CN103447062A - Preparing method and application of lanthanum-doped gallium zinc nitrogen oxygen solid solution photocatalyst - Google Patents
Preparing method and application of lanthanum-doped gallium zinc nitrogen oxygen solid solution photocatalyst Download PDFInfo
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- CN103447062A CN103447062A CN201310459632XA CN201310459632A CN103447062A CN 103447062 A CN103447062 A CN 103447062A CN 201310459632X A CN201310459632X A CN 201310459632XA CN 201310459632 A CN201310459632 A CN 201310459632A CN 103447062 A CN103447062 A CN 103447062A
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Abstract
The invention discloses a preparing method and application of a lanthanum-doped gallium zinc nitrogen oxygen solid solution photocatalyst, and relates to a preparing method and application of a photocatalyst. The problem that in the prior art, a prepared solid solution photocatalyst for water decomposition oxygen generation is low in water decomposition performance, and visible-light response range is narrow is solved. The preparing method comprises the steps that compounds of Ga2O3, ZnO and La are weighed and placed in an agate mortar for grinding; then high-temperature calcination is carried out for a period of time in ammonia gas atmosphere; the compounds are cooled to a certain temperature in ammonia gas atmosphere and taken out, and finally the lanthanum-doped gallium zinc nitrogen oxygen solid solution photocatalyst is obtained. The lanthanum-doped gallium zinc nitrogen oxygen solid solution photocatalyst is used for water decomposition oxygen generation. When the lanthanum-doped gallium zinc nitrogen oxygen solid solution photocatalyst is used for water decomposition oxygen generation, oxygen yield is high, and water decomposition oxygen generation performance is high.
Description
Technical field
The present invention relates to a kind of preparation method and application of photochemical catalyst.
Background technology
Along with becoming increasingly conspicuous of the aggravation of contradictions between the energy demand of limited fossil fuel and mankind's sharp increase and environmental problem, exploitation is clean, new forms of energy are very urgent efficiently.H
2fuel value is high, and odorless is nontoxic, and combustion product is pollution-free, is a kind of regenerative resource.H
2can directly the act as a fuel fuel of battery, for electric motor car provides power, solve current tail gas pollution problem, also Hydrogen Energy can be converted into to electric energy, for the electrical appliance power supply, is the new forms of energy that have broad prospect of application.Utilize the solar energy photocatalytic hydrogen production by water decomposition, energy density is low, dispersed strong solar energy is converted into Hydrogen Energy, then by fuel cell by the H generated
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 the solar energy photocatalytic hydrogen production by water decomposition to be known as " technology of 21 century dream ", received concern extensively and profoundly.
After photoelectrolysis aquatic products hydrogen phenomenon on early 1970s Japan scientist Fujishaima and Honda discovery TiO2 electrode, the research of photocatalytic hydrogen production by water decomposition becomes the focus that the whole world is paid close attention to gradually.1985, the people such as Kakuta found that, under visible ray, non-loaded ZnS-CdS mischcrystal photocatalyst and Pt/CdS catalyzing manufacturing of hydrogen activity are basic identical.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 shown excellent photocatalysis Decomposition pure water performance under radiation of visible light.When adopting the addition agent modified (Ga of Rh-Cr mixed oxide
1-xzn
x) (N
1-xo
x) time, the photocatalytic activity of this solid solution catalyst significantly improves, and in the average quantum efficiency of 420-440nm, reaches 5.9%.The researcher utilizes conventional method to Ga
2o
3carry out the synthetic gallium zinc nitrogen oxygen solid solution photochemical catalyst of high-temperature ammonolysis method with ZnO.But its still exist the decomposition water performance low, to the problem of visible light-responded narrow range.
Summary of the invention
The present invention be to solve the mischcrystal photocatalyst decomposition water performance of carrying out the water decomposition oxygen prepared by prior art low, to the problem of visible light-responded narrow range, and provide a kind of preparation method and application of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst.
The preparation method of a kind of lanthanum doped gallium of the present invention zinc nitrogen oxygen solid solution photochemical catalyst, carry out according to the following steps:
One, take Ga
2o
3, ZnO and La compound be placed in agate mortar as raw material, at room temperature ground, milling time is 20min～60min, obtains the presoma of lanthanum doped gallium zinc nitrogen oxygen solid solution; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the mol ratio of Ga element and Zn element is 1:1; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the doping mole percent of La element is 1%～6%;
The presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution two, step 1 obtained is calcined in 750 ℃～900 ℃ and the flow velocity ammonia atmosphere that is 200mL/min～300mL/min in temperature, calcination time is 5h～30h, the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after being calcined;
Be cooled to 100 ℃ under the ammonia atmosphere that the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after the calcining three, step 2 obtained is 200mL/min～300mL/min at flow velocity, then take out after naturally cooling to room temperature, finally obtain lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst.
The preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst of the present invention and application be using lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst as photochemical catalyst for the decomposition water oxygen.
The present invention adopts the standby lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst of high-temperature ammonolysis legal system, comprises following characteristics:
1, raw material of the present invention is cheap and easy to get, simple to operate, uses the high-temperature ammonolysis method to synthesize first lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst;
2, the lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst that prepared by the present invention has visible light-responded, responds the more visible ray of long-wave band with the sample phase specific energy of the La element that do not adulterate, the about red shift 15nm of ABSORPTION EDGE;
3, the lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst that prepared by the present invention has higher oxygen-producing amount and decomposition water oxygen performance, the oxygen-producing amount of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is greater than 70 μ mol/h, and the oxygen-producing amount of the gallium zinc nitrogen oxygen solid solution photochemical catalyst of the La element that do not adulterate is only 48 μ mol/h, lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is compared with the gallium zinc nitrogen oxygen solid solution photochemical catalyst of the La element that do not adulterate, and the oxygen performance of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst has improved more than 50%.
The accompanying drawing explanation
The X-ray diffraction comparison diagram of the gallium zinc nitrogen oxygen solid solution photochemical catalyst that Fig. 1 makes for the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made and contrast test, wherein curve 1 means the X-ray diffraction curve of the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made, and wherein curve 2 means the X-ray diffraction curve of the gallium zinc nitrogen oxygen solid solution photochemical catalyst that contrast test makes;
Fig. 2 is the microscopic appearance figure of the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made;
Fig. 3 is the gallium zinc nitrogen oxygen solid solution photochemical catalyst microscopic appearance figure that contrast test makes;
The UV, visible light absorption light comparison diagram of the gallium zinc nitrogen oxygen solid solution photochemical catalyst that Fig. 4 makes for the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made and contrast test, wherein curve 1 means that the UV, visible light of the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made absorbs light curve, and wherein curve 2 means the UV, visible light absorption curves of the lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst that contrast test makes;
The gallium zinc nitrogen oxygen solid solution photochemical catalyst oxygen performance comparison figure that Fig. 5 makes for testing a lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made and contrast test.
The specific embodiment
The specific embodiment one: the preparation method of a kind of lanthanum doped gallium of present embodiment zinc nitrogen oxygen solid solution photochemical catalyst, carry out according to the following steps:
One, take Ga
2o
3, ZnO and La compound be placed in agate mortar as raw material, at room temperature ground, milling time is 20min～60min, obtains the presoma of lanthanum doped gallium zinc nitrogen oxygen solid solution; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the mol ratio of Ga element and Zn element is 1:1; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the doping mole percent of La element is 1%～6%;
The presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution two, step 1 obtained is calcined in 750 ℃～900 ℃ and the flow velocity ammonia atmosphere that is 200mL/min～300mL/min in temperature, calcination time is 5h～30h, the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after being calcined;
Be cooled to 100 ℃ under the ammonia atmosphere that the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after the calcining three, step 2 obtained is 200mL/min～300mL/min at flow velocity, then take out after naturally cooling to room temperature, finally obtain lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst.
In the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution described in the present embodiment step 1, the mole percent of La element is 1%～6% to refer to that the number of La atom in the presoma of lanthanum doped gallium zinc nitrogen oxygen solid solution is 1%～6% of Ga, Zn total atom number.
Room temperature described in present embodiment step 1 and step 3 is 25 ℃.
The present embodiment Raw is cheap and easy to get, simple to operate, uses the high-temperature ammonolysis method to synthesize first lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst.
Lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst prepared by present embodiment has visible light-responded, responds the more visible ray of long-wave band with the sample phase specific energy of the La element that do not adulterate, the about red shift 15nm of ABSORPTION EDGE.
Lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst prepared by present embodiment has higher oxygen-producing amount and decomposition water oxygen performance, the oxygen-producing amount of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is greater than 70 μ mol/h, and the oxygen-producing amount of the gallium zinc nitrogen oxygen solid solution photochemical catalyst of the La element that do not adulterate is only 48 μ mol/h, lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is compared with the gallium zinc nitrogen oxygen solid solution photochemical catalyst of the La element that do not adulterate, and the oxygen performance of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst has improved more than 50%.
