CN102603205A - Forming process of anti-reflecting coating for hood glass tube of solar heat collector tube - Google Patents
Forming process of anti-reflecting coating for hood glass tube of solar heat collector tube Download PDFInfo
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- CN102603205A CN102603205A CN2012100711983A CN201210071198A CN102603205A CN 102603205 A CN102603205 A CN 102603205A CN 2012100711983 A CN2012100711983 A CN 2012100711983A CN 201210071198 A CN201210071198 A CN 201210071198A CN 102603205 A CN102603205 A CN 102603205A
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- glass tube
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- collection pipe
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Abstract
The invention discloses a forming process of an anti-reflecting coating for a hood glass tube of a solar heat collector tube. The forming process comprises the steps of cleaning and further drying and also comprises the following steps that: a processing step at high temperature of placing the hood glass tube into a furnace, and keeping the temperature for 30-40min at the condition of 600 DEG C-625 DEG C; a temperature reducing step of adopting controlled temperature reduction, and basically reducing the temperature to the room temperature with constant speed; an acid etching step of corroding micro pits on the surface of the hood glass tube; a SiO2 film layer preparing step and a film layer curing step. According to the forming process, the controllability is good, the cost is low, and the anti-reflecting coating for the hood glass tube of the solar heat collector tube with higher anti-reflecting effect can be obtained.
Description
Technical field
The present invention relates to a kind of moulding process of solar energy heat collection pipe cover glass tube antireflection coatings, belong to solar heat rete/coating technology field, wherein antireflection coatings also is antireflecting coating.
Background technology
Along with the continuous progress of photothermal technique, increasingly high at the high temperature power field to the requirement of thermal-collecting tube collecting efficiency, there are two kinds of approach to increase the collecting efficiency of thermal-collecting tubes at present, in increasing, the first manages solar absorptance, and another kind then is antireflective, and is promptly anti-reflection.The main similar glass that uses high borosilicate 3.3 glass and modification thereof is as cover glass tube in the industry; Its solar transmission is than generally about 0.89; The sunshine that glass material itself absorbs is about 2%, and therefore reducing the cover glass tube surface reflection through methods such as surface-treateds has important meaning for improving the photo-thermal transformation efficiency.
The anti-reflection technology of current market upper flat plate glass is comparatively extensive, mainly contains magnetron sputtering method, plasma spraying method, chemical Vapor deposition process, sol-gel method, acid corrosion method etc.Physics method plated film mainly is that film hardness is lower, be difficult for being exposed in the physical environment for a long time, and it is more higher than the cost that needs to obtain high solar transmission, is unfavorable for the large-scale application of high-temperature heat-collection pipe in generating.The chemical method cost is comparatively cheap, and film hardness improves, and there is certain degree of difficulty in control but technology is with prescription, is the anti-reflection technology that might be applied to the high temperature pipe.
Summary of the invention
The object of the present invention is to provide that a kind of controllability is good, cost is low and can obtain the moulding process of the solar energy heat collection pipe cover glass tube antireflecting coating of higher antireflective effect.
The present invention adopts following technical scheme:
The moulding process of this invention solar energy heat collection pipe cover glass tube antireflecting coating comprises the step of cleaning and then drying, and is further comprising the steps of:
High temperature processing step: put into stove to cover glass tube, under 600 ℃-625 ℃ condition, be incubated 30 ~ 40 minutes;
Cooling step: adopt controlled cooling, be cooled to room temperature basically evenly;
Acid etching step: go out microscopic pockets in the cover glass tube surface corrosion;
SiO
2Rete preparation process and rete curing schedule.
