CN107552034A - A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet - Google Patents
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet Download PDFInfo
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- CN107552034A CN107552034A CN201710717906.9A CN201710717906A CN107552034A CN 107552034 A CN107552034 A CN 107552034A CN 201710717906 A CN201710717906 A CN 201710717906A CN 107552034 A CN107552034 A CN 107552034A
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Abstract
The present invention provides a kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：（1）The basic zinc carbonate and small organic molecule for weighing certain mass respectively are ground, and both is sufficiently mixed uniformly；（2）By step（1）In be well mixed basic zinc carbonate and small organic molecule be placed under airfree vacuum environment, carry out calcination processing, naturally cool to room temperature afterwards；（3）By step（2）Middle obtained powder of calcining is ground, and the powder for grinding to obtain is exactly the Zinc oxide nano sheet of carbon doping.Zinc oxide nano sheet prepared by the present invention is laminated structure, the size of laminated structure is 1 microns, thickness is at 20 30 nanometers, in photocatalytic process, nanometer sheet has higher specific surface area, also there is stronger adsorption capacity, and present invention operation and process it is simple, it is quick, reproducible, beneficial to industrialized production.
Description
Technical field
The present invention relates to a kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet.
Background technology
Nano zine oxide is as important photochemical catalyst, and compared with traditional catalyst, it has higher catalytic activity, more
Because of its unique photochemical properties and photocatalysis performance, there is vast potential for future development in photocatalysis field.Pass through simple oxygen
Change reduction reaction, zinc oxide directly can efficiently degrade the multiple pollutant in sewage, and research of the researcher to its process is more.
The substantially process of catalyzing and degrading pollutant is carried out using nano zine oxide is：After surface of nanometer zinc oxide, photon can for illumination
The electron hole pair that exciting makes its surface is separated, and electronics leaves the hole with oxidisability after being transmitted away, can be right
Organic pollution oxidative degradation, ultimately form the H of environmental sound2O and CO2.But during practical study, it is nano oxidized
The photocatalytic degradation efficiency of zinc is simultaneously good not as desired, because nano zine oxide energy gap is larger, about
3.37 eV, and it is lower to sun light utilization efficiency, and the time is very short existing for electron hole pair, so as to reduce urging for it
Change activity, result in the reduction of photocatalysis efficiency.This to receive when nano zine oxide is tackling pollution problem very big
Limitation.
At present, light element is passed through（C, the nonmetalloid such as N, F）Zinc oxide is doped to widen its absorption spectrum, entered
It is one of focus of environmentally conscious materialses research field that one step, which improves photocatalysis efficiency,.Some existing relevant carbon-doped nanos that prepare aoxidize
The related application of zinc, for example, Chinese invention patent 201210466728.4 report it is a kind of easy prepare it is carbon-doped mesoporous
The method of zinc oxide hamburger structure nano assembly.This method is using ethylene glycol as reaction dissolvent, with the inorganic salts vinegar of transition metal
Sour zinc and the alkali source of excess are pre-reaction material, add structure directing agent glucose, pass through induced polymerization and twin polarity
Field driving realizes the Zinc oxide nanoparticle self assembly of carbon doping.Chinese invention patent 201110332997.7 reports one kind
Carbon doping conductor oxidate with visible light catalysis activity and preparation method thereof.Metal salt, urea and carbon source are dissolved in
Stirring obtains precursor solution in distilled water, is placed in autoclave and seals reaction；Cooling, deionized water washing, vacuum are done
It is dry；Then it is calcined, carbon doping conductor oxidate is made.Publication No. CN103496733A Chinese patent applications report one kind
Zinc gluconate is dissolved in water, obtains gluconic acid zinc solution, the pH value for then adjusting gluconic acid zinc solution is 6-8；
Gluconic acid zinc solution after regulation pH value is put into microwave attenuation materials instrument, synthetic reaction is carried out under 180-250 degree, so
After naturally cool to room temperature, obtain product；Product is centrifuged, collect solid, then solid is washed, dry after must
To zinc oxide precursor；Zinc oxide precursor is calcined again to obtain carbon doping zinc oxide.Above-mentioned preparation method preparation condition is harsh,
Technique is more and complicated, is unfavorable for industrializing.
The content of the invention
To solve the above problems, the present invention provides a kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, behaviour
Make and process it is simple, it is quick, reproducible, beneficial to industrialized production.
