CN114280700B - Anti-reflection anti-fog lens and preparation method and application thereof - Google Patents
Anti-reflection anti-fog lens and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an anti-reflection anti-fog lens and a preparation method and application thereof, wherein the method comprises the following steps: evaporation coating of MgF on glass lens 2 Material of forming MgF 2 An anti-reflection film; at MgF 2 Plating Al on the surface of the anti-reflection film 2 O 3 Material of forming Al 2 O 3 An anti-reflection film; in Al 2 O 3 SiO plated on the surface of the anti-reflection film 2 Material of forming SiO 2 An anti-reflection film; to SiO on the glass lens 2 After the anti-reflection film is subjected to plasma activation treatment, the SiO film is subjected to plasma activation treatment 2 Coating a composite hydrophilic antifogging liquid on the surface of the antireflection film and curing to obtain the antireflection antifogging lens, wherein the composite hydrophilic antifogging liquid mainly comprises sulfonic group modified polyvinyl alcohol-SiO 2 And (3) nano coating. In the invention, the nano-particles in the antifogging liquid are self-assembled with activated SiO on the surface of the lens 2 The hydroxyl on the surface of the antireflection film is subjected to condensation reaction to form a firm silicon hydroxyl bond, so that the antifogging layer is bonded on the SiO in a chemical bond manner 2 The anti-reflection film surface ensures that the anti-reflection anti-fog lens has better long-acting anti-fog capability; and the anti-reflection film is arranged on the anti-reflection anti-fog lens, so that the anti-reflection anti-fog lens has better light transmittance.
Description
Technical Field
The invention relates to the field of antifogging materials, in particular to an anti-reflection antifogging lens and a preparation method and application thereof.
Technical Field
With the improvement of the safety precaution consciousness of people, in addition to installation and monitoring in public places such as supermarkets, shops, urban traffic roads, office buildings and the like, more and more families start installation and monitoring. The monitoring equipment is easy to generate fog on the surface of the lens in a humid environment, especially in northern climates with low temperature and high humidity. If various types of monitoring are fogged, monitoring is fuzzy, and quality is seriously affected. The reason is that the temperature of the place where the camera is used is low, when the air humidity is high, the infrared lamp and the CCD plate in the camera generate heat when working, and saturated vapor in the air is condensed into fog on the surface of the lens of the camera due to the temperature difference, so that the shot video picture is very fuzzy.
The main antifogging methods at present are super-hydrophilic antifogging and surface heating antifogging. The surface heating antifogging method is characterized in that the temperature of the surface of a base material is higher than the ambient temperature through a loaded heating device, and the method is complex in design, high in cost and energy consumption and only limited to be applied in a few industries such as automobiles. The super-hydrophilic antifogging agent is formed by coating an antifogging agent on the surface of a base material, so that the contact angle of water on the surface of the base material is reduced, and water drops condensed on the surface are quickly spread to form a water film, so that the aim of antifogging is fulfilled. The antifogging agent on the market is mainly of a surfactant type, and the antifogging agent has the defect of short antifogging time because the surfactant is adsorbed on a substrate through physical adsorption, and the antifogging agent gradually runs off along with the increase of a water film and finally loses the antifogging function. Meanwhile, the requirement of the lens of the camera on light transmission is high, and the light transmission can directly influence the quality of imaging quality, so that the light transmittance of the lens is required to be ensured while the excellent antifogging performance of the lens is maintained.
The prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide an anti-reflection anti-fog lens, a preparation method and an application thereof, and aims to solve the problems of short anti-fog time and poor light transmittance of the existing anti-fog lens.
The technical scheme of the invention is as follows:
a preparation method of an anti-reflection antifogging lens comprises the following steps:
providing a glass lens, and evaporating MgF on the glass lens 2 Material of forming MgF 2 An anti-reflection film;
at the MgF 2 Al plating on antireflection film surface 2 O 3 Material of forming Al 2 O 3 An anti-reflection film;
in the presence of the Al 2 O 3 Anti-reflection film watchSurface-plated SiO 2 Material of forming SiO 2 An anti-reflection film;
for SiO on the glass lens 2 After the anti-reflection film is subjected to plasma activation treatment, the SiO film is subjected to plasma activation treatment 2 Coating a composite hydrophilic antifogging liquid on the surface of the antireflection film and curing to obtain the antireflection antifogging lens, wherein the composite hydrophilic antifogging liquid mainly comprises sulfo-modified polyvinyl alcohol-SiO 2 。
The preparation method of the anti-reflection antifogging lens comprises the step of evaporating MgF on the glass lens 2 Material of forming MgF 2 The antireflection film comprises the following steps:
sequentially carrying out ultrasonic treatment on the glass lens by using a sodium hydroxide solution, ethanol and pure water, and then cleaning and drying for later use;
MgF is evaporated by vacuum evaporation 2 The vacuum degree of a vacuum chamber of a film plating machine is controlled to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, and adjusting the film forming rate to be 1-3nm/s by controlling the current of the electron beam to prepare MgF with the film thickness of 100-200nm 2 And (4) an anti-reflection film.
