CN105088344B - It is a kind of that the method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet - Google Patents
It is a kind of that the method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet Download PDFInfo
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Abstract
The method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet the invention discloses a kind of, sample is made in zinc metal sheet, is polished with sand paper, is rinsed with water, then is respectively cleaned by ultrasonic with absolute ethyl alcohol, deionized water.N-butylamine and lanthanum nitrate aqueous solution are added in autoclave liner, stirring mixing, while the sample after processing is stood in autoclave liner；It is placed in air dry oven and heats, then takes out autoclave, cooling, taking-up sample are cleaned three times with absolute ethyl alcohol, deionized water, be dried in vacuo to obtain La doped ZnO respectively；Plumbi nitras and sodium sulfide solution is respectively configured, La doped ZnO are sequentially placed into lead nitrate solution, deionized water, sodium sulfide solution, deionized water and soaked respectively, repeated deposition 3 12 times.After deposition terminates, sample is taken out, respectively with deionized water, washes of absolute alcohol three times, vacuum drying is produced.The present invention ensures to form the PbS quantum layer of uniform fold on ZnO surfaces, while being combined well between the nano-wire array of gained and zinc metal sheet.
Description
Technical field
It is specifically a kind of that the side that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet the present invention relates to field of nanometer technology
Method.
Background technology
CdS, CdSe, PbS, the quantum dot such as Ag2S can be by continuous ionic layer sedimentation growth in situ in broad-band gap ZnO
Semiconductor surface, constructs quantum dot sensitized ZnO compound structure films, and this film has in fields such as solar cell, photocatalysis
Have wide practical use.Continuous ionic layer sedimentation is the cation and anion precursor solution quantum dot to be deposited
It is individually positioned in two containers, deposited ZnO film is first soaked in the precursor solution containing cation and then rushed
Wash clean, it next be immersed in the precursor solution containing anion and then rinsed well.Two step immersion processes are referred to as
One continuous ionic layer deposition cycle.In a cycle, each deposition process can be controlled to control the growth of quantum dot.Again
The size of quantum dot is controlled by controlling deposition cycle.Deposited using continuous ionic layer, because quantum dot has shorter life
Growth process and near-stoichiometric synthesis, and uniform, level of coverage is high respectively, it is considered to be preferable quantum dot deposition process.
Quantum dot is deposited on using continuous ionic layer sedimentation SnO2 electro-conductive glass (FTO), ITO and the titanium-based bottom growth of fluorine doped
Construct the existing considerable report of quantum dot sensitized ZnO laminated films on ZnO nano-structure, such as Liao Xin (《Inorganic material
Report》, volume 27 the 1st phase, 59-63 pages in 2012) and ZnO nano piece is grown on FTO first with electrochemical process, then in ZnO
Pass through continuous ionic layer deposition method PbS quantum formation PbS/ZnO composite membranes in nanometer sheet；The U.S.《Applied Surface Chemistry》
(AppliedSurfaceScience, volume 257 the 16th phase, 7041-7046 pages in 2011), which are reported, utilizes continuous ionic layer
Sedimentation obtains the ZnO nanorod that CdS and PbS are sensitized altogether.If but consider conventional quantum dot sensitizer such as CdS, CdSe,
PbS, Ag2S etc. are deposited on the ZnO nanorod grown on zinc-base bottom, then because the metal belonging to these quantum dot cations is active
Property is weaker than Zn, and when zinc-base ZnO film soaks in the precursor solution containing cation, exposed Zn can occur with cation
Displacement reaction, so that ZnO film is destroyed, causes deposition to fail.
The content of the invention
It is an object of the invention to provide a kind of PbS uniform folds in the nano-wire array and Zn obtained by ZnO surfaces, guarantee
What is combined well between piece prepares the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, to solve in above-mentioned background technology
The problem of proposition.
