CN108893728A - The preparation method of ultra-thin ZnO nano chip arrays with high-specific surface area - Google Patents
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Abstract
The preparation method of ultra-thin ZnO nano chip arrays with high-specific surface area, the invention belongs to photoelectric semiconductor material fields, it is lower for the specific surface area for solving the problems, such as existing two-dimensional nano piece array structure.Preparation method:One, the zinc acetate-ethyl alcohol seed liquor for being 0.1~0.5mol/L with circumfluence method preparation concentration;Two, even application zinc acetate-ethyl alcohol seed liquor is multiple in conductive substrates after cleaning, with temperature calcination 20~40 minutes of 400~450 DEG C under air atmosphere, obtains the conductive substrates with ZnO seed layer;Three, the conductive substrates with ZnO seed layer are immersed in reaction solution, and wherein reaction solution is the mixed aqueous solution containing zinc source, HMT, fluoride and sodium citrate;Four, sintering processes.The specific surface area for the ultrathin nanometer chip arrays that preparation method through the invention obtains is up to 90.7m2/ g has class graphene-structured, while having both quick electronic transport property.
Description
Technical field
The invention belongs to photoelectric semiconductor material fields, and in particular to one kind has class graphene-structured, high-specific surface area
ZnO nano chip arrays preparation method.
Background technique
Photoelectric semiconductor material is the hot spot studied now because of its many potential application.As the important of semiconductor family
A member, ZnO are a kind of environmental-friendly, cheap broad-band gap n-type semiconductors, and in transistor, gas sensor, catalysis
There is important application in the fields such as agent, solar cell.Due to the anisotropy that ZnO is excellent, keep its pattern changeable, and different patterns
Correspond to different property and application.Wherein, ZnO nano-structure array due to its unique optics, electricity and mechanical property and
It is widely studied, if it can be used for the light anode of dye-sensitized solar cells (DSSCs), can be used for formaldehyde gas sensor and receive
The fields such as rice generator, therefore designing and control synthesis, there is the ZnO nano array of unique texture to be very important.
It is had been a concern using hydro-thermal method preparation ZnO nano array, because the method is easy to operate, energy consumption is lower, and
And it is easy to regulate and control the time and temperature of reaction.Since One-Dimensional ZnO array in 2001 occurs, the One-Dimensional ZnOs such as nanometer rods, nano wire
Array is constantly developed.However one-dimensional array structure (nanometer rods, nano wire etc.) is although maintain guiding certain in dimension
Property, conducive to the transmission of electronics, but relatively low specific surface area limits its electricity as dye-sensitized solar cells light anode
Pond efficiency.Traditional two-dimensional nano piece array structure, since the thickness of nanometer sheet is thicker, generally all at ten nanometers or more, even
Tens nanometers, specific surface area is not also high, this greatly limits the battery efficiency of solar battery.
As the light anode of photoelectric device, big specific surface area and quick electronic transmission performance are to determine resulting devices
Two key factors of performance.
Summary of the invention
The purpose of the present invention is to solve the lower problems of the specific surface area of existing two-dimensional nano piece array structure, and mention
For a kind of preparation method of ultra-thin ZnO nano chip arrays with high-specific surface area.
There is the present invention preparation method of the ultra-thin ZnO nano chip arrays of high-specific surface area to follow these steps to realize:
One, seed layer solution is prepared:Zinc acetate is added in dehydrated alcohol, use circumfluence method preparation concentration for 0.1~
The zinc acetate of 0.5mol/L-ethyl alcohol seed liquor;
Two, ZnO seed layer is prepared in conductive substrates:Even application zinc acetate-ethyl alcohol kind in conductive substrates after cleaning
Sub- liquid is multiple, and drying is placed in Muffle furnace, with temperature calcination 20~40 minutes of 400~450 DEG C under air atmosphere, obtains band
There are the conductive substrates of ZnO seed layer;
Three, the preparation of ultra-thin Zn (OH) F nanometer sheet:The conductive substrates with ZnO seed layer that step 2 is obtained immerse
It reacts 3~6 hours, obtains after cleaning-drying with ultra-thin Zn (OH) F nanometer sheet in the reaction solution for being 80~92 DEG C to temperature
Conductive substrates;
Four, it calcines:The conductive substrates with ultra-thin Zn (OH) F nanometer sheet that step 3 is obtained at 400 DEG C~500 DEG C
It is sintered, obtains the conductive substrates of the ultra-thin ZnO nano chip arrays with high-specific surface area;
Reaction solution described in step 3 is to contain zinc source, HMT (hexamethylene tetramine), fluoride and sodium citrate
The mixed aqueous solution of (or citric acid), the fluoride are tetrabutyl ammonium fluoride or ammonium fluoride;
The concentration in zinc source is 0.01~0.05mol/L in reaction solution, and the concentration of HMT is 0.01~0.05mol/L, fluoride
Concentration be 0.03~0.0475mol/L.
