CN104588014A - Method for depositing gold nanoparticles on surface of one-dimensional ZnO material - Google Patents
Method for depositing gold nanoparticles on surface of one-dimensional ZnO material Download PDFInfo
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- CN104588014A CN104588014A CN201510073100.1A CN201510073100A CN104588014A CN 104588014 A CN104588014 A CN 104588014A CN 201510073100 A CN201510073100 A CN 201510073100A CN 104588014 A CN104588014 A CN 104588014A
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Abstract
The invention discloses a method for depositing gold nanoparticles on the surface of a one-dimensional ZnO material. The method comprises the following steps: dispersing the one-dimensional ZnO material and HAuCl4 in water, performing ultrasonic treatment in the absence of a reducing agent, reducing Au<3+> into gold nanoparticles, and depositing the gold nanoparticles onto the surface of the one-dimensional ZnO material. The chloroauric acid is reduced by adopting an ultrasonic method, the nanometer Au particles are loaded on multiple one-dimensional ZnO nanometer materials, the technology bias is overcome, the process flow is simple, fewer raw materials are used, the obtained nanometer Au particles in the Au/ZnO composite one-dimensional nanometer material are high in crystallinity, small in particle size, uniform in dispersion and uniform in size, the separation of electron-hole pairs is promoted, the photocatalytic efficiency is greatly improved, and the product is superior to products prepared by most of liquid phase methods and has wide applications in the fields of sensors, batteries, catalysts, organisms and new energy.
Description
Technical field
The present invention relates to the method for a kind of One-Dimensional ZnO material (i.e. One-Dimensional ZnO nano material) surface deposition gold nano grain, be specifically related to a kind of without additional reducing agent exist, only adopt ultrasonic process in the method for One-Dimensional ZnO material surface deposited gold nano particle.
Background technology
ZnO is a kind of n-type semiconductor, and energy gap is 3.2 eV, is II-VI important race's conductor oxidate, has higher exciton bind energy, can be widely used in the numerous areas such as pottery, chemical industry, electronics, optics, biology, medicine.The pattern of ZnO material is very abundant, wherein, One-Dimensional ZnO material has the chemical stability of higher elevated temperature strength, hardness and excellence, and such as, the application of ZnO whisker in AFM and scanning tunnelling microscope probe with big L/D ratio achieves progress.At present, various one dimension novel forms is by a large amount of synthesis and research, and its performance test shows huge application potential.But, due to some limitation and the various destabilizing factors that occur in preparation process of the ZnO of one dimension oriented growth itself, limit its practical ranges.In order to overcome this shortcoming, by ZnO and noble metal Au nano material compound, to preparing the composite having bi-material excellent properties concurrently, and show the performance more excellent than pure ZnO nano material.
At present, the preparation method of One-Dimensional ZnO and Au nano material is comparatively ripe, and can industrial production be realized, the main method of the preparation Au/ ZnO nano composite of current report has high-molecular gel method, dipping light decomposition method, photo-reduction sedimentation, laser composite heating evaporation technique etc., these methods all need additionally to add play reduction reagent by Au
3+be reduced to Au, the reducing agent selected by method difference of use is also different.In addition, also there is following problem in these methods: in (1) ZnO material, the noble metal Au particle size of compound is comparatively large, makes active reduction; (2) Au particle disperses unevenly to cause coupling effect on ZnO, reduces composite property; (3) particle diameter prepared is uncontrollable, easily agglomeration occurs, thus is difficult to accomplish scale production, and it applies the low concentration material be mostly confined in laboratory; (4) complicated process of preparation of composite, cost is higher, is difficult to realize industrial production.Therefore, still need to carry out continuous mend gene to the preparation of ZnO and Au composite nano materials.
Summary of the invention
The deficiency that the composite nano materials that the present invention is directed to current One-Dimensional ZnO and Au exists in the preparation, provide a kind of method of One-Dimensional ZnO material surface deposited gold nano particle, the method does not need to add any electronation reagent, raw materials used few, flow process is simple, is applicable to industrialized production.
