CN106882834B - A kind of method that ZnO nano-rod array film is prepared in situ and its film obtained - Google Patents
A kind of method that ZnO nano-rod array film is prepared in situ and its film obtained Download PDFInfo
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- CN106882834B CN106882834B CN201710214272.5A CN201710214272A CN106882834B CN 106882834 B CN106882834 B CN 106882834B CN 201710214272 A CN201710214272 A CN 201710214272A CN 106882834 B CN106882834 B CN 106882834B
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- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of methods that ZnO nano-rod array film is prepared in situ, by the preparation of organic ammonium salt, the preparation of two-dimensional layer chlorination zinc-base hydridization perovskite, the sintering of chlorination zinc-base hydridization perovskite spin coating film, chlorination zinc-base hydridization perovskite film layer, to be prepared in situ to obtain nanometic zinc oxide rod array film in substrate.The present invention utilizes chlorination zinc-base hydridization perovskite crystalline template, and organic component is removed by calcining, and nanometic zinc oxide rod array pattern made from original position is uniform in substrate, vertical ordered arrangement, and the size and shape of nanometer rods is controllable.Preparation process of the present invention is simple, at low cost, is conducive to promotion and application.
Description
Technical field
The present invention relates to nano zinc oxide material technical field more particularly to one kind, that ZnO nano-rod array is prepared in situ is thin
The method of film and its film obtained.
Background technology
The energy gaps of ZnO at normal temperatures are 3.37eV, are that a kind of band gap is wide, exciton bind energy is high, thermal stability is good, system
Preparation Method is simple, appearance and size is various and cheap semi-conducting material.The speed of growth of each crystal faces of ZnO has very very much not
It together, can be by regulating and controlling experiment condition, to change the growth rate of different directions, to obtain therefore during preparing ZnO
Various nanotopography structures.ZnO has nano particle, nano-comb, nano-array, nano-hollow ball, nanobelt, nanometer
The different morphologies structure such as ring, nanotube, can be widely applied to the fields such as ceramics, chemical industry, optics, electronics and biology.
Wherein, one-dimensional nano zinc oxide material structure uniformly, good crystallinity, crystal defect it is less, be conducive to electronics
Directional transmissions have excellent optics, the performances such as electrically and thermally, are provided for the nanosizing of electronic device, low-dimensionalization development
Basis, therefore, one-dimensional zinc oxide nanometer material have attracted the sight of numerous researchers.
The preparation method of existing Synthetic Routes of One-dimensional ZnO Nanorods mainly has crystal seed revulsion, chemical vapour deposition technique and hydro-thermal
Method etc., these methods are prepared by crystallization nucleation and the process of growth.Currently, the prior art is although synthesis ZnO receives
Rice stick method it is more but still poor in the prevalence of the zinc oxide nano rod size adjustable of preparation and be easier to reunite,
The technological deficiencies such as the order and controllability deficiency of nanometic zinc oxide rod array.Therefore, it explores and develops novel low cost original position
Nanometic zinc oxide rod array growing method is prepared to be of great significance.
Invention content
Chlorination zinc-base hydridization perovskite crystalline is utilized it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of
The method that ZnO nano-rod array film is prepared in situ in template in substrate, to obtain vertical ordered arrangement, pattern uniform, controllable
ZnO nano-rod array.Another object of the present invention is to provide utilize film made from above-mentioned preparation method.
