CN102389828B - Preparation and application of high-dispersity ZnO/GaN solid solution - Google Patents
Preparation and application of high-dispersity ZnO/GaN solid solution Download PDFInfo
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- CN102389828B CN102389828B CN2011102930707A CN201110293070A CN102389828B CN 102389828 B CN102389828 B CN 102389828B CN 2011102930707 A CN2011102930707 A CN 2011102930707A CN 201110293070 A CN201110293070 A CN 201110293070A CN 102389828 B CN102389828 B CN 102389828B
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Abstract
The invention discloses a preparation method and application of high-dispersity ZnO/GaN solid solution. The preparation method comprises the following step of: preparing high-dispersity layered double hydroxides (LDHs) by utilizing a co-precipitation and hydrothermal treatment method, and thus preparing a high-dispersity ZnO/GaN solid solution material in various forms such as thin film, powder and the like. The high-dispersity ZnO/GaN solid solution thin film, which is prepared by the steps of spin-coating the high-dispersity LDHs on a substrate and carrying out high-temperature ammoniation, can be used for photocatalytic water decomposing, thus the use efficiency of the catalyst is greatly improved, the use amount of the catalyst is reduced, the defect that powder is difficult to recover in powder water catalysis process is overcome, and the high-dispersity ZnO/GaN solid solution has good application prospects.
Description
Technical field
The present invention relates to a kind of solid solution, particularly a kind of preparation method of polymolecularity ZnO/GaN solid solution and the application in photocatalysis thereof.
Background technology
Solid solution is that composition can change alloy phase within the specific limits continuously, and this variation does not change the lattice type of solvent metal.According to solute atoms residing position in the solvent dot matrix, can be divided into interstitial solid solution and substitutional solid solution.Content of solute is adjustable, and then can regulate the performance of solid solution, so that solid solution shows wide application prospect in a plurality of fields such as ion-exchange, absorption, catalysis, light, electricity, magnetic.The method for preparing solid solution has multiple, comprise ion implantation, sintering process, ion-exchange, doping etc., wherein utilize layered double-hydroxide (LDHs) material be solid solution that presoma obtains after Overheating Treatment have structure height in order, have evenly multiple advantages such as distribution of porous, high-specific surface area, element.
The energy crisis environmental problem that in addition fossil fuel causes that becomes increasingly conspicuous is serious all the more in recent years, and the new forms of energy of seeking cleaning are key subjects of new century.Utilize conductor photocatalysis water H processed
2Be one of effective way of obtaining clean energy resource, wide or conduction band position is not suitable for not being suitable for photocatalysis water H processed but most of semiconductor is because of energy gap
2Japan Patent JP2005144210-A report has prepared a kind of ZnO/GaN solid solution, can regulate energy gap, and absorbing wavelength is transferred to about 420nm, is used for catalysis thereby can absorb visible light.(the Junpeng Wang such as Chinese patent CN102166527A and Wang Junpeng
Et al.J. Mater. Chem., 2011 (21): 4562) reported with (Zn
2+/ Ga
3+) layered double-hydroxide (LDHs) prepared ZnO/GaN solid solution for presoma, can with the content to 50% of GaN ~ 20%, can save the consumption of expensive GaN, thereby reduce cost.
Above-mentioned two kinds of methods all adopt nanocrystalline preparation powder method, nanocrystalline agglomeration is obvious in the preparation process, so that powder diameter is larger, cause that most of ZnO/GaN solid solution is nanocrystalline can not to contact visible light, make also simultaneously that most electronics, hole these effective catalytic centers migration distance in powder are long to cause its compound consumption and can not be used for catalysis water in inside, so that ZnO/GaN solid solution catalytic efficiency is lower.And because the catalyst that above-mentioned two kinds of methods make is Powdered, powder is difficult to reclaim in the water catalytic process, has caused the waste of catalyst.
