CN106564944A - CdS sensitized titanium dioxide nanoflower cluster composite material, and preparation method and application thereof - Google Patents
CdS sensitized titanium dioxide nanoflower cluster composite material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a CdS sensitized titanium dioxide nanoflower cluster composite material, and a preparation method and an application thereof. The preparation method comprises: preparing titanium dioxide nanoribbons, and preparing the CdS sensitized titanium dioxide nanoflower cluster composite material. A solvothermal technology, an induced growth technology and a successive ionic layer adsorption and reaction (SILAR) technology are combined, so the prepared CdS sensitized titanium dioxide nanoflower cluster composite material has a multilevel structure, and can be widely applied to the photoelectric field.
Description
Technical field
The invention belongs to nano composite material preparing technical field, and in particular to a kind of CdS sensitized titanium dioxides nano flower
String composite and preparation and application.
Background technology
In order to meet demand continuous to clear energy sources, researchers are to probing into lot of materials in solar photoelectric and correlation
Solar energy collecting device put into great energy.The metal oxide of various patterns such as TiO2, ZnO and WO3Deng semiconductor
The excellent performance of metal oxide nano-material, is widely used in sensing, is catalyzed, the field such as photoelectricity.However, most of
All than larger, exactly this reason limits their absorptions for visible ray to the band gap of these metal oxides, so as to
Have impact on overall efficiency.Correlative study is it has been shown that adulterating and using transition metal, carbon or nitrogen etc. to reduce these nanostructureds
The band gap of metal oxide.
Wherein, the quantum dot such as cadmium sulfide of individual layer is deposited（CdS）, cadmium selenide（CdSe）, cadmium antimonide（CdTe）Deng even two
Plant quantum dot to be sensitized jointly, the absorption of ultraviolet-visible can be strengthened, therefore, it can be filled by being sensitized the recombination energy of the mode such as modified
The excellent properties of bi-material are waved in distribution, and show the property more more superior than homogenous material in some aspects.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of CdS sensitized titanium dioxides nano flower string is answered
Condensation material and preparation method.
Another object of the present invention is the CdS sensitized titanium dioxides nano flower string composite answering in photoelectric field
With.
By solvent-thermal method, induced growth method and continuous ionic layer adsorption reaction（SILAR）Method combines, and obtains with multistage
The CdS sensitized titanium dioxide nano flower string composites of structure.Comprise the following steps that：
A kind of preparation method of CdS sensitized titanium dioxides nano flower string composite, it is characterised in that the concrete steps of the method
For：
（1）The preparation of titanium dioxide nano-belts：Anatase titanium dioxide is added in NaOH solution, both add mole
Than for TiO2: NaOH=1:200~600；The min of magnetic agitation 30 to solution is clarified, and has been then transferred into polytetrafluoroethyllining lining
Hydrothermal reaction kettle in, sealing, carry out hydro-thermal reaction in an oven 24 ~ 48 hours at 200 DEG C；After reaction terminates, centrifugation will
Sediment is cleaned repeatedly with the watery hydrochloric acid of 0.1 mol/L, and is stood after 24 h, and deionized water and absolute ethanol washing are multiple,
And at 60 ~ 80 DEG C be dried, be subsequently placed in Muffle furnace at 500 DEG C and calcine 2 h, with agate mortar it is finely ground after obtain titanium dioxide
Titanium nanobelt powder.
（2）The preparation of titanium oxide nanoflower string：By AgNO3Mix with acetic acid, the mol ratio that both add is AgNO3:
CH3COOH=1:200 ~ 500, solution A is obtained until completely dissolved；Butyl titanate TBOT is added drop-wise in solution A, and is added
Titanium dioxide nano-belts, wherein, with the AgNO for adding3Measure to measure, the mol ratio of addition is AgNO3: TBOT:TiO2=1:1:
0.2, continue to stir after 10 min, in being transferred to hydrothermal reaction kettle, and hydro-thermal reaction is carried out at 160 DEG C, after question response terminates
Take out, be then centrifuged for, clean, being dried, and the h of roasting 3 at 450 DEG C, obtain titanium oxide nanoflower string sample；
（3）The preparation of CdS sensitized titanium dioxide nano flower string composites：Be respectively configured 0.1 M chromic nitrates ethanol solution and
The methanol solution of 0.1 M vulcanized sodium, and titanium oxide nanoflower string sample is placed on the filter paper in Suction filtration device, by vulcanized sodium
Methanol solution be added drop-wise in titanium oxide nanoflower string sample so as to fully infiltration, suction filtration, then methanol solution cleaning is added dropwise,
Then the ethanol of cadmium nitrate is added drop-wise in titanium oxide nanoflower string sample again so as to fully infiltration, suction filtration, then ethanol is added dropwise
Solution is cleaned, and this is a circulation, and repetitive cycling is multiple, mol ratio CdS:TiO2=1:10 ~ 30, drying to obtain CdS are sensitized
Titanium oxide nanoflower string composite.
