CN100495123C - Ultrahard antifouling resin eyeglass and method for making same - Google Patents
Ultrahard antifouling resin eyeglass and method for making same Download PDFInfo
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- CN100495123C CN100495123C CNB2005101123936A CN200510112393A CN100495123C CN 100495123 C CN100495123 C CN 100495123C CN B2005101123936 A CNB2005101123936 A CN B2005101123936A CN 200510112393 A CN200510112393 A CN 200510112393A CN 100495123 C CN100495123 C CN 100495123C
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Abstract
The invention relates to super rigid antifouling resin eye glasses and manufacturing method, in particular the super rigid, super lubrication, waterproof, anti-fog, and anti-smeary eye glasses and manufacturing method. The main technical characteristics are that it overcomes the disadvantages of low resisting abrasion of resin eye glasses, adsorbing water and oil pollution easily, and a super rigid film is covered on the resin eye glasses, the super rigid film is produced by adding 5%-13% particles of titania in the hardening solution, additionally, the ion assisting hard coat technics is adopted when producing the multilayer antireflecting films, the multilayer antireflecting films is covered with nm films with super bi-dregging performance, and the multilayer antireflecting films have compactability and gliding property, and stable air films are formed to recuperate the insufficiency of air space of multilayer antireflecting films. The productions in the invention have simple structure, convenient manufacturing technique, and stable performance, and make the production super hard, super lubrication and uneasy to absorb the oil pollution.
Description
Affiliated field
The present invention relates to a kind of manufacturing of lens, the resin eyeglass and the manufacture method thereof of especially a kind of superhard, super lubricated, waterproof, antifog, anti-greasy dirt.
Background technology
Resin eyeglass has at home and abroad obtained widely using, though resin eyeglass is in light weight, can be used for making the glasses of framework or multiple style such as frameless, and it also exists short shortcoming in serviceable life.Its in serviceable life short main cause be resin material after making lens because resin material is as organic material, its material self-characteristic makes the resin eyeglass skin hardness of making lower, so antiwear property is poor.Though, still can cause the lens wearing and tearing in actual use through being coated with the film that resistance to wears, double-layer reflection reducing coating and teleblem on the surface.In addition, in actual use, problems such as water smoke, greasy dirt absorption also can occur, make the people with glasses look the thing sharpness and descend, bring extremely inconvenient to the user.
Goal of the invention
The object of the present invention is to provide the resin lens and the manufacture method thereof of a kind of superhard property, super lubricated, waterproof, antifog, anti-greasy dirt.
Technical scheme
Resin material has ultralight as a kind of thermosets, shock proof characteristics, but its rigid degree is lower, and antifraying force is relatively poor.The inventor is poor in order to overcome the resin eyeglass antifraying force, easily adsorb deficiencies such as water smoke, greasy dirt, the substrate of resin glasses is cooked stiffened handles, and on the outermost top layer of resin eyeglass, be coated with again one deck have ultra-amphosphobic can effectively waterproof, antifog, prevent greasy dirt and rete easy to clean.For reaching the object of the invention, add titanium dioxide fine particles in the hardening liquid that employing is used and reach hardness and the refractive index that abundant quantity improves hardening liquid in the resin eyeglass manufacture process, adopt nanometer technology to be coated with special layers as teleblem at the skin of double-layer reflection reducing coating, and when being coated with double-layer reflection reducing coating, adopt the Ion Aided Film Coating method, thereby improve the quality of the composite film of resin eyeglass comprehensively.
Concrete scheme of the present invention is:
A, stiffened are handled
Concrete steps are as follows:
One, alkali is invaded turbid
Getting one of resin eyeglass substrate puts into aqueous slkali and soaks
Aqueous slkali composition: can adopt the NaOH weight percent concentration to be: 35-37%
Solution temperature: 35-40 ℃
Soak time: 8-10 divides kind
This soaks to strengthen the active coating firmness that increases of resin eyeglass substrate surface.
