CN103418394B - Method for synthesizing nickel-doped indium vanadate nanocrystalline photocatalyst by adopting microwave heating method and application thereof for water decomposition under visible light - Google Patents
Method for synthesizing nickel-doped indium vanadate nanocrystalline photocatalyst by adopting microwave heating method and application thereof for water decomposition under visible light Download PDFInfo
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Abstract
The invention belongs to the technical field of functional inorganic nano-material preparation, and relates to a method for synthesizing nickel-doped indium vanadate (Ni-InVO4) nanocrystalline photocatalyst by adopting a microwave heating method and application thereof for water decomposition under visible light. The method for synthesizing the nickel-doped indium vanadate nanocrystalline photocatalyst comprises the following steps: preparing a liquid precursor, then placing the liquid precursor in a microwave reactor for reaction, centrifugal washing and drying to obtain the nickel-doped indium vanadate (Ni-InVO4) nanocrystalline photocatalyst; the liquid precursor is prepared through the following steps: dissolving soluble indium salt and nickel salt to form aqueous solutions, weighing aqueous solutions of indium salt and nickel salt into deionized water, adding metavanadate solid particles under agitation, adjusting pH value by virtue of dilute nitric acid, and stirring to obtain faint yellow emulsion. According to the invention, the nickel-doped indium vanadate nanocrystalline photocatalyst is synthesized by adopting the microwave heating method; by changing the proportion of Ni/In in the liquid precursor, the controlled adjustment for the energy band of the Ni-InVO4 nanocrystalline photocatalyst can be realized, and the prepared Ni-InVO4 nanocrystalline is greatly improved in visible-light activity as compared with a non-doped sample. The method and the application are simple and convenient to operate, and the synthesis can be realized through one step.
Description
Technical field
The invention belongs to technical field of functional inorganic nano-material preparation, relate to a kind of preparation of photochemical catalyst, particularly relate to the method for microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst and the application of decomposition water under visible light thereof.
Background technology
Under energy crisis and environmental problem dual-pressure, development new forms of energy become the active demand of human kind sustainable development.Hydrogen Energy because of its fuel value high, free of contamination feature, becomes the new forms of energy of 21 century most possible substitute fossil fuels.Avoid photocatalytic hydrogen production by water decomposition technology effective cracking fossil energy hydrogen manufacturing that traditional industry adopts and water electrolysis hydrogen production mode consume energy high, pollute the shortcomings such as large, be considered to ideal and the most promising Hydrogen Energy development approach.From solar spectrum composition, ultraviolet region is less than 5%, and visible region is up to more than 43%.Therefore, develop can practical application visible-light response type progress of hydrogen production from water by photodecomposition catalyst and to build photocatalysis hydrogen production system be key scientific problems urgently to be resolved hurrily in this technical field current.
From the actual application prospect in future, the visible light-responded peroxide breaks down water hydrogen production photocatalyst that stability is high has more future.But wherein the overwhelming majority is the body phase material obtained by high temperature solid state reaction, and specific area is very low, is the main cause causing such material producing hydrogen efficiency always not high.Vanadic acid indium is a kind of arrowband oxide semiconductor photochemical catalyst, and its band gap, at about 2.0eV, has good visible light activity.But due to quantum size effect, the undersized vanadic acid indium nano-photocatalyst with bigger serface often has poor visible light activity.Transition metal element doped is a kind of effective Photocatalyst means, and Ni atomic size is suitable with In atomic size, easily replaces.By introducing impurity energy level, the visible light activity of the vanadic acid nanocrystal In photochemical catalyst after nickel doping strengthens greatly, is a kind of visible photocatalysis water photochemical catalyst preferably.Meanwhile, obtained nickel doping vanadic acid indium is of a size of 20 nanometers, has extra small size and huge specific area, provide a large amount of reactivity sites, fully can contact with reaction substrate, increase the reaction chance of photogenerated charge, thus improve the efficiency of photochemical catalyzing.
Summary of the invention
The object of the invention is by introducing containing transition metal element impurity, to strengthen the visible light activity of vanadic acid nanocrystal In photochemical catalyst, the hydrogen-producing speed of decomposition water under raising visible ray.
A kind of method of microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst, comprise preparation precursor liquid, then reaction in microwave reactor is placed in, and form through centrifuge washing drying, described preparation precursor liquid, that solubility indium salt and nickel salt are dissolved into the aqueous solution respectively, measure indium salt and nickel salt aqueous solution in deionized water, under agitation add metavanadate solid particle, with dust technology, pH value is adjusted between 2 ~ 3, form orange-yellow suspension, continue to stir 30min, until suspension is stirred into faint yellow emulsion, wherein indium salt: nickel salt: the mol ratio of metavanadate is 1:0 ~ 1:1, the molal quantity of nickel salt is not 0, preferably, indium salt: nickel salt: the mol ratio of metavanadate is 1:0 ~ 0.2:1, the molal quantity of nickel salt is not 0.
