CN110052279A - A kind of TiO2The preparation method of (hollow)/CdTe/BiOBr composite material - Google Patents
A kind of TiO2The preparation method of (hollow)/CdTe/BiOBr composite material Download PDFInfo
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- CN110052279A CN110052279A CN201810042029.4A CN201810042029A CN110052279A CN 110052279 A CN110052279 A CN 110052279A CN 201810042029 A CN201810042029 A CN 201810042029A CN 110052279 A CN110052279 A CN 110052279A
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- tio
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- 229910004613 CdTe Inorganic materials 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 77
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 229910004273 TeO3 Inorganic materials 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PWKSKIMOESPYIA-BYPYZUCNSA-N L-N-acetyl-Cysteine Chemical compound CC(=O)N[C@@H](CS)C(O)=O PWKSKIMOESPYIA-BYPYZUCNSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of TiO2The preparation method of (hollow)/CdTe/BiOBr composite material, the preparation method include: that the present invention uses laminated assembling technology to finally obtain TiO2(hollow)/CdTe/BiOBr composite material.The BiOBr semiconductor selected in the present invention, can be with TiO due to its suitable forbidden bandwidth, unique structure2It is compounded to form heterojunction structure, to widen TiO2To the absorption region of visible light, inhibits the compound of photo-generated carrier, greatly improve TiO2Photocatalysis performance.And the absorption intensity to visible area under control not only can be enhanced in CdTe quantum, increases the separation rate of photo-generate electron-hole, it also has multiple exciton effect, so that photo-quantum efficiency greatly improves, further increases conventional semiconductors TiO2Photocatalysis performance.Method of the invention is easy to operate, and reaction condition is mild, provides a kind of optimization TiO2The method of photocatalysis performance.TiO2(hollow)/CdTe/BiOBr composite material has hollow structure, and specific surface area is larger, is conducive to the raising of photocatalysis performance.
Description
Technical field:
The present invention relates to a kind of preparation method of inorganic composite materials, in particular to a kind of TiO2(hollow)/CdTe/BiOBr is multiple
The preparation method of condensation material, more specifically, finally obtaining TiO using laminated assembling technology2(hollow)/CdTe/BiOBr is compound
Material.This technology belongs to the preparation field of nano material.
Background technique:
TiO was found by two professors of Fujishima A and Honda K from 19722Single Crystalline Electrodes can divide under illumination condition
Xie Shui and after generating hydrogen, photocatalysis technology and catalysis material enter the visual field of people and become research hotspot, band
Significant change is carried out.Wherein, catalysis material is the key that in photocatalysis technology.Invent a kind of photocatalysis performance it is high and
Prepare emphasis of the simple photochemical catalyst as enterprise and researcher, various new catalysts and technology of preparing application and
It is raw.
TiO2As a kind of traditional photochemical catalyst, air cleaning indoors, automatic cleaning coating and sterilizing
Etc. achieve substantive result.But since the catalyst loading needed for the fields such as sewage and Photocatalyzed Hydrogen Production of degradation is big,
Efficiency requirements are high, lead to TiO2Utilization of the photochemical catalyst in these fields is difficult to obtain biggish breakthrough.Therefore, pass through at this stage
Optimize TiO that obtain can satisfy functional need, high performance2Photochemical catalyst is the Main way of researchers.
In TiO2Study on the modification in, composite modified is currently used method, it can make TiO2Light abstraction width is from purple
Outskirt expands to visible region, additionally it is possible to photogenerated charge-hole utilization rate is improved, so that the photocatalytic of compound rear catalyst
It can greatly improve.In recent years, BiOBr is shown due to its special crystal structure and band structure to the wider suction of sunlight
Range and certain photocatalysis performance are received, it is widely studied.
TiO2The advantages of combination with CdTe, BiOBr very likely obtains these types of material simultaneously, to solve matrix TiO2
There are the problem of.Therefore, it is necessary to one kind can prepare TiO2The straightforward procedure of (hollow)/CdTe/BiOBr composite material.
Summary of the invention:
The object of the present invention is to provide a kind of TiO2The preparation method of (hollow)/CdTe/BiOBr composite material is to overcome existing skill
Semiconductors coupling may be implemented to improve the catalytic activity of catalyst in deficiency in art, the program.