To achieve the above object, the present invention provides following technical scheme：
It is a kind of that the method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet, comprise the following steps that：
1) sample is made in zinc metal sheet, is polished with sand paper, rinsed with water, then be respectively cleaned by ultrasonic with absolute ethyl alcohol, deionized water
10min；
2) it is that 0.005 ± 0.001mol/L lanthanum nitrate aqueous solutions add autoclave by 10mL n-butylamines and 40mL concentration
In liner, stirring mixing, while the sample after above-mentioned processing is stood in autoclave liner by wall；
3) closed autoclave is placed in air dry oven and is heated to 140 ± 5 DEG C, and be incubated 13 ± 1 hours；
4) after reaction terminates, autoclave is taken out, after room temperature, examination is taken out from autoclave
Sample, is cleaned three times with absolute ethyl alcohol, deionized water respectively, and sample is dried in vacuo 4 hours at 50 DEG C, obtains La doped ZnO productions
Product, are designated as La-doped ZnO；
5) be respectively configured 0.05-0.1mol/L plumbi nitras and sodium sulfide solution, plumbi nitras and sodium sulfide solution it is dense
Degree is identical, and obtained La-doped ZnO are sequentially placed into lead nitrate solution, deionized water, sodium sulfide solution, deionized water
Soak 60 ± 10 seconds, 20 ± 5 seconds, 30 ± 5 seconds, 40 ± 10 seconds respectively, in this, as primary depositing, repeated deposition 3-12 times；
6) after deposition terminates, sample is taken out, respectively with deionized water, washes of absolute alcohol three times, by sample at 50 DEG C
Vacuum drying is produced for 4 hours.
It is used as further scheme of the invention：Step 1) in sample size be 2cm × 2cm sizes.
It is used as further scheme of the invention：The concentration of lanthanum nitrate aqueous solution is 0.005mol/L.
It is used as further scheme of the invention：Step 3) in the heating-up temperature of air dry oven be 140 DEG C, insulation is 14 small
When.
It is used as further scheme of the invention：Step 5) in the concentration of plumbi nitras and sodium sulfide solution be 0.1mol/
L。
It is used as further scheme of the invention：Step 5) in that obtained La-doped ZnO are sequentially placed into plumbi nitras is molten
Soaked respectively in liquid, deionized water, sodium sulfide solution, deionized water 60 seconds, 20 seconds, 30 seconds, 40 seconds.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention uses simple hydro-thermal reaction method, by toward add in hydrothermal system a small amount of lanthanum nitrate aqueous solution come
ZnO nucleation and growth are controlled, ZnO grows the ZnO nanorod display of densification in the primary a large amount of forming cores of reaction, so that plumbi nitras
Solution can not be penetrated into Zn pieces by fine and close ZnO layer and occur displacement reaction with zinc, and this is the pass for ensureing PbS successful depositions
Key.When ZnO nanorod soaks in lead nitrate solution, lead nitrate solution displays to be formed logical by diffusing into ZnO nanorod
Road, uniform adsorption removes the excessive lead nitrate solution in surface on the surface of ZnO nanorod by deionized water, makes next logical
Cross the vulcanized sodium diffused into passage to react therewith, so that the final PbS quantum for forming uniform fold on ZnO surfaces
Layer.In addition, in the inventive method, because the zinc metal sheet of grinding process is both as the growth substrate of ZnO nano-rod array, offerization again
Learn reaction in ZnO nano-rod array grow zinc source, therefore can ensure gained nano-wire array and Zn pieces between well
With reference to.
Brief description of the drawings
Fig. 1 is that the La doped ZnO nanorod (La-doped ZnO) prepared for 14 hours in 140 DEG C, hydro-thermal reaction is old
The stereoscan photograph of 100000 times of row amplification.
Fig. 2 is the full analysis of spectrum figures of XPS of the La doped ZnO nanorod prepared for 14 hours in 140 DEG C, hydro-thermal reaction.
Fig. 3 is that the narrow of lanthanum element sweeps XPS spectrum figure.
Fig. 4 is PbS quantum sensitization ZnO nanorod (3PbS/La-doped ZnO) amplification obtained through 3 repeated depositions
100000 times of stereoscan photograph.
Fig. 5 is the PbS quantum sensitization ZnO nanorod 10PbS/La-doped ZnO amplifications obtained through 10 repeated depositions
100000 times of stereoscan photograph.
Fig. 6 is the EDS spectrograms of 10PbS/La-doped ZnO products.
Fig. 7 is not deposit PbS ZnO nanorod (La-doped ZnO), the PbS quantum through 3 repeated depositions to be sensitized
ZnO nanorod (3PbS/La-doped ZnO), the PbS quantum through 10 repeated depositions are sensitized ZnO nanorod (10PbS/La-
Doped ZnO) fluorescence emission spectrogram of compound.