The technical scheme is that：A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including it is following
Preparation process：
（1）The basic zinc carbonate and small organic molecule for weighing certain mass respectively are ground, and both is sufficiently mixed
It is even；
（2）By step（1）In be well mixed basic zinc carbonate and small organic molecule be placed under airfree vacuum environment,
Calcination processing is carried out, naturally cools to room temperature afterwards；
（3）By step（2）Middle obtained powder of calcining is ground, and the powder for grinding to obtain is exactly the zinc oxide nano of carbon doping
Rice piece.
Step（1）In, small organic molecule is sucrose, oxalic acid, glucose, fructose or citric acid.
Step（1）The middle basic zinc carbonate and small organic molecule for weighing certain mass respectively, is placed in agate mortar
Row grinding 10-60min, makes both be sufficiently mixed uniformly.
Step（2）In be well mixed basic zinc carbonate and small organic molecule, quartz boat is uniformly laid in, by quartz
Boat is put into the quartz ampoule of tube furnace, and tube furnace is vacuumized, and quartz ampoule is placed under airfree vacuum environment,
Calcination processing is carried out at 300-800 DEG C, heating rate is 5 DEG C/min -20 DEG C/min, and room is naturally cooled to after insulation 2h-3h
Temperature.
Step（3）In, by step（2）Obtained powder is calcined to be ground with agate mortar.
The content of basic zinc carbonate and small organic molecule ratio is 4:1~8:1.
The present invention has the following advantages that compared with prior art:
1st, Zinc oxide nano sheet prepared by the present invention is laminated structure, and the size of laminated structure is 1 microns, and thickness is in 20-
30 nanometers, inhaled because nanometer sheet is made up of nano particle the pollutant for having space between nano particle and being easy to make to be catalyzed
It is attached in nanometer sheet, to be exactly secondly one-dimensional material nanometer sheet be more beneficial for light induced electron in photocatalytic process than zero dimension material passes
It is defeated, therefore in photocatalytic process, nanometer sheet has higher specific surface area than nano particle, it may have stronger energy of adsorption
Power.
2nd, the cost of raw material is low, and technique is simple, easy to operate, reproducible, and yield is high.
3rd, reaction condition can control, and the reaction time is short, reaction temperature is low, reproducible, beneficial to industrialized production.
4th, it is observed that carbon doping Zinc oxide nano sheet structure size prepared by the present invention is uniform by SEM pictures, leads to
It is pure phase to cross the carbon doping Zinc oxide nano sheet that X-ray diffraction spectrogram is observed that prepared by the present invention, is deposited without other impurity
It can make the carbon content of doping carbon dopings that are different, and preparing by the amount difference of carbon source fluorescence probe in, carbon doping amount
Zinc oxide is black, and the carbon doping zinc oxide of black has the characteristics of excellent to visible absorption.
5th, agate mortar has corrosion resistance in itself, resistance to pressure, will not make the material of mortar body dirty in process of lapping
The basic zinc carbonate and small organic molecule being ground in dye mortar body.
Brief description of the drawings
Fig. 1 is the ESEM of carbon doping Zinc oxide nano sheet prepared by the present invention（SEM）Picture.
Fig. 2 is the powder picture of carbon doping Zinc oxide nano sheet prepared by the present invention.
Fig. 3 is the X-ray diffraction of carbon doping Zinc oxide nano sheet prepared by the embodiment of the present invention 1（XRD）Figure.
Embodiment
Embodiment 1：
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）The basic zinc carbonate and small organic molecule of certain mass are weighed respectively, is ground, and both is sufficiently mixed
It is even.
（2）By step（1）In be well mixed basic zinc carbonate and small organic molecule be placed in airfree vacuum environment
Under, calcination processing is carried out, naturally cools to room temperature afterwards.
（3）By step（2）Middle obtained powder of calcining is ground, and the powder for grinding to obtain is exactly the oxidation of carbon doping
Zinc nanometer sheet.
Embodiment 2：
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）Weigh the basic zinc carbonate and small organic molecule of certain mass respectively, basic zinc carbonate and small organic molecule
Mass ratio is 4:1—8:1, basic zinc carbonate and small organic molecule are placed in agate mortar and are ground 10-60 min, make two
Person is sufficiently mixed uniformly；Small organic molecule is sucrose, oxalic acid, glucose, fructose or citric acid.
（2）By step（1）In be well mixed basic zinc carbonate and small organic molecule be uniformly laid in quartz boat,
Quartz boat is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 1 DEG C/min -10 DEG C/min, and room temperature is naturally cooled to after insulation 1h-5h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 3
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）2g basic zinc carbonate and 0.5g sucrose are weighed respectively, are placed in agate mortar and are ground 10-60 min, make
Both are sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and sucrose be uniformly laid in quartz boat, by quartz boat
It is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 10 DEG C/min, and room temperature is naturally cooled to after insulation 2h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
The Zinc oxide nano sheet of the carbon doping prepared to embodiment 3 detects
1st, the Zinc oxide nano sheet of the carbon doping prepared to embodiment 3 is scanned Electronic Speculum（SEM）, Fig. 1 is prepared by embodiment 3
The ESEM of carbon doping Zinc oxide nano sheet（SEM）Picture, with reference to Fig. 2 it can be seen that carbon doping oxidation prepared by embodiment 3
Zinc nanometer sheet is laminated structure, and the sheet size of nanometer sheet is about 800nm, thickness about 10nm, therefore deduces that the present invention
What is be prepared is the Zinc oxide nano sheet of carbon doping.
2nd, Fig. 2 is the powder picture of the Zinc oxide nano sheet of carbon doping prepared by 3-12 of the embodiment of the present invention, and wherein a figures are
The powder picture of pure zinc oxide, b illustrate the powder picture of carbon doping zinc oxide, pure zinc oxide powder can be could see with reference to picture
It is white, the Zinc oxide powder after carbon doping is black, because the presence of carbon causes powder that black is presented, also thus
The visible region of the zinc oxide of carbon doping, which can be illustrated, response.
3rd, the Zinc oxide nano sheet of the carbon doping prepared to embodiment 3 carries out X-ray diffraction, and Fig. 3 is prepared by embodiment 3
The X-ray diffraction of carbon doping Zinc oxide nano sheet（XRD）Figure, wherein illustration are partial enlarged drawings, and a, b curve are to be respectively in figure
The X-ray diffraction spectrogram of carbon doping Zinc oxide nano sheet prepared by pure zinc oxide and embodiment 3, is readily seen with reference to picture
Pure zinc oxide can be completely with zinc oxide standard card JCPDSNO.79-0704 coincide, and from X-ray diffraction spectrogram
It can be seen that the two is all pure phase and is all six side's fibre ore structures, exist without other impurities phases, while we can be young
Illustration can be seen that there occurs inclined to wide-angle direction for the diffraction maximum position of the Zinc oxide nano sheet of carbon doping in thin observation Fig. 3
Moving, the zinc oxide lattice in this explanation carbon doping Zinc oxide nano sheet is distorted, because the radius of covalent carbon is 77 micromicrons,
The far smaller than micromicron of radius 140 of oxonium ion, illustrate that carbon successfully instead of part oxygen in zinc oxide and realize doping.
Simple in the present invention, the quick method for preparing carbon doping Zinc oxide nano sheet can also be such as embodiment 4- embodiments
12, specific data parameters are changed, and sucrose replaces with oxalic acid, glucose, fructose or citric acid.
Embodiment 4
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）8g basic zinc carbonate and 0.5g sucrose are weighed respectively, are placed in agate mortar and are ground 20-60 min, make
Both are sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and sucrose be uniformly laid in quartz boat, by quartz boat
It is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 5 DEG C/min, and room temperature is naturally cooled to after insulation 3h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 5
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）2g basic zinc carbonate and 0.5g oxalic acid are weighed respectively, are placed in agate mortar and are ground 10-60 min, make
Both are sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and oxalic acid be uniformly laid in quartz boat, by quartz boat
It is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 15 DEG C/min, and room temperature is naturally cooled to after insulation 2h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 6
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）4g basic zinc carbonate and 0.5g oxalic acid are weighed respectively, are placed in agate mortar and are ground 10-50 min, make
Both are sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and oxalic acid be uniformly laid in quartz boat, by quartz boat
It is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 20 DEG C/min, and room temperature is naturally cooled to after insulation 3h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 7
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）3.2g basic zinc carbonate and 0.5g glucose are weighed respectively, are placed in agate mortar and are ground 10-
40min, both are made to be sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and glucose be uniformly laid in quartz boat, by quartz
Boat is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 5 DEG C/min, and room temperature is naturally cooled to after insulation 3h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 8
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）2.8g basic zinc carbonate and 0.5g glucose are weighed respectively, are placed in agate mortar and are ground 20-50
Min, both are made to be sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and glucose be uniformly laid in quartz boat, by quartz
Boat is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 8 DEG C/min, and room temperature is naturally cooled to after insulation 2h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 9
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）3g basic zinc carbonate and 0.5g fructose are weighed respectively, are placed in agate mortar and are ground 10-60 min, make
Both are sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and fructose be uniformly laid in quartz boat, by quartz boat
It is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 12 DEG C/min, and room temperature is naturally cooled to after insulation 2h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 10
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）3.5g basic zinc carbonate and 0.5g fructose are weighed respectively, are placed in agate mortar and are ground 10-60 min,
Both are made to be sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and fructose be uniformly laid in quartz boat, by quartz boat
It is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 6 DEG C/min, and room temperature is naturally cooled to after insulation 2.5h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 11
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）2.5g basic zinc carbonate and 0.5g citric acid are weighed respectively, are placed in agate mortar and are ground 10-60
Min, both are made to be sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and citric acid be uniformly laid in quartz boat, by quartz
Boat is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 18 DEG C/min, and room temperature is naturally cooled to after insulation 2.8h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Embodiment 12
A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet, including following preparation process：
（1）4g basic zinc carbonate and 0.8g citric acid are weighed respectively, are placed in agate mortar and are ground 30-60 min,
Both are made to be sufficiently mixed uniformly.