Summary of the invention
Lower for ZnO/GaN solid solution catalytic efficiency in the prior art, in catalytic process, be difficult to the deficiency that reclaims, the invention provides a kind of preparation method who prepares polymolecularity ZnO/GaN solid solution, and the scheme that solid solution can be prepared into variform is to solve the deficiency in the above-mentioned technology.
For this reason, the invention provides a kind of preparation method of polymolecularity ZnO/GaN solid solution, comprise the steps:
(1) water-soluble Zn salt and Ga salt are dissolved in deionized water, be mixed with mixing salt solution, then in this mixing salt solution, drip precipitating reagent, accompany by simultaneously stirring, regulating the pH value is 8 ~ 9, until continue to stir 10～15 minutes after generating coprecipitate, obtains suspension again;
(2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle and carry out hydrothermal treatment consists under 100 ℃ ~ 130 ℃ temperature, obtains the polymolecularity layered double-hydroxide aqueous solution in upper solution;
(3) utilize the above-mentioned aqueous solution can make respectively polymolecularity ZnO/GaN solid solution membrane or Powdered polymolecularity ZnO/GaN solid solution, its method is respectively: the polymolecularity layered double-hydroxide aqueous solution that step (2) is obtained is spin-coated on the substrate, the substrate that spin coating is good is put into tube furnace, obtains polymolecularity ZnO/GaN solid solution membrane through ammonification under 750 ℃ ~ 850 ℃ temperature; The sediment that obtains behind the polymolecularity layered double-hydroxide aqueous solution centrifugal drying that step (2) is obtained is put into tube furnace, obtains Powdered polymolecularity ZnO/GaN solid solution through ammonification under 750 ℃ ~ 850 ℃ temperature.
Wherein, the water-soluble Zn salt described in the step (1) is ZnCl
2, ZnSO
4Or Zn (NO
3)
2, water-soluble Ga salt is GaCl
3Or Ga (NO
3)
3, the mol ratio of water-soluble Zn salt and water-soluble Ga salt is 1:1 ~ 10:1, precipitating reagent is NaOH, sodium carbonate, urea or ammoniacal liquor.
Among the preparation method of polymolecularity ZnO/GaN solid solution membrane, described substrate is Si substrate or glass substrate, and the thickness of polymolecularity ZnO/GaN solid solution membrane is less than 300nm.
In addition, the present invention also provides the polymolecularity ZnO/GaN solid solution membrane that will the make purposes as the photochemical catalyst decomposition water: the ZnO/GaN solid solution membrane is put into water, is H through radiation of visible light with water decomposition
2And O
2
It was the polymolecularity state before heat treatment that the ZnO/GaN solid solution that obtains polymolecularity must make its presoma, in heat treatment process, keep like this its original polymolecularity just can obtain the ZnO/GaN solid solution of polymolecularity, so the key of the ZnO/GaN solid solution of preparation polymolecularity is the presoma that obtains polymolecularity, namely will make polymolecularity (Zn
2+/ Ga
3+) layered double-hydroxide (LDHs).The ZnO/GaN solid solution of polymolecularity is not reunited mutually because of its nanometer sheet, so that all nanometer sheet can contact visible light, simultaneously since the polymolecularity of ZnO/GaN solid solution reduced the migration distance in electronics, hole and then reduced electronics, hole-recombination consumption, thereby can increase substantially utilization rate and the catalytic efficiency of ZnO/GaN solid solution.The ZnO/GaN solid solution catalyst is made film morphology makes it be easy to use, and is convenient to collect.And because polymolecularity (Zn
2+/ Ga
3+) layered double-hydroxide is not because contacting with each other between its nanometer sheet, so that contact fully with ammonia, reduced the ammonification time, thereby reduced the evaporation of Zn in the heat treatment process, so that Zn content loses hardly, surpass 90% ZnO/GaN solid solution so can make ZnO content.The Ga element is the resource of very rare costliness, and said method has not only reduced the consumption of Ga, has also reduced cost.
