CN108423707A - A method of preparing Mn doping ZnO - Google Patents
A method of preparing Mn doping ZnO Download PDFInfo
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- CN108423707A CN108423707A CN201810316318.9A CN201810316318A CN108423707A CN 108423707 A CN108423707 A CN 108423707A CN 201810316318 A CN201810316318 A CN 201810316318A CN 108423707 A CN108423707 A CN 108423707A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of methods for preparing Mn and adulterating ZnO, belong to technical field of material.The ZnO powders that Mn doping is prepared by hydro-thermal method, to analyze the Zn (CH of pure grade3COO)2·2H2O, Mn (CH3COO)2·4H2Load weighted drug is dissolved in the dust technology of 15ml by O as reaction source, stirs 20min, and the ammonium hydroxide for instilling 28wt% dropwise in clear solution causes to be co-precipitated, and is cleaned when pH value is 10 ~ 11；Then, it weighs certain KOH to be dissolved in the deionized water of 15ml, stirs 10min, the KOH solution of gained is poured into above-mentioned precipitation, continuously stirs 1h；Finally, the precursor liquid prepared is moved in reaction kettle, reacts 16h at 120 DEG C, after reaction, sample is put into after cleaning repeatedly in 60 DEG C of vacuum drying chamber by cooled to room temperature, gained sample deionized water and absolute ethyl alcohol, is obtained required sample and is characterized.It is characteristic of the invention that：Method is simple, at low cost, and yield is high, small to environmental hazard, easy to spread.
Description
Technical field
The invention belongs to Material growth fields, are related to preparation and the OPTICAL PROPERTIES of nano material, and mainly study water
Hot method prepares the ZnO particle of transition elements Mn doping.
Background technology
Due to the specific physical performance of ZnO, researchers are more and more extensive to the research of ZnO, main in recent years right
It is magnetic, and optical property, dielectric properties etc. conduct extensive research.
The method for preparing ZnO has very much, and such as solid sintering technology, sol-gel method, hydro-thermal method etc., wherein hydro-thermal method are these
A kind of minimum method of synthesis temperature needed for multi-method, and prepare that pattern is relatively uniform, ZnO of easy control of components
A kind of method, and preparation process is fairly simple；In recent years, study metal-doped nano zine oxide synthesis and property always
It is the hot spot of scientists concern.Duan Man-Yi in 2007 et al. have carried out transition metal and nitrogen co-doped ZnO electronic structures
It is studied with the first principle of optical property, refering to the 9th the 5359-5365 pages of the phases of ACTA PHYSICA SINICA.2008
Wang Ai-Hua et al. are studied Developing Ferromagnetic Properties of Transition-metal-doped ZnO Diluted Magnetic Semiconductors, refering to JOURNAL OF
The 1st the 114-123 pages of the phases of SYNTHETIC CRYSTALS.Liu Xue-Zhen in 2012 et al. are carried out with pulse laser deposition method
The research of magnetic property ZnO thin film doped Co, refering to the 4th phase 369- of JOURNAL OF INORGANIC MATERIALS
Page 374.
The ZnO of Cr doping is prepared with hydro-thermal method：Such as Zhang Fu-Chun in 2010 prepare Cr using hydro-thermal method and adulterate
ZnO samples, refering to the 12nd the 1-7 pages of the phases of Acta Phys.Sin..
The ZnO nano particle of In doping is prepared with hydro-thermal method：Such as ManDe Qiu in 2009 are using hydro-thermal method at 430 DEG C
At a temperature of prepare the ZnO nano particle of In doping, refering to Journal of Synthetic Crystals. volumes 38 the 1st
The 48-52 pages of phase.
The ZnO of Co doping is prepared with hydro-thermal method：As Qingwei Li et al. in 2010 prepares the ZnO that Co is adulterated with hydro-thermal method
Crystallite, refering to the 2nd the 253-257 pages of the phases of Chinese Journal of Luminescence..
