CN103496733A - Method for preparing carbon doped zinc oxide - Google Patents
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Abstract
The invention provides a method for preparing carbon doped zinc oxide. The method comprises the following steps: dissolving zinc gluconate in water to obtain a zinc gluconate solution, and then, regulating pH value of the zinc gluconate solution to be 6-8; adding the zinc gluconate solution, of which pH value is regulated, into a microwave hydrothermal synthesis instrument, performing a synthetic reaction at 180-250 DEG C, and then, cooling naturally to room temperature to get a product; centrifugally separating the product, collecting solid, and then, washing and drying the solid to obtain a brown zinc oxide precursor; and calcining the brown zinc oxide precursor to obtain the carbon doped zinc oxide. The method has the characteristics of short reaction time, high efficiency and excellent repeatability; the zinc gluconate is used as the raw material, thus, the method is environmental-friendly and pollution-free. The carbon doped zinc oxide prepared by the method has uniform granularity, has a loose and porous structure, and has the characteristics of high specific surface area, high purity, excellent carbon doping amount controllability and good visible light absorption.
Description
Technical field
The invention belongs to the semiconductor material preparing technical field, be specifically related to a kind of preparation method of carbon doping zinc-oxide.
Background technology
ZnO is a kind of novel direct band-gap semicondictor material, its energy gap is 3.2eV, exciton bind energy is 60meV, good photoelectric characteristic is arranged, can be widely used in the fields such as photodiode, photochemical catalysis, solar cell, gas sensor, biosensor, cause scientific worker's concern.In recent years, along with the develop rapidly of nanosecond science and technology, the nano-ZnO of different-shape is made by several different methods by people, shows the physical and chemical performance of a lot of uniquenesses.Wherein, extremely researchist's favor of the photocatalysis performance of nano-ZnO.At present, people have carried out large quantity research for it, but mainly concentrate on the pattern of controlling ZnO, improve its specific surface area, have only improved the catalytic activity of material under UV-irradiation.And UV-light only accounts for 5% of sunlight, although these work intention novelties are also not within the foreseeable future from practical application.With UV-light, compare, visible ray accounts for 46% of sunlight.Therefore, on the basis of preparing the high-specific surface area pattern, developing the ZnO photocatalyst material with high visible light catalytic activity has very important meaning for its practical application.
At present, usually by the metallic element ion doping, as Fe, Cr, Sb, Co, Mn and Ni or non-metallic element N, C, S, adulterate to improve the receptivity of conductor oxidate to visible ray, also obtain certain achievement.But, with respect to take transition metal ion as main cation doping, the research of anion doped photocatalyst is less, and method is more complicated.Chinese invention patent 201210466728.4 has been reported the method for the carbon-doped mesoporous ZnO of a kind of simple preparation hamburger structure nano assembly.The method be take ethylene glycol as reaction solvent, inorganic salt zinc acetate and the excessive alkali source of transition metal of take is pre-reaction material, add structure directing agent glucose, drive the ZnO nano particle self-assembly that has realized the carbon doping by induced polymerization and twin polarity field.Chinese invention patent 201110332997.7 has been reported a kind of carbon doped semiconductor oxide compound with visible light catalysis activity and preparation method thereof, metal-salt, urea and carbon source are dissolved in distilled water and stir and obtain precursor solution, be placed in the autoclave sealed reaction; Cooling, deionized water wash, vacuum-drying; Then roasting, make carbon doped semiconductor oxide compound.Above-mentioned preparation method all need to add structure directing agent in reaction system or add urea and the material such as carbon source participate in synthetic, the condition harshness, complex process, be unfavorable for industrialization.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who prepares the carbon doping zinc-oxide, the method has that the reaction times is short, and temperature of reaction is low, simple to operate, reproducible advantage.
