CN114042931A - Method for synthesizing gold nanorods by using CTAC (cetyl trimethyl ammonium chloride) and NaOL (NaOL) as double surfactants - Google Patents
Method for synthesizing gold nanorods by using CTAC (cetyl trimethyl ammonium chloride) and NaOL (NaOL) as double surfactants Download PDFInfo
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- CN114042931A CN114042931A CN202111400807.0A CN202111400807A CN114042931A CN 114042931 A CN114042931 A CN 114042931A CN 202111400807 A CN202111400807 A CN 202111400807A CN 114042931 A CN114042931 A CN 114042931A
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 47
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims abstract description 8
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960001553 phloroglucinol Drugs 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 101710134784 Agnoprotein Proteins 0.000 claims description 3
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 10
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 8
- 238000003917 TEM image Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- -1 iodide ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- XBECFEJUQZXMFE-UHFFFAOYSA-N n-(4-aminobutyl)acetamide;hydrochloride Chemical compound Cl.CC(=O)NCCCCN XBECFEJUQZXMFE-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for synthesizing gold nanorods by using CTAC and NaOL as double surfactants, which comprises the following steps: (1) preparing a seed solution; (2) preparing a growth solution; (3) and generating the gold nanorods. According to the invention, CTAC and NaOL are used as double surfactants, phloroglucinol is used as a reducing agent, the cost is low, the reaction condition is simple, the reaction process is stable and controllable, and the purity and the yield of the synthesized gold nanorod are high.
Description
Technical Field
The invention relates to the technical field of metal nano material synthesis, in particular to a method for synthesizing gold nanorods by taking CTAC and NaOL as double surfactants.
Background
In recent years, research in the field of precious metal nanoparticles has been in the field of researchers, and gold nanorods can display Local Surface Plasmon Resonance (LSPRs) related to size and shape due to the unique one-dimensional nanostructure, so that the gold nanorods have attracted extensive attention in the fields of sensing, Surface Enhanced Raman Scattering (SERS), biological diagnosis, photothermal therapy and the like and have wide application prospects. Therefore, industrialization of gold nanorods has become one of the major research directions of researchers.
The application publication No. CN112974829A, Chinese patent of 6.18.2021, discloses a method for preparing gold nanorod material by reducing hydroquinone under the action of double surfactants, under the combined action of Cetyl Trimethyl Ammonium Bromide (CTAB) and sodium oleate (NaOL), the gold nanorod is synthesized by adopting a seed-mediated method, which comprises the following steps: mixing a certain amount of CTAB and chloroauric acid, adding sodium borohydride prepared from an ice water mixture, and violently stirring for 2 minutes by a magnetic stirrer to change the solution from golden yellow to brown yellow; standing for 30 minutes to obtain a seed solution; dissolving CTAB and NaOL with corresponding low concentrations in another bottle at 50 deg.C as growth solution, cooling to about 30 deg.C, and adding silver nitrate and chloroauric acid; stirring at room temperature for 60-90 min, and clarifying the solution by golden yellow; adding hydroquinone and the seed solution in sequence, stirring vigorously by using a magnetic stirrer, and standing for 12 hours at constant temperature of 30 ℃ to obtain a final product. The gold nanorod synthesis method has the following defects: CTAB is used as a surfactant, and a certain amount of iodide ions are stored in the CTAB, so that the purity of the synthesized gold nanorods can be reduced; the hydroquinone is used as a reducing agent, the gold element in the solution can not be completely converted into the gold nanorods, and the yield is low.
Disclosure of Invention
The invention aims to solve the technical problems of the gold nanorod synthesis method in the prior art, provides the method for synthesizing the gold nanorods by taking CTAC and NaOL as double surfactants, and has the advantages of simple reaction conditions, stable and controllable reaction process and high purity and yield of the gold nanorods.
In order to achieve the purpose, the invention adopts the following technical scheme: the invention discloses a method for synthesizing gold nanorods by using CTAC and NaOL as double surfactants, which comprises the following steps:
(1) preparation of seed solutions
10mL of a 0.1M CTAB solution and 0.25mL of 10mM HAuCl4After the solutions were mixed, 0.6mL of 0.01M NaBH was added4Stirring the solution, and standing at constant temperature to obtain a seed solution.
(2) Preparation of growth solution
10mL of 0.1M CTAC solution and 0.061g of NaOL were dissolved in 8.4mL of water; 40 μ L of 0.1M AgNO was added3The solution was allowed to stand at a constant temperature, and 1mL of 10mM HAuCl was added4Stirring, and standing at constant temperature until the solution becomes clear to obtain a growth solution. In the invention, phloroglucinol is used as a reducing agent, the phloroglucinol can be added in an excessive amount without influencing the reaction, and the gold element can be ensured to be completely reduced, so that the yield is higher.
