CN103466955B - A kind of preparation method of anti reflection glass and filming equipment thereof - Google Patents
A kind of preparation method of anti reflection glass and filming equipment thereof Download PDFInfo
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- CN103466955B CN103466955B CN201310363764.2A CN201310363764A CN103466955B CN 103466955 B CN103466955 B CN 103466955B CN 201310363764 A CN201310363764 A CN 201310363764A CN 103466955 B CN103466955 B CN 103466955B
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Abstract
The invention discloses a kind of preparation method and filming equipment thereof of anti reflection glass.This equipment comprises container for storing liquid and plated film reactor, between container for storing liquid and plated film reactor, be serially connected with under meter and force (forcing) pump from front to back; Its feature is: this plated film reactor is articulated in the top in annealing furnace, and its lower end is 20-40mm apart from the distance of glass delivery roller-way; Under meter is connected with the plating solution import of plated film reactor by force (forcing) pump; The plating solution outlet of plated film reactor is connected with the liquid discharge pipe port at container for storing liquid top by liquid discharge pipe, forms circulation loop.Its preparation method comprises step: 1) prepare plating solution; Place 3-5 days, make its abundant homogenizing; 2) plating solution of homogenizing is put into container for storing liquid, utilize the high pressure that force (forcing) pump produces, through atomizing nozzle atomization, spraying plating, on the glass-board surface passed through, is processed into anti reflection glass; It has, and cost is low, film material is combined jail with substrate glass, weather resisteant is strong, without advantages such as waste gas generations; Be of value to and apply.
Description
Technical field
The present invention relates to a kind of preparation method and filming equipment thereof of anti reflection glass, belong to float glass deep process technology field.
Background technology
Anti reflection glass is coated with anti-reflection film at glass surface, reduces the reflectivity of glass surface, makes glass surface have low reflection and high perspective performance, also referred to as low-reflection glass, anti-glare glass.The reflectivity of simple glass, generally about 8%, also exists the problems such as the dazzling and sharpness that is transmitted image of dazzle is low, even causes the light pollution of environment.Light reflectance is reduced to below 2-3% by 8% by anti reflection glass, makes the light of more than 90% to penetrate simultaneously, creates Clear & Transparent visual space, considerably reduce the reflective of glass, improve the transparent effect of glass.Anti reflection glass has been widely used in photovoltaic cell, television splicing wall, flat panel TV, back projection TV, liquid-crystal display, touch-screen, industrial instrument, senior frame and the occasion need applying low reflection high-penetration glass etc.
A lot, anti reflection glass film based material mainly contains: SiO for antireflecting film based material and technique
2, MgF
2, the single such as ZnSe or multiple material mixed monolayer or multilayer film.Main technique has: magnetron sputtering coating method, sol-gel film coating method, roller coating film coating method, above technique be all must first by finished product float glass through cutting, edging, cleaning, carry out coating film treatment again; Owing to being batch production, efficiency is low, and cost is high, and rete firmness is not strong, and work-ing life is short, seriously hinders applying of this technology.
Summary of the invention
In order to solve the defect existed in above-mentioned prior art, the object of the invention is to provide a kind of method directly can preparing anti reflection glass on floatation glass production line, additionally provides the special filming equipment realizing the method simultaneously.
To achieve these goals, the present invention adopts following technical scheme: a kind of filming equipment of anti reflection glass, and it is positioned on floatation glass production line, and it comprises container for storing liquid and plated film reactor; Its feature is: the top of described plated film reactor hangs and is fixed on the annealing furnace inner cavity top of described floatation glass production line; This plated film reactor is the jacket structure of a rectangular parallelepiped, is provided with plating solution chamber, cooling sap cavity and thermal insulation layer from the inside to the outside successively; 1 gas sampling storehouse be sticked with this thermal insulation layer sidewall is respectively provided with in the outside of thermal insulation layer two side; Described plating solution chamber base plate, cooling sap cavity base plate and thermal insulation layer base plate form the base plate of described plated film reactor; The base plate in 2 described gas sampling storehouses concordant all lower than described plated film reactor base plate and lay respectively at the both sides of this plated film reactor base plate, leave opening between the base plate in gas sampling storehouse and plated film reactor base plate, form the waste gas suction port in described gas sampling storehouse; The base plate of this plated film reactor is provided with some atomization jetting devices by vertically wearing outside thermal insulation layer in plating solution chamber; The bottom distance of this atomization jetting device is 20-40mm by the vertical range of the glass-board surface in described annealing furnace;
Be provided with some atomization jetting devices by vertically wearing outside thermal insulation layer in plating solution chamber on which floor plate; The bottom distance of this atomization jetting device is 20-40mm by the vertical range of the glass-board surface in described annealing furnace;
The liquid exit of described container for storing liquid passes through the plating solution inlet communication of a water influent pipeline and this plated film reactor, and the plating solution outlet of plated film reactor is communicated with the liquid inlet of this container for storing liquid by a drain line; In described water influent pipeline, by container for storing liquid liquid exit to plated film reactor plating solution import between be serially connected with two-way under meter, flowrate control valve, force (forcing) pump and a ball valve successively; Described container for storing liquid is communicated with formation one plating solution circulation loop with described plated film reactor with described drain line by described water influent pipeline.
Above-mentioned atomization jetting device is made up of atomizing nut and atomizing nozzle; The top of this atomizing nut and the lower surface of plating solution chamber base plate affixed, the body of atomizing nut is arranged in cooling sap cavity base plate and thermal insulation layer base plate and affixed with the lower surface of this thermal insulation layer base plate; Plating solution chamber base plate respectively has relative to joint, atomizing nut top the through hole that diameter is less than this atomizing nut internal diameter; Described atomizing nut is arranged in downwards and the atomizing nozzle stretched out by its lower end by through hole.
