CN105753333A - Reflection reducing film on basis of silica sol for glass for heat collecting cover tubes and method for preparing reflection reducing film - Google Patents

Reflection reducing film on basis of silica sol for glass for heat collecting cover tubes and method for preparing reflection reducing film Download PDF

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Publication number
CN105753333A
CN105753333A CN201610047744.8A CN201610047744A CN105753333A CN 105753333 A CN105753333 A CN 105753333A CN 201610047744 A CN201610047744 A CN 201610047744A CN 105753333 A CN105753333 A CN 105753333A
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Prior art keywords
ludox
content
ethanol
weight
auxiliary agent
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CN201610047744.8A
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Inventor
赵其
张文庆
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SHANDONG BEACONERGY ASSOCIATED EQUIPMENT CORP Ltd
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SHANDONG BEACONERGY ASSOCIATED EQUIPMENT CORP Ltd
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Priority to CN201610047744.8A priority Critical patent/CN105753333A/en
Publication of CN105753333A publication Critical patent/CN105753333A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C03C17/009Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/001General methods for coating; Devices therefor
    • C03C17/003General methods for coating; Devices therefor for hollow ware, e.g. containers
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/29Mixtures
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2217/00Coatings on glass
    • C03C2217/40Coatings comprising at least one inhomogeneous layer

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Surface Treatment Of Optical Elements (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention discloses a reflection reducing film on the basis of silica sol for glass of heat collecting cover tubes and a method for preparing the reflection reducing film.The reflection reducing film which is a silicon dioxide anti-reflection film comprises, by weight, 15-20% of the silica sol, 65-80% of ethyl alcohol and additives.The sum of the weight proportions of various components of the reflection reducing film is 100%.The reflection reducing film and the method have the advantages that tetraethyl orthosilicate is directly replaced by the silica sol, inorganic acid or ammonia water which is used as a catalyst can be omitted, hydrolytic processes are omitted, accordingly, the manufacturing cycle can be shortened, and technological processes can be simplified.

Description

Thermal-arrest outer tube glass antireflective coating based on Ludox and preparation method
One, technical field
The present invention relates to a kind of thermal-arrest outer tube glass antireflective coating and preparation method, a kind of thermal-arrest based on Ludox Outer tube glass antireflective coating and preparation method.
Two, background technology
Consisting of of groove type solar high-temperature heat-collection pipe: outer glass enclosure tube, built-in metal pipe, metal sealing part and bellows etc.; Described built-in metal pipe is coated with selective absorbing film, for absorbing the sunshine through outer glass pipe, therefore except built-in metal pipe Absorptivity outside, the transmitance of outer glass pipe is also one of key factor affecting thermal-collecting tube heat absorption efficiency, in identical Putting under the absorptivity of metal tube, the transmitance of sunshine is improved 1% by outer glass enclosure tube, is equivalent to solar thermal collector year effect Rate increases by 2%, and therefore improving transmitance is a kind of extremely effective approach improving thermal-collecting tube efficiency, general high-boron-silicon glass Light transmittance about 91%, by plating antireflection film, its light transmittance stably can be improved to 96%~98%, therefore base Thermal-arrest outer tube glass antireflective coating and preparation method in Ludox are the plated films in a kind of important field of solar energy utilization And process, in existing thermal-arrest outer tube glass antireflective coating based on Ludox and preparation method, solar energy heating The preparation method of the anti-reflection film of pipe outer glass pipe generally uses sol-gel process, colloidal sol prepare current commonly used positive silicic acid Ethyl ester is as preparation SiO2The precursor of colloidal sol, absolute ethyl alcohol as solvent, inorganic acid or ammoniacal liquor as catalyst, by a step Or two step hydrolysis method, prepare silicon dioxide gel, then pulling film forming, during this legal system prepared silicon dioxide colloidal sol, environment warm and humid Spending the impact on finished product very big, and the digestion time needing more than three days and fabrication cycle are long, technique is relative complex, simultaneously The light transmittance of thermal-arrest outer tube and the efficiency absorbing sunshine of thermal-collecting tube are the highest.
Three, summary of the invention
In order to overcome above-mentioned technical disadvantages, it is an object of the invention to provide a kind of thermal-arrest outer tube glass anti-reflection based on Ludox Penetrate film and preparation method, therefore shorten fabrication cycle and simplify technical process.