(3) Generation of gold nanorods
Adjusting the pH value of the growth solution to 7.9-8.1, sequentially adding 0.9mL of 0.1M phloroglucinol solution and 32 mu L of seed solution, stirring, standing at constant temperature, centrifuging to remove supernatant, and obtaining a centrifugal product, namely the gold nanorod.
Preferably, in step (1), the NaBH is4The solution was prepared by the following method: with ice-water mixture and the required amount of NaBH4And (4) mixing.
Preferably, in the step (1), the stirring conditions are as follows: the stirring speed is 1500rpm, and the stirring time is 1-2 min; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 30 min.
Preferably, in step (2), 110mL of 0.1M CTAC solution and 0.061g of NaOL are dissolved in 50 ℃ water, and then cooled to 30 ℃.
Preferably, in the step (2), the stirring conditions are as follows: the rotating speed is 400rpm, and the stirring time is 60-90 min; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 30 min.
Preferably, in step (2), 0.1M NaHCO is used3The pH value of the growth solution is adjusted to 7.9-8.1 by the solution. In the invention, NaHCO is used3Adjusting the pH, NaHCO3The alkalescence of the reaction kettle can better regulate and control the pH value, and the reaction cannot be too excessiveAnd the purity of the synthesized gold nanorods is reduced.
Preferably, in the step (3), the stirring speed is 1500 rpm; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 2 hr. The reaction condition is water bath heating, the water bath temperature is 30 ℃, the reaction condition is easy to control, the purity of the gold nanorods can be greatly improved by the water bath heating at the temperature of 30 ℃, and the final yield is higher.
Therefore, the invention has the following beneficial effects: the method has the advantages of simple reaction conditions, stable and controllable reaction process, low cost, simple reaction conditions, stable and controllable reaction process, and high purity and yield of the synthesized gold nanorods.
Drawings
FIG. 1 is a transmission electron micrograph of the gold nanorods obtained in example 1.
FIG. 2 is a transmission electron micrograph of the gold nanorods obtained in comparative example 1.
FIG. 3 is a transmission electron micrograph of the gold nanorods obtained in comparative example 2.
FIG. 4 is a transmission electron micrograph of the gold nanorods obtained in comparative example 3.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
(1) Preparation of seed solutions
10mL of a 0.1M CTAB solution and 0.25mL of 10mM HAuCl4After the solutions were mixed, 0.6mL of 0.01M NaBH was added4Stirring the solution, standing at constant temperature, wherein the stirring speed is 1500rpm, and the stirring time is 1 min; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, standing for 30min to obtain seed solution; in which NaBH4The solution was prepared by the following method: with ice-water mixture and the required amount of NaBH4And (4) mixing.
(2) Preparation of growth solution
Dissolving 10mL of 0.1M CTAC solution and 0.061g of NaOL in 8.4mL of water at 50 ℃, and cooling to 30 ℃ after dissolving; 40 μ L of 0.1M AgNO was added3The solution was allowed to stand at a constant temperature, and 1mL of 10mM HAuCl was added4Stirring, wherein the stirring conditions are as follows: the rotating speed is 400rpm, and the stirring time is 90 min; constant temperature staticPlacing the solution until the solution becomes clear to obtain a growth solution; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 30 min.
(3) Generation of gold nanorods
The growth solution pH was adjusted with 0.1M NaHCO3After the pH value of the solution is adjusted to 7.9, 0.9mL of 0.1M phloroglucinol solution and 32 mu L of seed solution are sequentially added, the mixture is stirred and then kept stand at a constant temperature, the mixture is centrifuged twice (7000rpm, 30min) to remove supernatant, the centrifugal product is the gold nanorod, and the stirring speed is 1500 rpm; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 2 hr. The purity of the obtained gold nanorods is 94%, the yield is 98%, and a transmission electron microscope image thereof is shown in FIG. 1.
As can be seen from FIG. 1, the length of the gold nanorods is approximately 114.2nm, the diameter is 43.8nm, and the aspect ratio is 2.6.
Comparative example 1
Comparative example 1 differs from example 1 in that 10mL of 0.1M CTAB solution is used instead of 10mL of 0.1M CTAC solution, and the rest is exactly the same as example 1.
The purity of the obtained gold nanorods is 85%, the yield is 66%, and a transmission electron microscope image is shown in FIG. 2.
Comparative example 2
Comparative example 2 differs from example 2 in that 0.44g of 5-bromosalicylic acid was used instead of 0.061g of NaOL, and the rest was exactly the same as example 1.
The purity of the obtained gold nanorods is 70%, the yield is 95%, and a transmission electron microscope image thereof is shown in FIG. 3.
Comparative example 3
Comparative example 3 is identical to example 1 except that a hydroquinone solution is used instead of a phloroglucinol solution.
The purity of the obtained gold nanorods is 80%, the yield is 76%, and a transmission electron microscope image thereof is shown in FIG. 4.