（2）By step（1）In be well mixed basic zinc carbonate and citric acid be uniformly laid in quartz boat, by quartz
Boat is put into the quartz ampoule of tube furnace.
（3）Tube furnace is vacuumized, makes step（2）Middle quartz ampoule is placed under airfree vacuum environment, in 300-
Calcination processing is carried out at 800 DEG C, heating rate is 9 DEG C/min, and room temperature is naturally cooled to after insulation 2.5h.
（4）By step（3）Middle obtained powder of calcining is ground with agate mortar, and the powder for grinding to obtain is exactly carbon
The Zinc oxide nano sheet of doping.
Above-described is only the preferred embodiment of the present invention, it is noted that for those skilled in the art,
Under the premise of general idea of the present invention is not departed from, some changes and improvements can also be made, these should also be considered as the present invention's
Protection domain.
Claims (6)
- A kind of 1. simple, quick method for preparing carbon doping Zinc oxide nano sheet, it is characterised in that：Including following preparation process：（1）The basic zinc carbonate and small organic molecule for weighing certain mass respectively are ground, and both is sufficiently mixed It is even；（2）By step（1）In be well mixed basic zinc carbonate and small organic molecule be placed under airfree vacuum environment, Calcination processing is carried out, naturally cools to room temperature afterwards；（3）By step（2）Middle obtained powder of calcining is ground, and the powder for grinding to obtain is exactly the zinc oxide nano of carbon doping Rice piece.
- 2. simple, the quick method for preparing carbon doping Zinc oxide nano sheet according to claim 1, it is characterised in that：Step Suddenly（1）In, small organic molecule is sucrose, oxalic acid, glucose, fructose or citric acid.
- 3. simple, the quick method for preparing carbon doping Zinc oxide nano sheet according to claim 1, it is characterised in that：Step Suddenly（1）The middle basic zinc carbonate and small organic molecule for weighing certain mass respectively, is placed in agate mortar and is ground 10- 60min, both are made to be sufficiently mixed uniformly.
- 4. simple, the quick method for preparing carbon doping Zinc oxide nano sheet according to claim 1, it is characterised in that：Step Suddenly（2）In be well mixed basic zinc carbonate and small organic molecule, be uniformly laid in quartz boat, quartz boat be put into tubular type In the quartz ampoule of stove, tube furnace is vacuumized, quartz ampoule is placed under airfree vacuum environment, at 300-800 DEG C Calcination processing is carried out, heating rate is 5 DEG C/min -20 DEG C/min, and room temperature is naturally cooled to after insulation 2h-3h.
- 5. simple, the quick method for preparing carbon doping Zinc oxide nano sheet according to claim 1, it is characterised in that：Step Suddenly（3）In, by step（2）Obtained powder is calcined to be ground with agate mortar.
- 6. simple, the quick method for preparing carbon doping Zinc oxide nano sheet according to claim 1, it is characterised in that：Alkali The content of formula zinc carbonate and small organic molecule ratio is 4:1~8:1.
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| US11472715B2 (en) * | 2020-10-23 | 2022-10-18 | King Faisal University | Method of making carbon-zinc oxide nanoparticles |
| CN114950295A (en) * | 2022-01-27 | 2022-08-30 | 昆明理工大学 | Preparation of Cu by gas-solid reaction 3 Method of P |
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