CN106277824A - The manufacture method of silicon dioxide film - Google Patents
The manufacture method of silicon dioxide film Download PDFInfo
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- CN106277824A CN106277824A CN201510270416.XA CN201510270416A CN106277824A CN 106277824 A CN106277824 A CN 106277824A CN 201510270416 A CN201510270416 A CN 201510270416A CN 106277824 A CN106277824 A CN 106277824A
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- liquid
- silicon dioxide
- dioxide film
- reactant
- manufacture method
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Abstract
The present invention discloses the manufacture method of a kind of silicon dioxide film, including: first, a reactant is immersed in a liquid, and stops the response time.Reactant includes that at least one body and body surface are coated with a polysiloxane.The Celsius temperature of liquid is less than 80 degree.Then, in liquid, reactant is then taken out in the response time.So, the polysilazane constituent of reactant and liquid generation oxidation reaction, therefore, the response time then, after the drying, polysilazane constituent is to be transformed into silicon dioxide film to the reactant taken out in liquid.
Description
Technical field
The present invention is relevant with surface treatment method, particularly relates to the manufacture method of a kind of silicon dioxide film.
Background technology
No. 201245045 publication of TaiWan, China discloses the manufacture method of a kind of silicon dioxide film, and it is mat
By in hydrogen peroxide gas environment, the substrate scribbling polysilazane is heated, and make to be formed on substrate titanium dioxide
Silicon fiml.
Owing to the disclosure case is to be used as oxidation reaction environment, and oxidation reaction by hydrogen peroxide gas environment
Time need the hydrogen peroxide gas concentration in monitor closely environment and ambient temperature, avoid causing danger.Institute
With, the reaction efficiency of obvious the disclosure case is mainly affected by hydrogen peroxide gas concentration.
Summary of the invention
Because above-mentioned disappearance, it is an object of the invention to provide the manufacture method of a kind of silicon dioxide film, and
This manufacture method is not affected by hydrogen peroxide gas concentration, and can be applicable to Celsius temperature less than 80 degree.
For reaching above-mentioned purpose, the manufacture method of the silicon dioxide film of the present invention includes: first, reacts one
Thing is immersed in a liquid, and stops the response time.Reactant includes that at least one body and body surface are coated with
Cloth one polysiloxane.The Celsius temperature of liquid is less than 80 degree.Then, the response time then
Reactant is taken out in liquid.
So, when being immersed in liquid due to reactant, the polysilazane constituent of reactant occurs with liquid
Oxidation reaction, and be transformed into silicon dioxide film, subsequently, the reactant taken out in liquid, and allow this body surface
Face forms the silicon dioxide film that matter is close.
It is preferred that to the reactant baking taken out in this liquid, so, silicon dioxide film hardening will be accelerated
Time.
About the detailed step of manufacture method, feature, the result of silicon dioxide film provided by the present invention or hold
Line mode, is described by describing in detail in follow-up embodiment.But, have in field of the present invention
Usually intellectual should be able to understand, and those describe in detail and implement the specific embodiment cited by the present invention,
It is only for illustrating the present invention, and is not used to limit scope of the presently claimed invention.
Describe the present invention below in conjunction with the drawings and specific embodiments, but not as to the present invention's
Limit.
Accompanying drawing explanation
1st figure is the manufacture method flow chart of the silicon dioxide film of the present invention.
Step S10-S12
Detailed description of the invention
Hereinafter, the preferred embodiment hereby coordinating each accompanying drawing to enumerate correspondence carrys out the system of the silicon dioxide film to the present invention
Make the composition component of method and reach effect and explain.The manufacture method of silicon dioxide film in right each accompanying drawing
Result is only used for illustrating the technical characteristic of the present invention, rather than limits the invention.
As it is shown in figure 1, the manufacture method of inventive silica film comprises the following steps:
First, step, S10 a: reactant is immersed in a liquid, and stop the response time.Instead
At least one body and body surface are coated with a polysiloxane to answer thing to include.The temperature of liquid is temperature Celsius
Spend less than 80 degree.
Then, step S11: then take out reactant in liquid in the response time.
Soak and refer to that the polysiloxane of body surface impregnates in a liquid, or the whole immersion of reactant
In a liquid, in other words, reactant can soak in a liquid all or in part.
So, polysiloxane and liquid generation oxidation reaction, and allow polysiloxane change
Silicon dioxide film, the reactant taken out in liquid subsequently, stay in normal temperature environment dried, body surface
Polysiloxane can change the close silicon dioxide film of matter (i.e. glass-film).
It is converted into harder silicon dioxide film time, therefore, the present invention's to shorten polysiloxane
Manufacture method also includes step S12: to the reactant baking taken out in liquid.Curing environment temperature between
Between Celsius temperature 70-120 degree, so, the dioxy that hardness is harder is become shortening polysiloxane
SiClx film.
