CN107020391A - A kind of method of utilization mercaptan controlledly synthesis nano gold sol - Google Patents
A kind of method of utilization mercaptan controlledly synthesis nano gold sol Download PDFInfo
- Publication number
- CN107020391A CN107020391A CN201710327251.4A CN201710327251A CN107020391A CN 107020391 A CN107020391 A CN 107020391A CN 201710327251 A CN201710327251 A CN 201710327251A CN 107020391 A CN107020391 A CN 107020391A
- Authority
- CN
- China
- Prior art keywords
- mercaptan
- ammonium bromide
- gold
- nano
- gold seeds
- 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
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
- B22F1/0545—Dispersions or suspensions of nanosized particles
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- 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)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of method of utilization mercaptan controlledly synthesis nano gold sol.Present invention mercaptan first in the gold seeds surface-assembled that protective agent is covered; then the heating process of seed growth is carried out using reducing agent; change the concentration of mercaptan; realize the different extent of growth of gold seeds; in general; synthesizing mercaptan consumption in sub-processes seldom, needs mercaptan to play main function in seed growth process, therefore used in amounts increases severely.The method of the present invention can accurately control the size of nano Au particle, obtain preferable monodispersity, and the size and pattern of nanogold are obtained by ESEM means, the final concentration in mercaptan is associated with being set up between both nanogold particle diameters, and it has important directive significance to the selection of nanoparticle surface controlling agent in field of nanometer technology and the controllable preparation of nano-particle.
Description
Technical field
The invention belongs to field of material synthesis technology, specifically, it is related to a kind of molten using mercaptan controlledly synthesis nanogold
The method of glue.
Background technology
Many researchs show that the exploitation of nanoparticle surface performance and its particle diameter monodispersity are closely related, this correlation
Property is for exploring their chemistry, bioanalysis, biomedicine, optics and in electronics, optics and chemical/biological property side
The nanometer technology in face is critically important.The synthetic method for preparing gold nano grain using crystal seed in aqueous has repeatedly been reported.
For example, in the presence of citrate is as end-capping reagent, the Jin Jing's kind prepared by gold salt reducing process.And in seed growth,
The basic understandings of growth mechanism be at room temperature by citrate or azanol as reducing agent less nano particle table
Au (III) is reduced on face.Such growth mechanism is already used to consider to synthesize Au nanometers in the presence of trace silver ion
Rod (20-100nm).
Although how the method for existing a variety of synthesis gold nano grains, realize size, shape in the range of certain size
The control of shape and monodispersity detailed mechanism still lack understanding.Also increasing in the report of organic synthesis nano-particle,
Trace it to its cause is that organic phase can play the purpose for suppressing nano-particle undue growth in nanoparticle surface formation protective layer.But
Be different types of organic phase concentration to the accurate control of Nanoparticle Size and the monodispersity of size in terms of
Influence need to be groped.
The content of the invention
For problem above, the purpose of present invention profit is to provide a kind of side of utilization mercaptan controlledly synthesis nano gold sol
Method, it is possible to achieve the controlledly synthesis of less than 20 nanometers of gold particle.
To achieve these goals, the technical solution adopted by the present invention is as follows.
The present invention provides a kind of method of utilization mercaptan controlledly synthesis nano gold sol, comprises the following steps that：
(1) gold seeds is prepared
Ammonium bromide and tetraoctyl ammonium bromide forms organic phase in toluene first, then adds golden forerunner's agent tetra chlorauric acid, adds alkane
Base mercaptan, is eventually adding reducing agent, and stirring obtains displacing ammonium bromide and tetraoctyl ammonium bromide is assembled in particle surface using alkyl hydrosulfide
Gold seeds/toluene solution of the particle diameter at 1~3 nanometer；
(2) the various sizes of nano gold sol of controlledly synthesis
In above-mentioned gold seeds/toluene solution, above-mentioned alkyl hydrosulfide of the same race, and tetra chlorauric acid solution are added, 147 ±
50~60min is reacted at a temperature of 2 DEG C, 6~20 nanometers of aurosol is obtained.
In the present invention, in step (1), ammonium bromide and tetraoctyl ammonium bromide, tetra chlorauric acid, the mass ratio of alkyl hydrosulfide and reducing agent are
(200~300)：(150~200)：1：(20~30).
In the present invention, in step (1), reducing agent is sodium borohydride.
In the present invention, the mass ratio of step (1) and the alkyl hydrosulfide in step (2) is 1:780~1：3725；Step (1)
Mass ratio with tetra chlorauric acid in step (2) is 14：1~18：1.
