CN102284705A - Method for preparing gold nanorod capable of regulating length-diameter ratio in large range - Google Patents
Method for preparing gold nanorod capable of regulating length-diameter ratio in large range Download PDFInfo
- Publication number
- CN102284705A CN102284705A CN201110232796XA CN201110232796A CN102284705A CN 102284705 A CN102284705 A CN 102284705A CN 201110232796X A CN201110232796X A CN 201110232796XA CN 201110232796 A CN201110232796 A CN 201110232796A CN 102284705 A CN102284705 A CN 102284705A
- Authority
- CN
- China
- Prior art keywords
- solution
- gold
- preparation
- growth
- gold nanorods
- 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
Images
Abstract
The invention discloses a method for preparing a gold nanorod capable of regulating the length-diameter ratio in a large range, specifically comprising the following steps of: the preparation for gold seed solution, i.e. reducing hydrogen tetrachloroaurate hydrate by a strong reducing agent sodium borohydride in cetyl trimethyl ammonium bromide (CTAB) surface modifying agent solution to obtain the gold seed solution; the preparation for growth solution, i.e. preparing the mixed solution of the CTAB, the hydrogen tetrachloroaurate hydrate and silver nitrate in a molar ratio of 20: 1: (0.1 to 20): 1: 5, and adding butenoic acid solution to obtain the growth solution; and the growth of a gold nanorod: injecting the gold seed solution in the growth solution, and reacting for 6 to 12 hours to obtain the gold nanorod. In the invention, butenoic acid is used as a growth solution modifying agent, which solves the biotoxicity and biologic modification problems brought by the CTAB. The prepared gold nanorod with a low length-diameter ratio has a high yield up to about 90%, a narrow size distribution and a length-diameter ratio of about 1.92. The length-diameter ratio of the prepared gold nanorod can be regulated in a large range from 1.9 to 7.5.
Description
Technical field:
The present invention relates to the nano material preparation technical field, be specifically related to the preparation method of the regulatable gold nanorods of a kind of draw ratio.
Background technology:
The physical chemistry of golden nanometer particle and photoelectric property and its pattern and size are closely related, common gold nanorods draw ratio is 2-7, because accurate one dimension pattern, the surface plasma body resonant vibration absworption peak is split into two, lateral surfaces plasma resonance absworption peak and a special vertical table surface plasma resonance absworption peak near the 520nm, wherein vertical table surface plasma resonance absworption peak position can be regulated by changing the gold nanorods draw ratio, crosses the near infrared region from visible region.Gold nanorods has special nano-meter characteristic, makes it have broad application prospects in fields such as biomedical chemical catalysis optics photoelectrons.
The preparation method of gold nanorods mainly contains template electrochemical process seed mediated growth method photochemical method at present.Wherein by Catherine J. Murphy propose (
Adv. Mater., 2003,13,1389-1393), the improved seed mediated growth method of Mostafa A.El-Sayed (
Chem. Mater., 2003,15,1957-1962), easy and simple to handle because of the reaction condition gentleness, be used widely.This method often adopts the CTAB(softex kw) simultaneously as the shape inducer of the coating material and the growth solution of seed solution, in the seed growth process, induce reagent to come controlling dimension and shape as pattern by CTAB, can realize regulation and control, thereby realize that its optical property is from the fine adjustments of visible region to the near infrared region gold nanorods draw ratio and vertical table surface plasma resonance absworption peak.Yet, in the disclosed seed mediated growth method of above-mentioned document, adopt CTAB as part.Existing experiment report result shows that CTAB has bigger bio-toxicity, has limited the application of the gold nanorods of this method preparation in fields such as biological detection and sensings.In addition, be difficult to obtain the gold nanorods with higher yields and Size Distribution broad of short draw ratio (about 2.0) according to seed mediated growth method of the prior art.
Thereby this area presses for provides a kind of have low bio-toxicity, the preparation method of the gold nanorods that draw ratio can be regulated on a large scale.
Summary of the invention
Technical problem:The object of the present invention is to provide gold nanorods that a kind of draw ratio can regulate and control on a large scale
The preparation method, this method is easy and simple to handle, productive rate height, the narrow size distribution of gold nanorods.
Technical scheme:The preparation method of the gold nanorods that draw ratio of the present invention can be regulated and control on a large scale is specially:
The preparation of step 1) gold seeds solution: in softex kw finishing agent solution, obtain gold seeds solution with strong reductant sodium borohydride reduction tetra chlorauric acid;
Step 2) preparation of growth solution: the mixed solution of preparation softex kw, tetra chlorauric acid and silver nitrate, three's mol ratio is 20:1:0.1 ~ 20:1:5, adds butenoic acid solution, obtains growth solution;
The growth of step 3) gold nanorods: gold seeds solution is injected growth solution, reacted 6-12 hour, obtain gold nanorods.