Solubility indium salt of the present invention is indium nitrate or inidum chloride, and described soluble nickel salt is nickel nitrate or nickel chloride, and described metavanadate is ammonium metavanadate or sodium metavanadate.
It is of the present invention that to be placed in reaction in microwave reactor be that prepared precursor liquid is moved into flask, be positioned in microwave reactor and stir, with 600 ~ 1000W power, 90 ~ 110 DEG C of heating using microwave 4 ~ 8h, in heating process, constant agitation speed is 2000rpm, obtained yellow product; Preferably, with 800W power 100 DEG C of heating using microwave 5h, in heating process, constant agitation speed is 2000rpm.
Centrifuge washing of the present invention drying are that obtained yellow product is taken out nature cooling, centrifugal after skimming supernatant liquor, after deionized water washs three times and after putting into vacuum drying chamber 50 ~ 80 DEG C oven dry and get final product.
The nickel doping vanadic acid indium (Ni-InVO that method disclosed according to the present invention is obtained
4) nano-crystalline photocatalysis agent, this catalyst is the nano-crystalline granule of about 20nm, and band-gap energy is 2 ~ 3.5eV.
The nickel doping vanadic acid indium (Ni-InVO obtained according to preparation method of the present invention
4) nano-crystalline photocatalysis agent, can be applicable to decomposition water under visible light.
Vanadic acid indium (the InVO of undoped nickel
4) synthetic method of nano-crystalline photocatalysis agent is shown in blank test in detailed description of the invention, so that as Experimental Comparison.
photocatalytic water activity experiment:
Carry out in CEL-SPH2N photocatalytic water system (purchased from Zhong Jiaojin source, Beijing Science and Technology Ltd.), radiation of visible light (500W xenon lamp, add 420nm optical filter), 200mL 0.5M liquor argenti nitratis ophthalmicus is added in reactor, then add 50 mg photochemical catalysts, magnetic agitation is in suspension or floating state, 30min sample analysis in interval in During Illumination to keep catalyst, with F2000 gas chromatograph to the concentration row test that produces oxygen, thus calculate the reaction rate of photodissociation aquatic products oxygen.
Nickel nitrate used in the present invention, nickel chloride, indium nitrate, inidum chloride, silver nitrate, ammonium metavanadate, it is pure that sodium metavanadate is analysis, is purchased from traditional Chinese medicines chemical reagent Co., Ltd.
beneficial effect
The present invention utilizes microwave heating method to synthesize nickel doping vanadic acid indium (Ni-InVO
4) nano-crystalline photocatalysis agent, by changing the Ni/In ratio in precursor liquid, achieve Ni-InVO
4nano-crystalline photocatalysis agent can be with and be carried out controllable adjustment.The present invention is simple to operation, one-step synthesis, is one Nano semiconductor In Researches On Modified Techniques of Photocatalysts very efficiently.Through introducing impurity energy level, obtained Ni-InVO
4nanocrystalline visible light activity greatly promotes compared with non-doped samples, has possessed the ability of decomposition water under visible light.
Accompanying drawing explanation
In Fig. 1, a is Ni-InVO
4nanocrystalline transmission electron microscope (TEM) figure,
B is Ni-InVO
4nanocrystalline high resolution TEM (HRTEM) figure.
Fig. 2 is different Ni-InVO
4the ultraviolet-visible absorption spectroscopy figure of nanocrystalline sample, in figure, the corresponding Ni/In of N0-N20 is than the Ni-InVO for 0-20%
4sample.
Fig. 3 is different Ni-InVO
4the direct energy band analysis figure of nanocrystalline sample, in figure, the corresponding Ni/In of N0-N20 is than the Ni-InVO for 0-20%
4sample.
Fig. 4 is obtained different Ni-InVO
4the light of nanocrystalline sample decomposes aquatic products oxygen figure, and in figure, the corresponding Ni/In of N0-N20 is than the Ni-InVO for 0-20%
4sample.
Fig. 5 is obtained different Ni-InVO
4the product oxygen RATES figure of nanocrystalline sample, in figure, the corresponding Ni/In of N0-N20 is than the Ni-InVO for 0-20%
4sample.
Detailed description of the invention
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
blank test
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution is added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) InVO
4the preparation of nano-crystalline photocatalysis agent (N0)
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain InVO
4nano-crystalline photocatalysis agent (N0).
(3) get sample in (2) to measure it by ultraviolet-visible absorption spectroscopy and can be with as 3.4eV.