Two, clean
Taking-up resin eyeglass substrate is put into the tank that contains general detersive (as daily washing powder) and is cleaned
Detersive composition: general detersive
Detersive weight percent concentration: 20-25%
Soaking temperature: 35-40%
Soak time: 120-150S
To remove the residual liquid of resin eyeglass substrate surface NaOH.
Three, softening water, ultrasonic cleaning
The resin eyeglass substrate is put into pure water ultrasonic cleaning after purifying
Softening water conductivity 18m Ω
Temperature: 20-25 ℃
Impurity with thorough removing resin eyeglass substrate surface;
Use anhydrous alcohol, ultrasonic cleaning resin eyeglass substrate again
Alcohol concentration: 99.9%, temperature: 20-25 ℃
To remove resin eyeglass substrate surface moisture content, increase dehydrating effect
Four, dehydration is received and is done
Adopting the IPA dehydration to receive does
Five, stiffened dipping
The resin eyeglass substrate is put into hardening liquid to be flooded
Each main weight percent concentration of hardening liquid:
Dioxane 18%
T-butanols 30%
Polysiloxane 12%
Methyl alcohol 22-30%
Other are 5% years old
Hardening liquid proportion proportion under 10 ℃ temperature is: 1.010～1.030
Hardening liquid temperature: 10-12 ℃
TiO in the hardening liquid
2Weight percent concentration: 5-13%
The relative humidity of stiffened groove: 40-45%
Dip time: 35-40S
So that hardening liquid adheres to the resin eyeglass substrate surface
Six, the lifting of resin eyeglass substrate
The resin eyeglass substrate stopped in hardening liquid do behind the 35-40S at the uniform velocity to promote
At the uniform velocity speed: 6-8mm/s makes hardening liquid form the uniform rete of thickness at the resin eyeglass substrate surface
Seven, precuring
The resin eyeglass substrate is put into baking oven precuring
Precuring temperature: 65-70 ℃
Precuring time: 15-18 minute
Eight, heat curing
The resin eyeglass substrate is put into baking oven to be toasted
Temperature: 115-120 ℃
Time: 3 hours
Above-mentioned steps is the processing overall process of finished product stiffened resin eyeglass.In order further to improve the quality of resin eyeglass, cater to the consumption requirement, can in hardening liquid, add TiO
2Particulate matter, and make it to have refractive index and the hardness that abundant quantity is used for improving hardening liquid.Its ultimate principle is: choose one or more cooperations from the raw silicon compound, hydrolysis generates silanol, makes several molecule condensations form oligomer simultaneously.The terminal silanol of oligomer combines with alcohol in hardening liquid again, by heat curing, remove alcohol carry out crosslinked, by adjuvant, as TiO
2, acrylic acid etc., improve hardening liquid refractive index and hardness, guarantee the performance of hardening liquid and the rerum natura of cured film.Our hard technology that adds of employing is the membrane technology that resistance to wore in the 4th generation at present, owing to contain organic substrate, contains the inorganic ultra micron thing such as the polysiloxane of element silicon again in the hardening liquid, when making the film that resistance to wears possess toughness, has improved hardness again.
B, coating process
Concrete steps are as follows:
One, eyeglass is installed
In temperature: 20-25 ℃, the environment of humidity: 35-40%, get the stiffened resin eyeglass of a cleaning
Be installed on the anchor clamps;
Two, vacuumize
Anchor clamps are put into vacuum chamber together with resin eyeglass heats and vacuumizes
The temperature of vacuum chamber: 90-95 ℃
Set vacuum tightness: 5 x 10
-3Torr
Three, resin eyeglass prerinse before the plated film
When vacuum tightness reaches 5 x 10
-3Utilizing ion to discharge high-purity argon generation ion pair resin eyeglass surface during Torr bombards
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
Four, vacuum coating
Adopt Ion Aided Film Coating technology to be coated with double-layer reflection reducing coating in the following manner.