For achieving the above object, the present invention adopts following technical scheme:
The present invention includes following steps:
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, the pH value of then regulating the gluconic acid zinc solution is 6-8; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.1～1mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value is put into the microwave hydrothermal synthesizer, under 180 ℃～250 ℃, carries out building-up reactions, then naturally cools to room temperature, obtains product;
3) product is carried out to centrifugation, collect solid, then will after solids wash, oven dry, obtain brown zinc oxide precursor;
4) brown zinc oxide precursor is calcined under 200～400 ℃, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
PH value in described step 1) is to adopt KOH solution, and NaOH solution or ammoniacal liquor are regulated.
The concentration of described KOH solution, NaOH solution, ammoniacal liquor be 0.2 ?1mol/L.
Described step 2) in, the time of building-up reactions is 1h～3h.
In described step 3), washing is specially respectively with deionized water and absolute ethanol washing solid.
The time of calcining in described step 4) is 0.5～2 hour.
The present invention has following beneficial effect: the present invention be take Zinc Gluconate as starting material, without inductor or the carbon source of adding other, utilize the presoma of microwave-assisted hydro-thermal method synthesizing zinc oxide, then by the synthetic carbon doping zinc-oxide with vesicular structure of the method for low temperature calcination.In the present invention, calcining temperature is low, can complete the doping of carbon at the temperature of 200～400 ℃; Adopt the hydrothermal synthesis method of microwave-assisted to make the present invention have the reaction times short, efficiency is high, reproducible characteristics; Take Zinc Gluconate as the starting material environmental friendliness pollution-free; The carbon doping zinc-oxide epigranular that the present invention makes, have loose and porous structure, and the characteristics that specific surface area is high, purity is high, carbon doping controllability is good, visible absorption is excellent, can be applicable to visible light photocatalysis, field of solar energy utilization.
The accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the carbon doping zinc-oxide that prepared by the present invention; Wherein Fig. 1 (a) is the XRD contrast of product before and after calcining; Fig. 1 (b) is the XRD partial enlarged drawing of calcining after product;
Fig. 2 is scanning electron microscope (SEM) photo of the carbon doping zinc-oxide for preparing of the present invention; Wherein Fig. 2 (a) is the pattern of 5000 times of carbon doping zinc-oxides; Fig. 2 (b) is the pattern of 20000 times of carbon doping zinc-oxides; Fig. 2 (c) is the pattern of 100000 times of carbon doping zinc-oxides;
Fig. 3 is the uv-visible absorption spectra of the carbon doping zinc-oxide for preparing of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the NaOH solution of 0.2mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 6; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.1mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 3h under 180 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 2 hours in 200 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
The visible absorption intensity of the present embodiment gained carbon doping zinc-oxide is 0.23.
Embodiment 2
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the NaOH solution of 1mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 8; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 1mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 1h under 250 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 0.5 hour in 400 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
The visible absorption intensity of the present embodiment gained carbon doping zinc-oxide is 0.15.
Embodiment 3
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the NaOH solution of 0.5mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 7; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.5mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 2h under 200 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 1 hour in 300 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
The visible absorption intensity of the present embodiment gained carbon doping zinc-oxide is 0.45.
Embodiment 4
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the NaOH solution of 0.8mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 7; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.3mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 2h under 220 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 0.5 hour in 350 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
The visible absorption intensity of the present embodiment gained carbon doping zinc-oxide is 0.30.
