阅读说明：本技术 一种玻璃表面的磨砂处理工艺 (Frosted treatment process for glass surface ) 是由 常彩侠 于 2019-10-24 设计创作，主要内容包括：本发明公开了一种玻璃表面的磨砂处理工艺,具体工艺步骤如下：1)玻璃表面的羟基化处理、2)玻璃表面硅烷膜的形成以及3)玻璃表面涂层的制备；本发明通过在玻璃表面形成一层连续完整的硅烷底膜,然后再利用气化的八甲基环四硅氧烷作为携载气体,在等离子体的作用下,使得八甲基环四硅氧烷可以稳定的沉积在玻璃表面,从而使得气化的八甲基环四硅氧烷中携带的混合物粉末可以均匀的沉积分布在玻璃表面的硅烷膜上,经过热处理从而在硅烷膜表面形成一层外层密实内层多孔的梯度多孔结构涂层,使得玻璃表面的磨砂效果好,而且光洁度高、阻挡视线较好,并且后期清洗方便,具有广泛的应用前景。(The invention discloses a frosted treatment process for a glass surface, which comprises the following specific process steps: 1) hydroxylation treatment of the glass surface, 2) formation of a silane film on the glass surface and 3) preparation of a glass surface coating; according to the invention, a layer of continuous and complete silane basement membrane is formed on the surface of the glass, then the gasified octamethylcyclotetrasiloxane is used as carrying gas, under the action of plasma, the octamethylcyclotetrasiloxane can be stably deposited on the surface of the glass, so that the mixture powder carried in the gasified octamethylcyclotetrasiloxane can be uniformly deposited and distributed on the silane membrane on the surface of the glass, and a gradient porous structure coating with a compact outer layer and a porous inner layer is formed on the surface of the silane membrane through heat treatment, so that the glass surface has a good frosting effect, high smoothness, good sight blocking performance, convenience in later cleaning and wide application prospect.)

1. The frosting treatment process for the glass surface is characterized by comprising the following specific process steps:

1) hydroxylation treatment of glass surfaces

Putting glass into a container filled with deionized water, treating for 10-20min under 300-400W ultrasonic waves, pouring out the deionized water, respectively treating for 5-10min with 50-70% ethanol and 40-50% acetone through ultrasonic waves respectively at the power of 200-300W, taking out the glass, drying the glass by blowing with nitrogen, putting the glass into a mixed solution filled with sulfuric acid and hydrogen peroxide, heating for 1-2h in a water bath at the temperature of 90-100 ℃, cooling bath liquid to room temperature, washing the glass with the deionized water until filtrate is neutral, and drying the glass by blowing with the nitrogen;

2) formation of silane film on glass surface

Adding carbonyl iron fiber into a silane coupling agent solution, adding a 3-5% polyethylene glycol aqueous solution by mass, stirring for 2-3h at 500r/min under 300-;

3) preparation of glass surface coatings

Putting the hydroxylated glass into a low-temperature plasma reaction cavity, mixing the gasified octamethylcyclotetrasiloxane and the atomized mixture powder dispersion liquid, introducing the mixture into the plasma reaction cavity, and controlling the flow rate of the gasified octamethylcyclotetrasiloxane to be 2 x 10^-6-5×10^-6ml/min.cm²Setting the vacuum degree in the reaction cavity at 15-25Pa, controlling the plasma discharge power at 200-plus-one (300W), continuing to discharge for 20-30min, taking out the glass, drying at 50-60 ℃ for 3-4h, taking out, placing into a heating furnace, heating to 350-plus-one (400 ℃), preserving heat for 10-15min, heating to 500-plus-one (600 ℃), continuing to preserve heat for 10-20min, taking out, and naturally cooling to room temperature.

2. The frosting treatment process of the glass surface according to claim 1, wherein in the step 1), the preparation method of the mixed solution of sulfuric acid and hydrogen peroxide is as follows: respectively taking 80-90% concentrated sulfuric acid and 30-35% hydrogen peroxide according to the volume ratio of 3-4:1, slowly adding the hydrogen peroxide into the concentrated sulfuric acid solution, and stirring at the rotation speed of 50-70r/min in the adding process.

