CN105944738A - Preparation method of TiO2/MoS2 composite material based on surface modification - Google Patents
Preparation method of TiO2/MoS2 composite material based on surface modification Download PDFInfo
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- CN105944738A CN105944738A CN201610260441.4A CN201610260441A CN105944738A CN 105944738 A CN105944738 A CN 105944738A CN 201610260441 A CN201610260441 A CN 201610260441A CN 105944738 A CN105944738 A CN 105944738A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 35
- 238000012986 modification Methods 0.000 title claims abstract description 34
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 32
- 230000004048 modification Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000000137 annealing Methods 0.000 claims abstract description 4
- 239000002127 nanobelt Substances 0.000 claims description 49
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 235000015393 sodium molybdate Nutrition 0.000 claims description 11
- 239000011684 sodium molybdate Substances 0.000 claims description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000007246 mechanism Effects 0.000 abstract description 2
- 239000002074 nanoribbon Substances 0.000 abstract 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 4
- 238000010306 acid treatment Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005352 clarification 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
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of TiO2/MoS2 composite material based on surface modification. The method mainly includes 3 steps: 1) obtaining the nanoribbon of titanium dioxide with P25TiO2 powder and concentrated NaOH solution under the hydrothermal condition; 2) performing surface modification processing for the nanoribbon to make the surface of the nanoribbon become rough, and performing annealing to obtain the modified titanium dioxide nanoribbon; and 3) preparing a molybdenum disulfide layer on the surface of titanium dioxide directly with the hydrothermal method to obtain TiO2/MoS2 composite material. The method uses the hydrothermal-surface modification-hydrothermal technology to prepare the TiO2/MoS2 composite material, and the composite material can affect the interfacial electronic performance with the surface modification processing, so that the energy band structure of TiO2/MoS2 heterojunction is affected. Moreover, the composite material is beneficial to improve the photocatalytic performance of the composite material, and has important effect on researching interface electronic performance of the composite material and growth mechanism.
Description
Technical field:
The invention belongs to field of composite material preparation, relate to a kind of TiO2/MoS2The preparation method of hetero-junctions, especially
It relates to a kind of TiO based on surface modification2/MoS2The preparation method of composite.
Background technology:
TiO2As one widely used material in terms of photocatalysis and green environment, due to its native band gap relatively
Wide and separation of charge is inefficient, its light sensitive characteristic is only limitted to ultraviolet light range low to the utilization ratio of sunlight.
In order to make catalyst have catalysis activity under visible light, cause people with the composite that titanium dioxide is formed for base
Extensive concern.Recently, more and more people recognize that electronic behavior plays important at aspects such as photocatalysis performances
Effect, the most surface-functionalized have substantial role to realizing visible light catalytic.This is to be come by Surface Engineering
Improve visible light catalytic performance and provide brand-new idea.
It addition, MoS2Detecting at light, photocatalysis, the aspect such as electronics and photoelectric project has the biggest application potential,
Therefore widely studied functional material is had become as.Many peculiar physical phenomenons are especially limited in monolayer
MoS2In.The scope that suitable energy bandgaps and higher light absorb makes MoS2Be suitably applied in photovoltaic and
Photocatalysis aspect.It is the new method in material science research that coupling bi-material forms novel functional material.
Summary of the invention:
Present invention aims to the deficiencies in the prior art, it is provided that the TiO of a kind of surface modification2/MoS2
The preparation method of composite, the method produces impact by surface modification treatment to its interface Electronic Performance, from
And affect TiO2/MoS2The band structure of hetero-junctions, improves the photocatalysis performance of composite.
Technical scheme is as follows:
A kind of TiO of surface modification2/MoS2The preparation method of composite, comprises the following steps:
(1) configuration TiO 2 precursor solution, uses hydro-thermal method to prepare nano belt；
(2) above-mentioned nano belt is carried out surface modification treatment and make nano belt rough surface, after annealing, obtain modified TiO2
Nano belt；
(3) by modification TiO2Nano belt is placed in molybdenum bisuphide precursor solution, uses hydro-thermal method at modified TiO2
Layer of molybdenum-disulfide is prepared on nano belt surface, obtains the TiO of surface modification2/MoS2Composite.
