CN105314884B - Antireflective coating and preparation method thereof - Google Patents
Antireflective coating and preparation method thereof Download PDFInfo
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- CN105314884B CN105314884B CN201410322964.8A CN201410322964A CN105314884B CN 105314884 B CN105314884 B CN 105314884B CN 201410322964 A CN201410322964 A CN 201410322964A CN 105314884 B CN105314884 B CN 105314884B
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Abstract
The invention discloses a kind of antireflective coating and preparation method thereof, available for improving solar battery efficiency.The antireflective coating is on glass basis by the siliceous sol coating using inorganic matter phosphoric acid as template.Prepared antireflective coating can not only reach pore-creating, antireflective and the antireflective effect suitable with organic formwork agent, and can reduce production cost.The invention discloses its preparation method, its simple preparation technology and operability are adapted to large-scale industrial production;Its cheap raw material helps further to reduce production cost simultaneously.
Description
Technical field
The invention belongs to antireflective coating technical field, and in particular to a kind of antireflective coating and preparation method thereof.
Background technology
Solar cell has expressed great expectations as one kind in clean energy resource by people;And improve constantly solar cell
Efficiency is the target that people make great efforts all the time.Due to the difference of refractive index between photovoltaic glass and air, can produce about 8% it is visible
Light loss, so as to reduce the light-inletting quantity in solar cell and finally influence battery efficiency.
To solve visible light loss, reach the purpose of lifting light-inletting quantity, currently used method is in photovoltaic glass surface
Coat antireflective coating (or anti-reflection film).The antireflective coating, can be one layer of SiO2Or TiO2Film or MULTILAYER COMPOSITE are thin
Film.For SiO2Antireflective coating, because its intrinsic refractive index (about 1.45) is higher than its theoretical optimal refractive index 1.22, it is therefore necessary to
Increase SiO2The porosity of film can realize anti-reflection effect.In order to increase porosity, conventional method is in SiO2In colloidal sol
Add template.Such as:(the Long-term durability of sol-gel porous such as San Vicnetre
Coatings for solar glass covers, Thin Solid Films, 2009 3157-3160 pages of volume 517) use
It is template with triblock copolymer Triton X-100 (Triton X-100) and is prepared under acid catalysed conditions
SiO2Film so that glass transmitance has reached 97%.(the Preparation of silica such as Yudong Xu
Antireflective films for solar energy application, Materials Letters, 2013 94
89-91 pages of volume) disclose a kind of SiO with acid as catalyst2The method that colloidal sol prepares antireflective coating, in acid catalyzed SiO2It is molten
Organic matter CTAB (cetab) is added in glue and is used as template, the film prepared is coated using this colloidal sol, thoroughly
Cross rate and improve 6% than non-film substrate glass.
But the template up to the present reported is substantially organic matter;In consideration of it, it is necessary to explore a kind of energy
Enough play the inorganic template agent of same purpose.
The content of the invention
It is an object of the invention to at present in SiO2Antireflective coating lacks the present situation of inorganic template agent in preparing, there is provided
It is a kind of available for solar energy and the SiO using inorganic template agent of other association areas2Antireflective coating and preparation method thereof.This
The inorganic template agent that invention uses can not only play the pore-creating effect to match with organic formwork agent, and can reduce anti-reflection
Penetrate film production cost.
The purpose of the present invention is achieved through the following technical solutions:
The present invention relates to a kind of antireflective coating, the antireflective coating is will to be coated using phosphoric acid as template containing Ludox
In what is be prepared on glass.
The invention further relates to a kind of preparation method of above-mentioned antireflective coating, methods described comprises the following steps:
A, inorganic silicon alkoxide, deionized water and the acid catalyst mixing that mol ratio is 1: 1~8: 0.002~1.0, frozen water bar
Stirring obtains solution A under part;The mol ratio of more preferably inorganic silicon alkoxide, deionized water and acid catalyst be 1: 3~5: 0.004~
0.3:
B, phosphoric acid and diluent, stirring obtain B solution;The mol ratio of the inorganic silicon alkoxide, phosphoric acid and diluent is 1:
0.2~1.0: 10~400;The mol ratio of more preferably inorganic silicon alkoxide, phosphoric acid and diluent is 1: 0.67~0.8: 29~100;
C, the solution A and B solution are mixed, obtains coating solution;The coating solution is coated on glass, is obtained
To coated glass;
D, the coated glass is heat-treated under the conditions of 200~1000 DEG C;It is placed in the deionized water of room temperature~100 DEG C
Cleaning, drying, is produced coated on the antireflective coating on glass.
Preferably, the inorganic silicon alkoxide is the mixing of one or both of tetraethyl orthosilicate, methyl silicate.
Preferably, the acid catalyst is hydrochloric acid or nitric acid.
Preferably, the mass fraction of the phosphoric acid is 10%~85%.More preferably mass fraction is 85% phosphoric acid.
Preferably, the diluent is low alcohol;The low alcohol include methanol, ethanol, propyl alcohol, one kind in butanol or
It is several.More preferably ethanol.
