CN107200579B - A kind of nano ceramics target and preparation method thereof - Google Patents
A kind of nano ceramics target and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to technical field of ceramic material, specially a kind of nano ceramics target and preparation method thereof.There are easy to aging applied to that can solve the problems, such as existing heat insulating function glass on heat insulating function glass for nano ceramics target of the present invention.By each technological parameter in control preparation process, the material that can effectively reduce nano ceramics target in preparation process is reduced the problem of precipitating metal simple substance, and made nano ceramics target is avoided stomata occur and cause consistency not high enough.Using the nano ceramics target of the method for the present invention preparation on heat insulating function glass, be conducive to further increase the physical properties such as the visible transmission ratio of heat insulating function glass, heat insulating function glass can be made to be provided simultaneously with the performance of selective absorbing and selective reflecting to solar spectrum simultaneously, it again can good absorption and reflection ultraviolet and infrared ray while guaranteeing visible light high permeability, and structure is simple, not metal-containing layer can reduce the production cost of heat insulating function glass, be suitble to industrial production.
Description
Technical field
The present invention relates to technical field of ceramic material more particularly to a kind of nano ceramics target and preparation method thereof.
Background technique
As developing country, the storage level that China is faced with the energy is insufficient, the not high Pressure on Energy of utilization rate.The energy
Consume excessively and bring environment and ecological problem are increasingly severe therewith, influence even to involve the whole world.With
The deterioration of environment, ecological problem are on the rise, and more and more people have been obtained in protection environment and the importance to economize on resources
Concern and attention.China is as the biggish country of global construction scope, and building energy consumption is just gradually by the attention of government.Firmly build
Portion points out in publication building energy conservation " 13 plan " overall goal, builds energy-saving low-carbon, intensive efficient energy for building body
System accelerates to promote building energy-saving standard, and specific to the year two thousand twenty, cities and towns new building efficiency level promoted 20% than 2015, part
Building energy-saving standard is close to or up to international advanced level at this stage.
Door glass energy consumption accounts for the 50% of building energy consumption, and energy-saving glass can enhance the heat-proof quality of door glass, be reduced to
Hot-cool environment in equalization chamber and bring energy consumption, therefore produce the better glass of thermal insulation and reducing energy consumption, promote building section
Energy aspect plays increasingly important role.The high heat-proof quality of energy-saving glass is mainly reflected in barrier solar radiation at present
On infrared ray and imparted energy.Industrially mostly use the method for magnetron sputtering that various functional materials preparation film forming is attached to glass
Above or directly the sputtering of various functional materials is used on the glass substrate.Chinese patent CN103342022A, which is disclosed, passes through magnetic control
Sputtering method is by ZnO or ZnSnOx, silver, which sputters at, forms MULTILAYER COMPOSITE layer on glass, the glass of fire prevention and Low emissivity, this glass is made
The transmitting of glass heat is less and can block sunlight to a certain extent.But glass disclosed in the research is only reducing heat transmitting and is stopping
It plays a role in terms of the sunlight of part, it is limited to the ability for stopping sunlight irradiation bring heat, interior can not be effectively reduced
Temperature reduces air conditioner load to reach energy-efficient effect.Chinese patent CN103587167A discloses a kind of visible light transmission increasing
The outer layer of low emissivity glass, this glass posts TiO2And MgF2The anti-reflection film of composition, internal layer post Ag system low-radiation film, this kind of glass
Glass is to visible light transmissivity with higher, to infrared and far infrared reflectivity with higher.Chinese patent
CN205416573U disclose it is a kind of can hot bending infrared block energy conservation coated glass, by the method for vacuum magnetic-control sputtering in glass
Glass surface sputters 20 layer films, including the metal alloy layers such as Ag, Cu and SnO2、ZnSnOx、TiOx、ZrO2And Si3N4Deng multiple
Layer is closed, the solar energy transmission for the glass that the method is worked it out is low, and summer use can make the substantially impervious mistake of infrared energy, winter
Using heating can be kept not to be lost, play the role of energy-efficient.But it is coated with the glass of metal Ag, Cu film, when using one section
Between after it is easy to oxidize rotten, it is at high cost in addition, multilayer magnetron sputtering membrane process is complicated, be unfavorable for industrial production.
Nano ceramic material is a kind of transparent conductive oxide (TCO), mainly with the aluminium oxide of different size, zirconium oxide,
Titanium oxide and silica etc. are fired through surface coating, high temperature, and chemical stability is good, have low reflective, high light transmission, it is high every
The features such as hot and be widely used.Nano ceramic material is existing mostly on plastics or nanometer heat isolation paint.Chinese patent
CN102643037A discloses a kind of eva film of functionalization, successively plated on film by way of coating nano yttrium oxide,
Nano silica, nano aluminium oxide, nano zircite, nano calcium oxide, nano-titanium dioxide, nano zine oxide, nano oxygen
Change oxides and the nano cerium doped stannum oxide antimony such as cerium and is made, the visible light transmittance height of the eva film, ultraviolet light and infrared
Light shield is higher.Chinese patent CN104130725A also discloses 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 is made of the stannic oxide of Doped Tungsten cerium antimony with EVA resin and organic solvent, EVA
Gummosis film is not made of EVA resin, counter infrared ray auxiliary agent, coupling agent, crosslinking agent and ultraviolet absorber, and gummosis film does not significantly improve for this
The rejection rate of ultraviolet and infrared ray, thickness homogeneity are high.Chinese patent CN104275889A discloses a kind of high-performance and receives
Rice compound heat-insulation film, the manufacturing process of this thermal isolation film are to form sputtering layer by sputtering first on pet layer, are then coated with one layer
Tungstic acid adiabatic gum, then compound one layer of pet layer, are coated one layer of peace being made of polyacrylate resin and ultraviolet absorber
Layer is filled, finally for by surface-treated laminated polyester film.This film has excellent visible light transmittance and infrared and ultraviolet
Rejection rate, and there is good mechanical performance, scratch resistant performance and high and low temperature resistance.Chinese patent CN105778830A is disclosed
The preparation method of the heat-insulated PVB film of spectral selectivity nano a kind of, this patent disperse near-infrared long wave barrier nano material
Liquid, near-infrared shortwave nano dispersion fluid and near-infrared reflection nano dispersion fluid are mixed with PVB, so that film is in visible light high transmission
While rate is high, and can good absorption and reflection near infrared ray.Near-infrared length wave resistance every nano material dispersion liquid by
LaB is added in dispersing agent6、ScB6Deng be made, near-infrared long wave barrier by wetting dispersing agent and defoaming agent add ITO,
The metal oxides such as ATO, AZO and Ce-ATO are made.EVA disclosed in the above research, PET, PVB are organic polymer polymerization
Object, is chronically exposed to easy to aging in air, and has the energy-absorbings group such as-C-O-, C=O ,-OH in polymer, easily causes nanometer
The thermal contraction of material.