Invention content
The purpose of the present invention is under the premise of improving leakproofness, by simple hydro-thermal method at a temperature of 120 DEG C at
Work(prepares the ZnO crystallites of transition metal element Mn doping, and has studied the optical property of Mn doping ZnO samples.
The present invention is realized by following technical process：Zinc source used is Zn (CH3COO)2·2H2O（99%）,
（0.05mol）, manganese source is Mn (CH3COO)2·4H2O (99.9%),（0.05mol）；It is dense that load weighted sample is dissolved in 15ml
Degree is in the dust technology of 10wt%, and magnetic agitation 20min to solution becomes transparence；It is instilled dropwise in above-mentioned transparent liquid
The ammonium hydroxide of 28wt% causes to be co-precipitated, and precipitates Mn2+And Zn2+Precipitation is centrifuged when pH value is 10 ~ 11, uses deionized water by ion
It cleans repeatedly, is washed till neutrality；Then it weighs certain KOH to be dissolved in the deionized water of 15ml, magnetic agitation 10min, by institute
The KOH solution obtained pours into above-mentioned precipitation, and 1h is continuously stirred on magnetic stirring apparatus；Finally, the precursor liquid prepared is put into appearance
Product is that reaction kettle is put into hydro-thermal in the constant temperature oven that set temperature is 120 DEG C in the polytetrafluoroethylene (PTFE) hydrothermal reaction kettle of 50ml
16h is reacted, after hydro-thermal reaction, by reaction kettle cooled to room temperature, the sample deionized water and absolute ethyl alcohol of gained
It is cleaned repeatedly until removing all soluble-salts, is put into dry acquisition sample in the vacuum drying chamber that set temperature is 60 DEG C.
Sample obtained by the present invention is the ZnO particle of Mn doping, XRD diagram such as Fig. 1 institutes of sample under different levels of doping
Show, the UV-Visible absorption figure of sample obtained by different levels of doping and corresponding Tauc figures are as shown in Figure 2.Difference doping is dense
The SEM figures of the obtained sample of degree are as shown in Figure 2,.Compared with prior art, the method have the characteristics that：It is prepared using hydro-thermal method
Go out the ZnO particle of Mn doping, preparation process is simple, obtains small energy gap（Less than 3eV）.This experimental product uniformity is good,
Environmental pollution is small, and controllability is good, easy to spread, thus has important researching value and wide application prospect.
Description of the drawings
Fig. 1 is the ZnO XRD diagram for adulterating Mn, wherein（1）、（2）、（3）Be respectively KOH be 6mM, temperature be 120 DEG C, instead
Be between seasonable corresponded under 16h doping concentration be 0% Mn, the XRD diagram of sample synthesized by 2% Mn, 4% Mn and its（110）、
（103）、（112）Enlarged drawing at diffraction maximum.
Fig. 2 KOH are 6mM, and doping concentration is respectively 0% Mn, 2% Mn, 4% Mn at a temperature of 120 DEG C, and reaction 16h synthesizes sample
The SEM of product schemes, wherein（1）（3）（5）Scheme for the SEM of different levels of doping sample under low power number,（2）（4）（6）It is counter sample
SEM enlarged drawings.
Fig. 3 KOH are 6mM, and doping concentration is respectively 0% Mn, 2% Mn, 4% Mn at a temperature of 120 DEG C, and reaction 16h synthesizes sample
The Uv-vis of product schemes.