The invention has the beneficial effects as follows:
1) adopt method of the present invention can prepare the aqueous solution of polymolecularity ZnO/GaN layered double-hydroxide (LDHs), its dispersiveness is fine, places three weeks not occur precipitation, and the particle in the solution is not reunited, do not assembled, and particle diameter is little and be evenly distributed;
2) the polymolecularity ZnO/GaN layered double-hydroxide (LDHs) that adopts method of the present invention to make can be prepared into the polymolecularity ZnO/GaN solid-solution material of variform, thereby has widened the application of this material;
3) polymolecularity layered double-hydroxide (LDHs) can be preserved in the aqueous solution, has overcome traditional layered double-hydroxide (LDHs) and can only be kept at defective in the organic solvent, has reduced environmental pollution;
4) ZnO/GaN layered double-hydroxide (LDHs) is prepared into filminess, the stacking minimizing of nanometer sheet can reduce high temperature ammonification required time greatly, significantly reduces the consumption of LDHs;
5) with the ZnO/GaN solid solution membrane photocatalyst of polymolecularity, solve the difficult problem that powder is difficult to reclaim in the catalytic process, and can avoid the waste of catalyst;
6) the ZnO/GaN solid solution of polymolecularity can reduce electron-hole recombinations, can improve catalyst utilization rate and catalytic efficiency;
7) method of the present invention is simple, easy implements, and helps the industrial applications of ZnO/GaN solid solution.
Description of drawings
Fig. 1 is (Zn
2+/ Ga
3+) X-ray diffraction (XRD) collection of illustrative plates of layered double-hydroxide (LDHs);
Fig. 2 is (Zn
2+/ Ga
3+) transmission electron microscope (TEM) figure of layered double-hydroxide (LDHs);
Fig. 3 is (Zn
2+/ Ga
3+) SEM (SEM) figure of layered double-hydroxide (LDHs) precipitation;
Fig. 4 is X-ray diffraction (XRD) collection of illustrative plates of ZnO/GaN solid solution membrane;
Fig. 5 is ZnO/GaN solid solution membrane catalysis water H processed under different-waveband light
2Productive rate figure.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be appreciated that these embodiment only are not used in for explanation the present invention and limit the scope of the invention.Should be understood that in addition after the content of having read instruction of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1: the preparation of polymolecularity layered double-hydroxide (LDHs)
1) with mol ratio is the Zn (NO of 4:1
3)
2And Ga (NO
3)
3Dissolve in deionized water, be mixed with mixing salt solution, then drip urea in this mixing salt solution, regulating the pH value is 9, accompanies by simultaneously stirring, until continue to stir 10 minutes after generating coprecipitate, obtains suspension again;
2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle 115 ℃ of hydrothermal treatment consists, obtains (the Zn of polymolecularity in upper solution
2+/ Ga
3+) the layered double-hydroxide aqueous solution;
Fig. 1 is (Zn
2+/ Ga
3+) X-ray diffraction (XRD) collection of illustrative plates of layered double-hydroxide (LDHs), that show among the figure is (Zn
2+/ Ga
3+) peak position of layered double-hydroxide (LDHs), as can be seen from the figure have typical layered double-hydroxide (LDHs) at the characteristic peak of 23 ° and 34 °, illustrate that product is layered double-hydroxide (LDHs).
Embodiment 2: the dispersiveness checking of the layered double-hydroxide aqueous solution
1) with mol ratio is the ZnCl of 1:1
2And GaCl
3Dissolve in deionized water, be mixed with mixing salt solution, then drip NaOH in this mixing salt solution, regulating the pH value is 8, accompanies by simultaneously stirring, until continue to stir 12 minutes after generating coprecipitate, obtains suspension again;
2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle 120 ℃ of hydrothermal treatment consists, obtains (the Zn of polymolecularity in upper solution
2+/ Ga
3+) the layered double-hydroxide aqueous solution;
3) (the Zn of polymolecularity will be obtained in the upper solution
2+/ Ga
3+) after the layered double-hydroxide aqueous solution left standstill for three weeks at ambient temperature, do not separate out precipitation in the aqueous solution, the bulky grain that also find to suspend illustrates that this aqueous solution has fabulous dispersiveness, and transmission electron microscope (TEM) collection of illustrative plates has also confirmed (the Zn that makes
2+/ Ga
3+) polymolecularity of layered double-hydroxide (LDHs).