A kind of CdS sensitized titanium dioxides nano flower string composite, it is characterised in that prepared according to methods described.
A kind of application of CdS sensitized titanium dioxides nano flower string composite in photoelectric field.
The present invention is by solvent-thermal method, induced growth method and continuous ionic layer adsorption reaction（SILAR）Method combines, prepared
CdS sensitized titanium dioxide nano flower string composites there is multilevel hierarchy, the composite can be widely applied to photoelectric field.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the CdS sensitized titanium dioxide nano flower string composites of the synthesis of the embodiment of the present invention 1.
Fig. 2 be the embodiment of the present invention it is 2-in-1 into CdS sensitized titanium dioxide nano flower string composites scanning electron microscope (SEM) photograph.
Specific embodiment
The present invention is described in detail by following instantiation, but protection scope of the present invention is not only restricted to these realities
Apply example.
Embodiment 1：
（1）The preparation of titanium dioxide nano-belts：0.2 g anatase titanium dioxides are added to into the mol/L's of 150 ml 10
In NaOH solution, the mol ratio that both add is TiO2:NaOH=1:600；The min of magnetic agitation 30 to solution is clarified, Ran Houzhuan
In having moved on to teflon-lined hydrothermal reaction kettle, sealing carries out in an oven hydro-thermal reaction 24 hours at 200 DEG C；
After reaction terminates, centrifugation is repeatedly cleaned sediment, and stand after 24 h with the watery hydrochloric acid of 0.1 mol/L, deionized water with
Absolute ethanol washing repeatedly, and is dried at 60 DEG C, is subsequently placed in Muffle furnace at 500 DEG C and calcines 2 h, finely ground with agate mortar
Titanium dioxide nano-belts powder is obtained afterwards.
（2）The preparation of titanium oxide nanoflower string：Weigh 0.6 gAgNO3In being added to 55 ml acetic acid, what both added
Mol ratio is AgNO3: CH3COOH=1:274, solution A is obtained until completely dissolved；1.2 ml butyl titanates TBOT are added dropwise
To in solution A, and 0.06 g titanium dioxide nano-belts are added, wherein, with the AgNO for adding3Measure as metering, the mol ratio of addition
For AgNO3: TBOT:TiO2=1:1:0.2, continue to stir after 10 min, in being transferred to hydrothermal reaction kettle, and carry out at 160 DEG C
Hydro-thermal reaction.Question response takes out after terminating, and is then centrifuged for, cleans, being dried, and the h of roasting 3 at 450 DEG C, obtains titanium dioxide
Nano flower string sample.
（3）The preparation of CdS sensitized titanium dioxide nano flower string composites：It is respectively configured the M chromic nitrates of 10 ml 0.1
The methanol solution of ethanol solution and the M vulcanized sodium of 10 ml 0.1, and 1.76 g titanium oxide nanoflower string samples are placed on into suction filtration
On filter paper in device, the methanol solution of vulcanized sodium is added drop-wise in titanium oxide nanoflower string sample so as to fully infiltration, is taken out
Filter, then methanol solution cleaning is added dropwise, then the ethanol of cadmium nitrate is added drop-wise in titanium oxide nanoflower string sample again so as to fill
Sub-dip is moistened, suction filtration, then ethanol solution cleaning is added dropwise, and this is a circulation, and repetitive cycling is multiple, mol ratio CdS:TiO2 =1:
22, drying to obtain CdS sensitized titanium dioxide nano flower string composites.Fig. 1 is the stereoscan photograph of the composite.
