CN104209135B - A kind of efficient visible light excites catalyst of water decomposition hydrogen making and oxygen and preparation method thereof - Google Patents
A kind of efficient visible light excites catalyst of water decomposition hydrogen making and oxygen and preparation method thereof Download PDFInfo
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- CN104209135B CN104209135B CN201310217532.6A CN201310217532A CN104209135B CN 104209135 B CN104209135 B CN 104209135B CN 201310217532 A CN201310217532 A CN 201310217532A CN 104209135 B CN104209135 B CN 104209135B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a kind of efficient visible light excites catalyst of water decomposition hydrogen making and oxygen and preparation method thereof, this photochemical catalyst is by element tantalum, indium, nickel, oxygen and nitrogen into taking solid-solution approach, pre-dried raw material oxide powder In2O3, NiO and Ta2O5Tabletting machine is used after being well mixed according to stoichiometric proportion, in high-temperature roasting.Grinding is sieved, and most carries out Nitrizing Treatment under ammonia.As a result show that the catalyst of the present invention can produce hydrogen and oxygen by decomposition water under visible light.
Description
Technical field
The invention belongs to photocatalytic water splitting technical field, more particularly, is related to photocatalytic water catalyst and its preparation
Method.
Background technology
With the increasingly depleted of fossil fuel, and its severe environments harm for bringing, seeking a kind of alternative cleaning can
The renewable sources of energy are the eager desires of the mankind.Solar energy is a kind of inexhaustible natural energy source, is sent out using solar energy
Electricity is early to have had turned into reality.Also with solar energy by the focus direction that water decomposition is hydrogen and oxygen is recent studies,
This have the advantage that, energy is stored easily more than being got up with electric energy or thermal energy storage with hydrogen form；Hydrogen rubs
Your calorific value is high（～140kJ/g）, energy storage capacity is big, clean environment firendly, and nonhazardous is a kind of fuel with very big potential advantages and energy
Source；And, hydrogen is produced by water, after burning, water is regenerated, its net result is that luminous energy changes for chemical energy, if realizing light
Xie Shui obtains hydrogen and can then reach energy sustainability；Hydrogen is not only a kind of clean energy resource for storing high-energy, Er Qieyi
It is a kind of particularly important industrial chemicals, the reaction such as such as synthesis ammonia, methyl alcohol, and participation hydrogenation, desulfurization, denitrogenation, demetalization is special
Not being can be with hydrogenating reduction GHG carbon dioxide.So, finding a kind of favourable complete water decomposition mode becomes pass
Key.1971, Japanese Scientists Fujishima and Honda reported firsts titanium dioxide under ultraviolet light, with pole of closing
Little applied voltage can just decompose the science and technology discovery of pure water, and the new page of modern age photocatalysis field has been started in this discovery.In order to
With the help of without applied voltage can also decomposition water completely, in the time of nearly 40 years, innumerable photocatalytic water catalysis
Agent is developed, and reaction mechanism and reaction model are also constantly built and updated.Typical photocatalytic water catalyst has TiO2, CdS,
(Ga1-xZnx)(N1-xOx), TaON, SrTiO3Deng, also numerous research and develop to overcome single photochemical catalyst not enough compound
Photocatalytic water catalyst such as Pt/TiO2, CdS/TiO2, ZnO/CdS, TiO2/RuO2Deng.Scientists have tried to, and have developed a large amount of
New catalyst, but the report quantity that can reach decomposition water purpose is little.
Content of the invention
It is an object of the invention to overcoming the deficiencies in the prior art, there is provided a kind of efficient visible light excites water decomposition preparing hydrogen
Catalyst of gas and oxygen and preparation method thereof.