In technique scheme, described TiO 2 precursor solution is that P25 powder mixes with 10MNaOH
Suspension.
In described step (2), surface modification treatment is: by TiO2Nano belt is first placed in the NaOH of 0.01-10M
Solution reacts at 150 DEG C 4h, then cleans to neutral with 0.1MHCl；Or by TiO2Nano belt is placed in
0.02-0.2M H2SO4Solution 100 DEG C reaction 12h；Or first by TiO2Nano belt is placed in 0.01-10M's
NaOH solution is reacted at 150 DEG C 4h, cleans and be placed in 0.02-0.2M H again to neutrality2SO4Solution 100 DEG C
Reaction 12h.
Described molybdenum bisuphide precursor solution is the mixed liquor of sodium molybdate, thiourea and deionized water, the most often
35-40ml deionized water correspondence sodium molybdate 30-50mg, thiourea 60-100mg.
Further, specifically comprise the following steps that
1) P25 powder addition 10M NaOH will be mixed into suspension, it is thus achieved that TiO 2 precursor solution, put
In reactor, hydro-thermal reaction 21h, product 0.1MHCl cleaning at 210-230 DEG C, obtains nano belt；
2) nano belt is first placed in the NaOH solution of 10M and at 150 DEG C, reacts 4h, then clean with 0.1MHCl
To neutral；Or by TiO2Nano belt is placed in 0.02M H2SO4Solution 100 DEG C reaction 12h；Or first will
TiO2Nano belt is placed in the NaOH solution of 10M reacts 4h at 150 DEG C, clean and be placed in neutrality again
0.02M H2SO4Solution 100 DEG C reaction 12h；Product after above-mentioned surface processes is placed in thermostatic drying chamber and dries
Dry, then anneal 1 hour at 600-750 DEG C, obtain modified TiO2Nano belt；
3) sodium molybdate, thiourea are added in deionized water, every 35-40ml deionized water correspondence sodium molybdate 30-50mg,
Thiourea 60-100mg, configures molybdenum bisuphide precursor solution, with modified TiO2Nano belt is together placed in reactor
In, hydro-thermal reaction 18-21h at 180-210 DEG C, obtain the TiO of surface modification2/MoS2Composite.
Beneficial effect: the present invention uses the technique of hydro-thermal-surface modification-hydro-thermal to prepare TiO2/MoS2Composite,
The Electronic Performance at interface can be affected by surface modification treatment, thus affect TiO2/MoS2Tying by band of hetero-junctions
Structure, is conducive to improving the photocatalysis performance of composite.Simultaneously to research composite material interface Electronic Performance and life
Long mechanism plays an important role.
Accompanying drawing illustrates:
Fig. 1. the scanning electron microscope (SEM) photograph of surface-modified process titanium dioxide nano-belts in the present invention.
Wherein: (a) unmodified process, (b) sulfuric acid treatment, (c) sodium hydroxide+hydrochloric acid+sulphuric acid processes, (d) hydrogen-oxygen
Change sodium+HCl treatment；
Fig. 2. the TiO of the present invention2/MoS2The transmission electron microscope picture of composite.
Wherein: (a-c) sulfuric acid treatment respectively, sodium hydroxide+hydrochloric acid+sulphuric acid processes, sodium hydroxide+HCl treatment
TiO2/MoS2Composite transmission plot；The High-Resolution Map of the composite after (d) sulfuric acid treatment.
Fig. 3. the final TiO obtained after different surfaces modification in the present invention2/MoS2The valence band of composite is inclined
Move and the energy band schematic diagram of conduction band offset.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in more detail.Should be appreciated that described herein
Specific embodiment only in order to explain the present invention, is not intended to limit the present invention.