Wherein the molar concentration of softex kw is 0.05 ~ 0.3 in the described gold seeds solution of step 1)
, the mol ratio of strong reductant and tetra chlorauric acid is 1:10 ~ 50.
Wherein in step 2) in, the molar concentration of softex kw is 0.001 ~ 0.03
Beneficial effect:Compared with prior art, gold nanorods preparation method of the present invention has following advantage:
1, adopts butenoic acid as the growth solution dressing agent, solved bio-toxicity and bio-modification problem that CTAB brings.
The productive rate height of the golden nano stick with short length-diameter ratio that 2, prepares can be up to about 90%, and Size Distribution is narrower, and draw ratio is about 1.92.
The draw ratio of the gold nanorods that 3, prepares can 1.9 ~ 7.5 on a large scale in regulation and control.
Above-mentioned advantage has been improved the character of existing gold nanorods, helps further enlarging its application, especially in fields such as biological detections.
Description of drawings
Fig. 1 is the delustring spectrum of the product gold nanorods of the embodiment of the invention 1 preparation;
Fig. 2 is the delustring spectrum of the product gold nanorods of the embodiment of the invention 2 preparations;
The specific embodiment
To achieve these goals, preparation technology's flow process of gold nanorods of the present invention is: by in softex kw finishing agent solution, obtain gold seeds solution with strong reductant sodium borohydride reduction tetra chlorauric acid; The mixed solution of preparation softex kw tetra chlorauric acid and silver nitrate adds butenoic acid solution, obtains growth solution; A certain amount of seed solution is injected growth solution, reacted 6-12 hour, and obtain gold nanorods.The mol ratio by regulating silver nitrate and tetra chlorauric acid and the gold element mole of seed solution and growth solution are recently controlled the different draw ratios of gold nanorods.
Described gold nanorods is characterized in that adopting butenoic acid as the growth solution coating material gold nanorods of growing, and its draw ratio can recently be controlled by regulating the silver nitrate and the mol ratio of tetra chlorauric acid and the gold element mole of seed solution and growth solution.
Below illustrate the specific embodiment of the present invention, but content of the present invention be not limited to for example.
Embodiment one
1) preparation of gold seeds solution:
Under the stirring at room condition, be in the concentration of 20 mL
Softex kw and
In the mixed solution of tetra chlorauric acid, add rapidly
Fully cool off in the ice-water bath
Solution 2 ml, vigorous stirring stops after 2 minutes stirring, and obtains isabelline seed solution after the reaction.
2) preparation of growth solution:
The mixed liquor of preparation 10ml softex kw, tetra chlorauric acid and silver nitrate in clean reactor, wherein the softex kw molar concentration is
, the molar concentration of tetra chlorauric acid is
, the silver nitrate molar concentration is
At last mixed solution is placed
Water-bath in add
Butenoic acid solution stirs, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3) growth of gold nanorods:
In above-mentioned steps 2) in add the seed solution that 2ml has made in the growth solution of configuration in step 1).
The gold element mol ratio that makes seed solution and growth solution is 8:3, and gold nanorods promptly begins growth.Having added the growth solution behind the seed solution exists
Down reaction 12 hours of water-bath, obtain gold nanorods, the UV, visible light absorption spectra of product is seen accompanying drawing 1, as seen, vertical plasma absworption peak of gold nanorods is golden nano stick with short length-diameter ratio near 600 nm in the accompanying drawing 1.Referring to the gold nanorods draw ratio of accompanying drawing more than 2,90% is 1.92
0.1 average major axis is 25
3nm, average minor axis is 13
2nm, Size Distribution is narrower.
Embodiment two
1) preparation of gold seeds solution:
Under the stirring at room condition, be in the concentration of 20mL
Softex kw and
In the mixed solution of tetra chlorauric acid, add rapidly
Fully cool off in the ice-water bath
Solution 2 ml, vigorous stirring stops after 2 minutes stirring, and obtains isabelline seed solution after the reaction.
