CN112974829A - Method for preparing gold nanorod material by reducing hydroquinone under double surfactants - Google Patents
Method for preparing gold nanorod material by reducing hydroquinone under double surfactants Download PDFInfo
- Publication number
- CN112974829A CN112974829A CN202011603115.1A CN202011603115A CN112974829A CN 112974829 A CN112974829 A CN 112974829A CN 202011603115 A CN202011603115 A CN 202011603115A CN 112974829 A CN112974829 A CN 112974829A
- Authority
- CN
- China
- Prior art keywords
- solution
- ctab
- hydroquinone
- gold
- gold nanorod
- 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
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 17
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 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 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 230000009471 action Effects 0.000 claims abstract description 10
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 9
- 239000005457 ice water Substances 0.000 claims abstract description 7
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 4
- 230000001404 mediated effect Effects 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 28
- 239000010931 gold Substances 0.000 claims description 21
- 235000010323 ascorbic acid Nutrition 0.000 claims description 14
- 239000011668 ascorbic acid Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 230000009467 reduction Effects 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000002159 nanocrystal Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 230000009977 dual effect Effects 0.000 claims description 4
- 238000005054 agglomeration Methods 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229940072107 ascorbate Drugs 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 101710134784 Agnoprotein Proteins 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 229910001961 silver nitrate Inorganic materials 0.000 abstract 1
- 229960005070 ascorbic acid Drugs 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 238000001308 synthesis method Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
Abstract
The invention discloses a method for preparing a gold nanorod material by reducing hydroquinone under the action of a double surfactant, which synthesizes gold nanorods by adopting a seed-mediated method under the combined action of Cetyl Trimethyl Ammonium Bromide (CTAB) and sodium oleate (NaOL). The method comprises the following steps: mixing CTAB with chloroauric acid (HAuCl)4) Mixing ofMixing with a bottle, adding ice-water mixture to obtain sodium borohydride (NaBH)4) After 2 minutes of vigorous stirring with a magnetic stirrer, the solution turned from golden yellow to brown-yellow. Standing for 30 minutes to obtain a seed solution; dissolving CTAB and NaOL at low concentration in another bottle at 50 deg.C to obtain growth solution, cooling to about 30 deg.C, and adding silver nitrate (AgNO)3) And chloroauric acid. Stirring at room temperature for 60-90 min, and clarifying the solution by golden yellow; hydroquinone and seed solution are added in sequence. And vigorously stirred by a magnetic stirrer, and then kept standing for 12 hours at the constant temperature of 30 ℃ to obtain a final product.
Description
Technical Field
The invention relates to the field of preparation of photonic nanocrystal materials, in particular to a method for preparing a gold nanorod material by reducing hydroquinone under the action of a double-surfactant.
Background
In recent years, gold nanorods have attracted much attention because of their application prospects in the fields of biomedicine, sensing, optics, imaging, and the like. Because the length, width, length-diameter ratio and other parameters of the gold nanorods greatly influence the function and role of the materials in the field, a more excellent synthetic method is explored, and the gold nanorod materials with high monodispersity, wide adjustable range and high conversion rate are very meaningful. In 2013, Murray et al proposed a method for synthesizing a dual surfactant, and continued the traditional method in the growth solution, using ascorbic acid. Ascorbic acid as an excellent reducing agent is widely applied to the field of gold nanorod synthesis, but in the traditional synthesis process, the quality of a gold nanorod product is greatly influenced by the ascorbic acid, and slight change of the ascorbic acid can cause excessive impurities generated by the product and influence the monodispersity and the practicability of the product. Therefore, hydroquinone is introduced as a reducing agent in the method, compared with ascorbic acid, the sensitivity of the gold nanorod in the synthesis process to the change is reduced, and the gold nanorod sample with wider adjustable range is successfully synthesized.