The purpose of the present invention is achieved by the following technical programs：
A kind of method that ZnO nano-rod array film is prepared in situ provided by the invention, includes the following steps：
(1) preparation of organic ammonium salt
Organic monoamine RNH2Or organic diamine NH2RNH2Ethanol solution, wherein R=CnH2n, n >=1 is added with hydrochloric acid
Organic mono-ammonium RNH is made after vacuum distillation, filtering, recrystallization, drying in hot back flow reaction3Cl or organic di-ammonium salts
NH3ClRNH3Cl；
(2) preparation of two-dimensional layer chlorination zinc-base hydridization perovskite
According to molal weight than organic mono-ammonium RNH3Cl: zinc chloride=2: 1 or described organic di-ammonium salts
NH3ClRNH3Cl: zinc chloride=1: 1, by organic mono-ammonium RNH3The ethanol solution of Cl or organic di-ammonium salts
NH3ClRNH3The ethanol solution of Cl is mixed with the ethanol solution of zinc chloride, carry out heating reflux reaction, through vacuum distillation, filtering,
After recrystallization, drying, two-dimensional layer chlorination zinc-base hydridization perovskite (RNH is made3)2ZnCl4Or NH3RNH3ZnCl4；
(3) the perovskite spin coating of chlorination zinc-base hydridization is film-made
By the hydridization perovskite (RNH3)2ZnCl4Or NH3RNH3ZnCl4After being dissolved in solvent, cleaned using sol evenning machine
Substrate on chlorination zinc-base hydridization perovskite film layer is prepared by spin coating；
(4) sintering of chlorination zinc-base hydridization perovskite
The chlorination zinc-base hydridization perovskite film layer is sintered, i.e., is prepared in situ to obtain zinc-oxide nano in substrate
Rod array film.
Further, heating reflux reaction temperature is 70~80 DEG C in step (1) of the present invention, step (2), when reaction
Between be 0.5~2h.By hydridization perovskite (RNH described in 20~100mg in the step (3)3)2ZnCl4Or NH3RNH3ZnCl4It is molten
In 1mL solvents；Solvent is absolute ethyl alcohol, propyl alcohol, isobutanol, DMF or DMSO；The speed of spin coating is 2000~5000rpm.
In said program, substrate of the present invention be ITO electro-conductive glass, FTO electro-conductive glass, AZO electro-conductive glass, it is flexible thoroughly
Bright conductive substrates, quartz glass or silicon-based substrate.
Further, step (4) of the present invention is sintered 0.5~2h in oxygen atmosphere at a temperature of 300~500 DEG C.
It is a diameter of using film, the ZnO nanorod made from the above-mentioned method that ZnO nano-rod array film is prepared in situ
100~150nm, length are 400~500nm.
The invention has the advantages that：
The present invention utilizes the crystallization template of chlorination zinc-base hydridization perovskite, organic component is removed by calcining, in substrate
The nanometic zinc oxide rod array of uniform, the vertical ordered arrangement of obtained pattern in situ, and the size and shape of nanometer rods is controllable.This
Invention preparation process is simple, at low cost, is conducive to promotion and application.
Description of the drawings
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail：
Fig. 1 is the scanning electron microscopy picture SEM of ZnO nano-rod array film made from the embodiment of the present invention（(a)：10
Wan Bei, (b)：50000 times, (c)：20000 times, (d)：10000 times）；
Fig. 2 is the image K-M EDX of ZnO nano-rod array film made from the embodiment of the present invention；
Fig. 3 is the X-ray diffraction image XRD of ZnO nano-rod array film made from the embodiment of the present invention.
Specific implementation mode
Fig. 1~Fig. 3 show a kind of embodiment for the method that ZnO nano-rod array film is prepared in situ of the present invention.
The embodiment of the present invention uses FTO electro-conductive glass slide for substrate, and cleaning process is as follows：Slide is sequentially placed into and is washed
In clean essence, deionized water, ethyl alcohol, isopropanol, acetone solvent, 15min is respectively cleaned by ultrasonic with ultrasonic cleaner, will finally be washed
Slide nitrogen gun dry up and be put into baking oven and dried at a temperature of 80 DEG C.
The organic monoamine RNH of the embodiment of the present invention2Or organic diamine NH2RNH2, zinc chloride be analyze it is pure；The quality of hydrochloric acid
Purity is 36~38%, is solution shape.
