CN106830706A - A kind of method that broccoli shape graduation zinc stannate film material is prepared on electro-conductive glass - Google Patents
A kind of method that broccoli shape graduation zinc stannate film material is prepared on electro-conductive glass Download PDFInfo
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- CN106830706A CN106830706A CN201710065065.8A CN201710065065A CN106830706A CN 106830706 A CN106830706 A CN 106830706A CN 201710065065 A CN201710065065 A CN 201710065065A CN 106830706 A CN106830706 A CN 106830706A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/24—Doped oxides
- C03C2217/241—Doped oxides with halides
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
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Abstract
The invention discloses a kind of method that broccoli shape graduation zinc stannate film material is prepared on electro-conductive glass.It is the FTO electro-conductive glass that will be cleaned, and is dried naturally, the Zn that will be prepared in the form of spraying with spray gun2SnO4Seed Layer solution is sprayed onto on FTO electro-conductive glass, obtains the thick Zn of 100 nm2SnO4The FTO electro-conductive glass of Seed Layer；Then pink salt, zinc salt and surfactant are dissolved in the mixed solvent of alkohol and amine, add alkali regulation pH value, placed into and be coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer is leant against in ptfe autoclave inner bag, and conduction faces down, and is tamping reactor stainless steel outer sleeve, is put into baking oven, 200 DEG C of h of isothermal reaction 24, and room temperature is down to naturally, and taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film is post-treated, that is, obtaining the length on FTO electro-conductive glass has fine and close graduation " broccoli " shape Zn2SnO4Thin-film material.The inventive method is simple, easily and fast, favorable reproducibility, graduation " broccoli " the shape Zn of synthesis2SnO4Thin-film material can be widely used for the fields such as solar cell, lithium ion battery, photocatalysis.
Description
Technical field
The present invention obtains National Nature fund youth fund (51502205), Tianjin Normal University's technician introduction project
(5RL131), Tianjin Normal University's school application and development fund (52XK1508) and Tianjin Normal University Students' Innovation wound in 2016
The subsidy of industry drill program project (201610065012.00).
The present invention relates to synthesize zinc stannate (Zn on FTO electro-conductive glass2SnO4) thin-film material preparation field, specifically relate to
And one kind prepares graduation " broccoli " shape graduation Zn on electro-conductive glass2SnO4Thin-film material method, is especially applied
On dye-sensitized solar cells.
Background technology
Zn2SnO4It is a kind of very important broad-band gap (Eg=3.6-3.8 eV) ternary oxide, it is special that it not only has
Property, and performance easily adjusts, and conduction band positions only compare TiO2Low 0.1 eV, isoelectric point (IEP pH=6.5), its electronics is moved
Shifting rate is up to 10-15 cm2 V-1s-1, Zn2SnO4Stable chemical nature, there is stabilization well in acid N719 dyestuffs
Property, therefore Zn2SnO4Turn into the focus that DSSC is studied as light anode material.Zn2SnO4As a class weight
The nano structural material wanted, its technology of preparing has reached its maturity and progressively practical, in solar cell, photocatalysis, gas sensing
The fields such as device, lithium ion battery, insoluble drug release have many important application prospects.
Graduation Zn2SnO4Structural material not only has preferable light scattering ability, while having electric transmission speed faster
Many advantages, such as rate, electric transmission life-span more long and cause numerous researchers concern growing day by day, therefore graduation
Zn2SnO4Structural material is considered as being possible to the photoelectric transformation efficiency for greatly improving solar cell.Although document report some points
Grade Zn2SnO4Application of the light anode material in dye-sensitized solar cells, but due to the graduation Zn for synthesizing2SnO4Receive
Rice material needs to be prepared into slurry brushing to electro-conductive glass and then be applied on dye-sensitized solar cells, makes battery step
It is cumbersome.Synthesize graduation Zn on FTO electro-conductive glass2SnO4Thin-film material, due to possessing above-mentioned all of advantage, is to close at present
In Zn2SnO4The research tendency and study hotspot of light anode material.But on directly preparing graduation on FTO electro-conductive glass
Zn2SnO4Thin-film material and then it is applied in dye-sensitized solar cells, reports less on current document, and opto-electronic conversion imitates
Rate is relatively low.