(4) get sample in (2) in photocatalytic water test macro, carry out the test of visible photocatalysis aquatic products oxygen, recording this photochemical catalyst product oxygen speed is under visible light 237 μm of ol/h.
embodiment 1
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 0.1mL nickel nitrate (Ni/In=1%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent (N1).
(3) get sample in (2) to measure it by ultraviolet-visible absorption spectroscopy and can be with as 3.0eV.
(4) get sample in (2) in photocatalytic water test macro, carry out the test of visible photocatalysis aquatic products oxygen, recording this photochemical catalyst product oxygen speed is under visible light 394 μm of ol/h.
embodiment 2
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 0.3mL nickel nitrate (Ni/In=3%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent (N3).
(3) get sample in (2) to measure it by ultraviolet-visible absorption spectroscopy and can be with as 2.8eV.
(4) get sample in (2) in photocatalytic water test macro, carry out the test of visible photocatalysis aquatic products oxygen, recording this photochemical catalyst product oxygen speed is under visible light 274 μm of ol/h.
embodiment 3
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 0.5mL nickel nitrate (Ni/In=5%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent (N5).
(3) get sample in (2) to measure it by ultraviolet-visible absorption spectroscopy and can be with as 2.7eV.
(4) get sample in (2) in photocatalytic water test macro, carry out the test of visible photocatalysis aquatic products oxygen, recording this photochemical catalyst product oxygen speed is under visible light 272 μm of ol/h.
embodiment 4
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 1mL nickel nitrate (Ni/In=10%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent (N10).
(3) get sample in (2) to measure it by ultraviolet-visible absorption spectroscopy and can be with as 2.6eV.
(4) get sample in (2) in photocatalytic water test macro, carry out the test of visible photocatalysis aquatic products oxygen, recording this photochemical catalyst product oxygen speed is under visible light 293 μm of ol/h.
embodiment 5
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 2mL nickel nitrate (Ni/In=20%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent (N20).
(3) get sample in (2) to measure it by ultraviolet-visible absorption spectroscopy and can be with as 2.5eV.
(4) get sample in (2) in photocatalytic water test macro, carry out the test of visible photocatalysis aquatic products oxygen, recording this photochemical catalyst product oxygen speed is under visible light 282 μm of ol/h.
Shown in comprehensive above data and accompanying drawing 4 and accompanying drawing 5, can find, the adulterate product oxygen speed of vanadic acid nanocrystal In photochemical catalyst (N1) of 1% nickel is the highest, reaches 394 μm of ol/h, improve 66% compared with unadulterated vanadic acid nanocrystal In (N0).Along with nickel addition is increased to 20% gradually from 1%, produce oxygen speed and reduce gradually, but all the time higher than unadulterated vanadic acid nanocrystal In.
embodiment 6
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 0.3mL nickel nitrate (Ni/In=3%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 4 hours at constant 90 DEG C of 600W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent.
embodiment 7
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 0.5mL nickel nitrate (Ni/In=5%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 8 hours at constant 110 DEG C of 1000W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent.
embodiment 8
(1) preparation of precursor liquid
By indium nitrate (In (NO
3)
3 .4.5H
2o) with nickel nitrate (Ni (NO
3)
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indium nitrate solution and 0.7mL nickel nitrate (Ni/In=7%) are added after in 100mL deionized water, under stirring, 0.117g (1mmol) ammonium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 9 hours at constant 100 DEG C of 1000W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent.
embodiment 9
(1) preparation of precursor liquid
By inidum chloride (InCl
3or InCl
3 .4H
2o) with nickel chloride (NiCl
2or NiCl
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indiumchloride solution and 1mL nickel chloride (Ni/In=10%) are added after in 100mL deionized water, under stirring, 0.121g (1mmol) sodium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 100 DEG C of 800W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent.
embodiment 10
(1) preparation of precursor liquid
By inidum chloride (InCl
3or InCl
3 .4H
2o) with nickel chloride (NiCl
2or NiCl
2 .6H
2o) the 100mmol/L aqueous solution is mixed with respectively.10mL indiumchloride solution and 0.2mL nickel chloride (Ni/In=2%) are added after in 100mL deionized water, under stirring, 0.121g (1mmol) sodium metavanadate solid is added in above-mentioned mixed liquor, with dust technology, pH value is adjusted between 2-3, forms orange-yellow suspension.Continue stirring 30 minutes, until after suspension is stirred into faint yellow emulsion, namely obtain the precursor liquid of microwave reaction.