The process of the preparation of the composite of the present invention mainly includes three parts: (a) hydro-thermal method obtains nano belt
B () modification titanium dioxide nano-belts (c) hydro-thermal method prepares titanium dioxide and molybdenum bisuphide composite.
Embodiment 1:
A () hydro-thermal method prepares nano belt
By the P25TiO of 0.15g2With the suspension that the concentrated NaOH solution of 10M makes uniform 30ml, in
In the anti-still of high pressure, at 210-230 DEG C, it is incubated 24h, natural cooling, the dilute HCl of whiteness 0.1M obtained
Solution and deionized water clean to neutral or faintly acid.
(b) modification nano belt
Prepared white nano belt is mixed homogeneously with the 0.02M dilute sulfuric acid of 40ml, is placed in tetrafluoroethene inner bag
Being incubated 12 hours at 100 DEG C, cooling also cleans up with deionized water.Again nano belt is placed in thermostatic drying chamber
In, dry 6 hours 600-750 DEG C of annealing 1h in the tube furnace of logical oxygen again at 80 DEG C, obtain modification
Titanium dioxide nano-belts, its SEM schemes as shown in Fig. 1 (b).
C () hydro-thermal method prepares TiO2/MoS2Composite
Weigh in 30mg sodium molybdate and 60mg thiourea addition 30ml deionized water and stir into transparent liquid, by 30mg
Modified titanium dioxide nano-belts is placed in ultrasonic 15min in 30ml clear liquor and makes white suspension, by suspended
Liquid is placed in autoclave and 210 DEG C of insulation 21h in thermostatic drying chamber.Natural cooling room temperature, obtains
The composite of black, and use deionized water eccentric cleaning.Within last 6 hours in 80 DEG C of thermostatic drying chambers, dry
Dry obtain TiO2/MoS2Composite, its transmission electron microscope picture is as shown in Figure 2.
Research shows, through dilute H2SO4Modification, can make titanium dioxide nano-belts Surface Creation nano-particle and
Nano-pore, is become coarse from smooth surface, thus affects its interface electronic state, through H2SO4Modified dioxy
The work function changing its surface of titanium can reduce 0.07eV.
Embodiment 2:
A () hydro-thermal method prepares nano belt
The concentrated NaOH solution of P25 Yu 10M of 0.15g is made uniform transparent liquid 30ml altogether, will clarification
Liquid is placed in high pressure and answers in still, is incubated 24h, natural cooling, the whiteness 0.1M obtained at 210-230 DEG C
Dilute HCl solution and deionized water clean to neutral or faintly acid.
(b) modification nano belt
By prepared white nano belt, with the 10M concentrated NaOH solution mix homogeneously of 40ml, it is placed in tetrafluoroethene
Inner bag is incubated 4 hours at 150 DEG C, cleans to neutral with the dilute HCl solution of 0.1M and deionized water afterwards.
Then product is mixed homogeneously with 0.02M dilute sulfuric acid (40ml), be placed in tetrafluoroethene inner bag and be incubated at 100 DEG C
12 hours, cooling also cleaned up with deionized water.By the white nano belt that obtains at 80 DEG C of thermostatic drying chambers
Middle drying 6 hours.Finally calcining 1h at logical oxygen at 600-750 DEG C, the titanium dioxide obtaining modification is received
Rice band.
C () hydro-thermal method prepares TiO2/MoS2Composite
Weigh in 30mg sodium molybdate and 60mg thiourea addition 30ml deionized water and stir into transparent liquid, by 30mg
Modified titanium dioxide nano-belts is placed in ultrasonic 15min in transparent liquid and makes white suspension, is placed in by suspension
21h it is incubated in autoclave and in 210-230 DEG C of calorstat.Natural cooling room temperature, obtains black
Composite, and use deionized water separation and Extraction, and drying in 6 hours obtains in 80 DEG C of thermostatic drying chambers
TiO2/MoS2Composite.