In the present invention, alkyl hydrosulfide is selected from CH3(CH2)7SH、CH3(CH2)8SH、CH3(CH2)9SH、CH3(CH2)10SH or
CH3(CH2)11SH medium chain lengths 1~2 nanometer length scope molecule any one.
In the present invention, alkyl hydrosulfide is CH3(CH2)9SH。
Compared to the prior art, the beneficial effects of the present invention are：Technical solution of the present invention is simple, nanogold can be achieved molten
The controlledly synthesis of glue, it has to the selection of nanoparticle surface controlling agent in field of nanometer technology and the controllable preparation of nano-particle
There is important directive significance.
Brief description of the drawings
Fig. 1 is based on 2.5 nanometers of gold seedses, by changing the mercaptan of various concentrations, to obtain various sizes of big grain
Particle diameter and the dependency graph of mercaptan that the period of the day from 11 p.m. to 1 a.m is obtained.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.
Various raw materials used, are commercially available unless otherwise specified in various embodiments of the present invention.
Embodiment 1
Preparation and the sign of 15 nano Au particles are synthesized using mercaptan heating：
The preparation of (1) 2.5 nanometer of gold seeds：
3.0 grams first of ammonium bromide and tetraoctyl ammonium bromide forms organic phase in 160 milliliters of toluene, then adds .1.92 grams
50 milliliters of reactant tetra chlorauric acid, adds 11mg decyl mercaptan, is eventually adding 0.38 gram of sodium borohydride of 25 milliliters of reducing agent
Solution, is stirred 12 hours, is obtained mercaptan and is displaced ammonium bromide and tetraoctyl ammonium bromide and then be assembled in the gold seeds of particle surface (2.5 receive
Rice), it is dispersed in toluene solution；
(2) the mercaptan control gold seeds of various concentrations is grown up
In above-mentioned 235 milliliters of gold seeds/toluene solution, decyl mercaptan 8.60g (0.21 mol/L in system) is added,
I.e. 10 milliliters pure decyl mercaptans, and reactant tetra chlorauric acid solution 112mg (0.0014 mol/L in system), lead at 147 DEG C
Cross reflux condensation mode reaction and maintain a hour.The nano gold sol for determining to obtain~15 nanometers is characterized using ESEM.
Embodiment 2
Preparation and the sign of 9 nano Au particles are synthesized using mercaptan heating：
The preparation of (1) 2.5 nanometer of gold seeds：The present invention is to investigate the mercaptan changing factor in gold seeds growth process
Influence to particle diameter, therefore change is reduced because of amount, do not change the synthesis step of gold seeds, namely method be the same as Example 1.Use reagent
Species and concentration keep constant.
(2) the mercaptan control gold seeds of various concentrations is grown up
It is in order to investigate influence of the mercaptan changing factor to particle diameter in gold seeds growth process, therefore in view of the present invention
Reduce and become because of amount, do not change the species of mercaptan, namely：In above-mentioned 235 milliliters of gold seeds/toluene solution, 13.32g is added
The decyl mercaptan of (0.325 mol/L in system), i.e., 15.8 milliliters pure decyl mercaptans, and reactant tetra chlorauric acid 120mg solution
(concentration is 0.0015 mol/L in system), a hour is maintained at 148 DEG C by reflux condensation mode reaction.Utilize scanning electricity
Mirror characterizes the nano gold sol for determining to obtain~9 nanometers.
Embodiment 3
Preparation and the sign of 6 nano Au particles are synthesized using mercaptan heating：
The preparation of (1) 2.5 nanometer of gold seeds：The present invention is to investigate the mercaptan changing factor in gold seeds growth process
Influence to particle diameter, therefore change is reduced because of amount, do not change the synthesis step of gold seeds, namely method be the same as Example 1.Use reagent
Species and concentration keep constant.
(2) the mercaptan control gold seeds of various concentrations is grown up
It is in order to investigate influence of the mercaptan changing factor to particle diameter in gold seeds growth process, therefore in view of the present invention
Reduce and become because of amount, do not change the species of mercaptan, namely：In above-mentioned 235 milliliters of gold seeds/toluene solution, 40.97g is added
Decyl mercaptan (1.0 mol/L in system), i.e. 48.7 milliliters of pure decyl mercaptans, and reactant tetra chlorauric acid 128mg solution (body
Concentration is 0.0016 mol/L in system), a hour is maintained by reflux condensation mode reaction at 147 DEG C.Utilize ESEM table
Levy the nano gold sol for determining to obtain~6 nanometers.