For reaching above-mentioned purpose, the present invention adopts the technical scheme that: a kind of thermal-arrest outer tube glass based on Ludox Antireflective coating, the raw material of preparing of antireflecting silicon dioxide film is set to include according to part by weight: Ludox 15-20%, ethanol The part by weight sum of 65-80% and adjuvant and each component is set to 100%.
Owing to devising Ludox, ethanol and adjuvant, Ludox is directly used to substitute tetraethyl orthosilicate, not in use by nothing Machine acid or ammoniacal liquor, as catalyst, simplify and have fallen hydrolytic process, therefore shorten fabrication cycle and simplify technical process.
The present invention devises, and a kind of thermal-arrest outer tube glass antireflective coating based on Ludox, refractive index is set to 1.22- The antireflecting silicon dioxide film of 1.34 and prepare raw material and be set to include according to part by weight: Ludox 15-20%, ethanol 65- 80% and the part by weight sum of hole auxiliary agent 0.15-1.3 % and each component be set to 100%, adjuvant is set to hole auxiliary agent.
Owing to devising hole auxiliary agent, after glass tube pulling film forming, when being heat-treated, the pore-forming principle master of pore-forming auxiliary agent If utilizing C-C bond fission at 280 DEG C, form little molecule type organic, thus the pore-forming that volatilizees, make film layer be formed loose porous Structure, therefore improves the light transmittance of thermal-arrest outer tube and the efficiency absorbing sunshine of thermal-collecting tube.
The present invention devises, and Ludox is set to the SiO that particle diameter is 10-100nm2According to part by weight: content is 4.5%- 5% Ludox.
The present invention devises, hole auxiliary agent be set to TrtionX-100, P123, F127 or P103 block copolymer and Include according to part by weight: the content of TrtionX-100 1.1-1.3%, P123 is that the content of 0.15-0.3%, F127 is The content of 0.5-0.55% and P103 is 0.18-0.45%.
The present invention devises, and prepares raw material and includes according to part by weight: Ludox 17-19%, ethanol 77-80% and The content of TrtionX-100 1.2-1.25%, P123 be the content of 0.25-0.3%, F127 be containing of 0.5-0.55% or P103 Amount is set to 100% for the part by weight sum of 0.18-0.45% and each component.
The present invention devises, a kind of thermal-arrest outer tube glass antireflective coating based on Ludox and preparation method, its step It is:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-550 DEG C in temperature Film layer is carried out solidification by border and processes 30-50min.
The present invention devises, and plated film colloidal sol is set to include according to part by weight: Ludox 15-20%, ethanol 65- 80%。
The present invention devises, and it is to be the hydrochloric acid of 0.1-0.5% according to part by weight that the regulation of pH value is set to by addition The pH of ethanol and pore-creating auxiliary agent mixed liquor is adjusted.
The present invention devises, and hole auxiliary agent is set to the block copolymer of TrtionX-100, P123, F127 or P103, in plating Film sol is set to include according to part by weight: the content of TrtionX-100 1.1-1.3%, P123 be 0.15-0.3%, The content of F127 be the content of 0.5-0.55% and P103 be 0.18-0.45%.
The present invention devises, and the refractive index of antireflecting silicon dioxide film is set to 1.22-1.34.
The present invention devises, and the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-380 DEG C in temperature Film layer is carried out solidification by border and processes 30-40min;
Wherein: according to part by weight: Ludox 17-19%, ethanol 77-80% and TrtionX-100 1.2-1.25%, P123's Content be the content of 0.25-0.3% or F127 be 0.5-0.55%.
In the technical program, Ludox is nano level silica dioxide granule dispersion liquid in water or in solvent.By SiO in Ludox2Containing substantial amounts of water and hydroxyl, therefore Ludox can also be expressed as SiO2.nH2O.In the technical program In, TrtionX-100 i.e. Triton X-100,100 (Triton X-100s) are a kind of non-ionic surface Activating agent (or claiming detergent).Molecular weight is 646.86(C34H62O11).
In the technical program, P123 is a kind of triblock copolymer, and full name is: PEO-PPOX- PEO triblock copolymer, its molecular formula is: PEO-PPO-PEO.