The content of the invention
It is an object of the invention to be based on the Zn that classifies at present2SnO4The technology of preparing of structural material increasingly it is ripe simultaneously
And be done step-by-step it is practical, the fields such as solar cell, lithium ion battery, photocatalysis, gas sensor insoluble drug release have very
More important application, there is provided one kind directly prepares graduation " broccoli " shape Zn on FTO electro-conductive glass2SnO4Thin-film material
Solvothermal preparation method, the method has many advantages, such as：Synthetic method is simple, convenient and favorable reproducibility etc..By adjustment
Optimal Experimental condition control graduation " broccoli " shape Zn2SnO4Size, and by prepared graduation " broccoli " shape
Zn2SnO4Materials application studies Zn in dye-sensitized solar cells2SnO4Battery performance influence.
The object of the invention is achieved through the following technical solutions：
A kind of method that " broccoli " shape graduation zinc stannate film material is prepared on electro-conductive glass, it is characterised in that by as follows
The step of carry out：
（1）Zn is sprayed on FTO electro-conductive glass2SnO4Seed Layer：The FTO electro-conductive glass for cleaning in advance is taken out, is dried naturally,
The Zn that will be prepared in the form of spraying with spray gun2SnO4Seed Layer solution is sprayed onto on FTO electro-conductive glass, obtains 100 nm thickness
Zn2SnO4The FTO electro-conductive glass of Seed Layer；
（2）Pink salt, zinc salt and surfactant are dissolved in the mixed solvent of alkohol and amine, alkali regulation pH value is added, placed into
It is coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer is leant against in ptfe autoclave inner bag, and conduction faces down, envelope
Tight reactor stainless steel outer sleeve, is put into baking oven, and dry temperature is 70 ~ 120 DEG C, and reaction temperature is 180-220 DEG C, and hydro-thermal is anti-
The time answered is 6h ~ 30 h, and room temperature is down to naturally, and taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, washed,
Alcohol is washed each 3 times, is dried in drying box, that is, obtaining the length on FTO electro-conductive glass has fine and close graduation " broccoli " shape
Zn2SnO4Thin-film material, a diameter of 250 nm, Zn of petal2SnO4A diameter of 2.0 μm, the thickness of film is 7.0 μm；
Wherein described pink salt molar concentration is 0.001 ~ 0.05 mol/L, and the molar concentration of zinc salt is 0.002 ~ 0.1 mol/L,
The quality of surfactant is 0.1-1.0g.It is preferred that pink salt molar concentration is 0.01 ~ 0.05 mol/L, the molar concentration of zinc salt is
0.02 ~ 0.1 mol/L, the quality of surfactant is 0.1-1.0g.
Pink salt of the present invention is stannic chloride pentahydrate, stannous chloride dihydrate, stannous sulfate or stannous oxalate；Zinc salt is
Zinc acetate dihydrate, zinc nitrate, zinc chloride or zinc sulfate；Surfactant is PVP, CTAB or SDS.
The alcohol is ethylene glycol, diglycol or 1,4- butanediols；Amine be ethylenediamine, triethylamine, diethanol amine,
The volume ratio of triethanolamine or DMF, wherein alkohol and amine is 20-90%.
The alkali is NaOH or potassium hydroxide, and pH value is 9 ~ 13.Dry temperature is 70 ~ 120 DEG C.
More detailed description of the present invention is as follows：
（1）Zn is sprayed on FTO electro-conductive glass2SnO4Seed Layer：The FTO electro-conductive glass for cleaning in advance is taken out, is dried naturally,
The Zn that will be prepared in the form of spraying with spray gun2SnO4Seed Layer solution is sprayed onto on FTO electro-conductive glass, obtains 100 nm thickness
Zn2SnO4The FTO electro-conductive glass of Seed Layer；
（2）Pink salt, zinc salt and surfactant are dissolved in the mixed solvent of alkohol and amine, alkali regulation pH value is added, placed into
It is coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer is leant against in ptfe autoclave inner bag, and conduction faces down, envelope
Tight reactor stainless steel outer sleeve, is put into baking oven, 200 DEG C of h of isothermal reaction 24, and room temperature is down to naturally, and taking out length has densification
Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, is dried in 70 DEG C of drying boxes, that is, obtain
Length has fine and close graduation " broccoli " shape Zn on FTO electro-conductive glass2SnO4Thin-film material.