The purpose of the present invention is achieved by following technical proposals：
A kind of efficient visible light excites the catalyst of water decomposition hydrogen making and oxygen, by element tantalum（Ta）, indium（In）, nickel
（Ni）, oxygen（O）, nitrogen（N）Composition, chemical constituent are expressed as In1-xNixTaO4-zNz, present monocrystalline state, wherein x represent elemental nickel and
The molar ratio of tantalum, 0<X≤0.2, preferably 0.1≤x≤0.2, more preferably 0.1；Z represents the mol ratio of elemental nitrogen and oxygen
Example, 0<z<1.
Preparation method is prepared using solid-solution approach, is carried out as steps described below：
Step 1, by oxide powder In2O3, NiO and Ta2O5Carry out according to the stoichiometric proportion that above-mentioned chemical constituent is represented
It is well mixed rear compressing tablet；
Step 2, by compressing tablet after sample carry out high-temperature roasting；
Step 3, by high-temperature roasting after sample grinding sieve；
Powder after sieving is carried out Nitrizing Treatment under ammonia by step 4, obtains final catalyst In1-xNixTaO4-zNz.
In above-mentioned technical proposal, in the step 1, the oxide powder of selection is pure for chemical pure or analysis, in advance
It is dried to exclude the impact of moisture, sieves after being then ground（200 300 mesh）, the more homogeneous oxygen of selection particle diameter
Compound powder is mixed；Ball mill is selected in mixed process, and rotating speed is 500 700 revs/min, and the duration is in 30min
More than, preferably 30 60min also may be selected hand lapping, to reach for the purpose of oxide powder is well mixed；Select during compressing tablet
Tablet press machine is carried out, and pressure selects 1 to 5Mpa, preferably 2 5MPa.
In the step 2, the high-temperature roasting technique is：Sintering temperature be 1,000 1200 DEG C, preferably 1,100 1150
℃；Roasting temperature retention time at least 20 hours, such as 20 72 hours, preferably 24 48 hours；Start to warm up from room temperature 20 25,
After being incubated the time required to reaching, to room temperature, calcination atmosphere selects air, conventional Muffle of the roasting machine from temperature control to natural air cooling
Stove.
In the step 3, by high-temperature roasting after sample grinding sieve and obtain the more homogeneous powder particle of particle diameter, while
The area of increase nitriding, such as 100 300 mesh.
In the step 4, the powder after sieving is carried out under ammonia Nitrizing Treatment, temperature selects 750 1100 DEG C, excellent
Select 800 850 DEG C；The time control of nitriding is selected according to required z sizes, and generally, nitriding time is longer, z
Value is bigger, shows that the elemental nitrogen content for penetrating into is bigger, while the oxide diameter sizes through high-temperature roasting can be made to be declined by micron order
Arrive nanoscale, you can by nitriding time regulate and control nitrogen content and particle diameter size, such as 5 60 hours.
Shown in attached Figure 12, according to In prepared by technical solution of the present invention0.9Ni0.1TaO3.226N0.774Catalyst, particle
It is uniformly dispersed, in irregular shape, average grain diameter is 500 rans, assumes monocrystalline state, and crystal formation is good, lattice fringe in figure
Width is 3.99 angstroms.As shown in Figure 3, raw material Ta2O5Less than 320 nanometers of ultraviolet light, oxide catalyst can only be absorbed
In0.9Ni0.1TaO4In the only a small amount of absorption of visible region.With itrogen content of getter with nitrogen doped increase response that catalyst gone in visible ray also by
Step increases, and energy gap is reduced, the reason for so as to explain decomposition water activity.
It can be seen that In from the XRD of accompanying drawing 40.9Ni0.1TaO4Diffraction spectra correspond to oxide standard spectrogram
（JCPDSNo.25-0391）, with the prolongation of nitrating time, new nitrogen oxides（JCPDSNo.70-1193）Diffraction maximum increase
Height, oxide peak decline, and up to nitriding 60 hours, oxide diffraction maximum disappeared, and now catalyst is
In0.9Ni0.1TaO3.226N0.774Catalyst, and average grain diameter is 500 rans.Constituent content analysis are by x-ray photoelectron spectroscopy
Measure（XPS;Perkinelmer,PHI1600ESCA）, it is seen that as the prolongation nitrogen content of nitrating time increases.Specific surface area by
BET is measured（QuantachromeQuadraSorbSI）, the nitrating time is longer, and catalyst particle size is less, and specific surface area is got over
Greatly.The sample average particle diameter of non-nitrating in 5 microns, nitrating after 60 hours average grain diameter be reduced to 500 nanometers.Aerogenesis activity
Drawn by active testing system（The luxuriant and rich with fragrance Lay of pool, III AG types of LabSolar-）, the increase of nitrogen content as can be seen from the table causes work
The increase of property.