Summary of the invention
The present invention needs to be further increased for existing heat insulating function glass energy-saving effect, and the problems such as easy aging,
There is provided that a kind of heat insulating function plate can make energy-conserving plate material non-aging and to can be improved the visible light of energy-conserving plate material saturating for making
Have the nano ceramics target and this kind of nanometer pottery that good spectral selection is absorbed and reflected to sunlight while crossing rate
The preparation method of porcelain target.
To achieve the above object, the present invention uses following technical scheme.
A kind of nano ceramics target, the nano ceramics target are XmZnCs0.33WO3；Wherein, X is Ce or Y or Er or Yb
And Gd, Z are Sn or Sb or Bi, m 0.001-0.1, n 0.001-0.1.
Preferably, m 0.005-0.05, n 0.002-0.06；It is furthermore preferred that m is 0.01-0.05, n 0.01-
0.06。
Preferably, consistency >=98% of the nano ceramics target, purity >=99.99%.
The preparation method of nano ceramics target described above, comprising the following steps:
S1 prepares precursor powder: solution B, solution C and colloidal sol D being uniformly mixed, solution E is obtained；Then by solution E with it is transparent
Sol A is uniformly mixed, and colloidal sol F is made；Then make colloidal sol F gelation, and after washed and drying process, obtain precursor powder.
Preferably, solution E is added drop-wise to dropwise in vitreosol A, 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, its gelation is made, simultaneously centrifugal treating is washed out, gel is set
It is freeze-dried 10-24h in -40-20 DEG C of vacuum environment, obtains precursor powder.
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 the compound of Bi；The colloidal sol D is the transparent molten of the compound containing Ce or Y or Er or Yb or Gd
Glue.The ratio between element X contained in the vitreosol A, solution B, solution C and colloidal sol D, amount of substance of element Z, Cs and W are
0.001-0.1:0.001-0.1:0.33:1。
Preferably, the tungsten compound is tungsten hexachloride, and the cesium compound is cesium chloride.
Preferably, the vitreosol A is dissolved in dehydrated alcohol by tungsten compound is made into clear solution, and clear solution exists
It is formed within return stirring 2-4 hours at 70-80 DEG C.
Preferably, the solution B is dissolved in deionized water by cesium compound, stirs evenly to be formed.
Preferably, the solution C is dissolved in deionized water for the chloride containing Sn or Sb or Bi and being formed.
Preferably, the colloidal sol D is dissolved in dehydrated alcohol for the chloride containing Ce or Y or Er or Yb or Gd, and in 70-80
It is formed within return stirring 1 hour at DEG C.
S2 prepares nano-ceramic powder: nano-ceramic powder is made after high temperature sintering is handled in precursor powder.
Preferably, precursor powder is placed in high temperature furnace, while is passed through hydrogen and nitrogen/inert gas, nitrogen/indifferent gas
Body and hydrogen flowing quantity ratio are 3-10:1, and temperature is risen to 350-650 DEG C with the heating rate of 1-3 DEG C/min, keeps the temperature 2-3h；Then
Stop heating, is ground after cooling down, obtains nano-ceramic powder.
S3 prepares nano ceramics target: nano-ceramic powder being fitted into mold, nano-ceramic powder and mold are placed in very
Reciprocal of duty cycle is 6.0 × 10-3In the environment of Pa, nano-ceramic powder is 10-30Mpa, the condition that temperature is 500-1000 DEG C in pressure
Lower heat-insulation pressure keeping 1-3h；Obtain nano ceramics target.
Preferably, first apply the pressure of 5-15Mpa to the nano-ceramic powder in mold, then vacuumize, vacuum degree 10-2-10-3Pa, and heating while vacuumizing, heating rate are 1-20 DEG C/min, heat preservation when temperature rises to 100-300 DEG C
10-40min；Then the nano-ceramic powder in mold is pressurized and heating, pressure rises to 15-30Mpa, temperature rises to 500-
1000℃；It is cooling after heat preservation 1-3h, obtain nano ceramics target.
Preferably, heat resistant spacer layer is equipped between the nano-ceramic powder and mold.It is furthermore preferred that the separation layer is
The boron nitride of polyvinyl alcohol dispersion.