A kind of TiO2The preparation method of (hollow)/CdTe/BiOBr composite material, includes following step:
Step 1: weighing 4.4 mL tetraisopropyl titanates (TTIP) and be dissolved in 200 mL dehydrated alcohols and 0.8 mL KNO3(0.1
Mol/L in mixed solution), precipitation handles 24 h, is cleaned and dried to obtain solid TiO2;Take 0.2 g TiO240 mL are successively added
H2O2(0.05 wt%) solution and 0.48 g NaOH, after 20 min of magnetic agitation, by mixed liquor be transferred in water heating kettle 180 DEG C it is anti-
Answer 4 h, eccentric cleaning;Sample obtained above is immersed in 20 mL HCl (0.1 mol/L) solution, is centrifuged, is washed to
Property, hollow titanium dioxide (TiO is calcined to obtain in drying2(hollow));
Step 2: taking above-mentioned 2 g TiO2It is dissolved in 40 mL deionized waters, ultrasound is uniformly;Weigh 0.0979 g N- acetyl-L- half
Cystine and 0.1145 g CdCl2·2.5H2Above-mentioned solution is successively added in O, and 30 min are respectively stirred at room temperature;Then it is added
0.178 g KBH4, then with the 10 mL Na of speed dropwise addition of 5 mL/min2TeO3(0.01 mol/L);By above-mentioned mixed system liter
Temperature is controlled the heating-up time in 30 min, is condensed back using Aqueous phase, samples after 6 h, make after washing and drying to 100 DEG C
TiO2(hollow)/CdTe powder;
Step 3: on the basis of the above, with BiNO3, KBr be raw material using solvent thermal process adjust (TiO2/ CdTe): BiOBr's
TiO is prepared in mol ratio2(hollow)/CdTe/BiOBr composite material.
The beneficial effects of the present invention are:
The BiOBr semiconductor selected in this patent, can be with TiO due to its suitable forbidden bandwidth, unique structure2Complex
At heterojunction structure, to widen TiO2To the absorption region of visible light, inhibits the compound of photo-generated carrier, greatly improve
TiO2Photocatalysis performance.And the absorption intensity to visible area under control not only can be enhanced in CdTe quantum, increases light induced electron-sky
The separation rate in cave, it also has multiple exciton effect, so that photo-quantum efficiency greatly improves, further increases conventional semiconductors
TiO2Photocatalysis performance.Method of the invention is easy to operate, and reaction condition is mild, provides a kind of optimization TiO2Photocatalytic
The method of energy.TiO2(hollow)/CdTe/BiOBr composite material has hollow structure, and specific surface area is larger, is conducive to photocatalysis
The raising of performance.
Detailed description of the invention:
Fig. 1, TiO2The SEM picture of (hollow)/CdTe/BiOBr composite material
Fig. 2, TiO2The EDS picture of (hollow)/CdTe/BiOBr composite material
Fig. 3, TiO2The TEM picture of (hollow)/CdTe/BiOBr composite material
Fig. 4, TiO2The HRTEM picture of (hollow)/CdTe/BiOBr composite material
Specific embodiment:
Embodiment 1
Step 1: preparing hollow titania powder.It weighs 4.4 mL tetraisopropyl titanates (TTIP) and is dissolved in the anhydrous second of 200 mL
Alcohol and 0.8 mL KNO3In the mixed solution of (0.1 mol/L), precipitation handles 24 h, is cleaned and dried to obtain solid TiO2;Take 0.2 g
TiO240 mL H are successively added2O2After 20 min of magnetic agitation, mixed liquor is turned by (0.05 wt%) solution and 0.48 g NaOH
Move on to 180 DEG C of 4 h of reaction, eccentric cleaning in water heating kettle;Sample obtained above is immersed in 20 mL HCl (0.1 mol/L)
It in solution, is centrifuged, is washed to neutrality, hollow titanium dioxide is calcined to obtain in drying.
Step 2: being condensed back method using water phase and prepare TiO2(hollow)/CdTe.Take above-mentioned 2 g TiO240 mL are dissolved in go
In ionized water, ultrasound is uniformly;Weigh 0.0979 g N-acetyl-L-cysteine and 0.1145 g CdCl2·2.5H2O successively adds
Enter above-mentioned solution, 30 min are respectively stirred at room temperature;0.178 g KBH is then added4, then with the speed dropwise addition 10 of 5 mL/min
mL Na2TeO3(0.01 mol/L);Above-mentioned mixed system is warming up to 100 DEG C, the heating-up time is controlled in 30 min, utilizes water phase
Method is condensed back, and is sampled after 6 h, the TiO made after washing and drying2(hollow)/CdTe powder.
Step 3:TiO2The preparation of (hollow)/CdTe/BiOBr nanocomposite is (with TiO2/ CdTe:BiOBr=1:1 is
Example).Weigh 0.258 g TiO2/CdTe、0.1596 g BiONO3, 0.0385 g KBr be dissolved in 10 mL, 7 mL, 6 mL respectively
In ethylene glycol solution, ultrasound is simultaneously stirred evenly;Under continuing magnetic force stirring, by BiNO3With KBr solution with the speed of the every drop of 5 s
It is added drop-wise to TiO2In/CdTe solution, continue to stir 1 h;Above-mentioned mixed liquor is put into reaction kettle and reacts 3 h at 80 DEG C, is washed
It is dry, obtain TiO2(hollow)/CdTe/BiOBr composite material.
