CN107200580A

CN107200580A - A kind of optical nano ceramic insulation glass for strengthening visible light-transmissive and preparation method thereof

Info

Publication number: CN107200580A
Application number: CN201710478161.5A
Authority: CN
Inventors: 崔明培; 余力; 韩金保; 龙甫强; 邝耀庭; 梁文平; 林改; 苏龙庆
Original assignee: FOSHAN CITY JUSHITAI POWDER METALLURGY Co Ltd
Current assignee: FOSHAN CITY JUSHITAI POWDER METALLURGY Co Ltd
Priority date: 2017-06-21
Filing date: 2017-06-21
Publication date: 2017-09-26
Anticipated expiration: 2037-06-21
Also published as: CN107200580B

Abstract

The present invention relates to functional glass technical field, specially a kind of optical nano ceramic insulation glass for strengthening visible light-transmissive and preparation method thereof.Consistency >=98% for the nano ceramics target being prepared by the method for the present invention, purity >=99.99%.The nano ceramics target prepared on heat insulating function glass using the inventive method, and the first TiO is sequentially formed on the glass substrate₂Layer, by X_mZ_nCs_0.3WO₃The nano ceramics film layer and the 2nd TiO of composition₂Layer, in nano ceramics film layer, the first TiO₂Layer and the 2nd TiO₂Prepared nano ceramics heat-protecting glass is set to be provided simultaneously with the performance of selective absorbing and selective reflecting to solar spectrum under the collective effect of layer, ensure to absorb and reflect well again ultraviolet and infrared ray while visible ray high permeability, and it is simple in construction, not metal-containing layer, the production cost of heat insulating function glass can be reduced, is adapted to industrial production.

Description

A kind of optical nano ceramic insulation glass for strengthening visible light-transmissive and preparation method thereof

Technical field

The present invention relates to functional glass technical field, more particularly to a kind of optical nano ceramics for strengthening visible light-transmissive every Hot glass and preparation method thereof.

Background technology

As developing country, the storage level that China is faced with the energy is not enough, the not high Pressure on Energy of utilization rate.Door and window Glass energy consumption accounts for the 50% of building energy consumption, and energy-saving glass can strengthen the heat-proof quality of door glass, is reduced to cold and hot in equalization chamber Environment and the energy consumption brought, therefore produce the more preferable glass of thermal insulation and reducing energy consumption, played more in terms of promoting building energy conservation Carry out more important effect.The high heat-proof quality of current energy-saving glass is mainly reflected in infrared ray in barrier solar radiation and ultraviolet On linear energy.Various functions preparing film forming of material is attached on glass or directly will be each by industrial many methods using magnetron sputtering Functional material sputtering is planted to use on the glass substrate.Chinese patent CN103342022A is disclosed ZnO by magnetron sputtering method Or ZnSnO_x, silver sputter on glass formed MULTILAYER COMPOSITE layer, be made fire prevention and Low emissivity glass, this glass heat transfer it is few and Can block sunlight to a certain extent.But, glass disclosed in the research is only in terms of heat transfer and stop portions sunlight is reduced Play a role, to stopping that sunshine irradiation brings the limited in one's ability of heat, can not effectively reduce indoor temperature, reduce air-conditioning and bear Lotus is to reach the effect of energy-conservation.Chinese patent CN103587167A discloses a kind of visible ray transmission increasing low emissivity glass, this glass The outer layer of glass posts TiO₂And MgF₂The anti-reflection film of composition, internal layer posts Ag systems low-radiation film, such a glass have to visible ray compared with High transmissivity, has higher reflectivity to infrared and far infrared.Chinese patent CN205416573U discloses one kind can heat Curved infrared block energy-conservation coated glass, sputters 20 layer films, wherein wrapping by the method for vacuum magnetic-control sputtering in glass surface Include the metal alloy layers such as Ag, Cu and SnO₂、ZnSnO_x、TiO_x、ZrO₂And Si₃N₄Deng composite bed, the glass that the method is worked it out Solar energy transmission is low, and winter use can keep heating not to be lost in, play using that can make infrared energy substantially impervious mistake summer The effect of energy-conservation.But, the glass of metal Ag, Cu film is coated with, using easy oxidation deterioration after a period of time, in addition, many Layer magnetron sputtering membrane process is complicated, and cost is high, is unfavorable for industrial production.

Nano ceramic material is a kind of transparent conductive oxide (TCO), mainly with the aluminum oxide of different size, zirconium oxide, Titanium oxide and silica etc. are formed through surface coating, high-temperature firing, and its chemical stability is good, with low reflective, high printing opacity, it is high every Hot the features such as and be widely used.Nano ceramic material is now mostly with plastics or nanometer heat isolation paint.Chinese patent CN102643037A discloses a kind of eva film of functionalization, plated successively on film by way of coating nano yttrium oxide, Nano silicon, nano aluminium oxide, nano zircite, nano calcium oxide, nano titanium oxide, nano zine oxide, nano oxygen Change oxide and the nano cerium doped stannum oxide antimony such as cerium and be made, the visible light transmissivity height of the eva film, ultraviolet light and infrared Light shield is higher.Chinese patent CN104130725A also discloses that a kind of core-shell type infrared resistant auxiliary agent and heat-insulated EVA not gummosis The preparation method of film, wherein counter infrared ray auxiliary agent are made up of the tin ash of Doped Tungsten cerium antimony with EVA resin and organic solvent, EVA Gummosis film is not made up of EVA resin, counter infrared ray auxiliary agent, coupling agent, crosslinking agent and ultraviolet absorber, this not gummosis film significantly improve Ultraviolet and ultrared rejection rate, thickness homogeneity are high.Chinese patent CN104275889A discloses a kind of high-performance and received Then rice compound heat-insulation film, the manufacturing process of this thermal isolation film be coated with one layer to form sputtering layer by sputtering first on pet layer Tungstic acid adiabatic gum, is combined one layer of pet layer, is coated one layer of installation being made up of polyacrylate resin and ultraviolet absorber Layer, finally for by surface-treated laminated polyester film.This film has excellent visible light transmissivity and infrared and ultraviolet resistance Every rate, and with good mechanical performance, scratch resistant performance and high and low temperature resistance.Chinese patent CN105778830A is disclosed A kind of preparation method of the heat-insulated PVB films of spectral selectivity nano, this patent by near-infrared long wave obstruct nano material dispersion liquid, Near-infrared shortwave nano dispersion fluid and near-infrared reflection nano dispersion fluid are mixed with PVB so that film is in visible ray high transmittance While high, near infrared ray can be absorbed and reflected well again.Near-infrared length wave resistance is every nano material dispersion liquid by dividing LaB is added in powder₆、ScB₆Deng be made, near-infrared long wave barrier by wetting dispersing agent and defoamer add ITO, ATO, The metal oxides such as AZO and Ce-ATO are made.EVA disclosed in studying above, PET, PVB is organic high molecular polymer, Easy aging is chronically exposed in air, and has the energy-absorbing group such as-C-O-, C=O ,-OH in polymer, easily causes a nanometer material The thermal contraction of material.