Fig. 2 is the (Zn of upper solution
2+/ Ga
3+) transmission electron microscope (TEM) figure of layered double-hydroxide (LDHs), the LDHs in the visible upper solution does not reunite, and LDHs has polymolecularity.
Embodiment 3: the preparation of Powdered polymolecularity ZnO/GaN solid solution
1) with mol ratio is the ZnSO of 2:1
4And GaCl
3Dissolve in deionized water, be mixed with mixing salt solution, then drip ammoniacal liquor in this mixing salt solution, regulating the pH value is 8, accompanies by simultaneously stirring, until continue to stir 10 minutes after generating coprecipitate, obtains suspension again;
2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle 100 ℃ of hydrothermal treatment consists, obtains (the Zn of polymolecularity in upper solution
2+/ Ga
3+) the layered double-hydroxide aqueous solution;
3) with (Zn of the polymolecularity that obtains
2+/ Ga
3+) be precipitated thing behind the layered double-hydroxide aqueous solution centrifugal drying;
4) sediment that drying is good is put into tube furnace, carries out 750 ℃ of ammonifications and can obtain Powdered polymolecularity ZnO/GaN solid solution in 5 minutes.
Fig. 3 SEM (SEM) figure shows (Zn among the figure
2+/ Ga
3+) layered double-hydroxide (LDHs) is the nanometer sheet form and kept good hexagon pattern.
Embodiment 4: the preparation of Powdered polymolecularity ZnO/GaN solid solution
1) with mol ratio is the ZnCl of 2:1
2And GaCl
3Dissolve in deionized water, be mixed with mixing salt solution, then drip ammoniacal liquor in this mixing salt solution, regulating the pH value is 8, accompanies by simultaneously stirring, until continue to stir 15 minutes after generating coprecipitate, obtains suspension again;
2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle 130 ℃ of hydrothermal treatment consists, obtains (the Zn of polymolecularity in upper solution
2+/ Ga
3+) the layered double-hydroxide aqueous solution;
3) with (Zn of the polymolecularity that obtains
2+/ Ga
3+) be precipitated thing behind the layered double-hydroxide aqueous solution centrifugal drying;
4) sediment that drying is good is put into tube furnace, carries out 850 ℃ of ammonifications and can obtain Powdered polymolecularity ZnO/GaN solid solution in 3 minutes.
Embodiment 5: the preparation of polymolecularity ZnO/GaN solid solution membrane
1) with mol ratio is the ZnCl of 3:1
2And GaCl
3Dissolve in deionized water, be mixed with mixing salt solution, then drip sodium carbonate in this mixing salt solution, regulating the pH value is 8.5, accompanies by simultaneously stirring, until continue to stir 15 minutes after generating coprecipitate, obtains suspension again;
2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle 130 ℃ of hydrothermal treatment consists, obtains (the Zn of polymolecularity in upper solution
2+/ Ga
3+) the layered double-hydroxide aqueous solution;
3) will obtain (the Zn of polymolecularity
2+/ Ga
3+) the layered double-hydroxide aqueous solution is spin-coated on the glass substrate, thickness is 250nm;
4) substrate that spin coating is good is put into tube furnace, 850 ℃ of lower ammonifications 3 minutes, can obtain polymolecularity ZnO/GaN solid solution membrane.