2) preparation of growth solution:
Preparation 10ml softex kw tetra chlorauric acid and silver nitrate mixes in clean reactor
Close liquid, wherein the softex kw molar concentration is
, the molar concentration of tetra chlorauric acid is
, the mol ratio of silver nitrate and tetra chlorauric acid is 16:3, at last mixed solution is placed
Water-bath in add
Butenoic acid solution stirs, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3) growth of gold nanorods:
In above-mentioned steps 2) in add the seed solution that 0.3ml has made in the growth solution of configuration in step 1), the gold element mol ratio that makes seed solution and growth solution is 2:5, gold nanorods promptly begins to grow.Having added the growth solution behind the seed solution exists
Down reaction 12 hours of water-bath, obtain gold nanorods, the UV, visible light absorption spectra of product is seen accompanying drawing 2, as seen, vertical plasma absworption peak of gold nanorods is longer draw ratio gold nanorods near 750nm in the accompanying drawing 2.Gold nanorods draw ratio more than 90% is 7.5
0.1 average major axis is 45
3nm, average minor axis is 6
2nm, Size Distribution is narrower.
Embodiment three
1) preparation of gold seeds solution:
Under the stirring at room condition, be in the concentration of 20mL
Softex kw and
In the mixed solution of tetra chlorauric acid, add rapidly
Fully cool off in the ice-water bath
Solution 2ml, vigorous stirring stops after 2 minutes stirring, and obtains isabelline seed solution after the reaction.
2) preparation of growth solution:
Preparation 10ml softex kw tetra chlorauric acid and silver nitrate mixes in clean reactor
Close liquid, wherein the softex kw molar concentration is
, the molar concentration of tetra chlorauric acid is
, the silver nitrate molar concentration is
, at last mixed solution is placed
Water-bath in add
Butenoic acid solution stirs, and solution becomes colorless from orange-yellow, promptly obtains growth solution.
3) growth of gold nanorods:
In above-mentioned steps 2) in add the gold seeds solution that 0.3ml has made in the growth solution of configuration in step 1), the gold element mol ratio that makes seed solution and growth solution is 2:5, gold nanorods promptly begins to grow.Having added the growth solution behind the seed solution exists
Down reaction 12 hours of water-bath, obtain draw ratio 4.0
0.1 gold nanorods.
The above only is a preferred implementation of the present invention; be noted that for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. the preparation method of the gold nanorods that can regulate and control on a large scale of a draw ratio is characterized in that this preparation method is specially:
The preparation of step 1) gold seeds solution: in softex kw finishing agent solution, obtain gold seeds solution with strong reductant sodium borohydride reduction tetra chlorauric acid;
Step 2) preparation of growth solution: the mixed solution of preparation softex kw, tetra chlorauric acid and silver nitrate, three's mol ratio is 20:1:0.1 ~ 20:1:5, adds butenoic acid solution, obtains growth solution;
The growth of step 3) gold nanorods: gold seeds solution is injected growth solution, reacted 6-12 hour, obtain gold nanorods.
2. the preparation method of the gold nanorods that a kind of draw ratio according to claim 1 can be regulated and control on a large scale, wherein the molar concentration of softex kw is 0.05 ~ 0.3 in the described gold seeds solution of step 1)
, the mol ratio of strong reductant and tetra chlorauric acid is 1:10 ~ 50.
3. the preparation method of the gold nanorods that a kind of draw ratio according to claim 1 and 2 can be regulated and control on a large scale, wherein step 2) in, the molar concentration of softex kw is 0.001 ~ 0.03
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110232796XA CN102284705A (en) | 2011-08-15 | 2011-08-15 | Method for preparing gold nanorod capable of regulating length-diameter ratio in large range |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110232796XA CN102284705A (en) | 2011-08-15 | 2011-08-15 | Method for preparing gold nanorod capable of regulating length-diameter ratio in large range |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102284705A true CN102284705A (en) | 2011-12-21 |
Family
ID=45331607
