CN110240415A - A kind of preparation method of the ultralow reflecting glass of sunlight all band - Google Patents
A kind of preparation method of the ultralow reflecting glass of sunlight all band Download PDFInfo
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- CN110240415A CN110240415A CN201910468177.7A CN201910468177A CN110240415A CN 110240415 A CN110240415 A CN 110240415A CN 201910468177 A CN201910468177 A CN 201910468177A CN 110240415 A CN110240415 A CN 110240415A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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Abstract
The invention discloses a kind of preparation methods of ultralow reflecting glass of sunlight all band.The present invention is that glass matrix is first passed through to the pretreatment of HF solution, then it is immersed in special corrosive liquid (mixed liquor of phosphate, carbonate and silicate), HF solution corrosion is finally used again, by control corrosion rate temperature and etching time, to realize the preparation of the ultralow reflecting glass of sunlight all band.The reflectivity of all band sunlight (300nm-2500nm) effectively can be down to 1% hereinafter, improving the transmitance of light by the ultralow reflecting glass of gained sunlight all band.The preparation method reaction condition is controllable, and equipment requirement is simple, it is easy to accomplish batch production is conducive to environmental protection.
Description
Technical field
The present invention relates to a kind of glass surface antireflective processing method, in particular to a kind of corrosion corrosion prepares sunlight
The method of the ultralow reflecting glass of all band belongs to clean energy resource utilization and green building material technology of preparing and application field.
Background technique
With society and expanding economy, how more preferably the reasonable utilization energy, reduces the damage to environment as full generation
One important subject on boundary.Solar energy can be used for solar energy since it has the characteristics that cleanliness without any pollution and widely distributed
The fields such as photovoltaic, solar energy optical-thermal and solar energy photocatalytic achieve the purpose that energy saving, environmentally protective.Either photovoltaic,
In photoelectricity or photocatalysis field, most equipment all use the good glass of translucency as isolated material and play light transmission and guarantor
Protect the effect of equipment inner structure.Therefore, the sunlight of glass surface is reflected and is eliminated, improve the transmitance of all band sunlight
Facilitate the utilization efficiency for further promoting sunlight, with good economic efficiency and social value.
The preparation method of anti reflection glass has very much, mainly there is magnetron sputtering method, sol-gel dip coating, vacuum evaporation
Method and acid and alkali corrosion method etc..For acid and alkali corrosion method, the preparation method of preceding several anti reflection glasses exists certain
Defect or deficiency.It is magnetron sputtering method complex process, high to environment and equipment requirement, thus higher cost, it is high to be appropriate only for manufacture
Hold technical products；Although cost is relatively low for sol-gel dip coating, sun light transmission rate is relatively low, while the antireflective sun
The wave band of light is relatively narrow；Vacuum vapour deposition work higher cost, the not corrosion resistant under the harsh conditions such as strong illumination or outdoor wind and weather
It loses and anti-scratch performance is poor.Therefore the research that anti reflection glass is glass surface treatment field is prepared using acid and alkali corrosion method
Hot spot.Related scientific research personnel using alkaline etching it is available reach in photovoltaic range transmitance 99% photovoltaic glass
(Liqiang Liu,Broad band and Omnidirectional,Nearly zero reflective
Photovoltaic Glass, Adv.Mater.2012,24,6318-6322.).
So far, although there is the preparation method of many excellent anti reflection glasses, these methods only play glass
Antireflective of the glass in visible-range or visible light+near infrared range (400~1200nm).For sunlight, radiation
There is the stronger Energy distribution to be always in recent years especially in the energy of infrared band in all band of 300~2500nm
The important subject of Solar use.Therefore, the preparation method for obtaining a kind of ultralow reflecting glass of sunlight all band has
Significance.
Summary of the invention
Exist in terms of preparing the ultralow reflecting glass of sunlight all band for existing anti reflection glass process for treating surface
Deficiency, the present invention provides a kind of preparation methods of ultralow reflecting glass of sunlight all band.The present invention is by glass matrix
The pretreatment of HF solution is first passed through, is then immersed in special corrosive liquid (mixed liquor of phosphate, carbonate and silicate), most
Structure optimization is carried out with HF solution corrosion again afterwards, by control corrosion rate temperature and etching time, to realize that sunlight all band is super
The preparation of low-reflection glass.The ultralow reflecting glass of gained sunlight all band can be effectively by all band sunlight (300nm-
Reflectivity 2500nm) is down to 1% hereinafter, improving the transmitance of light.The preparation method reaction condition is controllable, equipment requirement letter
It is single, it is easy to accomplish batch production is conducive to environmental protection.