Disclosure of Invention
In order to improve the stability of the gold nanorod in the synthesis process, the invention provides a method for preparing a gold nanorod material by reducing hydroquinone under a double-surfactant condition, wherein CTAB and NaOL are used as double-surfactant and combined with hydroquinone to reduce chloroauric acid. Successfully synthesizes the gold nanorod product with higher length-diameter ratio and high monodispersity.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a preparation method for reducing gold nanorods by using hydroquinone is characterized by comprising the following steps:
step S1, a seed solution is prepared.
Step S2, a growth solution is prepared and grown. The C-C double bond in sodium oleate will grow the Au in solution3+Reduction to Au+Hydrochloric acid is added to regulate the hydrolysis rate of the ascorbate, and the reaction rate is controlled. Ag+Aims to adjust the conversion rate and the morphology of the gold nanorods and enable the gold nanocrystals to grow into rods along two ends under the combined action of the gold nanorods and CTAB.
And step S3, cleaning and purifying the growth solution, extracting a gold nanorod sample through centrifugation, and dispersing the gold nanorod sample in a surfactant solution to prevent agglomeration.
Wherein the step S1 includes the steps of:
s10 mixing 10mL of 0.1M CTAB with 0.25mL of 10mM HAuCl4Mixing in a bottle, mixing with ice-water mixture and certain weighed NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution.
Wherein the step S2 further comprises the steps of:
s20 18.5mL of 0.1M CTAB and 0.124g of NaOL were dissolved in 29mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and 1.8mL of 4mM AgNO was added3And (3) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.5mL of 10mM HAuCl was added4. After 60-90 minutes, the solution turned from golden yellow to colorless with stirring at 400 rpm. This is the growth solution.
S21, adding 800 mu L hydroquinone solution 0.1M and seed solution 80 mu L into the growth solution in sequence and stirring vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath.
The step S3 further includes the steps of:
s30: the solution after growth was centrifuged at 7000rpm for 30 minutes (1-2 mM CTAB was added after removal of the supernatant and a second centrifugation at 7000rpm for 30 minutes the solution was concentrated ten times after removal of the supernatant and dispersed in a corresponding volume of 1-2mM CTAB.
The invention adopts a seed-mediated method for preparation, and the whole reaction process is as follows: sodium borohydride in seed solution to Au3+Ions are reduced into Au, and crystal gold seeds with the diameter of 1-2nm grow among Au under the action of a surfactant CTAB. In the growth solution, sodium oleate first Au3+Reduction to Au+After the seed solution is added, Au is acted under the action of hydroquinone+Is reduced into Au, and the Ag and CTAB lead the Au to grow mainly on two sides, thereby forming a rod-shaped gold nano crystal. The method is simple to operate, the gold nanorod sample with a large length-diameter ratio can be obtained more easily, and the stability in the synthesis process is improved under the condition that the same CTAB and NaOL are used as double surfactants and ascorbic acid is used as a reducing agent.
The invention prepares a gold nanorod material generated by hydroquinone reduction under double surfactants, the length of the gold nanorod material is about 80-160nm, and the diameter of the gold nanorod material is about 10-20 nm. The aspect ratio is about 2 to 8.
In the existing synthesis method, a mainstream ascorbic acid synthesis method can generate a plurality of impurities when a gold nanorod sample with a high length-diameter ratio grows, and the purity and the quality of a synthesized product are very sensitive to the concentration and the proportion of ascorbic acid. Compared with the prior art, the gold nanorod and the preparation method thereof combine a CTAB + NaOL double surfactant, and compared with the method that only one CTAB is used as the surfactant, the purity and the conversion rate of the gold nanorod are improved; hydroquinone is used as a reducing agent, so that the high-length-diameter ratio and the high-dispersity are ensured. The gold nanorods prepared by the method combines the advantages, and solves the problems of excessive impurities, poor monodispersity of products and the like in the traditional process of preparing the gold nanorods by using ascorbic acid as a reducing agent. Has the following beneficial effects:
(1) compared with the traditional synthesis method, the method uses hydroquinone as a reducing agent, and solves the problem of sensitivity to ascorbic acid in the synthesis process of the gold nanorods.
(2) CTAB and NaOL are used as double surfactants to be matched with hydroquinone, so that the monodispersity and purity of the product with high length-diameter ratio are greatly improved.