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110232796XA Pending CN102284705A (en) | 2011-08-15 | 2011-08-15 | Method for preparing gold nanorod capable of regulating length-diameter ratio in large range |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102284705A (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103722177A (en) * | 2013-11-07 | 2014-04-16 | 中国科学院长春应用化学研究所 | Method for preparing gold nanorods |
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN104249158A (en) * | 2013-06-26 | 2014-12-31 | 梁萍 | Growth solution for largely preparing gold nanorods |
| CN104249159A (en) * | 2013-06-26 | 2014-12-31 | 梁萍 | Method for largely preparing gold nanorods |
| CN104907578A (en) * | 2015-04-29 | 2015-09-16 | 福州大学 | Method for preparing gold nanorods |
| CN103243391B (en) * | 2013-05-02 | 2016-04-27 | 西安交通大学 | The preparation method of the gold nanorods of hydrogen peroxide-induced under a kind of alkaline condition |
| CN105562711A (en) * | 2016-01-13 | 2016-05-11 | 宁波欣能环境技术有限公司 | Method for preparing silver nanowire |
| CN106124476A (en) * | 2016-06-21 | 2016-11-16 | 中山大学 | Based on surface enhanced raman spectroscopy and the glucose sensing approach of bi-molecular probe |
| CN106825606A (en) * | 2017-01-23 | 2017-06-13 | 湖北大学 | A kind of preparation method and application of many size monodisperse gold nano grains |
| CN106984830A (en) * | 2017-05-25 | 2017-07-28 | 上海应用技术大学 | The preparation method of different draw ratio gold nanorods |
| CN108788177A (en) * | 2018-06-18 | 2018-11-13 | 上海大学 | The preparation method of gold nano grain |
| CN108817415A (en) * | 2018-06-29 | 2018-11-16 | 张贤芝 | A kind of preparation method of polyhedral structure Au nano particle |
| CN109570485A (en) * | 2018-11-08 | 2019-04-05 | 安徽中科赛飞尔科技有限公司 | A kind of gold nanorods and its preparation method and application |
| CN111774582A (en) * | 2020-07-28 | 2020-10-16 | 南京医科大学第二附属医院 | Method for accurately regulating and controlling length of gold nanorod |
| CN111893503A (en) * | 2020-07-20 | 2020-11-06 | 济南大学 | Preparation method of gold-iron oxyhydroxide-cuprous oxide-copper sulfide composite paper |
| CN114918425A (en) * | 2022-06-20 | 2022-08-19 | 杭州电子科技大学富阳电子信息研究院有限公司 | Gold nanorod with broadband adjustable absorption characteristic and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1795141A (en) * | 2003-05-13 | 2006-06-28 | 新留康郎 | Method for preparation of metal nano-rod and use thereof |
| WO2008130999A1 (en) * | 2007-04-20 | 2008-10-30 | William Marsh Rice University | Gram-scale synthesis of well-defined gold nanorods |
| CN101343778A (en) * | 2008-08-29 | 2009-01-14 | 北京航空航天大学 | Process for producing golden nano stick with short length-diameter ratio |
| JP2009270128A (en) * | 2008-04-30 | 2009-11-19 | Osaka Prefecture Univ | Method for producing gold nanorod |
| CN101758243A (en) * | 2010-01-28 | 2010-06-30 | 中国科学院长春应用化学研究所 | Preparation method of hollow gold nanometer cage |
-
2011
- 2011-08-15 CN CN201110232796XA patent/CN102284705A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1795141A (en) * | 2003-05-13 | 2006-06-28 | 新留康郎 | Method for preparation of metal nano-rod and use thereof |
| WO2008130999A1 (en) * | 2007-04-20 | 2008-10-30 | William Marsh Rice University | Gram-scale synthesis of well-defined gold nanorods |
| JP2009270128A (en) * | 2008-04-30 | 2009-11-19 | Osaka Prefecture Univ | Method for producing gold nanorod |
| CN101343778A (en) * | 2008-08-29 | 2009-01-14 | 北京航空航天大学 | Process for producing golden nano stick with short length-diameter ratio |
| CN101758243A (en) * | 2010-01-28 | 2010-06-30 | 中国科学院长春应用化学研究所 | Preparation method of hollow gold nanometer cage |
Non-Patent Citations (2)
| Title |
|---|
| 王明星等: "金纳米棒的合成及应用研究进展", 《广东化工》 * |
| 王立英等: "金属纳米颗粒制备中的还原剂与修饰剂", 《化学进展》 * |
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243391B (en) * | 2013-05-02 | 2016-04-27 | 西安交通大学 | The preparation method of the gold nanorods of hydrogen peroxide-induced under a kind of alkaline condition |
| CN104249158A (en) * | 2013-06-26 | 2014-12-31 | 梁萍 | Growth solution for largely preparing gold nanorods |
| CN104249159A (en) * | 2013-06-26 | 2014-12-31 | 梁萍 | Method for largely preparing gold nanorods |
| CN103722177B (en) * | 2013-11-07 | 2016-07-06 | 中国科学院长春应用化学研究所 | A kind of preparation method of gold nanorods |
| CN103722177A (en) * | 2013-11-07 | 2014-04-16 | 中国科学院长春应用化学研究所 | Method for preparing gold nanorods |
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN104907578A (en) * | 2015-04-29 | 2015-09-16 | 福州大学 | Method for preparing gold nanorods |