Fig. 1 is the TiO of preparation2The SEM picture of (hollow)/CdTe/BiOBr composite material, it can be seen that the nanometer of preparation
Composite material is in micro-sphere structure, a large amount of nanometer sheet of area load, thus it is speculated that is BiOBr, and can be seen that microballoon is hollow
Structure.Fig. 2 is the TiO of preparation2The EDS picture of (hollow)/CdTe/BiOBr composite material, can learn the composite material of preparation
In contain the elements such as Ti, O, Bi, Br, Cd, Te.Fig. 3 is the TiO of preparation2The TEM of (hollow)/CdTe/BiOBr composite material schemes
Piece, the nanocomposite for further demonstrating preparation is hollow micro-sphere structure.Fig. 4 is TiO2(hollow)/CdTe/BiOBr
The HRTEM picture of composite material, through measurement it can be found that spacing of lattice therein respectively corresponds TiO2de (101) crystal face, BiOBr
(110) crystal face and CdTe (111) crystal face, show that the inventive method can be by BiOBr, CdTe and TiO2Success is compound, system
Obtain the TiO of composite construction2(hollow)/CdTe/BiOBr material.
Claims (5)
1. a kind of TiO2The preparation method of (hollow)/CdTe/BiOBr composite material, it is characterised in that preparation method includes following step
It is rapid:
Step 1: weighing 4.4 mL tetraisopropyl titanates (TTIP) and be dissolved in 200 mL dehydrated alcohols and 0.8 mL KNO3(0.1
Mol/L in mixed solution), precipitation handles 24 h, is cleaned and dried to obtain solid TiO2;Take 0.2 g TiO240 mL are successively added
H2O2(0.05 wt%) solution and 0.48 g NaOH, after 20 min of magnetic agitation, by mixed liquor be transferred in water heating kettle 180 DEG C it is anti-
Answer 4 h, eccentric cleaning;Sample obtained above is immersed in 20 mL HCl (0.1 mol/L) solution, is centrifuged, is washed to
Property, hollow titanium dioxide (TiO is calcined to obtain in drying2(hollow));
Step 2: taking above-mentioned 2 g TiO2It is dissolved in 40 mL deionized waters, ultrasound is uniformly;Weigh 0.0979 g N- acetyl-L- half
Cystine and 0.1145 g CdCl2·2.5H2Above-mentioned solution is successively added in O, and 30 min are respectively stirred at room temperature;Then it is added
0.178 g KBH4, then with the 10 mL Na of speed dropwise addition of 5 mL/min2TeO3(0.01 mol/L);By above-mentioned mixed system liter
Temperature is controlled the heating-up time in 30 min, is condensed back using Aqueous phase, samples after 6 h, make after washing and drying to 100 DEG C
TiO2(hollow)/CdTe powder;
Step 3: on the basis of the above, with BiNO3, KBr be raw material using solvent thermal process adjust (TiO2/ CdTe): BiOBr's
TiO is prepared in mol ratio2(hollow)/CdTe/BiOBr composite material.
2. a kind of TiO as described in claim 12The preparation method of (hollow)/CdTe/BiOBr composite material, it is characterised in that
In TiO2Under the premise of based on (hollow)/CdTe, TiO is prepared using solvent thermal process2(hollow)/CdTe/BiOBr is multiple
(the TiO of condensation material2/ CdTe): the mol ratio of BiOBr is 0.1 ~ 10.
3. a kind of TiO as described in claim 12The preparation method of (hollow)/CdTe/BiOBr composite material, it is characterised in that
In TiO2Under the premise of based on (hollow)/CdTe, TiO is prepared using solvent thermal process2(hollow)/CdTe/BiOBr is multiple
The BiNO of condensation material3, KBr ethylene glycol solution concentration be the mol/L of 0.001 mol/L ~ 1.0.
4. a kind of TiO as described in claim 12The preparation method of (hollow)/CdTe/BiOBr composite material, it is characterised in that
In TiO2Under the premise of based on (hollow)/CdTe, TiO is prepared using solvent thermal process2(hollow)/CdTe/BiOBr is multiple
The reaction temperature of condensation material is 30 ~ 200 DEG C, and the reaction time is 0.5 ~ 24 h.
5. a kind of TiO as described in claim 12The preparation method of (hollow)/CdTe/BiOBr composite material, it is characterised in that
In TiO2Under the premise of based on (hollow)/CdTe, TiO is prepared using solvent thermal process2(hollow)/CdTe/BiOBr is multiple
The subsequent drying temperature of condensation material is 40 ~ 140 DEG C, and drying time is 0.5 ~ 24 h.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116212843A (en) * | 2023-02-14 | 2023-06-06 | 甘肃自然能源研究所 | Preparation method and application of self-template capable of realizing structural regulation and control of flower-like, hollow and solid titanium dioxide microspheres |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116212843A (en) * | 2023-02-14 | 2023-06-06 | 甘肃自然能源研究所 | Preparation method and application of self-template capable of realizing structural regulation and control of flower-like, hollow and solid titanium dioxide microspheres |
CN116212843B (en) * | 2023-02-14 | 2024-01-19 | 甘肃自然能源研究所 | Preparation method and application of self-template capable of realizing structural regulation and control of flower-like, hollow and solid titanium dioxide microspheres |
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Application publication date: 20190726 |