The preparation method of the anti-reflection antifogging lens is characterized in that the MgF 2 Plating Al on the surface of the anti-reflection film 2 O 3 Material of forming Al 2 O 3 The antireflection film comprises the following steps:
coating by adopting a vacuum magnetron sputtering mode, taking an Al target as a sputtering source, taking argon and oxygen as working gases, wherein the oxygen accounts for 30-60 percent;
controlling the vacuum degree of a vacuum chamber of a film plating machine to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, the sputtering pressure to be 1-5Pa and the sputtering power to be 50-200W, and preparing the Al with the film thickness of 10-100nm 2 O 3 And (4) an anti-reflection film.
The preparation method of the anti-reflection antifogging lens comprises the step of preparing Al 2 O 3 SiO plated surface of antireflection film 2 Material of forming SiO 2 The antireflection film comprises the following steps:
coating by adopting a vacuum magnetron sputtering mode, taking a Si target as a sputtering source, taking argon and oxygen as working gases, wherein the oxygen accounts for 30-60 percent;
controlling the vacuum degree of a vacuum chamber of a film plating machine to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, the sputtering pressure to be 1-5Pa and the sputtering power to be 50-200W to prepare SiO with the film thickness of 80-200nm 2 And (4) an anti-reflection film.
The preparation method of the anti-reflection antifogging lens comprises the step of coating SiO on the glass lens 2 In the step of performing plasma activation treatment on the antireflection film, a radio frequency power supply is adopted as equipment for the plasma activation treatment, the power of the plasma activation treatment is 600-1000W, the background vacuum degree of a vacuum plasma box is 10-35 Pa, the ratio of introduced oxygen to argon is 1: 0.5-1.2, the flow rate of the oxygen to the argon is 180-300SCCM, and the time of the plasma activation treatment is 180-600 seconds.
The preparation method of the anti-reflection antifogging lens comprises the following steps of:
adding gamma-mercaptopropyl trimethoxy silane and nano-silica sol into a polyvinyl alcohol aqueous solution, and stirring at a preset temperature to obtain a mixed solution;
adding hydrogen peroxide into the mixed solution and stirring to obtain sulfonated polyvinyl alcohol-SiO 2 Compounding hydrophilic silica sol;
to the sulfonated polyvinyl alcohol-SiO 2 And adding a dispersing agent, a film forming agent, a diluent and sodium dodecyl sulfate into the composite hydrophilic silica sol, and stirring to obtain the composite hydrophilic antifogging solution.
The preparation method of the anti-reflection antifogging lens comprises the following steps of:
dissolving 20 parts by weight of polyvinyl alcohol into 100 parts by weight of hot water at the temperature of 60-100 ℃ to obtain a polyvinyl alcohol solution;
adding 5-15 parts of gamma-mercaptopropyl-trimethoxysilane and 10-40 parts of nano-silica sol into the polyvinyl alcohol aqueous solution, and stirring for 1-24 hours at 75-100 ℃ to obtain a mixed solution;
adding 5-15 parts of hydrogen peroxide into the mixed solution, and stirring for 1-24 hours to obtainSulfonated polyvinyl alcohol-SiO 2 Compounding hydrophilic silica sol;
to 100 parts of sulfonated polyvinyl alcohol-SiO 2 And adding 1-5 parts of dispersing agent, 1-5 parts of film forming agent, 30-50 parts of diluent and 1-5 parts of sodium dodecyl sulfate into the composite hydrophilic silica sol, and stirring for 1-10 hours to obtain the composite hydrophilic antifogging solution.
The preparation method of the anti-reflection and anti-fog lens comprises the steps of preparing a dispersing agent, a film forming agent and a diluent, wherein the dispersing agent is hydroxyethyl cellulose, the film forming agent is propylene glycol monobutyl ether, and the diluent is isopropanol.
An anti-reflection antifogging lens is prepared by the preparation method of the anti-reflection antifogging lens.
The application of the anti-reflection anti-fog lens is characterized in that the anti-reflection anti-fog lens prepared by the preparation method is used for preparing an anti-fog camera.
