CN108947266A - A kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film - Google Patents
A kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film Download PDFInfo
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- CN108947266A CN108947266A CN201811000935.4A CN201811000935A CN108947266A CN 108947266 A CN108947266 A CN 108947266A CN 201811000935 A CN201811000935 A CN 201811000935A CN 108947266 A CN108947266 A CN 108947266A
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- collecting pipe
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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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/29—Mixtures
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Composite Materials (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)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a kind of preparation methods of solar vacuum heat-collecting pipe surface anti-reflection film, first prepare acidic sol liquid and alkaline sol liquid respectively；The nano-powder of silica cladding is prepared with sodium metasilicate and titanium dioxide, zinc oxide, aluminium oxide again, and it is modified that surface is carried out to it；Then acidic sol liquid and alkaline sol liquid are mixed, modified nano-powder is added in sealing ageing, and ultrasound obtains coating liquid；Anti-reflection film is finally prepared using dipping-pulling method.Anti-reflection film of the invention not only has good mechanical performance, and wear resistance is good, also has excellent refractive index.
Description
Technical field
The invention belongs to technical field of solar, and in particular to a kind of preparation of solar vacuum heat-collecting pipe surface anti-reflection film
Method.
Background technique
The utilization of solar energy can be avoided environmental crisis brought by fossil energy, while meet growing energy need
It asks.Solar energy optical-thermal, solar photovoltaic utilization technology can solve the supply of industry with thermal energy and electric energy in people's livelihood field.
High-temperature vacuum heat-collecting tube is the key building block in solar light-heat power-generation system, and performance directly determines entirely
The collecting efficiency of system.In order to make sunlight maximumlly penetrate the core that glass enters thermal-collecting tube, sunlight is promoted
Utilization efficiency needs to prepare one layer of optical thin film with anti-reflection effect in glass pipe surface.On the outer glass pipe of thermal-collecting tube,
The reasonable employment of anti-reflection film can reduce the reflection of light, so that more light is entered photo-thermal photoelectric conversion system, making for light is substantially improved
With efficiency, make solar-thermal generating system that there is higher source benefit.Anti-reflection film process production techniques will be solar energy optical-thermal photoelectricity
The important component of system, performance requirement and technical level play a significant role the development of solar energy optical-thermal electro-optical system.
Simultaneously as the use environment of thermal-collecting tube is outdoors, the attachment of dust and pollutant influences whether the light transmission of glass tube, this
Just to the self-cleaning performance of anti-reflection film, more stringent requirements are proposed.Currently, common solar vacuum heat-collecting pipe surface anti-reflection film
It is not able to satisfy self-cleaning requirement.
Summary of the invention
Present invention aim to address above-mentioned deficiencies to provide a kind of preparation side of solar vacuum heat-collecting pipe surface anti-reflection film
Method, anti-reflection film not only have good mechanical performance, and wear resistance is good, also have excellent refractive index.
A kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film, comprising the following steps:
Step 1, in parts by weight, 5-10 parts and hydrochloric acid solution 6-13 parts of ethyl alcohol are mixed, silica solution 7- is added under stirring condition
15 parts, after mixing evenly, 80-150 parts of ethyl alcohol are added, be uniformly mixed, sealing ageing obtains acidic sol liquid；
Step 2, in parts by weight, 2-5 parts of silica solution are added in 20-50 parts of ethyl alcohol, after mixing evenly, under agitation plus
Enter 1-4 parts of ethanol solution of ammonium hydroxide, continue to stir evenly, sealing ageing obtains alkaline sol liquid；
Step 3, in parts by weight, titanium dioxide 3-7 parts of addition, 0.5-1 parts of zinc oxide and aluminium oxide in 100 parts of deionized water
0.5-1 parts, ultrasonic disperse is added sodium silicate aqueous solution 5-10 parts, stirs evenly, and is added dropwise dilute hydrochloric acid solution 10-20 parts and carries out instead
It answers, after being added dropwise, stands, stir, filtering, sediment is calcined, and the nano-powder of silica cladding is obtained；
Step 4, in parts by weight, 10 parts of the nano-powder and silane coupling agent 0.2-0.4 parts, potassium hydroxide step 3 obtained
0.2-0.5 parts of mixing, grinding obtain the modified nano-powder in surface；
Step 5, acidic sol liquid and alkaline sol liquid are mixed, the nano-powder of step 4 is added in sealing ageing, and ultrasound obtains
Coating liquid；
Step 6, in coating liquid substrate slide immersion step 5 obtained, liquid level is lifted out by the speed of 1mm/s, at 20-30 DEG C
After standing is dried, be sent into Muffle furnace be sintered and cooled to get.