In the technical program, F127 i.e. expoxy propane and the copolymer of oxirane;Polyoxyethylene polyoxypropylene, it leads to Formula is HO (C2H4O)a(C3H6O)b(C2H4O)cH.Wherein a and c be 2-130, b be 15-67.It is 81.8 ± 1.9% containing polyoxyethylene.
In the technical program, P103 i.e. chain alkyl triethylamine, is the surfactant of a kind of block structure, and it leads to Formula is EO17PO59EO17
In the technical program, fall during the Ludox of hydrolytic process, ethanol and adjuvant be important for simplifying, had Novelty, creativeness and practicality, the term in the technical program is all can to enter with patent document in the art Row is explained and understands.
Four, accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing skill In art description, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only the present invention Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to according to These accompanying drawings obtain other accompanying drawing.
Fig. 1 is the transmission measurement figure for Sample A 1 of the present invention.
Five, detailed description of the invention
Below in conjunction with embodiment, further describing the present invention, following example are intended to illustrate rather than the present invention Further restriction.
A kind of thermal-arrest outer tube glass antireflective coating based on Ludox,
First embodiment, refractive index be set to 1.22 antireflecting silicon dioxide film and prepare raw material be set to include according to Part by weight: the part by weight sum of Ludox 15%, ethanol 65% and hole auxiliary agent 0.15% and each component is set to 100%.
In the present embodiment, Ludox is set to the SiO that particle diameter is 10nm2According to part by weight: content is that 4.5% silicon is molten Glue.
In the present embodiment, hole auxiliary agent be set to TrtionX-100, P123, F127 or P103 block copolymer and Include according to part by weight: TrtionX-100 1.1%, the content of P123 are 0.15%, the content of F127 is 0.5% and The content of P103 is 0.18%.
Second embodiment, refractive index is set to the antireflecting silicon dioxide film of 1.34 and prepares raw material and be set to include According to part by weight: the part by weight sum of Ludox 20%, ethanol 80% and hole auxiliary agent 1.3 % and each component is set to 100%。
In the present embodiment, Ludox is set to the SiO that particle diameter is 100nm2According to part by weight: content is that 5% silicon is molten Glue.
In the present embodiment, hole auxiliary agent be set to TrtionX-100, P123, F127 or P103 block copolymer and Include according to part by weight: TrtionX-100 1.3%, the content of P123 are 0.3%, the content of F127 is 0.55% and The content of P103 is 0.45%.
3rd embodiment, refractive index is set to the antireflecting silicon dioxide film of 1.29 and prepares raw material and be set to include According to part by weight: the part by weight sum of Ludox 17.5%, ethanol 72.5% and hole auxiliary agent 0.75 % and each component is arranged It is 100%.
In the present embodiment, Ludox is set to the SiO that particle diameter is 55nm2According to part by weight: content is that 4.75% silicon is molten Glue.
In the present embodiment, hole auxiliary agent be set to TrtionX-100, P123, F127 or P103 block copolymer and Include according to part by weight: TrtionX-100 1.2%, the content of P123 are 0.23%, the content of F127 is 0.52% and The content of P103 is 0.32%.
4th embodiment, refractive index is set to the antireflecting silicon dioxide film of 1.22-1.34 and prepares raw material and be set to Include according to part by weight: Ludox 15-20%, ethanol 65-80% and hole auxiliary agent 0.15-1.3 % and the weight of each component Ratio sum is set to 100%.
In the present embodiment, Ludox is set to the SiO that particle diameter is 10-100nm2According to part by weight: content is 4.5%- 5% Ludox.
In the present embodiment, hole auxiliary agent be set to TrtionX-100, P123, F127 or P103 block copolymer and Include according to part by weight: the content of TrtionX-100 1.1-1.3%, P123 is that the content of 0.15-0.3%, F127 is The content of 0.5-0.55% and P103 is 0.18-0.45%.
5th embodiment, prepares raw material and includes according to part by weight: Ludox 17%, ethanol 77% and TrtionX- 100 1.2%, the content of P123 be 0.25%, the content that content is 0.5% or P103 of F127 be 0.18% and each component Part by weight sum is set to 100%.
6th embodiment, prepares raw material and includes according to part by weight: Ludox 19%, ethanol 80% and TrtionX- 100 1.25%, the content of P123 be 0.3%, the content that content is 0.55% or P103 of F127 be 0.45% and each component Part by weight sum is set to 100%.