Fig. 8 is the XRD spectra that the PbS quantum obtained through 10 cyclic depositions is sensitized ZnO nanorod.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of that the method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet, specific steps are such as
Under：
1) sample that size is 2cm × 2cm sizes is made in zinc metal sheet, is polished, rinsed with water with sand paper, then use anhydrous second
Alcohol, deionized water are respectively cleaned by ultrasonic 10min.
2) it is that 0.006mol/L lanthanum nitrate aqueous solutions are added in autoclave liner by 10mL n-butylamines and 40mL concentration,
Stirring mixing, while the zinc metal sheet after above-mentioned processing is stood in autoclave liner by wall；
3) closed autoclave is placed in air dry oven and is heated to 135 DEG C, and be incubated 12 hours；
4) after reaction terminates, reactor is taken out, after room temperature, sample is taken out from reactor, is used respectively
Absolute ethyl alcohol, deionized water are cleaned three times, remove the reactant and solvent of its surface, sample is dried in vacuo into 4 at 50 DEG C
Hour, La doped ZnO products are obtained, La-doped ZnO are designated as；
5) 0.05mol/L plumbi nitras and sodium sulfide solution is respectively configured, obtained La-doped ZnO are sequentially placed into
Soak 50 seconds in lead nitrate solution, deionized water, sodium sulfide solution, deionized water respectively, 15 seconds, 25 seconds, 30 seconds, in this, as
Primary depositing, such 3 products obtained therefroms of repeated deposition are designated as 3PbS/La-doped ZnO, 10 products obtained therefrom notes of repeated deposition
For 10PbS/La-doped ZnO.
6) after deposition terminates, sample is taken out, respectively with deionized water, washes of absolute alcohol three times, its surface is removed residual
The ion stayed, sample is dried in vacuo 4 hours at 50 DEG C.
Embodiment 2
In the embodiment of the present invention, a kind of that the method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet, specific steps are such as
Under：
1) sample that size is 2cm × 2cm sizes is made in zinc metal sheet, is polished, rinsed with water with sand paper, then use anhydrous second
Alcohol, deionized water are respectively cleaned by ultrasonic 10min；
2) it is that 0.005mol/L lanthanum nitrate aqueous solutions are added in autoclave liner by 10mL n-butylamines and 40mL concentration,
Stirring mixing, while the zinc metal sheet after above-mentioned processing is stood in autoclave liner by wall；
3) closed autoclave is placed in air dry oven and is heated to 140 DEG C, and be incubated 14 hours；
4) after reaction terminates, reactor is taken out, after room temperature, sample is taken out from reactor, is used respectively
Absolute ethyl alcohol, deionized water are cleaned three times, remove the reactant and solvent of its surface, sample is dried in vacuo into 4 at 50 DEG C
Hour, La doped ZnO products are obtained, La-doped ZnO are designated as；
5) 0.1mol/L plumbi nitras and sodium sulfide solution is respectively configured, obtained La-doped ZnO are sequentially placed into nitre
Soaked respectively in lead plumbate solution, deionized water, sodium sulfide solution, deionized water 60 seconds, 20 seconds, 30 seconds, 40 seconds, in this, as one
Secondary deposition, such 3 products obtained therefroms of repeated deposition are designated as 3PbS/La-doped ZnO, and 10 products obtained therefroms of repeated deposition are designated as
10PbS/La-doped ZnO。
6) after deposition terminates, sample is taken out, respectively with deionized water, washes of absolute alcohol three times, its surface is removed residual
Sample, is finally dried in vacuo 4 hours by the ion stayed at 50 DEG C.
Embodiment 3
In the embodiment of the present invention, a kind of that the method that PbS is sensitized ZnO nano-rod array is prepared on zinc metal sheet, specific steps are such as
Under：
1) sample that size is 2cm × 2cm sizes is made in zinc metal sheet, is polished, rinsed with water with sand paper, then use anhydrous second
Alcohol, deionized water are respectively cleaned by ultrasonic 10min.