The body of reactant can be substrate, thin film or particle, and its material can be resistant to elevated temperatures metal or
The glass of non-refractory, wood, plastic cement, acrylic etc., particle can be the millimeter such as fluorescent powder, crystal grain
Particle to nano-scale.Additionally, body do not limit its face shaping.
Polysiloxane refers to the composition in solvent containing polysiloxane, and is current material, the most not
Repeat.
The coating method of polysiloxane can be the sides such as dip coated, roller type coating, rotary coating
Formula.Wherein, if the body of reactant is particle, it is thus preferable to coating method is to select dip coated.
So, the manufacture method of the silicon dioxide film of the present invention can allow poly-silicon effectively in cold liquid environment
Oxygen alkane constituent produces oxidation reaction with liquid, and is changed into silicon dioxide film, to improve conventional high-temperature heating
And the shortcoming carrying out oxidation reaction in gaseous environment.Also, tradition uses hydrogen peroxide gas to transfer as oxidation
Reaction, if but the too high meeting of hydrogen peroxide gas concentration cause danger, review, the present invention be select Celsius temperature
80 degree or less than the liquid of Celsius temperature 80 degree, owing to the present invention is employing liquid, and unconventional gas
Or high-temp liquid, therefore the present invention is without considering the problem of concentration of hydrogen peroxide, and is applicable to non-refractory
On the body of reactant.
Enumerate 3 results of the test that the manufacture method of the silicon dioxide film by the present invention is carried out subsequently, in
In this experiment, the body of reactant is glass substrate, such as table 1 to 3:
Table 1
Table 1 is as a example by water, wherein liquid be with pH value equal to 7 water, and its temperature scope be temperature Celsius
As a example by between degree 25-80 degree.In this experiment, common condition is reactant poly-(before i.e. soaking) before reaction
The applied thickness of siloxanes constituent is 0.2um, and its water droplet angle is 85 degree, and hardness is also less than 1H.
Wherein, water droplet angle is also referred to as contact angle (contact angle).
Continuous with reference to table 1, when reactant soaks the liquid of different Celsius temperature (25,50 and 80 degree) respectively,
After about 5 minutes response time, the polysiloxane of body surface and water generation oxidation reaction, and make this
Surface forms the silicon dioxide film more than 1H, and the reactant then reaction completed takes out in liquid,
And selectively by baking, to improve the silicon dioxide film hardness of body surface.Wherein, when polysiloxanes group
After becoming thing to be transformed into more than the silicon dioxide film of 1H, also can change in its water droplet angle, and can from table 1
Finding that hardness reaches the silicon dioxide film of 9H, its water droplet angle is minimum.In experiment, temperature of liquid is Celsius
Temperature 80 degree can obtain optimal water droplet angle and hardness, but temperature of liquid the most all can allow poly-silicon at 25 and 50 degree
Oxygen alkane constituent is transformed into hardness more than 1H silicon dioxide film.
Table 2
As a example by table 2 is acidic liquid, its pH value is about 0.96, and carries out with two Celsius temperatures, respectively
It it is Celsius temperature 25 degree and 50 degree.It is the most superfluous that reactant condition before the reaction is substantially same as this with table 1
State.In reactant is separately immersed in different temperatures acid solution, after reacting 1 minute, gathering of body surface
There is oxidation reaction in siloxanes constituent in acidic liquid, and it is big to allow polysiloxane be transformed into hardness
In the silicon dioxide film of 1H, subsequently, reactant reaction completed takes out in acidic liquid, and selects
Ground is by baking, to improve the silicon dioxide film hardness of body surface.Wherein, at the acid solution of 50 degree
Middle immersion 1 minute, the polysiloxane composition of body surface just can be transformed into the titanium dioxide of hardness 9H smoothly
Silicon fiml, and its water droplet angle is the least.
Compared to the pH value aqueous solution equal to 7, acidic liquid carries out oxidation reaction and not only can shorten instead
Between Ying Shi, it is also with relatively low temperature of liquid, allows polysiloxane be transformed into hardness smoothly and reach
The silicon dioxide film of 9H.
Table 3
As a example by table 3 is akaline liquid, its pH value is 12.87 and 14.64 respectively.Wherein, reactant is instead
Condition before Ying is substantially same as this with table 1 and repeats no more.Difference is, the akaline liquid of different pH value
It is all at room temperature (i.e. Celsius temperature about 25 degree), and (reaction) time of immersion is all 1 minute.So, reaction
The polysiloxane of thing and akaline liquid generation oxidation reaction, and allow the polysiloxanes of body surface form
Thing can change the hardness silicon dioxide film more than 1H, and subsequently, reactant reaction completed is from akaline liquid
Middle taking-up, and selectively by baking, to improve the silicon dioxide film hardness of body surface.
Compared to aqueous solution and acidic liquid, can aoxidize with the short time in Normal Atmospheric Temperature Liquid at akaline liquid
Reaction, improves reaction efficiency and reduces reaction temperature, therefore polysiloxane can obtain in akaline liquid
Obtain reaction efficiency most preferably.