Using hydro-thermal of the invention, synthetic method is prepared for " broccoli " shape Zn on FTO electro-conductive glass2SnO4Thin-film material,
The diameter of " broccoli " petal is about 250 nm, Zn2SnO4Diameter is about 2.0 μm, and the thickness of film is about 7.0 μm.
The obtained graduation zinc stannate Asia/micro-sphere material of the inventive method is entered using X-ray powder diffraction, ESEM etc.
Detailed sign is gone.
Graduation " broccoli " the shape Zn2SnO4The preparation method of thin-film material is a direct step by solvent thermal reaction
And obtain.
The inventive method " broccoli " shape graduation Zn obtained on FTO electro-conductive glass2SnO4Thin-film material can be used extensively
In fields such as solar cell, lithium ion battery, photocatalysis, gas sensors.
A kind of method that " broccoli " shape graduation zinc stannate film material is prepared on electro-conductive glass disclosed by the invention
Compared with prior art, the invention has the advantages that：
（1）The present invention prepares " broccoli " shape graduation Zn using solvent-thermal method on FTO electro-conductive glass2SnO4Thin-film material,
This synthetic method has many characteristics such as simple, convenient and favorable reproducibility；
（2）" broccoli " shape graduation Zn obtained by preparation method of the present invention2SnO4It is quick that thin-film material can directly be used as dyestuff
Change the light anode of solar cell, eliminate and prepare the cumbersome of light model machine film；
（3）Dye-sensitized solar cells are mainly a kind of new solar cell for imitating photosynthesis principle and developing, its
Main advantage is：A () low cost, abundant raw materials, technology are relatively easy, in large area industrialized production have compared with
Big advantage;B () while all raw material and production technology are nontoxic, pollution-free, portion of material can obtain sufficiently reclaiming profit
With exploitation and protection human environment to new energy and regenerative resource have great importance.
Brief description of the drawings
Fig. 1 is the Zn after solvent thermal reaction2SnO4The powder diagram of film；
Fig. 2 (a) is " broccoli " shape graduation Zn2SnO4Film scanning electron microscope, upper right corner insertion is its corresponding high power
Scanning electron microscope (SEM) photograph；B () is Zn2SnO4The profile scanning electron microscope of film.
Fig. 3 is based on ~ 7.0 μm " broccoli " shape graduation Zn2SnO4Film and Zn2SnO4The diffusing reflection of nano particle
Spectrogram；
Fig. 4 is based on ~ 15.0 μm " broccoli " shape graduation Zn2SnO4The photoelectricity of the dye-sensitized solar cells of thin-film material
Stream-voltage curve.
Specific embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention
Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
On the premise of invention spirit and scope, the various changes that are carried out to the material component and consumption in these embodiments or change
Belong to protection scope of the present invention.Raw materials used and reagent of the invention is commercially available.
Embodiment 1
Claim 0.42 g SnCl respectively first4·5H2O, 0.53 g Zn (CH3COO)2·2H2O and 0.5 g PVP are added to 50
In mL beakers, 20 mL ethylene glycol (EG) and 20 mL ethylenediamines (En) are subsequently adding, stir 30 min, under stirring again
0.3 g NaOH are added, continues to stir 15 min, become homogeneous solution.The solution then is fully transferred into 50 mL to gather
In tetrafluoroethene reactor inner bag, place into and be coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer leans against polytetrafluoroethyl-ne
In alkene reaction kettle inner bag, conduction faces down, and is tamping reactor stainless steel outer sleeve, is put into baking oven, 200 DEG C of h of isothermal reaction 24,
Naturally room temperature is down to, taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, dry at 70 DEG C
It is dried in dry case.