Has the beneficial effects that: the invention provides a preparation method of an anti-reflection antifogging lens, which comprises the steps of firstly preparing MgF on a glass lens in sequence 2 Antireflection film, al 2 O 3 Antireflection film and SiO 2 The anti-reflection film ensures that the glass lens has better light transmittance; then SiO on the glass lens 2 Carrying out plasma activation treatment on the anti-reflection film; finally in activated SiO 2 Coating a composite hydrophilic anti-fogging liquid on the surface of the anti-reflection film and curing to form an anti-fogging layer, wherein the main component of the composite hydrophilic anti-fogging liquid is sulfo-group-modified polyvinyl alcohol-SiO 2 . In the present invention, the SiO 2 After the antireflection film is subjected to plasma activation treatment, hydroxyl on the surface of the antireflection film is activated, and the reaction activity is higher; after coating the composite hydrophilic antifogging fluid, the nano-particles (comprising sulfonic acid group modified polyvinyl alcohol-SiO) 2 And SiO not completely participating in the reaction 2 Particles) on the lens surface by self-assembly with plasma activated SiO 2 The hydroxyl on the surface of the antireflection film is subjected to condensation reaction to form a firm silicon hydroxyl bond, so that the sulfonic group modified polyvinyl alcohol-SiO 2 Chemically bonded to SiO 2 The anti-reflection film surface ensures that the prepared anti-reflection antifogging lens has better long-acting antifogging capability.
Drawings
Fig. 1 is a flow chart of a preparation method of an anti-reflection anti-fog lens provided by the invention.
Fig. 2 is a schematic structural diagram of an anti-reflection anti-fog lens prepared by the invention.
Detailed Description
The invention provides an anti-reflection anti-fog lens and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The existing antifogging lens is usually coated with an antifogging agent on the surface of the lens, so that the contact angle of water on the surface of the lens is reduced, water drops condensed on the surface are quickly spread to form a water film, and the aim of preventing fog is fulfilled. However, the antifogging agent in the market is mainly of a surfactant type, and the antifogging agent has the defect of short antifogging time because the surfactant is adsorbed on a substrate through physical adsorption, and the antifogging agent gradually runs off along with the increase of a water film and finally loses an antifogging function; and the light transmission of the existing antifogging lens is also poor.
Based on this, the invention provides a preparation method of an anti-reflection anti-fog lens, as shown in fig. 1, which comprises the following steps:
s10, providing a glass lens, and evaporating MgF on the glass lens 2 Material of forming MgF 2 An anti-reflection film;
s20, in the MgF 2 Al plating on antireflection film surface 2 O 3 Material of forming Al 2 O 3 An anti-reflection film;
s30 in the above-mentioned Al 2 O 3 SiO plated on the surface of the anti-reflection film 2 Material of forming SiO 2 An anti-reflection film;
s40, for SiO on the glass lens 2 After the anti-reflection film is subjected to plasma activation treatment, the SiO film is subjected to plasma activation treatment 2 Coating a composite hydrophilic antifogging liquid on the surface of the antireflection film and curing to obtain the antireflection antifogging lens, wherein the composite hydrophilic antifogging liquid mainly comprises sulfonic group modified polyvinyl alcohol-SiO 2 。
The invention firstly prepares MgF on a glass lens in turn 2 Antireflection film, al 2 O 3 Antireflection film and SiO 2 The anti-reflection film ensures that the glass lens has better light transmittance; then SiO on the glass lens 2 Carrying out plasma activation treatment on the anti-reflection film; finally in activated SiO 2 Coating a composite hydrophilic antifogging liquid on the surface of the antireflection film and curing to form an antifogging layer to prepare the antireflection antifogging lens, wherein the composite hydrophilic antifogging liquid mainly comprises sulfonic group modified polyvinyl alcohol-SiO 2 . In the present invention, the SiO 2 After the anti-reflection film is subjected to plasma activation treatment, hydroxyl on the surface of the anti-reflection film is activated, and the reaction activity is higher; after the composite hydrophilic antifogging liquid is coated, the nano particles in the antifogging liquid are self-assembled with activated SiO on the surface of the lens 2 The hydroxyl on the surface of the antireflection film is subjected to condensation reaction to form firm silicon hydroxyl bonds, so that the antifogging layer is bonded on the SiO in a chemical bond mode 2 The anti-reflection film surface enables the prepared anti-reflection antifogging lens to have good long-acting antifogging capability.
In the invention, if a single-layer antireflection film is arranged, the frequency-width ratio of the prepared antireflection antifogging lens is smaller, and in order to enable the antireflection antifogging lens to be used in a wider light-transmitting wave band and have higher transmissivity, mgF is sequentially prepared on the glass lens 2 Antireflection film, al 2 O 3 Antireflection film and SiO 2 The antireflection film comprises three layers of antireflection films, and the light transmission effect can be further enhanced by adopting the alternative design of low-refractive-index films and high-refractive-index films.