We know, ultrasonic can make each reaction raw materials disperse more even, contact more abundant, the carrying out that ultrasonic wave added reacts all is adopted in a lot of reaction, also have in reduction reaction and adopt carrying out fast of ultrasonic wave added reduction reaction, but in reduction reaction disclosed at present, especially by HAuCl
4be reduced in solution environmental in the reaction of Au, also do not adopt additional reducing agent, by means of only ultrasonic come reduction reaction.Inventor finds in the linguistic term of the preparation method to one dimension Au/ZnO composite, when only adopt ultrasonic and do not add additional reducing agent when, still can well by HAuCl
4be reduced to Au, and successfully by the Au nanoparticle deposition of gained to One-Dimensional ZnO material surface, this result has broken the cognition of traditional " ultrasonic only can assisted reaction carry out ", " reduction reaction must add reducing agent " thought, overcomes technology prejudice.
The present invention only adopts the ultrasonic concrete technical scheme at One-Dimensional ZnO material surface deposited gold nano particle as follows:
A method for One-Dimensional ZnO material surface deposited gold nano particle, step comprises: by One-Dimensional ZnO material and HAuCl
4be distributed in water, under existing without reducing agent, carry out ultrasonic process, by Au
3+be reduced to gold nano grain and deposit to One-Dimensional ZnO material surface.
Why the present invention only adopts and ultrasonicly just can realize HAuCl
4reduction, very large relation is had with adopted raw material, research finds, when adopting One-Dimensional ZnO material, the energy of ultrasonic generation can produce being separated of electronics and hole at One-Dimensional ZnO material surface, and gold ion reduces by these electronic energies be separated, thus forms the Au nano particle of 3 ~ 15 nm, make gold nano grain and One-Dimensional ZnO material tight compound simultaneously, improve the character of composite.And adopt other materials, such as, during spherical ZnO, electronics can not be separated with hole, only ultrasonic reduction and the deposition that just cannot complete gold ion.
The present invention only adopts the ultrasonic gold nano grain not adding reducing agent gained to be evenly distributed at One-Dimensional ZnO material surface.
In said method, the size of nanometer gold grain depositing to One-Dimensional ZnO material surface is homogeneous.
In said method, the particle diameter depositing to the gold nano grain of One-Dimensional ZnO material surface is 3 ~ 15 nm.
In said method, described One-Dimensional ZnO material is the monodimension nanometer materials such as ZnO nanorod, ZnO nano-wire, ZnO nano-band, ZnO nano fiber, ZnO nano array, ZnO nano whisker.
Said method specifically comprises the following steps:
(1) by One-Dimensional ZnO dispersion of materials in water, ultrasonic process 30-60min;
(2) in the mixture after the ultrasonic process of step (1), HAuCl is added
4the aqueous solution, and then carry out ultrasonic process and make Au
3+be reduced to Au;
(3) after ultrasonic process by reactant liquor centrifugation, washing, obtain Au/ZnO compound monodimension nanometer material.
In above-mentioned steps (1), the concentration of One-Dimensional ZnO material in water is 1.0 ~ 5.0 mmol/L.Within the scope of this, the concentration of ZnO is larger, and it is more sparse that Au particle distributes on ZnO.
In above-mentioned steps (2), ZnO and HAuCl
4mol ratio be 40:0.25 ~ 5.Within the scope of this, this ratio is larger, and it is more sparse that Au particle distributes on ZnO.
In above-mentioned steps (1) and (2), ultrasonic power is 50 ~ 500 W.Within the scope of this, power is larger, and Au particle is more closely knit in the distribution of ZnO, and particle diameter is larger, and the required time is fewer.
In above-mentioned steps (2), HAuCl
4the concentration of the aqueous solution is 0.1 ~ 5.0 mmol/L.Within the scope of this, HAuCl
4concentration larger, it is more closely knit that Au particle distributes on ZnO.