Compared with prior art, the beneficial effects of the present invention are: the present invention passes through suitable vitreosol A, solution B, molten
Liquid C and colloidal sol D, which prepares the nano ceramics target to be formed, has the characteristics that stability is good, not oxidizable and aging, is applied to heat-insulated
It can solve the problems, such as that there are easy to aging for existing heat insulating function glass on functional glass.Pass through each technique ginseng in control preparation process
Number, the material that can effectively reduce nano ceramics target in preparation process are reduced the problem of precipitating metal simple substance, and avoid institute
There is stomata and causes consistency not high enough in nano ceramics target processed.The cause of the nano ceramics target prepared by the method for the invention
Density >=98%, purity >=99.99%.Using the nano ceramics target of the method for the present invention preparation on heat insulating function glass, have
Conducive to physical properties such as the visible transmission ratios for further increasing heat insulating function glass, while heat insulating function glass can be made to the sun
Spectrum is provided simultaneously with the performance of selective absorbing and selective reflecting, again can good absorption while guaranteeing visible light high permeability
With reflection ultraviolet and infrared ray, and structure is simple, and metal-containing layer, can not reduce the production cost of heat insulating function glass, is suitble to
Industrial production.
Detailed description of the invention
Fig. 1 is the XRD diagram of the nano-ceramic powder in embodiment 4；
Fig. 2 is the grain size distribution of the nano-ceramic powder of embodiment 6.
Specific embodiment
In order to more fully understand technology contents of the invention, combined with specific embodiments below to technical solution of the present invention
It is described further and illustrates.
Embodiment 1
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 2 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 1.14g antimony trichloride, which is dissolved in deionized water, forms solution C, 1.23g
Cerous chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D stirring are mixed
Uniform solution E is closed, solution E is slowly dropped in Sol A, 76 DEG C form homogeneous and transparent colloidal sol in return stirring 4 hours.It will
Colloidal sol is placed in 90 DEG C of vacuum environments, and after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum environments and is freezed
Drying for 24 hours, obtains Ce0.01Sb0.01Cs0.33WO3Precursor powder.
Again by Ce0.01Sb0.01Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 500 DEG C, and heating rate is 1 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2.5h in the range of 3-10:1 after heating, wait drop
Dispersion is ground up to Ce after temperature is cooling0.01Sb0.01Cs0.33WO3Nano-ceramic powder.
By Ce obtained0.01Sb0.01Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 5MPa to powder to nano-ceramic powder
Precompressed is carried out, then is vacuumized, vacuum degree is 3.0 × 10-3Pa is started to warm up while vacuumizing, and heating rate is 6 DEG C/min,
20min is kept the temperature when being warming up to 300 DEG C, continues to heat up after heat preservation and pressurize, and heating rate is 6 DEG C/min, and pressure is upgraded to
20MPa stops heating up when temperature is 550 DEG C and carries out heat-insulation pressure keeping, 2.5h maintained under this process conditions, then annealing obtains height
The Ce of consistency0.01Sb0.01Cs0.33WO3Nano ceramics target is denoted as BC1, consistency 98.5%, purity 99.99%.
Embodiment 2
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 2 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 5.7g antimony trichloride, which is dissolved in deionized water, forms solution C, 6.15g tri-
Cerium chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
It is uniform to obtain solution E, solution E is slowly dropped in Sol A, 76 DEG C form homogeneous and transparent colloidal sol in return stirring 4 hours.It will be molten
Glue is placed in 90 DEG C of vacuum environments, and after gelation, by washing, alcohol is washed three times, then is placed in freeze in -20 DEG C of vacuum environments and be done
It is dry for 24 hours, obtain Ce0.05Sb0.05Cs0.33WO3Precursor powder.
Again by Ce0.05Sb0.05Cs0.33WO3Be placed in high temperature furnace, sintering temperature be 450 DEG C, heating rate be 1.5 DEG C/
Min, while it being passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, to
Dispersion is ground up to Ce after cooling down0.05Sb0.05Cs0.33WO3Nano-ceramic powder.
By Ce obtained0.05Sb0.05Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 10MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, and vacuum degree is 8.0 × 10-3Pa is started to warm up while vacuumizing, heating rate be 10 DEG C/
Min keeps the temperature 30min, continues to heat up after heat preservation and pressurize when being warming up to 250 DEG C, heating rate is 10 DEG C/min, pressure
It is upgraded to 20MPa, stop heating up when temperature is 750 DEG C and carries out heat-insulation pressure keeping, 1h is maintained under this process conditions, then annealing obtains
The Ce of high-compactness0.05Sb0.05Cs0.33WO3Nano ceramics target, is denoted as BC2, consistency 99.5%, and purity is
99.995%.
Embodiment 3
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 2 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 6.3g bismuth trichloride, which is dissolved in deionized water, forms solution C, 2.73g chlorine
Change erbium to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
It is even to obtain solution E, solution E is slowly dropped in Sol A, 76 DEG C form homogeneous and transparent colloidal sol in return stirring 4 hours.By colloidal sol
It is placed in 80 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in freeze in -30 DEG C of vacuum environments and be done
Dry 20h, obtains Er0.02Bi0.04Cs0.33WO3Precursor powder.
Again by Er0.02Bi0.04Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 550 DEG C, and heating rate is 3 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Er after cooling0.02Bi0.04Cs0.33WO3Nano-ceramic powder.
By Er obtained0.02Bi0.04Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-2Pa is started to warm up while vacuumizing, and heating rate is 15 DEG C/min, is risen
30min is kept the temperature when temperature is to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
25MPa stops heating up when temperature is 800 DEG C and carries out heat-insulation pressure keeping, 1.5h maintained under this process conditions, then annealing obtains height
The Er of consistency0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC3, consistency 99.8%, purity 99.99%.