In some embodiments, mgF is evaporated on the glass lens 2 Material of forming MgF 2 The antireflection film comprises the following steps: sequentially carrying out ultrasonic treatment on the glass lens by using a sodium hydroxide solution, ethanol and pure water, and then cleaning and drying for later use; mgF is evaporated by vacuum evaporation 2 The vacuum degree of a vacuum chamber of a film plating machine is controlled to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, and adjusting the film forming rate to be 1-3nm/s by controlling the current of the electron beam to obtain MgF with the film thickness of 100-200nm 2 Antireflection film。
In the implementation, after light enters the antireflection film, the light is reflected on two surfaces of the film, and the light reflected on the back can be interfered with the light reflected on the front surface film only after passing through the thicknesses of the two antireflection films. And the optical wave is weakened as much as possible, the wave path difference is equal to odd times of 1/2 wavelength, and the antireflection film is made to be thinnest, so that the thickness of 2 times of the antireflection film is equal to 1/2 wavelength, and the thickness of the antireflection film is equal to 1/4 wavelength. The film thickness below or above the above range greatly increases the reflection loss of light and reduces the intensity of transmitted light, so that the embodiment selects to prepare MgF of 100-200nm 2 And (4) an anti-reflection film. Preferably MgF 2 The thickness of the antireflection film is 100-120nm.
In some embodiments, the MgF is present in the composition 2 Plating Al on the surface of the anti-reflection film 2 O 3 Material of forming Al 2 O 3 The antireflection film comprises the following steps: coating by adopting a vacuum magnetron sputtering mode, taking an Al target as a sputtering source, taking argon and oxygen as working gases, wherein the oxygen accounts for 30-60 percent; controlling the vacuum degree of a vacuum chamber of a film plating machine to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, the sputtering pressure to be 1-5Pa and the sputtering power to be 50-200W, and preparing the Al with the film thickness of 10-100nm 2 O 3 And (3) an anti-reflection film. Preferably Al 2 O 3 The thickness of the antireflection film is 90-100nm.
In some embodiments, the Al is in the alloy 2 O 3 SiO plated on the surface of the anti-reflection film 2 Material of forming SiO 2 The antireflection film comprises the following steps: coating by adopting a vacuum magnetron sputtering mode, taking a Si target as a sputtering source, taking argon and oxygen as working gases, wherein the oxygen accounts for 30-60 percent; controlling the vacuum degree of a vacuum chamber of a film plating machine to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, the sputtering pressure to be 1-5Pa and the sputtering power to be 50-200W to prepare SiO with the film thickness of 80-200nm 2 And (4) an anti-reflection film. SiO is preferred 2 The thickness of the antireflection film is 100-130nm.
In some embodiments, the SiO on the glass lens 2 In the step of performing plasma activation treatment on the antireflection film, a radio frequency power supply is required to be adopted as equipment for the plasma activation treatment,the plasma activating treatment power is 600-1000W, the background vacuum degree of the vacuum plasma box is 10Pa-35Pa, the ratio of the introduced oxygen to the introduced argon is 1: 0.5-1.2, the flow rate of the oxygen and the argon is 180-300SCCM, and the plasma activating treatment time is 180-600 seconds. This example is carried out by subjecting SiO 2 The anti-reflection film is subjected to plasma activation treatment, so that hydroxyl on the surface of the anti-reflection film is activated, the reaction activity is higher, condensation reaction is convenient to occur between the anti-reflection film and hydroxyl in the composite hydrophilic anti-fog liquid, and the anti-fog layer is combined on SiO in a chemical bond mode 2 The anti-reflection film surface enables the prepared anti-reflection antifogging lens to have good long-acting antifogging capability.
In some embodiments, the preparation of the composite hydrophilic antifogging fluid comprises the steps of: adding gamma-mercaptopropyl trimethoxy silane and nano-silica sol into a polyvinyl alcohol aqueous solution, and stirring at a preset temperature to obtain a mixed solution; adding hydrogen peroxide into the mixed solution and stirring to obtain sulfonated polyvinyl alcohol-SiO 2 Compounding hydrophilic silica sol; to the sulfonated polyvinyl alcohol-SiO 2 And adding a dispersing agent, a film forming agent, a diluent and sodium dodecyl sulfate into the composite hydrophilic silica sol, and stirring to obtain the composite hydrophilic antifogging solution.
In some specific embodiments, the preparation of the composite hydrophilic antifogging fluid specifically comprises the steps of: dissolving 20 parts by weight of polyvinyl alcohol into 100 parts by weight of hot water at the temperature of 60-100 ℃ to obtain a polyvinyl alcohol solution; adding 5-15 parts of gamma-mercaptopropyl-trimethoxysilane and 10-40 parts of nano-silica sol into the polyvinyl alcohol aqueous solution, and stirring for 1-24 hours at 75-100 ℃ to obtain a mixed solution; adding 5-15 parts of hydrogen peroxide into the mixed solution, and stirring for 1-24 hours to obtain sulfonated polyvinyl alcohol-SiO 2 Compounding hydrophilic silica sol; to 100 parts of sulfonated polyvinyl alcohol-SiO 2 And adding 1-5 parts of dispersing agent, 1-5 parts of film forming agent, 30-50 parts of diluent and 1-5 parts of sodium dodecyl sulfate into the composite hydrophilic silica sol, and stirring for 1-10 hours to obtain the composite hydrophilic antifogging solution.