1, SiO
2(the 1st layer)
Evaporation power: 19.5
Rate of evaporation speed: 20.0A/S
Evaporation thickness: 0.58KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
2, ZrO
2(the 2nd layer)
Evaporation power: 25
Rate of evaporation speed: 6.5A/S
Evaporation thickness: 0.27KA
3, SiO
2(the 3rd layer)
Evaporation power: 13
Evaporation rate: 5.0A/S
Evaporation thickness: 0.18KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Filament current: 5.5-6A
Argon flow amount: 9SCCM
4, ZrO
2(the 4th layer)
Evaporation power: 25
Evaporation rate: 6.5A/S
Evaporation thickness: 0.58KA
5, SiO
2(the 5th layer)
Evaporation power: 13
Evaporation rate: 7.0A/S
Evaporation thickness: 0.74KA
Ion gun anode voltage: 55-60V
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
Utilize electron gun to adopt such scheme that Coating Materials is fused, and then evaporate, make the Coating Materials of gaseous state be attached on the resin eyeglass surface, form the multilayer antireflective film, the about 0.3um of its thickness.
Five, be coated with teleblem (fluoride)
In order to make resin eyeglass have waterproof, oil rub resistance ability, increase one deck teleblem again at the double-layer reflection reducing coating skin, utilize the molybdenum boat thermal evaporation, make the fluoride materials gasification, on double-layer reflection reducing coating, form teleblem, thickness is about 0.005～0.01um.The steps include:
1 vacuumize before, the superhard film material that will contain fluoride is put into molybdenum boat.
2 after having plated double-layer reflection reducing coating, and molybdenum boat the two poles of the earth are heated with 80～82A electric current, makes the temperature of molybdenum boat reach 420～450 ℃
3 fully fuse the superhard film material in the molybdenum boat, and distilling is gaseous state.
4 fluorine molecules shift and are deposited on the resin eyeglass substrate from evaporation source, rearrange or bonding on the double-layer reflection reducing coating surface, finally form teleblem.
Its technological parameter is as follows:
Molybdenum boat electric current: 80-82A
Temperature: 420-450 ℃
Evaporation thickness: 0.26kA
Evaporation rate: 10.0A/S
Evaporation power: 0.1
Ion gun anode voltage: 35-40V
Ion gun anode current: 3.5-4A
Ion gun lamp line electric current: 4.5-5A
Argon flow amount: 4SCCM
Through above-mentioned processing, finished product is product ultrahard antifouling resin eyeglass of the present invention.
Because plated film itself and resin eyeglass are difficult to the contradiction that is in harmonious proportion a bit, as: heat sensitivity, thermal expansivity etc.These character make between substrate and the conventional lenses rete very large internal stress, rete easily splits, and the film that resistance to wears is the basic rete of whole composite membrane, the double-layer reflection reducing coating layer is a kind of extremely thin inorganic, metal oxide material, hard and crisp, have only the hardness that constantly improves the film that resistance to wears, make it to be complementary with multilayer anti-reflection rete, the whole rigid degree that improves resin lens of ability, not easy to wear.The tradition hardening process is put into resin eyeglass and is contained dioxane and recall alkane, T-butanols, soaks in the hardening liquid of potpourris such as methyl alcohol, forms wear-resistant protective seam on the resin eyeglass surface.
The present invention carries out organic silication to resin eyeglass; form chemistry and mechanical protection sheath at the resin eyeglass surfaces externally and internally; the TiO2 scintilla particle that has added q.s in hardening liquid makes it to adhere to the surface of resin eyeglass substrate with the Si atom Ti-Si key that forms high bond energy that blends mutually; pass through heat curing again; improved the rigid degree of resin eyeglass like this, its resin eyeglass surface abrasion resistance and glass mirror have been close (as shown in Figure 2) through experiment.