The comparison shows that the yield and purity of the gold nanorods are greatly improved in example 1 compared with those in comparative examples 1-3, which shows that the yield and purity of the gold nanorods can be greatly improved by using CTAC and NaOL as double surfactants and phloroglucinol as a reducing agent in the invention.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (7)
- A method for synthesizing gold nanorods by using CTAC and NaOL as double surfactants is characterized in that,the method comprises the following steps:(1) preparation of seed solutions10mL of a 0.1M CTAB solution and 0.25mL of 10mM HAuCl4After the solutions were mixed, 0.6mL of 0.01M NaBH was added4Stirring the solution, and standing at constant temperature to obtain a seed solution;(2) preparation of growth solution10mL of 0.1M CTAC solution and 0.061g of NaOL were dissolved in 8.4mL of water; 40 μ L of 0.1M AgNO was added3The solution was allowed to stand at a constant temperature, and 1mL of 10mM HAuCl was added4Stirring, and standing at constant temperature until the solution becomes clear to obtain a growth solution;(3) generation of gold nanorodsAdjusting the pH value of the growth solution to 7.9-8.1, sequentially adding 0.9mL of 0.1M phloroglucinol solution and 32 mu L of seed solution, stirring, standing at constant temperature, centrifuging to remove supernatant, and obtaining a centrifugal product, namely the gold nanorod.
- 2. The method for CTAC and NaOL synthesis of gold nanorods for bi-surfactant synthesis according to claim 1, wherein in step (1), the NaBH is added4The solution was prepared by the following method: with ice-water mixture and the required amount of NaBH4And (4) mixing.
- 3. The method for synthesizing gold nanorods with CTAC and NaOL as double surfactants according to claim 1 or 2, wherein in the step (1), the stirring condition is: the stirring speed is 1500rpm, and the stirring time is 1-2 min; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 30 min.
- 4. The method for synthesizing gold nanorods with CTAC and NaOL as double surfactants according to claim 1, wherein in step (2), 110mL of 0.1M CTAC solution and 0.061g of NaOL are dissolved in 50 ℃ water, and then cooled to 30 ℃.
- 5. The method for synthesizing gold nanorods with CTAC and NaOL as double surfactants according to claim 1, wherein in the step (2), the stirring condition is: the rotating speed is 400rpm, and the stirring time is 60-90 min; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 30 min.
- 6. The method for synthesizing gold nanorods with CTAC and NaOL as double surfactants according to claim 1, wherein in step (3), 0.1M NaHCO is used3The pH value of the growth solution is adjusted to 7.9-8.1 by the solution.
- 7. The method for synthesizing gold nanorods with CTAC and NaOL as double surfactants according to claim 1, wherein in the step (3), the stirring speed is 1500 rpm; the constant temperature standing condition is as follows: heating in water bath at 30 deg.C, and standing for 2 hr.
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|---|---|---|---|
| CN202111400807.0A CN114042931A (en) | 2021-11-19 | 2021-11-19 | Method for synthesizing gold nanorods by using CTAC (cetyl trimethyl ammonium chloride) and NaOL (NaOL) as double surfactants |
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| CN202111400807.0A CN114042931A (en) | 2021-11-19 | 2021-11-19 | Method for synthesizing gold nanorods by using CTAC (cetyl trimethyl ammonium chloride) and NaOL (NaOL) as double surfactants |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN107931627A (en) * | 2017-11-10 | 2018-04-20 | 厦门斯贝克科技有限责任公司 | A kind of ultra-thin shell isolated gold nanorods synthetic method |
| CN108672716A (en) * | 2018-05-23 | 2018-10-19 | 厦门斯贝克科技有限责任公司 | A kind of preparation method of silver gold-covered nano stick |
| WO2020254630A1 (en) * | 2019-06-20 | 2020-12-24 | Universite Claude Bernard Lyon 1 | Method for preparing high-concentration penta-twinned gold nanoparticles |
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- 2021-11-19 CN CN202111400807.0A patent/CN114042931A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN107931627A (en) * | 2017-11-10 | 2018-04-20 | 厦门斯贝克科技有限责任公司 | A kind of ultra-thin shell isolated gold nanorods synthetic method |
| CN108672716A (en) * | 2018-05-23 | 2018-10-19 | 厦门斯贝克科技有限责任公司 | A kind of preparation method of silver gold-covered nano stick |
| WO2020254630A1 (en) * | 2019-06-20 | 2020-12-24 | Universite Claude Bernard Lyon 1 | Method for preparing high-concentration penta-twinned gold nanoparticles |
Non-Patent Citations (1)
| Title |
|---|
| ZHUOXUAN LU ET AL.: "Preparation of Gold Nanorods Using 1, 2, 4-Trihydroxybenzene as a Reducing Agent", JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY, 31 August 2015 (2015-08-31), pages 6230 - 6235 * |
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