Embodiment one：
A kind of method that ZnO nano-rod array film is prepared in situ of the present embodiment, its step are as follows：
(1) preparation of organic ammonium salt
Weigh 0.2mol CH3CH2NH2It is dissolved in 10mL absolute ethyl alcohols, 0.22mL hydrochloric acid, 80 DEG C of temperature is added dropwise under ice-water bath
Ammonium salt CH is made after vacuum distillation, filtering, recrystallization, drying in lower condensing reflux 1h3CH2NH3Cl；
(2) preparation of two-dimensional layer chlorination zinc-base hydridization perovskite
Weigh above-mentioned 0.1mol ammonium salts CH3CH2NH3Cl is dissolved in 20mL absolute ethyl alcohols, 0.05mol ZnCl2It is dissolved in 10mL
In absolute ethyl alcohol, chlorine is made after vacuum distillation, filtering, recrystallization, drying in condensing reflux 1h at a temperature of 80 DEG C after mixing
Change zinc-base hydridization perovskite (CH3CH2NH3)2ZnCl4；
(3) the perovskite spin coating of chlorination zinc-base hydridization is film-made
Weigh above-mentioned 40mg chlorinations zinc-base hydridization perovskite (CH3CH2NH3)2ZnCl4After being dissolved in 1mL absolute ethyl alcohols, use is even
Glue machine, with the speed spin coating 30s of 2000rpm, obtains chlorination zinc-base hydridization perovskite (CH in the substrate cleaned3CH2NH3)2ZnCl4Film layer；
(4) sintering of chlorination zinc-base hydridization perovskite
By above-mentioned chlorination zinc-base hydridization perovskite (CH3CH2NH3)2ZnCl4Film layer is placed in Muffle furnace and is sintered, warp
50min is raised to 300 DEG C, heat preservation 10min, is raised to 350 DEG C, heat preservation 15min through 15min, i.e., is prepared in situ to obtain oxygen in substrate
Change zinc nano-stick array thin film.
Embodiment two：
A kind of method that ZnO nano-rod array film is prepared in situ of the present embodiment, its step are as follows：
(1) preparation of organic ammonium salt
Weigh 0.2mol NH2CH2CH2NH2It is dissolved in 10mL absolute ethyl alcohols, dropwise addition 0.44mL hydrochloric acid under ice-water bath, 80 DEG C
At a temperature of condensing reflux 1h, through vacuum distillation, filtering, recrystallization, it is dry after, ammonium salt NH is made3ClCH2CH2NH3Cl；
(2) preparation of two-dimensional layer chlorination zinc-base hydridization perovskite
Weigh above-mentioned 0.1mol ammonium salts NH3ClCH2CH2NH3Cl is dissolved in 20mL absolute ethyl alcohols, 0.1mol ZnCl2It is dissolved in
In 20mL absolute ethyl alcohols, condensing reflux 1h makes after vacuum distillation, filtering, recrystallization, drying at a temperature of 80 DEG C after mixing
Obtain chlorination zinc-base hydridization perovskite NH3CH2CH2NH3ZnCl4；
(3) the perovskite spin coating of chlorination zinc-base hydridization is film-made
Weigh above-mentioned 60mg chlorinations zinc-base hydridization perovskite NH3CH2CH2NH3ZnCl4After being dissolved in 1mL absolute ethyl alcohols, use is even
Glue machine, with the speed spin coating 30s of 3000rpm, obtains chlorination zinc-base hydridization perovskite in the substrate cleaned
NH3CH2CH2NH3ZnCl4Film layer；
(4) sintering of chlorination zinc-base hydridization perovskite
By above-mentioned chlorination zinc-base hydridization perovskite NH3CH2CH2NH3ZnCl4Film layer is placed in Muffle furnace and is sintered, warp
50min is raised to 325 DEG C, heat preservation 10min, is raised to 400 DEG C, heat preservation 15min through 15min, i.e., is prepared in situ to obtain oxygen in substrate
Change zinc nano-stick array thin film.