3. The frosting treatment process of claim 1, wherein in the step 2), the carbonyl iron fiber has a diameter of 200-500nm and an aspect ratio of 30-50; the silane coupling agent solution is prepared by uniformly mixing 1 part of KH-550, 1 part of absolute ethyl alcohol and 100-130 parts of deionized water.

4. The frosted glass surface treatment process of claim 1, wherein in the step 2), the components in the slurry are weighed according to the mixture ratio, and the components comprise the following components in percentage by weight: 30-40% carbonyl iron fiber, 40-50% silane coupling agent solution and 10-30% polyethylene glycol aqueous solution.

5. The frosting treatment process of claim 1, wherein in step 2), the pulling method comprises the following steps: and (2) putting the glass into the slurry, dipping for 2-3min, slowly taking out the glass according to the pulling speed of 10-15cm/min, then carrying out heat treatment for 5-8min at the temperature of 80-100 ℃, and repeatedly pulling for 6-10 times to form a base film with the thickness of 1-3um on the surface of the glass.

6. The process of claim 1, wherein in step 3), the atomized mixture powder dispersion is prepared by:

1) respectively taking 20-30 parts of borax, 10-15 parts of silicon powder and 3-5 parts of glass powder, mixing, putting into a ball milling tank, adding 50-80 parts of ethanol and 3-5 parts of 1-3% carboxymethyl cellulose, mixing and ball milling for 5-6 hours at the rotation speed of 500r/min, wherein the ball-material ratio is 5-8:1, repeatedly settling and washing by using deionized water after ball milling to be neutral, and drying in an oven at 50-60 ℃ to constant weight;

2) pulverizing and grinding the dried product to obtain powder with the average particle size of 10-20um, adding the powder into 80-120 parts of deionized water, oscillating and dispersing for 1-2h under 300-400W ultrasonic wave, and passing through a pressure type atomizer, wherein the pressure of the pressure type atomizer is 10-20 MPa.

7. The process of claim 1, wherein the vaporized octamethylcyclotetrasiloxane and the atomized mixture powder dispersion in step 3) have a flow volume ratio of 6-8: 1.

Technical Field

The invention belongs to the technical field of glass processing, and particularly relates to a frosted treatment process for a glass surface.

Background

The frosted glass is also called as ground glass and dark glass, because of the rough surface, the light rays are diffused, the transmitted light rays are soft and not dazzling, and the frosted glass is projected and not transparent, so that a semitransparent fog face effect is formed, the frosted glass has a hazy aesthetic feeling, is mostly applied to indoor partitions, doors and windows, and is also used for trademarks, artware, decoration and the like.

The prior art for preparing ground glass has three processes: one method is that a special grinding tool such as a grinding wheel is adopted, the grinding wheel rotates at a high speed relative to the glass, the glass is ground after the grinding wheel is contacted with the glass, the smooth surface of the glass is damaged to form frosted glass, the method is flexible to operate, however, the artificial influence factor is large, the strength is not easy to master, uneven frosting is generated, thin glass is not suitable for manual grinding, destructive cracks are easily generated on a glass substrate, the processing environment is severe, glass dust is filled in a processing space, the physical health of an operator is threatened, the processing efficiency is low, and the yield is low; the second process is that hard particles with a certain diameter are sprayed on the surface of glass by utilizing high-pressure air, and the hard particles collide with the surface of the glass to form small pits which are uniformly distributed to generate a frosted effect, but the process cannot prepare steel-treated frosted glass, because a large amount of stress is remained on the surface after the glass is toughened, and the collision of the hard particles can cause the toughened glass to be broken; the third process is to soak the toughened glass in HF-containing special medicinal liquid, the HF corrodes the glass and forms a rugged frosted effect on the surface of the glass, and the process needs to use HF with high toxicity in the production process and has serious pollution to the environment.

