CN100391848C - Process for preparing zinc oxide nano stick - Google Patents
Process for preparing zinc oxide nano stick Download PDFInfo
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- CN100391848C CN100391848C CNB2006100496799A CN200610049679A CN100391848C CN 100391848 C CN100391848 C CN 100391848C CN B2006100496799 A CNB2006100496799 A CN B2006100496799A CN 200610049679 A CN200610049679 A CN 200610049679A CN 100391848 C CN100391848 C CN 100391848C
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Abstract
The present invention discloses a method for preparing a zinc oxide nanostick, which comprises the following steps that: step 1, zinc nitrate is dissolved in deionized water, and then hexamethylenetetramine and organic matter dispersant are added and uniformly mixed; step 2, the mixed solution is heated to 70 to 95 DEG C, zinc oxide seed solution is added to react for 1 for 10 hours, and the zinc oxide nanostick is obtained through centrifugal drying. The present invention which utilizes a zinc oxide seed aided chemical reaction method can overcome the problem that straight and fine zinc oxide nanostick is difficult to prepare. The length and the diameter of the zinc oxide nanostick can be effectively controlled by changing the kinds of organic matter dispersant and the use quantity of the zinc oxide seed. The present invention has the advantages of simple method, high yield and low cost.
Description
Technical field
The present invention relates to a kind of method for preparing zinc oxide nano rod.
Background technology
Zinc oxide is with a wide range of applications it, thereby becomes current research focus owing to has the energy gap of broad and big exciton bind energy on luminous particularly blue light.And the development of nanotechnology makes nano zine oxide have many new character and Application Areas, as nano laser, an emission and field-effect transistor etc.Method by gas phase or chemistry has prepared various nano structure of zinc oxide at present.But as the elementary cell of following nano-device, it is particularly important that the research of zinc oxide one-dimensional nanomaterial seems.Because the formation temperature of zinc oxide in solution have only 60 ℃, so chemical method has advantages such as simple, that cost is low, a large amount of in the preparation nano zine oxide, becomes the most potential method.Prepare in the process of nano structure of zinc oxide at chemical method at present,, make to be difficult to the straight zinc oxide nano rod of growth because the dendritic growth of zinc oxide is difficult to avoid.The recent zinc-oxide film on substrate of discovering can effectively be controlled the one-dimensional growth of nano zine oxide.Therefore based on above-mentioned thought, the present invention proposes an a large amount of method for preparing straight and thin zinc oxide nano rod, seed assisted chemical reactions method.
Summary of the invention
The method that the purpose of this invention is to provide the straight and thin zinc oxide nano rod of a kind of a large amount of preparation.
The method for preparing zinc oxide nano rod of the present invention, step is as follows:
1) zinc nitrate is dissolved in the deionized water, add hexamethylenetetramine then and the organism dispersant is even, the weight ratio of zinc nitrate and organism dispersion agent is 1: 1, the mol ratio of hexamethylenetetramine and zinc nitrate 〉=1, said organism dispersion agent is polyvinyl alcohol, polyoxyethylene glycol or Polyvinylpyrolidone (PVP);
2) mixing solutions is heated to 70～95 ℃, adds zinc oxide seed solution, reacted 1～10 hour, centrifugal drying obtains the nanometer rod of zinc oxide, and the mol ratio of zinc oxide seed and zinc nitrate is 1: 40～400.
Among the present invention, said organism dispersion agent can be polyvinyl alcohol, polyoxyethylene glycol or Polyvinylpyrolidone (PVP).By adding different organism dispersion agents, the length that can make zinc oxide nano rod is in 200～800nm range.Zinc oxide seed can adopt the method preparation of people such as Yang Pei east at " German applied chemistry " (Angew.Chem.Int.Ed.2002,41,1188) bibliographical information.By changing the molar ratio in zinc oxide seed and zinc source, the diameter that can make zinc oxide nano rod is in 20～200nm range.
Beneficial effect of the present invention is:
1. utilize zinc oxide seed assisted chemical reactions method can solve the problem of the difficult preparation of straight and thin zinc oxide nano rod; The kind by changing the organism dispersion agent and the usage quantity of zinc oxide seed be the length and the diameter of controlled oxidation zinc nanometer rod effectively.