Embodiment 3:
A () hydro-thermal method prepares nano belt
The concentrated NaOH solution of P25 Yu 10M of 0.15g is made the suspension of 30ml, answers still to put high pressure
Being incubated 24h in 210-230 DEG C of calorstat, natural cooling, the dilute HCl of whiteness 0.1M obtained is molten
Liquid and deionized water clean to neutral or faintly acid.
(b) modification nano belt
Prepared white metatitanic acid nano belt is mixed homogeneously with the 10M concentrated NaOH solution of 40ml, is placed in tetrafluoro
Ethylene inner bag (50ml) is incubated 4 hours at 150 DEG C, clear with the dilute HCl solution of 0.1M and deionized water afterwards
It is washed till neutrality.Then white powder is placed in thermostatic drying chamber, dries 6 hours at 80 DEG C.Last at oxygen
In the tube furnace of atmosphere, 600-750 DEG C of calcining 1h, obtains the titanium dioxide nano-belts of modification.
C () hydro-thermal method prepares titanium dioxide and molybdenum bisuphide composite.
Weigh 30mg sodium molybdate and 60mg thiourea deionized water is configured to the transparent liquid of 30ml, by 30mg
Modified titanium dioxide nano-belts be placed in ultrasonic 15min in transparent liquid and make white suspension, suspension is put
With 210-230 DEG C of insulation 21h in autoclave and at thermostatic drying chamber.Natural cooling room temperature, uses it
Ionized water eccentric cleaning obtains the composite of black.In thermostatic drying chamber, it is placed in 80 DEG C dry 6 hours
To TiO2/MoS2Composite.
Although the present invention combines above example and is described, but the present invention is not limited to above-mentioned enforcement
Example, it easily can be modified and change by those of ordinary skill in the art, but and without departing from the reality of the present invention
Matter spirit and scope.
Claims (5)
1. a TiO based on surface modification2/MoS2The preparation method of composite, it is characterised in that include with
Lower step:
(1) configuration TiO 2 precursor solution, uses hydro-thermal method to prepare TiO2Nano belt；
(2) to above-mentioned TiO2Nano belt carries out surface modification treatment makes nano belt rough surface, obtains modification after annealing
TiO2Nano belt；
(3) by modification TiO2Nano belt is placed in molybdenum bisuphide precursor solution, uses hydro-thermal method at modified TiO2
Layer of molybdenum-disulfide is prepared on nano belt surface, obtains the TiO of surface modification2/MoS2Composite.
2. TiO based on surface modification as claimed in claim 12/MoS2The preparation method of composite, it is special
Levying and be, described TiO 2 precursor solution is the suspension that P25 powder mixes with 10MNaOH.
3. TiO based on surface modification as claimed in claim 12/MoS2The preparation method of composite, it is special
Levying and be, in described step (2), surface modification treatment is by TiO2Nano belt is first placed in 0.01-10M's
NaOH solution is reacted at 150 DEG C 4h, then cleans to neutral with 0.1MHCl；Or by TiO2Nano belt
It is placed in 0.02-0.2M H2SO4Solution 100 DEG C reaction 12h；Or first by TiO2Nano belt is placed in 0.01-10M
NaOH solution in react 4h at 150 DEG C, clean and be placed in 0.02-0.2M H again to neutrality2SO4Solution 100 DEG C
Reaction 12h.
4. TiO based on surface modification as claimed in claim 12/MoS2The preparation method of composite, its feature
Being, described molybdenum bisuphide precursor solution is the mixed liquor of sodium molybdate, thiourea and deionized water, the most often
35-40ml deionized water correspondence sodium molybdate 30-50mg, thiourea 60-100mg.