In above-mentioned steps (2), temperature during ultrasonic process is 15 ~ 80 DEG C.Within the scope of this, reaction temperature is higher, and the particle diameter of the Au particle of the upper load of ZnO is larger.
In above-mentioned steps (2), the time of ultrasonic process is 5 ~ 30 min.Within the scope of this, the reaction time is longer, and it is more closely knit that Au particle distributes on ZnO.
The present invention only adopts ultrasonic just Au nano particle in One-Dimensional ZnO nano-material surface deposition, utilizes ultrasonic provided electron reduction HAuCl
4, need not add other chemical reagent any, avoid the Au germination of chemical reagent caused by sodium borohydride too fast, the problems such as skewness, effectively control the size of Au nano particle.
The present invention adopts ultrasonic method reduction gold chloride, at multiple ZnO monodimension nanometer material loaded with nano Au particle, overcome technology prejudice, technological process is simple, raw material is few, Au nano particle good crystallinity in gained Au/ZnO compound monodimension nanometer material, particle diameter is little, be uniformly dispersed, size uniformity, advantageously in the separation of electron-hole pair, substantially increases photocatalysis efficiency, be better than the product prepared by most liquid phase method, be widely used in fields such as sensor, battery, catalyst, biology, new forms of energy.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) photo of the Au/ZnO compound monodimension nanometer material that the embodiment of the present invention 1 is synthesized.
Fig. 2 is transmission electron microscope (TEM) photo with the Au/ZnO compound monodimension nanometer material obtained in the not ultrasonic situation of reducing agent in comparative example 1 of the present invention.
Detailed description of the invention
Below by embodiment, the present invention will be further elaborated, and following explanation is only to explain the present invention, does not limit its content.In following embodiment, ZnO nanorod used, ZnO nano-band, ZnO nano-wire, ZnO nano fiber, ZnO nano crystalline substance is commercial, and those skilled in the art also can adopt method disclosed in document to synthesize.
embodiment 1
1.1 take 8.1 mg ZnO nanorod powder, are dispersed in 40 mL deionized waters, obtain the white suspension of 2.5 mM, in advance ultrasonic 30 min, ultrasonic power 50W;
1.2 HAuCl adding 2.5 mL in the suspension of step (1)
4the aqueous solution (1.0 mM), under room temperature condition, continues ultrasonic (50w) 5 min;
1.3 reaction terminate after, through centrifugation, washing, obtain Au/ZnO composite Nano bar material, wherein Au nano particle diameter is about 4 nm, and be evenly distributed on ZnO nanorod, comparatively closely knit, concrete shape characteristic is shown in Fig. 1.
embodiment 2
2.1 take 2.01 mg ZnO nano-band powder, are dispersed in 40 mL deionized waters, obtain the white suspension of 1.0 mM, in advance ultrasonic 60min, ultrasonic power 100W;
2.2 HAuCl adding 2.5 mL in being suspended of step (1)
4the aqueous solution (1.25 mM), is heated to 80 DEG C, continues ultrasonic (100w) 20 min;
2.3 reaction terminate after, through centrifugation, washing, obtain Au/ZnO composite Nano carrying material, wherein Au nano particle diameter is about 4 nm, and be evenly distributed on ZnO nano-band, comparatively sparse.
embodiment 3
3.1 take 3.24 mgZnO nanobelt powder, are dispersed in 40 mL deionized waters, obtain the white suspension of 1.0 mM, in advance ultrasonic 40min, ultrasonic power 400W;
3.2 HAuCl adding 2.5 mL in the suspension in step (1)
4the aqueous solution (1.5 mM), is heated to 80 DEG C, continues ultrasonic (400w) 20 min;
After 3.3 reactions terminate, through centrifugation, washing, obtain Au/ZnO composite Nano carrying material, wherein Au nano particle diameter is about 10 nm, and is evenly distributed on ZnO nano-band.
embodiment 4
4.1 take 16.2 mg ZnO nano-wire powder, are dispersed in 40 mL deionized waters, obtain the white suspension of 5.0 mM, in advance ultrasonic 30 min, ultrasonic power 500W;
4.2 HAuCl adding 2.5 mL in the suspension in step (1)
4the aqueous solution (1.0 mM), is heated to 30 DEG C, continues ultrasonic (500w) 15 min;
After 4.3 reactions terminate, through centrifugation, washing, obtain Au/ZnO composite Nano wire material, wherein Au nano particle diameter is about 4 nm, ZnO nano-wire is evenly distributed and sparse.
embodiment 5
5.1 take 8.1 mg ZnO nano fiber dusts, are dispersed in 40 mL deionized waters, obtain the white suspension of 2.5 mM, in advance ultrasonic 30 min, ultrasonic power 80W;
5.2 HAuCl adding 2.5 mL in the suspension in step (1)
4the aqueous solution (0.5 mM), continues ultrasonic (80w) and reacts 30 min under room temperature;
After 5.3 reactions terminate, through centrifugal, washing, obtain Au/ZnO composite nano-fiber material, wherein the particle diameter of Au nano particle is about 5 nm, and ZnO nano fiber is evenly distributed.
embodiment 6
6.1 take 8.1 mg ZnO nano whisker powder, are dispersed in 40 mL deionized waters, obtain the white suspension of 2.5 mL, in advance ultrasonic 30 min, ultrasonic power 400W;
6.2 HAuCl adding 2.5 mL in the suspension in step (1)
4the aqueous solution (5.0 mM), is heated to 40 DEG C of continuation ultrasonic (400w) and reacts 10 min;
After 6.3 reactions terminate, through centrifugal, washing, obtain Au/ZnO composite Nano crystal whisker materials, wherein the particle diameter of Au nano particle is 15 nm to the maximum, ZnO nano whisker is evenly distributed and sparse.
comparative example 1
Take 8.1 mg ZnO nanorod powder, be dispersed in 40 mL deionized water for stirring, obtain the white suspension of 2.5 mM;
The HAuCl of 4 mL is added in the suspension of above-mentioned steps
4the aqueous solution (1.0 mM), under room temperature condition, continues stirring 5 min; Add sodium borohydride reduction agent afterwards and stir 10min.
After reaction terminates, through centrifugation, washing, obtain Au/ZnO composite Nano bar material, wherein Au nano particle diameter is 20 nm to the maximum, and skewness, concrete shape characteristic are shown in Fig. 2 on ZnO nanorod.
comparative example 2
Take 8.1 mg ZnO micron ball powder, be dispersed in 40 mL deionized waters, obtain the white suspension of 2.5 mM, in advance ultrasonic 30 min, ultrasonic power 50W;
The HAuCl of 2.5 mL is added in the suspension of above-mentioned steps
4the aqueous solution (1.0 mM), under room temperature condition, continues ultrasonic (50w) 5 min;
After reaction terminates, after centrifugation, washing, find not Au nanoparticle deposition through electron microscopic observation, illustrate that one-dimensional material is the key that ultrasonic acquisition electron hole is separated.
Claims (10)
1. a method for One-Dimensional ZnO material surface deposited gold nano particle, is characterized in that: by One-Dimensional ZnO material and HAuCl
4be distributed in water, under existing without reducing agent, carry out ultrasonic process, by Au
3+be reduced to gold nano grain and deposit to One-Dimensional ZnO material surface.
2. method according to claim 1, is characterized in that: gold nano grain is evenly distributed at One-Dimensional ZnO material surface.
3. method according to claim 1 and 2, is characterized in that: gold nano grain particle diameter is 3 ~ 15 nm.
4. method according to claim 1 and 2, is characterized in that: described One-Dimensional ZnO material is ZnO nanorod, ZnO nano-wire, ZnO nano-band, ZnO nano fiber, ZnO nano array or ZnO nano whisker.