Further, the concentration of hydrochloric acid solution is 1mol/L in step 1.
Further, digestion time is 10-15h in step 1.
Further, the concentration of ammonium hydroxide is 20-30% v/v in the ethanol solution of ammonium hydroxide in step 2.
Further, digestion time is 10-15h in step 2.
Further, the concentration of dilute hydrochloric acid solution is 0.1-0.5 mol/L in step 3.
Further, in step 3 calcination temperature be 500-600 DEG C, calcination time 20-30min.
Further, in step 6 sintering temperature be 300-500 DEG C, sintering time 20-30min.
Anti-reflection film of the invention not only has good mechanical performance, and wear resistance is good, also has excellent refractive index.
Specific embodiment
Embodiment 1
A kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film, comprising the following steps:
Step 1, in parts by weight, it is 6 parts of the hydrochloric acid solution mixing of 1mol/L with concentration by 5 parts of ethyl alcohol, is added under stirring condition
7 parts of silica solution, after mixing evenly, 80 parts of ethyl alcohol are added, be uniformly mixed, sealing ageing 12h obtains acidic sol liquid；
Step 2, in parts by weight, 2 parts of silica solution are added in 20 parts of ethyl alcohol, after mixing evenly, ammonia is added under agitation
The concentration of 1 part of the ethanol solution of water, ammonium hydroxide is 20% v/v, continues to stir evenly, and sealing ageing 12h obtains alkaline sol liquid；
Step 3, in parts by weight, 3 parts of titanium dioxide, 0.5 part of zinc oxide and aluminium oxide 0.5 are added in 100 parts of deionized water
Part, ultrasonic disperse is added 5 parts of 40% sodium silicate aqueous solution, stirs evenly, and the dilute hydrochloric acid solution 10 that concentration is 0.5 mol/L is added dropwise
Part is reacted, and after being added dropwise, stands, stirs, filtering, sediment is through calcining, and calcination temperature is 500 DEG C, calcination time is
30min obtains the nano-powder of silica cladding；
Step 4, in parts by weight, 10 parts of the nano-powder and 0.2 part of silane coupling agent, 0.2 part of potassium hydroxide step 3 obtained
Mixing, grinding obtain the modified nano-powder in surface；
Step 5, acidic sol liquid and alkaline sol liquid are mixed, the nano-powder of step 4 is added in sealing ageing, and ultrasound obtains
Coating liquid；
Step 6, in coating liquid substrate slide immersion step 5 obtained, liquid level is lifted out by the speed of 1mm/s, at 20-30 DEG C
After standing is dried, be sent into Muffle furnace sintering, sintering temperature is 300 DEG C, sintering time 30min, it is cooling to get.
Gained anti-reflection film is under 10N loading force, and after the friction of 600s or so, coefficient of friction starts to increase severely, anti-reflection film
Start damaged.It is rubbed 1000 times with wet cotton (alcohol soaks), pressure is 1kg counterweight, and friction velocity is set as 90mm/min, is passed through
It is intact after 1000 frictions.
Under 300nm-800nm visible light, the highest transmissivity of the anti-reflection film is 98.2%.