5. a TiO based on surface modification2/MoS2The preparation method of composite, it is characterised in that include with
Lower step:
1) P25 powder addition 10M NaOH will be mixed into suspension, it is thus achieved that TiO 2 precursor solution, put
In reactor, hydro-thermal reaction 21h, product 0.1MHCl cleaning at 210-230 DEG C, obtains TiO2Nanometer
Band；
2) by TiO2Nano belt is first placed in the NaOH solution of 10M reacts 4h at 150 DEG C, then uses 0.1MHCl
Clean to neutral；Or by TiO2Nano belt is placed in 0.02M H2SO4Solution 100 DEG C reaction 12h；Or first
By TiO2Nano belt is placed in the NaOH solution of 10M reacts 4h at 150 DEG C, clean and be placed in neutrality again
0.02M H2SO4Solution 100 DEG C reaction 12h；Product after above-mentioned surface processes is placed in thermostatic drying chamber and dries
Dry, then anneal 1 hour at 600-750 DEG C, obtain modified TiO2Nano belt；
3) sodium molybdate, thiourea are added in deionized water, every 35-40ml deionized water correspondence sodium molybdate 30-50mg,
Thiourea 60-100mg, configures molybdenum bisuphide precursor solution, with modified TiO2Nano belt is together placed in reactor
In, hydro-thermal reaction 18-21h at 180-210 DEG C, obtain the TiO of surface modification2/MoS2Composite.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106492792A (en) * | 2017-01-05 | 2017-03-15 | 吉林化工学院 | A kind of loaded catalyst of eliminating formaldehyde at room temperature and preparation method thereof |
| CN106799244A (en) * | 2017-01-10 | 2017-06-06 | 江苏大学 | The preparation method and purposes of a kind of Three-element composite photocatalyst |
| CN107574454A (en) * | 2017-09-19 | 2018-01-12 | 河北工业大学 | It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite and preparation method thereof for electrochemistry liberation of hydrogen |
| CN108609657A (en) * | 2018-04-20 | 2018-10-02 | 西安交通大学 | A kind of titanium dioxide/molybdenum disulfide metal composite oxide micro Nano material and preparation method thereof |
| CN110787815A (en) * | 2019-11-13 | 2020-02-14 | 南京工程学院 | TiO 22/MoS2Three-dimensional photonic crystal composite material with core-shell structure and preparation method thereof |
| CN112831800A (en) * | 2020-12-30 | 2021-05-25 | 河南科技大学 | Preparation method of molybdenum-based composite material electrode plate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106492792A (en) * | 2017-01-05 | 2017-03-15 | 吉林化工学院 | A kind of loaded catalyst of eliminating formaldehyde at room temperature and preparation method thereof |
| CN106799244A (en) * | 2017-01-10 | 2017-06-06 | 江苏大学 | The preparation method and purposes of a kind of Three-element composite photocatalyst |
| CN106799244B (en) * | 2017-01-10 | 2019-10-01 | 江苏大学 | A kind of preparation method and purposes of Three-element composite photocatalyst |
| CN107574454A (en) * | 2017-09-19 | 2018-01-12 | 河北工业大学 | It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite and preparation method thereof for electrochemistry liberation of hydrogen |
| CN107574454B (en) * | 2017-09-19 | 2019-04-05 | 河北工业大学 | It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material and preparation method for electrochemistry liberation of hydrogen |
| CN108609657A (en) * | 2018-04-20 | 2018-10-02 | 西安交通大学 | A kind of titanium dioxide/molybdenum disulfide metal composite oxide micro Nano material and preparation method thereof |
| CN110787815A (en) * | 2019-11-13 | 2020-02-14 | 南京工程学院 | TiO 22/MoS2Three-dimensional photonic crystal composite material with core-shell structure and preparation method thereof |
| CN110787815B (en) * | 2019-11-13 | 2022-07-29 | 南京工程学院 | TiO (titanium dioxide) 2 /MoS 2 Three-dimensional photonic crystal composite material with core-shell structure and preparation method thereof |
| CN112831800A (en) * | 2020-12-30 | 2021-05-25 | 河南科技大学 | Preparation method of molybdenum-based composite material electrode plate |
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