Drawings
FIG. 1 is a flow chart of the steps of the method for preparing gold nano-materials by reducing hydroquinone with low bi-surfactant content according to the present invention;
FIG. 2 is a transmission electron microscope photograph of gold nanorod products of example 1 of the present invention.
Detailed Description
The technical solution provided by the present invention will be further explained with reference to the accompanying drawings.
Referring to fig. 1, the method for preparing the gold nano-material grown under the low surfactant concentration provided by the invention specifically comprises the following steps
Step S1, a seed solution is prepared.
Step S2, a growth solution is prepared and grown. The C-C double bond in sodium oleate will grow the Au in solution3+Reduction to Au+Adding hydroquinone to prepare Au+Reduction to Au, Ag+
Aims to adjust the conversion rate and the morphology of the gold nanorods and enable the gold nanocrystals to grow into rods along two ends under the combined action of the gold nanorods and CTAB.
Step S3, cleaning and purifying the growth solution, extracting a gold nanorod sample through centrifugation,
dispersing in surfactant solution to prevent agglomeration.
Wherein the step S1 includes the steps of:
s10 mixing 10mL of 0.1M CTAB with 0.25mL of 10mM HAuCl4Mixing in a bottle, mixing with ice-water mixture and certain weighed NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution.
Wherein the step S2 further comprises the steps of:
s20 18.5mL of 0.1M CTAB and 0.124g of NaOL were dissolved in 29mL of water at 50 ℃. Dissolving the solutionThe temperature was reduced to 30 ℃ and 1.8mL of 4mM AgNO was added3And (3) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.5mL of 10mM HAuCl was added4. After 60-90 minutes, the solution turned from golden yellow to colorless with stirring at 400 rpm. This is the growth solution.
S21, adding 800 mu L hydroquinone solution 0.1M and seed solution 80 mu L into the growth solution in sequence and stirring vigorously. The final solution was left to stand for 12 hours in a 30 ℃ water bath.
The step S3 further includes the steps of:
s30: the solution after growth was centrifuged at 7000rpm for 30 minutes (1-2 mM CTAB was added after removal of the supernatant and a second centrifugation at 7000rpm for 30 minutes the solution was concentrated ten times after removal of the supernatant and dispersed in a corresponding volume of 1-2mM CTAB.
In the existing synthesis method, a mainstream ascorbic acid synthesis method can generate a plurality of impurities when a gold nanorod sample with a high length-diameter ratio grows, and the purity and the quality of a synthesized product are very sensitive to the concentration and the proportion of ascorbic acid. The method has the advantages over other methods that: the double surfactants CTAB and NaOL are combined, and compared with the method that only one CTAB is used as the surfactant, the purity and the conversion rate of the gold nanorod are improved; hydroquinone is used as a reducing agent, so that the high-length-diameter ratio and the high-dispersity are ensured. The gold nanorods prepared by the method have the advantages. The obtained result is shown in fig. 2, which is a transmission electron microscope picture of the gold nanorod material finally prepared by the invention. The length of the gold nanorod shown in the figure is 153nm, the diameter is 19nm, and the length-diameter ratio is 8.0. And the thickness is uniform, the ratio of more than 99 percent is rod-shaped, the purity is higher, and the impurities are less. The surface plasmon resonance effect is stronger in a near infrared region.
Example 1:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 18.5mL CTAB (0.1M) was dissolved with 0.124g NaOL at 50 deg.CDissolve in 29mL of water. After dissolution, the solution was cooled to 30 ℃ and 1.8mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.5mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 800. mu.L of hydroquinone solution (0.1M) and 80. mu.L of seed solution in that order with vigorous stirring (1200 rpm). The final solution was left to stand for 12 hours in a 30 ℃ water bath.
Example 2:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 18.5mL CTAB (0.1M) and 0.124g NaOL were dissolved in 29mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and 1.8mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.5mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 1000. mu.L of hydroquinone solution (0.1M) and 80. mu.L of seed solution in that order with vigorous stirring (1200 rpm). The final solution was left to stand for 12 hours in a 30 ℃ water bath.