Embodiment 2：
（1）The preparation of titanium dioxide nano-belts：0.15 g anatase titanium dioxides are added to into the mol/L's of 68 ml 10
In NaOH solution, the mol ratio that both add is TiO2: NaOH=1:360；The min of magnetic agitation 30 to solution is clarified, Ran Houzhuan
In having moved on to teflon-lined hydrothermal reaction kettle, sealing carries out in an oven hydro-thermal reaction 48 hours at 200 DEG C；
After reaction terminates, centrifugation is repeatedly cleaned sediment, and stand after 24 h with the watery hydrochloric acid of 0.1 mol/L, deionized water with
Absolute ethanol washing repeatedly, and is dried at 80 DEG C, is subsequently placed in Muffle furnace at 500 DEG C and calcines 2 h, finely ground with agate mortar
Titanium dioxide nano-belts powder is obtained afterwards.
（2）The preparation of titanium oxide nanoflower string：Weigh 0.3 gAgNO3In being added to 57 ml acetic acid, what both added
Mol ratio is AgNO3: CH3COOH=1:500, solution A is obtained until completely dissolved；By 0.68 ml butyl titanate TBOT drops
In being added to solution A, and 0.03 g titanium dioxide nano-belts are added, wherein, with the AgNO for adding3Measure for metering, addition mole
Than for AgNO3: TBOT:TiO2=1:1:0.2, continue to stir after 10 min, in being transferred to hydrothermal reaction kettle, and enter at 160 DEG C
Water-filling thermal response.Question response takes out after terminating, and is then centrifuged for, cleans, being dried, and the h of roasting 3 at 450 DEG C, obtains titanium dioxide
Titanium nano flower string sample.
（3）The preparation of CdS sensitized titanium dioxide nano flower string composites：It is respectively configured the M chromic nitrates of 10 ml 0.1
The methanol solution of ethanol solution and the M vulcanized sodium of 10 ml 0.1, and 2.4 g titanium oxide nanoflower string samples are placed on into suction filtration dress
On the filter paper put, the methanol solution of vulcanized sodium is added drop-wise in titanium oxide nanoflower string sample so as to fully infiltration, is taken out
Filter, then methanol solution cleaning is added dropwise, then the ethanol of cadmium nitrate is added drop-wise in titanium oxide nanoflower string sample again so as to fill
Sub-dip is moistened, suction filtration, then ethanol solution cleaning is added dropwise, and this is a circulation, and repetitive cycling is multiple, mol ratio CdS:TiO2 =1:
30, drying to obtain CdS sensitized titanium dioxide nano flower string composites.Fig. 2 is the stereoscan photograph of the composite.
Embodiment 3：
（1）The preparation of titanium dioxide nano-belts：0.12 g anatase titanium dioxides are added to into the mol/L's of 30 ml 10
In NaOH solution, the mol ratio that both add is TiO2: NaOH=1:200；The min of magnetic agitation 30 to solution is clarified, Ran Houzhuan
In having moved on to teflon-lined hydrothermal reaction kettle, sealing carries out in an oven hydro-thermal reaction 36 hours at 200 DEG C；
After reaction terminates, centrifugation is repeatedly cleaned sediment, and stand after 24 h with the watery hydrochloric acid of 0.1 mol/L, deionized water with
Absolute ethanol washing repeatedly, and is dried at 75 DEG C, is subsequently placed in Muffle furnace at 500 DEG C and calcines 2 h, finely ground with agate mortar
Titanium dioxide nano-belts powder is obtained afterwards.
（2）The preparation of titanium oxide nanoflower string：Weigh 0.45 gAgNO3In being added to 30 ml acetic acid, what both added
Mol ratio is AgNO3: CH3COOH=1:200, solution A is obtained until completely dissolved；By 0.89 ml butyl titanate TBOT drops
In being added to solution A, and 0.04 g titanium dioxide nano-belts are added, wherein, with the AgNO for adding3Measure for metering, addition mole
Than for AgNO3: TBOT:TiO2=1:1:0.2, continue to stir after 10 min, in being transferred to hydrothermal reaction kettle, and enter at 160 DEG C
Water-filling thermal response.Question response takes out after terminating, and is then centrifuged for, cleans, being dried, and the h of roasting 3 at 450 DEG C, obtains titanium dioxide
Titanium nano flower string sample.