2) it is that 0.004mol/L lanthanum nitrate aqueous solutions are added in autoclave liner by 10mL n-butylamines and 40mL concentration,
Stirring mixing, while the zinc metal sheet after above-mentioned processing is stood in autoclave liner by wall；
3) closed autoclave is placed in air dry oven and is heated to 145 DEG C, and be incubated 13 hours；
4) after reaction terminates, reactor is taken out, after room temperature, sample is taken out from reactor, is used respectively
Absolute ethyl alcohol, deionized water are cleaned three times, remove the reactant and solvent of its surface, sample is dried in vacuo into 4 at 50 DEG C
Hour, La doped ZnO products are obtained, La-doped ZnO are designated as.
5) 0.07mol/L plumbi nitras and sodium sulfide solution is respectively configured, obtained La-doped ZnO are sequentially placed into
Soak 70 seconds in lead nitrate solution, deionized water, sodium sulfide solution, deionized water respectively, 25 seconds, 35 seconds, 50 seconds, in this, as
Primary depositing, such 3 products obtained therefroms of repeated deposition are designated as 3PbS/La-doped ZnO, 10 products obtained therefrom notes of repeated deposition
For 10PbS/La-doped ZnO.
6) after deposition terminates, sample is taken out, respectively with deionized water, washes of absolute alcohol three times, its surface is removed residual
The ion stayed, sample is dried in vacuo 4 hours at 50 DEG C.
The present invention detects to the result of embodiment 2, as a result as Figure 1-Figure 8.It is described in detail below.
As seen from Figure 1, one layer of fine and close hexagonal prism ZnO nanorod is grown on Zn substrates.
Fig. 2-Fig. 3 be XPS compose full display sample in include tri- kinds of elements of Zn, O, La, the narrow spectrogram of sweeping of lanthanum element illustrates La
With+trivalent form presence.XPS analysis show that La is entered in ZnO lattices with the doping of+trivalent form.
Fig. 4 shows after 3 repeated depositions, one layer of PbS particle of uniform deposition on ZnO nanorod.
Fig. 5 shows that after 10 repeated depositions the PbS particle sizes deposited on ZnO nanorod substantially become big, nanometer rods top
More large scale PbS particles are accumulated in end.
Fig. 6 gives the energy spectrum diagram of the PbS quantum sensitization ZnO nano-rod array of 10 preparations of repeated deposition, can from Fig. 6
To find out, there was only two kinds of materials of ZnO, PbS in reaction product, without other impurities, the result of quantitative analysis shows Zn:O≈1:
1, Pb:S≈1:1, show that ZnO and PbS in preparation-obtained PbS quantum sensitization ZnO nano-rod array meet chemistry
Metering ratio, and it is not introduced into other impurity.
Fig. 7 gives the ZnO nanorod for not depositing PbS, the PbS quantum sensitization ZnO nano of repeated deposition 3 times and 10 times
The fluorescence emission spectrum of rod, excitation wavelength is 325nm.As seen from the figure, the ZnO for PbS not being deposited has the last one at 383nm
Ultra-violet light-emitting peak, this is the intrinsic luminous of ZnO, is produced by free exciton is compound.After deposition has PbS on ZnO nanorod,
The intrinsic luminous effective fluorescence that ZnO has been quenched of deposition for substantially weakening, illustrating PbS of ZnO, PbS repeated deposition number of times is more, deposition
PbS quantum on ZnO nanorod is more, and the effect that ZnO fluorescence is quenched is more obvious.
The PbS sensitization ZnO nanorods that Fig. 8 gives repeated deposition 10 times display the X-ray diffraction pattern of laminated film, can
To find out, in all diffraction maximums, PbS and ZnO diffraction maximum contains only.It was found that, both obtain the diffraction pattern of PbS in sample
Spectrum is consistent with JCPDS cards (JCPD card number NO.05-0592, tetragonal crystal system, space group Fm-3m, a=5.9362).ZnO's spreads out
Penetrate collection of illustrative plates and hexagonal wurtzite ZnO structure JCPDS cards (JCPD card number NO.36-1451, hexagonal crystal system, space group p63mc, a
=3.250A, c=5.206A) it is consistent.