Example 3:
10mL CTAB (0.1M) and 0.25mL HAuCl4(10mM) are mixed in a bottle with an ice-water mixture and a weighed quantity of NaBH4Mix to make 0.01M solution, and add 0.6mL into the bottle and stir vigorously. The solution changed from golden yellow to brown yellow, which is a seed solution. 18.5mL CTAB (0.1M) and 0.124g NaOL were dissolved in 29mL of water at 50 ℃. After dissolution, the solution was cooled to 30 ℃ and 1.8mL of AgNO was added3(4mM) solution. And left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.5mL of HAuCl was added4(10 mM). After stirring (400rpm) for 60-90 minutes, the solution turned from golden yellow to colorless. This is the growth solution. To the growth solution was added 600. mu.L of hydroquinone solution (0.1M), 80. mu.L of seed solution in that order and vigorously stirred (1200 rpm). The final solution was allowed to stand for 12 hoursIn a water bath at 30 ℃.
Finally, it should be noted that the above embodiments are only used to help understand the method of the present invention and its core idea, and not to limit it. Those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present invention's device solution. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. A method for preparing a gold nanorod material by hydroquinone reduction under the action of a double-surfactant is characterized by comprising the following steps:
step S1, preparing a seed solution;
step S2, preparing a growth solution and growing; the C-C double bond in sodium oleate will grow the Au in solution3+Reduction to Au+Adding hydrochloric acid to regulate the hydrolysis rate of the ascorbate, and controlling the reaction rate; ag+Aiming at adjusting the conversion rate and the morphology of the gold nanorods and enabling the gold nanocrystals to grow into rods along two ends under the combined action of the gold nanorods and CTAB;
step S3, cleaning and purifying the growth solution, extracting a gold nanorod sample through centrifugation, and dispersing the gold nanorod sample in a surfactant solution to prevent agglomeration;
wherein the step S1 includes the steps of:
s10 mixing 10mL of 0.1M CTAB with 0.25mL of 10mM HAuCl4Mixing in a bottle, mixing with ice-water mixture and certain weighed NaBH4Mixing to prepare 0.01M solution, and adding 0.6mL of the solution into a bottle for vigorous stirring; the solution turns from golden yellow to brown yellow, which is a seed solution;
wherein the step S2 further comprises the steps of:
s20 dissolving 18.5mL of 0.1M CTAB and 0.124g of NaOL in 29mL of water at 50 ℃; after dissolution, the solution was cooled to 30 ℃ and 1.8mL of the solution was added 4mM AgNO3A solution; and left to stand at a constant temperature of 30 ℃ for 15 minutes, after which 0.5mL of 10mM HAuCl was added4(ii) a After stirring at 400rpm for 60-90 minutes, the solution turns from golden yellow to colorless; this is the growth solution;
s21, adding 800 mu L hydroquinone solution of 0.1M and seed solution of 80 mu L into the growth solution in sequence and stirring vigorously; standing the final solution for 12 hours in a water bath at 30 ℃;
the step S3 further includes the steps of:
s30: the solution after growth was centrifuged at 7000rpm for 30 minutes (1-2 mM CTAB was added after removing the supernatant, followed by a second centrifugation at 7000rpm for 30 minutes; ten times concentrated after removing the supernatant, and dispersed in a corresponding volume of 1-2mM CTAB.
2. The method for preparing gold nanorod material by hydroquinone reduction under dual surfactants as claimed in claim 1, wherein 0.037M CTAB and 0.008M NaOL are used as dual surfactants.
3. The method for preparing gold nanorod material through hydroquinone reduction under double surfactants according to claim 1, wherein the steps S1 and S2 adopt a seed-mediated method.
4. The method for preparing gold nanorod material by hydroquinone reduction under double surfactants as claimed in claim 1, wherein 1-2nm gold nanoparticles are first prepared as seeds using sodium borohydride, a strong reducing agent; au of chloroauric acid in growth solution3+Reduced to Au by sodium oleate+Then reduced to Au by hydroquinone, via CTAB and Ag+The combined action of the two components is oriented to grow at the two ends of the seed particles, and finally the gold nanorods are grown.