Prepare the moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating according to the present invention, introduce the antireflection film layer principle, this principle is shown in the theory of Acta PhySico-Chimica Sinica the 13rd volume the 6th interim " the NMR research of phase-splitting of sodium borosilicate glass and leaching " for the boron glass pre-treatment: the certain uniform glass of component is after phase-splitting is handled; Occur inhomogeneous district in the structure, comprise Si-rich phase, rich sodium boron phase, with the rising of phase-splitting treatment temp with submicroscopic size; There are two mechanism to work at the same time: to consider from kinetic factor; Temperature is higher, and glass viscosity is lower, and structural adjustment is accelerated; Phase-splitting speed increases, and the size of phase-separating section increases; Consider that from the thermodynamics angle temperature is higher, the miscible degree of its equilibrium state is bigger, and promptly the sodium in the Si-rich phase, boron and the rich sodium boron silicon in mutually increases.When the rich sodium boron phase size of separating out during much smaller than the visible light optical wavelength, it is transparent that glass keeps.When phase-splitting causes rich sodium boron phase size to surpass the visible light optical wavelength, then cause macroscopic milkiness.Formulate this experimental program, preparation graded films system with anti-reflection the combining of collosol and gel.This belongs to the controllability factor of moulding process.
Adopt this programme can obtain higher solar transmission ratio based on aforementioned principles.Technology has absorbed collosol and gel and surface erosion technology; It is contemplated that the making thinking of advanced gradient film; It can play good antireflective effect anti-reflection ultimate principle and experiment conclusion proof in the long scope of broad harmonic, the solar transmission ratio can improve 2.5%-3%.Key is that film hardness and sticking power improve significantly.Because the corrosion of pre-treatment technology, the cover glass tube surface has produced the concavo-convex of microcosmic, can be good at making SiO
2Rete adheres to, and improves the sticking power of rete, and it is very fast to solve the antireflective coating rate of decay, can't leak aerial unfavorable factor for a long time cruelly, helps large-scale application.In addition, the rete appearance looks elegant, because can be anti-reflection in the wavelength region of broad, so the cover glass tube surface do not show obvious interference color, and surface be light blue, and similar with the cover glass tube background color, defective is less, suitable high temperature pipe application.Simultaneously production cost is lower, utilizes physics method and part chemical process to need three, four layers, even the multilayer wide wavelength antireflective effect that can reach more, the two steps technology of finishing dealing with only, and cost performance is higher.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating is after the acid etching step, SiO
2Also contain a step cleaning step before the rete preparation process, this step requires in the clean room, to use the deionized water rinsing cover glass tube, removes the cover glass tube surface contaminants.
Above-mentioned described solar energy heat collection pipe cover glass tube antireflecting coating moulding process, said high temperature processing step, put into stove to cover glass tube after, the control furnace temperature heats up with the speed of 10 ℃/min.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, the cooling rate of said cooling step are 20 ℃/min.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, said acid etching step are specially the mixing solutions that cover glass tube is put into 25 ℃ of hydrofluoric acid concentration 3%-4% and sulfuric acid concentration 2%-3% and leave standstill 18min ~ 22min, take out.The big solution damage of the concentration of hydrofluoric acid glass surface is serious, the very few function that can not play the cleaner surface; Sulfuric acid mainly is that the dissolved hydrogen fluoric acid corrodes the impurity that gets off, makes cleaning surfaces.Time of repose and temperature and solution are rounded systems, if change can have influence on corrosion layer micropore size and density.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, the acid etching time of acid etching step is preferably 20min.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, the temperature of mixed solution need strict control, guarantee that temperature variation is no more than 1 ℃ up and down.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, said SiO
2It is H that the rete preparation process is specially in mol ratio
2O:TEOS:HCl:C
2H
5Adopt the crystal pulling method plated film in the OH=2.5:1:0.4:20 sol solutions, plated film requires SiO
220 ℃-25 ℃ of envrionment temperatures, humidity 20%-35%.The proportioning of colloidal sol influences the performance and the nanometer SiO of plated film
2Globule size, therefore significantly to the influence of rete transmittance; There is influence in humiture to the apparent mass of rete, and humidity is low excessively, rete solution cracking, and point appears in humidity too high rete easily.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, said rete curing schedule need carry out under envrionment temperature identical with the acid etching step and humidity condition.