In view of the above technical problems, improvements are needed.

Disclosure of Invention

The invention aims to provide a frosting treatment process for a glass surface aiming at the existing problems.

The invention is realized by the following technical scheme:

a frosted treatment process for a glass surface comprises the following specific process steps:

1) hydroxylation treatment of glass surfaces

Putting glass into a container filled with deionized water, treating for 10-20min under 300-400W ultrasonic waves, pouring out the deionized water, respectively treating for 5-10min with 50-70% ethanol and 40-50% acetone through ultrasonic waves respectively at the power of 200-300W, taking out the glass, drying the glass by blowing with nitrogen, putting the glass into a mixed solution filled with sulfuric acid and hydrogen peroxide, heating for 1-2h in a water bath at the temperature of 90-100 ℃, cooling bath liquid to room temperature, washing the glass with the deionized water until filtrate is neutral, and drying the glass by blowing with the nitrogen; the hydroxylation treatment is carried out on the glass surface, and hydroxyl is introduced into the glass surface, so that the subsequent chemical bond and reaction between silicon alkoxide adsorbed on the glass surface and the hydroxyl on the glass surface are facilitated, the formation of Si-O-Si can be promoted, the bond and the density of Si-O-Si are improved, the polycondensation film forming reaction of the silicon alkoxide on the glass surface can be promoted, and a high-coverage, continuous and complete silane film can be obtained;

2) formation of glass surface modified silane films

Adding carbonyl iron fiber into a silane coupling agent solution, adding a 3-5% polyethylene glycol aqueous solution by mass, stirring for 2-3h at 500r/min under 300-; the method comprises the following steps of (1) utilizing a polyethylene glycol aqueous solution as a dispersing agent, utilizing silanol in a silane coupling agent to have a good adsorption effect, introducing silanol groups on the surfaces of carbonyl iron fibers through mixing and ball milling, and forming Si-O-Si through chemical bonding and reaction between the silanol groups and hydroxyl on the surfaces of glass, so that a silane film embedded with the carbonyl iron fibers is formed on the surfaces of the glass;

3) preparation of glass surface coatings

Putting the hydroxylated glass into a low-temperature plasma reaction cavity, mixing the gasified octamethylcyclotetrasiloxane and the atomized mixture powder dispersion liquid, introducing the mixture into the plasma reaction cavity, and controlling the flow rate of the gasified octamethylcyclotetrasiloxane to be 2 x 10^-6-5×10^-6ml/min.cm²Setting the vacuum degree in the reaction cavity at 15-25Pa, controlling the plasma discharge power at 200-plus-one (300W), continuously discharging for 20-30min, taking out the glass, drying at 50-60 ℃ for 3-4h, taking out, putting into a heating furnace, heating to 350-plus-one (400 ℃), preserving heat for 10-15min, heating to 500-plus-one (600 ℃), continuing preserving heat for 10-20min, taking out, and naturally cooling to room temperature; after plasma treatment, C = O bonds in carbonyl iron fibers embedded in a silane film on the surface of the glass are broken to form oxygen radicals, meanwhile, partial C-Si bonds in the octamethylcyclotetrasiloxane are broken under the action of plasma, Si-containing free radical parts formed after breaking can be combined with the oxygen radicals formed on the surface of the glass to form Si-O bonds, the octamethylcyclotetrasiloxane can be initiated to be polymerized by itself, and formed polymers and the C-containing free radical bonds formed by C = O breaking on the surface of the glass are formedCombining to form Si-O-C bonds, thereby stably depositing on the glass surface, wherein with the deposition of octamethylcyclotetrasiloxane on the glass surface, the mixture powder carried by octamethylcyclotetrasiloxane can be uniformly bonded on a silane film on the glass surface to form a coating, then the borax in the coating can be fully converted to form boron trioxide with low melting point through a section of low-temperature heat treatment, and then the boron trioxide can be promoted to volatilize through a section of high-temperature heat treatment, so that a large number of pores are formed in the coating, the coating is internally in a loose porous structure, meanwhile, silicon in the coating reacts with oxygen at high temperature to generate silicon dioxide, a compact silicon dioxide film is formed on the surface of the coating, so that the coating is externally in a compact structure, and the interface of the external coating and the internal coating has no layering and cracking phenomena, so that the glass surface presents a gradient porous structure with a compact external layer and a porous internal layer, not only can realize the dull polish effect on glass surface, closely knit outer layer structure is unfavorable for the adnexed of dust moreover for glass easily washs, and the glass powder that contains in the coating then can improve the plumpness of coating simultaneously, is favorable to improving the smoothness of coating.