Preferably, in step C, the coating uses spin-coating method, czochralski method or spraying process.
Preferably, in step D, the heat treatment time is 0.5~10b.
Preferably, in step D, the temperature of the drying is 80~200 DEG C;Time is 0.5~4h.
Compared with prior art, the present invention has the advantages that:
1st, the inorganic template agent that the present invention uses can play the pore-creating effect to match with organic formwork agent;
2nd, the invention provides a kind of low production cost, technique is simple and the SiO of strong operability2The preparation of antireflective coating
Method, it is adapted to large-scale industrial production.
Brief description of the drawings
The detailed description made by reading with reference to the following drawings to non-limiting example, further feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is glass basis and the transmitance correlation curve of embodiment 3,5,7;
Fig. 2 is the surface SEM image of embodiment 3,5.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made;These belong to the present invention
Protection domain.
Embodiment 1
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 3: 0.01 molar ratio first
Close, and stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and ethanol are 1: 0.55: 10, the phosphorus that mass fraction is 85% is measured
Acid and ethanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 2000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 2h in 400 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 100 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 2
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 1: 0.002 molar ratio first
Close, and stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and methanol are 1: 0.2: 15, the phosphorus that mass fraction is 15% is measured
Acid and methanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 3000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 6h in 260 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 50 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 3
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 3: 0.004 molar ratio first
Close, and stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and ethanol are 1: 0.67: 29, the phosphorus that mass fraction is 85% is measured
Acid and ethanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 4000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 2h in 400 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 100 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 4
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Methyl silicate, deionized water and nitric acid are mixed with 1: 4: 0.05 molar ratio first, and in ice
Stirring obtains solution A under water condition.
Step 2:According to the molar ratio that TEOS, phosphoric acid, ethanol and butanol are 1: 0.8: 50: 50, measuring mass fraction is
45% phosphoric acid, ethanol and butanol, stirring obtain B solution.
Step 3:The B solution of solution A in step 1 and step 2 is mixed, obtains coating solution.
Step 4:By gained coating solution in step 3, it is coated on the sheet glass cleaned up, is carried using coating method is lifted
Pulling rate degree is 8cm/s, obtains coated glass.
Step 5:Coated glass is heat-treated 1h in 800 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is room temperature and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 5
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 3: 0.004 molar ratio first
Close, and stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and ethanol are 1: 0.67: 43, the phosphorus that mass fraction is 85% is measured
Acid and ethanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 3000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 2h in 400 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 100 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 6
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:First by tetraethyl orthosilicate (TEOS), methyl silicate, deionized water and nitric acid with 0.5: 0.5: 5:
0.8 molar ratio mixing, and stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and butanol are 1: 0.8: 150, the phosphorus that mass fraction is 60% is measured
Acid and butanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 2000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 30mins in 1000 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 60 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 7
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 3: 0.004 molar ratio first
Close, and stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and ethanol are 1: 0.67: 72, the phosphorus that mass fraction is 85% is measured
Acid and ethanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 4000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 2h in 400 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 100 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 8
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 6: 0.6 molar ratio first,
And stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid, methanol and propyl alcohol are 1: 0.9: 100: 100, mass fraction is measured
For 75% phosphoric acid, methanol and propyl alcohol, stirring obtains B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, it is coated on the sheet glass cleaned up using spraying process and is only applied
Cover the one side of glass, quantity for spray 0.01g/em2, obtain coated glass.
Step 5:Coated glass is heat-treated 4h in 300 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 100 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 9
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 8: 1.0 molar ratio first,
And stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and propyl alcohol are 1: 1: 300, the phosphoric acid that mass fraction is 85% is measured
And propyl alcohol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, it is coated on the sheet glass cleaned up using spraying process and is only applied
Cover the one side of glass, quantity for spray 0.008g/cm2, obtain coated glass.
Step 5:Coated glass is heat-treated 45mins in 800 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water that temperature is 80 DEG C and cleans, dry,
Thus obtain coated on the SiO on glass2Antireflective coating.
Embodiment 10
The present embodiment is related to the preparation method of antireflective coating, specifically comprises the following steps:
Step 1:Tetraethyl orthosilicate (TEOS), deionized water and hydrochloric acid are mixed with 1: 2: 0.3 molar ratio first,
And stirring obtains solution A under the conditions of frozen water.
Step 2:According to the molar ratio that TEOS, phosphoric acid and ethanol are 1: 0.35: 400, it is 50% to measure mass fraction
Phosphoric acid and ethanol, stirring obtain B solution.
Step 3:By the solution A in step 1 and the B solution of step 2, mix, obtain coating solution.
Step 4:By gained coating solution in step 3, be coated in using spin-coating method on the sheet glass that cleans up and
The one side of coating glass, film speed is 4000rpm, obtains coated glass.
Step 5:Coated glass is heat-treated 3h in 600 DEG C.
Step 6:Coated glass after step 5 is heat-treated, it is placed in the deionized water of 75 DEG C of temperature and cleans, dries, by
This is obtained coated on the SiO on glass2Antireflective coating.
