CN1686820A - Method for repairing nano stick of zinc oxide in even diameter - Google Patents
Method for repairing nano stick of zinc oxide in even diameter Download PDFInfo
- Publication number
- CN1686820A CN1686820A CN 200510049581 CN200510049581A CN1686820A CN 1686820 A CN1686820 A CN 1686820A CN 200510049581 CN200510049581 CN 200510049581 CN 200510049581 A CN200510049581 A CN 200510049581A CN 1686820 A CN1686820 A CN 1686820A
- Authority
- CN
- China
- Prior art keywords
- solution
- zinc oxide
- lithium hydroxide
- zinc acetate
- reaction kettle
- 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.)
- Granted
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002073 nanorod Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004246 zinc acetate Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims abstract 12
- 239000011259 mixed solution Substances 0.000 claims abstract 2
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明涉及制备直径均匀氧化锌纳米棒的方法，包括以下步骤：1)把醋酸锌溶解于无水乙醇或无水甲醇中，0℃下充分搅拌，配制成浓度为0.5～30％的悬浊液，室温下将氢氧化锂溶解于无水乙醇或无水甲醇中，配制成摩尔浓度两倍于醋酸锌的氢氧化锂溶液；2)在0℃温度下，将等体积的氢氧化锂溶液，逐滴地加入到搅拌着的醋酸锌溶液中，得白色胶体状混合溶液；3)将胶体溶液放入水热反应釜中，将密封后的反应釜，在80～200℃下保温5～24小时，取出反应溶液；4)离心分离反应溶液，用无水乙醇对分离物充分洗涤，室温下干燥，即可。本发明方法简便，易于操作，成本低，通过调节反应物浓度，反应釜温度，可以控制直径均匀的氧化锌纳米棒。The invention relates to a method for preparing zinc oxide nanorods with uniform diameters, comprising the following steps: 1) dissolving zinc acetate in absolute ethanol or absolute methanol, fully stirring at 0°C, and preparing a suspension with a concentration of 0.5-30%. solution, dissolve lithium hydroxide in absolute ethanol or methanol at room temperature, and prepare a lithium hydroxide solution with a molar concentration twice that of zinc acetate; , added dropwise into the stirring zinc acetate solution to obtain a white colloidal mixed solution; 3) Put the colloid solution in a hydrothermal reaction kettle, and keep the sealed reaction kettle at 80-200°C for 5- After 24 hours, take out the reaction solution; 4) centrifuge the reaction solution, wash the isolate fully with absolute ethanol, and dry it at room temperature. The method of the invention is simple, easy to operate and low in cost, and can control the zinc oxide nanorods with uniform diameters by adjusting the concentration of reactants and the temperature of the reaction kettle.
Description
Technical field
The present invention relates to prepare the method for the even zinc oxide nano rod of diameter.
Background technology
Nano zine oxide is a kind of polyfunctional new inorganic material, and its granular size is about 1～100 nanometer.Because the granular of crystal grain, its surface electronic structure and crystalline structure change, and have produced characteristics such as the surface effects that macro object did not have, volume effect, quantum size effect and macroscopical tunnel effect and high-clarity, polymolecularity.It shows many specific functions at aspects such as catalysis, optics, magnetics, mechanics discovered in recent years, make it have important use to be worth in many fields such as pottery, chemical industry, electronics, optics, biology, medicine, have common zinc oxide the singularity and the purposes that can't compare.With respect to common zinc oxide, nano zine oxide product activity height has infrared, ultraviolet of shielding and germ-resistant function.Can be applied in high-grade paint, printing ink, coating, the plastics, can obviously improve product opacifying power and tinting strength, in ceramic industry, can make the fusing assistant of breast erosion glaze.Zinc oxide one-dimensional nanomaterial has many special physics, chemical property, having huge application potential aspect structure nanoelectronic and the optics, is subjected to paying close attention to widely.But the uniform zinc oxide nano rod of the difficult preparation diameter of present process for preparing sol-gel.