Embodiment 5
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the KOH solution of 0.2mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 6.5; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.6mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 1.5h under 190 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 1.5 hours in 250 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
Embodiment 6
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the ammoniacal liquor of 1mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 7.5; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.8mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 2.5h under 235 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 2 hours in 200 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
Embodiment 7
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the KOH solution of 1mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 6; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.6mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 3h under 180 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 1 hour in 400 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
Embodiment 8
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, then use the ammoniacal liquor of 0.2mol/L as pH adjusting agent, the pH value of regulating the gluconic acid zinc solution is 8; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.8mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value joins in micro-wave diminishing pot, then micro-wave diminishing pot is moved in the microwave hydrothermal synthesizer, carries out building-up reactions 1h under 250 ℃, then naturally cools to room temperature, obtains product;
3) by product by centrifugation, collect solid, then by solid respectively with deionized water and absolute ethanol washing, after oven dry, obtain brown zinc oxide precursor;
4) product is calcined 2 hours in 200 ℃ of lower air atmospheres, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
Refer to shown in Fig. 1 the XRD figure spectrum that Fig. 1 is the carbosphere for preparing of the inventive method.By Fig. 1 (a), can be found out: the ZnO crystallinity before calcining is bad, purity is not high, and the ZnO after calcining is pure phase and the ZnO with hexagonal wurtzite structure.By Fig. 1 (b), can be found out: the diffraction peak position of the zinc oxide after calcining is offset to the wide-angle direction, illustrate that distortion has occurred the ZnO lattice, because the radius of covalency carbon is 77 micromicrons, be far smaller than radius 140 micromicrons of oxonium ion, illustrate that carbon has successfully replaced partial oxygen in zinc oxide, has realized doping.
Refer to shown in Fig. 2 the SEM pattern that Fig. 2 is the carbon doping zinc-oxide for preparing of the present invention.By Fig. 2 (a), can be found out: the size of carbon doping zinc-oxide prepared by the present invention is in 5 about μ m, and has the structure of porosity and looseness; By Fig. 2 (b), can be found out: the particle surface at the carbon doping zinc-oxide has many nano level holes; By Fig. 2 (c), can be found out: the carbon doping zinc-oxide is to be assembled by a lot of nano particles, and the size of these particles is about 50-100nm.
Refer to shown in Fig. 3, Fig. 3 is the uv-visible absorption spectra of the carbon doping zinc-oxide for preparing of the present invention.As can be seen from Figure 3: compare pure zinc oxide, carbon doping zinc-oxide prepared by the present invention not only has stronger receptivity in the UV-light zone, and absorption peak is to the light zone being offset, in visible region, (400nm～800nm) also shown stronger receptivity, carbon doping zinc-oxide prepared by the present invention has excellent visible light-responded ability, in visible light photocatalysis, field of solar energy utilization, is well worth doing.
The present invention is usingd Zinc Gluconate as raw material, after it is dissolved in water, regulates pH to 6-8, again through microwave hydrothermal reaction, washing, drying, obtain zinc oxide precursor, then, by low temperature calcination (200-400 ℃), can obtain the highly purified carbon doping zinc-oxide with vesicular structure.The present invention be take Zinc Gluconate as starting material, without adding other inductors or carbon source, utilizes the presoma of microwave-assisted hydro-thermal method synthesizing zinc oxide, then by the synthetic carbon doping zinc-oxide with loose and porous structure of the method for low temperature calcination.The carbon doping zinc-oxide that the present invention obtains has the advantages that specific surface area is high, purity is high, carbon doping controllability is good, visible absorption is excellent.
Claims (6)
1. a method for preparing the carbon doping zinc-oxide, is characterized in that, comprises the following steps:
1) Zinc Gluconate is dissolved in water, obtains the gluconic acid zinc solution, the pH value of then regulating the gluconic acid zinc solution is 6-8; Wherein, Zinc Gluconate glucose in solutions acid zinc concentration is 0.1～1mol/L;
2) the gluconic acid zinc solution that will regulate after the pH value is put into the microwave hydrothermal synthesizer, under 180 ℃～250 ℃, carries out building-up reactions, then naturally cools to room temperature, obtains product;
3) product is carried out to centrifugation, collect solid, then will after solids wash, oven dry, obtain brown zinc oxide precursor;
4) brown zinc oxide precursor is calcined under 200～400 ℃, naturally cooled to room temperature, obtain the carbon doping zinc-oxide.
2. a kind of method for preparing the carbon doping zinc-oxide according to claim 1, is characterized in that, the pH value in described step 1) is to adopt KOH solution, and NaOH solution or ammoniacal liquor are regulated.
3. a kind of method for preparing the carbon doping zinc-oxide according to claim 2, is characterized in that, the concentration of described KOH solution, NaOH solution, ammoniacal liquor be 0.2 ?1mol/L.
4. a kind of method for preparing the carbon doping zinc-oxide according to claim 1, is characterized in that described step 2) in time of building-up reactions be 1h～3h.
5. a kind of method for preparing the carbon doping zinc-oxide according to claim 1, is characterized in that, in described step 3), washing is specially respectively with deionized water and absolute ethanol washing solid.
6. a kind of method for preparing the carbon doping zinc-oxide according to claim 1, is characterized in that, the time of calcining in described step 4) is 0.5～2 hour.
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Cited By (7)
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| CN104148047A (en) * | 2014-08-31 | 2014-11-19 | 华东理工大学 | Macro preparation method for carbon doped zinc oxide-based visible-light catalyst |
| CN104445372A (en) * | 2014-11-26 | 2015-03-25 | 燕山大学 | Method for preparing carbon doped zinc oxide nanoparticles |
| CN105272206A (en) * | 2015-10-13 | 2016-01-27 | 北京科技大学 | Preparation method of C and Ni co-doped ZnO thermoelectric material |
| CN109638244A (en) * | 2018-12-05 | 2019-04-16 | 岭南师范学院 | A kind of zinc sulphide@carbon complex microsphere and the preparation method and application thereof |
| CN110203963A (en) * | 2019-04-30 | 2019-09-06 | 昆明理工大学 | A method of recycling expired zinc gluconate |
| CN113680291A (en) * | 2021-09-09 | 2021-11-23 | 吉林农业大学 | Preparation method of paramagnetic metal oxide/spinel/carbon composite microsphere |
| CN116253315A (en) * | 2023-03-13 | 2023-06-13 | 山东大学 | Glucose-zinc gluconate carbonized polymer dot and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104148047A (en) * | 2014-08-31 | 2014-11-19 | 华东理工大学 | Macro preparation method for carbon doped zinc oxide-based visible-light catalyst |
| CN104148047B (en) * | 2014-08-31 | 2017-02-01 | 华东理工大学 | Macro preparation method for carbon doped zinc oxide-based visible-light catalyst |
| CN104445372A (en) * | 2014-11-26 | 2015-03-25 | 燕山大学 | Method for preparing carbon doped zinc oxide nanoparticles |
| CN104445372B (en) * | 2014-11-26 | 2016-03-02 | 燕山大学 | A kind of method preparing carbon doping Zinc oxide nanoparticle |
| CN105272206A (en) * | 2015-10-13 | 2016-01-27 | 北京科技大学 | Preparation method of C and Ni co-doped ZnO thermoelectric material |
| CN105272206B (en) * | 2015-10-13 | 2017-08-08 | 北京科技大学 | A kind of preparation method of C and Ni codopes ZnO thermoelectric materials |
| CN109638244A (en) * | 2018-12-05 | 2019-04-16 | 岭南师范学院 | A kind of zinc sulphide@carbon complex microsphere and the preparation method and application thereof |
| CN110203963A (en) * | 2019-04-30 | 2019-09-06 | 昆明理工大学 | A method of recycling expired zinc gluconate |
| CN113680291A (en) * | 2021-09-09 | 2021-11-23 | 吉林农业大学 | Preparation method of paramagnetic metal oxide/spinel/carbon composite microsphere |
| CN113680291B (en) * | 2021-09-09 | 2023-12-01 | 吉林农业大学 | Preparation method of paramagnetic metal oxide/spinel/carbon composite microsphere |
| CN116253315A (en) * | 2023-03-13 | 2023-06-13 | 山东大学 | Glucose-zinc gluconate carbonized polymer dot and preparation method and application thereof |
| CN116253315B (en) * | 2023-03-13 | 2024-05-24 | 山东大学 | Glucose-zinc gluconate carbonized polymer dot and preparation method and application thereof |
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Application publication date: 20140108 |