Embodiment performance test
SiO is coated with using prepared by spectrophotometric determination2The transmitance of the glass of antireflective coating, measurement range are
330~1000nm.
Fig. 1 is to scribble SiO prepared by the glass basis and embodiment 3,5,7 determined2The sheet glass of antireflective coating
Transmitance.It will be seen from figure 1 that template used in the present invention and preparation method can significantly improve transmitance.
Fig. 2 is the surface SEM image of embodiment 3,5.Figure it is seen that phosphoric acid can play a part of template, make
The SiO that must be coated on glass substrate2Film, after cleaning in deionized water and removing phosphoric acid, form porous SiO2Antireflective coating,
And its porosity is relevant with phosphoric acid concentration in final colloidal sol.
Phosphoric acid concentration is too high or too low in final colloidal sol can all have a negative impact to the reflection preventing ability of film, therefore too high
Or too low phosphoric acid solubility is not suitable for the present invention.Concrete reason is as follows:In colloidal sol, phosphoric acid molecules can produce aggregation because of hydrogen bond
(hydrogen bond includes the hydrogen bond between hydrogen bond and phosphoric acid molecules and silanol group between phosphoric acid molecules).When phosphoric acid concentration is too high,
Institute's phosphoric acid is excessive in unit volume in final colloidal sol, and phosphoric acid aggregation extent in colloidal sol significantly increases, so as to form big phosphorus
Sour aggregation, these phosphoric acid aggregations can cause occur many oversized holes (> 50nm) in final antireflective coating.This
Subwave grows close hole in a little oversized holes, more especially itself aperture and incident light, can serve as reflection kernel reflect into
Penetrate light, ultimately result in antireflective coating do not have not only antireflective effect conversely can also reduce the transmitance of glass in itself, and phosphoric acid
Concentration is higher, and transmitance declines more.On the contrary, when phosphoric acid concentration is too low, institute's phosphoric acid in final gained colloidal sol unit volume
It is very few, while phosphoric acid aggregation extent is substantially reduced so that the quantity in the hole with suitable dimension is drastically reduced in most telolemma, so as to
The antireflective ability of film is caused to be seriously impaired.
SiO is scribbled described in each embodiment2The transmitance of the sheet glass of antireflective coating is summarized, as shown in table 1.Wherein, pass through
Rate test is to measure at ambient temperature.
SiO is scribbled described in the embodiment of table 12The transmitance of the sheet glass of antireflective coating film is summarized
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (7)
1. a kind of preparation method of antireflective coating, it is characterised in that the antireflective coating is by containing using phosphoric acid as template
Ludox is coated on what is be prepared on glass;The preparation method comprises the following steps:
A, silicon alkoxide, deionized water and the acid catalyst that mol ratio is 1: 3~5: 0.004~0.3 mix, and are stirred under the conditions of frozen water
Obtain solution A;
B, phosphoric acid and diluent, stirring obtain B solution;The mol ratio of the silicon alkoxide, phosphoric acid and diluent is 1: 0.67~0.8
: 29~100;
C, the solution A and B solution are mixed, obtains coating solution;The coating solution is coated on glass, is applied
Film glass;
D, the coated glass is heat-treated under the conditions of 200~1000 DEG C;It is placed in the deionized water of room temperature~100 DEG C clear
Wash, dry, produce coated on the antireflective coating on glass;
The silicon alkoxide is the mixing of one or both of tetraethyl orthosilicate, methyl silicate.
2. the preparation method of antireflective coating as described in claim 1, it is characterised in that the acid catalyst is hydrochloric acid or nitre
Acid.
3. the preparation method of antireflective coating as described in claim 1, it is characterised in that the mass fraction of the phosphoric acid is
10%~85%.
4. the preparation method of antireflective coating as described in claim 1, it is characterised in that the diluent is low alcohol;Institute
Stating low alcohol includes the one or more in methanol, ethanol, propyl alcohol, butanol.
5. the preparation method of antireflective coating as described in claim 1, it is characterised in that in step C, the coating is using rotation
Transfer film method, czochralski method or spraying process.
6. the preparation method of antireflective coating as described in claim 1, it is characterised in that in step D, the heat treatment time
For 0.5~10h.
7. the preparation method of antireflective coating as described in claim 1, it is characterised in that in step D, the temperature of the drying
For 80~200 DEG C;Time is 0.5~4h.
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CN1991411A (en) * | 2005-12-31 | 2007-07-04 | 财团法人工业技术研究院 | Nano aperture type anti-reflection film and method for making same |
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JP2002338303A (en) * | 2001-05-22 | 2002-11-27 | Nissan Motor Co Ltd | Low reflection member |
CN1456523A (en) * | 2002-03-06 | 2003-11-19 | 肖特玻璃制造厂 | Glass with porous coating |
CN1991411A (en) * | 2005-12-31 | 2007-07-04 | 财团法人工业技术研究院 | Nano aperture type anti-reflection film and method for making same |
CN102294179A (en) * | 2011-08-16 | 2011-12-28 | 上海交通大学 | Preparation method of inorganic mesoporous membrane |
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