5. The method for preparing gold nanorod material by hydroquinone reduction under dual surfactants according to claim 1, wherein the prepared gold nanorods have a length of about 80-160nm and a diameter of about 10-20 nm. The aspect ratio is about 2 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011603115.1A CN112974829A (en) | 2020-12-29 | 2020-12-29 | Method for preparing gold nanorod material by reducing hydroquinone under double surfactants |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011603115.1A CN112974829A (en) | 2020-12-29 | 2020-12-29 | Method for preparing gold nanorod material by reducing hydroquinone under double surfactants |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112974829A true CN112974829A (en) | 2021-06-18 |
Family
ID=76345209
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011603115.1A Pending CN112974829A (en) | 2020-12-29 | 2020-12-29 | Method for preparing gold nanorod material by reducing hydroquinone under double surfactants |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112974829A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114042930A (en) * | 2021-11-19 | 2022-02-15 | 杭州电子科技大学 | Method for large-scale synthesis of gold nanorods |
| CN114082936A (en) * | 2021-11-19 | 2022-02-25 | 杭州电子科技大学 | Synthesis method of gold nanorods with good monodispersity |
| CN114082977A (en) * | 2021-11-19 | 2022-02-25 | 杭州电子科技大学 | Method for synthesizing gold nanorods by using catechol as reducing agent |
| CN115351289A (en) * | 2022-09-01 | 2022-11-18 | 杭州师范大学 | Method for preparing micro gold nanorods by using ternary surfactant and product thereof |
| CN116809947A (en) * | 2023-06-30 | 2023-09-29 | 广东药科大学 | Method for preparing Au nano-rod by imidazole and/or cyclic quaternary ammonium salt surfactant |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060196309A1 (en) * | 2003-05-13 | 2006-09-07 | Yasuro Niidome | Method for manufacturing metal nanorods and use thereof |
| CN103567458A (en) * | 2013-10-29 | 2014-02-12 | 张立明 | Preparation method of synthesizing nano gold rod taking phenol substance as reducing agent by aspermous method |
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN104707998A (en) * | 2015-03-13 | 2015-06-17 | 盐城工学院 | Nanometer golden rod used for detecting bovine serum albumin and preparation method and application thereof |
| CN104907578A (en) * | 2015-04-29 | 2015-09-16 | 福州大学 | Method for preparing gold nanorods |
| CN106363192A (en) * | 2016-11-11 | 2017-02-01 | 南京东纳生物科技有限公司 | Continuous feeding parallel reaction device for preparation of gold nanorods and application thereof |
| 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 |
| CN108356277A (en) * | 2018-02-24 | 2018-08-03 | 浙江大学 | A kind of preparation method of gold nanorods |
| 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 |
| CN111659903A (en) * | 2020-07-14 | 2020-09-15 | 国家纳米科学中心 | Gold nanorod and preparation method thereof |
-
2020
- 2020-12-29 CN CN202011603115.1A patent/CN112974829A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060196309A1 (en) * | 2003-05-13 | 2006-09-07 | Yasuro Niidome | Method for manufacturing metal nanorods and use thereof |
| CN103567458A (en) * | 2013-10-29 | 2014-02-12 | 张立明 | Preparation method of synthesizing nano gold rod taking phenol substance as reducing agent by aspermous method |
| CN104209533A (en) * | 2014-07-21 | 2014-12-17 | 苏州大学 | Method for rapidly preparing gold nanorod |
| CN104707998A (en) * | 2015-03-13 | 2015-06-17 | 盐城工学院 | Nanometer golden rod used for detecting bovine serum albumin and preparation method and application thereof |
| CN104907578A (en) * | 2015-04-29 | 2015-09-16 | 福州大学 | Method for preparing gold nanorods |
| CN106363192A (en) * | 2016-11-11 | 2017-02-01 | 南京东纳生物科技有限公司 | Continuous feeding parallel reaction device for preparation of gold nanorods and application thereof |
| 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 |