Embodiment three：
A kind of method that ZnO nano-rod array film is prepared in situ of the present embodiment, its step are as follows：
(1) preparation of organic ammonium salt
Weigh 0.2mol CH3CH2CH2NH2It is dissolved in 10mL absolute ethyl alcohols, dropwise addition 0.22mL hydrochloric acid under ice-water bath, 80 DEG C
At a temperature of condensing reflux 1h, through vacuum distillation, filtering, recrystallization, it is dry after, ammonium salt CH is made3CH2CH2NH3Cl；
(2) preparation of two-dimensional layer chlorination zinc-base hydridization perovskite
Weigh above-mentioned 0.1mol ammonium salts CH3CH2CH2NH3Cl is dissolved in 20mL absolute ethyl alcohols, 0.05mol ZnCl2It is dissolved in
In 10mL absolute ethyl alcohols, condensing reflux 1h makes after vacuum distillation, filtering, recrystallization, drying at a temperature of 80 DEG C after mixing
Obtain chlorination zinc-base hydridization perovskite (CH3CH2CH2NH3)2ZnCl4；
(3) the perovskite spin coating of chlorination zinc-base hydridization is film-made
Weigh above-mentioned 80mg chlorinations zinc-base hydridization perovskite (CH3CH2CH2NH3)2ZnCl4After being dissolved in 1mL absolute ethyl alcohols, adopt
With sol evenning machine in the substrate cleaned with the speed spin coating 30s of 4000rpm, obtain chlorination zinc-base hydridization perovskite
(CH3CH2CH2NH3)2ZnCl4Film layer；
(4) sintering of chlorination zinc-base hydridization perovskite
By above-mentioned chlorination zinc-base hydridization perovskite (CH3CH2CH2NH3)2ZnCl4Film layer is placed in Muffle furnace and is sintered, warp
50min is raised to 375 DEG C, heat preservation 10min, is raised to 450 DEG C, heat preservation 15min through 15min, i.e., is prepared in situ to obtain oxygen in substrate
Change zinc nano-stick array thin film.
Example IV：
A kind of method that ZnO nano-rod array film is prepared in situ of the present embodiment, its step are as follows：
(1) preparation of organic ammonium salt
Weigh 0.2mol NH2(CH2)6NH2It is dissolved in 10mL absolute ethyl alcohols, dropwise addition 0.44mL hydrochloric acid under ice-water bath, 80 DEG C
At a temperature of condensing reflux 1h, through vacuum distillation, filtering, recrystallization, it is dry after, ammonium salt NH is made3Cl(CH2)6NH3Cl；
(2) preparation of two-dimensional layer chlorination zinc-base hydridization perovskite
Weigh above-mentioned 0.1mol ammonium salts NH3Cl(CH2)6NH3Cl is dissolved in 20mL absolute ethyl alcohols, 0.1mol ZnCl2It is dissolved in
In 20mL absolute ethyl alcohols, condensing reflux 1h makes after vacuum distillation, filtering, recrystallization, drying at a temperature of 80 DEG C after mixing
Obtain chlorination zinc-base hydridization perovskite NH3(CH2)6NH3ZnCl4；
(3) the perovskite spin coating of chlorination zinc-base hydridization is film-made
Weigh above-mentioned 100mg chlorinations zinc-base hydridization perovskite NH3(CH2)6NH3ZnCl4After being dissolved in 1mL absolute ethyl alcohols, use
Sol evenning machine, with the speed spin coating 30s of 3000rpm, obtains chlorination zinc-base hydridization perovskite NH in the substrate cleaned3(CH2)6NH3ZnCl4Film layer；
(4) sintering of chlorination zinc-base hydridization perovskite
By above-mentioned chlorination zinc-base hydridization perovskite NH3(CH2)6NH3ZnCl4Film layer is placed in Muffle furnace and is sintered, warp
40min is raised to 325 DEG C, heat preservation 5min, is raised to 375 DEG C, heat preservation 10min through 10min, 450 DEG C, heat preservation are raised to through 15min
15min is raised to 500 DEG C, heat preservation 10min through 15min, i.e., is prepared in situ to obtain nanometic zinc oxide rod array film in substrate.