The specific embodiment two: present embodiment is different from the specific embodiment one: the compound of the La described in step 1 is La
2o
3or LaCl
3.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from the specific embodiment one or two: in the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution described in step 1, the mole percent of La element is 2%～5%.Other is identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three: in the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution described in step 1, the mole percent of La element is 4%.Other are identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four: the milling time described in step 1 is 30min.Other are identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five: being calcined in 850 ℃ and the flow velocity ammonia atmosphere that is 200mL/min～300mL/min in temperature described in step 2.Other are identical with one of specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six: being calcined in 750 ℃～900 ℃ and the flow velocity ammonia atmosphere that is 250mL/min in temperature described in step 2.Other are identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different from one of specific embodiment one to seven: the calcination time described in step 2 is 15h.Other are identical with one of specific embodiment one to seven.
The specific embodiment nine: present embodiment is different from one of specific embodiment one to eight: under the ammonia atmosphere that is 250mL/min at flow velocity described in step 3, be cooled to 100 ℃.Other are identical with one of specific embodiment one to eight.
The specific embodiment ten: the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst of present embodiment and application be using lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst as catalyst for the decomposition water oxygen.
The method that the described lanthanum doped gallium of present embodiment zinc nitrogen oxygen solid solution photochemical catalyst is used for to the decomposition water oxygen is: 0.1g lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is added to 100mL distilled water and uses H
2sO
4regulate pH=4.5, add again AgNO3 as sacrifice agent, obtain mixed solution, and in mixed solution, the concentration of AgNO3 is 0.1mol/L, then with vavuum pump, make reactor reach vacuum state with except anhydrating middle dissolved gases, then under the xenon lamp of 300W irradiates, use simulated solar irradiation to carry out the decomposition water oxygen.
In present embodiment, lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is had to higher oxygen-producing amount and decomposition water oxygen performance for the decomposition water oxygen.
By following verification experimental verification effect of the present invention:
Test one: one, take 0.54gGa
2o
3, 0.47gZnO and LaCl
3be placed in agate mortar as raw material, at room temperature ground, milling time is 30min, obtains the presoma of lanthanum doped gallium zinc nitrogen oxygen solid solution; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the doping mole percent of La element is 2%;
The presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution two, step 1 obtained is calcined in 850 ℃ and the flow velocity ammonia atmosphere that is 250mL/min in temperature, and calcination time is 15h, the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after being calcined;
Be cooled to 100 ℃ under the ammonia atmosphere that the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after the calcining three, step 2 obtained is 250mL/min at flow velocity, take out after then naturally cooling to room temperature, finally obtain lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst.
Contrast test: one, take 0.54gGa
2o
3, 0.47gZnO is placed in agate mortar as raw material, at room temperature ground, milling time is 30min, obtains the presoma of gallium zinc nitrogen oxygen solid solution;
The presoma of the gallium zinc nitrogen oxygen solid solution two, step 1 obtained is calcined in 850 ℃ and the flow velocity ammonia atmosphere that is 250mL/min in temperature, and calcination time is 15h, the presoma of the gallium zinc nitrogen oxygen solid solution after being calcined;
Be cooled to 100 ℃ under the ammonia atmosphere that the presoma of the gallium zinc nitrogen oxygen solid solution after the calcining three, step 2 obtained is 250mL/min at flow velocity, take out after then naturally cooling to room temperature, finally obtain gallium zinc nitrogen oxygen solid solution photochemical catalyst.
Get each 0.1g of photochemical catalyst powder that test one and contrast test make, add respectively 100mL distilled water and regulate pH=4.5 with H2SO4, add again AgNO3 as sacrifice agent, obtain mixed solution, and in mixed solution, the concentration of AgNO3 is 0.1mol/L, then with vavuum pump, make reactor reach vacuum state with except anhydrating middle dissolved gases, then under the xenon lamp of 300W irradiates, use simulated solar irradiation to carry out the test of decomposition water performance comparison to it.
The X-ray diffraction comparison diagram of the gallium zinc nitrogen oxygen solid solution photochemical catalyst that test result: Fig. 1 makes for the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made and contrast test, wherein curve 1 means the X-ray diffraction curve of the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made, and wherein curve 2 means the X-ray diffraction curve of the gallium zinc nitrogen oxygen solid solution photochemical catalyst that contrast test makes.As shown in Figure 1, the sharp-pointed degree at X-ray diffraction peak and the intensity of mixing the lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst of La element all increase to some extent, illustrate that its degree of crystallinity improves; Half-peak breadth diminishes, and illustrates that its crystallite dimension becomes large.Can also find, due to mixing of La element, the characteristic peak of diffraction maximum is offset to the low angle direction.This be because, La
3+enter (Ga
1-xzn
x) (N
1-xo
x) in structure, and La
3+ 
radius ratio Zn
2+radius
and Ga
3+radius
greatly, make lattice paprmeter increase, interplanar distance increases, so cause the characteristic peak at X-ray diffraction peak to be offset to the low angle direction.