Embodiment 2
A kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film, comprising the following steps:
Step 1, in parts by weight, it is 9 parts of the hydrochloric acid solution mixing of 1mol/L with concentration by 8 parts of ethyl alcohol, is added under stirring condition
10 parts of silica solution, after mixing evenly, 120 parts of ethyl alcohol are added, be uniformly mixed, sealing ageing 12h obtains acidic sol liquid；
Step 2, in parts by weight, 4 parts of silica solution are added in 35 parts of ethyl alcohol, after mixing evenly, ammonia is added under agitation
The concentration of 2 parts of the ethanol solution of water, ammonium hydroxide is 25% v/v, continues to stir evenly, and sealing ageing 10h obtains alkaline sol liquid；
Step 3, in parts by weight, 5 parts of titanium dioxide, 0.8 part of zinc oxide and aluminium oxide 0.6 are added in 100 parts of deionized water
Part, ultrasonic disperse is added 8 parts of 40% sodium silicate aqueous solution, stirs evenly, and the dilute hydrochloric acid solution 14 that concentration is 0.5 mol/L is added dropwise
Part is reacted, and after being added dropwise, stands, stirs, filtering, sediment is through calcining, and calcination temperature is 500 DEG C, calcination time is
30min obtains the nano-powder of silica cladding；
Step 4, in parts by weight, 10 parts of the nano-powder and 0.3 part of silane coupling agent, 0.4 part of potassium hydroxide step 3 obtained
Mixing, grinding obtain the modified nano-powder in surface；
Step 5, acidic sol liquid and alkaline sol liquid are mixed, the nano-powder of step 4 is added in sealing ageing, and ultrasound obtains
Coating liquid；
Step 6, in coating liquid substrate slide immersion step 5 obtained, liquid level is lifted out by the speed of 1mm/s, at 20-30 DEG C
After standing is dried, be sent into Muffle furnace sintering, sintering temperature is 300 DEG C, sintering time 30min, it is cooling to get.
Gained anti-reflection film is under 10N loading force, and after the friction of 600s or so, coefficient of friction starts to increase severely, anti-reflection film
Start damaged.It is rubbed 1000 times with wet cotton (alcohol soaks), pressure is 1kg counterweight, and friction velocity is set as 90mm/min, is passed through
It is intact after 1000 frictions.
Under 300nm-800nm visible light, the highest transmissivity of the anti-reflection film is 97.8%.
Embodiment 3
A kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film, comprising the following steps:
Step 1, in parts by weight, it is 13 parts of the hydrochloric acid solution mixing of 1mol/L with concentration by 10 parts of ethyl alcohol, adds under stirring condition
Enter 15 parts of silica solution, after mixing evenly, add 150 parts of ethyl alcohol, be uniformly mixed, sealing ageing 12h obtains acidic sol liquid；
Step 2, in parts by weight, 5 parts of silica solution are added in 50 parts of ethyl alcohol, after mixing evenly, ammonia is added under agitation
The concentration of 4 parts of the ethanol solution of water, ammonium hydroxide is 30% v/v, continues to stir evenly, and sealing ageing obtains alkaline sol liquid；
Step 3, in parts by weight, 7 parts of titanium dioxide of addition, 1 part of zinc oxide and 1 part of aluminium oxide in 100 parts of deionized water, surpass
Sound dispersion, is added 10 parts of sodium silicate aqueous solution, stirs evenly, and 20 parts of the dilute hydrochloric acid solution progress that concentration is 0.1 mol/L are added dropwise
Reaction after being added dropwise, stands, stirs, and filtering, sediment is through calcining, and calcination temperature is 600 DEG C, calcination time 20min,
Obtain the nano-powder of silica cladding；
Step 4, in parts by weight, 10 parts of the nano-powder and 0.4 part of silane coupling agent, 0.5 part of potassium hydroxide step 3 obtained
Mixing, grinding obtain the modified nano-powder in surface；
Step 5, acidic sol liquid and alkaline sol liquid are mixed, the nano-powder of step 4 is added in sealing ageing, and ultrasound obtains
Coating liquid；
Step 6, in coating liquid substrate slide immersion step 5 obtained, liquid level is lifted out by the speed of 1mm/s, at 20-30 DEG C
After standing is dried, be sent into Muffle furnace sintering, sintering temperature is 500 DEG C, sintering time 20min, it is cooling to get.
Gained anti-reflection film is under 10N loading force, and after the friction of 600s or so, coefficient of friction starts to increase severely, anti-reflection film
Start damaged.It is rubbed 1000 times with wet cotton (alcohol soaks), pressure is 1kg counterweight, and friction velocity is set as 90mm/min, is passed through
It is intact after 1000 frictions.
Under 300nm-800nm visible light, the highest transmissivity of the anti-reflection film is 98.4%.