The moulding process of above-mentioned solar energy heat collection pipe cover glass tube antireflecting coating, said rete curing schedule are specially cover glass tube are warmed up to 550 ℃ with stove with 5 ℃/min speed, and insulation 50min cools to room temperature with 20 ℃/min speed then.The curing system mainly is to guarantee that ethanol volatilizees with suitable speed, and makes rete produce porous SiO uniformly
2Structure, and make rete have higher physical strength, use value preferably can be arranged.
Description of drawings
Fig. 1 is the structural representation of high-temperature heat-collection pipe cover glass tube antireflection film layer.
Among the figure, 1, cover glass tube, 2, the cover glass tube corrosion layer, 3, SiO
2Antireflection layer.
Embodiment
Moulding process according to a kind of solar energy heat collection pipe cover glass tube antireflecting coating of the present invention; Comprise the step of cleaning and then drying; Wherein cleaning step needs the tube wall of team's cover glass tube to clean; Assurance does not have dirt, to improve the sticking power of rete, need in the clean room, use the deionized water rinsing cover glass tube usually; Then comparatively simple for baking step, fully dry in the drying shed again and get final product; And then this moulding process is further comprising the steps of:
High temperature processing step: put into stove to cover glass tube, under 600 ℃-625 ℃ condition, be incubated 30 ~ 40 minutes; If can obtain reasonable temperature constant state about temperature control is preferable selection, the best control temperature is 610 ℃, in case confirmed controlled temperature, will guarantee the stability of temperature, preferably is controlled in 3 ℃ of scopes up and down of this controlled temperature; Through pyroprocessing can be that the final film hardness that obtains improves; Simultaneously, about the relation between soaking time and the controlled temperature, need guarantee that basically this high temperature processing step controlled temperature interval is a linear relationship substantially in soaking time, best corresponding relation is under 610 ℃ temperature control condition, to be incubated 35 minutes;
Cooling step: adopt controlled cooling; Basically evenly be cooled to room temperature; The influence that refers to the inevitable influence cooling under the controlled condition basically here under existing technical conditions, accomplishes that the absolute linearity cooling is impossible; Has only relative linearity cooling, the cooling that just allows basically;
The acid etching step: go out microscopic pockets in the cover glass tube surface corrosion, the size of microscopic pockets changes through the change of acid etching parameter, confirms through manufacturability;
SiO
2Rete preparation process and rete curing schedule.
Latter two steps can be used conventional similar step and handle under the condition of preceding several steps.
In the above on the basis of general planning, preferable selection be after the acid etching step, SiO
2Be preferably in before the rete preparation process cleaning step is set, this step requires in the clean room, to use the deionized water rinsing cover glass tube, removes the cover glass tube surface contaminants, with the controllability of assurance acid etching and the homogeneity of acid etching.
Preferably, said high temperature processing step, put into stove to cover glass tube after, the control furnace temperature heats up with the speed of 10 ℃/min, avoids violent temperature variation to cause cover glass tube to become fragile, the speed here also is a linear relatively speed certainly, guarantees as much as possible.
Further, the cooling rate of said cooling step is 20 ℃/min, also is based on as a same reason, prevents that the acute variation of temperature from causing cover glass tube to become fragile.Need to prove that intensification here and cooling are not that cover glass self will keep such intensification or cooling extent, but the intensification and the cooling rate of relevant furnace chamber, cover glass tube furnace cooling afterwards.
Preferably, said acid etching step is specially the mixed solution that cover glass tube is put into 25 ℃ of hydrofluoric acid concentration 3%-4% and sulfuric acid concentration 2%-3% and leaves standstill 18min ~ 22min, takes out.Corroding overweight meeting influence cover glass tube intensity, and can hair side occur because produce scattering.Corrosion kicks the beam and is limited to desired influential effect.