It is above-mentioned based on 2.5 nanometers of gold seedses, by changing the mercaptan of various concentrations, obtain various sizes of big grain
Son, does dependency graph by particle diameter and mercaptan, sees Fig. 1.
Claims (6)
1. a kind of method of utilization mercaptan controlledly synthesis nano gold sol, it is characterised in that comprise the following steps that：
(1) gold seeds is prepared
Ammonium bromide and tetraoctyl ammonium bromide forms organic phase in toluene first, then adds golden forerunner's agent tetra chlorauric acid, adds alkyl sulfide
Alcohol, is eventually adding reducing agent, and stirring obtains displacing the particle diameter that ammonium bromide and tetraoctyl ammonium bromide is assembled in particle surface using alkyl hydrosulfide
In 1~3 nanometer of gold seeds/toluene solution；
(2) the various sizes of nano gold sol of controlledly synthesis
In above-mentioned gold seeds/toluene solution, above-mentioned alkyl hydrosulfide of the same race, and tetra chlorauric acid solution are added, at 147 ± 2 DEG C
At a temperature of react 50~60min, obtain 6~20 nanometers of aurosol.
2. according to the method described in claim 1, it is characterised in that in step (1), ammonium bromide and tetraoctyl ammonium bromide, tetra chlorauric acid, alkyl
The mass ratio of mercaptan and reducing agent is (200~300)：(150~200)：1：(20~30).
3. according to the method described in claim 1, it is characterised in that in step (1), reducing agent is sodium borohydride.
4. according to the method described in claim 1, it is characterised in that the mass ratio of step (1) and the alkyl hydrosulfide in step (2)
For 1:780~1：3725；The mass ratio of tetra chlorauric acid is 14 in step (1) and step (2)：1~18：1.
5. according to the method described in claim 1, it is characterised in that alkyl hydrosulfide is selected from CH3(CH2)7SH、CH3(CH2)8SH、
CH3(CH2)9SH、CH3(CH2)10SH or CH3(CH2)11SH medium chain lengths 1~2 nanometer length scope molecule it is any one
Kind.
6. method according to claim 1 or 5, it is characterised in that alkyl hydrosulfide is CH3(CH2)9SH。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710327251.4A CN107020391A (en) | 2017-05-10 | 2017-05-10 | A kind of method of utilization mercaptan controlledly synthesis nano gold sol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710327251.4A CN107020391A (en) | 2017-05-10 | 2017-05-10 | A kind of method of utilization mercaptan controlledly synthesis nano gold sol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107020391A true CN107020391A (en) | 2017-08-08 |
Family
ID=59529699
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710327251.4A Pending CN107020391A (en) | 2017-05-10 | 2017-05-10 | A kind of method of utilization mercaptan controlledly synthesis nano gold sol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107020391A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109434133A (en) * | 2018-12-20 | 2019-03-08 | 江苏经贸职业技术学院 | A kind of synthetic method based on phase transfer method Au nano material |
| CN110898831A (en) * | 2019-11-27 | 2020-03-24 | 中国科学院青岛生物能源与过程研究所 | Nano-gold micelle catalyst, and preparation method and application thereof |
| CN111250726A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Synthesis of heterogeneous AuAg alloy nanocluster with controllable number of atoms and size |
| CN112008093A (en) * | 2020-09-01 | 2020-12-01 | 吉林大学 | Quantum dot-gold nanoparticle heterogeneous superlattice and preparation method and application thereof |
| CN112191860A (en) * | 2020-09-29 | 2021-01-08 | 浙江工业大学 | Chemical synthesis method for continuously adjusting surface roughness of gold nanoparticles |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101268946A (en) * | 2008-04-30 | 2008-09-24 | 东北师范大学 | Method for latency fingerprint appearance of surface functionalization nano-gold particle |
| CN101458242A (en) * | 2007-12-11 | 2009-06-17 | 郑州轻工业学院 | Nanogold Colloid for responding heavy metal ion and method for making same |
| CN102500287A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Graphene/modified titanium dioxide nano sol composite material and preparation method thereof |
| CN106270549A (en) * | 2016-09-23 | 2017-01-04 | 上海应用技术大学 | A kind of method utilizing surface dopant to control golden nanometer particle growth |
-
2017