(2) Ni-InVO
4the preparation of nano-crystalline photocatalysis agent
Moved in 250mL there-necked flask by microwave reaction precursor liquid, be positioned in microwave reactor (the auspicious dove board in Beijing), with the heating using microwave 5 hours at constant 110 DEG C of 600W power, in heating process, constant agitation speed is 2000rpm.After having heated, yellow product is taken out nature cooling, centrifugal after cooled solution is skimmed supernatant liquor, wash and put into vacuum drying chamber and dry, obtain Ni-InVO
4nano-crystalline photocatalysis agent.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or the conversion of equivalent flow process, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (8)
1. a method for microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst, comprises preparation precursor liquid, is then placed in reaction in microwave reactor, and forms through centrifuge washing drying, it is characterized in that:
Described preparation precursor liquid, that solubility indium salt and nickel salt are dissolved into the aqueous solution respectively, measure indium salt and nickel salt aqueous solution in deionized water, under agitation add metavanadate solid particle, with dust technology, pH value is adjusted between 2 ~ 3, form orange-yellow suspension, continue to stir 30min, until suspension is stirred into faint yellow emulsion, wherein indium salt: nickel salt: the mol ratio of metavanadate is 1:0 ~ 1:1, the molal quantity of nickel salt is not 0;
The described reaction in microwave reactor that is placed in is that prepared precursor liquid is moved into flask, be positioned in microwave reactor and stir, with 600 ~ 1000W power, 90 ~ 110 DEG C of heating using microwave 4 ~ 8h, in heating process, constant agitation speed is 2000rpm, obtained yellow product;
Described centrifuge washing drying is that yellow product that will be obtained takes out nature cooling, centrifugal after skimming supernatant liquor, puts into vacuum drying chamber 50 ~ 80 DEG C oven dry after deionized water washs three times.
2. the method for microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst according to claim 1, is characterized in that, participate in the indium salt of reaction: nickel salt: the mol ratio of metavanadate is 1:0 ~ 0.2:1, the molal quantity of nickel salt is not 0.
3. the method for microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst according to claim 1, it is characterized in that, described solubility indium salt is indium nitrate or inidum chloride, described soluble nickel salt is nickel nitrate or nickel chloride, and described metavanadate is ammonium metavanadate or sodium metavanadate.
4. the method for microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst according to claim 2, it is characterized in that, described solubility indium salt is indium nitrate or inidum chloride, described soluble nickel salt is nickel nitrate or nickel chloride, and described metavanadate is ammonium metavanadate or sodium metavanadate.
5. the method for the microwave heating method synthesis nickel doping vanadic acid nanocrystal In photochemical catalyst according to aforementioned arbitrary claim, it is characterized in that, the described reaction in microwave reactor that is placed in is that prepared precursor liquid is moved into flask, be positioned in microwave reactor and stir, with 800W power 100 DEG C of heating using microwave 5h, in heating process, constant agitation speed is 2000rpm, obtained yellow product.
6. the nickel doping vanadic acid nanocrystal In photochemical catalyst that the method that the microwave heating method synthesis nickel described in aforementioned arbitrary claim adulterates vanadic acid nanocrystal In photochemical catalyst prepares.
7. nickel doping vanadic acid nanocrystal In photochemical catalyst according to claim 6, it is characterized in that, described catalyst is the nano-crystalline granule of 20nm, and band-gap energy is 2 ~ 3.5eV.
8. the nickel doping vanadic acid nanocrystal In photochemical catalyst according to claim 6 or 7, is characterized in that, can be applicable to decomposition water under visible light.
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| CN107376960A (en) * | 2017-07-11 | 2017-11-24 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of nickel doping phosphoric acid indium photochemical catalyst |
| CN107252698A (en) * | 2017-07-11 | 2017-10-17 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of Copper-cladding Aluminum Bar indium phosphate photochemical catalyst |
| CN107262125A (en) * | 2017-07-11 | 2017-10-20 | 柳州若思纳米材料科技有限公司 | A kind of preparation method of Ag doping indium phosphate photochemical catalyst |
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| CN1845342A (en) * | 2006-04-30 | 2006-10-11 | 南京大学 | Solar cell and its preparing method |
| US7682594B2 (en) * | 2006-06-21 | 2010-03-23 | National Central University | Method for producing photocatalyst |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1845342A (en) * | 2006-04-30 | 2006-10-11 | 南京大学 | Solar cell and its preparing method |
| US7682594B2 (en) * | 2006-06-21 | 2010-03-23 | National Central University | Method for producing photocatalyst |
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| Yan Yan,et al.InVO4 nanocrystal photocatalysts: Microwave-assisted synthesis and size-dependent activities of hydrogen production from water splitting under visible light.《Chemical Engineering Journal》.2013,第233卷第1-7页. * |
| Zhigang Zou,et al.Direct splitting of water under visible light irradiation with an oxide semiconductor photocatalyst.《NATURE》.2001,第414卷第625-627页. * |
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