The content of the invention

The present invention needs further raising for existing energy-saving glass energy-saving effect, and the problems such as easy aging there is provided A kind of number of plies is less, non-aging, possess good spectral selection to sunshine while can improve visible light transmissivity Absorb and reflection optical nano ceramic insulation glass, and this kind of optical nano ceramic insulation glass preparation method.

To achieve the above object, the present invention uses following technical scheme.

It is a kind of to strengthen the optical nano ceramic insulation glass of visible light-transmissive, including glass baseplate, in the glass baseplate On be sequentially provided with the first TiO₂Layer, nano ceramics film layer and the 2nd TiO₂Layer；The nano ceramics film layer is by X_mZ_nCs_0.33WO₃Structure Into；Wherein, X is Ce or Y or Er or Yb and Gd, Z are Sn or Sb or Bi, m are 0.001-0.1, and n is 0.001-0.1.

It is preferred that, the first TiO₂Layer is rutile type nano TiO₂Layer.It is furthermore preferred that the first TiO₂The thickness of layer Spend for 15-50nm.

It is preferred that, the 2nd TiO₂Layer is anatase type nano TiO₂Layer.It is furthermore preferred that the 2nd TiO₂The thickness of layer Spend for 25-65nm.

It is preferred that, the thickness of the nano ceramics film layer is 100-300nm.

The preparation method of the optical nano ceramic insulation glass of enhancing visible light-transmissive described above, comprises the following steps：

S1 prepares precursor powder：Solution B, solution C and colloidal sol D are well mixed, solution E is obtained；Then by solution E with it is transparent Sol A is well mixed, and colloidal sol F is made；Then make after colloidal sol F gelations, and scrubbed and drying process, obtain precursor powder.

It is preferred that, solution E is added drop-wise in vitreosol A dropwise, and return stirring 3-5 hours at 70-80 DEG C, is formed Colloidal sol F；Colloidal sol F is placed in 70-120 DEG C of vacuum environment, makes its gelation, is washed out and centrifugal treating, gel is put 10-24h is freeze-dried in -40-20 DEG C of vacuum environment, precursor powder is obtained.

The vitreosol A is the vitreosol of tungsten compound；The solution B is the solution of cesium compound；The solution C For the solution containing Sn or Sb or Bi compound；The colloidal sol D is transparent molten for the compound containing Ce or Y or Er or Yb or Gd Glue.The ratio between contained element X, element Z, Cs and W amount of material are in the vitreosol A, solution B, solution C and colloidal sol D 0.001-0.1:0.001-0.1:0.33:1。

It is preferred that, the tungsten compound is tungsten hexachloride, and the cesium compound is cesium chloride.

It is preferred that, the vitreosol A is dissolved in absolute ethyl alcohol by tungsten compound is made into clear solution, and clear solution exists Formed within return stirring 2-4 hours at 70-80 DEG C.

It is preferred that, the solution B is dissolved in deionized water by cesium compound, stirs to be formed.

It is preferred that, the solution C is that the chloride containing Sn or Sb or Bi is dissolved in formation in deionized water.

It is preferred that, the colloidal sol D is that the chloride containing Ce or Y or Er or Yb or Gd is dissolved in absolute ethyl alcohol, and in 70-80 Return stirring is formed for 1 hour at DEG C.

S2 prepares nano-ceramic powder：After precursor powder is handled through high temperature sintering, nano-ceramic powder is made.

It is preferred that, precursor powder is placed in high temperature furnace, while hydrogen and nitrogen/inert gas are passed through, nitrogen/indifferent gas Body is 3-10 with hydrogen flowing quantity ratio：1, temperature is risen to 350-650 DEG C with 1-3 DEG C/min programming rate, 2-3h is incubated；Then Stop heating, after carrying out milled processed after cooling down, obtain nano-ceramic powder.

S3 prepares nano ceramics target：Nano-ceramic powder is fitted into mould, nano-ceramic powder is placed in very with mould Reciprocal of duty cycle is 6.0 × 10^-3In Pa environment, nano-ceramic powder is 10-30Mpa in pressure, and temperature is 500-1000 DEG C of condition Lower heat-insulation pressure keeping 1-3h；Obtain nano ceramics target.

It is preferred that, consistency >=98% of the nano ceramics target, purity >=99.99%.

It is preferred that, first apply 5-15Mpa pressure to the nano-ceramic powder in mould, then vacuumize, vacuum is 10^-2-10^-3Pa, and heated while vacuumizing, heating rate is 1-20 DEG C/min, is incubated when temperature rises to 100-300 DEG C 10-40min；Then the nano-ceramic powder in mould is pressurized and heated up, pressure rises to 15-30Mpa, and temperature rises to 500- 1000℃；It is incubated after 1-3h and cools down, obtains nano ceramics target.

It is preferred that, heat resistant spacer layer is provided between the nano-ceramic powder and mould.It is furthermore preferred that the separation layer is The scattered boron nitride of polyvinyl alcohol.

S4 makes functional layer：Respectively with TiO₂It is magnetic control spattering target with nano ceramics target, on the glass substrate successively Plate the first TiO₂Layer, nano ceramics film layer and the 2nd TiO₂Layer, is made optical nano ceramic insulation glass.

It is preferred that, in vacuum<2.0×10^-3In the environment of Pa, argon gas and oxygen, the stream of the argon gas and oxygen are passed through Amount is than being 2-8:1, magnetron sputtering plating is then carried out with 50-200W power.