Specific implementation mode
Embodiment 1
Weigh 1.875g Zn (CH3COO)2·2H2O (99%).Load weighted sample is dissolved in the dilute of a concentration of 10wt% of 15ml
In nitric acid, magnetic agitation 20min to solution becomes transparence；The ammonium hydroxide for instilling 28wt% dropwise in above-mentioned transparent liquid causes altogether
Precipitation precipitates Zn2+Precipitation is centrifuged when pH value is 10 ~ 11, is cleaned repeatedly with deionized water, be washed till neutrality by ion；Then
It weighs certain KOH to be dissolved in the deionized water of 15ml, magnetic agitation 10min, it is above-mentioned heavy that the KOH solution of gained is poured into
It forms sediment, 1h is continuously stirred on magnetic stirring apparatus；Finally, the precursor liquid prepared is put into the polytetrafluoroethylene (PTFE) water that volume is 50ml
In thermal response kettle, it is hydro-thermal reaction 16h in 120 DEG C of constant temperature oven that reaction kettle, which is put into set temperature, after hydro-thermal reaction,
By reaction kettle cooled to room temperature, the sample deionized water and absolute ethyl alcohol of gained are cleaned repeatedly until removal is all solvable
Property salt, be put into set temperature be it is dry in 60 DEG C of vacuum drying chamber after obtain pure ZnO samples.Sample in XRD such as Fig. 1（1）
It is shown, in SEM such as Fig. 2（1）With（2）It is shown, in uv-visible absorption spectrum such as Fig. 3（1）It is shown.
Embodiment 2
Weigh 1.875g Zn (CH3COO)2·2H2O (99%) weighs 0.02083g Mn (CH3COO)2·4H2O (99.9%)。
Load weighted sample is dissolved in the dust technology of a concentration of 10wt% of 15ml, magnetic agitation 20min to solution becomes transparence；
The ammonium hydroxide for instilling 28wt% dropwise in above-mentioned transparent liquid causes to be co-precipitated, and precipitates Zn2+And Mn2+Ion, when pH value is 10 ~ 11
When, precipitation is centrifuged, is cleaned repeatedly with deionized water, is washed till neutrality；Then the deionization that certain KOH is dissolved in 15ml is weighed
In water, the KOH solution of gained is poured into above-mentioned precipitation, 1h is continuously stirred on magnetic stirring apparatus by magnetic agitation 10min；Finally,
The precursor liquid prepared is put into the polytetrafluoroethylene (PTFE) hydrothermal reaction kettle that volume is 50ml, reaction kettle, which is put into set temperature, is
Hydro-thermal reaction 16h in 120 DEG C of constant temperature oven, after hydro-thermal reaction, by reaction kettle cooled to room temperature, the sample of gained
It is cleaned repeatedly with deionized water and absolute ethyl alcohol until removing all soluble-salts, is put into the vacuum drying that set temperature is 60 DEG C
The ZnO samples of 2% Mn of doping are obtained in case after drying.Sample in XRD such as Fig. 1（2）It is shown, in SEM such as Fig. 2（3）With（4）Institute
Show, in uv-visible absorption spectrum such as Fig. 3（2）It is shown.
Embodiment 3
Weigh 1.875g Zn (CH3COO)2·2H2O (99%）, weigh 0.010415g Mn (CH3COO)2·4H2O (99.9%)。
Load weighted sample is dissolved in the dust technology of a concentration of 10wt% of 15ml, magnetic agitation 20min to solution becomes transparence；
The ammonium hydroxide for instilling 28wt% dropwise in above-mentioned transparent liquid causes to be co-precipitated, and precipitates Zn2+And Mn2+Ion, when pH value is 10 ~ 11
When, precipitation is centrifuged, is cleaned repeatedly with deionized water, is washed till neutrality；Then the deionization that certain KOH is dissolved in 15ml is weighed
In water, the KOH solution of gained is poured into above-mentioned precipitation, 1h is continuously stirred on magnetic stirring apparatus by magnetic agitation 10min；Finally,
The precursor liquid prepared is put into the polytetrafluoroethylene (PTFE) hydrothermal reaction kettle that volume is 50ml, reaction kettle, which is put into set temperature, is
Hydro-thermal reaction 16h in 120 DEG C of constant temperature oven, after hydro-thermal reaction, by reaction kettle cooled to room temperature, the sample of gained
It is cleaned repeatedly with deionized water and absolute ethyl alcohol until removing all soluble-salts, is put into the vacuum drying that set temperature is 60 DEG C
The ZnO samples of doping 4%Mn are obtained in case after drying.Sample in XRD such as Fig. 1（3）It is shown, in SEM such as Fig. 2（5）With（6）It is shown,
In uv-visible absorption spectrum such as Fig. 3（3）It is shown.
Claims (5)
1. a kind of simple hydro-thermal method prepares the ZnO of Mn doping, it is characterised in that after controlling doping concentration, and by following
Technical process is realized：The sources Zn used are Zn (CH3COO)2·2H2O (99%), (0.05mol), the sources Mn Mn (CH3COO)2·4H2O
(99.9%), (0.05mol)；Load weighted sample is dissolved in the dust technology of a concentration of 10wt% of 15ml, magnetic agitation
20min becomes transparence to solution；The ammonium hydroxide for instilling a concentration of 28wt% dropwise in above-mentioned transparent liquid causes to be co-precipitated, precipitation
Mn2+And Zn2+Precipitation is centrifuged when pH value is 10 ~ 11, is cleaned repeatedly with deionized water, be washed till neutrality by ion；Then it weighs
Certain KOH is dissolved in the deionized water of 15ml, magnetic agitation 10min, and the KOH solution of gained is poured into above-mentioned precipitation,
1h is continuously stirred on magnetic stirring apparatus；Finally, by the precursor liquid prepared be put into volume be 50ml polytetrafluoroethylene (PTFE) hydro-thermal it is anti-
It answers in kettle, it is hydro-thermal reaction 16h in 120 DEG C of constant temperature oven that reaction kettle, which is put into set temperature,, will be anti-after hydro-thermal reaction
Kettle cooled to room temperature, the sample deionized water and absolute ethyl alcohol of gained is answered to be cleaned repeatedly until removing all solubilities
Salt is put into the vacuum drying chamber that set temperature is 60 DEG C and obtains required sample after drying, using X-ray diffraction (XRD), sweeps
It retouches electron microscope (SEM) and uv-visible absorption spectrum (Uv-vis) carries out the structure of sample, pattern and optical property
Characterization.
2. as described in claim 1, which is characterized in that the source is the Zn (CH for analyzing pure grade3COO)2·2H2O(99%)、Mn
(CH3COO)2·4H2O (99.9%)。
3. as described in claim 1, which is characterized in that the practical doping concentration of Mn is respectively 0.75at% and 1.83at%.
4. as described in claim 1, which is characterized in that this patent is in a concentration of 6mM of KOH, and temperature is to be reacted at 120 DEG C
16h synthesizes the ZnO particle of transition elements Mn doping.
5. as described in claim 1, which is characterized in that this patent is prepare Mn doping using traditional hydro-thermal method ZnO
Grain, and study its optical property.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810316318.9A CN108423707A (en) | 2018-04-10 | 2018-04-10 | A method of preparing Mn doping ZnO |
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| CN201810316318.9A CN108423707A (en) | 2018-04-10 | 2018-04-10 | A method of preparing Mn doping ZnO |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109835942A (en) * | 2019-03-11 | 2019-06-04 | 新疆大学 | A kind of method that coprecipitation prepares Mn doping zinc oxide nanometer particle |
| CN113023769A (en) * | 2021-03-12 | 2021-06-25 | 安徽景成新材料有限公司 | Synthesis method of manganese ion doped zinc oxide |
| CN114605860A (en) * | 2022-02-14 | 2022-06-10 | 华东理工大学 | Diluted magnetic solid solution type metal anti-corrosion pigment |
-
2018
- 2018-04-10 CN CN201810316318.9A patent/CN108423707A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109835942A (en) * | 2019-03-11 | 2019-06-04 | 新疆大学 | A kind of method that coprecipitation prepares Mn doping zinc oxide nanometer particle |
| CN113023769A (en) * | 2021-03-12 | 2021-06-25 | 安徽景成新材料有限公司 | Synthesis method of manganese ion doped zinc oxide |
| CN114605860A (en) * | 2022-02-14 | 2022-06-10 | 华东理工大学 | Diluted magnetic solid solution type metal anti-corrosion pigment |
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Application publication date: 20180821 |