Embodiment 4
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 0.23g antimony trichloride, which is dissolved in deionized water, forms solution C, 0.70g
Ytterbium chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
It is uniform to obtain solution E, solution E is slowly dropped in Sol A, 76 DEG C form homogeneous and transparent colloidal sol in return stirring 3 hours.It will be molten
Glue is placed in 90 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum environments and is freezed
Dry 15h, obtains Yb0.005Sb0.002Cs0.33WO3Precursor powder.
Again by Yb0.005Sb0.002Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 450 DEG C, and heating rate is 3 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Yb after cooling0.005Sb0.002Cs0.33WO3Nano-ceramic powder, XRD diagram are shown in Fig. 1.
By Yb obtained0.005Sb0.002Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-3Pa is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is risen
30min is kept the temperature when temperature is to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
25MPa stops heating up when temperature is 1000 DEG C and carries out heat-insulation pressure keeping, 1h maintained under this process conditions, then annealing obtains height
The Yb of consistency0.005Sb0.002Cs0.33WO3Nano ceramics target is denoted as BC4, consistency 99.9%, purity 99.99%.
Embodiment 5
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 5.70g anhydrous stannous chloride, which is dissolved in deionized water, forms solution C,
3.95g gadolinium chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
Mix uniformly mixed solution E, solution E be slowly dropped in Sol A, 76 DEG C formed within return stirring 5 hours it is homogeneous and transparent molten
Glue.Colloidal sol is placed in 80 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum environments
Middle freeze-drying 15h, obtains Gd0.03Sn0.06Cs0.33WO3Precursor powder.
Again by Gd0.03Sn0.06Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 500 DEG C, and heating rate is 3 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Gd after cooling0.03Sn0.06Cs0.33WO3Nano-ceramic powder.
By Gd obtained0.03Sn0.06Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-3Pa is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is risen
30min is kept the temperature when temperature is to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
25MPa stops heating up when temperature is 800 DEG C and carries out heat-insulation pressure keeping, 1h maintained under this process conditions, then annealing obtains high cause
The Gd of density0.03Sn0.06Cs0.33WO3Nano ceramics target is denoted as BC5, consistency 99.9%, purity 99.99%.
Embodiment 6
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and the anhydrous bismuth chloride of 15.76g, which is dissolved in deionized water, forms solution C,
0.10g yttrium chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
Mix uniformly mixed solution E, solution E be slowly dropped in Sol A, 76 DEG C formed within return stirring 4 hours it is homogeneous and transparent molten
Glue.Colloidal sol is placed in 90 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -30 DEG C of vacuum environments
Middle freeze-drying for 24 hours, obtains Y0.001Bi0.1Cs0.33WO3Precursor powder.
Again by Y0.001Bi0.1Cs0.33WO3It is placed in high temperature furnace, sintering temperature is 500 DEG C, and heating rate is 3 DEG C/min, together
When be passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, cold wait cool down
But dispersion is ground up to Y afterwards0.001Bi0.1Cs0.33WO3Nano-ceramic powder, the grain size distribution of nano-ceramic powder such as Fig. 2 institute
Show.
By Y obtained0.001Bi0.1Cs0.33WO3Nano-ceramic powder is added in graphite jig, and graphite jig connects with powder
Contacting surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 10MPa to powder to nano-ceramic powder
Precompressed is carried out, then is vacuumized, vacuum degree 10-3Pa is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, heating
30min is kept the temperature when to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
20MPa stops heating up when temperature is 700 DEG C and carries out heat-insulation pressure keeping, 1h maintained under this process conditions, then annealing obtains high cause
The Gd of density0.03Sn0.06Cs0.33WO3Nano ceramics target is denoted as BC6, consistency 99.93%, purity 99.99%.
Embodiment 7
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and the anhydrous bismuth chloride of 6.30g, which is dissolved in deionized water, forms solution C,
1.23g anhydrous cerium chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.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 formation in return stirring 4 hours are homogeneous and transparent
Colloidal sol.Colloidal sol is placed in 90 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -30 DEG C of vacuum rings
It is freeze-dried in border for 24 hours, obtains Ce0.01Bi0.04Cs0.33WO3Precursor powder.
Again by Ce0.01Bi0.04Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 400 DEG C, and heating rate is 2 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Ce after cooling0.01Bi0.04Cs0.33WO3Nano-ceramic powder.
By Ce obtained0.01Bi0.04Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 10MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-3Pa is started to warm up while vacuumizing, and heating rate is 8 DEG C/min, heating
40min is kept the temperature when to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
20MPa stops heating up when temperature is 600 DEG C and carries out heat-insulation pressure keeping, 1h maintained under this process conditions, then annealing obtains high cause
The Ce of density0.01Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC7, consistency 99.9%, purity 99.99%.
Embodiment 8
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and the anhydrous antimony chloride of 3.42g, which is dissolved in deionized water, forms solution C,
The anhydrous yttrium chloride of 1.95g is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.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 formation in return stirring 4 hours are homogeneous and transparent
Colloidal sol.Colloidal sol is placed in 85 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C of vacuum rings
It is freeze-dried in border for 24 hours, obtains Y0.02Sb0.03Cs0.33WO3Precursor powder.
Again by Y0.02Sb0.03Cs0.33WO3It is placed in high temperature furnace, sintering temperature is 450 DEG C, and heating rate is 3 DEG C/min, together
When be passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, cold wait cool down
But dispersion is ground up to Y afterwards0.02Sb0.03Cs0.33WO3Nano-ceramic powder.
