pencil determination methods》Measure, hardness number can reach 9H.
Embodiment 2
The present embodiment provides a kind of preparation method of hydrophobicity DLC film, comprises the following steps：
The ready transparent substrates are placed in reaction chamber, are in the reactor chamber 3 according to volume flow ratio：100：1
It is passed through the mixed gas of methane, hydrogen and oxygen.Preferably, the Standard Gases of methane, hydrogen and oxygen are controlled in the present embodiment
Body flow is respectively：Methane 12sccm and hydrogen 400sccm, oxygen 4sccm.Further, reaction condition is controlled：Selected frequency
For 915MHz high power solid state microwave source, 400 DEG C of temperature, power 3kw~4kw, 35~45mbar of air pressure, in the transparent base
The surface at bottom forms hydrophobicity DLC film.Specifically, coating speed is preferably that 45~60min deposits 1 μm, forms thickness
Close to the hydrophobicity DLC film of 5 μm (maximum gauge is no more than 10 μm).With reference to shown in Fig. 1 b, this hydrophobicity diamond-like
The crystal particle diameter size of stone film is 10~50nm, and compared with hydrophily DLC film, crystal particle diameter is smaller finer and close, is shown
Good hydrophobicity is shown.In addition, the present embodiment additionally provides the light transmittance test of this hydrophobicity DLC film.It is existing
DLC film, be coloured by being limited by production technology.And the DLC film that the present embodiment is produced
It is clear, colorless.With reference to shown in Fig. 3, its visible region light transmittance in 400~700nm reaches more than 90%, average
Light transmittance is 98.31%, illustrates that hydrophobicity DLC film has very high light transmittance.
In addition, this hydrophobicity DLC film also has good hardness.Using U.S.'s UMT-3 friction-wear tests
Machine, the friction and wear behavior of the DLC film on test lucite surface.Using GCr15 to mill pair, experimental period
20min, circular orbit abrasion (orbit radius 6mm), friction velocity 200Rpm, load 0.5N.By above-mentioned wear testing, obtain
Result as shown in Fig. 5 a, 5b：The coefficient of friction of DLC film is about 0.2, and wear rate is 7.75 × 10-17m3N-1m-1.Class
As, use《GB/T6739-1996 hardness of film pencil determination methods》Measure, hardness number can reach 9H.
Embodiment 3
With reference to shown in Fig. 3, the present embodiment provides a kind of eyeglass 10, and its composition includes：What is set gradually from below to up is antifog
The 13, first binder course 16 of layer, transparent substrates 14, the second binder course 17, hydrophobic layer 15.Wherein, the material of transparent substrates 14 can example
Such as it is lucite.First binder course 16, the material of the second binder course 17 may be, for example, that nano silicon-epoxy resin is multiple
Condensation material or organic siliconresin.
Preferably, the material of the anti-fog layer 13 is hydrophily DLC film, and thickness is not more than 5 μm.It is described hydrophobic
The material of layer 15 is hydrophobicity DLC film, and thickness is not more than 5 μm.The thickness of first binder course 16, the second binder course 17
About 1 μm, the introducing of the first binder course 16, the second binder course 17 can strengthen anti-fog layer in transparent substrates, hydrophobic layer in transparent
Adhesion between substrate.
The preparation method of above-mentioned eyeglass is described below, comprises the following steps：
Step 1：One transparent substrates 13 are provided.The transparent substrates may be, for example, lucite, is cleaned and removed by ultrasonic wave
Surface impurity, it is standby after drying.
Step 2：Using hardening of resin film production equipment, the first binder course is formed respectively on two surfaces of transparent substrates 13
16th, the second binder course 17.
Specifically, first transparent substrates 13 are cleaned, removes the surface impurity of transparent substrates 13.Then, to described transparent
Substrate 13 carries out sided corona treatment, improves the adhesive force of transparent substrates.