The technical scheme is that a kind of preparation method of the ultralow reflecting glass of sunlight all band, characterized in that packet
Include following steps:
(1) glass matrix cleaned up with deionized water the HF that concentration is 0.0001~10wt% is first placed into corrode
In slot, and set 0.1 in the decentralization of 20~80 DEG C of temperature condition~for 24 hours；
(2) phosphate, carbonate and silicate are mixed by mole 1~98%:1~98%:1~98% ratio
It closes, forms mixture；Add water to dissolve mixture, forms the special corrosive liquid that concentration is 0.0001~10wt%；
(3) glass matrix after HF corrosion treatment is cleaned up with deionized water, is put into special corrosive liquid, and in 20
0.1~48h is set in~80 DEG C of temperature condition decentralization；
(4) glass matrix for corroding corrosion is cleaned up with deionized water, being put into concentration is 0.0001~10wt%
HF etching tank in, and in 20~80 DEG C of temperature condition decentralization set 0.1~48h；
(5) glass matrix after HF corrosion treatment is cleaned up with deionized water, is dried, obtains all band anti-reflection
Penetrate glass.
Glass matrix in above-mentioned steps (1) is to be used using the photovoltaic of rolling process or float process, photo-thermal, building or decoration
Na2O-CaO-SiO2System glass.
In order to reach corrosion temperature in above-mentioned steps (1), it can be and etching tank is integrally put into baking oven, be also possible in corruption
It is put into heat riser in erosion slot, heat temperature raising is carried out to HF solution.
Phosphate in above-mentioned steps (2) can be Na2HPO4, NaH2PO4, K2HPO4, KH2PO4, Na3PO4And K3PO4In
It is one or more.
Carbonate in above-mentioned steps (2) can be Na2CO3, NaHCO3, K2CO3And KHCO3One of or it is a variety of.
Silicate in above-mentioned steps (2) can be Na2SiO3·9H2O, Na2SiO3And K2SiO3One of or it is a variety of.
In order to reach corrosion temperature in above-mentioned steps (3), it can be and etching tank is integrally put into baking oven, be also possible in corruption
It is put into heat riser in erosion slot, heat temperature raising is carried out to corrosive liquid.
In order to reach corrosion temperature in above-mentioned steps (4), it can be and etching tank is integrally put into baking oven, be also possible in corruption
It is put into heat riser in erosion slot, heat temperature raising is carried out to HF solution.
Drying process mode is dry, shady and cool ventilation drying or room temperature 100~1000 in drier in above-mentioned steps (5)
Vacuumizing for Pa is dried under reduced pressure, and drying to surface is without suspension water droplet.
Preferably, the present invention specifically includes the following steps:
(1) glass matrix surface is cleaned up with deionized water, is put into the HF solution that concentration is 0.01~0.1wt%
In, 0.5~2h is set in 30~50 DEG C of temperature condition decentralizations；
(2) by Na2HPO4、Na2CO3And Na2SiO3·9H2O by mole 35~45%:35~45%:15~
25% ratio mixing, forms mixture；Then plus water dissolves mixture, and forming concentration is the special of 0.01~0.1wt%
Corrosive liquid；
(3) HF solution corrosion treated glass matrix is cleaned up with deionized water, is put into special corrosive liquid, and
12~48h is set in 50~70 DEG C of temperature condition decentralizations；
(4) glass matrix for corroding corrosion is cleaned up with deionized water, being put into concentration is 0.05~0.5wt%'s
In HF etching tank, and 2~12h is set in the decentralization of 40~60 DEG C of temperature condition；
(5) glass matrix after HF corrosion treatment is cleaned up with deionized water, is dried, obtains sunlight all-wave
The ultralow reflecting glass of section.
The ultralow reflecting glass of above-mentioned preparation method preparation requires to be less than in the full wave reflectivity of 300nm~2500nm
1%, performance is as shown in Figs. 1-3.