Dried white powder is directly used in powder diffraction test, judges its crystal formation, as a result shows in FTO electro-conductive glass
Upper prepared film product is zinc stannate（Fig. 1, XRD）.Characterize its pattern with ESEM, the film that discovery is obtained is point
Grade " broccoli " shape Zn2SnO4Material（Fig. 2 a, b, FE-SEM）, the diameter of " broccoli " petal is about 250 nm, Zn2SnO4
Diameter is about 2.0 μm, and the thickness of film is about 7.0 μm.With the Zn of same thickness2SnO4Nanometer particle film is compared, graduation
" broccoli " shape Zn2SnO4The light scattering ability of material is better than Zn2SnO4Nano particle（Fig. 3, UV）, illustrate the former light capture
Ability is stronger；
Length obtained above is had fine and close " broccoli " shape Zn by us2SnO4The FTO electro-conductive glass of film is cut into be adapted to do and contaminates
The size of material sensitization solar cell, the effective area and thickness of each working electrode film are determined with step instrument, and length is had into densification
Zn2SnO4The FTO electro-conductive glass of film sinters 30 min under the conditions of 520 DEG C, when being cooled to 80 DEG C or so, is soaked in N719
About 20 hours in dyestuff, taking-up can obtain adsorbing the Zn of N719 dyestuffs2SnO4Working electrode.It is molten with the isopropanol containing chloroplatinic acid
Drop is calcined 15 minutes on another piece of FTO electro-conductive glass at 400 DEG C, is obtained containing Pt to electrode；On the working electrode (s finally
Electrolyte is added dropwise（The formula of electrolyte is：0.6 mol/L PMII, 0.03 mol/L I2, 0.05 mol/L LiI, 0.1
mol/L Guanidinium thiocyanate （GuSCN）, 0.5 mol/L 4-tert-butylpyridine（TBP）It is molten
Solution is 85 in volume ratio：In 15 acetonitrile and valeronitrile mixed liquor）, sun electricity is sensitized with the method encapsulated dye of " sandwich " formula
Pond；We have found that the graduation broccoli of ~ 7.0 μ m-thicks " shape Zn2SnO4The short circuit current of film is 1.96 mA cm-2, open circuit
Voltage is 807 mV, and fill factor, curve factor 0.65, photoelectric transformation efficiency reaches 1.03 %.
Embodiment 2
First, 0.42 g SnCl are weighed respectively4·5H2O, 0.53 g Zn (CH3COO)2·2H2O and 0.5 g PVP are added to
In 50 mL beakers, 10 mL ethylene glycol (EG) and 30 mL ethylenediamines (En) are subsequently adding, 30 min are stirred, in stirring
Under add 0.3 g NaOH, continue to stir 15 min, become homogeneous solution.The solution is then fully transferred to 50
In mL ptfe autoclave inner bags, place into and be coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer leans against poly- four
In PVF reactor inner bag, conduction faces down, and is tamping reactor stainless steel outer sleeve, is put into baking oven, 200 DEG C of isothermal reactions
24 h, are down to room temperature naturally, and taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, 70
It is dried in DEG C drying box.
Embodiment 3
First, 0.21 g SnCl are weighed respectively4·5H2O, 0.27 g Zn (CH3COO)2·2H2O and 0.25 g PVP are added to
In 50 mL beakers, 20 mL ethylene glycol (EG) and 20 mL ethylenediamines (En) are subsequently adding, 30 min are stirred, in stirring
Under add 0.15 g NaOH, continue to stir 15 min, become homogeneous solution.The solution is then fully transferred to 50
In mL ptfe autoclave inner bags, place into and be coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer leans against poly- four
In PVF reactor inner bag, conduction faces down, and is tamping reactor stainless steel outer sleeve, is put into baking oven, 200 DEG C of isothermal reactions
24 h, are down to room temperature naturally, and taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, 70
It is dried in DEG C drying box.
Embodiment 4
First, 0.022g stannous chloride dihydrates are weighed respectively, and 0.0575g zinc sulfate and 0.5g CTAB are added to 50 mL beakers
In, 10 mL BDOs and 30 mL triethylamines are subsequently adding, 30 min are stirred, 0.3 g is added under stirring
NaOH, continues to stir 15 min, becomes homogeneous solution.The solution is then fully transferred to 50 mL polytetrafluoroethylene (PTFE) anti-
Answer in kettle inner bag, place into and be coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer is leant against in ptfe autoclave
In courage, conduction is faced down, and is tamping reactor stainless steel outer sleeve, is put into baking oven, 220 DEG C of h of isothermal reaction 30, and room is down to naturally
Temperature, taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, is carried out in 70 DEG C of drying boxes
Dry.