By Y obtained0.02Sb0.03Cs0.33WO3Nano-ceramic powder is added in graphite jig, and graphite jig connects with powder
Contacting surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 12MPa to powder to nano-ceramic powder
Precompressed is carried out, then is vacuumized, vacuum degree 10-3Pa is started to warm up while vacuumizing, and heating rate is 8 DEG C/min, is warming up to
30min is kept the temperature at 300 DEG C, is continued to heat up after heat preservation and be pressurizeed, 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 heat-insulation pressure keeping, 1h is maintained under this process conditions, then annealing obtains high-compactness
Y0.02Sb0.03Cs0.33WO3Nano ceramics target is denoted as BC8, consistency 99.9%, purity 99.99%.
Embodiment 9
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, specific as follows: 0.136g the difference is that erbium chloride is different with the dosage of bismuth trichloride in the preparation step of precursor powder
Erbium chloride and 0.315g bismuth trichloride, precursor powder obtained are Er0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Er0.001Bi0.002Cs0.33WO3, it is denoted as BC9, consistency 98.2%, purity 99.99%.
Embodiment 10
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, specific as follows: 0.136g the difference is that erbium chloride is different with the dosage of bismuth trichloride in the preparation step of precursor powder
Erbium chloride and 0.158g bismuth trichloride, precursor powder obtained are Er0.001Bi0.001Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Er0.001Bi0.001Cs0.33WO3, it is denoted as BC10, consistency 98.8%, purity 99.99%.
Embodiment 11
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, specific as follows: 13.65g the difference is that erbium chloride is different with the dosage of bismuth trichloride in the preparation step of precursor powder
Erbium chloride and 14.18g bismuth trichloride, precursor powder obtained are Er0.1Bi0.09Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Er0.1Bi0.09Cs0.33WO3, it is denoted as BC11, consistency 98.6%, purity 99.99%.
Embodiment 12
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, specific as follows: 13.65g the difference is that erbium chloride is different with the dosage of bismuth trichloride in the preparation step of precursor powder
Erbium chloride and 15.75g bismuth trichloride, precursor powder obtained are Er0.1Bi0.1Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Er0.1Bi0.1Cs0.33WO3, it is denoted as BC12, consistency 98.1%, purity 99.99%.
Embodiment 13
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 70 DEG C of return stirrings, 2 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 6.3g bismuth trichloride, which is dissolved in deionized water, forms solution C, 2.73g chlorine
Change erbium to be dissolved in dehydrated alcohol, 70 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
It is even to obtain solution E, solution E is slowly dropped in Sol A, 70 DEG C form homogeneous and transparent colloidal sol in return stirring 4 hours.By colloidal sol
It is placed in 70 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -30 DEG C of vacuum environments and is freeze-dried
10h obtains Er0.02Bi0.04Cs0.33WO3Precursor powder.
Again by Er0.02Bi0.04Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 350 DEG C, and heating rate is 3 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 3h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Er after cooling0.02Bi0.04Cs0.33WO3Nano-ceramic powder.
By Er obtained0.02Bi0.04Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-2Pa is started to warm up while vacuumizing, and heating rate is 20 DEG C/min, is risen
40min is kept the temperature when temperature is to 100 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
30MPa stops heating up when temperature is 500 DEG C and carries out heat-insulation pressure keeping, 3h maintained under this process conditions, then annealing obtains high cause
The Er of density0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC13, consistency 99.8%, purity 99.99%.
Embodiment 14
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 80 DEG C of return stirrings, 2 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 6.3g bismuth trichloride, which is dissolved in deionized water, forms solution C, 2.73g chlorine
Change erbium to be dissolved in dehydrated alcohol, 80 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
It is even to obtain solution E, solution E is slowly dropped in Sol A, 80 DEG C form homogeneous and transparent colloidal sol in return stirring 4 hours.By colloidal sol
It is placed in 120 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in freeze in -30 DEG C of vacuum environments and be done
Dry 20h, obtains Er0.02Bi0.04Cs0.33WO3Precursor powder.
Again by Er0.02Bi0.04Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 650 DEG C, and heating rate is 3 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Er after cooling0.02Bi0.04Cs0.33WO3Nano-ceramic powder.
By Er obtained0.02Bi0.04Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-2Pa is started to warm up while vacuumizing, and heating rate is 1 DEG C/min, heating
10min is kept the temperature when to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
15MPa stops heating up when temperature is 1000 DEG C and carries out heat-insulation pressure keeping, 1.5h maintained under this process conditions, then annealing obtains
The Er of high-compactness0.02Bi0.04Cs0.33WO3Nano ceramics target, is denoted as BC14, consistency 98.3%, and purity is
99.99%.
Embodiment 15
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 2 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 1.14g antimony trichloride, which is 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 formation in return stirring 4 hours are uniform
Transparent colloidal sol.Colloidal sol is placed in 90 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in -40 DEG C
It is freeze-dried in vacuum environment for 24 hours, obtains Sb0.01Cs0.33WO3Precursor powder.
Again by Sb0.01Cs0.33WO3It is placed in high temperature furnace, sintering temperature is 500 DEG C, and heating rate is 1 DEG C/min, is led to simultaneously
Enter hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2.5h in the range of 3-10:1 after heating, to cooling down
Dispersion is ground up to Sb afterwards0.01Cs0.33WO3Nano-ceramic powder.