The principle of the present invention is: utilizing corrosion technology, changes the microstructure on glass matrix surface.Firstly, utilizing HF corruption
Erosion is cleaned and is pre-processed to glass surface；Then corroded using special corrosive liquid, building refractive index gradually changes
The ultralow reflective coating of sunlight all band；It recycles HF solution to optimize the structure of ultralow reflective coating, and then prepares
Obtain the ultralow reflecting glass of sunlight all band.
The present invention has the advantage that
1, reaction condition facilitates controllable, and the equipment needed is fairly simple, it is easy to accomplish low cost is produced in enormous quantities.
2, low in the pollution of the environment, preparation process whole process is environmentally protective.
3, the ultralow reflecting glass of sunlight all band prepared is, it can be achieved that in 300nm~2500nm all band sunlight
Ultralow reflection.
Detailed description of the invention
Fig. 1 is the comparison photo of sunlight all band prepared by the present invention ultralow reflecting glass and simple glass；Wherein a schemes
For simple glass, b figure is the ultralow reflecting glass of sunlight all band.
Fig. 2 is the scanning electron microscopic picture of the ultralow reflecting glass cross section of sunlight all band prepared by the present invention；
Fig. 3 is all band reflectance test of sunlight all band prepared by the present invention ultralow reflecting glass and simple glass
Curve.
Specific embodiment
Embodiment 1
(1) glass matrix surface is cleaned up with deionized water, is put into the HF solution that concentration is 0.01wt%, in 30
DEG C temperature condition decentralization set 1h；
(2) by Na2HPO4、Na2CO3And Na2SiO3·9H2O is mixed by mole the ratio of 40%:40%:20%,
Form mixture.Add water to dissolve mixture, forms the special corrosive liquid that concentration is 0.1wt%.
(3) HF solution corrosion treated glass matrix is cleaned up with deionized water, is put into special corrosive liquid, and
It is set for 24 hours in 50 DEG C of temperature condition decentralizations；
(4) glass matrix for corroding corrosion is cleaned up with deionized water, is put into the HF that concentration is 0.1wt% and corrodes
In slot, and 6h is set in the decentralization of 50 DEG C of temperature condition；
(5) glass matrix after HF corrosion treatment is cleaned up with deionized water, is dried, obtains sunlight all-wave
The ultralow reflecting glass of section.
The comparison photo of the ultralow reflecting glass of sunlight all band manufactured in the present embodiment and simple glass is as shown in Figure 1.
The reflectivity of all band anti reflection glass is significantly smaller as seen from Figure 1, and the reflectivity of simple glass is larger.
The scanning electron microscopic picture of the ultralow reflecting glass of sunlight all band manufactured in the present embodiment is as shown in Figure 2.From figure
It can be seen that using above-mentioned caustic solution a layer thickness uniformly ultralow reflective coating structure can be obtained in glass surface.
The ultralow reflecting glass of sunlight all band manufactured in the present embodiment and simple glass are in full wave reflectance test
Curve is as shown in Figure 3.Ultralow reflecting glass be can be seen that from curve in full wave reflectivity less than 1%, and simple glass
Reflectivity between 4%-5%.From Fig. 3 it can also be seen that: the reflectivity of the ultralow reflecting glass of sunlight all band is in 300nm
Reflectivity≤1% in~400nm wavelength band, in 400nm~2200nm wavelength band internal reflection rate≤0.5%,
2200~2500nm wavelength band internal reflection rate≤1%.
To sum up, the ultralow reflecting glass of sunlight all band prepared by the present invention can effectively reduce sunlight in all band model
Interior reflectivity is enclosed, improves the utilization efficiency of solar energy, and process is simple, it is convenient and practical.
Embodiment 2
As described in Example 1, the difference is that: in step (1) HF solution concentration be 0.0001wt%.
Embodiment 3
As described in Example 1, the difference is that: in step (1) HF solution concentration be 10wt%.
Embodiment 4
As described in Example 1, the difference is that: in step (1) corrosion temperature be 20 DEG C.
Embodiment 5
As described in Example 1, the difference is that: in step (1) corrosion temperature be 80 DEG C.
Embodiment 6
As described in Example 1, the difference is that: in step (1) etching time be 0.1h.
Embodiment 7
As described in Example 1, the difference is that: in step (1) etching time be for 24 hours.