Further, the acid etching time of acid etching step is preferably 20min, and the etching time for best under the above-mentioned sour environment condition can guarantee that the hardness of rete is best, and is minimum to the negative impact of matrix simultaneously.Adopting the standard test film hardness with this understanding of GB-T6739-1996 is 5H.
The temperature of mixed solution needs strict control, guarantees that temperature variation is no more than 1 ℃ up and down, and temperature variation is crossed the activity of affects acid solution, causes etching condition out of control.
Preferably, said SiO
2It is H that the rete preparation process is specially in mol ratio
2O:TEOS:HCl:C
2H
5Adopt the crystal pulling method plated film in the OH=2.5:1:0.4:20 sol solutions, plated film requires 20 ℃-25 ℃ of envrionment temperatures, humidity 20%-35%.The scope of above-mentioned envrionment temperature and humidity is an allowed band, should strict control, and ambient moisture is crossed conference makes film surface spot occur, and face is coarse, and the too small meeting of humidity causes the rete cracking.
Further, in order to guarantee to obtain the performance of rete, said rete curing schedule need carry out under envrionment temperature identical with the acid etching step and humidity condition.
Said rete curing schedule is specially cover glass tube is warmed up to 550 ℃ with stove with 5 ℃/min speed, and insulation 50min cools to room temperature with 20 ℃/min speed then, carries out to guarantee that the rete solidified is stable.
Claims (10)
1. the moulding process of a solar energy heat collection pipe cover glass tube antireflecting coating comprises the step of cleaning and then drying, and it is characterized in that, and is further comprising the steps of:
High temperature processing step: put into stove to cover glass tube, under 600 ℃-625 ℃ condition, be incubated 30 ~ 40 minutes;
Cooling step: adopt controlled cooling, be cooled to room temperature basically evenly;
Acid etching step: go out microscopic pockets in the cover glass tube surface corrosion;
SiO
2The rete preparation process; With
The rete curing schedule.
2. the moulding process of solar energy heat collection pipe cover glass tube antireflecting coating according to claim 1 is characterized in that, after the acid etching step, SiO
2Also contain a cleaning step before the rete preparation process, this step requires in the clean room, to use the deionized water rinsing cover glass tube, removes the cover glass tube surface contaminants.
3. the moulding process of described solar energy heat collection pipe cover glass tube antireflecting coating according to claim 1 and 2 is characterized in that, said high temperature processing step, put into stove to cover glass tube after, the control furnace temperature heats up with the speed of 10 ℃/min.
4. the moulding process of solar energy heat collection pipe cover glass tube antireflecting coating according to claim 3 is characterized in that, the cooling rate of said cooling step is 20 ℃/min.
5. the moulding process of solar energy heat collection pipe cover glass tube antireflecting coating according to claim 1 and 2; It is characterized in that; Said acid etching step is specially the mixing solutions that cover glass tube is put into 25 ℃ of wt hydrofluoric acid concentration 3%-4% and wt sulfuric acid concentration 2%-3% and leaves standstill 18min ~ 22min, takes out.
6. the moulding process of solar energy heat collection pipe cover glass tube antireflecting coating according to claim 5 is characterized in that, the acid etching time of acid etching step is preferably 20min.
7. the moulding process of described solar energy heat collection pipe cover glass tube antireflecting coating according to claim 5 is characterized in that, the temperature of mixed solution needs strict control, guarantees that temperature variation is no more than 1 ℃ up and down.
8. the moulding process of solar energy heat collection pipe cover glass tube antireflecting coating according to claim 1 is characterized in that, said SiO
2It is H that the rete preparation process is specially in mol ratio
2O:TEOS:HCl:C
2H
5Adopt the crystal pulling method plated film in the OH=2.5:1:0.4:20 sol solutions, plated film requires 20 ℃-25 ℃ of envrionment temperatures, humidity 20%-35%.
9. according to the moulding process of claim 1 or 8 described solar energy heat collection pipe cover glass tube antireflecting coatings, it is characterized in that said rete curing schedule need carry out under envrionment temperature identical with the acid etching step and humidity condition.