The hardening of resin film production equipment includes spray equipment, in the spray equipment equipped with nano silicon-
Epoxy resin dispersion liquid, the substrate moves corresponding to the spray equipment, to accept the showering liquid.In transparent substrates 13
Upper and lower surface sprays showering liquid, by Self-leveling process so that showering liquid uniformly, is entirely formed above and below transparent substrates 13
Two surfaces.Wherein, the showering liquid selects nano silicon-epoxy resin dispersion liquid, the viscosity of regulation showering liquid for 5~
20mpa.s, transparent substrates 13 are 1~5cm/s by the speed of spray；The ejection flow speed of showering liquid is 20~30ml/s.
Baked finally by infrared preliminary drying, after ultraviolet curing, first is formed respectively on two surfaces of transparent substrates 13
Binder course 16, the second binder course 17, the first binder course 16, the second binder course 17 are a spray process while formed.
Step 3：Using microwave plasma CVD method, anti-fog layer is deposited in the transparent substrates.
The ready transparent substrates are placed in reaction chamber, are in the reactor chamber 3 according to volume flow ratio：100：1
It is passed through the mixed gas of methane, hydrogen and oxygen.Preferably, the Standard Gases of methane, hydrogen and oxygen are controlled in the present embodiment
Body flow is respectively：Methane 12sccm and hydrogen 400sccm, oxygen 4sccm.Further, reaction condition is controlled：Microwave solid
The microwave frequency 915MHZ in source, 400 DEG C of temperature, microwave power 1.5kw~2.5kw, 20~30mbar of air pressure, in the transparent base
Bottom surface forms hydrophily DLC film.Specifically, the coating speed of hydrophily DLC film be preferably 45~
60min deposits 1 μm, forms thickness close to the hydrophily DLC film of 5 μm (maximum gauge is no more than 10 μm) as antifog
Layer.
Step 3：Using microwave plasma CVD method, the depositing hydrophobic layer in the transparent substrates.
The ready transparent substrates are placed in reaction chamber, are in the reactor chamber 3 according to volume flow ratio：100：1
It is passed through the mixed gas of methane, hydrogen and oxygen.Preferably, the Standard Gases of methane, hydrogen and oxygen are controlled in the present embodiment
Body flow is respectively：Methane 12sccm and hydrogen 400sccm, oxygen 4sccm.Further, selected frequency is the big of 915MHz
Power Solid State microwave source, 400 DEG C of temperature, power 3kw~4kw, 35~45mbar of air pressure, are formed in the transparent substrates upper surface
Hydrophobicity DLC film is as hydrophobic layer.Specifically, the coating speed of hydrophobicity DLC film be preferably 45~
60min deposits 1 μm, forms thickness close to the hydrophobicity DLC film of 5 μm (maximum gauge is no more than 10 μm) as hydrophobic
Layer.
Thus, can obtain it is hydrophilic, while hydrophobic eyeglass.
Certainly, step 2, the sequencing of the preparation process of step 3 can exchange.
The eyeglass obtained using the present embodiment, it is not easy to haze inside, does not allow water droplet easy to hang outside, and with good
Light transmittance and hardness, can be applied in the products such as swimming glasses, luntttes, people wear remains to keep clear, clean for a long time
The visual field.
Claims (10)
1. a kind of preparation method of eyeglass, it is characterised in that comprise the following steps：
One transparent substrates are provided；
Using microwave plasma CVD method, the mixed gas of methane, hydrogen and oxygen is passed through in the reactor chamber,
Solid state microwave sources that selected frequency is 915MHz, temperature are 400 DEG C, microwave power is 1.5kw~2.5kw, air pressure 20~
30mbar, hydrophily DLC film is formed in the transparent substrates lower surface；
Using microwave plasma CVD method, the mixed gas of methane, hydrogen and oxygen is passed through in the reactor chamber,
Solid state microwave sources that selected frequency is 915MHz, temperature are 400 DEG C, microwave power is 3kw~4kw, 35~45mbar of air pressure,
The transparent substrates upper surface forms hydrophobicity DLC film.
