CN103101964A - Preparation method of zinc oxide nanoflower of spiauterite structure - Google Patents
Preparation method of zinc oxide nanoflower of spiauterite structure Download PDFInfo
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- CN103101964A CN103101964A CN 201310015382 CN201310015382A CN103101964A CN 103101964 A CN103101964 A CN 103101964A CN 201310015382 CN201310015382 CN 201310015382 CN 201310015382 A CN201310015382 A CN 201310015382A CN 103101964 A CN103101964 A CN 103101964A
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Abstract
The invention relates to a preparation method of zinc oxide nanoflower of a spiauterite structure. The preparation method comprises the following steps of: preparing a zinc nitrate aqueous solution and a sodium citrate aqueous solution, respectively; mixing the zinc nitrate aqueous solution with the sodium citrate aqueous solution; adding tetramethylammonium hydroxide to the mixed solution to obtain a suspension precursor for hydrothermal reaction; sealing the precursor in a reaction kettle; and carrying out hydro-thermal treatment for 0.4 hour to 4 hours at 90 DEG C to 110 DEG C. The zinc oxide nanoflower, prepared by the preparation method disclosed by the invention, of the spiauterite structure is 3 microns to 5 microns in size, and the thickness of the nanosheet is 10nm to 20nm. Moreover, the product is stable in quality and high in purity, and the grains are good in dispersion; besides, the preparation process is simple, free of pollution, low in cost and easy to apply large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of zinc oxide nano popped rice of wurtzite structure, belong to ceramic material field.
Background technology
The inorganic materials of nanostructure is very extensive in the application in high-performance field, have excellent electricity, magnetics, optics, mechanical property, and the shape characteristic of nano material has a great impact its performance, therefore, the pattern of research control nano materials has caused the increasing interest of people and attention.
Zinc oxide is a kind of extraordinary novel inorganic semiconductor product, has good electricity, magnetics, optics, mechanics, chemistry and macro property, and low price, easily produces, and chemical stability is good.The zinc oxide of nanostructure is little due to its size of particles, specific surface area is large, thereby it has the characteristics such as obvious surface and interface effect, quantum size effect, volume effect, macroscopical two word size tunnel effects and high-clarity, polymolecularity.Make it all show many unique excellent physics and chemistry performances aspect chemistry, optics, biology and electricity.This new state of matter allows the zinc oxide of nanostructure show huge application prospect in above-mentioned field.Zinc oxide has good electric property, the theoretical capacity that has 978mAhg-1 as lithium ion battery negative material, theoretical capacity far above 372 mAhg-1 of present business-like graphite material, the zinc oxide of flower-like nanostructure emerges in embedding because having larger specific surface area and being more conducive to lithium ion, thereby has better electric property.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, the preparation method of the wurtzite structure zinc oxide nano popped rice that is easy to control.
The preparation method of the zinc oxide nano popped rice of wurtzite structure of the present invention comprises the following steps:
The preparation method of the zinc oxide nano popped rice of wurtzite structure is characterized in that comprising the following steps:
1) under the stirring, zinc nitrate fully is dissolved in deionized water, compound concentration is the zinc nitrate aqueous solution of 0.2 ~ 0.6mol/L;
2) stir under, citric acid received fully be dissolved in deionized water, compound concentration is that the citric acid of 0.05 ~ 0.15mol/L is received the aqueous solution;
3) stir under, with step 2) citric acid receive the aqueous solution and join in the zinc nitrate aqueous solution of step 1), obtain mixing solutions;
4) tetramethyl-ammonium is dissolved in the mixing solutions of step 3), compound concentration is that the tetramethyl-ammonium suspension of 0.5 ~ 2mol/L is as precursor pulp;
5) precursor pulp is changed over to reactor inner bag and be placed in reactor, sealing, be incubated 0.4 ~ 4 hour and carry out hydrothermal treatment consists under 90 ~ 110 ℃, then, allow reactor naturally cool to room temperature, take out reaction product, filter, use successively deionized water, ethanol, washed with de-ionized water, dry, obtain the zinc oxide nano popped rice of wurtzite structure.
The preparation method of the zinc oxide nano popped rice of wurtzite structure according to claim 1 is characterized in that said reactor is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
The preparation method of the zinc oxide nano popped rice of wurtzite structure according to claim 1 is characterized in that said zinc nitrate, citric acid are received, the purity of tetramethyl-ammonium and ethanol all is not less than chemical pure.