10. the moulding process of solar energy heat collection pipe cover glass tube antireflecting coating according to claim 9; It is characterized in that; Said rete curing schedule is specially cover glass tube is warmed up to 550 ℃ with stove with 5 ℃/min speed, and insulation 50min cools to room temperature with 20 ℃/min speed then.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210071198.3A CN102603205B (en) | 2012-03-19 | 2012-03-19 | Forming process of anti-reflecting coating for hood glass tube of solar heat collector tube |
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| CN201210071198.3A CN102603205B (en) | 2012-03-19 | 2012-03-19 | Forming process of anti-reflecting coating for hood glass tube of solar heat collector tube |
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| CN102603205B CN102603205B (en) | 2014-04-16 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898033A (en) * | 2012-10-26 | 2013-01-30 | 皇明太阳能股份有限公司 | Preparation method and device for antireflection films of outer glass tubes of solar heat collecting tube |
| CN104829144A (en) * | 2015-03-25 | 2015-08-12 | 张小琼 | Eye-moistening protective glass panel and manufacturing method thereof |
| CN109305757A (en) * | 2018-10-17 | 2019-02-05 | 东莞法克泰光电科技有限公司 | A kind of antireflection waterproof glass |
| CN113620597A (en) * | 2021-09-10 | 2021-11-09 | 秦皇岛弘华特种玻璃有限公司 | Borosilicate 3.3 high-performance monolithic fireproof thin glass and preparation method thereof |
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| US4088547A (en) * | 1976-09-01 | 1978-05-09 | Borg-Warner Corporation | Method for producing a coated metal nodular solar heat collector |
| CN1990402A (en) * | 2005-12-28 | 2007-07-04 | 庄大建 | Hurricane-proof glass manufacturing technique |
| CN101387445A (en) * | 2008-10-09 | 2009-03-18 | 姜振友 | High-efficiency vacuum glass thermal-collecting tube and fabrication technology thereof |
| CN101423934A (en) * | 2008-12-02 | 2009-05-06 | 山东力诺新材料有限公司 | Method for preparing solar thermal-collecting tube antireflecting coating |
-
2012
- 2012-03-19 CN CN201210071198.3A patent/CN102603205B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4088547A (en) * | 1976-09-01 | 1978-05-09 | Borg-Warner Corporation | Method for producing a coated metal nodular solar heat collector |
| CN1990402A (en) * | 2005-12-28 | 2007-07-04 | 庄大建 | Hurricane-proof glass manufacturing technique |
| CN101387445A (en) * | 2008-10-09 | 2009-03-18 | 姜振友 | High-efficiency vacuum glass thermal-collecting tube and fabrication technology thereof |
| CN101423934A (en) * | 2008-12-02 | 2009-05-06 | 山东力诺新材料有限公司 | Method for preparing solar thermal-collecting tube antireflecting coating |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898033A (en) * | 2012-10-26 | 2013-01-30 | 皇明太阳能股份有限公司 | Preparation method and device for antireflection films of outer glass tubes of solar heat collecting tube |
| CN102898033B (en) * | 2012-10-26 | 2015-04-15 | 皇明太阳能股份有限公司 | Preparation method and device for antireflection films of outer glass tubes of solar heat collecting tube |
| CN104829144A (en) * | 2015-03-25 | 2015-08-12 | 张小琼 | Eye-moistening protective glass panel and manufacturing method thereof |
| CN109305757A (en) * | 2018-10-17 | 2019-02-05 | 东莞法克泰光电科技有限公司 | A kind of antireflection waterproof glass |
| CN113620597A (en) * | 2021-09-10 | 2021-11-09 | 秦皇岛弘华特种玻璃有限公司 | Borosilicate 3.3 high-performance monolithic fireproof thin glass and preparation method thereof |
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| CN102603205B (en) | 2014-04-16 |
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