2. the preparation method of eyeglass according to claim 1, it is characterised in that in the mixed gas：The methane, hydrogen
It is 3 with the ratio between the volume flow of oxygen：100：1.
3. the preparation method of eyeglass according to claim 1 or claim 2, it is characterised in that in the mixed gas：The methane,
The volume flow of hydrogen and oxygen is respectively 12sccm, 400sccm, 4sccm.
4. the preparation method of eyeglass according to claim 1, it is characterised in that the hydrophily DLC film and/or
The formation speed of the hydrophobicity DLC film is 1 μm/45~60min.
5. the preparation method of eyeglass according to claim 1, it is characterised in that be additionally included in the following table of the transparent substrates
Face, upper surface are respectively formed with the first binder course, the second binder course, the hydrophily DLC film, hydrophobicity diamond-like
Stone film is respectively formed at first binder course, on the second binder course.
6. the preparation method of eyeglass according to claim 1, it is characterised in that first binder course and/or described second
The material of binder course is selected from nano silicon-epoxy resin, organic siliconresin.
7. a kind of preparation method of hydrophily DLC film, it is characterised in that comprise the following steps：
Using microwave plasma CVD method, the mixed gas of methane, hydrogen and oxygen is passed through in the reactor chamber,
Solid state microwave sources that selected frequency is 915MHz, temperature are 400 DEG C, microwave power is 1.5kw~2.5kw, air pressure 20~
30mbar, hydrophily DLC film is formed in substrate surface.
8. a kind of preparation method of hydrophobicity DLC film, it is characterised in that comprise the following steps：
Using microwave plasma CVD method, the mixed gas of methane, hydrogen and oxygen is passed through in the reactor chamber,
Solid state microwave sources that selected frequency is 915MHz, temperature are 400 DEG C, microwave power is 3kw~4kw, 35~45mbar of air pressure,
Substrate surface forms hydrophily DLC film.
9. a kind of preparation method of hardening of resin film, it is characterised in that comprise the following steps：
One substrate and the spray equipment equipped with showering liquid are provided；The substrate moves corresponding to the spray equipment, to accept
State showering liquid；
Wherein, the viscosity for adjusting showering liquid be 5~20mpa.s, the translational speed of the relatively described spray equipment of substrate is 1~
5cm/s；The ejection flow speed of showering liquid is 20~30ml/s；
The hardening of resin film is obtained after infrared drying, ultraviolet curing handle the showering liquid liquid.
10. the preparation method of hardening of resin film according to claim 1, it is characterised in that the substrate is accepting the leaching
Also include sided corona treatment before masking liquid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111188032A (en) * | 2020-02-17 | 2020-05-22 | 佛山市思博睿科技有限公司 | Hydrophobic film plating method by plasma chemical vapor deposition method in inter-film combination mode |
| CN111519171A (en) * | 2020-02-17 | 2020-08-11 | 佛山市思博睿科技有限公司 | Hydrophobic film plating method by plasma chemical vapor deposition method with compact film layer |
| JP7442459B2 (en) | 2018-04-24 | 2024-03-04 | アプライド マテリアルズ インコーポレイテッド | Plasma-enhanced chemical vapor deposition of carbon hard masks |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7442459B2 (en) | 2018-04-24 | 2024-03-04 | アプライド マテリアルズ インコーポレイテッド | Plasma-enhanced chemical vapor deposition of carbon hard masks |
| CN111188032A (en) * | 2020-02-17 | 2020-05-22 | 佛山市思博睿科技有限公司 | Hydrophobic film plating method by plasma chemical vapor deposition method in inter-film combination mode |
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| CN111188032B (en) * | 2020-02-17 | 2021-07-09 | 佛山市思博睿科技有限公司 | Hydrophobic film plating method by plasma chemical vapor deposition method in inter-film combination mode |
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