Traditional ZnO reaction solution is zinc nitrate and hexamethylene tetramine mixed aqueous solution, and ZnO is preferential under this reaction condition
It is grown along c-axis [001] direction, the columns pattern such as nanometer rods easily generated, this is because (001) crystal plane surface of ZnO can be high.?
In the present invention, fluoride and citrate in reaction solution can be preferentially adsorbed on ZnO (001) crystalline substance that surface can be high as complex
Face, it is suppressed that ZnO is grown along [001] direction, ratio between the two is deployed, to obtain ultra-thin ZnO nano chip arrays.
The preparation method with class graphene-structured, the ZnO nano chip arrays of bigger serface that the present invention provides a kind of,
The specific surface area of the ultrathin nanometer chip arrays obtained by the preparation method is up to 90.7m2/ g, while having both quick electronics and passing
Defeated property.
Detailed description of the invention
Fig. 1 is the XRD diffraction pattern of ultra-thin ZnO nano piece obtained in embodiment, and wherein ※ represents FTO conductive substrates;
Fig. 2 is the surface electron microscope of the ultra-thin ZnO nano piece obtained after calcining in embodiment;
Fig. 3 is the section electron microscope of the ultra-thin ZnO nano piece obtained after calcining in embodiment;
Fig. 4 is the transmission electron microscope picture for ultra-thin Zn (OH) the F nanometer sheet (without calcining) that step 3 obtains in embodiment;
Fig. 5 is the transmission electron microscope picture for the ultra-thin ZnO nano piece (after calcining) that step 4 obtains in embodiment;
Fig. 6 is the specific surface area figure of ultra-thin ZnO nano piece obtained in embodiment, wherein 1-absorption, 2-desorptions;
Fig. 7 is the graph of pore diameter distribution of ultra-thin ZnO nano piece obtained in embodiment;
Fig. 8 is the surface photovoltage spectrogram of ultra-thin ZnO nano chip arrays obtained in embodiment;
Fig. 9 is the battery efficiency test chart of ultra-thin ZnO nano chip arrays obtained in embodiment.
Specific embodiment
Specific embodiment one:Present embodiment has the preparation method of the ultra-thin ZnO nano chip arrays of high-specific surface area
It follows these steps to realize:
One, seed layer solution is prepared:Zinc acetate is added in dehydrated alcohol, use circumfluence method preparation concentration for 0.1~
The zinc acetate of 0.5mol/L-ethyl alcohol seed liquor;
Two, ZnO seed layer is prepared in conductive substrates:Even application zinc acetate-ethyl alcohol kind in conductive substrates after cleaning
Sub- liquid is multiple, and drying is placed in Muffle furnace, with temperature calcination 20~40 minutes of 400~450 DEG C under air atmosphere, obtains band
There are the conductive substrates of ZnO seed layer;
Three, the preparation of ultra-thin Zn (OH) F nanometer sheet:The conductive substrates with ZnO seed layer that step 2 is obtained immerse
It reacts 3~6 hours, obtains after cleaning-drying with ultra-thin Zn (OH) F nanometer sheet in the reaction solution for being 80~92 DEG C to temperature
Conductive substrates;
Four, it calcines:The conductive substrates with ultra-thin Zn (OH) F nanometer sheet that step 3 is obtained at 400 DEG C~500 DEG C
It is sintered, obtains the conductive substrates of the ultra-thin ZnO nano chip arrays with high-specific surface area;
Reaction solution described in step 3 is to contain zinc source, HMT (hexamethylene tetramine), fluoride and sodium citrate
The mixed aqueous solution of (or citric acid), the fluoride are tetrabutyl ammonium fluoride or ammonium fluoride;
The concentration in zinc source is 0.01~0.05mol/L in reaction solution, and the concentration of HMT is 0.01~0.05mol/L, fluoride
Concentration be 0.03~0.0475mol/L.
Present embodiment is to further increase the specific surface area of ZnO nano piece, improves dyestuff in dye-sensitized solar cells
Adsorbance, design a kind of new type superthin ZnO nano chip arrays, form this array ultra-thin ZnO nano piece have class graphite
Alkene structure, and there is high specific surface area, the photoelectric conversion efficiency of DSSCs can be improved.
Specific embodiment two:The present embodiment is different from the first embodiment in that by acetic anhydride zinc in step 1
It is put into reactor, dehydrated alcohol is then added, be heated to reflux 2.5~3.5h at 80 DEG C.