Above-mentioned plated film reactor is rectangular structure, and the top of thermal insulation layer is concordant with the top in 2 gas sampling storehouses, and on it, level is fixed with a crossbeam; Described plated film reactor is connected with the Interal fixation of described annealing furnace inner cavity top by this crossbeam; The waste gas suction port in 2 gas sampling storehouses is 10-20mm by the vertical range between the base plate of plated film reactor base plate distance gas sampling storehouse; Length in each gas sampling storehouse is equipped with to the upside of end walls the waste gas exhaust pipe be communicated with the waste gas collection device of peripheral hardware respectively.
Above-mentioned atomizing nut is individual to being evenly equipped with 6-12 along the center line length of chamber, described plating chamber base plate, and wide to being evenly equipped with 2-3 row, through hole between row and row misplaces each other; The opening part of each atomizing nozzle lower end is equipped with nozzle plug.
Plating solution import on cooling sap cavity and plating solution chamber is provided with cooling liquid outlet and cooling liquid inlet with on the wallboard held; Wherein, cooling liquid outlet is positioned at the top of this front sheet, and cooling liquid inlet is positioned at the bottom of this front sheet; Described cooling liquid inlet is with thermal insulation layer described in the equal break-through in the outer end of cooling liquid outlet and be communicated with the gangway of peripheral hardware coolant pump respectively by connected pipeline.
Above-mentioned thermal insulation layer is identical with the length in 2 gas sampling storehouses, is 6000-12000mm, forms the length of this plated film reactor; Distance between 2 gas sampling storehouse outer walls is 1000-1900mm, forms the width of this plated film reactor; Be 730-1240mm by the distance between bottom top to the gas sampling storehouse of plated film reactor crossbeam, form the height of this plated film reactor; Wherein, the length in chamber, plating solution chamber is 5700-11400mm, and width is 300-500mm, is highly 400-600mm; Be around in the described cooling sap cavity of periphery, plating solution chamber, its thickness is identical, is 100-200mm; Be around in the described thermal insulation layer of cooling sap cavity periphery, its thickness is identical, is 50-100mm; The transverse width in 2 described gas sampling storehouses is identical, is 200-400mm.
The two-way flow arranged in above-mentioned admission passage is counted 2 flow meter be connected in parallel and is formed; The two ends of every road under meter are all serially connected with Inlet ball valve and the vent ball valve of plating solution flow control, by circulation and the disconnection of the on-off control under meter of Inlet ball valve and vent ball valve; On the pipeline that above-mentioned force (forcing) pump is connected with above-mentioned flowrate control valve and above-mentioned force (forcing) pump with and the pipeline that is connected of the described Inlet ball valve exit connect respectively is serially connected with damping metal soft pipe.
The wallboard in above-mentioned plating solution chamber is welded by anti-corrosion steel plate; The wallboard of cooling sap cavity is welded by high temperature resistant steel plate; Thermal insulation layer is made up of filling alumina silicate fiber felt in heating resisting metal overcoat; The wallboard in 2 gas sampling storehouses is welded by heating resisting metal plate.
Spacing between adjacent 2 atomizing nuts is 50-100mm; Spacing between adjacent two row's atomizing nuts is 50-100mm; The distance that each atomizing nozzle stretches out atomizing nut is 5-10mm; Atomizing nozzle is affixed for being threaded or welding with its plating solution chamber bottom hole; Affixed for being threaded between atomizing nozzle lower end with this atomizing nut bottom.
To achieve these goals, the present invention additionally provides a kind of method utilizing above-mentioned filming equipment to prepare anti reflection glass simultaneously, it comprise floatation glass production line formed glass step and described glass enter and by annealing furnace time, described plated film reactor start-up, plating solution is sprayed, the step of formation of deposits antireflection film layer on this glass-board surface by the glass-board surface in advancing below described atomizing nozzle Vertical dimension; Its concrete operations are as follows:
1) described plating solution is prepared; Get by weight: 90 ~ 95 parts, silicon source, fluorine source doping agent 3 ~ 7 parts, stablizer 0.2 ~ 1 part, catalyzer 0.1 ~ 1 part and 1 ~ 3 part, oxygenant are pre-mixed evenly, place 3-5 days, make its abundant homogenizing;
2) plating solution of step 1) homogenizing is put into container for storing liquid, squeezed in the plating solution chamber of plated film reactor by force (forcing) pump, the high pressure utilizing the pressurization of described force (forcing) pump to be formed, makes its plating solution be atomized by described atomizing nozzle, be ejected on the described glass-board surface that passes through, form antireflection film layer described in one deck;
Wherein, described plated film reactor is mounted in the temperature province of in described annealing furnace 500-600 DEG C.
Above-mentioned steps 1) in silicon source used can select any one in tetraethyl silicate, butyl silicate or silane; Fluorine source doping agent used can select any one in trifluoroacetic acid or magnesium fluoride; Stablizer used can select any one in ethyl acetate, methyl methacrylate, butyl methacrylate or methyl iso-butyl ketone (MIBK); Catalyzer used can select any one in ammoniacal liquor or water; Oxygenant used can select any one in hydrogen peroxide or clorox.
Above-mentioned steps 2) in, the moulding pressure of force (forcing) pump is 5 ~ 10MPa;
Above-mentioned steps 3) in, the antireflective coating thickness that deposition plating solution is formed is 200-500nm.
Owing to have employed technique scheme, beneficial effect of the present invention is as follows: when 1) the present invention utilizes float glass, high, the active strong feature of its surface temperature after glass ware forming, directly anti reflection glass is prepared in the annealing furnace of floatation glass production line, take full advantage of sheet glass heat, be sprayed onto by antireflective coating layer material on the glass surface in advancing and carry out decomposing, depositing, the method forming one deck anti-reflection film at its glass surface is prepared into and subtracts transmitting glass.Effectively reduce that production cost, film material are combined jail with substrate glass, weather resisteant is strong.2) structure of plated film reactor is simple, easy handling, and the setting of atomizing nozzle makes its plating solution spray evenly, effectively ensure that the planeness of rete on glass-board surface.3) whole filming equipment is circularly set, by the totally-enclosed connection of pipeline, and plating solution reusable edible, the waste gas produced in production process is sucked by waste gas suction port at any time, and is discharged at any time by waste gas exhaust pipe, not pollution film layer, ensure the purity of rete, effectively improve the quality of antireflective coating.4) the fluorine-containing silicon-dioxide basement membrane due to admixture in plating solution, its specific refractory power is low; Again because rete reflectivity is different from substrate glass, light has the characteristic of ripple, make use of the principle of interference of light, makes the reflected light of Same Wavelength just in time produce interference at reflex time, rete reflection is reflected with substrate glass just in time offset, reach the object reducing glass-reflected rate.5) owing to there being oxygenant to mix in plating solution, chemical reaction is complete, and coating raw material utilization ratio is high, improves plated film efficiency.6) plating solution used is single fluid, good uniformity, and during by nozzle, drop is tiny, and size is even, produces atomizing effect and can effectively ensure the even of rete.7) owing to adopting high pressure plating solution to be directly atomized, without atomizing medium, greatly reduce exhausted air quantity and produce, be i.e. decreasing pollution, be beneficial to again glass-board surface and clean.Be of value to and apply.
Accompanying drawing explanation
Fig. 1 is the one-piece construction connection diagram of filming equipment of the present invention.
Fig. 2 is that Figure 1A-A is to cross-sectional view.
Fig. 3 is that Figure 1B-B is to cross-sectional view.
Fig. 4 is that Fig. 1 C is to two dimensional structure schematic diagram.
Embodiment
The invention discloses a kind of filming equipment of anti reflection glass, it is positioned on floatation glass production line, and it comprises container for storing liquid and plated film reactor; Wherein, the top of plated film reactor hangs and the annealing furnace inner cavity top be fixed on floatation glass production line; This plated film reactor is the jacket structure of a rectangular parallelepiped, is provided with plating solution chamber, cooling sap cavity and thermal insulation layer from the inside to the outside successively; 1 gas sampling storehouse be sticked with this thermal insulation layer sidewall is respectively provided with in the outside of thermal insulation layer two side; Described plating solution chamber base plate, cooling sap cavity base plate and thermal insulation layer base plate form the base plate of described plated film reactor; The base plate in 2 gas sampling storehouses concordant all lower than described plated film reactor base plate and lay respectively at the both sides of this plated film reactor base plate, leave opening between the base plate in gas sampling storehouse and plated film reactor base plate, form the waste gas suction port in this gas sampling storehouse; Be provided with some atomization jetting devices by vertically wearing outside thermal insulation layer in plating solution chamber on which floor plate; The bottom distance of this atomization jetting device is 20-40mm by the vertical range of the glass-board surface in described annealing furnace.
Container for storing liquid is provided with liquid exit and liquid inlet, and plated film reactor is provided with plating solution outlet and plating solution import; Wherein, liquid exit passes through
onethe plating solution inlet communication of water influent pipeline and this plated film reactor, the plating solution outlet of plated film reactor is passed through
onedrain line is communicated with the liquid inlet of this container for storing liquid; In described water influent pipeline, by container for storing liquid liquid exit to plated film reactor plating solution import between be serially connected with two-way under meter, flowrate control valve, force (forcing) pump and a ball valve successively; Described container for storing liquid is communicated with formation one plating solution circulation loop with described plated film reactor with described drain line by described water influent pipeline.
Cooling liquid outlet and cooling liquid inlet is provided with on the wallboard held at cooling sap cavity and plating solution import; Wherein, cooling liquid outlet is positioned at the top of this front sheet, and cooling liquid inlet is positioned at the bottom of this front sheet; Thermal insulation layer described in the outer end break-through of described cooling liquid inlet and described cooling liquid outlet and being communicated with the gangway of peripheral hardware coolant pump respectively by connected pipeline.
The wallboard in above-mentioned plating solution chamber is welded by anti-corrosion steel plate; The wallboard of cooling sap cavity is welded by high temperature resistant steel plate; Thermal insulation layer is made up of filling alumina silicate fiber felt in heating resisting metal overcoat; The wallboard in gas sampling storehouse is welded by heating resisting metal plate.
Atomization jetting device used is made up of atomizing nut and atomizing nozzle; Wherein, the top of some atomizing nuts is affixed with the lower surface of uniform form and plating solution chamber base plate, and the body of atomizing nut is arranged in cooling sap cavity base plate and thermal insulation layer base plate and affixed with the lower surface of this thermal insulation layer base plate; Plating solution chamber base plate respectively has relative to the joint on some atomizing nut tops the through hole that diameter is less than this atomizing nut internal diameter; Be equipped with downwards by atomizing nut by through hole and the atomizing nozzle stretched out by its lower end; The spacing that atomizing nut bottom is stretched out in this atomizing nozzle lower end is 5-10mm.
Some atomizing nuts are individual to being evenly equipped with 6-12 at the center line length of plating chamber, chamber base plate, and the spacing between adjacent 2 atomizing nuts is 50-100mm; Wide to being evenly equipped with 2-3 row, the spacing between adjacent two row's atomizing nuts is 50-100mm; Through hole between row and row misplaces each other; Atomizing nozzle is affixed for being threaded or welding with plating solution chamber bottom hole; The opening part of each atomizing nozzle lower end is equipped with nozzle plug, and the connection between nozzle plug with atomizing nozzle is for being threaded.
Above-mentioned plated film reactor is rectangular structure, and wherein, the top of thermal insulation layer is concordant with the top in gas sampling storehouse, and on it, level is fixed with a crossbeam; Plated film reactor is connected with the Interal fixation of annealing furnace inner cavity top by this crossbeam; The base plate in 2 gas sampling storehouses is concordant and lower than the base plate of thermal insulation layer, the opening reserved forms the waste gas suction port in this gas sampling storehouse; Length in each gas sampling storehouse is equipped with to the upside of end walls the waste gas exhaust pipe be communicated with the waste gas collection device of peripheral hardware respectively.
The length in thermal insulation layer and gas sampling storehouse is equal, is 6000-12000mm, forms the length of this plated film reactor; Distance between 2 gas sampling storehouse outer walls is 1000-1900mm, forms the width of this plated film reactor; Be 730-1240mm by the distance between bottom cross rail top to gas sampling storehouse, form the height of this plated film reactor; Wherein, the length in plating solution chamber is 5700-11400mm, and width is 300-500mm, is highly 400-600mm; Be around in the cooling sap cavity of periphery, plating solution chamber, its thickness is identical, is 100-200mm; Be around in the thermal insulation layer of cooling sap cavity periphery, its thickness is identical, is 50-100mm; The transverse width in 2 gas sampling storehouses is identical, is 200-400mm; The base plate in this gas sampling storehouse is 10-20mm apart from the spacing of described thermal insulation layer base plate opening.
The two-way flow that water influent pipeline of the present invention is installed is counted 2 flow meter be connected in parallel and is formed; The two ends of every road under meter are all serially connected with Inlet ball valve and the vent ball valve of plating solution flow control, by circulation and the disconnection of the on-off control under meter of Inlet ball valve and vent ball valve; On the pipeline that described force (forcing) pump is connected with described flowrate control valve and described force (forcing) pump with and the pipeline that is connected of the described Inlet ball valve exit connect respectively is serially connected with damping metal soft pipe.
The present invention also disclosed second technical scheme is that provide a kind of method utilizing above-mentioned filming equipment to prepare anti reflection glass, it comprises the conventional steps of floatation glass production line formed glass; Glass to be formed enter and by annealing furnace time, plated film reactor start-up, sprays plating solution, by the step of chemical Vapor deposition process formation of deposits antireflection film layer on this glass-board surface by the glass-board surface in advancing below atomizing nozzle Vertical dimension; This plated film reactor is contained in the temperature province of annealing furnace inner chamber 500-600 DEG C, and its concrete operations are as follows:
1) plating solution used is prepared; Get by weight: 90 ~ 95 parts, silicon source, fluorine source doping agent 3 ~ 7 parts, stablizer 0.2 ~ 1 part, catalyzer 0.1 ~ 1 part and 1 ~ 3 part, oxygenant are pre-mixed evenly, place 3-5 days, make its abundant homogenizing; Put in container for storing liquid and squeeze into plated film reactor plating solution chamber by force (forcing) pump, utilize the high pressure that force (forcing) pump produces, be atomized by atomizing nozzle, spraying plating glass-board surface, form one deck and there is anti-reflection performance film, make glass have reflection preventing ability.
2) plating solution of step 1) homogenizing is put into container for storing liquid, being forced into 5 ~ 10MPa by force (forcing) pump squeezes in the plating solution chamber of plated film reactor, the high pressure formed after utilizing pressurization, by atomizing nozzle, its plating solution is atomized, be ejected on the glass-board surface by annealing furnace again, forming a layer thickness is the antireflection film layer of 200-500nm.
Wherein, any one in tetraethyl silicate, butyl silicate or silane can be selected in silicon source used in step 1); Fluorine source doping agent used can select any one in trifluoroacetic acid or magnesium fluoride; Stablizer used is any one in ethyl acetate, methyl methacrylate, butyl methacrylate or methyl iso-butyl ketone (MIBK); Catalyzer used is any one in ammoniacal liquor or water; Oxygenant used is any one in hydrogen peroxide or clorox.
Below in conjunction with accompanying drawing, technical scheme of the present invention is described in further detail.
As shown in Figure 1, Figure 2, Figure 3 shows, the filming equipment of anti reflection glass of the present invention comprise container for storing liquid 1, two-way under meter, flowrate control valve 6, force (forcing) pump 9, plated film reactor 13 serial connection be integrated form loop.
Specifically be provided with: container for storing liquid 1, waste liquid relief outlet ball valve 2, Inlet ball valve 3,3 ', under meter 4,4 ', vent ball valve 5,5 ', flowrate control valve 6, damping metal soft pipe 8, force (forcing) pump 9, damping metal soft pipe 10, liquid-inlet pipe 11, ball valve 12 and plated film reactor 13; Ball valve 14, plating solution liquid discharge pipe 15, plating solution chamber 16, cooling sap cavity 17, thermal insulation layer 18, cooling fluid goes out pipe 19, cooling fluid inlet pipe 20, gas sampling storehouse 21,21 ', waste gas exhaust pipe 22,22 ', crossbeam 23, atomizing nozzle 24, nozzle plug 25, glass-board surface 26.
Wherein, container for storing liquid 1 is welded with anti-corrosion steel plate, a liquid exit is provided with in the bottom of container for storing liquid 1 sidewall, top is provided with a liquid inlet, a waste liquid relief outlet is provided with in the bottom of container for storing liquid 1, be communicated with the liquid waste collector of peripheral hardware by a drain line, this drain line monitors the ball valve 2 that this waste liquid relief outlet place is also serially connected with a control draining flow, and drain line used selects corrosion-proof steel pipe.
With container for storing liquid 1 liquid outlet on the pipeline of plated film reactor 13 plating solution import, be serially connected with a two-way under meter, flowrate control valve 6 and force (forcing) pump 9 from front to back successively; Wherein, two-way under meter is connected in parallel by 2 under meters 4,4 ', and the front end of each under meter is all serially connected with Inlet ball valve 3,3 ', and rear end is all serially connected with vent ball valve 5,5 '; Flowrate control valve 6 is serially connected in the exit end of two-way under meter; In normal production run, 2 under meters 4,4 ' tunnel work that two-way is arranged, another road is for subsequent use.Opening or closing of the inlet end ball valve be all connected in series by respective front end and exit end ball valve, controls flow meters work that two-way arranges or stopping.