The microscopic appearance figure that the lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst that Fig. 2 makes for test one adopts SEM to obtain, Fig. 3 is the microscopic appearance figure that the gallium zinc nitrogen oxygen solid solution photochemical catalyst that makes of contrast test adopts SEM to obtain, and two figure contrasts can find out that the mischcrystal photocatalyst particle of the La element that adulterated becomes more regular.
The UV, visible light absorption light comparison diagram of the gallium zinc nitrogen oxygen solid solution photochemical catalyst that Fig. 4 makes for the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made and contrast test, wherein curve 1 means that the UV, visible light of the test one lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made absorbs light curve, and wherein curve 2 means the UV, visible light absorption curves of the lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst that contrast test makes.As can be seen from Figure 4, the ABSORPTION EDGE generation red shift of mischcrystal photocatalyst after doping La element.
The gallium zinc nitrogen oxygen solid solution photochemical catalyst oxygen performance comparison figure that Fig. 5 makes for testing a lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst made and contrast test, after the La element that adulterates as we can see from the figure, the oxygen performance of mischcrystal photocatalyst is improved.
Claims (10)
1. the preparation method of a lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst is characterized in that the preparation method of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst carries out according to the following steps:
One, take Ga
2o
3, ZnO and La compound be placed in agate mortar as raw material, at room temperature ground, milling time is 20min～60min, obtains the presoma of lanthanum doped gallium zinc nitrogen oxygen solid solution; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the mol ratio of Ga element and Zn element is 1:1; In the presoma of described lanthanum doped gallium zinc nitrogen oxygen solid solution, the doping mole percent of La element is 1%～6%;
The presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution two, step 1 obtained is calcined in 750 ℃～900 ℃ and the flow velocity ammonia atmosphere that is 200mL/min～300mL/min in temperature, calcination time is 5h～30h, the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after being calcined;
Be cooled to 100 ℃ under the ammonia atmosphere that the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution after the calcining three, step 2 obtained is 200mL/min～300mL/min at flow velocity, then take out after naturally cooling to room temperature, finally obtain lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst.
2. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, the compound that it is characterized in that the La described in step 1 is La
2o
3or LaCl
3.
3. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that the mole percent of La element in the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution described in step 1 is 2%～5%.
4. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that the mole percent of La element in the presoma of the lanthanum doped gallium zinc nitrogen oxygen solid solution described in step 1 is 4%.
5. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that the milling time described in step 1 is 30min.
6. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that being calcined in 850 ℃ and the flow velocity ammonia atmosphere that is 200mL/min～300mL/min in temperature described in step 2.
7. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that being calcined in 750 ℃～900 ℃ and the flow velocity ammonia atmosphere that is 250mL/min in temperature described in step 2.
8. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that the calcination time described in step 2 is 15h.
9. the preparation method of a kind of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst according to claim 1, is characterized in that being cooled to 100 ℃ under the ammonia atmosphere that is 250mL/min at flow velocity described in step 3.
10. the application of lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst as claimed in claim 1, it is characterized in that lanthanum doped gallium zinc nitrogen oxygen solid solution photochemical catalyst as photochemical catalyst for the decomposition water oxygen.
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Cited By (3)
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| CN103878011A (en) * | 2014-04-17 | 2014-06-25 | 哈尔滨工业大学 | Method for synthesizing GaN: ZnO solid solution photocatalyst |
| CN103878010A (en) * | 2014-04-15 | 2014-06-25 | 哈尔滨工业大学 | Preparation method of VB-group metal ion doped (Ga<1-x>Znx)(N<1-x>Ox) solid solution photocatalyst |
| CN109746019A (en) * | 2018-12-28 | 2019-05-14 | 西安交通大学 | A kind of preparation method and applications of gallium indium-zinc ternary nitrogen oxides |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103878010A (en) * | 2014-04-15 | 2014-06-25 | 哈尔滨工业大学 | Preparation method of VB-group metal ion doped (Ga<1-x>Znx)(N<1-x>Ox) solid solution photocatalyst |
| CN103878011A (en) * | 2014-04-17 | 2014-06-25 | 哈尔滨工业大学 | Method for synthesizing GaN: ZnO solid solution photocatalyst |
| CN109746019A (en) * | 2018-12-28 | 2019-05-14 | 西安交通大学 | A kind of preparation method and applications of gallium indium-zinc ternary nitrogen oxides |
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Application publication date: 20131218 |