CN103145113A - Micro-nano structure zinc oxide-carbon composite pellet and preparation method thereof - Google Patents
Micro-nano structure zinc oxide-carbon composite pellet and preparation method thereof Download PDFInfo
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- CN103145113A CN103145113A CN201110415313XA CN201110415313A CN103145113A CN 103145113 A CN103145113 A CN 103145113A CN 201110415313X A CN201110415313X A CN 201110415313XA CN 201110415313 A CN201110415313 A CN 201110415313A CN 103145113 A CN103145113 A CN 103145113A
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Abstract
The invention discloses a micro-nano structure zinc oxide-carbon composite pellet and a preparation method thereof. The micro-nano structure zinc oxide-carbon composite pellet is obtained by hybridization compounding of zinc oxide and carbon to obtain a solid pellet having the diameter of 6-12 micrometers, wherein vertical nanosheets having the length of 700-900 nanometers, the height of 700-900 nanometers and the thickness of 15 to 25 nanometers are formed on surfaces of the solid pellet and are connected with each other into a nest; a mole ratio of zinc oxide to carbon is (60-70%): (30-40%); zinc oxide has a hexagonal structure; and carbon comprises amorphous carbon and graphitized carbon and a weight ratio of the amorphous carbon to the graphitized carbon is (85-95%): (5-15%). The preparation method comprises the following steps of dissolving zinc acetate dihydrate, urea, sodium citrate dihydrate and glucose in water to obtain a mixed solution, carrying out hydrothermal treatment on the mixed solution to obtain a reaction solution, orderly carrying out solid-liquid separation, washing and drying to obtain an intermediate product, putting the intermediate product in an inert gas atmosphere, and carrying out annealing to obtain the micro-nano structure zinc oxide-carbon composite pellet. The micro-nano structure zinc oxide-carbon composite pellet can be widely used for fields of catalysis, adsorption and photoelectricity.
Description
Technical field
The present invention relates to a kind of compound ball and preparation method, especially a kind of micro-nano structure zinc oxide-carbon compound ball and preparation method thereof.
Background technology
Zinc oxide is the good semiconductor material of a class, and application is very widely being arranged aspect environmental improvement and opto-electronic device; Photocatalysis performance as good in it can even be degraded into carbonic acid gas and water with toxic organic pollutant under the irradiation of daylight in UV-light, utilize its good piezoelectric property it can be made the nano generator device, its good opto-electronic conversion performance can make it be applied in solar cell on a large scale.Carbon material with excellent conductive capability and absorption property all has a wide range of applications at photoelectricity and Chu Qing field.Based on above 2 points, in the recent period, people are in order to obtain zinc oxide-carbon composite, made unremitting effort, as (Chinese excellent MA theses full-text database o. 11th, Cao Yang) the 26th～27 page of a literary composition discloses a kind of ZnO-carbosphere and its preparation method in " preparation of carbon, ZnO/ carbon porous microsphere and the applied research on lithium ion battery negative thereof ".The spherical diameter of the ZnO-carbosphere of mentioning in this article is 300nm～3 μ m, and surface and inside that its spherical ZnO uniform particles that is 80nm by diameter is distributed in carbosphere consist of, and having bore dia on the surface of carbosphere is the hole defect of receiving of 5～10nm; The preparation method for first with glucose crystal and zinc acetate ultrasonic dissolution in distilled water, obtain clear solution, again clear solution is placed in air-tight state, react 12～18h under 180 ℃, obtain the reaction product of brown or black particle, through to its centrifugation, repeatedly after washing and drying, be placed under argon atmospher in 500 ℃ of high temperature annealing 2h, obtain final product--the ZnO-carbosphere.Yet, no matter be final product, or its preparation method, the shortcoming part is arranged, at first too smooth also though hole defect is received on the surface of ZnO-carbosphere, make its difficulty that larger specific surface area be arranged; Secondly, obvious interface is arranged between Zinc oxide particles and carbosphere, this illustrates that the tightness of both combinations is not too desirable; At last, the temperature of reaction in the preparation method is higher, overlong time, and the temperature during annealing is also higher, makes it both during energy charge, can not obtain again the final product of high specific surface area.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of have high specific surface area, constitutionally stable micro-nano structure zinc oxide-carbon compound ball for overcoming shortcoming part of the prior art.
Another technical problem that the present invention will solve is for providing the preparation method of a kind of above-mentioned micro-nano structure zinc oxide-carbon compound ball.
For solving technical problem of the present invention, the technical scheme that adopts is: micro-nano structure zinc oxide-carbon compound ball consists of solid sphere by zinc oxide and carbon, particularly,
Described solid sphere is formed by zinc oxide and carbon hybridization compounding, and its spherical diameter is 6～12 μ m, the nanometer sheet of ball surface for standing;
The length of a film of described nanometer sheet is the high 700～900nm of being of 700～900nm, sheet, the thick 15～25nm of being of sheet, is interconnected to nest between sheet and sheet;
The molar percentage of described zinc oxide and carbon is 60～70%: 30～40%, and wherein, zinc oxide is six side's phase structures, and carbon is amorphous carbon and graphitized carbon, and the weight percent of described amorphous carbon and graphitized carbon is 85～95wt%: 5～15wt%.
As the further improvement of micro-nano structure zinc oxide-carbon compound ball, described nest is Polygons; Described Polygons is trilateral, or tetragon, or sexangle.
For solving another technical problem of the present invention, another technical scheme that adopts is: the preparation method of above-mentioned micro-nano structure zinc oxide-carbon compound ball comprises hydrothermal method, and particularly completing steps is as follows:
Step 1, be first 0.64～0.68: 0.52～0.56 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: 0.05～0.07: 0.8～1.2: 48～52 ratio, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution, again mixed solution is placed in air-tight state, be to react 2h at least under 120～160 ℃ in temperature, obtain reaction solution;
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution, obtains intermediate product, then intermediate product is placed in inert gas atmosphere, and the 1h at least that anneals under 300～400 ℃ makes micro-nano structure zinc oxide-carbon compound ball.
As the preparation method's of micro-nano structure zinc oxide-carbon compound ball further improvement, described solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 3000～5000r/min; Described carrying out washing treatment is for using deionized water and ethanol to clean; Described drying treatment is for to dry under 10～50 ℃; Described is that rare gas element is one or more the mixed gas in nitrogen, argon gas, helium.
Beneficial effect with respect to prior art is, one uses respectively scanning electron microscope, transmission electron microscope, X-ray diffractometer and Raman spectrometer to characterize to the target product that makes, and by its result as can be known, target product is the stand solid sphere of nanometer sheet of its surface; Wherein, the spherical diameter of solid sphere is 6～12 μ m, and the length of a film of nanometer sheet is the high 700～900nm of being of 700～900nm, sheet, the thick 15～25nm of being of sheet, is interconnected to nest between sheet and sheet.Target product is formed by zinc oxide and carbon hybridization compounding; The molar percentage of zinc oxide and carbon is 60～70%: 30～40%, and zinc oxide wherein is six side's phase structures, and carbon is amorphous carbon and graphitized carbon, and the weight percent of amorphous carbon and graphitized carbon is 85～95wt%: 5～15wt%.They are two years old, preparation method's science, effective, both energy-and time-economizing, be beneficial to commercial scale production, make again the target product that makes that higher specific surface area is arranged, also because of the carbon surface contain a large amount of functional groups make zinc oxide and carbon after hybridization compounding in conjunction with very tight, greatly improved the stability of its structure, more the existence due to a large amount of functional groups in carbon surface makes target product in absorption and catalytic field, potential application prospect be arranged.
As the further embodiment of beneficial effect, the one, nest is preferably Polygons, and Polygons is preferably trilateral, or tetragon, or sexangle, is beneficial to leaning on each other for support between nanometer sheet, has improved the stability that nanometer sheet is stood.The 2nd, solid-liquid separation is processed and is preferably centrifugation, and the rotating speed during separation is preferably 3000～5000r/min, is convenient to the effective separation between solid-liquid.The 3rd, carrying out washing treatment is preferably uses deionized water and ethanol to clean, and has guaranteed the pure of intermediate product.The 4th, drying treatment is preferably under 10～50 ℃ dries, and has guaranteed the quality of intermediate product.The 5th, rare gas element is preferably one or more the mixed gas in nitrogen, argon gas, helium, not only makes the source of raw material than horn of plenty, preparation technology is more easily implemented and flexibly.
Description of drawings
Below in conjunction with accompanying drawing, optimal way of the present invention is described in further detail.
Fig. 1 uses one of result that scanning electron microscope (SEM) characterizes to the target product that makes.Wherein, Fig. 1 a is the low range SEM photo of target product, and Fig. 1 b is the high magnification photo of Fig. 1 a, Fig. 1 c is the high magnification photo of Fig. 1 b, can be found out by Fig. 1 b and Fig. 1 c, and target product is globe, its surface a large amount of nanometer sheet of standing is interconnected to nest between nanometer sheet; The EDS spectrogram of Fig. 1 d for obtaining after the target product shown in Fig. 1 a being used subsidiary power spectrum (EDS) test component of scanning electron microscope characterize, can find out that by the EDS spectrogram target product contains zinc, oxygen and three kinds of elements of carbon, wherein, the ratio of Zn and 0 relative atom molar content is approximately 1: 1, be the structure of ZnO, the atomic molar content of C is about 30～40%.
Fig. 2 uses one of result that transmission electron microscope (TEM) characterizes to the target product that makes.Wherein, Fig. 2 a is the TEM photo of single target product, and by it as can be known, spherical target product is solid construction; Fig. 2 b is the high resolving power TEM photo of the nanometer sheet of target product shown in Fig. 2 a, and the high resolving power TEM photo of this single nanometer sheet has demonstrated the nanometer sheet surface carbon striped clearly.
Fig. 3 uses one of result that X-ray diffraction (XRD) instrument characterizes to the target product that makes.Can be found out by XRD spectra, the spectrogram of target product is identical with the standard spectrogram JCPDS Number:36-1451 of zinc oxide six side's phase structures.
Fig. 4 is one of result that respectively intermediate product that obtains and the target product use Raman spectrometer that makes is characterized.Curve a in spectrogram is the spectral line of target product, and curve b is the spectral line of intermediate product; Can be found out by spectrogram, intermediate product and target product are all at 1340cm
-1And 1580cm
-1Near amorphous peak and the greying peak of two carbon are arranged, illustrate and wherein contain amorphous carbon and graphited carbon.
Embodiment
At first buy from market or make with ordinary method:
Two hydration zinc acetates; Urea; Two hydration Trisodium Citrates; Glucose; Water; Deionized water; Ethanol; As one or more the mixed gas in the nitrogen of rare gas element, argon gas, helium.
Then,
Embodiment 1
The concrete steps of preparation are:
Step 1, it it is first 0.64: 0.56: 0.05 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: the ratio of 1.2: 48, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution.Again mixed solution being placed in air-tight state, is to react 4h under 120 ℃ in temperature, obtains reaction solution.
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution; Wherein, solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 3000r/min, and carrying out washing treatment is for using deionized water and ethanol to clean, and drying treatment obtains intermediate product for to dry under 10 ℃.Again intermediate product is placed in inert gas atmosphere, 2h anneals under 300 ℃; Wherein, rare gas element is nitrogen, make be similar to illustrated in figures 1 and 2, and the zinc oxide of the micro-nano structure as shown in the curve in Fig. 3 and Fig. 4-carbon compound ball.
Embodiment 2
The concrete steps of preparation are:
Step 1, it it is first 0.65: 0.55: 0.055 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: the ratio of 1.1: 49, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution.Again mixed solution being placed in air-tight state, is to react 3.5h under 130 ℃ in temperature, obtains reaction solution.
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution; Wherein, solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 3500r/min, and carrying out washing treatment is for using deionized water and ethanol to clean, and drying treatment obtains intermediate product for to dry under 20 ℃.Again intermediate product is placed in inert gas atmosphere, 1.8h anneals under 330 ℃; Wherein, rare gas element is nitrogen, make be similar to illustrated in figures 1 and 2, and the zinc oxide of the micro-nano structure as shown in the curve in Fig. 3 and Fig. 4-carbon compound ball.
Embodiment 3
The concrete steps of preparation are:
Step 1, it it is first 0.66: 0.54: 0.06 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: the ratio of 1: 50, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution.Again mixed solution being placed in air-tight state, is to react 3h under 140 ℃ in temperature, obtains reaction solution.
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution; Wherein, solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 4000r/min, and carrying out washing treatment is for using deionized water and ethanol to clean, and drying treatment obtains intermediate product for to dry under 30 ℃.Again intermediate product is placed in inert gas atmosphere, 1.5h anneals under 350 ℃; Wherein, rare gas element is nitrogen, make as depicted in figs. 1 and 2, and the zinc oxide of the micro-nano structure as shown in the curve in Fig. 3 and Fig. 4-carbon compound ball.
Embodiment 4
The concrete steps of preparation are:
Step 1, it it is first 0.67: 0.53: 0.065 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: the ratio of 0.9: 51, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution.Again mixed solution being placed in air-tight state, is to react 2.5h under 150 ℃ in temperature, obtains reaction solution.
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution; Wherein, solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 4500r/min, and carrying out washing treatment is for using deionized water and ethanol to clean, and drying treatment obtains intermediate product for to dry under 40 ℃.Again intermediate product is placed in inert gas atmosphere, 1.3h anneals under 380 ℃; Wherein, rare gas element is nitrogen, make be similar to illustrated in figures 1 and 2, and the zinc oxide of the micro-nano structure as shown in the curve in Fig. 3 and Fig. 4-carbon compound ball.
Embodiment 5
The concrete steps of preparation are:
Step 1, it it is first 0.68: 0.52: 0.07 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: the ratio of 0.8: 52, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution.Again mixed solution being placed in air-tight state, is to react 2h under 160 ℃ in temperature, obtains reaction solution.
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution; Wherein, solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 5000r/min, and carrying out washing treatment is for using deionized water and ethanol to clean, and drying treatment obtains intermediate product for to dry under 50 ℃.Again intermediate product is placed in inert gas atmosphere, 1h anneals under 400 ℃; Wherein, rare gas element is nitrogen, make be similar to illustrated in figures 1 and 2, and the zinc oxide of the micro-nano structure as shown in the curve in Fig. 3 and Fig. 4-carbon compound ball.
Select respectively again one or more the mixed gas in nitrogen as rare gas element, argon gas, helium, repeat above-described embodiment 1～5, made equally as or be similar to illustrated in figures 1 and 2, and the zinc oxide of the micro-nano structure as shown in the curve in Fig. 3 and Fig. 4-carbon compound ball.
Obviously, those skilled in the art can carry out various changes and modification and not break away from the spirit and scope of the present invention micro-nano structure zinc oxide of the present invention-carbon compound ball and preparation method thereof.Like this, if of the present invention these are revised and within modification belongs to the scope of claim of the present invention and equivalent technologies thereof, the present invention also is intended to comprise these changes and modification interior.
Claims (8)
1. micro-nano structure zinc oxide-carbon compound ball, consist of solid sphere by zinc oxide and carbon, it is characterized in that:
Described solid sphere is formed by zinc oxide and carbon hybridization compounding, and its spherical diameter is 6～12 μ m, the nanometer sheet of ball surface for standing;
The length of a film of described nanometer sheet is the high 700～900nm of being of 700～900nm, sheet, the thick 15～25nm of being of sheet, is interconnected to nest between sheet and sheet;
The molar percentage of described zinc oxide and carbon is 60～70%: 30～40%, and wherein, zinc oxide is six side's phase structures, and carbon is amorphous carbon and graphitized carbon, and the weight percent of described amorphous carbon and graphitized carbon is 85～95wt%: 5～15wt%.
2. micro-nano structure zinc oxide according to claim 1-carbon compound ball, is characterized in that nest is Polygons.
3. micro-nano structure zinc oxide according to claim 2-carbon compound ball, is characterized in that Polygons is trilateral, or tetragon, or sexangle.