Specific embodiment three:The present embodiment is different from the first and the second embodiment in that step 2 is after cleaning
Use film balance with speed even application zinc acetate-ethyl alcohol seed liquor 3~5 times of 200mm/min in conductive substrates.
Specific embodiment four:Unlike one of present embodiment and specific embodiment one to three described in step 2
Drying temperature be 80 DEG C.
Specific embodiment five:Unlike one of present embodiment and specific embodiment one to four described in step 2
Conductive substrates be FTO conductive substrates.
Specific embodiment six:Unlike one of present embodiment and specific embodiment one to five described in step 3
Zinc source be zinc nitrate, zinc acetate or zinc sulfate.
Specific embodiment seven:Described in step 3 unlike one of present embodiment and specific embodiment one to six
The concentration of sodium citrate is 0.001~0.01mol/L in reaction solution.
Specific embodiment eight:The reaction of step 3 unlike one of present embodiment and specific embodiment one to seven
The concentration in zinc source is 0.02~0.04mol/L in liquid, and the concentration of HMT is 0.02~0.04mol/L, and the concentration of fluoride is 0.04
~0.0475mol/L, the concentration of sodium citrate are 0.004~0.006mol/L.
Specific embodiment nine:Step 4 is with super unlike one of present embodiment and specific embodiment one to eight
The conductive substrates of thin Zn (OH) F nanometer sheet are put into tube furnace, are passed through O2、N2Or air, the sintering processes at 400 DEG C~500 DEG C
0.8~1.2h.
Specific embodiment ten:Step 4 conductive base unlike one of present embodiment and specific embodiment one to nine
Ultra-thin ZnO nano chip arrays on bottom with a thickness of 5~15 microns.
Embodiment:There is the present embodiment the preparation method of the ultra-thin ZnO nano chip arrays of high-specific surface area to follow these steps
It realizes:
One, seed layer solution is prepared:It weighs 0.367g acetic anhydride zinc to be put into round-bottomed flask, then be drawn with liquid-transfering gun
20ml dehydrated alcohol is set in a round bottom flask, and 3h, zinc acetate-ethyl alcohol that preparation concentration is 0.1mol/L are heated to reflux at 80 DEG C
Seed liquor;
Two, ZnO seed layer is prepared in conductive substrates:FTO glass successively uses deionized water, acetone, ethyl alcohol, acetone and second
Alcohol is cleaned by ultrasonic 10 minutes respectively, uses N2Drying, the conductive substrates after being cleaned use the conductive base of film balance after cleaning
Even application zinc acetate-ethyl alcohol seed liquor 3 times on bottom is dried at 80 DEG C and is placed in Muffle furnace, with 450 DEG C under air atmosphere
Temperature calcination 30 minutes, obtain the conductive substrates with ZnO seed layer;
Three, the preparation of ultra-thin Zn (OH) F nanometer sheet:The conductive substrates with ZnO seed layer that step 2 is obtained immerse
It reacts 3 hours into 92 DEG C of reaction solutions, with deionized water repeated flushing, is obtained after natural drying with F nanometers of ultra-thin Zn (OH)
The conductive substrates of piece;
Four, it calcines:Conductive substrates with ultra-thin Zn (OH) F nanometer sheet are put into tube furnace, at 400 DEG C under oxygen atmosphere
Lower sintering processes 1h obtains the conductive substrates of the ultra-thin ZnO nano chip arrays with high-specific surface area;
Reaction solution described in step 3 is the mixed aqueous solution containing zinc nitrate, HMT, ammonium fluoride and sodium citrate,
Middle nitric acid zinc concentration is 0.03mol/L, and the concentration of HMT is 0.03mol/L, and the concentration of ammonium fluoride is 0.0475mol/L, lemon
The concentration of sour sodium is 0.005mol/L.
Fig. 1 is the XRD diffraction pattern for the ZnO nano piece that the present embodiment obtains, the compound wurtzite structure of sample, diffraction maximum and card
Piece PDF-36-1451 is completely corresponding, and since sample is grown in FTO substrate, the peak of FTO is labeled.
Fig. 2 and Fig. 3 is the electron microscope through calcined ZnO nano piece, and electron microscope shows the porous knot of ZnO nano piece
Structure, section electron microscope show uncollapsed holding porous structure.
The transmission electron microscope picture of ZnO nano piece without calcining is as shown in figure 4, show class graphene super-thin sheet-shaped structure.
The specific surface area of the ultra-thin ZnO nano chip arrays with high-specific surface area obtained as can be seen from FIG. 6 is
90.67m2/g。
Fig. 8 is the surface photovoltage spectrogram of ultra-thin ZnO nano chip arrays, it is known that photoelectric signal is positive signal, illustrates ZnO
It is typical n-type semiconductor, ultra-violet (UV) band photoelectric signal is obvious, and peak light voltage strength reaches 17.5 μ V, with excellent point
From efficiency.