Embodiment 8
As described in Example 1, the difference is that: Na2HPO4、Na2CO3And Na2SiO3·9H2The molar percentage of O is
98%:1%:1%.
Embodiment 9
As described in Example 1, the difference is that: Na2HPO4、Na2CO3And Na2SiO3·9H2The molar percentage of O is
1%:98%:1%.
Embodiment 10
As described in Example 1, the difference is that: Na2HPO4、Na2CO3And Na2SiO3·9H2The molar percentage of O is
1%:1%:98%.
Embodiment 11
As described in Example 1, the difference is that: in step (2) phosphate be K2HPO4。
Embodiment 12
As described in Example 1, the difference is that: in step (2) phosphate be Na2HPO4With K2HPO4Mixture.
Embodiment 13
As described in Example 1, the difference is that: in step (2) carbonate be NaHCO3。
Embodiment 14
As described in Example 1, the difference is that: in step (2) phosphate be Na2CO3With K2CO3Mixture.
Embodiment 15
As described in Example 1, the difference is that: in step (2) silicate be Na2SiO3。
Embodiment 16
As described in Example 1, the difference is that: silicate is and Na in step (2)2SiO3·9H2O and K2SiO3It is mixed
Close object.
Embodiment 17
As described in Example 1, the difference is that: in step (3) corrosion temperature be 20 DEG C.
Embodiment 18
As described in Example 1, the difference is that: in step (3) corrosion temperature be 80 DEG C.
Embodiment 19
As described in Example 1, the difference is that: in step (3) etching time be 0.5h.
Embodiment 20
As described in Example 1, the difference is that: in step (3) etching time be 48h.
Embodiment 21
As described in Example 1, the difference is that: in step (4) HF solution concentration be 0.0001wt%.
Embodiment 22
As described in Example 1, the difference is that: in step (4) HF solution concentration be 10wt%.
Embodiment 23
As described in Example 1, the difference is that: in step (4) corrosion temperature be 20 DEG C.
Embodiment 24
As described in Example 1, the difference is that: in step (4) corrosion temperature be 80 DEG C.
Embodiment 25
As described in Example 1, the difference is that: in step (4) etching time be 0.1h.
Embodiment 26
As described in Example 1, the difference is that: in step (4) etching time be 48h.
Embodiment 27
As described in Example 1, the difference is that: glass product, which is placed at shady and cool ventilation, in step (5) is dried.
Embodiment 28
As described in Example 1, the difference is that: glass product is placed in a vacuum drying oven in step (5), and 100 Pa are normal
Temperature is dried under reduced pressure.
Embodiment 29
As described in Example 1, the difference is that: glass product is placed in a vacuum drying oven in step (5), 1000 Pa
Room temperature is dried under reduced pressure.
Claims (8)
1. a kind of preparation method of the ultralow reflecting glass of sunlight all band, characterized in that include the following steps:
(1) glass matrix cleaned up with deionized water is first placed into the HF etching tank that concentration is 0.0001~10wt%
It is interior, and set 0.1 in the decentralization of 20~80 DEG C of temperature condition~for 24 hours；
(2) phosphate, carbonate and silicate are mixed by mole 1~98%:1~98%:1~98% ratio,
Form mixture；Add water to dissolve mixture, forms the special corrosive liquid that concentration is 0.0001~10wt%；
(3) glass matrix after HF corrosion treatment is cleaned up with deionized water, is put into special corrosive liquid, and in 20~80
DEG C temperature condition decentralization set 0.1~48h；
(4) glass matrix for corroding corrosion is cleaned up with deionized water, is put into the HF that concentration is 0.0001~10wt%
In etching tank, and 0.1~48h is set in the decentralization of 20~80 DEG C of temperature condition；
(5) glass matrix after HF corrosion treatment is cleaned up with deionized water, is dried, obtains all band antireflective glass
Glass.
2. a kind of preparation method of the ultralow reflecting glass of sunlight all band as described in claim 1, characterized in that the step
Suddenly the glass matrix in (1) is to use Na using the photovoltaic of rolling process or float process, photo-thermal, building or decoration2O-CaO-SiO2Body
It is glass.
3. a kind of preparation method of the ultralow reflecting glass of sunlight all band as described in claim 1, characterized in that the step
Suddenly the phosphate in (2) is Na2HPO4, NaH2PO4, K2HPO4, KH2PO4, Na3PO4And K3PO4One of or it is a variety of.