The main component of the composite hydrophilic antifogging fluid prepared in the embodiment is polyvinyl alcohol-SiO modified by sulfonic acid group 2 The toolHas better hydrophilic ability and can be mixed with SiO 2 The active hydroxyl on the surface of the antireflection film is subjected to condensation reaction, so that the antifogging layer is stably combined on the SiO in a chemical bond mode 2 The anti-reflection film surface enables the prepared anti-reflection antifogging lens to have good long-acting antifogging capability. By way of example, the dispersant is hydroxyethyl cellulose, the film former is propylene glycol butyl ether, and the diluent is isopropyl alcohol.
In some embodiments, an anti-reflection anti-fog lens is also provided, which is prepared by the preparation method of the anti-reflection anti-fog lens. As shown in figure 2, the anti-reflection anti-fog lens prepared by the invention comprises a glass lens 1 and MgF sequentially prepared on the surface of the glass lens 1 2 Antireflection film 2, al 2 O 3 Antireflection film 3, siO 2 The anti-reflection film 4 and the anti-fog layer 5, wherein the anti-fog layer 5 is formed by solidifying a composite hydrophilic anti-fog liquid, and the main component of the composite hydrophilic anti-fog liquid is sulfonic group modified polyvinyl alcohol-SiO 2 The sulfonic acid group-modified polyvinyl alcohol-SiO 2 With SiO 2 The activated hydroxyl groups in antireflection film 4 are bonded by chemical bonds.
The anti-reflection and anti-fog lens provided by the embodiment is provided with MgF 2 Antireflection film, al 2 O 3 Antireflection film and SiO 2 The anti-reflection film ensures that the anti-reflection antifogging lens has better light transmittance, and the SiO film is used for preventing the fog from being formed 2 The surface of the antireflection film is also connected with high-hydrophilic sulfonic group modified polyvinyl alcohol-SiO through chemical bonds 2 So that the anti-reflection anti-fog lens has long-acting anti-fog capability.
In some embodiments, the anti-reflection anti-fog lens prepared by the preparation method is used for preparing an anti-fog camera. The anti-reflection anti-fog lens prepared by the invention has the characteristics of low refractive index and anti-reflection, and SiO on the outermost layer 2 After being activated, the anti-reflection film layer can be firmly combined with the anti-fog film in a chemical bond mode, so that the coating has the characteristics of water resistance, wear resistance and long service life, and therefore, the anti-reflection anti-fog lens can be used for preparing an anti-fog camera, and a clear visual field can be obtained.
The invention is further illustrated by the following specific examples:
example 1
A preparation method of an antifogging anti-reflection lens comprises the following steps:
step 1: degreasing the glass sheet by using 10% alkali liquor, cleaning, and removing oil in N 2 Drying in the atmosphere;
step 2: mgF 2 The anti-reflection film is coated by vacuum evaporation, and the vacuum degree of a vacuum chamber of a coating machine is controlled at 10 -4 Pa, the temperature of the glass lens is 180 ℃, and the film forming rate is adjusted to be 2nm/s and MgF by controlling the current of the electron beam 2 The film thickness is 150nm;
and step 3: al (Al) 2 O 3 The anti-reflection film is coated by adopting a vacuum magnetron sputtering mode, an Al target material is taken as a sputtering source, argon and oxygen are taken as working gases, the oxygen accounts for 50 percent, and the vacuum degree of a vacuum chamber of a coating machine is controlled to be 10 -4 Pa, the temperature of the glass lens is 180 ℃, the sputtering pressure is 3Pa, the sputtering power is 160W 2 O 3 The film thickness is 70nm;
and 4, step 4: siO2 2 The anti-reflection film is coated by adopting a vacuum magnetron sputtering mode, a Si target material is taken as a sputtering source, argon and oxygen are taken as working gases, the oxygen accounts for 50 percent, and the vacuum degree of a vacuum chamber of a coating machine is controlled to be 10 -4 Pa, the temperature of the glass lens is 180 ℃, the sputtering pressure is 3Pa, the sputtering power is 160W 2 The film thickness is 120nm;
and 5: preparing an antifogging liquid: according to the weight, 20 parts of polyvinyl alcohol (with the polymerization degree of 1000) is dissolved by 100 parts of hot water at 80 ℃, 10 parts of gamma-mercaptopropyltrimethoxysilane and 25 parts of nano silica sol (with the particle size of 40 nm) are added, the mixture is stirred for 10 hours at 85 ℃, 10 parts of 20% hydrogen peroxide is added, and the mixture is stirred for 10 hours to obtain the sulfonated polyvinyl alcohol-SiO 2 composite hydrophilic silica sol. Finally, adding 3 parts of hydroxyethyl cellulose serving as a dispersing agent, 3 parts of propylene glycol butyl ether serving as a film forming agent, 3 parts of sodium dodecyl sulfate serving as a surfactant and 40 parts of isopropanol serving as a diluent into 100 parts of sulfonated polyvinyl alcohol-SiO 2 composite hydrophilic silica sol, and continuously stirring for 5 hours to obtain an antifogging solution (sulfonic group modified polyvinyl alcohol-SiO 2 composite hydrophilic antifogging solution);
step 6: carrying out plasma activation treatment on the coated anti-reflection glass, wherein a radio frequency power supply is adopted by plasma activation equipment, the plasma treatment power is 800W, the background vacuum degree of a vacuum plasma box is 25Pa, the ratio of introduced oxygen to argon is 1: 1.0, the flow rate of mixed gas is 230SCCM, and the treatment time of plasma activation is 400 seconds;
and 7: and coating hydrophilic antifogging liquid on the surface of the anti-reflection glass in a spin coating manner, and curing and reacting for 5 hours at 150 ℃ to obtain the anti-reflection antifogging lens.