As shown in Figure 1, film made from the embodiment of the present invention is uniformly dispersed, a diameter of 100~150nm of ZnO nanorod, length
Degree is 400~500nm.As shown in Fig. 2, what is obtained on electron diffraction diagram is the ZnO nano-rod array grown in substrate.Such as figure
Shown in 3, the ZnO nanorod crystallization that x-ray diffraction pattern illustrates is preferable.
Claims (7)
1. a kind of method that ZnO nano-rod array film is prepared in situ, it is characterised in that include the following steps：
(1) preparation of organic ammonium salt
Organic monoamine RNH2Or organic diamine NH2RNH2Ethanol solution, wherein R=CnH2n, n >=1 is heated back with hydrochloric acid
Organic mono-ammonium RNH is made after vacuum distillation, filtering, recrystallization, drying in stream reaction3Cl or organic di-ammonium salts
NH3ClRNH3Cl；
(2) preparation of two-dimensional layer chlorination zinc-base hydridization perovskite
According to molal weight than organic mono-ammonium RNH3Cl: zinc chloride=2: 1 or described organic di-ammonium salts NH3ClRNH3Cl
: zinc chloride=1: 1, by organic mono-ammonium RNH3The ethanol solution of Cl or organic di-ammonium salts NH3ClRNH3The second of Cl
Alcoholic solution is mixed with the ethanol solution of zinc chloride, carries out heating reflux reaction, after vacuum distillation, filtering, recrystallization, drying,
Two-dimensional layer chlorination zinc-base hydridization perovskite (RNH is made3)2ZnCl4Or NH3RNH3ZnCl4；
(3) the perovskite spin coating of chlorination zinc-base hydridization is film-made
By the hydridization perovskite (RNH3)2ZnCl4Or NH3RNH3ZnCl4After being dissolved in solvent, using sol evenning machine in the base cleaned
Chlorination zinc-base hydridization perovskite film layer is prepared by spin coating on bottom；
(4) sintering of chlorination zinc-base hydridization perovskite
The chlorination zinc-base hydridization perovskite film layer is sintered, i.e., is prepared in situ to obtain zinc oxide nano rod battle array in substrate
Row film.
2. the method according to claim 1 that ZnO nano-rod array film is prepared in situ, it is characterised in that：The step
(1), heating reflux reaction temperature is 70~80 DEG C in step (2), and the reaction time is 0.5~2h.
3. the method according to claim 1 that ZnO nano-rod array film is prepared in situ, it is characterised in that：The step
(3) by hydridization perovskite (RNH described in 20~100mg in3)2ZnCl4Or NH3RNH3ZnCl4It is dissolved in 1mL solvents.
4. the method according to claim 2 or 3 that ZnO nano-rod array film is prepared in situ, it is characterised in that：The step
Suddenly solvent is absolute ethyl alcohol, propyl alcohol, isobutanol, DMF or DMSO in (3).
5. the method according to claim 1 that ZnO nano-rod array film is prepared in situ, it is characterised in that：The step
(3) speed of spin coating is 2000~5000rpm in.
6. the method according to claim 1 that ZnO nano-rod array film is prepared in situ, it is characterised in that：The substrate
For ITO electro-conductive glass, FTO electro-conductive glass, AZO electro-conductive glass, flexible and transparent conductive substrate, quartz glass or silicon-based substrate.
7. the method according to claim 1 that ZnO nano-rod array film is prepared in situ, it is characterised in that：The step
(4) 0.5~2h is sintered at a temperature of 300~500 DEG C in oxygen atmosphere.
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