- 2017-05-10 CN CN201710327251.4A patent/CN107020391A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101458242A (en) * | 2007-12-11 | 2009-06-17 | 郑州轻工业学院 | Nanogold Colloid for responding heavy metal ion and method for making same |
| CN101268946A (en) * | 2008-04-30 | 2008-09-24 | 东北师范大学 | Method for latency fingerprint appearance of surface functionalization nano-gold particle |
| CN102500287A (en) * | 2011-09-28 | 2012-06-20 | 重庆大学 | Graphene/modified titanium dioxide nano sol composite material and preparation method thereof |
| CN106270549A (en) * | 2016-09-23 | 2017-01-04 | 上海应用技术大学 | A kind of method utilizing surface dopant to control golden nanometer particle growth |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111250726A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Synthesis of heterogeneous AuAg alloy nanocluster with controllable number of atoms and size |
| CN109434133A (en) * | 2018-12-20 | 2019-03-08 | 江苏经贸职业技术学院 | A kind of synthetic method based on phase transfer method Au nano material |
| CN110898831A (en) * | 2019-11-27 | 2020-03-24 | 中国科学院青岛生物能源与过程研究所 | Nano-gold micelle catalyst, and preparation method and application thereof |
| CN112008093A (en) * | 2020-09-01 | 2020-12-01 | 吉林大学 | Quantum dot-gold nanoparticle heterogeneous superlattice and preparation method and application thereof |
| CN112191860A (en) * | 2020-09-29 | 2021-01-08 | 浙江工业大学 | Chemical synthesis method for continuously adjusting surface roughness of gold nanoparticles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107020391A (en) | A kind of method of utilization mercaptan controlledly synthesis nano gold sol | |
| Gu et al. | Ultrasmall near-infrared Ag2Se quantum dots with tunable fluorescence for in vivo imaging | |
| KR100738003B1 (en) | Dendrimer-Modified Nanoparticles | |
| Tian et al. | Synthesis of N-(aminobutyl)-N-(ethylisoluminol) functionalized gold nanomaterials for chemiluminescent bio-probe | |
| CN103582690B (en) | A kind of method of preparing core-shell nano and solution thereof | |
| EP2716733B1 (en) | Preparation method for near-infrared silver sulfide quantum dots | |
| CN100572500C (en) | The aqueous phase preparation method of cyclodextrin modified CdTe quantum dot | |
| CN108659817B (en) | Synthesis method of core-shell quantum dot and core-shell quantum dot | |
| EP1514838A1 (en) | Process for producing nanoparticle and nanoparticle produced by the process | |
| CN107470648B (en) | DNA functionalized gold nanocluster and preparation method thereof | |
| CN101905328B (en) | Method for preparing water-soluble Au10 nano-cluster molecules | |
| Liu et al. | Synthesis of highly stable CdTe/CdS quantum dots with biocompatibility | |
| Yin et al. | Au x Ag1–x nanocomposites with 40-fold emission enhancement formed by the electrostatic assembly of gold nanoclusters and silver nanoclusters for bioimaging and bioanalysis | |
| US20210138549A1 (en) | Method for preparing silver nano-rings | |
| Muñoz et al. | Ternary quantum dots in chemical analysis. Synthesis and detection mechanisms | |
| CN101787285A (en) | Method for preparing water-soluble fluorescent ZnSe/ZnS core-shell quantum dots | |
| CN106001606A (en) | Preparing method capable of adjusting particle size of gold nanoparticles based on sodium citrate reduction method | |
| CN108059955A (en) | Quantum dot and preparation method thereof | |
| JPWO2006059664A1 (en) | Stabilized inorganic nanoparticles, stabilized inorganic nanoparticles, method for producing stabilized inorganic nanoparticles, and method for using stabilized inorganic nanoparticles | |
| Rambukwella et al. | Synthesis of Au38 (SCH2CH2Ph) 24, Au36 (SPh-t Bu) 24, and Au30 (S-t Bu) 18 Nanomolecules from a Common Precursor Mixture | |
| Huo et al. | Aggregation induced emission of amino-thiol capped gold nanoparticles (GNPs) through metal-amino-coordination | |
| CN107225236A (en) | A kind of preparation method of gold nanorods/zinc oxide core-shell nano composite construction | |
| CN103878382B (en) | A kind of preparation method of the special appearance gold nano-crystal detecting tripolycyanamide for surface enhanced raman spectroscopy | |
| CN104722773A (en) | Preparation method of thorn-shaped gold nanoparticles and thrust-shaped gold nanoparticles prepared through method | |
| Knoppe et al. | HPLC of monolayer-protected gold clusters with baseline separation |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170808 |