（3）The preparation of CdS sensitized titanium dioxide nano flower string composites：It is respectively configured the M chromic nitrates of 10 ml 0.1
The methanol solution of ethanol solution and the M vulcanized sodium of 10 ml 0.1, and 0.8 g titanium oxide nanoflower string samples are placed on into suction filtration dress
On the filter paper put, the methanol solution of vulcanized sodium is added drop-wise in titanium oxide nanoflower string sample so as to fully infiltration, is taken out
Filter, then methanol solution cleaning is added dropwise, then the ethanol of cadmium nitrate is added drop-wise in titanium oxide nanoflower string sample again so as to fill
Sub-dip is moistened, suction filtration, then ethanol solution cleaning is added dropwise, and this is a circulation, and repetitive cycling is multiple, mol ratio CdS:TiO2 =1:
10, drying to obtain CdS sensitized titanium dioxide nano flower string composites.
Claims (3)
1. a kind of preparation method of CdS sensitized titanium dioxides nano flower string composite, it is characterised in that the concrete step of the method
Suddenly it is：
（1）The preparation of titanium dioxide nano-belts：Anatase titanium dioxide is added in NaOH solution, both add mole
Than for TiO2: NaOH=1:200~600；The min of magnetic agitation 30 to solution is clarified, and has been then transferred into polytetrafluoroethyllining lining
Hydrothermal reaction kettle in, sealing, carry out hydro-thermal reaction in an oven 24 ~ 48 hours at 200 DEG C；After reaction terminates, centrifugation will
Sediment is cleaned repeatedly with the watery hydrochloric acid of 0.1 mol/L, and is stood after 24 h, and deionized water and absolute ethanol washing are multiple,
And at 60 ~ 80 DEG C be dried, be subsequently placed in Muffle furnace at 500 DEG C and calcine 2 h, with agate mortar it is finely ground after obtain titanium dioxide
Titanium nanobelt powder；
（2）The preparation of titanium oxide nanoflower string：By AgNO3Mix with acetic acid, the mol ratio that both add is AgNO3:
CH3COOH=1:200 ~ 500, solution A is obtained until completely dissolved；Butyl titanate TBOT is added drop-wise in solution A, and is added
Titanium dioxide nano-belts, wherein, with the AgNO for adding3Measure to measure, the mol ratio of addition is AgNO3: TBOT:TiO2=1:1:
0.2, continue to stir after 10 min, in being transferred to hydrothermal reaction kettle, and hydro-thermal reaction is carried out at 160 DEG C, after question response terminates
Take out, be then centrifuged for, clean, being dried, and the h of roasting 3 at 450 DEG C, obtain titanium oxide nanoflower string sample；
（3）The preparation of CdS sensitized titanium dioxide nano flower string composites：Be respectively configured 0.1 M chromic nitrates ethanol solution and
The methanol solution of 0.1 M vulcanized sodium, and titanium oxide nanoflower string sample is placed on the filter paper in Suction filtration device, by vulcanized sodium
Methanol solution be added drop-wise in titanium oxide nanoflower string sample so as to fully infiltration, suction filtration, then methanol solution cleaning is added dropwise,
Then the ethanol of cadmium nitrate is added drop-wise in titanium oxide nanoflower string sample again so as to fully infiltration, suction filtration, then ethanol is added dropwise
Solution is cleaned, and this is a circulation, and repetitive cycling is multiple, mol ratio CdS:TiO2=1:10 ~ 30, drying to obtain CdS are sensitized
Titanium oxide nanoflower string composite.
2. a kind of CdS sensitized titanium dioxides nano flower string composite, it is characterised in that method system according to claim 1
It is standby to obtain.
3. application of the CdS sensitized titanium dioxides nano flower string composite in photoelectric field according to claim 2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109395758A (en) * | 2018-11-12 | 2019-03-01 | 江苏大学 | A kind of dimensional thinlayer CdS/g-C3N4The Preparation method and use of composite photo-catalyst |
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