5. method according to claim 1 and 2, is characterized in that comprising the following steps:
(1) by One-Dimensional ZnO dispersion of materials in water, ultrasonic process 30-60min;
(2) in the mixture after the ultrasonic process of step (1), HAuCl is added
4the aqueous solution, then carry out ultrasonic process and make Au
3+be reduced to Au;
(3) after ultrasonic process by reactant liquor centrifugation, washing, obtain Au/ZnO compound monodimension nanometer material.
6. method according to claim 5, is characterized in that: in step (1), and the concentration of One-Dimensional ZnO material in water is 1.0 ~ 5.0 mmol/L.
7. method according to claim 5, is characterized in that: ZnO and HAuCl
4mol ratio be 40:0.25 ~ 5.
8. method according to claim 5, is characterized in that: in step (1) and (2), ultrasonic power is 50 ~ 500 W.
9. method according to claim 5, is characterized in that: HAuCl
4the concentration of the aqueous solution is 0.1 ~ 5.0 mmol/L.
10. method according to claim 5, is characterized in that: in step (2), and temperature during ultrasonic process is 15 ~ 80 DEG C; The time of ultrasonic process is 5 ~ 30 min.
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Cited By (7)
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| CN105195144A (en) * | 2015-10-15 | 2015-12-30 | 吉林大学 | Method for synthetizing Au/ZnO bar-shaped heterojunction photocatalyst |
| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN106391008A (en) * | 2016-09-21 | 2017-02-15 | 苏州大学 | Method for loading three-dimensional zinc oxide surface with metal nanoparticles |
| CN107175339A (en) * | 2017-05-23 | 2017-09-19 | 天津工业大学 | A kind of method and device without reducing agent Fast back-projection algorithm gold nano grain |
| CN108440767A (en) * | 2018-04-18 | 2018-08-24 | 西北大学 | It is a kind of that nanometer Au is combined to the new method for preparing Au@MOF composite materials with porous MOF |
| CN110150317A (en) * | 2019-05-30 | 2019-08-23 | 吉林大学 | A kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure and preparation method thereof |
| CN111157595A (en) * | 2019-12-26 | 2020-05-15 | 红河学院 | Composite nano material and preparation method thereof, and electrochemical detection method of chrysophanol |
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Cited By (10)
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| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN105215347B (en) * | 2015-09-07 | 2017-03-29 | 济南大学 | A kind of Zinc Oxide and gold nano grain composite and preparation method thereof |
| CN105195144A (en) * | 2015-10-15 | 2015-12-30 | 吉林大学 | Method for synthetizing Au/ZnO bar-shaped heterojunction photocatalyst |
| CN106391008A (en) * | 2016-09-21 | 2017-02-15 | 苏州大学 | Method for loading three-dimensional zinc oxide surface with metal nanoparticles |
| CN107175339A (en) * | 2017-05-23 | 2017-09-19 | 天津工业大学 | A kind of method and device without reducing agent Fast back-projection algorithm gold nano grain |
| CN108440767A (en) * | 2018-04-18 | 2018-08-24 | 西北大学 | It is a kind of that nanometer Au is combined to the new method for preparing Au@MOF composite materials with porous MOF |
| CN110150317A (en) * | 2019-05-30 | 2019-08-23 | 吉林大学 | A kind of PDMS-ZnO/Au sterilization material of noble metal decorated semiconductor nano-pillar array structure and preparation method thereof |
| CN110150317B (en) * | 2019-05-30 | 2021-12-07 | 吉林大学 | PDMS-ZnO/Au sterilization material with noble metal modified semiconductor nano-pillar array structure and preparation method thereof |
| CN111157595A (en) * | 2019-12-26 | 2020-05-15 | 红河学院 | Composite nano material and preparation method thereof, and electrochemical detection method of chrysophanol |
| CN111157595B (en) * | 2019-12-26 | 2023-02-07 | 红河学院 | Composite nano material and preparation method thereof, and electrochemical detection method of chrysophanol |
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