In order to cushion vibrations when force (forcing) pump 9 runs, damping metal soft pipe 8 and damping metal soft pipe 10 are all housed in the front and back end of this force (forcing) pump 9, damping metal soft pipe 8 is above connected with flowrate control valve 6, rear damping metal soft pipe 10 is connected with the plating solution ingress of plated film reactor 13, and the fluid inlet end that the plating solution exit of plated film reactor 13 is offered by a plating solution liquid discharge pipe 15 and container for storing liquid 1 top is communicated with.
Plated film reactor 13 is the rectangular structure of a multilayer, its length is 6000-12000mm, width is 1000-1900mm, is highly 730-1240mm, and its inner chamber is plating solution chamber 16, the periphery in plating solution chamber 16 is a cooling sap cavity 17, the periphery of cooling sap cavity 17 is thermal insulation layer 18; The gas sampling storehouse 21,21 ' of a rectangular parallelepiped is respectively housed outside two side in the length of thermal insulation layer 18.
Wherein, the length in plating solution chamber 16 is 5700-11400mm, and width is 300-500mm, is highly 400-600mm; Plating solution chamber 16 is welded by anti-corrosion steel plate, and its thickness of slab is 5-8mm; What be trapped among plating solution chamber 16 surrounding is cooling sap cavity 17, and the thickness of its surrounding is identical, is 100-200mm, and cooling sap cavity 17 is welded by high temperature resistant steel plate, and this steel plate can the high temperature of resistance to 600-700 DEG C; The thickness of this steel plate is 5-8mm; What be trapped among cooling sap cavity 17 surrounding is thermal insulation layer 18, and the thickness of its surrounding is identical, is 50-100 mm; This thermal insulation layer 18 is formed by filling out alumina silicate fiber felt in heating resisting metal overcoat, and its heat resisting temperature is 600-700 DEG C; The thickness of thermal insulation layer 18 is 40-90mm; In addition, the good lagging material of other heat insulation effect can also be adopted to make thermal insulation layer.
2 gas sampling storehouses 21,21 ' lay respectively at thermal insulation layer 18 long to two side outside, its cross-sectional width is identical, is 200-400mm; In gas sampling storehouse 21, the 21 ' respective length is all equipped with waste gas exhaust pipe 22,22 ' to the top of end walls, the top in gas sampling storehouse 21,21 ' is concordant with the top of thermal insulation layer 18, it is connected with the crossbeam 23 that a plane is greater than 2 tops, gas sampling storehouse and thermal insulation layer 18 top planes; Crossbeam 23 is fixedly connected with the girder steel at annealing furnace top, is hung by plated film reactor 13 and is fixed in below annealing furnace top board.
The base plate in 2 gas sampling storehouses 21,21 ' is concordant, all lower than thermal insulation layer 18 base plate, be an opening between the inner of 2 gas sampling storehouse 21,21 ' base plates and thermal insulation layer 18 base plate, this opening is 10-20mm by gas sampling storehouse 21,21 ' base plate to the vertical range of thermal insulation layer 18 base plate, forms the waste gas suction port in gas sampling storehouse 21,21 '.
2 gas sampling storehouses 21,21 ' are welded by heating resisting metal plate, and the thickness of its heating resisting metal plate is 8-10mm; Waste gas is taken away through connected waste gas pump to the waste gas exhaust pipe 22,22 ' in end walls by 2 gas sampling storehouses are long separately by the waste gas sucked by waste gas suction port.
Plating solution ingress and the plating solution exit of plated film reactor 13 communicate with the inner chamber in plating solution chamber respectively; Be specially: the length in plating solution chamber 16 has the plating solution feed liquor mouth of pipe to one end, the other end has the plating solution discharge opeing mouth of pipe; Wherein, the plating solution feed liquor mouth of pipe is connected with the plating solution liquid-inlet pipe 11 connected with rear damping metal soft pipe 10, and this plating solution liquid-inlet pipe 11 is connected to the ball valve 12 controlling plating solution inlet in the location strings of closing on plated film reactor 13 inlet end; The plating solution discharge opeing mouth of pipe is communicated with plating solution liquid discharge pipe 15, and plating solution liquid discharge pipe 15 is connected to the ball valve 14 controlling plating solution output in the location strings of closing on plated film reactor 13 exit end; The waste liquid foldback of discharging in plated film reactor 13 returns in container for storing liquid 1 by this plating solution liquid discharge pipe 15.
Be provided with cooling fluid liquid outlet at cooling sap cavity 17 and the plating solution inlet end in plating solution chamber 16 with the end wall top of holding, this end wall bottom is provided with cooling fluid fluid inlet; Wherein, cooling fluid fluid inlet is communicated with peripheral hardware cooling pump exit end by a cooling fluid liquid-inlet pipe 20; Cooling liquid outlet is communicated with the cooling fluid withdrawing can of peripheral hardware by a cooling fluid drain pipe 19.
Be positioned at the thermal insulation layer 18 of cooling sap cavity 17 periphery, its top board and crossbeam 23 are welded and fixed; Respectively be welded with thermal insulation layer 18 top is concordant and the rectangular parallelepiped gas sampling storehouse 21,21 ' that length is identical in the both sides of thermal insulation layer 18, the top board in gas sampling storehouse 21,21 ' is fixedly welded in the below of crossbeam 23, and the side plate at two ends, gas sampling storehouse 21,21 ' is respectively equipped with outlet and the extraneous exhaust emission tube 22,22 ' communicated apart from its top board 30-50mm place; The port of gas sampling storehouse 21,21 ' base plate is 10-20mm apart from the vertical range between thermal insulation layer 18 base plate; This spacing constitutes waste gas suction port; Waste gas in production process sucks in respective gas sampling storehouse by suction port bottom two gas sampling storehouses respectively, being discharged by respective exhaust emission tube 22,22 ' enters in the emission-control equipment of peripheral hardware again, make the collection of waste gas and discharge to be in closed state all the time, can not environmental pollution be caused.