Embodiment 5
First, 0.021g stannous sulfates are weighed respectively, and 0.059 g zinc nitrates and 0.5 g SDS are added in 50 mL beakers, so
After add 10 mL ethylene glycol (EG) and 30 mL DMFs, stir 30 min, added under stirring
0.3 g NaOH, continue to stir 15 min, become homogeneous solution.The solution is then fully transferred to 50 mL polytetrafluoros
In ethylene reaction kettle inner bag, place into and be coated with Zn in advance2SnO4It is anti-that the FTO electro-conductive glass of Seed Layer leans against polytetrafluoroethylene (PTFE)
Answer in kettle inner bag, conduction faces down, be tamping reactor stainless steel outer sleeve, be put into baking oven, 180 DEG C of h of isothermal reaction 18 are natural
Room temperature is down to, taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, in 70 DEG C of drying boxes
In be dried.
Claims (6)
1. the method that one kind prepares " broccoli " shape graduation zinc stannate film material on electro-conductive glass, it is characterised in that by such as
Under step carry out：
（1）Zn is sprayed on FTO electro-conductive glass2SnO4Seed Layer：The FTO electro-conductive glass for cleaning in advance is taken out, is dried naturally,
The Zn that will be prepared in the form of spraying with spray gun2SnO4Seed Layer solution is sprayed onto on FTO electro-conductive glass, obtains 100 nm thickness
Zn2SnO4The FTO electro-conductive glass of Seed Layer；
（2）Pink salt, zinc salt and surfactant are dissolved in the mixed solvent of alkohol and amine, alkali regulation pH value is added, placed into
It is coated with Zn in advance2SnO4The FTO electro-conductive glass of Seed Layer is leant against in ptfe autoclave inner bag, and conduction faces down, envelope
Tight reactor stainless steel outer sleeve, is put into baking oven, and reaction temperature is 180-220 DEG C, and the time of hydro-thermal reaction is 6h ~ 30 h, from
Room temperature is so down to, taking out length has fine and close Zn2SnO4The FTO electro-conductive glass of film, is washed, alcohol is washed each 3 times, in drying box
It is dried, that is, obtaining the length on FTO electro-conductive glass has fine and close graduation " broccoli " shape Zn2SnO4Thin-film material, petal it is straight
Footpath is 250 nm, Zn2SnO4A diameter of 2.0 μm, the thickness of film is 7.0 μm；
Wherein described pink salt molar concentration is 0.001 ~ 0.05 mol/L, and the molar concentration of zinc salt is 0.002 ~ 0.1 mol/L,
The quality of surfactant is 0.1-1.0g.
2. the preparation method described in claim 1, it is characterised in that step（2）Middle pink salt molar concentration is 0.01 ~ 0.05 mol/
L, the molar concentration of zinc salt is 0.02 ~ 0.1 mol/L, and the quality of surfactant is 0.1-1.0g.
3. the preparation method described in claim 1, it is characterised in that step（2）Middle pink salt is stannic chloride pentahydrate, two water chlorinations
Stannous, stannous sulfate or stannous oxalate；Zinc salt is zinc acetate dihydrate, zinc nitrate, zinc chloride or zinc sulfate；Surfactant is
PVP, CTAB or SDS.
4. the preparation method described in claim 1, it is characterised in that step（2）Middle alcohol be ethylene glycol, diglycol or 1,
4- butanediols；Amine is ethylenediamine, triethylamine, diethanol amine, triethanolamine or DMF, the wherein body of alkohol and amine
Product ratio is 20-90%.
5. the preparation method described in claim 1, it is characterised in that step（2）Middle alkali is NaOH or potassium hydroxide, pH value
It is 9 ~ 13.
6. the preparation method described in claim 1, it is characterised in that step（2）Middle hydro-thermal reaction is completed by baking oven, is done
Dry temperature is 70 ~ 120 DEG C.
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| CN108529896B (en) * | 2018-05-18 | 2021-04-23 | 江苏华玻光电技术有限公司 | Preparation method of anti-glare glass material |
| CN112537794A (en) * | 2020-11-17 | 2021-03-23 | 欣旺达电动汽车电池有限公司 | Zinc germanate nano material, preparation method thereof and lithium ion battery |
| CN112537794B (en) * | 2020-11-17 | 2023-04-07 | 欣旺达电动汽车电池有限公司 | Zinc germanate nano material, preparation method thereof and lithium ion battery |
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