Understanding by above-mentioned experiment, liquid preferably selects alkalescence, such as potassium hydroxide (KOH), four
Ammonium hydroxide (TMAH) or organic base, and its preferable pH value is between 12-15.Additionally,
Acidic liquid is also a selection, such as hydrochloric acid (HCI), and its preferable pH value is between 0-2.
Although can find from experimental result, it is can the most on the glass substrate by the manufacture method of the present invention
Form hardness and reach the silicon dioxide film of 9H, if but it practice, the body hardness of reactant is less than 9H (such as
Plastic plate, acrylic board, wood, powder etc.) then silicon dioxide film hardness be also not up to 9H, therefore this
Bright manufacture method does not reaches 9H with silicon dioxide film and is limited, but to form dioxy at various body surfaces
For the purpose of SiClx film.
The time that reactant is soaked in liquid is typically set in 0.5-30 minute, the most then be located at 1-10 and divide
Clock, to avoid the time acid too for a long time or akaline liquid etching reaction thing.Although aforesaid temperature of liquid is minimum it is
Room temperature, but it practice, the Celsius temperature of liquid can also be less than 25 degree, therefore temperature of liquid is not with temperature Celsius
Degree 80-25 degree is limited.
Also, it is to improve silicon dioxide film hardness that reactant carries out baking, but it practice, the step of baking
Suddenly can also be omitted.
In sum, the manufacture method of the silicon dioxide film of the present invention can be efficiently applied to various non-refractory
On body, so that the body surface of non-refractory forms the silicon dioxide film of high rigidity, to protect body.
Finally it is to be emphasized again that, the present invention takes off composed component disclosed in embodiment in front, is only for example
Bright, not it is used for limiting the scope of this case, the replacement of other equivalence elements or change, also should be the power of this case
Profit claimed range is contained.
Claims (9)
1. the manufacture method of a silicon dioxide film, it is characterised in that comprise the following steps:
Being immersed in a liquid by one reactant, and stop the response time, this reactant includes at least one
Body and this body surface are coated with a polysiloxane, the Celsius temperature of this liquid less than 80 degree；And
In this liquid, this reactant is then taken out in this response time.
The manufacture method of silicon dioxide film the most according to claim 1, it is characterised in that further include
To the reactant baking taken out in this liquid.
The manufacture method of silicon dioxide film the most according to claim 2, it is characterised in that baking ring
Border temperature is between Celsius temperature 70-120 degree.
The manufacture method of silicon dioxide film the most according to claim 1, it is characterised in that this liquid
For alkalescence.
The manufacture method of silicon dioxide film the most according to claim 3, it is characterised in that this liquid
PH value between 12-15.
The manufacture method of silicon dioxide film the most according to claim 1, it is characterised in that this liquid
For acidity.
The manufacture method of silicon dioxide film the most according to claim 6, it is characterised in that this liquid
PH value between 0-2.
The manufacture method of silicon dioxide film the most according to claim 1, it is characterised in that this reaction
Time is 0.5-30 minute.
The manufacture method of silicon dioxide film the most according to claim 1, it is characterised in that this body
It is a substrate, a thin film and the one of which of a particle.
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| CN201510270416.XA CN106277824A (en) | 2015-05-25 | 2015-05-25 | The manufacture method of silicon dioxide film |
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| CN201510270416.XA CN106277824A (en) | 2015-05-25 | 2015-05-25 | The manufacture method of silicon dioxide film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987014A (en) * | 2017-02-24 | 2017-07-28 | 上海与德信息技术有限公司 | The preparation method of acrylic combined housing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260763A (en) * | 1997-04-17 | 2000-07-19 | 联合讯号公司 | Process for producing manoporous dielectric films at high pH |
| CN1325541A (en) * | 1998-08-27 | 2001-12-05 | 联合讯号公司 | Nanoporous silica deposited through mixture |
| CN101965629A (en) * | 2008-03-06 | 2011-02-02 | Az电子材料（日本）株式会社 | Dipping solution for use in production of siliceous film and process for producing siliceous film using the dipping solution |
-
2015
- 2015-05-25 CN CN201510270416.XA patent/CN106277824A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260763A (en) * | 1997-04-17 | 2000-07-19 | 联合讯号公司 | Process for producing manoporous dielectric films at high pH |
| CN1325541A (en) * | 1998-08-27 | 2001-12-05 | 联合讯号公司 | Nanoporous silica deposited through mixture |
| CN101965629A (en) * | 2008-03-06 | 2011-02-02 | Az电子材料（日本）株式会社 | Dipping solution for use in production of siliceous film and process for producing siliceous film using the dipping solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987014A (en) * | 2017-02-24 | 2017-07-28 | 上海与德信息技术有限公司 | The preparation method of acrylic combined housing |
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