In addition, double-layer reflection reducing coating is according to the interference of light principle, makes the reflected light of minute surface and plated film reflected light interfere mutually and eliminate, and different retes is optionally eliminated the reflection of corresponding wave band light and removed stray light.The inventor increases the quality that visible light transmissivity improves picture, makes imaging more clear, but because of the Technology Need of double-layer reflection reducing coating, the space is bigger between this membrane molecule, is cavernous structure, and lens surface is easily sheltered evil people and countenance evil practices, and greasy dirt easily soaks into to antireflection film layer.For this reason, the present invention when being coated with double-layer reflection reducing coating, adopt prior art when being coated with this rete the Ion Aided Film Coating technology that do not adopt increase the compactness and the smoothness of rete, and utilize nanophase isolation technics in the macromolecule fluoride, be coated with the ultra-amphosphobic interface of nano-scale on the double-layer reflection reducing coating surface, on macroscopic view, show as and have certain stable gas membrane and cover the double-layer reflection reducing coating surface, remedy the big deficiency of double-layer reflection reducing coating molecule gap, reduce surface energy, thereby make the lens surface present extraordinary two thin property, at this moment the contact angle of water droplet or greasy dirt and eyeglass is tending towards maximal value, surpasses 110 degree (as shown in Figure 3).
Invention effect of the present invention
Product of the present invention with the strong film that resistance to wears as the basis, the low-surface-energy that has more fluorine molecule is as teleblem, thereby have ultralow friction factor, detect the 000# steel wool through national authority mechanism, with 1000 its haze values of 750g normal pressure reciprocating friction are 1/10 of like products, owing to adopt nanometer technology, make product of the present invention have excellent waterproof, resistant, grease proofing spy's energy, and more easy to clean.The present invention simultaneously is easily manufactured, the easy to learn and grasp of manufacture method.
Description of drawings
Fig. 1 is a lens sectional view of the present invention.
Wherein:
1, resin eyeglass substrate
2, the film that resistance to wears
3, double-layer reflection reducing coating
4, teleblem
Fig. 2 is that resin eyeglass of the present invention and glass eye eyeglass anti-wear performance compare synoptic diagram;
Fig. 3 is the contact angle synoptic diagram of greasy dirt or water droplet and eyeglass.
Best enforcement
Most preferred embodiment one of the present invention:
A kind of ultrahard antifouling resin eyeglass, form by resin eyeglass substrate (1), the film that resistance to wears (2), multilayer antireflection film (3), teleblem (4), it is characterized in that: the film that resistance to wears (2) is to stick to the dura mater that contains the Ti-Si key on the resin eyeglass substrate (1), and double-layer reflection reducing coating (3) adopts Ion Aided Film Coating technology to be coated with.
Its manufacture method is:
One, alkali is invaded turbid
Getting one of resin eyeglass substrate puts into aqueous slkali and soaks
Aqueous slkali composition: NaOH
Concentration: 35-37%
Temperature: 35-40 ℃
Time: 8-10 divides kind
Two, clean
Taking-up resin eyeglass substrate is put into the tank that contains detersive and is cleaned
Composition: general detersive
Concentration: 20-25%
Temperature: 35-40%
Time: 120-150S
Three, softening water, ultrasonic cleaning
The resin eyeglass substrate is put into purification back pure water ultrasonic cleaning
Softening water conductivity 18m Ω
Temperature: 20-25 ℃
Four, anhydrous alcohol, ultrasonic cleaning
Alcohol concentration: 99.9%
Temperature: 20-25 ℃
Five, dehydration is received and is done
Adopting the IPA dehydration to receive does
Six, stiffened dipping
The resin eyeglass substrate is put into hardening liquid to be flooded
Hardening liquid proportion proportion under 10 ℃ temperature is: 1.010～1.030