Example 2
A preparation method of an antifogging anti-reflection lens comprises the following steps:
step 1: deoiling the glass sheet with 5% alkali solution, cleaning, and washing in N 2 Drying in the atmosphere;
and 2, step: mgF 2 The anti-reflection film is coated by vacuum evaporation, and the vacuum degree of a vacuum chamber of a coating machine is controlled at 10 -3 Pa, the temperature of the glass lens is 150 ℃, and the film forming rate is adjusted to be 1nm/s and MgF by controlling the current of the electron beam 2 The film thickness is 100nm;
and 3, step 3: al (Al) 2 O 3 The anti-reflection film is coated by adopting a vacuum magnetron sputtering mode, an Al target material is taken as a sputtering source, argon and oxygen are taken as working gases, the oxygen accounts for 30 percent, and the vacuum degree of a vacuum chamber of a coating machine is controlled to be 10 -3 Pa, the temperature of the glass lens is 150 ℃, the sputtering pressure is 1Pa, the sputtering power is 50W 2 O 3 The film thickness is 40nm;
and 4, step 4: siO2 2 The anti-reflection film is coated by adopting a vacuum magnetron sputtering mode, a Si target material is taken as a sputtering source, argon and oxygen are taken as working gases, the oxygen accounts for 30 percent, and the vacuum degree of a vacuum chamber of a coating machine is controlled to be 10 -3 Pa, the temperature of the glass lens is 150 ℃, the sputtering pressure is 1Pa, the sputtering power is 50W 2 The film thickness is 80nm;
and 5: preparing an antifogging liquid: according to the weight, 20 parts of polyvinyl alcohol (with the polymerization degree of 300) is dissolved by 100 parts of 60 ℃ hot water, 5 parts of gamma-mercaptopropyltrimethoxysilane and 10 parts of nano silica sol (with the particle size of 10 nm) are added, the mixture is stirred for 1 hour at the temperature of 75 ℃, and 5 parts of 20% hydrogen peroxide is added and stirred for 1 hour to obtain the sulfonated polyvinyl alcohol-SiO 2 composite hydrophilic silica sol. Finally, adding 1 part of hydroxyethyl cellulose serving as a dispersing agent, 1 part of propylene glycol butyl ether serving as a film forming agent, 1 part of sodium dodecyl sulfate serving as a surfactant and 30 parts of isopropanol serving as a diluent into 100 parts of sulfonated polyvinyl alcohol-SiO 2 composite hydrophilic silica sol, and continuously stirring for 1 hour to obtain an antifogging solution (sulfonic group modified polyvinyl alcohol-SiO 2 composite hydrophilic antifogging solution);
step 6: carrying out plasma activation treatment on the coated anti-reflection glass, wherein a radio frequency power supply is adopted by plasma activation equipment, the plasma treatment power is 600W, the background vacuum degree of a vacuum plasma box is 10Pa, the ratio of introduced oxygen to argon is 1: 0.5, the flow rate of mixed gas is 180SCCM, and the treatment time of plasma activation is 180 seconds;
and 7: and coating hydrophilic antifogging liquid on the surface of the anti-reflection glass in a spin coating manner, and curing and reacting for 1h at 100 ℃ to obtain the anti-reflection antifogging lens.