In the present invention, said reactor is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
Described zinc nitrate, citric acid are received, the purity of tetramethyl-ammonium and ethanol all is not less than chemical pure.
The zinc oxide nano popped rice size that adopts the present invention to make wurtzite structure is 3～5 μ m, and nanometer sheet thickness is 10-20nm.Constant product quality, purity is high, and particle dispersion is good, is conducive to the lithium ion diffusion, improves the large current density performance of lithium ion battery.Preparation process of the present invention is simple, need not to do high temperature sintering and processes, and has avoided the powder reuniting that may form in the calcination process; Be easy to control, pollution-free, cost is low, is easy to large-scale production.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of zinc oxide nano popped rice;
Fig. 2 is scanning electronic microscope (SEM) photo of zinc oxide nano popped rice;
Fig. 3 is scanning electronic microscope (SEM) photo of zinc oxide nano popped rice;
Fig. 4 is that the zinc oxide nano popped rice that synthesizes of the present invention is as the charging and discharging curve of the lithium ion battery of negative material assembling.
Embodiment
Example 1
1) under the stirring, zinc nitrate fully is dissolved in deionized water, compound concentration is the zinc nitrate aqueous solution of 0.6mol/L;
2) stir under, citric acid received fully be dissolved in deionized water, compound concentration is that the citric acid of 0.15mol/L is received the aqueous solution;
3) under whipped state, with step 2) citric acid receive the aqueous solution and join in the zinc nitrate aqueous solution of step 1), obtain mixing solutions;
4) tetramethyl-ammonium is dissolved in the mixing solutions of step 3), obtains tetramethyl-ammonium concentration and be the white suspension solution of 2mol/L as precursor pulp;
5) precursor pulp is changed over to then be placed in reactor in the reactor inner bag, sealing, hydrothermal treatment consists was carried out in insulation in 4 hours under 110 ℃, then, allow reactor naturally cool to room temperature, take out reaction product, filter, clean with deionized water, ethanol, ionized water successively, dry, obtain the zinc oxide nano popped rice of wurtzite structure.
Its X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 1, and as seen from Figure 1, the zinc oxide that present method obtains is wurtzite structure, and crystallinity and purity better.Scanning electronic microscope (SEM) photo is seen Fig. 2, Fig. 3, and the product that obtains of present method is the flower-shaped nanostructure of homogeneous comparatively as seen from Figure 2, by figure
3As seen flower-shaped nanostructure is to be made of the sheet that thickness is 10nm-20nm, and the size of nano flower is 3-5 μ m size.
The zinc oxide nano popped rice of the wurtzite structure that this example makes is seen Fig. 4 as the charge-discharge performance of the lithium ion battery of negative material assembling, and by diagram data as seen, first discharge specific capacity reaches 1300mAh/g, drops to for the second time 678mAh/g, and reversible capacity is about 50%.
Example 2
1) under the stirring, zinc nitrate fully is dissolved in deionized water, compound concentration is the zinc nitrate aqueous solution of 0.4mol/L;
2) stir under, citric acid received fully be dissolved in deionized water, compound concentration is that the citric acid of 0.1mol/L is received the aqueous solution;
3) under whipped state, with step 2) citric acid receive the aqueous solution and join in the zinc nitrate aqueous solution of step 1), obtain mixing solutions;
4) tetramethyl-ammonium is dissolved in the mixing solutions of step 3), obtains tetramethyl-ammonium concentration and be the white suspension solution of 1mol/L as precursor pulp;
5) precursor pulp is changed over to then be placed in reactor in the reactor inner bag, sealing, hydrothermal treatment consists was carried out in insulation in 2 hours under 100 ℃, then, allow reactor naturally cool to room temperature, take out reaction product, filter, clean with deionized water, ethanol, ionized water successively, dry, obtain the zinc oxide nano popped rice of wurtzite structure.
Example 3
1) under the stirring, zinc nitrate fully is dissolved in deionized water, compound concentration is the zinc nitrate aqueous solution of 0.2mol/L;
2) stir under, citric acid received fully be dissolved in deionized water, compound concentration is that the citric acid of 0.05mol/L is received the aqueous solution;
3) under whipped state, with step 2) citric acid receive the aqueous solution and join in the zinc nitrate aqueous solution of step 1), obtain mixing solutions;
4) tetramethyl-ammonium is dissolved in the mixing solutions of step 3), obtains tetramethyl-ammonium concentration and be the white suspension solution of 0.5mol/L as precursor pulp;
5) precursor pulp is changed over to then be placed in reactor in the reactor inner bag, sealing, hydrothermal treatment consists was carried out in insulation in 0.4 hour under 90 ℃, then, allow reactor naturally cool to room temperature, take out reaction product, filter, clean with deionized water, ethanol, ionized water successively, dry, obtain the zinc oxide nano popped rice of wurtzite structure.
Claims (3)
1. the preparation method of the zinc oxide nano popped rice of wurtzite structure is characterized in that comprising the following steps:
1) under the stirring, zinc nitrate fully is dissolved in deionized water, compound concentration is the zinc nitrate aqueous solution of 0.2 ~ 0.6mol/L;
2) stir under, citric acid received fully be dissolved in deionized water, compound concentration is that the citric acid of 0.05 ~ 0.15mol/L is received the aqueous solution;
3) stir under, with step 2) citric acid receive the aqueous solution and join in the zinc nitrate aqueous solution of step 1), obtain mixing solutions;
4) tetramethyl-ammonium is dissolved in the mixing solutions of step 3), compound concentration is that the tetramethyl-ammonium suspension of 0.5 ~ 2mol/L is as precursor pulp;
5) precursor pulp is changed over to reactor inner bag and be placed in reactor, sealing, be incubated 0.4 ~ 4 hour and carry out hydrothermal treatment consists under 90 ~ 110 ℃, then, allow reactor naturally cool to room temperature, take out reaction product, filter, use successively deionized water, ethanol, washed with de-ionized water, dry, obtain the zinc oxide nano popped rice of wurtzite structure.
2. the preparation method of the zinc oxide nano popped rice of wurtzite structure according to claim 1, is characterized in that said reactor is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
3. the preparation method of the zinc oxide nano popped rice of wurtzite structure according to claim 1 is characterized in that said zinc nitrate, citric acid are received, the purity of tetramethyl-ammonium and ethanol all is not less than chemical pure.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445367A (en) * | 2014-11-13 | 2015-03-25 | 华侨大学 | Preparation method of nanoflower-shaped zinc oxide |
| CN105789602A (en) * | 2016-03-04 | 2016-07-20 | 河源广工大协同创新研究院 | Preparation method of zinc oxide nanosheet for negative electrode of lithium-ion battery |
| CN106044846A (en) * | 2016-06-08 | 2016-10-26 | 太原理工大学 | Preparation method and application of nanorod self-assembled spike-like nano-ZnO |
| CN107460514A (en) * | 2017-06-27 | 2017-12-12 | 江苏大学 | A kind of simple method for preparing zinc oxide nano popped rice |
| CN111785955A (en) * | 2020-01-09 | 2020-10-16 | 郑州轻工业大学 | High-capacity VNb9O25Nano-sheet lithium ion battery cathode material and preparation method thereof |
-
2013
- 2013-01-16 CN CN 201310015382 patent/CN103101964A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445367A (en) * | 2014-11-13 | 2015-03-25 | 华侨大学 | Preparation method of nanoflower-shaped zinc oxide |
| CN105789602A (en) * | 2016-03-04 | 2016-07-20 | 河源广工大协同创新研究院 | Preparation method of zinc oxide nanosheet for negative electrode of lithium-ion battery |
| CN106044846A (en) * | 2016-06-08 | 2016-10-26 | 太原理工大学 | Preparation method and application of nanorod self-assembled spike-like nano-ZnO |
| CN107460514A (en) * | 2017-06-27 | 2017-12-12 | 江苏大学 | A kind of simple method for preparing zinc oxide nano popped rice |
| CN111785955A (en) * | 2020-01-09 | 2020-10-16 | 郑州轻工业大学 | High-capacity VNb9O25Nano-sheet lithium ion battery cathode material and preparation method thereof |
| CN111785955B (en) * | 2020-01-09 | 2022-05-20 | 郑州轻工业大学 | High-capacity VNb9O25Nano-sheet lithium ion battery cathode material and preparation method thereof |
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Application publication date: 20130515 |