1. elementary analysis of table, Surface area analysis and gas production rate
Using the luxuriant and rich with fragrance Lay of pool, the test system of III AG type light decomposition waters of LabSolar-, shown in accompanying drawing 5 and 6, nickel content is deposited
In an optimum value（x=0.1）, and one preferably interval [0.1,0.2].Catalyst using the present invention is in 10 hours
Activity stabilized, hydrogen and oxygen can be produced by decomposition water under visible light.
Description of the drawings
Fig. 1 is the catalyst SEM of the present invention（SEM, Hitachi, S-4800）Photo.
Fig. 2 is the catalyst transmission electron microscope of the present invention（TEM, JEOLJEM-2100F）Photo.
Fig. 3 is the ultraviolet-visible absorption spectroscopy figure of catalyst of the present invention（Instrument is Perkinelmer, L750）, wherein a is
Ta2O5；B is In0.9Ni0.1TaO4；C is In0.9Ni0.1TaO3.846N0.154；D is In0.9Ni0.1TaO3.704N0.296；E is
In0.9Ni0.1TaO3.449N0.551；F is In0.9Ni0.1TaO3.333N0.667；G is In0.9Ni0.1TaO3.226N0.774.
Fig. 4 is the X-ray diffractogram of oxide raw material and nitriding catalyst（a,JCPDSNo.25-0391;b,
JCPDSNo.70-1193）（BrukerAXS,D8-S4）.
Fig. 5 is impact figure of the nickel content to complete water decomposition activity（Nickel content is abscissa, i.e. x values）.
Fig. 6 is the water decomposition activity figure using catalyst of the invention in 10 hours.
Specific embodiment
Technical scheme is further illustrated with reference to specific embodiment.From oxide powder for chemistry pure
Or analysis is pure, is dried in advance to exclude the impact of moisture；Ball mill is selected, rotating speed is 500 700 revs/min, continues
Time, in more than 30min, preferably 30 60min, also may be selected hand lapping, is well mixed as mesh with reaching oxide powder
's；Carried out from tablet press machine during compressing tablet, pressure selects 1 to 5Mpa, preferably 2 5MPa.
Embodiment 1
Weigh 1gTa2O5, 0.565gIn2O3, 0.0338gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.9Ni0.1TaO4Sample takes out, and grinding is sieved
（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 60 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.226N0.774Sample.
Embodiment 2
Weigh 1gTa2O5, 0.565gIn2O3, 0.0338gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.9Ni0.1TaO4Sample takes out, and grinding is sieved
（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 40 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.333N0.667Sample.
Embodiment 3
Weigh 1gTa2O5, 0.565gIn2O3, 0.0338gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.9Ni0.1TaO4Sample takes out, and grinding is sieved
（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 20 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.449N0.551Sample.
Embodiment 4
Weigh 1gTa2O5, 0.565gIn2O3, 0.0338gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.9Ni0.1TaO4Sample takes out, and grinding is sieved
（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.704N0.296Sample.
Embodiment 5
Weigh 1gTa2O5, 0.565gIn2O3, 0.0338gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.9Ni0.1TaO4Sample takes out, and grinding is sieved
（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 5 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.846N0.154Sample.