| CN105562711B (en) * | 2016-01-13 | 2018-07-20 | 宁波欣能环境技术有限公司 | A kind of preparation method of nano silver wire |
| CN105562711A (en) * | 2016-01-13 | 2016-05-11 | 宁波欣能环境技术有限公司 | Method for preparing silver nanowire |
| CN106124476A (en) * | 2016-06-21 | 2016-11-16 | 中山大学 | Based on surface enhanced raman spectroscopy and the glucose sensing approach of bi-molecular probe |
| CN106825606B (en) * | 2017-01-23 | 2019-04-30 | 湖北大学 | A kind of more size monodisperse gold nano grains and its preparation method and application |
| CN106825606A (en) * | 2017-01-23 | 2017-06-13 | 湖北大学 | A kind of preparation method and application of many size monodisperse gold nano grains |
| CN106984830A (en) * | 2017-05-25 | 2017-07-28 | 上海应用技术大学 | The preparation method of different draw ratio gold nanorods |
| CN108788177A (en) * | 2018-06-18 | 2018-11-13 | 上海大学 | The preparation method of gold nano grain |
| CN108817415A (en) * | 2018-06-29 | 2018-11-16 | 张贤芝 | A kind of preparation method of polyhedral structure Au nano particle |
| CN109570485A (en) * | 2018-11-08 | 2019-04-05 | 安徽中科赛飞尔科技有限公司 | A kind of gold nanorods and its preparation method and application |
| CN111893503A (en) * | 2020-07-20 | 2020-11-06 | 济南大学 | Preparation method of gold-iron oxyhydroxide-cuprous oxide-copper sulfide composite paper |
| CN111893503B (en) * | 2020-07-20 | 2021-10-26 | 济南大学 | Preparation method of gold-iron oxyhydroxide-cuprous oxide-copper sulfide composite paper |
| CN111774582A (en) * | 2020-07-28 | 2020-10-16 | 南京医科大学第二附属医院 | Method for accurately regulating and controlling length of gold nanorod |
| CN114918425A (en) * | 2022-06-20 | 2022-08-19 | 杭州电子科技大学富阳电子信息研究院有限公司 | Gold nanorod with broadband adjustable absorption characteristic and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102284705A (en) | Method for preparing gold nanorod capable of regulating length-diameter ratio in large range | |
| CN101343778B (en) | Process for producing golden nano stick with short length-diameter ratio | |
| CN106270543B (en) | The method for continuously preparing the controllable Triangular nanoplates of arrangement mode | |
| CN102554258B (en) | Method for preparing metal silver nanostructure in water solution | |
| CN104209533B (en) | Method for rapidly preparing gold nanorod | |
| CN104841950B (en) | A kind of preparation method of dog bone-shaped gold nanocrystals | |
| CN105036070B (en) | Gold nanorod-silicon dioxide core-shell structure nanometer material, preparation method and application | |
| CN102826585B (en) | Method for producing ultra-small water soluble near-infrared Ag2S quantum dots | |
| CN104070177B (en) | Preparation method for silver and gold nano-particles | |
| CN104625086A (en) | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method | |
| CN103722177B (en) | A kind of preparation method of gold nanorods | |
| CN105923636A (en) | Preparation method of monodisperse hollow mesoporous silica nanoparticle | |
| CN103613101B (en) | A kind of preparation method with dendroid pore passage structure mesoporous silicon oxide shape nanometer ball | |
| CN106563811B (en) | A kind of method that sea urchin shape Ag-ZnO nano-particles are continuously prepared using micro passage reaction | |
| CN104551012A (en) | Crystal seed growth method for preparing gold nano-particles | |
| WO2008081917A1 (en) | Spherical ferrite nanoparticle and method for production thereof | |
| CN102078617B (en) | Method for synthesizing mesoporous silica-based nanocomposite embedded with gold nanorods | |
| CN103243391A (en) | Method for preparing gold nanorods through induction of hydrogen peroxide under alkaline condition | |
| KR20080069058A (en) | Sythesis of gold nanoparticles of various crystal shapes using halide ion | |
| Chou et al. | Studies on the continuous precipitation of silver nanoparticles | |
| CN105712294B (en) | The oriented and ordered array of nanometer gold bar large area, its preparation method and application | |
| CN104551008A (en) | Adjustable spectrum gold nanoshell preparation method | |
| CN102502834B (en) | Method for preparing surfactant-directed grown superfine bismuth molybdate nano rods | |
| CN109604634B (en) | Preparation method of gold nanoparticles with different particle sizes | |
| CN104249158A (en) | Growth solution for largely preparing gold nanorods |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111221 |