7th embodiment, prepares raw material and includes according to part by weight: Ludox 18%, ethanol 78.5% and TrtionX- 100 1.225%, the content of P123 be 0.27%, the content that content is 0.52% or P103 of F127 be 0.32% and each component Part by weight sum be set to 100%.
8th embodiment, prepares raw material and includes according to part by weight: Ludox 17-19%, ethanol 77-80% and The content of TrtionX-100 1.2-1.25%, P123 be the content of 0.25-0.3%, F127 be containing of 0.5-0.55% or P103 Amount is set to 100% for the part by weight sum of 0.18-0.45% and each component.
A kind of preparation method of thermal-arrest outer tube glass antireflective coating based on Ludox,
First embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C and environment that humidity is 40%, according to the mode handle that pull rate is 25cm/min lifting plated film The antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, in the environment that temperature is 350 DEG C Film layer is carried out solidification and processes 30min.
In the present embodiment, plated film colloidal sol is set to include according to part by weight: Ludox 15%, ethanol 65%;Silicon is molten Glue and ethanol are set to technical grade.
In the present embodiment, the regulation of pH value is set to by addition is to second according to the hydrochloric acid that part by weight is 0.1% The pH of alcohol and pore-creating auxiliary agent mixed liquor is adjusted.
In the present embodiment, hole auxiliary agent is set to the block copolymer of TrtionX-100, P123, F127 or P103, in plating Film sol is set to include according to part by weight: TrtionX-100 content is 1.1%, the content of P123 is 0.15%, F127 The content that content is 0.5% and P103 be 0.18%.
In the present embodiment, the refractive index of antireflecting silicon dioxide film is set to 1.22.
Second embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 21 DEG C and environment that humidity is 50%, according to the mode handle that pull rate is 30cm/min lifting plated film The antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, in the environment that temperature is 550 DEG C Film layer is carried out solidification and processes 50min.
In the present embodiment, plated film colloidal sol is set to include according to part by weight: Ludox 20%, ethanol 80%;Silicon is molten Glue and ethanol are set to technical grade.
In the present embodiment, the regulation of pH value is set to by addition is to second according to the hydrochloric acid that part by weight is 0.5% The pH of alcohol and pore-creating auxiliary agent mixed liquor is adjusted.
In the present embodiment, hole auxiliary agent is set to the block copolymer of TrtionX-100, P123, F127 or P103, in plating Film sol is set to include according to part by weight: TrtionX-100 content is 1.3%, the content of P123 is 0.3%, F127 Content be the content of 0.55% and P103 be 0.45%.
In the present embodiment, the refractive index of antireflecting silicon dioxide film is set to 1.34.
3rd embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6.25, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 18 DEG C and environment that humidity is 45%, according to the mode that pull rate is 27.5cm/min lifting plated film Antireflecting silicon dioxide film plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, in the environment that temperature is 400 DEG C Film layer is carried out solidification and processes 40min.
In the present embodiment, plated film colloidal sol is set to include according to part by weight: Ludox 17.5%, ethanol 72.5%; Ludox and ethanol are set to technical grade.
In the present embodiment, the regulation of pH value is set to by addition is to second according to the hydrochloric acid that part by weight is 0.3% The pH of alcohol and pore-creating auxiliary agent mixed liquor is adjusted.
In the present embodiment, hole auxiliary agent is set to the block copolymer of TrtionX-100, P123, F127 or P103, in plating Film sol is set to include according to part by weight: TrtionX-100 content is 1.2%, the content of P123 is 0.22%, F127 The content that content is 0.52% and P103 be 0.32%.
In the present embodiment, the refractive index of antireflecting silicon dioxide film is set to 1.28.
4th embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-550 DEG C in temperature Film layer is carried out solidification by border and processes 30-50min.
In the present embodiment, plated film colloidal sol is set to include according to part by weight: Ludox 15-20%, ethanol 65- 80%;Ludox and ethanol are set to technical grade.
In the present embodiment, the regulation of pH value is set to by addition is to be the hydrochloric acid of 0.1-0.5% according to part by weight The pH of ethanol and pore-creating auxiliary agent mixed liquor is adjusted.
In the present embodiment, hole auxiliary agent is set to the block copolymer of TrtionX-100, P123, F127 or P103, in plating Film sol is set to include according to part by weight: TrtionX-100 content be the content of 1.1-1.3%, P123 be 0.15- 0.3%, the content of F127 be the content of 0.5-0.55% and P103 be 0.18-0.45%.