Embodiment 6
Weigh 1gTa2O5, 0.627gIn2O3Grinding stirring mixing, forms uniform mixed-powder, using tablet press machine and compressing tablet
Grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the InTaO for obtaining4Sample takes out, and grinding is sieved（300 mesh）.Gained powder
In the lower nitridation of 800 DEG C of ammonia atmospheres point 60 hours, ammonia flow velocity 150mL/min.Finally give InTaO3.896N0.104Sample.
Embodiment 7
Weigh 1gTa2O5, 0.611gIn2O3, 0.008gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.975Ni0.025TaO4Sample takes out, ground
Sieve（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.650N0.350Sample.
Embodiment 8
Weigh 1gTa2O5, 0.596gIn2O3, 0.017gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.95Ni0.05TaO4Sample takes out, ground
Sieve（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.9Ni0.1TaO3.398N0.602Sample.
Embodiment 9
Weigh 1gTa2O5, 0.580gIn2O3, 0.025gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.925Ni0.075TaO4Sample takes out, ground
Sieve（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.925Ni0.075TaO3.267N0.733Sample.
Embodiment 10
Weigh 1gTa2O5, 0.548gIn2O3, 0.042gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.875Ni0.125TaO4Sample takes out, ground
Sieve（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.875Ni0.125TaO3.220N0.780Sample.
Embodiment 11
Weigh 1gTa2O5, 0.533gIn2O3, 0.051gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.85Ni0.15TaO4Sample takes out, ground
Sieve（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.85Ni0.15TaO3.200N0.800Sample.
Embodiment 12
Weigh 1gTa2O5, 0.517gIn2O3, 0.059gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.825Ni0.175TaO4Sample takes out, ground
Sieve（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.825Ni0.175TaO3.190N0.810Sample.
Embodiment 13
Weigh 1gTa2O5, 0.502gIn2O3, 0.067gNiO grinding stirring mixing, the uniform mixed-powder of formation, using pressure
Piece machine and compressing tablet grinding tool compressing tablet, roasting 48 hours at 1150 DEG C.By the In for obtaining0.8Ni0.2TaO4Sample takes out, and grinding is sieved
（300 mesh）.Gained powder is in the lower nitridation of 800 DEG C of ammonia atmospheres point 10 hours, ammonia flow velocity 150mL/min.Finally give
In0.8Ni0.2TaO3.175N0.825Sample.
In high-temperature calcination process, it is 1,000 1200 DEG C, preferably 1,100 1150 DEG C to change sintering temperature；Change roasting
Temperature retention time 20 72 hours, preferably 24 48 hours.In Nitrizing Treatment, change temperature and select 750 1100 DEG C, preferably
800 850 DEG C, extend nitriding time as needed, to obtain the catalyst of different z sizes, such as 5 60 hours, by oozing
The content of nitrogen time-controllable nitrogen and the size of particle diameter.
Exemplary description has been done above, it should explanation, in the situation of the core without departing from the present invention to the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent of creative work equal
Fall into protection scope of the present invention.
Claims (11)
1. a kind of efficient visible light excites the catalyst of water decomposition hydrogen making and oxygen, it is characterised in that by element tantalum, indium,
Nickel, oxygen and nitrogen composition, chemical constituent are expressed as In1-xNixTaO4-zNz, assuming monocrystalline state, wherein x represents rubbing for elemental nickel and tantalum
That ratio, 0<x≤0.2；Z represents the molar ratio of elemental nitrogen and tantalum, 0<z<1, it is prepared as steps described below：
Step 1, by oxide powder In2O3, NiO and Ta2O5After being well mixed according to the stoichiometric proportion that chemical formula is represented
Compressing tablet；
Step 2, by compressing tablet after sample carry out high-temperature roasting, the high-temperature roasting technique is：Sintering temperature is 1,000 1200
℃；Roasting temperature retention time at least 20 hours；
Step 3, by high-temperature roasting after sample grinding sieve；
Powder after sieving is carried out Nitrizing Treatment under ammonia by step 4, obtains final catalyst In1-xNixTaO4-zNz, temperature
Select 750 1100 DEG C；The time control of nitriding is selected according to required z sizes.