Several atomizing nuts 27 be laid in plating solution chamber 16 long to base plate on, and to be worn vertically downward by the base plate in plating solution chamber 16; Atomizing nozzle 24 is set with separately in atomizing nut 27; The upper end of atomizing nozzle 24 communicates with plating solution chamber inner chamber, and atomizing nozzle 24 stretches out downwards through in atomizing nut 27, and its distance of stretching out is 5-10mm; At the lower opening of atomizing nozzle, nozzle plug 25 is housed; The perforate joint of the bottom of the top of atomizing nozzle sleeve 27 and the lower surface of plating solution chamber 16 base plate, atomizing nozzle sleeve 27 and cooling sap cavity 17 base plate and thermal insulation layer 18 base plate is for welding.
Several atomizing nuts 27 are uniform to medullary ray along the length of this plated film reactor 13, and its width arranges 2-3 row, the atomizing nut dislocation arrangement between two rows; 3 row's atomizing nuts are housed in the present embodiment, ranking in the middle of it in plating solution chamber 16 base plate length to medullary ray on, another 2 row's atomizing nuts are parallel with the atomizing nut that centre is arranged with equidistant from distance, and the distance between adjacent two row's atomizing nuts is equal, is 50-100mm; Often row is equipped with 7 atomizing nuts 27, and the distance between adjacent two atomizing nuts 27 is equal, is 50-100mm; 1 atomizing nozzle 24 to lower opening is arranged with in each atomizing nut 27, the length of atomizing nozzle 24 is longer than the length of atomizing nut 27, its top is stretched in plating solution chamber 16, and the bottom of atomizing nut 27 is stretched out in bottom, above the sheet glass that opening passes through in annealing furnace; Connection between atomizing nozzle 24 with plating solution chamber 16 base plate is for being threaded or welding; The opening end of each atomizing nozzle 24 is all equipped with nozzle plug 25, and the connection between nozzle plug 25 and atomizing nozzle 24 opening is that bolt connects.
Plating solution is by being ejected into after nozzle atomization on the glass-board surface 26 that travels through below.
The filming equipment of this anti reflection glass hangs in the temperature province of annealing furnace 500-600 DEG C that is fixed on floatation glass production line, below it process roller-way on be glass-board surface 26, glass-board surface 26 is 20-40mm apart from the distance of atomizing nozzle.
As shown in Figure 4, seen vertically downward by the upper end of this plated film reactor, atomizing nut is evenly equipped with 1 row for 6-12 along the length in this plating solution chamber 16 to medullary ray, be equipped with 7 in present embodiment; Distance between adjacent two atomizing nuts is equal, is 50-100mm; Wide to be laid with 2-3 row, 3 rows are housed in present embodiment, other 2 row lay respectively at medullary ray 1 arrange both sides; Spacing between adjacent two row's atomizing nuts is equal, is 50-100mm; Atomizing nut between adjacent two rows misplaces arrangement each other; Be set with atomizing nozzle 24 in each atomizing nut, the opening part of each atomizing nozzle 24 lower end is all equipped with the nozzle plug mated with this atomizing nozzle; Nozzle plug is threaded with atomizing nozzle 24 port.
Identical at the thickness of cooling sap cavity 17 surrounding of periphery, plating solution chamber 16; The thickness of thermal insulation layer 18 surrounding of cooling fluid intonation 7 periphery is identical; The plating solution feed liquor mouth of pipe communicated with plating solution chamber is connected with plating solution liquid-inlet pipe, and this plating solution liquid-inlet pipe is connected to the ball valve 12 for controlling plating solution inlet in the location strings of closing on the plating solution feed liquor mouth of pipe; The plating solution discharge opeing mouth of pipe communicated with plating solution chamber is connected with a plating solution liquid discharge pipe communicated with container for storing liquid, and this plating solution liquid discharge pipe is connected to the ball valve 14 for controlling plating solution output in the location strings of closing on the plating solution discharge opeing mouth of pipe.
Plating solution is respectively welded with the rectangular parallelepiped gas sampling storehouse 21,21 ' identical with thermal insulation layer 18 length in the both sides of thermal insulation layer 18, the top board in gas sampling storehouse 21,21 ' is fixedly welded in the below of crossbeam 23, and the side plate at two ends, gas sampling storehouse 21,21 ' is respectively equipped with the exhaust emission tube 22,22 ' exporting and be communicated with the emission-control equipment of peripheral hardware apart from its top board 30-50mm place.
In the technical solution of the present invention, under meter used, flowrate control valve and ball valve all can select commercially available any product, and damping metal soft pipe used, force (forcing) pump are the universal product.
In present embodiment, identical with the model that the ball valve 14 that the ball valve 12 that the plating solution liquid-inlet pipe 11 that plating solution chamber 16 communicates is connected in series and plating solution liquid discharge pipe 15 are connected in series is selected, be product that market is purchased, its model is Q41F-100P; The damping metal soft pipe 8 be connected in series with force (forcing) pump 9 and damping metal soft pipe 10 adopt model to be the damping metal soft pipe of 316l, DN25-40; Force (forcing) pump used, its model is 40LYFSB-80 force (forcing) pump.
In present embodiment, cool sap cavity by common stainless steel, as square steel seal welding forms; Be filled with heat conductive circulation oil in this cooling sap cavity, heat conductive circulation oil is commercial products, and its model is the silicone oil of 100#.In addition, sap cavity also available other stainless steel processing is cooled.
Atomizing nozzle used and nozzle plug all can select commercially available conventional atomizing nozzle and the nozzle plug of coupling according to production-scale needs.
Connecting pipeline used in filming equipment of the present invention all can select commercially available corrosion-resistant stainless steel pipe, and its specification is 316l, DN25-40 stainless steel tube; The size of caliber is mated with the interface caliber size of docking in this equipment.