In the present embodiment, the refractive index of antireflecting silicon dioxide film is set to 1.22-1.34.
5th embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-380 DEG C in temperature Film layer is carried out solidification by border and processes 30-40min;
Wherein: according to part by weight: Ludox 17-19%, ethanol 77-80% and TrtionX-100 1.2-1.25%, P123's Content be the content that content is 0.5-0.55% or P103 of 0.25-0.3%, F127 be 0.18-0.45%.
5th embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C and environment that humidity is 40%, according to the mode handle that pull rate is 25cm/min lifting plated film The antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, in the environment that temperature is 350 DEG C Film layer is carried out solidification and processes 30min;
Wherein: according to part by weight: Ludox 17%, ethanol 77% and TrtionX-100 1.2%, the content of P123 is 0.25%, The content of F127 be the content of 0.5% or P103 be 0.18%.
6th embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 21 DEG C and environment that humidity is 50%, according to the mode handle that pull rate is 30cm/min lifting plated film The antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, in the environment that temperature is 380 DEG C Film layer is carried out solidification and processes 40min;
Wherein: according to part by weight: Ludox 19%, ethanol 80% and TrtionX-100 1.25%, the content of P123 is 0.3%, The content of F127 be the content of 0.55% or P103 be 0.45%.
7th embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6.25, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 18 DEG C and environment that humidity is 45%, according to the mode that pull rate is 27.5cm/min lifting plated film Antireflecting silicon dioxide film plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, in the environment that temperature is 365 DEG C Film layer is carried out solidification and processes 35min;
Wherein: according to part by weight: Ludox 18%, ethanol 78% and TrtionX-100 1.22%, the content of P123 are 0.27%, the content of F127 be the content of 0.52% or P103 be 0.32%.
8th embodiment, the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-380 DEG C in temperature Film layer is carried out solidification by border and processes 30-40min;
Wherein: according to part by weight: Ludox 17-19%, ethanol 77-80% and TrtionX-100 1.2-1.25%, P123's Content be the content that content is 0.5-0.55% or P103 of 0.25-0.3%, F127 be 0.18-0.45%.
9th embodiment, it is embodied as step and is:
(1) taking the 200ml beaker of cleaning, 17.5ml industry silicasol and 130ml industry anhydrous ethanol are mixed, dropping hydrochloric acid is adjusted Joint pH to 6-6.5, adds 1.5g binding agent EAA, adds 1.5ml pore creating material triton x-100, stirs, 2h is stirred at room temperature;
(2) Ludox that step (1) prepares is coated with outer tube sheet glass, after having lifted, puts in curing oven, hot setting 30min;
By above step, obtain the surface glass sample with the present embodiment anti-reflection film, be designated as A1, by test, Sample A 1 Transmitance in visible-range up to 99%, mean transmissivity reaches more than 96%.Accompanying drawing 1 is the transmission measurement of Sample A 1 Figure.
Tenth embodiment, it is embodied as step and is:
(1) taking the 200ml beaker of cleaning, 17.5ml industry silicasol and 130ml industry anhydrous ethanol are mixed, dropping hydrochloric acid is adjusted Joint pH to 6-6.5, adds 1.5g binding agent EAA, adds 0.37g pore creating material P123, stirs, 2h is stirred at room temperature;
(3) Ludox that step (1) prepares is coated with outer tube sheet glass, after having lifted, puts in curing oven, hot setting 30min;
By above step, obtain the surface glass sample with the present embodiment anti-reflection film, be designated as A2, by test, Sample A 2 Transmitance in visible-range up to 99%, mean transmissivity reaches more than 96%.
11st embodiment, it is embodied as step and is:
(1) taking the 200ml beaker of cleaning, 17.5ml industry silicasol and 130ml industry anhydrous ethanol are mixed, dropping hydrochloric acid is adjusted Joint pH to 6-6.5, adds 1.5g binding agent EAA, 0.65g pore creating material F127, stirs, 2h is stirred at room temperature;
(2) Ludox that step (1) prepares is coated with outer tube sheet glass, after having lifted, puts in curing oven, hot setting 30min;
By above step, obtain the surface glass sample with the present embodiment anti-reflection film, be designated as A3, by test, Sample A 3 Transmitance in visible-range up to 99%, mean transmissivity reaches more than 96%.