2. a kind of efficient visible light according to claim 1 excites the catalyst of water decomposition hydrogen making and oxygen, and which is special
Levy and be, the x is 0.1≤x≤0.2.
3. a kind of efficient visible light according to claim 1 excites the catalyst of water decomposition hydrogen making and oxygen, and which is special
Levy and be, the x is 0.1.
4. a kind of efficient visible light according to claim 1 excites the catalyst of water decomposition hydrogen making and oxygen, and which is special
Levy and be, 4 the step of preparation method in, by nitriding time regulate and control nitrogen content and particle diameter size.
5. a kind of method for preparing catalyst as claimed in claim 1, it is characterised in that carry out as steps described below：
Step 1, by oxide powder In2O3, NiO and Ta2O5According to In1-xNixTaO4-zNzThe stoichiometric proportion of expression is mixed
Close uniform after compressing tablet, wherein x represents the molar ratio of elemental nickel and tantalum, 0<x≤0.2；Z represents the mol ratio of elemental nitrogen and tantalum
Example, 0<z<1；
Step 2, by compressing tablet after sample carry out high-temperature roasting, the high-temperature roasting technique is：Sintering temperature is 1,000 1200
℃；Roasting temperature retention time at least 20 hours；
Step 3, by high-temperature roasting after sample grinding sieve；
Powder after sieving is carried out Nitrizing Treatment under ammonia by step 4, obtains final catalyst In1-xNixTaO4-zNz, temperature
Select 750 1100 DEG C；Regulate and control the content of nitrogen and the size of particle diameter by nitriding time.
6. preparation method according to claim 5, it is characterised in that in the step 2, roasting temperature retention time are 20 72
Hour.
7. preparation method according to claim 5, it is characterised in that in the step 2, the high-temperature roasting technique is：
Sintering temperature is 1,100 1150 DEG C；Roasting temperature retention time is 24 48 hours；From room temperature, 20 25 DEG C start to warm up, and insulation reaches
To after required time, to room temperature, calcination atmosphere selects air, conventional Muffle furnace of the roasting machine from temperature control to natural air cooling.
8. preparation method according to claim 5, it is characterised in that in the step 1, the oxide powder of selection is for changing
Learn pure or analysis pure, be dried to exclude the impact of moisture in advance, sieved after being then ground, select particle diameter more equal
One oxide powder is mixed；Ball mill is selected in mixed process, rotating speed is 500 700 revs/min, the duration
In more than 30min, hand lapping is also may be selected, to reach for the purpose of oxide powder is well mixed；Tablet press machine is selected during compressing tablet
Carry out, pressure selects 1 to 5Mpa.
9. preparation method according to claim 8, it is characterised in that in the step 3, by high-temperature roasting after sample grind
Honed sieve obtains the more homogeneous powder particle of particle diameter, while increasing the area of nitriding, the grit number of crossing is 100 300 mesh.
10. preparation method according to claim 5, it is characterised in that in the step 1, the oxide powder of selection is
Chemistry is pure or analysis is pure, is dried to exclude the impact of moisture in advance, is sieved after being then ground, and selects particle diameter more
Homogeneous oxide powder is mixed；Ball mill is selected in mixed process, and rotating speed is 500 700 revs/min, when continuing
Between be 30 60min, hand lapping also may be selected, to reach for the purpose of oxide powder is well mixed；Compressing tablet is selected during compressing tablet
Machine is carried out, and pressure is chosen as 2 5MPa.
11. preparation methods according to claim 5, it is characterised in that in the step 4, the powder after sieving is existed
Nitrizing Treatment is carried out under ammonia, and temperature is 800 850 DEG C, and the time is 5 60 hours.
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| CN201611092053.6A CN106732717B (en) | 2013-05-31 | 2013-05-31 | Application in water generation hydrogen and oxygen is decomposed by the catalyst that element tantalum indium nickel oxygen and nitrogen form under visible light |
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