4. a kind of preparation method of the ultralow reflecting glass of sunlight all band as described in claim 1, characterized in that the step
Suddenly the carbonate in (2) is Na2CO3, NaHCO3, K2CO3And KHCO3One of or it is a variety of.
5. a kind of preparation method of the ultralow reflecting glass of sunlight all band as described in claim 1, characterized in that the step
Suddenly the silicate in (2) is Na2SiO3·9H2O, Na2SiO3And K2SiO3One of or it is a variety of.
6. a kind of preparation method of the ultralow reflecting glass of sunlight all band as described in claim 1, characterized in that the step
Suddenly (5) are middle is dried are as follows: dry in drier, shady and cool ventilation drying or the decompression that vacuumizes of 100~1000Pa of room temperature are done
Dry, drying to surface is without suspension water droplet.
7. special such as a kind of preparation method of the ultralow reflecting glass of sunlight all band of any of claims 1-6
Sign is to include the following steps:
(1) glass matrix surface is cleaned up with deionized water, is put into the HF solution that concentration is 0.01~0.1wt%, in
0.5~2h is set in 30~50 DEG C of temperature condition decentralization；
(2) by Na2HPO4、Na2CO3And Na2SiO3·9H2O is by mole 35~45%:35~45%:15~25% ratio
Example mixing, forms mixture；Then plus water dissolves mixture, forms the special corrosive liquid that concentration is 0.01~0.1wt%；
(3) HF solution corrosion treated glass matrix is cleaned up with deionized water, is put into special corrosive liquid, and in 50
12~48h is set in~70 DEG C of temperature condition decentralization；
(4) glass matrix for corroding corrosion is cleaned up with deionized water, it is rotten is put into the HF that concentration is 0.05~0.5wt%
It loses in slot, and sets 2~12h in the decentralization of 40~60 DEG C of temperature condition；
(5) glass matrix after HF corrosion treatment is cleaned up with deionized water, is dried, it is super to obtain sunlight all band
Low-reflection glass.
8. sunlight all band prepared by a kind of preparation method of ultralow reflecting glass of sunlight all band as claimed in claim 7
Ultralow reflecting glass, characterized in that reflectivity≤1% of the reflectivity in 300nm~2500nm wavelength band.
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| CN201910468177.7A CN110240415A (en) | 2019-05-31 | 2019-05-31 | A kind of preparation method of the ultralow reflecting glass of sunlight all band |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795785A (en) * | 2012-09-10 | 2012-11-28 | 刘立强 | Anti-reflecting glass and method for preparing same through secondary acid corrosion |
| CN103626400A (en) * | 2012-08-29 | 2014-03-12 | 悦城科技股份有限公司 | Production method for glass surface without glare and with low reflection |
| CN105143134A (en) * | 2012-11-30 | 2015-12-09 | 康宁股份有限公司 | Reduced reflection glass articles and methods for making and using same |
| US9616459B1 (en) * | 2014-04-17 | 2017-04-11 | Lockheed Martin Corporation | Polymeric coatings for fortification of visible, infrared, and laser optical devices |
| CN109081600A (en) * | 2018-10-25 | 2018-12-25 | 海南中航特玻科技有限公司 | Using the preparation method of salt chemical reagent etching anti reflection glass |
-
2019
- 2019-05-31 CN CN201910468177.7A patent/CN110240415A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626400A (en) * | 2012-08-29 | 2014-03-12 | 悦城科技股份有限公司 | Production method for glass surface without glare and with low reflection |
| CN102795785A (en) * | 2012-09-10 | 2012-11-28 | 刘立强 | Anti-reflecting glass and method for preparing same through secondary acid corrosion |
| CN105143134A (en) * | 2012-11-30 | 2015-12-09 | 康宁股份有限公司 | Reduced reflection glass articles and methods for making and using same |
| US9616459B1 (en) * | 2014-04-17 | 2017-04-11 | Lockheed Martin Corporation | Polymeric coatings for fortification of visible, infrared, and laser optical devices |
| CN109081600A (en) * | 2018-10-25 | 2018-12-25 | 海南中航特玻科技有限公司 | Using the preparation method of salt chemical reagent etching anti reflection glass |
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