Preferably, in the step 1), the preparation method of the mixed solution of sulfuric acid and hydrogen peroxide is as follows: respectively taking 80-90% concentrated sulfuric acid and 30-35% hydrogen peroxide according to the volume ratio of 3-4:1, slowly adding the hydrogen peroxide into the concentrated sulfuric acid solution, and stirring at the rotation speed of 50-70r/min in the adding process.

Preferably, the frosted glass surface treatment process comprises the step 2), wherein the carbonyl iron fiber has the diameter of 200-500nm and the length-diameter ratio of 30-50; the silane coupling agent solution is prepared by uniformly mixing 1 part of KH-550, 1 part of absolute ethyl alcohol and 100-130 parts of deionized water.

Preferably, in the step 2), the components in the slurry are weighed according to the mixture ratio, and the components comprise the following components in percentage by weight: 30-40% carbonyl iron fiber, 40-50% silane coupling agent solution and 10-30% polyethylene glycol aqueous solution.

Preferably, the glass surface frosting treatment process comprises the following step 2), wherein the pulling method comprises the following steps: and (2) putting the glass into the slurry, dipping for 2-3min, slowly taking out the glass according to the pulling speed of 10-15cm/min, then carrying out heat treatment for 5-8min at the temperature of 80-100 ℃, and repeatedly pulling for 6-10 times to form a base film with the thickness of 1-3um on the surface of the glass.

Preferably, the frosting treatment process for the glass surface, wherein in the step 3), the atomized mixture powder dispersion is prepared by the following method:

1) respectively taking 20-30 parts of borax, 10-15 parts of silicon powder and 3-5 parts of glass powder, mixing, putting into a ball milling tank, adding 50-80 parts of ethanol and 3-5 parts of 1-3% carboxymethyl cellulose, mixing and ball milling for 5-6 hours at the rotation speed of 500r/min, wherein the ball-material ratio is 5-8:1, repeatedly settling and washing by using deionized water after ball milling to be neutral, and drying in an oven at 50-60 ℃ to constant weight;

2) pulverizing and grinding the dried product to obtain powder with the average particle size of 10-20um, adding the powder into 80-120 parts of deionized water, oscillating and dispersing for 1-2h under 300-400W ultrasonic wave, and passing through a pressure type atomizer, wherein the pressure of the pressure type atomizer is 10-20 MPa.

Preferably, the flow volume ratio of the gasified octamethylcyclotetrasiloxane to the atomized mixture powder dispersion in the step 3) is 6-8: 1.

Compared with the prior art, the invention has the following advantages:

according to the frosting treatment process for the glass surface, provided by the invention, a layer of continuous and complete silane basement membrane is formed on the glass surface, then the gasified octamethylcyclotetrasiloxane is used as carrying gas, under the action of plasma, the octamethylcyclotetrasiloxane can be stably deposited on the glass surface, so that the mixture powder carried in the gasified octamethylcyclotetrasiloxane can be uniformly deposited and distributed on the silane membrane on the glass surface, and a gradient porous structure coating with a compact outer layer and a porous inner layer is formed on the silane membrane surface through heat treatment, so that the glass surface has a good frosting effect, high smoothness, better sight blocking performance, convenience in later-stage cleaning and wide application prospect.

Detailed Description

The present invention will be further described with reference to specific embodiments.