CN103878010B - VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst - Google Patents

VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst Download PDF

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CN103878010B
CN103878010B CN201410150483.3A CN201410150483A CN103878010B CN 103878010 B CN103878010 B CN 103878010B CN 201410150483 A CN201410150483 A CN 201410150483A CN 103878010 B CN103878010 B CN 103878010B
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mixing
mischcrystal photocatalyst
race metal
metal ion
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CN103878010A (en
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陈刚
周彦松
于麒麟
赵丽宸
何强
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Harbin Institute of Technology
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Abstract

VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, the present invention relates to VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst.The present invention utilizes decomposing water with solar energy to produce the low problem of oxygen performance to solve photochemical catalyst under visible ray, and preparation method is: one, by Ga 2o 3with ZnO mixing, add the compound of VB race metal after mixing, then grind under being placed in agate mortar room temperature; Two, by the presoma high-temperature calcination in ammonia atmosphere after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, be cooled to room temperature, through deionized water and absolute ethanol washing, namely complete.Preparation method of the present invention is easy and simple to handle, and obtained catalysis material product oxygen activity comparatively substance system has significantly high, improves solar energy transformation efficiency.The present invention is applied to the field of photocatalytic material in functional material.

Description

VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst
Technical field
The present invention relates to VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst.
Background technology
The deterioration of the energy and environmental problem, makes clean, the efficient new forms of energy of exploitation very urgent.H 2fuel value is high, and odorless is nontoxic, and combustion product is pollution-free, and renewable, is the new forms of energy having bright prospects.Traditional hydrogen production process is by brine electrolysis, and this method energy consumption is large, and there is transportation safety hidden danger.And utilizing solar energy photocatalytic hydrogen production by water decomposition, energy density is low, dispersed strong solar energy is converted into Hydrogen Energy, then by H that fuel cell will generate 2and O 2carry out electrochemical reaction, produce electric energy, its product water can be used as again the raw material of solar hydrogen making, and can not produce any pollution to environment, can form eucyclic energy system.Therefore, utilize solar energy photocatalytic hydrogen production by water decomposition to be called as and be referred to as " technology of 21 century dream ", receive extensively deep research.
TiO is found from early 1970s Japanese Scientists Fujishaima and Honda 2after photoelectrolysis aquatic products hydrogen phenomenon on electrode, the research of photocatalytic hydrogen production by water decomposition becomes the focus paid close attention in the whole world gradually.Current most of catalyst still can only respond ultraviolet light, and exploitation has the research emphasis that the photochemical catalyst decomposing pure water performance is this field always under visible light.Nearly ten years, the Domen seminar of Japan have studied and a series ofly has visible light-responded nitrogen oxide photochemical catalyst, wherein (Ga 1-xzn x) (N 1-xo x) mischcrystal photocatalyst shows excellent photocatalysis Decomposition pure water performance under visible light illumination, but its catalytic efficiency is also still lower, still has very large gap according to practical application.At present, researcher mainly studies about (Ga 1-xzn x) (N 1-xo x) mischcrystal photocatalyst finishing, and VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation of mischcrystal photocatalyst has no report.
Summary of the invention
The object of the invention is to utilize decomposing water with solar energy to produce the low problem of oxygen performance to solve photochemical catalyst under visible ray, providing VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst.
VB race metal ion mixing (Ga of the present invention 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be carry out according to the following steps: one, by Ga 2o 3with ZnO mixing, add the compound of VB race metal after mixing, then grind under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, the presoma after grinding is calcined in ammonia atmosphere, then take out be cooled to 100 DEG C under ammonia atmosphere after, be then cooled to room temperature, then obtain VB race metal ion mixing (Ga through deionized water and absolute ethanol washing 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be 1:(0.8 ~ 1.1 with the mol ratio of Ga element and Zn element in ZnO), the summation of Ga element and Zn element and the mol ratio of VB race metallic element are 1:(0.01 ~ 0.1).
The present invention is with Ga 2o 3, ZnO and VB race metal compound be raw material, adopt high-temperature ammonolysis legal system for the (Ga of visible light-responded VB race metal ion mixing first 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, easy and simple to handle, obtained catalysis material product oxygen activity comparatively substance system has significantly high, improves solar energy transformation efficiency.The present invention is after doping Ta compared with non-doped samples, and the performance that doping Ta produces oxygen with rear catalyst photochemical catalyzing is improved, and when 3%Ta doping, performance reaches the highest.
Accompanying drawing explanation
Fig. 1 is the (Ga of 3%Ta doping prepared by test 1 1-xzn x) (N 1-xo x) the XRD collection of illustrative plates of mischcrystal photocatalyst, wherein a is the (Ga of Ta of undoping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, b is the (Ga of 3%Ta doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst;
Fig. 2 is the (Ga of 3%Ta doping prepared by test 1 1-xzn x) (N 1-xo x) the SEM collection of illustrative plates of mischcrystal photocatalyst;
Fig. 3 is the (Ga of 3%Ta doping prepared by test 1 1-xzn x) (N 1-xo x) mischcrystal photocatalyst UV-VIS collection of illustrative plates, wherein a is the (Ga of Ta of undoping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, b is the (Ga of 3%Ta doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst;
Fig. 4 is the (Ga of 3%Ta doping prepared by test 1 1-xzn x) (N 1-xo x) resolution chart of mischcrystal photocatalyst oxygen performance.
Detailed description of the invention
Detailed description of the invention one: present embodiment VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be carry out according to the following steps: one, by Ga 2o 3with ZnO mixing, add the compound of VB race metal after mixing, then grind under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, the presoma after grinding is calcined in ammonia atmosphere, then take out be cooled to 100 DEG C under ammonia atmosphere after, be then cooled to room temperature, then obtain VB race metal ion mixing (Ga through deionized water and absolute ethanol washing 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be 1:(0.8 ~ 1.1 with the mol ratio of Ga element and Zn element in ZnO), the summation of Ga element and Zn element and the mol ratio of VB race metallic element are 1:(0.01 ~ 0.1).
Present embodiment is with Ga 2o 3, ZnO and VB race metal compound be raw material, adopt high-temperature ammonolysis legal system for the (Ga of visible light-responded VB race metal ion mixing doping first 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, easy and simple to handle, obtained catalysis material product oxygen activity comparatively substance system has significantly high, improves solar energy transformation efficiency.Present embodiment is after doping Ta compared with non-doped samples, and the performance that doping Ta produces oxygen with rear catalyst photochemical catalyzing is improved, and when 3%Ta doping, performance reaches the highest.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: the compound of the VB race metal described in step one is the oxide of VB race metal or the nitrate of VB race metal.Other are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two unlike: the time of grinding described in step one is 30 ~ 60min.Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: the temperature of the calcining described in step 2 is 750 ~ 900 DEG C.Other are identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: the time of the calcining described in step 2 is 10 ~ 30h.Other are identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: the flow velocity of the ammonia described in step 2 is 100 ~ 150mL/min.Other are identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six unlike: the deionized water described in step 2 and absolute ethanol washing are that deionized water washs 2 times, absolute ethanol washing 1 time.Other are identical with one of detailed description of the invention one to six.
By following verification experimental verification beneficial effect of the present invention:
Test 1, this test VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be carry out according to the following steps: one, by Ga 2o 3with ZnO mixing, after mixing, add Ta 2o 5, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtain (the Ga of 3%Ta doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be the summation of 1:1, Ga element and Zn element and the mol ratio of Ta element with the mol ratio of Ga element and Zn element in ZnO be 1:0.03, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
(the Ga of the 3%Ta doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst with undope (the Ga of Ta 1-xzn x) (N 1-xo x) mischcrystal photocatalyst XRD collection of illustrative plates as shown in Figure 1, as shown in Figure 1, Ta adulterates with rear catalyst still for hexagonal structure, but sample XRD diffraction maximum reduces after doping, degree of crystallinity declines, diffraction maximum is as the skew of wide-angle direction simultaneously, and this illustrates that Ta doping makes catalyst tie the degree of disorder and increases, and the distortion of lattice occurred to a certain degree causes.
(the Ga of the 3%Ta doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst SEM collection of illustrative plates as shown in Figure 2, the catalyst of Ta doping is as shown in Figure 2 hollow polyhedron pattern, and make catalyst have large specific area to participate in catalytic reaction, catalyst activity is improved.
(the Ga of the 3%Ta doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst with undope (the Ga of Ta 1-xzn x) (N 1-xo x) mischcrystal photocatalyst UV-VIS collection of illustrative plates as shown in Figure 3, as shown in Figure 3, compared with unadulterated catalyst, Ta doping catalyst adsorb limit freeed red shift, add catalyst to the absorption of visible ray and utilization.
To (the Ga of the 3%Ta doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst with undope (the Ga of Ta 1-xzn x) (N 1-xo x)) mischcrystal photocatalyst, 1%Ta doping (Ga 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, 2%Ta doping (Ga 1-xzn x) (N 1-xo x)) mischcrystal photocatalyst, 4%Ta doping (Ga 1-xzn x) (N 1-xo x)) the oxygen performance of mischcrystal photocatalyst tests, as shown in Figure 4, as shown in Figure 4 compared with non-doped samples, the performance that doping Ta produces oxygen with rear catalyst photochemical catalyzing is improved result, and when 3%Ta doping, performance reaches the highest.
Wherein (the Ga of 1%Ta doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, 2%Ta doping (Ga 1-xzn x) (N 1-xo x) mischcrystal photocatalyst and 4%Ta doping (Ga 1-xzn x) (N 1-xo x) (the Ga that adulterates of the preparation method of mischcrystal photocatalyst and 3%Ta 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst is identical.
(Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be carry out according to the following steps: one, by Ga 2o 3with ZnO mixing, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtains (Ga 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be 1:1 with the mol ratio of Ga element and Zn element in ZnO, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
Test 2, this test VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be carry out according to the following steps: one, by Ga 2o 3with ZnO mixing, after mixing, add V 2o 5, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtain (the Ga of 3%V doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be the summation of 1:1, Ga element and Zn element and the mol ratio of V element with the mol ratio of Ga element and Zn element in ZnO be 1:0.03, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
To (the Ga of the 3%V doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst with undope (the Ga of V 1-xzn x) (N 1-xo x)) the oxygen performance of mischcrystal photocatalyst tests, compared with non-doped samples, the performance that doping V produces oxygen with rear catalyst photochemical catalyzing is improved, and when 3%V doping, performance reaches the highest.
Test 3, this test VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be carry out according to the following steps: one, by Ga 2o 3with ZnO mixing, after mixing, add Nb 2o 5, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtain (the Ga of 6%Nb doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be the summation of 1:1, Ga element and Zn element and the mol ratio of Nb element with the mol ratio of Ga element and Zn element in ZnO be 1:0.06, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
To (the Ga of the 6%Nb doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst with undope (the Ga of Nb 1-xzn x) (N 1-xo x) the oxygen performance of mischcrystal photocatalyst tests, compared with non-doped samples, the performance that doping Nb produces oxygen with rear catalyst photochemical catalyzing is improved, and when 6%Nb doping, performance reaches the highest.
It can thus be appreciated that, (the Ga of the VB race metal ion mixing doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, easy and simple to handle, obtained catalysis material decomposition aquatic products oxygen activity comparatively substance system has significantly high, improves solar energy transformation efficiency.

Claims (3)

1.VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst carries out according to the following steps: one, by Ga 2o 3with ZnO mixing, after mixing, add Ta 2o 5, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtain (the Ga of 3%Ta doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be the summation of 1:1, Ga element and Zn element and the mol ratio of Ta element with the mol ratio of Ga element and Zn element in ZnO be 1:0.03, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
2.VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst carries out according to the following steps: one, by Ga 2o 3with ZnO mixing, after mixing, add V 2o 5, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtain (the Ga of 3%V doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be the summation of 1:1, Ga element and Zn element and the mol ratio of V element with the mol ratio of Ga element and Zn element in ZnO be 1:0.03, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
3.VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that VB race metal ion mixing (Ga 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst carries out according to the following steps: one, by Ga 2o 3with ZnO mixing, after mixing, add Nb 2o 5, then grind 30min under being placed in agate mortar room temperature, obtain the presoma after grinding; Two, by the 850 DEG C of calcining 15h in ammonia atmosphere of the presoma after grinding, then take out be cooled to 100 DEG C under ammonia atmosphere after, then be cooled to room temperature, then wash 2 times through deionized water, absolute ethanol washing 1 time, obtain (the Ga of 6%Nb doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, namely complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3be the summation of 1:1, Ga element and Zn element and the mol ratio of Nb element with the mol ratio of Ga element and Zn element in ZnO be 1:0.06, the flow velocity of the ammonia in step 2 is 100 ~ 150mL/min.
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