Temperature: 10-12 ℃
In the hardening liquid:
Dioxane concentration 18%
T-butanol concentration 30%
Polysiloxane concentration 12%
Methanol concentration 22-30%
Other concentration 5%
TiO
2Content: 5-13%
The relative humidity of stiffened groove: 40-45%
Dip time: 35-40S
Seven, the lifting of resin eyeglass substrate
The resin eyeglass substrate after stopping 35-40S, hardening liquid is done at the uniform velocity to promote
Speed: 6-8mm/s at the uniform velocity
Eight, precuring
The resin eyeglass substrate is put into baking oven precuring
Temperature: 65-70 ℃
Time: 15-18 minute
Nine, heat curing
The resin eyeglass substrate is put into baking oven to be toasted
Temperature: 115-120 ℃
Time: 3 hours
Ten, eyeglass is installed
The stiffened resin eyeglass of getting a cleaning is installed on the anchor clamps
To environment requirement
Temperature: 20-25 ℃
Humidity: 35-40%
11, vacuumize
Anchor clamps are put into vacuum chamber together with resin eyeglass heats and vacuumizes
The temperature of vacuum chamber: 90-95 ℃
Set vacuum tightness: 5 x 10
-3Torr
12, resin eyeglass prerinse before the plated film
When vacuum tightness reaches 5 x 10
-3Utilize ion to discharge high-purity argon during Torr and produce ion pair resin eyeglass surface
Drive out of
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
13, vacuum coating
Adopt Ion Aided Film Coating technology to be coated with the above double-layer reflection reducing coating of one deck in the following manner.
The steps include:
1, SiO
2(the 1st layer)
Evaporation power: 19.5
Rate of evaporation speed: 20.0A/S
Evaporation thickness: 0.58KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
2, ZrO
2(the 2nd layer)
Evaporation power: 25
Rate of evaporation speed: 6.5A/S
Evaporation thickness: 0.27KA
3, SiO
2(the 3rd layer)
Evaporation power: 13
Evaporation rate: 5.0A/S
Evaporation thickness: 0.18KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
4, ZrO
2(the 4th layer)
Evaporation power: 25
Evaporation rate: 6.5A/S
Evaporation thickness: 0.58KA
5, SiO
2(the 5th layer)
Evaporation power: 13
Evaporation rate: 7.0A/S
Evaporation thickness: 0.74KA
Ion gun anode voltage: 55-60V
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
Utilize electron gun to adopt such scheme that Coating Materials is fused, and then evaporate, make the Coating Materials of above-mentioned gaseous state be attached on the resin eyeglass surface, form double-layer reflection reducing coating.
14, teleblem (fluoride)
Increase one deck teleblem again at the double-layer reflection reducing coating skin, utilize the molybdenum boat thermal evaporation, make the fluoride materials gasification, form teleblem on double-layer reflection reducing coating, thickness is about 0.005～0.01um.
The steps include:
1. before vacuumizing, the superhard film material that will contain fluoride is put into molybdenum boat.
2. after having plated double-layer reflection reducing coating, molybdenum boat the two poles of the earth are heated with 80～82A electric current, make the temperature of molybdenum boat reach 420～450 ℃
3. the superhard film material in the molybdenum boat is fully fused, be evaporated to gaseous state.
4. fluorine molecule shifts and is deposited on the resin eyeglass substrate from evaporation source, rearranges or bonding on the double-layer reflection reducing coating surface, finally forms teleblem.
Its technological parameter is as follows:
Molybdenum boat electric current: 80-82A
Temperature: 420-450 ℃
Ion gun anode voltage: 35-40V
Ion gun anode current: 3.5-4A
Ion gun lamp line electric current: 4.5-5A
Argon flow amount: 4SCCM
Through above-mentioned processing, finished product is product ultrahard antifouling resin eyeglass of the present invention.
Claims (2)
1, a kind of ultrahard antifouling resin eyeglass, form by resin eyeglass substrate (1), the film that resistance to wears (2), multilayer antireflection film (3), teleblem (4), it is characterized in that: the film that resistance to wears (2) is the dura mater that contains the Ti-Si key that sticks on the resin eyeglass substrate (1), and double-layer reflection reducing coating (3) adopts Ion Aided Film Coating technology to be coated with.