It is preferred that, with rutile type nano TiO₂Form the first TiO on the glass substrate for magnetic control spattering target₂Layer, institute State the first TiO₂Layer is rutile type nano TiO₂Layer.

It is preferred that, with anatase type nano TiO₂Form the 2nd TiO on the glass substrate for magnetic control spattering target₂Layer, institute State the 2nd TiO₂Layer is anatase type nano TiO₂Layer.

Compared with prior art, the beneficial effects of the invention are as follows：The present invention passes through appropriate vitreosol A, solution B, molten Liquid C and colloidal sol D, which prepare the nano ceramics target to be formed, has the characteristics of good stability, not oxidizable and aging, applied to heat-insulated The problem of existing heat insulating function glass has easy aging can be solved on functional glass.By controlling each technique in preparation process to join Number, the material for being effectively reduced nano ceramics target in preparation process is reduced and the problem of precipitating metal simple substance, and avoids institute There is stomata and causes consistency not high enough in nano ceramics target processed.The cause for the nano ceramics target being prepared by the method for the present invention Density >=98%, purity >=99.99%.The nano ceramics target prepared on heat insulating function glass using the inventive method, and The first TiO is sequentially formed on the glass substrate₂Layer, by X_mZ_nCs_0.3WO₃The nano ceramics film layer and the 2nd TiO of composition₂Layer, is receiving Rice ceramic film, the first TiO₂Layer and the 2nd TiO₂Make prepared nano ceramics heat-protecting glass to the sun under the collective effect of layer Spectrum is provided simultaneously with the performance of selective absorbing and selective reflecting, it is ensured that can be absorbed well again while visible ray high permeability With reflection ultraviolet and infrared ray, and simple in construction, not metal-containing layer, it is possible to decrease the production cost of heat insulating function glass is adapted to Industrial production.

Brief description of the drawings

Fig. 1 is the nano ceramics film layer SEM cross-sectional views of embodiment 3；

Fig. 2 is UV-VL-NIR (300-2500nm) transmitted light of optical nano ceramic insulation glass prepared by embodiment 3 Spectrogram and reflectance spectrum figure；

Fig. 3 be embodiment 4 in nano-ceramic powder XRD；

Fig. 4 be embodiment 18 in optical nano ceramic insulation glass BL18 XRD.

Embodiment

In order to more fully understand the technology contents of the present invention, with reference to specific embodiment to technical scheme It is described further and illustrates.

Embodiment 1

The present embodiment provides a kind of optical nano ceramic insulation glass of enhancing visible light-transmissive, specific as follows：

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 2 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 1.14g trichloride antimonies, which are dissolved in deionized water, forms solution C, 1.23g Cerous chloride is dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D stirrings Solution E is well mixed to obtain, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form the colloidal sol of transparent and homogeneous for 4 hours. Colloidal sol is placed in 90 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in cold in -40 DEG C of vacuum environments Dry 24h is freezed, Ce is obtained_0.01Sb_0.01Cs_0.33WO₃Precursor powder.

Again by Ce_0.01Sb_0.01Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 500 DEG C, heating rate is 1 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2.5h is incubated after heating, waits to drop Disperse grinding after temperature cooling and produce Ce_0.01Sb_0.01Cs_0.33WO₃Nano-ceramic powder.

By obtained Ce_0.01Sb_0.01Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 5MPa pressure to powder to nano-ceramic powder Precompressed is carried out, then is vacuumized, vacuum is 3.0 × 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 6 DEG C/min, 20min is incubated when being warming up to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 6 DEG C/min, and pressure is upgraded to 20MPa, stops heating up and carries out maintaining 2.5h under heat-insulation pressure keeping, this process conditions when temperature is 550 DEG C, and then annealing is obtained The Ce of high-compactness_0.01Sb_0.01Cs_0.33WO₃Nano ceramics target, is designated as BC1, and consistency is 98.5%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1.5 × 10-3Pa, then is passed through argon gas and oxygen, argon gas Flow-rate ratio with oxygen is 2:1, magnetron sputtering power supply is then opened, power 80W is adjusted, 15nm rutile type nanos is plated successively Titanium dioxide layer, 150nm ternary doping nano ceramics film layers and 25nm anatase-type nanometer titanium dioxides layer.

Embodiment 2

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 2 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 5.7g trichloride antimonies, which are dissolved in deionized water, forms solution C, 6.15g tri- Cerium chloride is dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D stirrings are mixed Conjunction is uniform to obtain solution E, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form the colloidal sol of transparent and homogeneous for 4 hours.Will Colloidal sol is placed in 90 DEG C of vacuum environments, after after gelation, and by washing, alcohol is washed three times, then is placed in freezing in -20 DEG C of vacuum environments 24h is dried, Ce is obtained_0.05Sb_0.05Cs_0.33WO₃Precursor powder.

Again by Ce_0.05Sb_0.05Cs_0.33WO₃Be placed in high temperature furnace, sintering temperature be 450 DEG C, heating rate be 1.5 DEG C/ Min, while being passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, is treated Disperse grinding after cooling down and produce Ce_0.05Sb_0.05Cs_0.33WO₃Nano-ceramic powder.

By obtained Ce_0.05Sb_0.05Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 10MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 8.0 × 10^-3Pa, is started to warm up while vacuumizing, heating rate be 10 DEG C/ Min, is incubated 30min when being warming up to 250 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, pressure 20MPa is upgraded to, stops heating up when temperature is 750 DEG C and carries out maintaining 1h under heat-insulation pressure keeping, this process conditions, then anneal To the Ce of high-compactness_0.05Sb_0.05Cs_0.33WO₃Nano ceramics target, is designated as BC2, and consistency is 99.5%, and purity is 99.995%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 35nm rutile type nanos two is plated successively Titanium oxide layer, 250nm ternary doping nano ceramics film layers and 50nm anatase-type nanometer titanium dioxides layer.