The present invention utilizes above-mentioned filming equipment to prepare the method for anti reflection glass, is further illustrated by following specific examples:
Example 1: through the sheet glass that conventional float glass production line is shaping, enter in the temperature province of annealing furnace 500-600 DEG C, start plated film reactor, plating solution is sprayed, by chemical Vapor deposition process formation of deposits antireflection film layer on this glass-board surface by the glass-board surface in advancing below atomizing nozzle Vertical dimension; The wherein preparation of plating solution:
1) get by weight: tetraethyl silicate 90 parts is selected in silicon source, trifluoroacetic acid 7 parts is selected in the agent of fluorine source doping, stablizer ethyl acetate 0.2 part, catalyzer ammoniacal liquor 0.1 part and 2.7 parts, oxygenant hydrogen peroxide are pre-mixed evenly, place 5 days, make its abundant homogenizing.
2) plating solution of step 1) homogenizing is put into container for storing liquid, is forced into 5 ~ 10MPa by force (forcing) pump; Then squeeze in the plating solution chamber of plated film reactor; Utilize force (forcing) pump to pressurize the high pressure formed, by atomizing nozzle, its plating solution be atomized, then be ejected on the described glass-board surface that passes through, formation a layer thickness is the antireflection film layer of 200-500nm.
Example 2: basic step is with example 1, difference is in the preparation of plating solution: butyl silicate 95 parts is selected in silicon source, magnesium fluoride 3 parts is selected in the agent of fluorine source doping, stablizer methyl methacrylate 0.6 part, catalyzer ammoniacal liquor 0.4 part and oxygenant clorox 1 part are pre-mixed evenly, place 3 days, make its abundant homogenizing.
Example 3: basic step is with example 1, difference is in the preparation of plating solution: 92 parts, silane is selected in silicon source, magnesium fluoride 3 parts, stablizer butyl methacrylate or methyl iso-butyl ketone (MIBK) 1 part is selected in the agent of fluorine source doping, catalyzer ammoniacal liquor 1 part and 3 parts, oxygenant hydrogen peroxide are pre-mixed evenly, place 5 days, make its abundant homogenizing.
In above-mentioned example, plating solution forms the thickness of antireflection film layer usually at 200-500nm, generally determines according to product demand.
Principle of work of the present invention is: in float glass lehr 500-600 DEG C region, utilize annealing furnace temperature, high pressure plating solution extrudes through atomizing nozzle by plated film reactor, plating solution is cut into tiny, fine mist of uniform size, produce atomizing effect, then decompose, be deposited on the glass-board surface of annealing furnace, form vesicular and mix fluorodioxy SiClx film, its specific refractory power is low, because rete reflectivity is different from substrate glass, light has the characteristic of ripple, make use of the principle of interference of light, the reflected light of Same Wavelength is made just in time to produce interference at reflex time, rete reflection is reflected with substrate glass just in time offset, reach the object reducing glass-reflected rate.
The present invention's method used is directly atomized by plating solution, reduces plating solution and decompose in high temperature environments, and the oxide compound decomposing deposition is stablized, and rete void content is high, is all the advantage place being conducive to lowering thin-film refractive index.With the anti reflection glass that equipment of the present invention and method obtain, glass transmitance is greater than 95%, and reflectivity is less than 2%.
Claims (9)
1. a filming equipment for anti reflection glass, it is positioned on floatation glass production line, and it comprises container for storing liquid and plated film reactor; It is characterized in that: the top of described plated film reactor hangs and is fixed on the annealing furnace inner cavity top of described floatation glass production line; This plated film reactor is a jacket structure, is provided with plating solution chamber, cooling sap cavity and thermal insulation layer from the inside to the outside successively; 1 gas sampling storehouse be sticked with this thermal insulation layer sidewall is respectively provided with in the outside of thermal insulation layer two side; Described plating solution chamber base plate, cooling sap cavity base plate and thermal insulation layer base plate form the base plate of described plated film reactor; The base plate in 2 described gas sampling storehouses concordant all lower than described plated film reactor base plate and lay respectively at the both sides of this plated film reactor base plate, leave opening between the base plate in gas sampling storehouse and plated film reactor base plate, form the waste gas suction port in described gas sampling storehouse; The base plate of this plated film reactor is provided with some atomization jetting devices by vertically wearing outside thermal insulation layer in plating solution chamber; The bottom distance of this atomization jetting device is 20-40mm by the vertical range of the glass-board surface in described annealing furnace;
The liquid exit of described container for storing liquid passes through the plating solution inlet communication of a water influent pipeline and this plated film reactor, and the plating solution outlet of plated film reactor is communicated with the liquid inlet of this container for storing liquid by a drain line; In described water influent pipeline, by container for storing liquid liquid exit to plated film reactor plating solution import between be serially connected with two-way under meter, flowrate control valve, force (forcing) pump and a ball valve successively; Described container for storing liquid is communicated with formation one plating solution circulation loop with described plated film reactor with described drain line by described water influent pipeline;
Described atomization jetting device is made up of atomizing nut and atomizing nozzle; The top of described atomizing nut and the lower surface of described plating solution chamber base plate affixed, the body of atomizing nut is arranged in described cooling sap cavity base plate and thermal insulation layer base plate and affixed with the lower surface of this thermal insulation layer base plate; Described plating solution chamber base plate respectively has relative to joint, described atomizing nut top the through hole that diameter is less than this atomizing nut internal diameter; Described atomizing nozzle is arranged in described atomizing nut downwards by this through hole and is stretched out by its lower end;
Described plated film reactor is rectangular structure, and the top of described thermal insulation layer is concordant with the top in described gas sampling storehouse, and on it, level is fixed with a crossbeam; Described plated film reactor is connected with the Interal fixation of described annealing furnace inner cavity top by this crossbeam; Described waste gas suction port is 10-20mm by described plated film reactor base plate apart from the vertical range between the base plate of described gas sampling storehouse; Length in each gas sampling storehouse is equipped with to the upside of end walls the waste gas exhaust pipe be communicated with the waste gas collection device of peripheral hardware respectively.