Claims (8)
1. a kind of preparation method of solar vacuum heat-collecting pipe surface anti-reflection film, it is characterised in that: the following steps are included:
Step 1, in parts by weight, 5-10 parts and hydrochloric acid solution 6-13 parts of ethyl alcohol are mixed, silica solution 7- is added under stirring condition
15 parts, after mixing evenly, 80-150 parts of ethyl alcohol are added, be uniformly mixed, sealing ageing obtains acidic sol liquid；
Step 2, in parts by weight, 2-5 parts of silica solution are added in 20-50 parts of ethyl alcohol, after mixing evenly, under agitation plus
Enter 1-4 parts of ethanol solution of ammonium hydroxide, continue to stir evenly, sealing ageing obtains alkaline sol liquid；
Step 3, in parts by weight, titanium dioxide 3-7 parts of addition, 0.5-1 parts of zinc oxide and aluminium oxide in 100 parts of deionized water
0.5-1 parts, ultrasonic disperse is added sodium silicate aqueous solution 5-10 parts, stirs evenly, and is added dropwise dilute hydrochloric acid solution 10-20 parts and carries out instead
It answers, after being added dropwise, stands, stir, filtering, sediment is calcined, and the nano-powder of silica cladding is obtained；
Step 4, in parts by weight, 10 parts of the nano-powder and silane coupling agent 0.2-0.4 parts, potassium hydroxide step 3 obtained
0.2-0.5 parts of mixing, grinding obtain the modified nano-powder in surface；
Step 5, acidic sol liquid and alkaline sol liquid are mixed, the nano-powder of step 4 is added in sealing ageing, and ultrasound obtains
Coating liquid；
Step 6, in coating liquid substrate slide immersion step 5 obtained, liquid level is lifted out by the speed of 1mm/s, at 20-30 DEG C
After standing is dried, be sent into Muffle furnace be sintered and cooled to get.
2. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
The concentration of hydrochloric acid solution is 1mol/L in 1.
3. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
Digestion time is 10-15h in 1.
4. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
The concentration of ammonium hydroxide is 20-30% v/v in the ethanol solution of ammonium hydroxide in 2.
5. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
Digestion time is 10-15h in 2.
6. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
The concentration of dilute hydrochloric acid solution is 0.1-0.5 mol/L in 3.
7. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
In 3 calcination temperature be 500-600 DEG C, calcination time 20-30min.
8. the preparation method of solar vacuum heat-collecting pipe surface anti-reflection film according to claim 1, it is characterised in that: step
In 6 sintering temperature be 300-500 DEG C, sintering time 20-30min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109385687A (en) * | 2018-12-21 | 2019-02-26 | 王亚斌 | A kind of preparation method of ageing-resistant fiber |
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| CN101935168A (en) * | 2010-08-25 | 2011-01-05 | 常州大学 | Preparation method of self-cleaning antireflection film with photocatalytic function on surface |
| CN101980379A (en) * | 2010-09-27 | 2011-02-23 | 彩虹集团公司 | Method for preparing anti-reflection and self-cleaning composite membrane for solar cell |
| CN104725990A (en) * | 2015-04-01 | 2015-06-24 | 河北纳诺新材料科技有限公司 | Preparation method of self-cleaning paint based on modified nano titanium dioxide |
| CN106311199A (en) * | 2016-08-24 | 2017-01-11 | 河南大学 | SiO2@TiO2 nuclear shell structure with stable dispersion and controllable photocatalysis, preparing method and application thereof |
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2018
- 2018-08-30 CN CN201811000935.4A patent/CN108947266A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935168A (en) * | 2010-08-25 | 2011-01-05 | 常州大学 | Preparation method of self-cleaning antireflection film with photocatalytic function on surface |
| CN101980379A (en) * | 2010-09-27 | 2011-02-23 | 彩虹集团公司 | Method for preparing anti-reflection and self-cleaning composite membrane for solar cell |
| CN104725990A (en) * | 2015-04-01 | 2015-06-24 | 河北纳诺新材料科技有限公司 | Preparation method of self-cleaning paint based on modified nano titanium dioxide |
| CN106311199A (en) * | 2016-08-24 | 2017-01-11 | 河南大学 | SiO2@TiO2 nuclear shell structure with stable dispersion and controllable photocatalysis, preparing method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109385687A (en) * | 2018-12-21 | 2019-02-26 | 王亚斌 | A kind of preparation method of ageing-resistant fiber |
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Application publication date: 20181207 |