4. the preparation method of the described micro-nano structure zinc oxide of claim 1-carbon compound ball, comprise hydrothermal method, it is characterized in that completing steps is as follows:
Step 1, be first 0.64～0.68: 0.52～0.56 according to the weight ratio between two hydration zinc acetates, urea, two hydration Trisodium Citrates, glucose and water: 0.05～0.07: 0.8～1.2: 48～52 ratio, two hydration zinc acetates, urea, two hydration Trisodium Citrates and glucose are dissolved in the water, obtain mixed solution, again mixed solution is placed in air-tight state, be to react 2h at least under 120～160 ℃ in temperature, obtain reaction solution;
Step 2 is first carried out solid-liquid separation, washing and dry processing successively to reaction solution, obtains intermediate product, then intermediate product is placed in inert gas atmosphere, and the 1h at least that anneals under 300～400 ℃ makes micro-nano structure zinc oxide-carbon compound ball.
5. the preparation method of micro-nano structure zinc oxide according to claim 4-carbon compound ball, is characterized in that solid-liquid separation is treated to centrifugation, and the rotating speed during separation is 3000～5000r/min.
6. the preparation method of micro-nano structure zinc oxide according to claim 4-carbon compound ball, is characterized in that carrying out washing treatment is to use deionized water and ethanol to clean.
7. the preparation method of micro-nano structure zinc oxide according to claim 4-carbon compound ball, is characterized in that drying treatment is to dry under 10～50 ℃.
8. the preparation method of micro-nano structure zinc oxide according to claim 4-carbon compound ball is characterized in that rare gas element is one or more the mixed gas in nitrogen, argon gas, helium.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103877961A (en) * | 2014-03-05 | 2014-06-25 | 北京大学 | Carbon-based zinc oxide nanosphere composite material and preparation method thereof |
| CN103979525A (en) * | 2014-05-22 | 2014-08-13 | 辽宁大学 | Preparation method of acidyl-rich spherical carbon material |
| CN104307501A (en) * | 2014-10-31 | 2015-01-28 | 西南民族大学 | Method for preparing nano-zinc oxide used as photocatalyst |
| CN104857945A (en) * | 2015-04-30 | 2015-08-26 | 信阳师范学院 | Preparation method of zinc oxide/carbon micro-sphere composite material |
| CN104941625A (en) * | 2015-07-01 | 2015-09-30 | 盐城工学院 | Black zinc oxide and preparation method thereof |
| CN113772717A (en) * | 2021-01-15 | 2021-12-10 | 冯天生 | Nitrogen-doped mesoporous carbon-ZnO composite material and application thereof in super capacitor |
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| CN101311119A (en) * | 2007-05-25 | 2008-11-26 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
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| CN101311119A (en) * | 2007-05-25 | 2008-11-26 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103877961A (en) * | 2014-03-05 | 2014-06-25 | 北京大学 | Carbon-based zinc oxide nanosphere composite material and preparation method thereof |
| CN103877961B (en) * | 2014-03-05 | 2016-01-27 | 北京大学 | A kind of charcoal base zinc oxide nanosphere composite and preparation method thereof |
| CN103979525A (en) * | 2014-05-22 | 2014-08-13 | 辽宁大学 | Preparation method of acidyl-rich spherical carbon material |
| CN104307501A (en) * | 2014-10-31 | 2015-01-28 | 西南民族大学 | Method for preparing nano-zinc oxide used as photocatalyst |
| CN104857945A (en) * | 2015-04-30 | 2015-08-26 | 信阳师范学院 | Preparation method of zinc oxide/carbon micro-sphere composite material |
| CN104941625A (en) * | 2015-07-01 | 2015-09-30 | 盐城工学院 | Black zinc oxide and preparation method thereof |
| CN104941625B (en) * | 2015-07-01 | 2018-01-23 | 盐城工学院 | A kind of black oxidation zinc and preparation method thereof |
| CN113772717A (en) * | 2021-01-15 | 2021-12-10 | 冯天生 | Nitrogen-doped mesoporous carbon-ZnO composite material and application thereof in super capacitor |
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