Embodiment 3

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 2 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 6.3g bismuth trichlorides, which are dissolved in deionized water, forms solution C, 2.73g chlorine Change erbium to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D stirring mixing is equal It is even to obtain solution E, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form the colloidal sol of transparent and homogeneous for 4 hours.By colloidal sol Be placed in 80 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then be placed in -30 DEG C of vacuum environments freeze it is dry Dry 20h, obtains Er_0.02Bi_0.04Cs_0.33WO₃Precursor powder.

Again by Er_0.02Bi_0.04Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 550 DEG C, heating rate is 3 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, waits to cool Disperse grinding after cooling and produce Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

By obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-2Pa, is started to warm up while vacuumizing, and heating rate is 15 DEG C/min, is risen 30min is incubated when temperature is to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, stops heating up and carries out maintaining 1.5h under heat-insulation pressure keeping, this process conditions when temperature is 800 DEG C, and then annealing obtains height The Er of consistency_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC3, and consistency is 99.8%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 8:1, magnetron sputtering power supply is then opened, power 50W is adjusted, 30nm rutile type nano dioxies is plated successively Change titanium layer, 200nm ternary doping nano ceramics film layers and 40nm anatase-type nanometer titanium dioxides layer.Nano ceramics film layer SEM Cross section is as shown in Figure 1；UV-VL-NIR (300-2500nm) transmitted light spectrograms and reflected light of optical nano ceramic insulation glass Spectrogram is as shown in Figure 2.

Embodiment 4

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 0.23g trichloride antimonies, which are dissolved in deionized water, forms solution C, 0.70g Ytterbium chloride is dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D stirring mixing It is uniform to obtain solution E, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form the colloidal sol of transparent and homogeneous for 3 hours.Will be molten Glue is placed in 90 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum environments and is freezed 15h is dried, Yb is obtained_0.005Sb_0.002Cs_0.33WO₃Precursor powder.

Again by Yb_0.005Sb_0.002Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 450 DEG C, heating rate is 3 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, waits to cool Disperse grinding after cooling and produce Yb_0.005Sb_0.002Cs_0.33WO₃Nano-ceramic powder, XRD such as Fig. 3 institutes of nano-ceramic powder Show.

By obtained Yb_0.005Sb_0.002Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is risen 30min is incubated when temperature is to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, stops heating up and carries out maintaining 1h under heat-insulation pressure keeping, this process conditions when temperature is 1000 DEG C, and then annealing obtains height The Yb of consistency_0.005Sb_0.002Cs_0.33WO₃Nano ceramics target, is designated as BC4, and consistency is 99.9%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 50nm rutile type nanos two is plated successively Titanium oxide layer, 300nm ternary doping nano ceramics film layers and 65nm anatase-type nanometer titanium dioxides layer.

Embodiment 5

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 5.70g anhydrous stannous chlorides, which are dissolved in deionized water, forms solution C, 3.95g gadolinium chlorides are dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D is stirred Well mixed solution E is mixed, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form the molten of transparent and homogeneous in 5 hours Glue.Colloidal sol is placed in 80 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum rings 15h is freeze-dried in border, Gd is obtained_0.03Sn_0.06Cs_0.33WO₃Precursor powder.

Again by Gd_0.03Sn_0.06Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 500 DEG C, heating rate is 3 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, waits to cool Disperse grinding after cooling and produce Gd_0.03Sn_0.06Cs_0.33WO₃Nano-ceramic powder.

By obtained Gd_0.03Sn_0.06Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is risen 30min is incubated when temperature is to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, stops heating up and carries out maintaining 1h under heat-insulation pressure keeping, this process conditions when temperature is 800 DEG C, and then annealing obtains high cause The Gd of density_0.03Sn_0.06Cs_0.33WO₃Nano ceramics target, is designated as BC5, and consistency is 99.9%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 4:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 35nm rutile type nanos two is plated successively Titanium oxide layer, 250nm ternary doping nano ceramics film layers and 45nm anatase-type nanometer titanium dioxides layer.

Embodiment 6

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and the anhydrous bismuth chlorides of 15.76g, which are dissolved in deionized water, forms solution C, 0.10g yttrium chlorides are dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D is stirred Well mixed solution E is mixed, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form the molten of transparent and homogeneous in 4 hours Glue.Colloidal sol is placed in 90 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -30 DEG C of vacuum rings 24h is freeze-dried in border, Y is obtained_0.001Bi_0.1Cs_0.33WO₃Precursor powder.

Again by Y_0.001Bi_0.1Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 500 DEG C, heating rate is 3 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, waits to cool Disperse grinding after cooling and produce Y_0.001Bi_0.1Cs_0.33WO₃Nano-ceramic powder.

By obtained Y_0.001Bi_0.1Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, and graphite jig connects with powder Contacting surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 10MPa pressure to powder to nano-ceramic powder Precompressed is carried out, then is vacuumized, vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, heating 30min is incubated during to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 20MPa, stops heating up and carries out maintaining 1h under heat-insulation pressure keeping, this process conditions when temperature is 700 DEG C, and then annealing obtains high cause The Gd of density_0.03Sn_0.06Cs_0.33WO₃Nano ceramics target, is designated as BC6, and consistency is 99.93%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 50nm rutile type nanos two is plated successively Titanium oxide layer, 300nm ternary doping nano ceramics film layers and 50nm anatase-type nanometer titanium dioxides layer.

Embodiment 7

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and the anhydrous bismuth chlorides of 6.30g, which are dissolved in deionized water, forms solution C, 1.23g anhydrous cerium chlorides are dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D is uniformly mixed to obtain solution E, and solution E is slowly dropped in Sol A, and 76 DEG C of return stirrings form transparent and homogeneous in 4 hours Colloidal sol.Colloidal sol is placed in 90 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -30 DEG C of vacuum 24h is freeze-dried in environment, Ce is obtained_0.01Bi_0.04Cs_0.33WO₃Precursor powder.

Again by Ce_0.01Bi_0.04Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 400 DEG C, heating rate is 2 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, waits to cool Disperse grinding after cooling and produce Ce_0.01Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

By obtained Ce_0.01Bi_0.04Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 10MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 8 DEG C/min, heating 40min is incubated during to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 20MPa, stops heating up and carries out maintaining 1h under heat-insulation pressure keeping, this process conditions when temperature is 600 DEG C, and then annealing obtains high cause The Ce of density_0.01Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC7, and consistency is 99.9%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 40nm rutile type nanos two is plated successively Titanium oxide layer, 200nm ternary doping nano ceramics film layers and 60nm anatase-type nanometer titanium dioxides layer.

Embodiment 8

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and the anhydrous antimony chlorides of 3.42g, which are dissolved in deionized water, forms solution C, The anhydrous yttrium chlorides of 1.95g are dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D is uniformly mixed to obtain solution E, and solution E is slowly dropped in Sol A, and 76 DEG C of return stirrings form transparent and homogeneous in 4 hours Colloidal sol.Colloidal sol is placed in 85 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum rings 24h is freeze-dried in border, Y is obtained_0.02Sb_0.03Cs_0.33WO₃Precursor powder.

Again by Y_0.02Sb_0.03Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 450 DEG C, heating rate is 3 DEG C/min, together When be passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, treats that cooling is cold But disperse grinding afterwards and produce Y_0.02Sb_0.03Cs_0.33WO₃Nano-ceramic powder.

By obtained Y_0.02Sb_0.03Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, and graphite jig connects with powder Contacting surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 12MPa pressure to powder to nano-ceramic powder Precompressed is carried out, then is vacuumized, vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 8 DEG C/min, is warming up to 30min is incubated at 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 20MPa, Stop heating up when temperature is 600 DEG C and carry out maintaining 1h under heat-insulation pressure keeping, this process conditions, then annealing obtains high-compactness Y_0.02Sb_0.03Cs_0.33WO₃Nano ceramics target, is designated as BC8, and consistency is 99.9%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL1 is designated as.It is specific as follows：By the nitrogen drying that the glass baseplate cleaned up is dry, Coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then be passed through argon gas and oxygen, argon gas and The flow-rate ratio of oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 50nm rutile type nanos two is plated successively Titanium oxide layer, 250nm ternary doping nano ceramics film layers and 50nm anatase-type nanometer titanium dioxides layer.

Embodiment 9

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder that erbium chloride is different with the consumption of bismuth trichloride, tool Body is as follows：0.136g erbium chlorides and 0.315g bismuth trichlorides, obtained precursor powder are Er_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Er_0.001Bi_0.002Cs_0.33WO₃, BC9 is designated as, consistency is 98.2%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL9。

Embodiment 10

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder that erbium chloride is different with the consumption of bismuth trichloride, tool Body is as follows：0.136g erbium chlorides and 0.158g bismuth trichlorides, obtained precursor powder are Er_0.001Bi_0.001Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Er_0.001Bi_0.001Cs_0.33WO₃, BC10 is designated as, consistency is 98.8%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL10。

Embodiment 11

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder that erbium chloride is different with the consumption of bismuth trichloride, tool Body is as follows：13.65g erbium chlorides and 14.18g bismuth trichlorides, obtained precursor powder are Er_0.1Bi_0.09Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder

Er_0.1Bi_0.09Cs_0.33WO₃, BC11 is designated as, consistency is 98.6%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL11。

Embodiment 12

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder that erbium chloride is different with the consumption of bismuth trichloride, tool Body is as follows：13.65g erbium chlorides and 15.75g bismuth trichlorides, obtained precursor powder are Er_0.1Bi_0.1Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Er_0.1Bi_0.1Cs_0.33WO₃, BC12 is designated as, consistency is 98.1%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL12。

Embodiment 13

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 70 DEG C of return stirrings form vitreosol A in 2 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 6.3g bismuth trichlorides, which are dissolved in deionized water, forms solution C, 2.73g chlorine Change erbium to be dissolved in absolute ethyl alcohol, 70 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D stirring mixing is equal It is even to obtain solution E, solution E is slowly dropped in Sol A, 70 DEG C of return stirrings form the colloidal sol of transparent and homogeneous for 4 hours.By colloidal sol It is placed in 70 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in freeze-drying in -30 DEG C of vacuum environments 10h, obtains Er_0.02Bi_0.04Cs_0.33WO₃Precursor powder.

Again by Er_0.02Bi_0.04Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 350 DEG C, heating rate is 3 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,3h is incubated after heating, waits to cool Disperse grinding after cooling and produce Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

By obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-2Pa, is started to warm up while vacuumizing, and heating rate is 20 DEG C/min, is risen 40min is incubated when temperature is to 100 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 30MPa, stops heating up and carries out maintaining 3h under heat-insulation pressure keeping, this process conditions when temperature is 500 DEG C, and then annealing obtains high cause The Er of density_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC13, and consistency is 99.8%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL13。

Embodiment 14

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 80 DEG C of return stirrings form vitreosol A in 2 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 6.3g bismuth trichlorides, which are dissolved in deionized water, forms solution C, 2.73g chlorine Change erbium to be dissolved in absolute ethyl alcohol, 80 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D stirring mixing is equal It is even to obtain solution E, solution E is slowly dropped in Sol A, 80 DEG C of return stirrings form the colloidal sol of transparent and homogeneous for 4 hours.By colloidal sol It is placed in 120 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in freezing in -30 DEG C of vacuum environments and does Dry 20h, obtains Er_0.02Bi_0.04Cs_0.33WO₃Precursor powder.

Again by Er_0.02Bi_0.04Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 650 DEG C, heating rate is 3 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, waits to cool Disperse grinding after cooling and produce Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

By obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-2Pa, is started to warm up while vacuumizing, and heating rate is 1 DEG C/min, heating 10min is incubated during to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 15MPa, stops heating up and carries out maintaining 1.5h under heat-insulation pressure keeping, this process conditions when temperature is 1000 DEG C, and then annealing is obtained The Er of high-compactness_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC14, and consistency is 98.3%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL14。

Embodiment 15

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 2 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 1.14g trichloride antimonies, which are dissolved in deionized water, forms solution C, solution B, Solution C, is uniformly mixed to obtain solution D, solution D is slowly dropped in Sol A, and 76 DEG C of return stirrings form homogeneous for 4 hours Transparent colloidal sol.Colloidal sol is placed in 90 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C 24h is freeze-dried in vacuum environment, Sb is obtained_0.01Cs_0.33WO₃Precursor powder.

Again by Sb_0.01Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 500 DEG C, heating rate is 1 DEG C/min, simultaneously Hydrogen and nitrogen are passed through, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2.5h is incubated after heating, treats that cooling is cold But disperse grinding afterwards and produce Sb_0.01Cs_0.33WO₃Nano-ceramic powder.

By obtained Sb_0.01Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder contact surface Isolated with the boron nitride disperseed using polyvinyl alcohol, the pressure for first applying 5MPa to nano-ceramic powder is carried out to powder Precompressed, then vacuumize, vacuum is 3.0 × 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 6 DEG C/min, heating 20min is incubated during to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 6 DEG C/min, and pressure is upgraded to 20MPa, stops heating up and carries out maintaining 2.5h under heat-insulation pressure keeping, this process conditions when temperature is 550 DEG C, and then annealing is obtained Sb_0.01Cs_0.33WO₃Nano ceramics target, is designated as BC15, and consistency is 98.5%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL15 is designated as.It is specific as follows：The dry nitrogen of the glass baseplate cleaned up is blown It is dry, coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1.5 × 10^-3Pa, then it is passed through argon gas and oxygen, argon The flow-rate ratio of gas and oxygen is 2:1, magnetron sputtering power supply is then opened, power 80W is adjusted, 15nm rutile-types is plated successively and are received Rice titanium dioxide layer, 150nm ternary doping nano ceramics film layers and 25nm anatase-type nanometer titanium dioxides layer.

Embodiment 16

By obtained Y_0.02Sb_0.03Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, and graphite jig connects with powder Contacting surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 12MPa pressure to powder to nano-ceramic powder Precompressed is carried out, then is vacuumized, vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 8 DEG C/min, is warming up to 30min is incubated at 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 20MPa, Stop heating up when temperature is 600 DEG C and carry out maintaining 1h under heat-insulation pressure keeping, this process conditions, then annealing is obtained Y_0.02Sb_0.03Cs_0.33WO₃Nano ceramics target, is designated as BC16, and consistency is 99.9%, and purity is 99.99%.

Using nano ceramics target as magnetic control spattering target, nano ceramics film layer is plated on the glass substrate, and (ternary doping is received Rice ceramic film), optical nano ceramic insulation glass is made, BL16 is designated as.It is specific as follows：The glass baseplate cleaned up is used Dry nitrogen drying, is then placed in coating chamber, shuts coating chamber and start to vacuumize, and vacuum is 1 × 10^-3Pa, then it is passed through argon The flow-rate ratio of gas and oxygen, argon gas and oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, plates 250nm tri- First dopen Nano ceramic film.

Embodiment 17

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 3.95g gadolinium chlorides are dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings 1 hour Form vitreosol C.Solution B, colloidal sol C is uniformly mixed to obtain solution D, and solution D is slowly dropped in Sol A, and 76 DEG C are returned Stream stirring forms the colloidal sol of transparent and homogeneous for 5 hours.Colloidal sol is placed in 80 DEG C of vacuum environments, after after gelation, by washing, Alcohol is washed three times, then is placed in -40 DEG C of vacuum environments and is freeze-dried 15h, obtains Gd_0.03Cs_0.33WO₃Precursor powder.

Again by Gd_0.03Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 500 DEG C, heating rate is 3 DEG C/min, simultaneously Hydrogen and nitrogen are passed through, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, cooling down is treated Disperse grinding afterwards and produce Gd_0.03Cs_0.33WO₃Nano-ceramic powder.

By obtained Gd_0.03Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder contact surface Isolated with the boron nitride disperseed using polyvinyl alcohol, the pressure for first applying 15MPa to nano-ceramic powder is carried out to powder Precompressed, then vacuumize, vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is warming up to 300 DEG C when be incubated 30min, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, warm Spend for 800 DEG C when stop heat up and carry out maintaining 1h under heat-insulation pressure keeping, this process conditions, then annealing obtain Gd_0.03Cs_0.33WO₃Nano ceramics target, is designated as BC17, and consistency is 99.9%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL17 is designated as.It is specific as follows：The dry nitrogen of the glass baseplate cleaned up is blown It is dry, coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then it is passed through argon gas and oxygen, argon gas Flow-rate ratio with oxygen is 4:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 35nm rutile type nanos is plated successively Titanium dioxide layer, 250nm ternary doping nano ceramics film layers and 45nm anatase-type nanometer titanium dioxides layer.

Embodiment 18

Weigh 200g tungsten hexachlorides to be dissolved in absolute ethyl alcohol, 76 DEG C of return stirrings form vitreosol A in 3 hours, then weigh 28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 13.68g trichloride antimonies, which are dissolved in deionized water, forms solution C, 20.95g ytterbium chlorides are dissolved in absolute ethyl alcohol, and 76 DEG C of return stirrings form vitreosol D in 1 hour.Solution B, solution C, colloidal sol D Solution E is uniformly mixed to obtain, solution E is slowly dropped in Sol A, 76 DEG C of return stirrings form non-homogeneous colloidal sol in 3 hours. Colloidal sol is placed in 90 DEG C of vacuum environments, after after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum environments 15h is freeze-dried, Yb is obtained_0.15Sb_0.12Cs_0.33WO₃Precursor powder.Again by Yb_0.15Sb_0.12Cs_0.33WO₃It is placed in high temperature furnace, Sintering temperature is 450 DEG C, and heating rate is 3 DEG C/min, while being passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen exists 3-10:In the range of 1,2h is incubated after heating, Yb is produced after disperseing grinding after cooling down_0.15Sb_0.12Cs_0.33WO₃Nano ceramics Powder.

By obtained Yb_0.15Sb_0.12Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-3Pa, is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is risen 30min is incubated when temperature is to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, stops heating up and carries out maintaining 1h under heat-insulation pressure keeping, this process conditions when temperature is 1000 DEG C, and then annealing is obtained Yb_0.15Sb_0.12Cs_0.33WO₃Nano ceramics target, is designated as BC18, and consistency is 99.9%, and purity is 99.99%.

Respectively with rutile type nano TiO₂, nano ceramics target and anatase type nano TiO₂For magnetic control spattering target, The first TiO is plated on glass baseplate successively₂Layer, nano ceramics film layer (ternary doping nano ceramics film layer) and the 2nd TiO₂Layer, system Optical nano ceramic insulation glass is obtained, BL18 is designated as.It is specific as follows：The dry nitrogen of the glass baseplate cleaned up is blown It is dry, coating chamber is then placed in, coating chamber is shut and starts to vacuumize, vacuum is 1 × 10^-3Pa, then it is passed through argon gas and oxygen, argon gas Flow-rate ratio with oxygen is 6:1, magnetron sputtering power supply is then opened, power 100W is adjusted, 50nm rutile type nanos is plated successively Titanium dioxide layer, 300nm ternary doping nano ceramics film layers and 65nm anatase-type nanometer titanium dioxides layer.Optical nano ceramics Heat-protecting glass BL18 XRD is as shown in Figure 4.

Embodiment 19

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder that erbium chloride is different with the consumption of bismuth trichloride, tool Body is as follows：14.96g erbium chlorides and 17.32g bismuth trichlorides, obtained precursor powder are Er_0.11Bi_0.11Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Er_0.11Bi_0.11Cs_0.33WO₃, BC19 is designated as, consistency is 98.9%, and purity is 99.99%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL19。

Embodiment 20

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder that erbium chloride is different with the consumption of bismuth trichloride, tool Body is as follows：14.96g erbium chlorides and 18.9g bismuth trichlorides, obtained precursor powder are Er_0.11Bi_0.12Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Er_0.11Bi_0.12Cs_0.33WO₃, BC20 is designated as, consistency is 98.0%, and purity is 99.72%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL20。

Embodiment 21

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder to substitute chlorination with the equal scandium chloride of the amount of material Erbium, obtained precursor powder is Sc_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Sc_0.001Bi_0.002Cs_0.33WO₃, BC21 is designated as, consistency is 97.9%, and purity is 96.21%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL21。

Embodiment 22

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder to substitute chlorine with the mutually equal lanthanum chloride of the amount of material Change erbium, obtained precursor powder is La_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder La_0.001Bi_0.002Cs_0.33WO₃, BC22 is designated as, consistency is 97.9%, and purity is 96.21%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL22。

Embodiment 23

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder to substitute chlorination with the amount identical terbium chloride of material Erbium, obtained precursor powder is Tb_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Tb_0.001Bi_0.002Cs_0.33WO₃, BC23 is designated as, consistency is 97.2%, and purity is 95.95%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL23。

Embodiment 24

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder to substitute chlorination with the amount identical samarium trichloride of material Erbium, obtained precursor powder is Sm_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Sm_0.001Bi_0.002Cs_0.33WO₃, BC24 is designated as, consistency is 98.0%, and purity is 97.94%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL24。

Embodiment 25

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder to substitute trichlorine with the amount identical gallium chloride of material Change bismuth, obtained precursor powder is Ga_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Ga_0.001Bi_0.002Cs_0.33WO₃, BC25 is designated as, consistency is 98.0%, and purity is 99.87%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL25。

Embodiment 26

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, and difference is in the preparation process of precursor powder to substitute trichlorine with the amount identical germanium chloride of material Change bismuth, obtained precursor powder is Ge_0.001Bi_0.002Cs_0.33WO₃。

Nano ceramics target is made after preparation process as described in Example 3 in precursor powder Ge_0.001Bi_0.002Cs_0.33WO₃, BC26 is designated as, consistency is 97.2%, and purity is 99.71%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL26。

Embodiment 27

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, the step of difference is precursor powder nano-ceramic powder is made, specific as follows：

Again by Er_0.02Bi_0.04Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 700 DEG C, heating rate is 5 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,3h is incubated after heating, waits to cool Disperse grinding after cooling and produce Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

Last obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC27, and consistency is 96.1%, purity For 99.65%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL27。

Embodiment 28

Again by Er_0.02Bi_0.04Cs_0.33WO₃It is placed in high temperature furnace, sintering temperature is 300 DEG C, heating rate is 1 DEG C/min, Hydrogen and nitrogen are passed through simultaneously, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,3h is incubated after heating, waits to cool Disperse grinding after cooling and produce Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

Last obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC28, and consistency is 96.5%, purity For 99.71%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL28。

Embodiment 29

Again by Er_0.02Bi_0.04Cs_0.33WO₃Be placed in high temperature furnace, sintering temperature be 550 DEG C, heating rate be 0.5 DEG C/ Min, while being passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen is in 3-10:In the range of 1,2h is incubated after heating, is treated Disperse grinding after cooling down and produce Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder.

Last obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC29, and consistency is 96.8%, purity For 99.74%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL29。

Embodiment 30

The optical nano ceramic insulation glass for the enhancing visible light-transmissive that the present embodiment is provided and the preparation described in embodiment 3 Method is differed substantially, the step of difference is nano-ceramic powder nano ceramics target is made, specific as follows：

By obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 20MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-2Pa, is started to warm up while vacuumizing, and heating rate is 25 DEG C/min, is risen 60min is incubated when temperature is to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, stops heating up and carries out maintaining 3h under heat-insulation pressure keeping, this process conditions when temperature is 1000 DEG C, and then annealing is obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC30, and consistency is 95.8%, and purity is 99.61%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL30。

Embodiment 31

By obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano-ceramic powder is added in graphite jig, graphite jig and powder Contact surface is isolated with the boron nitride disperseed using polyvinyl alcohol, first applies 15MPa pressure to powder to nano-ceramic powder Body carries out precompressed, then vacuumizes, and vacuum is 10^-2Pa, is started to warm up while vacuumizing, and heating rate is 25 DEG C/min, is risen 30min is incubated when temperature is to 300 DEG C, insulation terminates follow-up temperature of continuing rising and pressurizeed, and heating rate is 25 DEG C/min, and pressure is upgraded to 25MPa, stops heating up and carries out maintaining 3h under heat-insulation pressure keeping, this process conditions when temperature is 1100 DEG C, and then annealing is obtained Er_0.02Bi_0.04Cs_0.33WO₃Nano ceramics target, is designated as BC31, and consistency is 96.3%, and purity is 99.76%.

Make on the glass substrate and optical nano ceramic insulation glass is made after functional layer as described in Example 3, be designated as BL31。

Test respectively above-mentioned obtained heat insulating function glass BL1-BL31 visible transmission ratio, ultraviolet (uv) transmission ratio, Total solar energy transmittance, shading coefficient, heat transfer coefficient, the reflectivity in 1000-2500nm wave-length coverages, to 950nm wavelength Shielding rate and the shielding rate to 1400nm wavelength, test result are as shown in table 1 below.

The optical nano ceramic insulation glass that the nano ceramics target BC1-31 that the Application Example 1-31 of table 1 makes makes BL1-31 physical property

As seen from the data in Table 1, nano ceramics target produces significant to the physical property of optical nano ceramic insulation glass Influence.When preparing nano ceramics target, the control of temperature is equal in the materials and consumption, or even preparation process of nano ceramics target Obvious influence can be produced on the property of nano ceramics target, so as to influence every the physical of optical nano ceramic insulation glass Energy.

The technology contents described above that the present invention is only further illustrated with embodiment, in order to which reader is easier to understand, But embodiments of the present invention are not represented and are only limitted to this, and any technology done according to the present invention extends or recreated, and is sent out by this Bright protection.

Claims

1. a kind of strengthen the optical nano ceramic insulation glass of visible light-transmissive, including glass baseplate, it is characterised in that described The first TiO is sequentially provided with glass baseplate₂Layer, nano ceramics film layer and the 2nd TiO₂Layer；The nano ceramics film layer by X_mZ_nCs_0.33WO₃Constitute；

Wherein, X is Ce or Y or Er or Yb and Gd, Z are Sn or Sb or Bi, m are 0.001-0.1, and n is 0.001-0.1.

2. a kind of according to claim 1 strengthen the optical nano ceramic insulation glass of visible light-transmissive, it is characterised in that institute State the first TiO₂Layer is rutile type nano TiO₂Layer.

3. a kind of according to claim 1 strengthen the optical nano ceramic insulation glass of visible light-transmissive, it is characterised in that institute State the 2nd TiO₂Layer is anatase type nano TiO₂Layer.

4. a kind of preparation method of the optical nano ceramic insulation glass of enhancing visible light-transmissive as claimed in claim 1, it is special Levy and be, comprise the following steps：

S1 prepares precursor powder：The solution B of cesium compound, solution C and colloidal sol D are well mixed, solution E is obtained；Then by solution E It is well mixed with vitreosol A, colloidal sol F is made；Then make after colloidal sol F gelations, and scrubbed and drying process, obtain forerunner Powder；

The vitreosol A is the vitreosol of tungsten compound；The solution B is the solution of cesium compound；The solution C be containing The solution of Sn or Sb or Bi compound；The colloidal sol D is the vitreosol of the compound containing Ce or Y or Er or Yb or Gd；

The ratio between contained element X, element Z, Cs and W amount of material are in the vitreosol A, solution B, solution C and colloidal sol D 0.001-0.1:0.001-0.1:0.33:1；

S2 prepares nano-ceramic powder：After precursor powder is handled through high temperature sintering, nano-ceramic powder is made；

S3 prepares nano ceramics target：Nano-ceramic powder is fitted into mould, nano-ceramic powder is placed in vacuum with mould For 6.0 × 10^-3In Pa environment, nano-ceramic powder is 10-30Mpa in pressure, and temperature is guarantor under conditions of 500-1000 DEG C Warm pressurize 1-3h；Obtain nano ceramics target；

S4 makes functional layer：Respectively with TiO₂It is magnetic control spattering target with nano ceramics target, plates the successively on the glass substrate One TiO₂Layer, nano ceramics film layer and the 2nd TiO₂Layer, is made optical nano ceramic insulation glass.

5. according to claim 4 it is a kind of strengthen visible light-transmissive optical nano ceramic insulation glass preparation method, its It is characterised by, in step S2, precursor powder is placed in high temperature furnace, while hydrogen and nitrogen/inert gas are passed through, nitrogen/lazy Property gas and hydrogen flowing quantity ratio be 3-10：1, temperature is risen to 350-650 DEG C with 1-3 DEG C/min programming rate, 2-3h is incubated； Then stop heating, after carrying out milled processed after cooling down, obtain nano-ceramic powder.

6. according to claim 4 it is a kind of strengthen visible light-transmissive optical nano ceramic insulation glass preparation method, its It is characterised by, in step S1, solution E is added drop-wise in vitreosol A dropwise, and return stirring 3-5 hours at 70-80 DEG C, Form colloidal sol F；Colloidal sol F is placed in 70-120 DEG C of vacuum environment, makes its gelation, is washed out and centrifugal treating, will be solidifying Glue is placed in -40-20 DEG C of vacuum environment and is freeze-dried 10-24h, obtains precursor powder.

7. according to claim 4 it is a kind of strengthen visible light-transmissive optical nano ceramic insulation glass preparation method, its It is characterised by, in step S3, first applies 5-15Mpa pressure to the nano-ceramic powder in mould, then vacuumize, vacuum is 10^-2-10^-3Pa, and heated while vacuumizing, heating rate is 1-20 DEG C/min, is protected when temperature rises to 100-300 DEG C Warm 10-40min；Then the nano-ceramic powder in mould is pressurized and heated up, pressure rises to 15-30Mpa, and temperature rises to 500- 1000℃；It is incubated after 1-3h and cools down, obtains nano ceramics target.

8. according to claim 4 it is a kind of strengthen visible light-transmissive optical nano ceramic insulation glass preparation method, its It is characterised by, in step S1, the vitreosol A is dissolved in absolute ethyl alcohol by tungsten compound is made into clear solution, clear solution Formed within return stirring 2-4 hours at 70-80 DEG C.

9. according to claim 4 it is a kind of strengthen visible light-transmissive optical nano ceramic insulation glass preparation method, its It is characterised by, in step S1, the colloidal sol D is that the chloride containing Ce or Y or Er or Yb or Gd is dissolved in absolute ethyl alcohol, and Return stirring is formed for 1 hour at 70-80 DEG C.

10. according to claim 4 it is a kind of strengthen visible light-transmissive optical nano ceramic insulation glass preparation method, its It is characterised by, in step S4, in vacuum<2.0×10^-3In the environment of Pa, inert gas and oxygen, the argon gas and oxygen are passed through The flow-rate ratio of gas is 2-8:1, magnetron sputtering plating is then carried out with 50-200W power.