Ultra-thin ZnO nano chip arrays are dipped in the N719 dye solution of 0.5mmol/L, immersion 1 hour is protected from light under room temperature.
Electrolyte by 0.8mol/L 1- hexyl -2,3- methylimidazole quinoline iodide and 50mmol/L methoxypropionitrile iodine solution group
At.It injects the electrolyte into anode diaphragm and between electrode, and accompanies one layer of insulating film.The J-V curve test of battery has
Effect area is 0.5cm2.The battery efficiency 0.96% of the ZnO array of 6 micron thickness, voltage 0.47V, current density 4.52mA/
cm2, impact factor 0.45, as shown in figure 9, showing excellent photoelectric conversion efficiency.
Claims (10)
1. the preparation method of the ultra-thin ZnO nano chip arrays with high-specific surface area, it is characterised in that this method is by following step
It is rapid to implement:
One, seed layer solution is prepared:Zinc acetate is added in dehydrated alcohol, use circumfluence method preparation concentration for 0.1~
The zinc acetate of 0.5mol/L-ethyl alcohol seed liquor;
Two, ZnO seed layer is prepared in conductive substrates:Even application zinc acetate-ethyl alcohol seed liquor in conductive substrates after cleaning
Repeatedly, drying is placed in Muffle furnace, with temperature calcination 20~40 minutes of 400~450 DEG C under air atmosphere, is had
The conductive substrates of ZnO seed layer;
Three, the preparation of ultra-thin Zn (OH) F nanometer sheet:The conductive substrates with ZnO seed layer that step 2 is obtained are immersed in temperature
Degree obtains the conduction with ultra-thin Zn (OH) F nanometer sheet to react 3~6 hours in 80~92 DEG C of reaction solution after cleaning-drying
Substrate;
Four, it calcines:The conductive substrates with ultra-thin Zn (OH) F nanometer sheet that step 3 obtains are carried out at 400 DEG C~500 DEG C
Sintering processes obtain the conductive substrates of the ultra-thin ZnO nano chip arrays with high-specific surface area;
Reaction solution described in step 3 is the mixed aqueous solution containing zinc source, HMT, fluoride and sodium citrate, the fluorine
Compound is tetrabutyl ammonium fluoride or ammonium fluoride;
The concentration in zinc source is 0.01~0.05mol/L in reaction solution, and the concentration of HMT is 0.01~0.05mol/L, fluoride it is dense
Degree is 0.03~0.0475mol/L.
2. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
Acetic anhydride zinc is put into reactor in step 1, dehydrated alcohol is then added, it is heated to reflux 2.5 at 80 DEG C~
3.5h。
3. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
In used in the conductive substrates of step 2 after cleaning film balance with speed even application zinc acetate-ethyl alcohol kind of 200mm/min
Sub- liquid 3~5 times.
4. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
Drying temperature described in step 2 is 80 DEG C.
5. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
Conductive substrates described in step 2 are FTO conductive substrates.
6. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
Zinc source described in step 3 is zinc nitrate, zinc acetate or zinc sulfate.
7. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
The concentration of sodium citrate is 0.001~0.01mol/L in reaction solution described in step 3.
8. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
The concentration in zinc source is 0.02~0.04mol/L in the reaction solution of step 3, and the concentration of HMT is 0.02~0.04mol/L, fluorination
The concentration of object is 0.04~0.0475mol/L, and the concentration of sodium citrate is 0.004~0.006mol/L.
9. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature exist
It is put into tube furnace in step 4 with the conductive substrates of ultra-thin Zn (OH) F nanometer sheet, is passed through O2、N2Or air, 400 DEG C~
0.8~1.2h of sintering processes at 500 DEG C.
10. the preparation method of the ultra-thin ZnO nano chip arrays according to claim 1 with high-specific surface area, feature
Be the ultra-thin ZnO nano chip arrays in step 4 conductive substrates with a thickness of 5~15 microns.
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CN110102333A (en) * | 2019-06-19 | 2019-08-09 | 牡丹江师范学院 | A kind of preparation method of C, N codope ZnO nano-structure array |
WO2020258959A1 (en) * | 2019-06-26 | 2020-12-30 | 五邑大学 | Zno nanosheet and preparation method therefor |
CN111018365A (en) * | 2019-12-30 | 2020-04-17 | 黑龙江省科学院高技术研究院 | Method for in-situ preparation of silver nanoparticle loaded ZnO nano-foam |
CN114887614A (en) * | 2022-05-16 | 2022-08-12 | 扬州大学 | Preparation method of ZnO flexible film with high optical performance |
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