12nd embodiment, it is embodied as step and is:
(1) taking the 200ml beaker of cleaning, 17.5ml industry silicasol and 130ml industry anhydrous ethanol are mixed, dropping hydrochloric acid is adjusted Joint pH to 6-6.5, adds 1.5g binding agent EAA, 0.76g pore creating material P103, stirs, 2h is stirred at room temperature;
(2) Ludox that step (1) prepares is coated with outer tube sheet glass, after having lifted, puts in curing oven, hot setting 30min;
By above step, obtain the surface glass sample with the present embodiment anti-reflection film, be designated as A4, by test, Sample A 4 Transmitance in visible-range up to 99%, mean transmissivity reaches more than 96%.
The present invention has a lower feature:
1, owing to devising Ludox, ethanol and adjuvant, Ludox is directly used to substitute tetraethyl orthosilicate, not in use by inorganic Acid or ammoniacal liquor, as catalyst, simplify and have fallen hydrolytic process, therefore shorten fabrication cycle and simplify technical process.
, owing to devising hole auxiliary agent, after glass tube pulling film forming, when being heat-treated, the pore-forming principle of pore-forming auxiliary agent Mainly by C-C bond fission at 280 DEG C, form little molecule type organic, thus the pore-forming that volatilizees, make film layer be formed loose porous Structure, therefore improve the efficiency absorbing sunshine of the light transmittance of thermal-arrest outer tube and thermal-collecting tube.
, process owing to devising solidification, improve the adhesive force of the quality of film layer and film layer and thermal-arrest outer tube, extend The service life of thermal-collecting tube.
, planform has been carried out the restriction of number range owing to devising, the technical side making number range be the present invention Technical characteristic in case, calculates or is tested by limited number of time the technical characteristic drawn not by formula, and test shows this numerical value The technical characteristic of scope achieves good technique effect.
, owing to devising the technical characteristic of the present invention, in the effect of the set individually and each other of technical characteristic, logical Overtesting shows, the property indices of the present invention is at least 1.7 times of existing property indices, is had by assessment Well market value.
Also have other with Ludox, ethanol and adjuvant be equal to or close technical characteristic is all the enforcement of the present invention One of example, and each technical characteristic of embodiment described above can combine, arbitrarily for meeting Patent Law, patent working Detailed rules and regulations and the requirement of guidelines for examination, no longer to the embodiment of all possible combination of each technical characteristic in above-described embodiment all It is described.
Above-described embodiment is thermal-arrest outer tube glass antireflective coating based on Ludox provided by the present invention and preparation A kind of way of realization of method, according to scheme provided by the present invention other deformation, increase or reduce composition therein or Step, or the present invention is used for other the technical field close with the present invention, belong to protection scope of the present invention.

Claims (10)

1. a thermal-arrest outer tube glass antireflective coating based on Ludox, is characterized in that: preparing of antireflecting silicon dioxide film is former Material is set to include according to part by weight: Ludox 15-20%, ethanol 65-80% and adjuvant and the weight ratio of each component Example sum is set to 100%.
Thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 1, is characterized in that: refractive index sets It is set to the antireflecting silicon dioxide film of 1.22-1.34 and prepares raw material and be set to include according to part by weight: Ludox 15- 20%, the part by weight sum of ethanol 65-80% and hole auxiliary agent 0.15-1.3 % and each component is set to 100%, and adjuvant is arranged For hole auxiliary agent.
Thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 2, is characterized in that: Ludox sets It is set to the SiO that particle diameter is 10-100nm2
Or according to part by weight: content is 4.5%-5% Ludox.
Thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 2, is characterized in that: hole auxiliary agent sets It is set to the block copolymer of TrtionX-100, P123, F127 or P103 and includes according to part by weight: TrtionX-100 The content of 1.1-1.3%, P123 be the content that content is 0.5-0.55% and P103 of 0.15-0.3%, F127 be 0.18- 0.45%。
Thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 2, is characterized in that: prepare raw material Include according to part by weight: Ludox 17-19%, ethanol 77-80% and the content of TrtionX-100 1.2-1.25%, P123 The content that content is 0.5-0.55% or P103 for 0.25-0.3%, F127 is 0.18-0.45% and the weight ratio of each component Example sum is set to 100%.