2. the inventive method technology is simple, output is big, cost is low.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the zinc oxide nano rod that makes of the present invention.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
1) preparation of zinc oxide seed: the zinc acetate of 270mg is dissolved in the methyl alcohol of 60ml, stir after 5 minutes, solution is heated to 60 ℃, then 65ml is contained the methanol solution of 210mg potassium hydroxide, slowly be added drop-wise in the above-mentioned solution, and react the seed solution that obtained zinc oxide in 3 hours.
2) preparation of zinc oxide nano rod: the 2.7g zinc nitrate is dissolved in the deionized water of 400ml, stir after 5 minutes, add the 2.7g polyvinyl alcohol, 1.26g hexamethylenetetramine, after mixing, solution is heated to 95 ℃, the seed solution that in above-mentioned solution, adds 30ml zinc oxide then, reaction 3h takes out sample, and centrifugal drying obtains the nanometer rod of zinc oxide.Fig. 1 is the transmission electron microscope photo of zinc oxide nano rod, and as can be seen from the figure the diameter of zinc oxide nano rod is approximately 20nm, and length is approximately 800nm.
Embodiment 2:
1) preparation of zinc oxide seed: the zinc acetate of 270mg is dissolved in the methyl alcohol of 60ml, stir after 5 minutes, solution is heated to 60 ℃, then 65ml is contained the methanol solution of 210mg potassium hydroxide, slowly be added drop-wise in the above-mentioned solution, and react the seed solution that obtained zinc oxide in 3 hours.
2) preparation of zinc oxide nano rod: the 2.7g zinc nitrate is dissolved in the deionized water of 400ml, stir after 5 minutes, add the 2.7g Polyvinylpyrolidone (PVP), 1.26g hexamethylenetetramine, after mixing, solution is heated to 70 ℃, the seed solution that in above-mentioned solution, adds 30ml zinc oxide then, reaction 3h takes out sample, and centrifugal drying obtains the nanometer rod of zinc oxide.Its diameter is approximately 20nm, and length approximately is 400nm.
Embodiment 3:
1) preparation of zinc oxide seed: the zinc acetate of 27mg is dissolved in the methyl alcohol of 60ml, stir after 5 minutes, solution is heated to 60 ℃, then 65ml is contained the methanol solution of 21mg potassium hydroxide, slowly be added drop-wise in the above-mentioned solution, and react the seed solution that obtained zinc oxide in 3 hours.
2) preparation of zinc oxide nano rod: the 2.7g zinc nitrate is dissolved in the deionized water of 400ml, stir after 5 minutes, add the 2.7g polyoxyethylene glycol, 1.26g hexamethylenetetramine, after mixing, solution is heated to 95 ℃, the seed solution that in above-mentioned solution, adds 30ml zinc oxide then, reaction 3h takes out sample at last, and centrifugal drying obtains the nanometer rod of zinc oxide.The nearly 200nm of its diameter, length approximately is 600nm.
Claims (1)
1. method for preparing zinc oxide nano rod, step is as follows:
1) zinc nitrate is dissolved in the deionized water, add hexamethylenetetramine then and the organism dispersant is even, the weight ratio of zinc nitrate and organism dispersion agent is 1: 1, the mol ratio of hexamethylenetetramine and zinc nitrate 〉=1, said organism dispersion agent is polyvinyl alcohol, polyoxyethylene glycol or Polyvinylpyrolidone (PVP);
2) mixing solutions is heated to 70～95 ℃, adds zinc oxide seed solution, reacted 1～10 hour, centrifugal drying obtains the nanometer rod of zinc oxide, and the mol ratio of zinc oxide seed and zinc nitrate is 1: 40～400.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100496799A CN100391848C (en) | 2006-03-02 | 2006-03-02 | Process for preparing zinc oxide nano stick |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100496799A CN100391848C (en) | 2006-03-02 | 2006-03-02 | Process for preparing zinc oxide nano stick |
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| CN1821081A CN1821081A (en) | 2006-08-23 |
| CN100391848C true CN100391848C (en) | 2008-06-04 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101357320B (en) * | 2008-09-18 | 2010-06-09 | 福州大学 | One-dimensional nano-array zinc oxide solid-phase micro-extraction coating and preparation method thereof |
| CN103043706B (en) * | 2012-12-04 | 2014-09-10 | 华南师范大学 | Preparation method of zinc oxide nanorod with strong blue-violet light after being excited |
| CN103303965B (en) * | 2013-05-14 | 2015-04-01 | 上海交通大学 | Method for preparing multi-point top type zinc oxide nanorod structure |
| CN106119961B (en) * | 2016-06-15 | 2018-07-06 | 河南师范大学 | A kind of preparation method of the controllable single-crystal zinc-oxide nano stick of size |
| CN106564929A (en) * | 2016-10-21 | 2017-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for Ag doped ZnO nanometer gas sensitive material |
| CN106475104A (en) * | 2016-11-20 | 2017-03-08 | 吉林师范大学 | A kind of recyclable Corallium Japonicum Kishinouye type photocatalyst and preparation method thereof |
| CN107815851A (en) * | 2017-11-11 | 2018-03-20 | 钱景 | Biology sensor based on zinc oxide nano rod function bafta |
Citations (5)
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| CN1533985A (en) * | 2003-03-31 | 2004-10-06 | 上海大学 | Preparation method of nano-grade zinc oxide powder |
| CN1562762A (en) * | 2004-04-22 | 2005-01-12 | 上海交通大学 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
| WO2005044722A1 (en) * | 2003-11-06 | 2005-05-19 | Nanohybrid Co., Ltd. | Method for forming zno nano-array and zno nanowall for uv laser on silicon substrate |
| CN1693205A (en) * | 2005-04-26 | 2005-11-09 | 华中师范大学 | Nano zine oxide with excitating light strength and frequency tuning fluorescent frequency and it preparation |
| CN1736876A (en) * | 2005-07-14 | 2006-02-22 | 天津大学 | Method for large scale quick preparation of one-dimension zinc oxide array thin film in aqueous solution |
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2006
- 2006-03-02 CN CNB2006100496799A patent/CN100391848C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1533985A (en) * | 2003-03-31 | 2004-10-06 | 上海大学 | Preparation method of nano-grade zinc oxide powder |
| WO2005044722A1 (en) * | 2003-11-06 | 2005-05-19 | Nanohybrid Co., Ltd. | Method for forming zno nano-array and zno nanowall for uv laser on silicon substrate |
| CN1562762A (en) * | 2004-04-22 | 2005-01-12 | 上海交通大学 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
| CN1693205A (en) * | 2005-04-26 | 2005-11-09 | 华中师范大学 | Nano zine oxide with excitating light strength and frequency tuning fluorescent frequency and it preparation |
| CN1736876A (en) * | 2005-07-14 | 2006-02-22 | 天津大学 | Method for large scale quick preparation of one-dimension zinc oxide array thin film in aqueous solution |
Non-Patent Citations (2)
| Title |
|---|
| 一步溶液法制备ZnO亚微米晶体棒及其发光性能. 陈建刚，郭常新，张琳丽，胡俊涛.发光学报，第27卷第1期. 2006 |
| 一步溶液法制备ZnO亚微米晶体棒及其发光性能. 陈建刚，郭常新，张琳丽，胡俊涛.发光学报，第27卷第1期. 2006 * |
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| CN1821081A (en) | 2006-08-23 |
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Assignee: Zhejiang Haina Polytron Technologies Inc Assignor: Zhejiang University Contract fulfillment period: 2008.10.20 to 2013.9.30 Contract record no.: 2008330001423 Denomination of invention: Process for preparing zinc oxide nano stick Granted publication date: 20080604 License type: Exclusive license Record date: 20081028 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.20 TO 2013.9.30; CHANGE OF CONTRACT Name of requester: ZHEJIANG PROVINCE HAINA TECHNOLOGY CO., LTD. Effective date: 20081028 |
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