Example 3
A preparation method of an antifogging anti-reflection lens comprises the following steps:
step 1: degreasing the glass sheet by using 20% alkali liquor, cleaning, and removing oil in N 2 Drying in the atmosphere;
step 2: mgF 2 The anti-reflection film is coated by vacuum evaporation, and the vacuum degree of a vacuum chamber of a coating machine is controlled at 10 -5 Pa, the temperature of the glass lens is 200 ℃, and the film forming speed is adjusted to be 3nm/s and MgF by controlling the current of the electron beam 2 The film thickness is 200nm;
and step 3: al (Al) 2 O 3 The anti-reflection film is coated by adopting a vacuum magnetron sputtering mode, an Al target material is taken as a sputtering source, argon and oxygen are taken as working gases, the oxygen accounts for 60 percent, and the vacuum degree of a vacuum chamber of a coating machine is controlled to be 10 -5 Pa, the temperature of the glass lens is 200 ℃, the sputtering pressure is 5Pa, the sputtering power is 200W 2 O 3 The film thickness is 100nm;
and 4, step 4: siO2 2 The anti-reflection film is coated by adopting a vacuum magnetron sputtering mode, a Si target material is taken as a sputtering source, argon and oxygen are taken as working gases, the oxygen accounts for 60 percent, and the vacuum degree of a vacuum chamber of a coating machine is controlled to be 10 -5 Pa, the temperature of the glass lens is 200 ℃, the sputtering pressure is 5Pa, the sputtering power is 200W 2 The film thickness is 200nm;
and 5: preparing an antifogging liquid: according to weight, 20 parts of polyvinyl alcohol (with the polymerization degree of 2000) is dissolved by 100 parts of hot water at 100 ℃, 15 parts of gamma-mercaptopropyltrimethoxysilane and 40 parts of nano silica sol (with the particle size of 60 nm) are added, stirring is carried out for 24 hours at 100 ℃, 15 parts of 20% hydrogen peroxide is added, and stirring is carried out for 24 hours, so that sulfonated polyvinyl alcohol-SiO 2 composite hydrophilic silica sol is obtained. Finally, adding 5 parts of dispersant hydroxyethyl cellulose, 5 parts of film-forming agent propylene glycol butyl ether, 5 parts of surfactant sodium dodecyl sulfate and 50 parts of diluent isopropanol into 100 parts of sulfonated polyvinyl alcohol-SiO 2 composite hydrophilic silica sol, and continuously stirring for 10 hours to obtain an antifogging liquid (sulfonic group modified polyvinyl alcohol-SiO 2 composite hydrophilic antifogging liquid);
and 6: performing plasma activation treatment on the coated anti-reflection glass, wherein a radio frequency power supply is adopted by plasma activation equipment, the plasma treatment power is 1000W, the background vacuum degree of a vacuum plasma box is 35Pa, the ratio of introduced oxygen to argon is 1: 1.2, the flow rate of mixed gas is 300SCCM, and the treatment time of plasma activation is 600 seconds;
and 7: and coating hydrophilic antifogging liquid on the surface of the anti-reflection glass in a spin coating manner, and curing and reacting for 24 hours at 200 ℃ to obtain the anti-reflection antifogging lens.
Example 4
The performance of the anti-reflection antifogging lens prepared in example 1 was tested:
1. contact angle test: and measuring the contact angle of a water drop on the anti-fog layer of the anti-reflection anti-fog lens by using a GB/T30447-2013 method.
2. And (3) testing antifogging performance: and (3) placing the anti-reflection antifogging lens above saturated water vapor at 85 ℃, and ensuring that the anti-reflection antifogging lens does not fog for 30 seconds continuously, so that the anti-fog is qualified.
3. And (3) testing light transmittance: the method for measuring the light transmittance and the haze of the transparent plastic is GB/T2410-2008, and the light transmittance of the anti-reflection antifogging lens in a visible light wave band (380-780 nm) is measured by a spectrophotometer.
4. And (3) testing water resistance: at normal temperature, the anti-reflection antifogging lens is immersed in normal-temperature chlorine water (0.1% concentration sodium dichloroisocyanurate pure water solution) with the effective chlorine content of 0.4 per mill for 12 hours, and the antifogging property is unchanged, so that the antifogging property is qualified.
5. And (3) hardness testing: the hardness of the anti-reflection and anti-fog lens is measured by a GB6739-1996 film coating pencil measuring method.