6. a preparation method for thermal-arrest outer tube glass antireflective coating based on Ludox, is characterized in that: the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-550 DEG C in temperature Film layer is carried out solidification by border and processes 30-50min.
The preparation method of thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 5, its feature It is: plated film colloidal sol is set to include according to part by weight: Ludox 15-20%, ethanol 65-80%;
Or the regulation of pH value is set to by addition be to help ethanol and pore-creating according to the hydrochloric acid that part by weight is 0.1-0.5% The pH of agent mixed liquor is adjusted.
The preparation method of thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 5, its feature It is: hole auxiliary agent is set to the block copolymer of TrtionX-100, P123, F127 or P103, is set to include at plated film colloidal sol According to part by weight: TrtionX-100 content is that the content that content is 0.15-0.3%, F127 of 1.1-1.3%, P123 is The content of 0.5-0.55% and P103 is 0.18-0.45%.
The preparation method of thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 5, its feature It is: the refractive index of antireflecting silicon dioxide film is set to 1.22-1.34.
The preparation method of thermal-arrest outer tube glass antireflective coating based on Ludox the most according to claim 5, its feature It is: the steps include:
A, hole auxiliary agent is added in ethanol, mix formation ethanol and hole auxiliary agent mixed liquor, regulation ethanol and hole auxiliary agent and mix Close the pH value of liquid, make pH value be set to 6-6.5, then add Ludox, obtain plated film colloidal sol;
B, in temperature is 15 DEG C-21 DEG C and environment that humidity is 40%-50%, be 25-30cm/min lifting according to pull rate The mode of plated film is the antireflecting silicon dioxide film of plated film colloidal sol;
C, the thermal-arrest outer tube being coated with antireflecting silicon dioxide film is carried out film layer solidification process, be the ring of 350-380 DEG C in temperature Film layer is carried out solidification by border and processes 30-40min;
Wherein: according to part by weight: Ludox 17-19%, ethanol 77-80% and TrtionX-100 1.2-1.25%, P123's Content be the content that content is 0.5-0.55% or P103 of 0.25-0.3%, F127 be 0.18-0.45%.
CN201610047744.8A 2016-01-25 2016-01-25 Reflection reducing film on basis of silica sol for glass for heat collecting cover tubes and method for preparing reflection reducing film Pending CN105753333A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106966604A (en) * 2017-04-21 2017-07-21 沧州天瑞星光热技术有限公司 Nanometer thin film layer, filming equipment and film plating process for collector tube glass outer tube
CN108609861A (en) * 2018-05-24 2018-10-02 沧州天瑞星光热技术有限公司 A kind of preparation method of resistance to ultraviolet high pull rate antireflective coating
CN112029474A (en) * 2020-09-18 2020-12-04 中国航发沈阳黎明航空发动机有限责任公司 Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof

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CN102225849A (en) * 2011-04-21 2011-10-26 常州大学 Preparation method of glass surface antireflection film without sintering
CN103121856A (en) * 2011-07-25 2013-05-29 重庆文理学院 Preparation method of mesoporous silicon oxide thin film material
CN103420619A (en) * 2013-07-08 2013-12-04 常州大学 Method for preparing anti-reflecting film from silicon dioxide hydrosol

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Publication number Priority date Publication date Assignee Title
CN102225849A (en) * 2011-04-21 2011-10-26 常州大学 Preparation method of glass surface antireflection film without sintering
CN103121856A (en) * 2011-07-25 2013-05-29 重庆文理学院 Preparation method of mesoporous silicon oxide thin film material
CN103420619A (en) * 2013-07-08 2013-12-04 常州大学 Method for preparing anti-reflecting film from silicon dioxide hydrosol

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106966604A (en) * 2017-04-21 2017-07-21 沧州天瑞星光热技术有限公司 Nanometer thin film layer, filming equipment and film plating process for collector tube glass outer tube
CN108609861A (en) * 2018-05-24 2018-10-02 沧州天瑞星光热技术有限公司 A kind of preparation method of resistance to ultraviolet high pull rate antireflective coating
CN112029474A (en) * 2020-09-18 2020-12-04 中国航发沈阳黎明航空发动机有限责任公司 Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof
CN112029474B (en) * 2020-09-18 2022-04-22 中国航发沈阳黎明航空发动机有限责任公司 Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof

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