Summary of the invention
The purpose of this invention is to provide a kind of controlled method for preparing the even zinc oxide nano rod of diameter.
The method for preparing the even zinc oxide nano rod of diameter of the present invention is characterized in that may further comprise the steps:
1) zinc acetate is dissolved in dehydrated alcohol or the anhydrous methanol, 0 ℃ is fully stirred down, be mixed with concentration and be 0.5～30% suspension liquid, under the room temperature lithium hydroxide is dissolved in dehydrated alcohol or the anhydrous methanol, be mixed with the lithium hydroxide solution that volumetric molar concentration doubles zinc acetate;
2) under 0 ℃ of temperature, with isopyknic lithium hydroxide solution, dropwise join in the zinc acetate solution that is stirring, get white colloidal mixing solutions;
3) with above-mentioned colloidal solution, put into hydrothermal reaction kettle,, be incubated 5～24 hours down, take out reaction soln at 80～200 ℃ with the reactor after the sealing;
4) the above-mentioned reaction soln of centrifugation,, dry under the room temperature with dehydrated alcohol to the isolate thorough washing, promptly get the even zinc oxide nano rod of diameter.
The diameter of the zinc oxide nano rod that makes is below 100 nanometers, and length-to-diameter ratio is 3～30.
The present invention has the following advantages:
1. the raw materials cost of preparation zinc oxide nano rod is cheap, technology is easy, do not need the pH value of regulator solution, operation easy to implement.
2. the diameter of prepared zinc oxide nano rod is even, by the conditioned reaction substrate concentration, and temperature of reaction kettle, and reaction times, diameter and length-to-diameter ratio that can controlled oxidation zinc nanometer rod.
3. temperature of reaction is low, and the product recovery that can circulate is a kind of preparation method of energy-conserving and environment-protective.
Description of drawings
Fig. 1 is the transmission electron microscope photo of product.
Embodiment
The inventive method prepares the example of zinc oxide nano rod:
Zinc acetate is dissolved in the dehydrated alcohol, and 0 ℃ is stirred down fully that to be mixed with concentration be 2% suspension liquid, at room temperature lithium hydroxide is dissolved in the dehydrated alcohol, is mixed with lithium hydroxide solution, and its volumetric molar concentration is the twice of zinc acetate solution.Adopt dropper isopyknic lithium hydroxide solution dropwise to be joined in the zinc acetate solution that is stirring, mixing solutions maintains 0 ℃.With above-mentioned mixing solutions, be sealed in the autoclave then, be incubated 10 hours down at 150 ℃, the centrifugation reaction soln, behind the dehydrated alcohol thorough washing, drying promptly obtains the uniform zinc oxide nano rod of diameter, and the transmission electron microscope photo of product is seen Fig. 1.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510049581 CN1281507C (en) | 2005-04-06 | 2005-04-06 | Method for repairing nano stick of zinc oxide in even diameter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510049581 CN1281507C (en) | 2005-04-06 | 2005-04-06 | Method for repairing nano stick of zinc oxide in even diameter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1686820A true CN1686820A (en) | 2005-10-26 |
| CN1281507C CN1281507C (en) | 2006-10-25 |
Family
ID=35304862
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510049581 Expired - Fee Related CN1281507C (en) | 2005-04-06 | 2005-04-06 | Method for repairing nano stick of zinc oxide in even diameter |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1281507C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390248C (en) * | 2006-01-06 | 2008-05-28 | 扬州大学 | Preparation method of semiconductor luminescent material ZnO nanocapsule |
| CN101407334B (en) * | 2007-10-12 | 2010-09-29 | 新疆大学 | A kind of synthetic method of rod-shaped nano zinc oxide |
