CN103101964A - Preparation method of zinc oxide nanoflower of spiauterite structure - Google Patents
Preparation method of zinc oxide nanoflower of spiauterite structure Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- aqueous solution
- zinc oxide
- preparation
- reactor
- citric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002057 nanoflower Substances 0.000 title abstract description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 54
- 241000209094 Oryza Species 0.000 claims description 21
- 235000007164 Oryza sativa Nutrition 0.000 claims description 21
- 235000009566 rice Nutrition 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000001509 sodium citrate Substances 0.000 abstract 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 abstract 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 abstract 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000002135 nanosheet Substances 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310015382 CN103101964A (en) | 2013-01-16 | 2013-01-16 | Preparation method of zinc oxide nanoflower of spiauterite structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310015382 CN103101964A (en) | 2013-01-16 | 2013-01-16 | Preparation method of zinc oxide nanoflower of spiauterite structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103101964A true CN103101964A (en) | 2013-05-15 |
Family
ID=48310209
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310015382 Pending CN103101964A (en) | 2013-01-16 | 2013-01-16 | Preparation method of zinc oxide nanoflower of spiauterite structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103101964A (en) |
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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Deng et al. | Controlled synthesis of anisotropic hollow ZnCo2O4 octahedrons for high-performance lithium storage | |
| CN104659358B (en) | Preparation method of nickel cobaltate nano hollow polyhedron | |
| CN1333474C (en) | Preparation method of spinel lithium titanate nano tube/wire for lithium battery and capacitor | |
| CN105552331B (en) | Iron cobalt/cobalt oxide/graphene composite material and its preparation method and application | |
| CN106711432B (en) | A kind of tridimensional network MoO2Nano material and its preparation and application | |
| TWI577640B (en) | Nickel-lithium metal composite oxide powder and method for producing same,positive electrode active material for lithium ion battery, positive electrode for lithium ion battery and lithium ion battery | |
| CN103101964A (en) | Preparation method of zinc oxide nanoflower of spiauterite structure | |
| CN110745790B (en) | Hydrothermal preparation method of bismuth selenide nano powder | |
| WO2011136258A1 (en) | Novel lithium titanate, method for producing same, electrode active material containing the lithium titanate, and electricity storage device using the electrode active material | |
| CN105060351A (en) | Flower-like cobaltosic oxide material composed of nanoparticles and preparation method thereof | |
| CN103991899A (en) | Preparation method of porous flowerlike stannic oxide micro-nano structure | |
| CN110600695A (en) | Yolk-eggshell structure tin @ hollow mesoporous carbon sphere material and preparation method thereof | |
| CN102790211B (en) | Preparation method of high-performance copper ferrite ultrafine powder for lithium ion battery cathode materials | |
| Zhang et al. | A novel porous tubular Co3O4: self-assembly and excellent electrochemical performance as anode for lithium-ion batteries | |
| CN110203976A (en) | Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material | |
| CN104183827B (en) | A kind of lithium iron phosphate nano rod and preparation method thereof | |
| CN103043630B (en) | Preparation method of spherical nickel diselenide powder | |
| CN112701280A (en) | Preparation method of hollow bicrystal phase cobalt nickel selenide microsphere material | |
| CN104402065B (en) | The preparation method of the spherical cobalt disulfide nano-powder of one kind | |
| CN105762354B (en) | A kind of flower-shaped ferric oxide nano-material and preparation method thereof, negative electrode of lithium ion battery and lithium ion battery | |
| CN105524617A (en) | Preparation method of molybdenum selenide quantum dots | |
| CN109671937B (en) | In-situ synthesis method of transition metal oxide/graphene composite material | |
| CN101319404B (en) | Method for preparation of hollow spherical cadmium sulfide nanocrystalline | |
| CN102877130A (en) | Preparation method of bismuth ferrite BiFeO3 monocrystal micrometer sheet | |
| CN107317019B (en) | Ferrous carbonate/graphene composite material for sodium ion battery cathode and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130515 |