The results of the above tests are shown in table 1:
TABLE 1
As can be seen from data in Table 1, the anti-reflection anti-fog lens prepared by the invention has better light transmittance and continuous anti-fog performance.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of an anti-reflection antifogging lens is characterized by comprising the following steps:
providing a glass lens, and evaporating MgF on the glass lens 2 Material of forming MgF 2 An anti-reflection film;
at the MgF 2 Plating Al on the surface of the anti-reflection film 2 O 3 Material of forming Al 2 O 3 An anti-reflection film;
in the Al 2 O 3 SiO plated on the surface of the anti-reflection film 2 Material of forming SiO 2 An anti-reflection film;
for SiO on the glass lens 2 After the anti-reflection film is subjected to plasma activation treatment, the SiO film is subjected to plasma activation treatment 2 Coating a composite hydrophilic antifogging liquid on the surface of the antireflection film and curing to obtain the antireflection antifogging lens, wherein the composite hydrophilic antifogging liquid mainly comprises sulfo-modified polyvinyl alcohol-SiO 2 ；
The preparation method of the composite hydrophilic antifogging solution specifically comprises the following steps:
dissolving 20 parts by weight of polyvinyl alcohol into 100 parts by weight of hot water at the temperature of 60-100 ℃ to obtain a polyvinyl alcohol solution;
adding 5-15 parts of gamma-mercaptopropyl-trimethoxysilane and 10-40 parts of nano-silica sol into the polyvinyl alcohol aqueous solution, and stirring for 1-24 hours at 75-100 ℃ to obtain a mixed solution;
adding 5-15 parts of hydrogen peroxide into the mixed solution, and stirring for 1-24 hours to obtain sulfonated polyvinyl alcohol-SiO 2 Compounding hydrophilic silica sol;
to 100 parts of sulfonated polyvinyl alcohol-SiO 2 And adding 1-5 parts of dispersing agent, 1-5 parts of film forming agent, 30-50 parts of diluent and 1-5 parts of sodium dodecyl sulfate into the composite hydrophilic silica sol, and stirring for 1-10 hours to obtain the composite hydrophilic antifogging solution.
2. The preparation method of the anti-reflection antifogging lens according to claim 1, characterized in that MgF is evaporated on the glass lens 2 Material of forming MgF 2 The antireflection film comprises the following steps:
sequentially carrying out ultrasonic treatment on the glass lens by using a sodium hydroxide solution, ethanol and pure water, and then cleaning and drying for later use;
adopting vacuum evaporation to evaporate MgF 2 The vacuum degree of a vacuum chamber of a film plating machine is controlled to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, and adjusting the film forming rate to be 1-3nm/s by controlling the current of the electron beam to prepare MgF with the film thickness of 100-200nm 2 And (4) an anti-reflection film.
3. The method for preparing the anti-reflection and anti-fog lens as claimed in claim 1, wherein the MgF is coated on the surface of the glass substrate 2 Plating Al on the surface of the anti-reflection film 2 O 3 Material of forming Al 2 O 3 The antireflection film comprises the following steps:
coating by adopting a vacuum magnetron sputtering mode, taking an Al target as a sputtering source, taking argon and oxygen as working gases, wherein the oxygen accounts for 30-60 percent;
controlling the vacuum degree of a vacuum chamber of a film plating machine to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, the sputtering pressure to be 1-5Pa and the sputtering power to be 50-200W, and preparing the Al with the film thickness of 10-100nm 2 O 3 And (4) an anti-reflection film.
4. The method for preparing the anti-reflection and anti-fog lens as claimed in claim 1, wherein Al is added to the glass 2 O 3 SiO plated on the surface of the anti-reflection film 2 Material of forming SiO 2 The antireflection film comprises the following steps:
coating by adopting a vacuum magnetron sputtering mode, taking a Si target as a sputtering source, taking argon and oxygen as working gases, wherein the oxygen accounts for 30-60 percent;
controlling the vacuum degree of a vacuum chamber of a film plating machine to be 10 -3 -10 -5 Pa, controlling the temperature of the glass lens to be 150-200 ℃, the sputtering pressure to be 1-5Pa and the sputtering power to be 50-200W to prepare SiO with the film thickness of 80-200nm 2 And (3) an anti-reflection film.
5. The method for preparing the anti-reflection and anti-fog lens as claimed in claim 1, wherein SiO is coated on the glass lens 2 In the step of carrying out plasma activation treatment on the antireflection film, a radio frequency power supply is adopted for equipment for plasma activation treatment, the power of the plasma activation treatment is 600-1000W, the background vacuum degree of a vacuum plasma box is 10-35 Pa, the ratio of introduced oxygen to argon is 1: 0.5-1.2, the flow rate of the oxygen and the argon is 180-300SCCM, and the time of the plasma activation treatment is 180-600 seconds.
6. The method for preparing the anti-reflection and anti-fog lens as claimed in claim 1, wherein the dispersing agent is hydroxyethyl cellulose, the film forming agent is propylene glycol butyl ether, and the diluent is isopropanol.
7. An anti-reflection antifogging lens, which is characterized by being prepared by the preparation method of the anti-reflection antifogging lens according to any one of claims 1 to 6.
8. The application of the anti-reflection anti-fog lens is characterized in that the anti-reflection anti-fog lens prepared by the preparation method of any one of claims 1 to 6 is used for preparing an anti-fog camera.
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