2. filming equipment as claimed in claim 1, is characterized in that: described atomizing nut is individual to being evenly equipped with 6-12 along the center line length of described plating solution chamber base plate, and wide to being evenly equipped with 2-3 row, through hole between row and row misplaces each other; The opening part of each atomizing nozzle lower end is equipped with nozzle plug;
Cooling liquid outlet and cooling liquid inlet is provided with on the wallboard held at described cooling sap cavity and described plating solution import; Wherein, cooling liquid outlet is positioned at the top of this front sheet, and cooling liquid inlet is positioned at the bottom of this front sheet; Thermal insulation layer described in the outer end break-through of described cooling liquid inlet and described cooling liquid outlet and being communicated with the gangway of peripheral hardware coolant pump respectively by connected pipeline.
3. filming equipment as claimed in claim 2, is characterized in that: the length in described thermal insulation layer and described gas sampling storehouse is equal, is 6000-12000mm, forms the length of described plated film reactor; Distance between 2 described gas sampling storehouse outer walls is 1000-1900mm, forms the width of this plated film reactor; Distance between bottom described cross rail top to described gas sampling storehouse is 730-1240mm, forms the height of this plated film reactor; Wherein, the length in described plating solution chamber is 5700-11400mm, and width is 300-500mm, is highly 400-600mm; Be around in the described cooling sap cavity of periphery, described plating solution chamber, its thickness is identical, is 100-200mm; Be around in the described thermal insulation layer of described cooling sap cavity periphery, its thickness is identical, is 50-100mm; The transverse width in 2 described gas sampling storehouses is identical, is 200-400mm.
4. the filming equipment as described in any one of claim 1-3, is characterized in that: described two-way flow is counted 2 flow meter be connected in parallel and formed; The two ends of every road under meter are all serially connected with Inlet ball valve and the vent ball valve of plating solution flow control, by circulation and the disconnection of the on-off control under meter of Inlet ball valve and vent ball valve; On the pipeline that described force (forcing) pump is connected with described flowrate control valve and described force (forcing) pump with and the pipeline that is connected of the described Inlet ball valve exit connect respectively is serially connected with damping metal soft pipe.
5. filming equipment as claimed in claim 4, is characterized in that: the wallboard in described plating solution chamber is welded by anti-corrosion steel plate; The wallboard of described cooling sap cavity is welded by high temperature resistant steel plate; Described thermal insulation layer is made up of filling alumina silicate fiber felt in heating resisting metal overcoat; The wallboard in described gas sampling storehouse is welded by heating resisting metal plate.
6. filming equipment as claimed in claim 5, is characterized in that: the spacing between adjacent 2 described atomizing nuts is 50-100mm; Spacing between the described atomizing nut of adjacent two row is 50-100mm; The spacing that described atomizing nut bottom is stretched out in described atomizing nozzle lower end is 5-10mm; Described atomizing nozzle is affixed for being threaded or welding with described plating solution chamber bottom hole; Connection between described nozzle plug with described atomizing nozzle is for being threaded.
7. one kind utilizes filming equipment described in any one of claim 1-6 to prepare the method for anti reflection glass, it comprise floatation glass production line formed glass conventional steps and described glass enter and by annealing furnace during, described plated film reactor start-up, plating solution is sprayed, the step of formation of deposits antireflection film layer on this glass-board surface by the glass-board surface in advancing below described atomizing nozzle Vertical dimension; Its concrete operations are as follows:
1) described plating solution is prepared; Get by weight: 90 ~ 95 parts, silicon source, fluorine source doping agent 3 ~ 7 parts, stablizer 0.2 ~ 1 part, catalyzer 0.1 ~ 1 part and 1 ~ 3 part, oxygenant are pre-mixed evenly, place 3-5 days, make its abundant homogenizing;
2) by step 1) plating solution of homogenizing puts into container for storing liquid, squeeze in the plating solution chamber of plated film reactor by force (forcing) pump, utilize the high pressure that the pressurization of described force (forcing) pump is formed, by described atomizing nozzle, its plating solution is atomized, be ejected on the described glass-board surface that passes through, form antireflection film layer described in one deck;
Wherein, described plated film reactor is mounted in the temperature province of in described annealing furnace 500-600 DEG C.
8. method as claimed in claim 7, is characterized in that: step 1) described silicon source is any one in tetraethyl silicate, butyl silicate or silane; The agent of described fluorine source doping is any one in trifluoroacetic acid or magnesium fluoride; Described stablizer is any one in ethyl acetate, methyl methacrylate, butyl methacrylate or methyl iso-butyl ketone (MIBK); Described catalyzer is any one in ammoniacal liquor or water; Described oxygenant is any one in hydrogen peroxide or clorox.
9. method as claimed in claim 8, is characterized in that: step 2) described force (forcing) pump is pressurised into 5 ~ 10MPa; Step 3) deposition plating solution formed antireflective coating thickness be 200-500nm.
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| CN105399342B (en) * | 2014-09-04 | 2018-05-25 | 秦皇岛玻璃工业研究设计院有限公司 | Continuous preparation method and its filming equipment with plural layers anti reflection glass |
| CN111420655A (en) * | 2020-04-18 | 2020-07-17 | 云南正邦科技有限公司 | Method for chemically plating metal catalyst on tube pass inner wall of continuous flow reaction module |
| CN114892144B (en) * | 2022-04-14 | 2023-08-08 | 重庆理工大学 | Atomization-assisted CVD reaction cavity |
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Address after: Hebei Street West Harbor area, 066004 Hebei city of Qinhuangdao province No. 91 Patentee after: Qinhuangdao glass industry research and Design Institute Co., Ltd. Address before: Hebei Street West Harbor area, 066004 Hebei city of Qinhuangdao province No. 91 Patentee before: Qinhuangdao Glass Industry Research and Design Inst. |