Fig. 4 is the X ray diffracting spectrum (XRD) of ZnO/GaN solid solution membrane, show among the figure, peak position between the peak position of the peak position of ZnO and GaN, assorted peak, visible ZnO/GaN solid solution is single-phase existence, does not have dephasign.
Embodiment 6: the preparation of polymolecularity ZnO/GaN solid solution membrane
1) with mol ratio is the ZnSO of 10:1
4And GaCl
3Dissolve in deionized water, be mixed with mixing salt solution, then drip sodium carbonate in this mixing salt solution, regulating the pH value is 8, accompanies by simultaneously stirring, until continue to stir 10 minutes after generating coprecipitate, obtains suspension again;
2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle 100 ℃ of hydrothermal treatment consists, obtains (the Zn of polymolecularity in upper solution
2+/ Ga
3+) the layered double-hydroxide aqueous solution;
3) will obtain (the Zn of polymolecularity
2+/ Ga
3+) the layered double-hydroxide aqueous solution is spin-coated on the Si substrate, thickness is 280nm;
4) substrate that spin coating is good is put into tube furnace, 750 ℃ of lower ammonifications 5 minutes, can obtain polymolecularity ZnO/GaN solid solution membrane.
In order to detect the content of ZnO in the polymolecularity ZnO/GaN solid solution membrane, this film is carried out elementary analysis, utilize energy disperse spectroscopy (EDS) detect N, O, each element of Zn, Ga in the solid solution membrane under the standard state content of (K represents that each element is in standard state), testing result sees Table 1.
Table 1 ZnO/GaN solid solution results of elemental analyses
| Element | Weight | Atom |
| ? | Percentage | Percentage |
| N K | 1.49 | 4.33 |
| O K | 17.92 | 45.68 |
| Zn K | 73.24 | 45.69 |
| Ga K | 7.35 | 4.30 |
| Total amount | 100.00 | ? |
The result of form shows, can be calculated ZnO content and be reached 91.4% by formula Zn K/(Zn K+Ga K) (formula numerical value is the atomic percent data)=45.69/(45.69+4.30), with initial ZnSO
4And GaCl
3Mol ratio 10:1 is basic identical.Explanation in the high temperature ammonifying process, (Zn
2+/ Ga
3+) Zn in the layered double-hydroxide do not have to run off substantially.
Embodiment 7:ZnO/GaN solid solution membrane is used for photodissociation water as catalyst
1) area that embodiment 5 is made is 1cm
2The ZnO/GaN solid solution membrane put into water;
2) regulate the radiation of visible light ZnO/GaN solid solution membrane that monochromatic burner uses identical light intensity under the different-waveband;
3) measure H under the different-waveband
2And O
2Output, can obtain the efficient of ZnO/GaN solid solution membrane under different-waveband.
Fig. 5 is ZnO/GaN solid solution membrane catalysis water H processed under different-waveband light
2Productive rate figure, show among the figure that the ZnO/GaN solid solution membrane realized catalysis water H processed under the visible light condition
2
Claims (9)
1. the preparation method of a polymolecularity ZnO/GaN solid solution comprises the steps:
(1) water-soluble Zn salt and Ga salt are dissolved in deionized water, be mixed with mixing salt solution, then in this mixing salt solution, drip precipitating reagent, accompany by simultaneously stirring, regulating the pH value is 8 ~ 9, until continue to stir 10～15 minutes after generating coprecipitate, obtains suspension again;
(2) with suspension washing, the sediment that obtains after centrifugal puts into water heating kettle and carry out hydrothermal treatment consists under 100 ℃ ~ 130 ℃ temperature, obtains the polymolecularity layered double-hydroxide aqueous solution in upper solution;
(3) the polymolecularity layered double-hydroxide aqueous solution that utilizes step (2) to obtain makes polymolecularity ZnO/GaN solid solution membrane or Powdered polymolecularity ZnO/GaN solid solution.
2. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 1, it is characterized in that: the polymolecularity layered double-hydroxide aqueous solution that step (2) is obtained is spin-coated on the substrate, the substrate that spin coating is good is put into tube furnace, obtains polymolecularity ZnO/GaN solid solution membrane through ammonification under 750 ℃ ~ 850 ℃ temperature.
3. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 1, it is characterized in that: the sediment that obtains behind the polymolecularity layered double-hydroxide aqueous solution centrifugal drying that step (2) is obtained is put into tube furnace, obtains Powdered polymolecularity ZnO/GaN solid solution through ammonification under 750 ℃ ~ 850 ℃ temperature.
4. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 1, it is characterized in that: water-soluble Zn salt is ZnCl in the step (1)
2, ZnSO
4Or Zn (NO
3)
2, water-soluble Ga salt is GaCl
3Or Ga (NO
3)
3
5. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 1, it is characterized in that: the mol ratio of water-soluble Zn salt and water-soluble Ga salt is 1:1 ~ 10:1 in the step (1).
6. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 1, it is characterized in that: the precipitating reagent in the step (1) is NaOH, sodium carbonate, urea or ammoniacal liquor.
7. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 2, it is characterized in that: described substrate is Si substrate or glass substrate.
8. the preparation method of polymolecularity ZnO/GaN solid solution according to claim 2, it is characterized in that: the thickness of described polymolecularity ZnO/GaN solid solution membrane is less than 300nm.
9. the polymolecularity ZnO/GaN solid solution membrane that makes of method according to claim 2 is as the purposes of photochemical catalyst decomposition water, and it is characterized in that: the ZnO/GaN solid solution membrane is put into water, is H through radiation of visible light with water decomposition
2And O
2
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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 |
| CN108117052B (en) * | 2016-11-29 | 2020-10-16 | 中国科学院金属研究所 | Two-dimensional mesoporous (GaN)1-x (ZnO) x solid solution nano material and preparation method thereof |
| CN106824242A (en) * | 2017-01-19 | 2017-06-13 | 京东方科技集团股份有限公司 | The preparation method and material for air purification of a kind of material for air purification |
| CN112675890B (en) * | 2020-12-21 | 2021-11-19 | 中国医科大学附属第一医院 | Visible light catalytic nano antibacterial material and preparation method thereof |
| CN113828343B (en) * | 2021-10-29 | 2023-05-23 | 厦门理工学院 | Surface-treated GaN-ZnO solid solution powder and surface treatment method thereof |
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| CN101429028A (en) * | 2008-11-28 | 2009-05-13 | 同济大学 | Method for producing Zr0.30Ce0.45Al0.25O1.87sosoloid nano-particle |
| CN101829557A (en) * | 2010-04-20 | 2010-09-15 | 上海大学 | Magnesium modified cerium-zirconium solid solution and preparation method thereof |
| CN102166527A (en) * | 2011-01-25 | 2011-08-31 | 山东大学 | Gallium nitride/zinc oxide solid solution with high zinc content and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101429028A (en) * | 2008-11-28 | 2009-05-13 | 同济大学 | Method for producing Zr0.30Ce0.45Al0.25O1.87sosoloid nano-particle |
| CN101829557A (en) * | 2010-04-20 | 2010-09-15 | 上海大学 | Magnesium modified cerium-zirconium solid solution and preparation method thereof |
| CN102166527A (en) * | 2011-01-25 | 2011-08-31 | 山东大学 | Gallium nitride/zinc oxide solid solution with high zinc content and preparation method thereof |
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Inventor after: Zhu Liping Inventor after: Li Yaguang Inventor after: Mei Weimin Inventor after: Yang Meijia Inventor after: Gu Jianlong Inventor after: Chen Dan Inventor after: Zhu Liyu Inventor after: Chen Qi Inventor after: Ren Yuping Inventor before: Zhu Liping Inventor before: Li Yaguang |
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Granted publication date: 20130320 Termination date: 20141001 |
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