| CN102219254A (en) * | 2011-06-20 | 2011-10-19 | 厦门大学 | Preparation method of zinc oxide nanorod |
| CN102765744A (en) * | 2012-07-31 | 2012-11-07 | 南京大学 | One-step preparation method of zinc oxide quantum dots |
| CN104609460A (en) * | 2015-01-29 | 2015-05-13 | 武汉大学 | A kind of nano zinc oxide with controllable length and preparation method thereof |
| CN105174300A (en) * | 2015-09-30 | 2015-12-23 | 景德镇陶瓷学院 | Preparation method of ZnO micro-nano ball powder with multilevel structure and product prepared with method |
| CN106563362A (en) * | 2016-10-25 | 2017-04-19 | 江苏大学 | Preparing method and usage of low-oxidization-degree graphene/zinc oxide nanometer composite film |
| CN113809272A (en) * | 2020-06-16 | 2021-12-17 | Tcl科技集团股份有限公司 | Zinc oxide nano material, preparation method, electron transmission film and light emitting diode |
| CN114409923A (en) * | 2021-11-25 | 2022-04-29 | 华南农业大学 | Multifunctional self-healing antibacterial hydrogel and preparation method and application thereof |
| CN115536054A (en) * | 2022-06-28 | 2022-12-30 | 山东科技职业学院 | Preparation method of zinc oxide nano-rods with different particle diameters |
-
2005
- 2005-04-06 CN CN 200510049581 patent/CN1281507C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390248C (en) * | 2006-01-06 | 2008-05-28 | 扬州大学 | Preparation method of semiconductor luminescent material ZnO nanocapsule |
| CN101407334B (en) * | 2007-10-12 | 2010-09-29 | 新疆大学 | A kind of synthetic method of rod-shaped nano zinc oxide |
| CN102219254A (en) * | 2011-06-20 | 2011-10-19 | 厦门大学 | Preparation method of zinc oxide nanorod |
| CN102765744A (en) * | 2012-07-31 | 2012-11-07 | 南京大学 | One-step preparation method of zinc oxide quantum dots |
| CN102765744B (en) * | 2012-07-31 | 2013-12-25 | 南京大学 | One-step preparation method of zinc oxide quantum dots |
| CN104609460A (en) * | 2015-01-29 | 2015-05-13 | 武汉大学 | A kind of nano zinc oxide with controllable length and preparation method thereof |
| CN105174300A (en) * | 2015-09-30 | 2015-12-23 | 景德镇陶瓷学院 | Preparation method of ZnO micro-nano ball powder with multilevel structure and product prepared with method |
| CN106563362A (en) * | 2016-10-25 | 2017-04-19 | 江苏大学 | Preparing method and usage of low-oxidization-degree graphene/zinc oxide nanometer composite film |
| CN113809272A (en) * | 2020-06-16 | 2021-12-17 | Tcl科技集团股份有限公司 | Zinc oxide nano material, preparation method, electron transmission film and light emitting diode |
| CN113809272B (en) * | 2020-06-16 | 2025-02-28 | Tcl科技集团股份有限公司 | Zinc oxide nanomaterial and preparation method, electron transport film, light-emitting diode |
| CN114409923A (en) * | 2021-11-25 | 2022-04-29 | 华南农业大学 | Multifunctional self-healing antibacterial hydrogel and preparation method and application thereof |
| CN114409923B (en) * | 2021-11-25 | 2023-10-20 | 华南农业大学 | Multifunctional self-healing antibacterial hydrogel and preparation method and application thereof |
| CN115536054A (en) * | 2022-06-28 | 2022-12-30 | 山东科技职业学院 | Preparation method of zinc oxide nano-rods with different particle diameters |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1281507C (en) | 2006-10-25 |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Zhejiang Henglin Chair Industrial Company Assignor: Zhejiang University Contract fulfillment period: 2009.9.7 to 2017.9.6 Contract record no.: 2009330002391 Denomination of invention: Method for repairing nano stick of zinc oxide in even diameter Granted publication date: 20061025 License type: Exclusive license Record date: 2009.9.27 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.9.7 TO 2017.9.6; CHANGE OF CONTRACT Name of requester: ZHEJIANG HENG LIN CHAIRS CO., LTD. Effective date: 20090927 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20061025 Termination date: 20180406 |
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| CF01 | Termination of patent right due to non-payment of annual fee |