| CN108356277A (en) * | 2018-02-24 | 2018-08-03 | 浙江大学 | A kind of preparation method of gold nanorods |
| 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 |
| CN111659903A (en) * | 2020-07-14 | 2020-09-15 | 国家纳米科学中心 | Gold nanorod and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114042930A (en) * | 2021-11-19 | 2022-02-15 | 杭州电子科技大学 | Method for large-scale synthesis of gold nanorods |
| CN114082936A (en) * | 2021-11-19 | 2022-02-25 | 杭州电子科技大学 | Synthesis method of gold nanorods with good monodispersity |
| CN114082977A (en) * | 2021-11-19 | 2022-02-25 | 杭州电子科技大学 | Method for synthesizing gold nanorods by using catechol as reducing agent |
| CN115351289A (en) * | 2022-09-01 | 2022-11-18 | 杭州师范大学 | Method for preparing micro gold nanorods by using ternary surfactant and product thereof |
| CN115351289B (en) * | 2022-09-01 | 2023-12-29 | 杭州师范大学 | Method for preparing miniature gold nanorods by using ternary surfactant and product thereof |
| CN116809947A (en) * | 2023-06-30 | 2023-09-29 | 广东药科大学 | Method for preparing Au nano-rod by imidazole and/or cyclic quaternary ammonium salt surfactant |
| CN116809947B (en) * | 2023-06-30 | 2024-02-02 | 广东药科大学 | Method for preparing Au nano-rod by imidazole and/or cyclic quaternary ammonium salt surfactant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112974829A (en) | Method for preparing gold nanorod material by reducing hydroquinone under double surfactants | |
| CN108723385B (en) | Single crystal silver nanosphere water phase preparation method | |
| US20120046482A1 (en) | Method for synthesizing gold nanoparticles | |
| US20070125196A1 (en) | Controlled synthesis of highly monodispersed gold nanoparticles | |
| CN104308175B (en) | A kind of spherical gold grain and its step by step fast synthesis method | |
| CN112809016B (en) | Preparation method of thickness-adjustable silicon dioxide material grown on surface of gold nanorod | |
| CN112828283B (en) | High-purity gold nanoparticles, selectively-coated gold nanoparticles and preparation method thereof | |
| CN112828284B (en) | Preparation method of mesoporous silica-coated gold nanorod surface-grown silver composite material | |
| CN112605392A (en) | Method for preparing silver nanowires | |
| CN108436098B (en) | Preparation method of silver nanoring | |
| CN112756622B (en) | Preparation method of gold nanorod material under low surfactant concentration | |
| CN112775435A (en) | Preparation method of gold nanorod surface-grown mesoporous silica material | |
| CN112743099A (en) | Preparation method of gold nanorod material with length-diameter ratio regulated and controlled by hydrochloric acid | |
| CN112846219A (en) | Preparation method of gold nanorod-palladium composite material | |
| CN112496337A (en) | Hydrothermal synthesis method of silver nanowires with high length-diameter ratio | |
| CN112846217A (en) | Preparation method of nano gold-platinum composite material in mesoporous silica | |
| CN112846218A (en) | Preparation method of gold-platinum-silver material with asymmetric structure | |
| CN113231632B (en) | Gold-palladium asymmetric heterogeneous nano structure and synthesis method thereof | |
| CN112809018B (en) | Synthesis method of gold-platinum bimetallic structural material | |
| CN112756623A (en) | Synthesis method of gold-platinum material with special structure | |
| CN113695584B (en) | Method for rapidly synthesizing high-purity gold nano triangular plate | |
| CN115283686B (en) | Room temperature seed mediated growth method for uniformly and stably multi-branch gold nanoparticles | |
| Do Thi et al. | Seeded Growth Synthesis of Uniform Gold Nanoparticles with Controlled Diameters up to 220 nm | |
| CN114082977A (en) | Method for synthesizing gold nanorods by using catechol as reducing agent | |
| CN112191860B (en) | Chemical synthesis method for continuously adjusting surface roughness of gold nanoparticles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |