CN103878010A - Preparation method of VB-group metal ion doped (Ga<1-x>Znx)(N<1-x>Ox) solid solution photocatalyst - Google Patents

Preparation method of VB-group metal ion doped (Ga<1-x>Znx)(N<1-x>Ox) solid solution photocatalyst Download PDF

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CN103878010A
CN103878010A CN201410150483.3A CN201410150483A CN103878010A CN 103878010 A CN103878010 A CN 103878010A CN 201410150483 A CN201410150483 A CN 201410150483A CN 103878010 A CN103878010 A CN 103878010A
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metal ion
photocatalyst
mischcrystal photocatalyst
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CN103878010B (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

The invention relates to a preparation method of VB-group metal ion doped (Ga<1-x>Znx)(N<1-x>Ox) solid solution photocatalyst. The invention relates to a preparation method of VB-group metal ion doped (Ga<1-x>Znx) (N<1-x>Ox) solid solution photocatalyst, which solves the problems that the performance of the photocatalyst for decomposing water to generate oxygen by utilizing the solar under the visible light is low. The preparation method comprises the following steps of I. mixing Ga2O3 and ZnO, adding a compound of VB-group metal, arranging the mixture into an agate mortar, and grinding the mixture under the room temperature; II. calcining the ground precursor in an ammonia gas atmosphere, cooling the precursor in the ammonia gas atmosphere to the temperature of 100 DEG C, taking out, cooling the precursor to the room temperature, and washing the precursor by utilizing deionized water and anhydrous ethanol. The preparation method is simple in operation, the activity of the oxygen generation of the prepared photocatalsyt material is greatly improved compared with that of the original system, and the conversion efficiency of the solar energy is improved. The preparation method is applicable to the field of the photocatalyst material in a functional material.

Description

Metal ion mixing (the Ga of VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst
Technical field
The present invention relates to the metal ion mixing (Ga of VB family 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 that have bright prospects.Traditional hydrogen production process is by brine electrolysis, and this method energy consumption is large, and has transportation safety hidden danger.And utilize solar energy photocatalytic hydrogen production by water decomposition, low energy density, dispersed strong solar energy is converted into Hydrogen Energy, then by fuel cell by the H generating 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 known as " technology of 21 century dream ", be subject to extensive deep research.
Find TiO from early 1970s Japan scientist Fujishaima and Honda 2after photoelectrolysis aquatic products hydrogen phenomenon on electrode, the research of photocatalytic hydrogen production by water decomposition becomes the focus that the whole world is paid close attention to gradually.Most catalyst still can only respond ultraviolet light, and the photochemical catalyst that exploitation has decomposition pure water performance under visible ray is the research emphasis in this field always.Nearly ten years, a series of have visible light-responded nitrogen oxide photochemical catalyst, wherein (Ga have studied in the Domen seminar of Japan 1-xzn x) (N 1-xo x) mischcrystal photocatalyst has shown excellent photocatalysis Decomposition pure water performance under radiation of visible light, 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 the metal ion mixing (Ga of VB family 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 in order to solve photochemical catalyst under visible ray, the metal ion mixing (Ga of VB family is provided 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst.
VB metal ion mixing (the Ga of family of the present invention 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be to carry out according to the following steps: one, by Ga 2o 3mix with ZnO, after mixing, add the compound of VB family metal, then be placed under agate mortar room temperature and grind, obtain the presoma after grinding; Two, the presoma after grinding is calcined in ammonia atmosphere, then taken out be cooled to 100 DEG C under ammonia atmosphere after, be then cooled to room temperature, then obtain the metal ion mixing (Ga of VB family through deionized water and absolute ethanol washing 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:(0.8～1.1), the mol ratio of the summation of Ga element and Zn element and VB family metallic element is 1:(0.01～0.1).
The present invention is with Ga 2o 3, ZnO and VB family metal compound be raw material, adopt first (the Ga of high-temperature ammonolysis legal system for visible light-responded VB family metal ion mixing 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, easy and simple to handle, the more former system of catalysis material product oxygen activity making has significantly high, has improved solar energy transformation efficiency.The present invention is after doping Ta compared with doped samples not, and the performance that doping Ta produces oxygen with rear catalyst photochemical catalyzing is improved, and in the time of 3%Ta doping, performance has reached the highest.
Brief description of the drawings
Fig. 1 is the (Ga of the 3%Ta doping of test 1 preparation 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 the 3%Ta doping of test 1 preparation 1-xzn x) (N 1-xo x) the SEM collection of illustrative plates of mischcrystal photocatalyst;
Fig. 3 is the (Ga of the 3%Ta doping of test 1 preparation 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 the 3%Ta doping of test 1 preparation 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: the metal ion mixing (Ga of present embodiment VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be to carry out according to the following steps: one, by Ga 2o 3mix with ZnO, after mixing, add the compound of VB family metal, then be placed under agate mortar room temperature and grind, obtain the presoma after grinding; Two, the presoma after grinding is calcined in ammonia atmosphere, then taken out be cooled to 100 DEG C under ammonia atmosphere after, be then cooled to room temperature, then obtain the metal ion mixing (Ga of VB family through deionized water and absolute ethanol washing 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:(0.8～1.1), the mol ratio of the summation of Ga element and Zn element and VB family metallic element is 1:(0.01～0.1).
Present embodiment is with Ga 2o 3, ZnO and VB family metal compound be raw material, adopt first (the Ga of high-temperature ammonolysis legal system for visible light-responded VB family metal ion mixing doping 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, easy and simple to handle, the more former system of catalysis material product oxygen activity making has significantly high, has improved solar energy transformation efficiency.Present embodiment is after doping Ta compared with doped samples not, and the performance that doping Ta produces oxygen with rear catalyst photochemical catalyzing is improved, and in the time of 3%Ta doping, performance has reached the highest.
Detailed description of the invention two: present embodiment is different from detailed description of the invention one: the compound of the VB family metal described in step 1 is the oxide of VB family metal or the nitrate of VB family metal.Other are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment is different from detailed description of the invention one or two: the time of grinding described in step 1 is 30～60min.Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment is different from one of detailed description of the invention one to three: 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: present embodiment is different from one of detailed description of the invention one to four: 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: present embodiment is different from one of detailed description of the invention one to five: 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: present embodiment is different from one of detailed description of the invention one to six: the deionized water described in step 2 and absolute ethanol washing are deionized water washing 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, the metal ion mixing (Ga of this test VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be to carry out according to the following steps: one, by Ga 2o 3mix with ZnO, after mixing, add Ta 2o 5, then be placed under agate mortar room temperature and grind 30min, 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 through deionized water washing 2 times, absolute ethanol washing 1 time, obtains (the Ga that 3%Ta adulterates 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:1, the summation of Ga element and Zn element and the mol ratio of Ta element are 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 taking rear catalyst still as hexagonal structure, but after doping, sample XRD diffraction maximum reduces, degree of crystallinity declines, diffraction maximum is as the skew of wide-angle direction simultaneously, and this explanation Ta doping increases the catalyst knot degree of disorder, and the distortion of lattice occurring 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 hollow polyhedron pattern as shown in Figure 2, makes 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, the catalyst ABSORPTION EDGE of Ta doping has been freeed red shift, has increased absorption and the utilization of catalyst to visible ray.
(the Ga of the 3%Ta doping to 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)) (Ga of mischcrystal photocatalyst, 1%Ta doping 1-xzn x) (N 1-xo x) (the Ga of mischcrystal photocatalyst, 2%Ta doping 1-xzn x) (N 1-xo x)) (Ga of mischcrystal photocatalyst, 4%Ta doping 1-xzn x) (N 1-xo x)) the oxygen performance of mischcrystal photocatalyst tests, as shown in Figure 4, compared with doped samples not, the performance that doping Ta produces oxygen with rear catalyst photochemical catalyzing is improved result as shown in Figure 4, and in the time of 3%Ta doping, performance has reached the highest.
Wherein (the Ga of 1%Ta doping 1-xzn x) (N 1-xo x) (the Ga of mischcrystal photocatalyst, 2%Ta doping 1-xzn x) (N 1-xo x) (the Ga of mischcrystal photocatalyst and 4%Ta doping 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst and the (Ga of 3%Ta doping 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 to carry out according to the following steps: one, by Ga 2o 3mix with ZnO, then be placed under agate mortar room temperature and grind 30min, 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, through deionized water washing 2 times, absolute ethanol washing 1 time, obtains (Ga 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:1, the flow velocity of the ammonia in step 2 is 100～150mL/min.
Test 2, the metal ion mixing (Ga of this test VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be to carry out according to the following steps: one, by Ga 2o 3mix with ZnO, after mixing, add V 2o 5, then be placed under agate mortar room temperature and grind 30min, 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 through deionized water washing 2 times, absolute ethanol washing 1 time, obtains (the Ga that 3%V adulterates 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:1, Ga element and the summation of Zn element and the mol ratio of V element are 1:0.03, the flow velocity of the ammonia in step 2 is 100～150mL/min.
(the Ga of the 3%V doping to 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 doped samples not, the performance that doping V produces oxygen with rear catalyst photochemical catalyzing is improved, and in the time of 3%V doping, performance has reached the highest.
Test 3, the metal ion mixing (Ga of this test VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, be to carry out according to the following steps: one, by Ga 2o 3mix with ZnO, after mixing, add Nb 2o 5, then be placed under agate mortar room temperature and grind 30min, 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 through deionized water washing 2 times, absolute ethanol washing 1 time, obtains (the Ga that 6%Nb adulterates 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:1, the summation of Ga element and Zn element and the mol ratio of Nb element are 1:0.06, the flow velocity of the ammonia in step 2 is 100～150mL/min.
(the Ga of the 6%Nb doping to 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 doped samples not, the performance that doping Nb produces oxygen with rear catalyst photochemical catalyzing is improved, and in the time of 6%Nb doping, performance has reached the highest.
Hence one can see that, (the Ga of the VB family metal ion mixing doping of this test preparation 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, easy and simple to handle, the more former system of catalysis material decomposition aquatic products oxygen activity making has significantly high, has improved solar energy transformation efficiency.

Claims (7)

  1. Metal ion mixing (the Ga of 1.VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that the metal ion mixing (Ga of VB family 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst carries out according to the following steps: one, by Ga 2o 3mix with ZnO, after mixing, add the compound of VB family metal, then be placed under agate mortar room temperature and grind, obtain the presoma after grinding; Two, the presoma after grinding is calcined in ammonia atmosphere, then taken out be cooled to 100 DEG C under ammonia atmosphere after, be then cooled to room temperature, then obtain the metal ion mixing (Ga of VB family through deionized water and absolute ethanol washing 1-xzn x) (N 1-xo x) mischcrystal photocatalyst, complete; Wherein (Ga 1-xzn x) (N 1-xo x) in x be 0<x<1, Ga 2o 3with the mol ratio of Ga element in ZnO and Zn element be 1:(0.8～1.1), Ga element and Zn element total mole is 1:(0.01～0.1 with the mol ratio of VB family metallic element).
  2. 2. the VB metal ion mixing (Ga of family according to claim 1 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that the compound of the VB family metal described in step 1 is the oxide of VB family metal or the nitrate of VB family metal.
  3. 3. the VB metal ion mixing (Ga of family according to claim 1 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that the time of grinding described in step 1 is 30～60min.
  4. 4. the VB metal ion mixing (Ga of family according to claim 1 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that the temperature of the calcining described in step 2 is 750～900 DEG C.
  5. 5. the VB metal ion mixing (Ga of family according to claim 1 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that the time of the calcining described in step 2 is 10～30h.
  6. 6. the VB metal ion mixing (Ga of family according to claim 1 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that the flow velocity of the ammonia described in step 2 is 100～150mL/min.
  7. 7. the VB metal ion mixing (Ga of family according to claim 1 1-xzn x) (N 1-xo x) preparation method of mischcrystal photocatalyst, it is characterized in that deionized water described in step 2 and absolute ethanol washing for first with deionized water washing 2 times, then use absolute ethanol washing 1 time.
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CN108342775A (en) * 2017-01-25 2018-07-31 中国科学院上海光学精密机械研究所 A kind of tantalum doping beta-oxidation gallium crystalline material and its preparation method and application
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CN108531989A (en) * 2017-03-03 2018-09-14 中国科学院上海光学精密机械研究所 Adulterate gallium oxide crystal and preparation method thereof

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CN108342775A (en) * 2017-01-25 2018-07-31 中国科学院上海光学精密机械研究所 A kind of tantalum doping beta-oxidation gallium crystalline material and its preparation method and application
WO2018137673A1 (en) * 2017-01-25 2018-08-02 中国科学院上海光学精密机械研究所 Gallium oxide-doped crystalline material, preparation method and application thereof
CN110325671A (en) * 2017-01-25 2019-10-11 中国科学院上海光学精密机械研究所 Adulterate gallium oxide crystalline material and its preparation method and application
KR20200002789A (en) * 2017-01-25 2020-01-08 상하이 인스티튜트 오브 옵틱스 앤 파인 메카닉스, 차이니즈 아카데미 오브 사이언시스 Doped Gallium Oxide Crystalline Material and Method of Making and Application thereof
US11098416B2 (en) 2017-01-25 2021-08-24 Shanghai Institute Of Optics And Fine Mechanics, Chinese Academy Of Sciences Doped gallium oxide crystalline material and preparation method and application thereof
KR102414621B1 (en) 2017-01-25 2022-06-30 상하이 인스티튜트 오브 옵틱스 앤 파인 메카닉스, 차이니즈 아카데미 오브 사이언시스 Doped gallium oxide crystalline material and its manufacturing method and application
CN108342775B (en) * 2017-01-25 2024-04-12 中国科学院上海光学精密机械研究所 Tantalum-doped beta gallium oxide crystalline material and preparation method and application thereof
CN108531989A (en) * 2017-03-03 2018-09-14 中国科学院上海光学精密机械研究所 Adulterate gallium oxide crystal and preparation method thereof

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