By Sb obtained0.01Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder contact surface
It is isolated with the boron nitride using polyvinyl alcohol dispersion, the pressure for first applying 5MPa to nano-ceramic powder carries out in advance powder
Pressure, then vacuumize, vacuum degree is 3.0 × 10-3Pa is started to warm up while vacuumizing, and heating rate is 6 DEG C/min, is warming up to
20min is kept the temperature at 300 DEG C, is continued to heat up after heat preservation and be pressurizeed, heating rate is 6 DEG C/min, and pressure is upgraded to 20MPa,
Stop heating up when temperature is 550 DEG C and carry out heat-insulation pressure keeping, 2.5h is maintained under this process conditions, then annealing obtains
Sb0.01Cs0.33WO3Nano ceramics target is denoted as BC15, consistency 98.5%, purity 99.99%.
Embodiment 16
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 3.95g gadolinium chloride is dissolved in dehydrated alcohol, 76 DEG C return stirring 1 hour
Form vitreosol C.Solution B, colloidal sol C are uniformly mixed to obtain solution D, solution D are slowly dropped in Sol A, and 76 DEG C are returned
Stream stirring forms homogeneous and transparent colloidal sol in 5 hours.Colloidal sol is placed in 80 DEG C of vacuum environments, after gelation, by washing,
Alcohol is washed three times, then is placed in -40 DEG C of vacuum environments and is freeze-dried 15h, and Gd is obtained0.03Cs0.33WO3Precursor powder.
Again by Gd0.03Cs0.33WO3It is placed in high temperature furnace, sintering temperature is 500 DEG C, and heating rate is 3 DEG C/min, is led to simultaneously
Enter hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, after cooling down
Dispersion is ground up to Gd0.03Cs0.33WO3Nano-ceramic powder.
By Gd obtained0.03Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder contact surface
It is isolated with the boron nitride using polyvinyl alcohol dispersion, the pressure for first applying 15MPa to nano-ceramic powder carries out powder
Precompressed, then vacuumize, vacuum degree 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 keep the temperature 30min, continue to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to 25MPa, temperature
Stop heating up when degree is 800 DEG C and carry out heat-insulation pressure keeping, 1h is maintained under this process conditions, then annealing obtains Gd0.03Cs0.33WO3
Nano ceramics target is denoted as BC16, consistency 99.9%, purity 99.99%.
Embodiment 17
It is specific as follows the present embodiment provides a kind of preparation method of nano ceramics target:
It weighs 200g tungsten hexachloride to be dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 3 hours formation vitreosol A, then weighs
28 grams of cesium chlorides are dissolved in deionized water and form solution B, and 13.68g antimony trichloride, which is dissolved in deionized water, forms solution C,
20.95g ytterbium chloride is dissolved in dehydrated alcohol, 76 DEG C of return stirrings, 1 hour formation vitreosol D.Solution B, solution C, colloidal sol D are stirred
Uniformly mixed solution E is mixed, solution E is slowly dropped in Sol A, 76 DEG C form non-uniform colloidal sols in return stirring 3 hours.It will
Colloidal sol is placed in 90 DEG C of vacuum environments, after gelation, by washing, alcohol is washed three times, then is placed in cold in -40 DEG C of vacuum environments
Dry 15h is lyophilized, obtains Yb0.15Sb0.12Cs0.33WO3Precursor powder.Again by Yb0.15Sb0.12Cs0.33WO3It is placed in high temperature furnace, is sintered
Temperature is 450 DEG C, and heating rate is 3 DEG C/min, while being passed through hydrogen and nitrogen, and the flow-ratio control of nitrogen and hydrogen is in 3-
In the range of 10:1,2h is kept the temperature after heating, dispersion is ground up to Yb after cooling down0.15Sb0.12Cs0.33WO3Nano-ceramic powder
Body.
By Yb obtained0.15Sb0.12Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-3Pa is started to warm up while vacuumizing, and heating rate is 10 DEG C/min, is risen
30min is kept the temperature when temperature is to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
25MPa stops heating up when temperature is 1000 DEG C and carries out heat-insulation pressure keeping, 1h maintained under this process conditions, then annealing obtains
Yb0.15Sb0.12Cs0.33WO3Nano ceramics target is denoted as BC17, consistency 99.9%, purity 99.99%.
Embodiment 18
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, specific as follows: 14.96g the difference is that erbium chloride is different with the dosage of bismuth trichloride in the preparation step of precursor powder
Erbium chloride and 17.32g bismuth trichloride, precursor powder obtained are Er0.11Bi0.11Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Er0.11Bi0.11Cs0.33WO3, it is denoted as BC18, consistency 98.9%, purity 99.99%.
Embodiment 19
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, specific as follows: 14.96g the difference is that erbium chloride is different with the dosage of bismuth trichloride in the preparation step of precursor powder
Erbium chloride and 18.9g bismuth trichloride, precursor powder obtained are Er0.11Bi0.12Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Er0.11Bi0.12Cs0.33WO3, it is denoted as BC19, consistency 98.0%, purity 99.72%.
Embodiment 20
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that erbium chloride is substituted with the equal scandium chloride of the amount of substance in the preparation step of precursor powder, before obtained
Drive powder is Sc0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Sc0.001Bi0.002Cs0.33WO3, it is denoted as BC20, consistency 97.9%, purity 96.21%.
Embodiment 21
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, obtained the difference is that substituting erbium chloride with the mutually same lanthanum chloride of the amount of substance in the preparation step of precursor powder
Precursor powder is La0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
La0.001Bi0.002Cs0.33WO3, it is denoted as BC21, consistency 97.9%, purity 96.21%.
Embodiment 22
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that erbium chloride is substituted with the identical terbium chloride of the amount of substance in the preparation step of precursor powder, before obtained
Drive powder is Tb0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Tb0.001Bi0.002Cs0.33WO3, it is denoted as BC22, consistency 97.2%, purity 95.95%.
Embodiment 23
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that erbium chloride is substituted with the identical samarium trichloride of the amount of substance in the preparation step of precursor powder, before obtained
Drive powder is Sm0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Sm0.001Bi0.002Cs0.33WO3, it is denoted as BC23, consistency 98.0%, purity 97.94%.
Embodiment 24
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, obtained the difference is that substituting bismuth trichloride with the identical gallium chloride of the amount of substance in the preparation step of precursor powder
Precursor powder is Ga0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Ga0.001Bi0.002Cs0.33WO3, it is denoted as BC24, consistency 98.0%, purity 99.87%.
Embodiment 25
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, obtained the difference is that substituting bismuth trichloride with the identical germanium chloride of the amount of substance in the preparation step of precursor powder
Precursor powder is Ge0.001Bi0.002Cs0.33WO3。
Nano ceramics target is made after preparation step as described in Example 3 in precursor powder
Ge0.001Bi0.002Cs0.33WO3, it is denoted as BC25, consistency 97.2%, purity 99.71%.
Embodiment 26
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that the step of nano-ceramic powder is made in precursor powder, specific as follows:
Again by Er0.02Bi0.04Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 700 DEG C, and heating rate is 5 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 3h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Er after cooling0.02Bi0.04Cs0.33WO3Nano-ceramic powder.
Last Er obtained0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC26, consistency 96.1%, purity
It is 99.65%.
Embodiment 27
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that the step of nano-ceramic powder is made in precursor powder, specific as follows:
Again by Er0.02Bi0.04Cs0.33WO3It being placed in high temperature furnace, sintering temperature is 300 DEG C, and heating rate is 1 DEG C/min,
It is passed through hydrogen and nitrogen simultaneously, the flow-ratio control of nitrogen and hydrogen keeps the temperature 3h in the range of 3-10:1 after heating, wait cool down
Dispersion is ground up to Er after cooling0.02Bi0.04Cs0.33WO3Nano-ceramic powder.
Last Er obtained0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC27, consistency 96.5%, purity
It is 99.71%.
Embodiment 28
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that the step of nano-ceramic powder is made in precursor powder, specific as follows:
Again by Er0.02Bi0.04Cs0.33WO3Be placed in high temperature furnace, sintering temperature be 550 DEG C, heating rate be 0.5 DEG C/
Min, while it being passed through hydrogen and nitrogen, the flow-ratio control of nitrogen and hydrogen keeps the temperature 2h in the range of 3-10:1 after heating, to
Dispersion is ground up to Er after cooling down0.02Bi0.04Cs0.33WO3Nano-ceramic powder.
Last Er obtained0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC28, consistency 96.8%, purity
It is 99.74%.
Embodiment 29
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that the step of nano ceramics target is made in nano-ceramic powder, specific as follows:
By Er obtained0.02Bi0.04Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 20MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-2Pa is started to warm up while vacuumizing, and heating rate is 25 DEG C/min, is risen
60min is kept the temperature when temperature is to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 10 DEG C/min, and pressure is upgraded to
25MPa stops heating up when temperature is 1000 DEG C and carries out heat-insulation pressure keeping, 3h maintained under this process conditions, then annealing obtains
Er0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC29, consistency 95.8%, purity 99.61%.
Embodiment 30
The preparation method of nano ceramics target provided in this embodiment and preparation method described in embodiment 3 not phase substantially
Together, the difference is that the step of nano ceramics target is made in nano-ceramic powder, specific as follows:
By Er obtained0.02Bi0.04Cs0.33WO3Nano-ceramic powder is added in graphite jig, graphite jig and powder
Contact surface is isolated with the boron nitride using polyvinyl alcohol dispersion, first applies the pressure of 15MPa to powder to nano-ceramic powder
Body carries out precompressed, then vacuumizes, vacuum degree 10-2Pa is started to warm up while vacuumizing, and heating rate is 25 DEG C/min, is risen
30min is kept the temperature when temperature is to 300 DEG C, continues to heat up after heat preservation and pressurize, heating rate is 25 DEG C/min, and pressure is upgraded to
25MPa stops heating up when temperature is 1100 DEG C and carries out heat-insulation pressure keeping, 3h maintained under this process conditions, then annealing obtains
Er0.02Bi0.04Cs0.33WO3Nano ceramics target is denoted as BC30, consistency 96.3%, purity 99.76%.
Heat insulating function glass, method are prepared using the nano ceramics target BC1-BC30 of above-described embodiment 1-30 preparation respectively
It is as follows:
By being dried with nitrogen for the glass baseplate cleaned up drying, it is then placed in coating chamber, coating chamber is shut and starts to take out
Vacuum, vacuum degree are 1 × 10-3Pa, then it is passed through argon gas and oxygen, the flow-rate ratio of argon gas and oxygen is 8:1, then opens magnetron sputtering
Power supply, regulation power 50W, successively plate the rutile type nano titanic oxide layer of 30nm thickness, 200nm it is thick using above-mentioned nanometer
The ternary doping nano ceramics film layer of ceramic target production and the anatase-type nanometer titanium dioxide layer of 40nm thickness, are made heat-insulated function
Energy glass, respectively corresponds and is denoted as BL1-BL30.
Test respectively the visible transmission ratio of above-mentioned obtained heat insulating function glass BL1-BL30, ultraviolet (uv) transmission ratio,
Total solar energy transmittance, shading coefficient, heat transfer coefficient, the reflectivity in 1000-2500nm wave-length coverage, to 950nm wavelength
Shielding rate and shielding rate to 1400nm wavelength, test result is as follows shown in table 1.
The object of the heat insulating function glass BL1-30 of the nano ceramics target BC1-30 production of 1 Application Example 1-30 of table production
Rationality energy
As seen from the data in Table 1, nano ceramics target generates significant impact to the physical property of heat insulating function glass.It is making
When standby nano ceramics target, the control of temperature can be to nanometer in the materials and dosage or even preparation process of nano ceramics target
The property of ceramic target generates apparent influence, to influence the physical property of heat insulating function glass.
It is described above that technology contents of the invention are 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, any technology done according to the present invention extends or recreation, is sent out by this
Bright protection.
Claims (10)
1. a kind of nano ceramics target, which is characterized in that the nano ceramics target is XmZnCs0.33WO3；Wherein, X is Ce or Y
Or Er or Yb or Gd, Z are Sn or Sb or Bi, m 0.001-0.1, n 0.001-0.1.
2. a kind of nano ceramics target according to claim 1, which is characterized in that m 0.005-0.05, n 0.002-
0.06。
3. a kind of nano ceramics target according to claim 2, which is characterized in that m 0.01-0.05, n 0.01-0.06.
4. any one of -3 a kind of nano ceramics target according to claim 1, which is characterized in that the nano ceramics target
Consistency >=98%, purity >=99.99%.
5. a kind of preparation method of nano ceramics target as described in claim 1, which comprises the following steps:
S1 prepares precursor powder: the solution B of cesium compound, solution C and colloidal sol D being uniformly mixed, solution E is obtained；Then by solution
E is uniformly mixed with vitreosol A, and colloidal sol F is made；Then make colloidal sol F gelation, and after washed and drying process, before obtaining
Drive 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 the compound of Sn or Sb or Bi；The colloidal sol D is the vitreosol of the compound containing Ce or Y or Er or Yb or Gd；
The ratio between element X contained in the vitreosol A, solution B, solution C and colloidal sol D, amount of substance of element Z, Cs and W are
0.001-0.1:0.001-0.1:0.33:1；
S2 prepares nano-ceramic powder: nano-ceramic powder is made after high temperature sintering is handled in precursor powder；
S3 prepares nano ceramics target: nano-ceramic powder being fitted into mold, nano-ceramic powder and mold are placed in vacuum degree
It is 6.0 × 10-3In the environment of Pa, nano-ceramic powder is 10-30MPa in pressure, and temperature is protected under conditions of being 500-1000 DEG C
Warm pressure maintaining 1-3h；Obtain nano ceramics target.
6. a kind of preparation method of nano ceramics target according to claim 5, which is characterized in that in step S2, by forerunner
Powder is placed in high temperature furnace, while being passed through hydrogen and inert gas, and inert gas and hydrogen flowing quantity ratio are 3-10:1, with 1-3 DEG C/
Temperature is risen to 350-650 DEG C by the heating rate of min, keeps the temperature 2-3h；Then stop heating, carried out at grinding after cooling down
Reason, obtains nano-ceramic powder.
7. a kind of preparation method of nano ceramics target according to claim 5, which is characterized in that in step S1, by solution E
It is added drop-wise in vitreosol A dropwise, and return stirring 3-5 hours at 70-80 DEG C, forms colloidal sol F；Colloidal sol F is placed in 70-
In 120 DEG C of vacuum environment, make its gelation, is washed out simultaneously centrifugal treating, gel is placed in -40 DEG C to -20 DEG C of vacuum
It is freeze-dried 10-24h in environment, obtains precursor powder.
8. a kind of preparation method of nano ceramics target according to claim 5, which is characterized in that in step S3, first to mould
Nano-ceramic powder in tool applies the pressure of 5-15MPa, then vacuumizes, vacuum degree 10-2-10-3Pa, and vacuumizing
It heats simultaneously, heating rate is 1-20 DEG C/min, keeps the temperature 10-40min when temperature rises to 100-300 DEG C；Then in mold
Nano-ceramic powder pressurization and heating, pressure rises to 15-30MPa, and temperature rises to 500-1000 DEG C；It is cooling after heat preservation 1-3h,
Obtain nano ceramics target.
9. a kind of preparation method of nano ceramics target according to claim 5, which is characterized in that described in step S1
Bright Sol A is dissolved in dehydrated alcohol by tungsten compound is made into clear solution, and clear solution return stirring 2-4 at 70-80 DEG C is small
When formed.
10. a kind of preparation method of nano ceramics target according to claim 5, which is characterized in that described molten in step S1
Glue D is dissolved in dehydrated alcohol for the chloride containing Ce or Y or Er or Yb or Gd, and 1 hour shape of return stirring at 70-80 DEG C
At.
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| CN102139371A (en) * | 2011-05-04 | 2011-08-03 | 佛山市钜仕泰粉末冶金有限公司 | Tungsten alloy target material and preparation method thereof |
| CN102321476A (en) * | 2011-06-03 | 2012-01-18 | 北京工业大学 | Near-infrared quantum cutting transparent film and preparation method thereof |
| CN103451600A (en) * | 2012-05-30 | 2013-12-18 | 海洋王照明科技股份有限公司 | Cerium doped alkali metal scandate luminescent thin film, and preparation method and application thereof |
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| CN102139371A (en) * | 2011-05-04 | 2011-08-03 | 佛山市钜仕泰粉末冶金有限公司 | Tungsten alloy target material and preparation method thereof |
| CN102321476A (en) * | 2011-06-03 | 2012-01-18 | 北京工业大学 | Near-infrared quantum cutting transparent film and preparation method thereof |
| CN103451600A (en) * | 2012-05-30 | 2013-12-18 | 海洋王照明科技股份有限公司 | Cerium doped alkali metal scandate luminescent thin film, and preparation method and application thereof |
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