Two-step method proposed by the present invention prepares PbS sensitization ZnO nano-rod arrays on zinc metal sheet, including elder generation is in n-butylamine and nitre
In the mixed solution of sour lanthanum, one layer of fine and close ZnO nanorod is grown on zinc metal sheet using hydro-thermal method；Then continuous ionic is utilized
Layer, which is deposited on ZnO nanorod, deposits PbS quantum.The control of hydrothermal condition on zinc metal sheet to preparing densification in the present invention
ZnO nanorod display is most important, and fine and close ZnO nanorod display layer is the key of follow-up PbS quantum successful deposition.This
Hydrothermal condition refers in invention：Mixed solution used be by 10mL n-butylamines and 40mL concentration be 0.005 ± 0.001mol/
L lanthanum nitrate aqueous solutions are mixed to get, 140 ± 5 DEG C of hydrothermal temperature, 13 ± 1h of hydro-thermal time.PbS for continuous ionic layer deposition
The precursor solution of quantum dot is plumbi nitras and sodium sulfide solution, and two kinds of concentration are prepared the same, controlled in 0.05-0.1mol/
L.Zinc-base ZnO nanorod sample by lead nitrate solution, deionized water, sodium sulfide solution, deionized water order respectively immersion 60 ±
10 seconds, 20 ± 5 seconds, 30 ± 5 seconds, 40 ± 10 seconds as an atomic layer deposition cycle, by above-mentioned immersion order carry out it is multiple from
Sublayer deposition cycle controls PbS quantum size.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It may be appreciated other embodiment.
Claims (6)
1. a kind of prepare the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, it is characterised in that comprises the following steps that：
1) sample is made in zinc metal sheet, is polished with sand paper, rinsed with water, then be respectively cleaned by ultrasonic with absolute ethyl alcohol, deionized water
10min；
2) it is that 0.005 ± 0.001mol/L lanthanum nitrate aqueous solutions add autoclave liner by 10mL n-butylamines and 40mL concentration
In, stirring mixing, while the sample after above-mentioned processing is stood in autoclave liner by wall；
3) closed autoclave is placed in air dry oven and is heated to 140 ± 5 DEG C, and be incubated 13 ± 1 hours；
4) after reaction terminates, autoclave is taken out, after room temperature, sample is taken out from autoclave, point
Do not cleaned three times with absolute ethyl alcohol, deionized water, sample is dried in vacuo 4 hours at 50 DEG C, obtain La doped ZnO products, remembered
For La-doped ZnO；
5) the concentration phase of 0.05-0.1mol/L plumbi nitras and sodium sulfide solution, plumbi nitras and sodium sulfide solution is respectively configured
Together, obtained La-doped ZnO are sequentially placed into lead nitrate solution, deionized water, sodium sulfide solution, deionized water respectively
Immersion 60 ± 10 seconds, 20 ± 5 seconds, 30 ± 5 seconds, 40 ± 10 seconds, in this, as primary depositing, repeated deposition 3-12 times；
6) after deposition terminates, take out sample, respectively with deionized water, washes of absolute alcohol three times, by sample at 50 DEG C vacuum
Drying is produced for 4 hours.
2. according to claim 1 prepare the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, it is characterised in that step
It is rapid 1) in sample size be 2cm × 2cm sizes.
3. according to claim 1 prepare the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, it is characterised in that nitre
The concentration of the sour lanthanum aqueous solution is 0.005mol/L.
4. according to claim 1 prepare the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, it is characterised in that step
It is rapid 3) in air dry oven heating-up temperature be 140 DEG C, be incubated 14 hours.
5. according to claim 1 prepare the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, it is characterised in that step
It is rapid 5) in the concentration of plumbi nitras and sodium sulfide solution be 0.1mol/L.
6. according to claim 1 prepare the method that PbS is sensitized ZnO nano-rod array on zinc metal sheet, it is characterised in that step
It is rapid 5) in obtained La-doped ZnO are sequentially placed into lead nitrate solution, deionized water, sodium sulfide solution, deionized water point
Jin Pao not be 60 seconds, 20 seconds, 30 seconds, 40 seconds.
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| CN102024573A (en) * | 2010-12-18 | 2011-04-20 | 西南交通大学 | Method for preparing sensitized ZnO nano-plate photo-anode of PbS quantum dot |
| CN102417201A (en) * | 2011-08-31 | 2012-04-18 | 北京大学 | Method for preparing one-dimensional self-assembly material with ZnO nanorod array as template |
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| CN102024573A (en) * | 2010-12-18 | 2011-04-20 | 西南交通大学 | Method for preparing sensitized ZnO nano-plate photo-anode of PbS quantum dot |
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