2, the manufacture method of the described ultrahard antifouling resin eyeglass of a kind of claim 1, its manufacturing step is:
A, stiffened are handled:
1) alkali is invaded turbid
Getting one of resin eyeglass substrate puts into aqueous slkali and soaks
2) clean
Taking-up resin eyeglass substrate is put into the tank that contains detersive and is cleaned
3) softening water, ultrasonic cleaning
The resin eyeglass substrate is put into purification back pure water ultrasonic cleaning, use anhydrous alcohol, ultrasonic cleaning resin eyeglass substrate again
4) dehydration is received and is done
Adopting the IPA dehydration to receive does
5) stiffened dipping
The resin eyeglass substrate is put into hardening liquid to be flooded
6) lifting of resin eyeglass substrate
7) precuring
The resin eyeglass substrate is put into baking oven precuring
8) heat curing
B, vacuum coating
C, making teleblem
It is characterized in that:
Hardening liquid proportion under 10 ℃ temperature is: 1.010-1.030
Hardening liquid temperature: 10-12 ℃
Each composition weight percent concentration in the hardening liquid:
Dioxane concentration 18%
T-butanol concentration 30%
Polysiloxane concentration 12%
Methanol concentration 22-30%
Other concentration 5%
TiO
2Weight percent concentration: 5-13%
The relative humidity of stiffened groove: 40-45%
Dip time: 35-40S
The resin eyeglass substrate stopped in hardening liquid do behind the 35-40S at the uniform velocity to promote
At the uniform velocity speed: 6-8mm/s makes hardening liquid form the uniform rete of thickness at the resin eyeglass substrate surface
Adopt Ion Aided Film Coating technology to be coated with more than one deck in the following manner:
(1) SiO
2(the 1st layer)
Evaporation power: 19.5
Rate of evaporation speed: 20.0A/S
Evaporation thickness: 0.58KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
(2) ZrO
2(the 2nd layer)
Evaporation power: 25
Rate of evaporation speed: 6.5A/S
Evaporation thickness: 0.27KA
(3) SiO
2(the 3rd layer)
Evaporation power: 13
Evaporation rate: 5.0A/S
Evaporation thickness: 0.18KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5-5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
(4) ZrO
2(the 4th layer)
Evaporation power: 25
Evaporation rate: 6.5A/S
Evaporation thickness: 0.58KA
(5) SiO
2(the 5th layer)
Evaporation power: 13
Evaporation rate: 7.0A/S
Evaporation thickness: 0.74KA
Ion gun anode voltage: 55-60V
Ion gun anode current: 4.5～5A
Ion source filament electric current: 5.5-6A
Argon flow amount: 9SCCM
Utilize electron gun to adopt such scheme that Coating Materials is fused, and then evaporate, make the Coating Materials of gaseous state stick to the resin eyeglass substrate surface, form double-layer reflection reducing coating (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101123936A CN100495123C (en) | 2005-12-30 | 2005-12-30 | Ultrahard antifouling resin eyeglass and method for making same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101123936A CN100495123C (en) | 2005-12-30 | 2005-12-30 | Ultrahard antifouling resin eyeglass and method for making same |
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| CN1991441A CN1991441A (en) | 2007-07-04 |
| CN100495123C true CN100495123C (en) | 2009-06-03 |
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- 2005-12-30 CN CNB2005101123936A patent/CN100495123C/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220317336A1 (en) * | 2021-04-01 | 2022-10-06 | Jiangsu Conant Optical Co., Ltd. | Dyeable 1.74 resin lens and preparation method thereof |
| US11772341B2 (en) * | 2021-04-01 | 2023-10-03 | Jiangsu Conant Optical Co., Ltd. | Dyeable 1.74 resin lens and preparation method thereof |
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| CN1991441A (en) | 2007-07-04 |
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