CN106825605B - A method of gold nanoclusters are prepared based on micro-fluidic chip - Google Patents

A method of gold nanoclusters are prepared based on micro-fluidic chip Download PDF

Info

Publication number
CN106825605B
CN106825605B CN201710036454.8A CN201710036454A CN106825605B CN 106825605 B CN106825605 B CN 106825605B CN 201710036454 A CN201710036454 A CN 201710036454A CN 106825605 B CN106825605 B CN 106825605B
Authority
CN
China
Prior art keywords
solution
micro
gold
fluidic chip
storage tank
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.)
Active
Application number
CN201710036454.8A
Other languages
Chinese (zh)
Other versions
CN106825605A (en
Inventor
牛利
许佳楠
贾菲
李风华
张齐贤
安清波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changchun Institute of Applied Chemistry of CAS
Original Assignee
Changchun Institute of Applied Chemistry of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Changchun Institute of Applied Chemistry of CAS filed Critical Changchun Institute of Applied Chemistry of CAS
Priority to CN201710036454.8A priority Critical patent/CN106825605B/en
Publication of CN106825605A publication Critical patent/CN106825605A/en
Application granted granted Critical
Publication of CN106825605B publication Critical patent/CN106825605B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • 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
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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

Abstract

The present invention provides a kind of method preparing gold nanoclusters based on micro-fluidic chip, belongs to gold nanoclusters synthetic method field.This method is to synthesize the small gold nanoclusters protected by alkyl carbon chain alkanethiol monolayer of single dispersing particle diameter based on micro-fluidic chip, and by doing hydrophobic modification to chip channel inner wall, drop formation is stable, smooth, and droplet coalescence is accurate, and droplet size is uniform；The method droplet size of the present invention is small simultaneously, and chaotic mixing mass transfer velocity is fast, and reactant is evenly distributed in channel, is conducive to nanoparticle nucleated, growth；The micro-fluidic chip of the present invention uses transparent PDMS material, can integrate the formation of microscope on-line real time monitoring materials and be regulated and controled, and chip design is simple, is easy to the multigroup parallel reaction channel of framework, carries out high-throughput synthesis, improves product yield.

Description

A method of gold nanoclusters are prepared based on micro-fluidic chip
Technical field
The invention belongs to gold nanoclusters synthetic method fields, and in particular to one kind preparing gold nanoclusters based on micro-fluidic chip Method.
Background technology
The gold nanoclusters of single ply protective have unique dimensional effect and outstanding physical chemistry and electronic property, from group All cause the concern of people in the various fields such as dress, biological identification, catalysis, electron transfer theory, DNA immunization analysis.Akola etc. People obtains Au by theoretical calculation25(SR)18The structure of cluster, Heaven et al. confirm its knot by Single Crystal X-ray crystallography Structure, Au25(SR)18Cluster becomes one of the Main way of scientists study gold cluster, and research purpose is that development is a kind of easy to operate The short method of synthesis cycle obtains having uniform pattern, particle diameter distribution narrow and the material of monodispersity, wherein how to utilize The methods of thermodynamics and kinetics ensures that the pattern of material is uniform and size is controllably core and the pass of gold nanoclusters material preparation Key.
The preparation method of the gold nanoclusters of ripe alkanethiol monolayer protection at this stage is usually the side Brust-Schiffrin Method.Brust-Schiffrin methods need to react to synthesize Au with very low mixing speed at 0 DEG C25Nanocluster material, reaction Condition is harsh, and later stage separation process is complicated, and synthesis cycle grows (3 days), and low yield (30%-40%), this has seriously blocked golden cluster The breakthrough and application of synthetic method.Therefore, structure new material synthetic method overcomes conventional method defect to have become urgently It needs.
Invention content
The purpose of the present invention is to provide a kind of method preparing gold nanoclusters based on micro-fluidic chip, the gold nanoclusters Particle shape looks are uniform, better crystallinity degree and grain size are small.
The present invention provides a kind of method preparing gold nanoclusters based on micro-fluidic chip, and this method includes：
Into the liquid storage tank A of micro-fluidic chip, liquid storage tank B and liquid storage tank C, aggressiveness is molten before Continuous Perfusion dispersed phase gold respectively Liquid, alkyl carbon chain thiol solution and monodisperse restore liquid solution, and continuous phase fluid flow velocity is 300nl/min in control liquid storage tank A The flow velocity of alkyl carbon chain mercaptan is 300nl/min in~800nl/min, liquid storage tank B, and monodisperse restores liquid solution in liquid storage tank C Flow velocity be 150nl/min~300nl/min, obtain gold nanoclusters；
The micro-fluidic chip is that the Y-Shaped channel of level-one is disposed on the chip using transparent PDMS as base material The Y-Shaped channel unit of unit, integrated unit, two level and mixed cell, the Y-Shaped channel unit of level-one include liquid storage tank A and liquid storage tank B, the Y-Shaped channel unit of two level include liquid storage tank C, and the port setting of the Y-Shaped channel unit of level-one and the Y-Shaped channel unit of two level is anti- Object fluid interface is answered, for injecting oligomer solution before dispersed phase gold, alkyl carbon chain thiol solution and monodisperse restore liquid solution；It is mixed Collection of products interface is arranged in the port for closing unit, for collecting product.
Preferably, the molar ratio of gold and alkyl carbon chain mercaptan is 1 in aggressiveness before the gold:5.
Preferably, the monodisperse restores the volume of oligomer solution and alkyl carbon chain thiol solution before liquid solution, gold Than being 5:0.07:1.
Preferably, oligomer solution includes gold chloride and the mixed solution of ammonium bromide and tetraoctyl ammonium bromide before the gold.
Preferably, the molar ratio of the gold chloride and ammonium bromide and tetraoctyl ammonium bromide is 1：(1.2-1.3).
Preferably, before the gold in oligomer solution gold chloride a concentration of 0.01~0.4mmol/L, four octyl brominations A concentration of 0.011~0.05mol/L of ammonium.
Preferably, the solvent of oligomer solution is tetrahydrofuran, methanol or acetone before gold used.
Preferably, the alkyl carbon chain mercaptan is n-dodecyl mercaptan solution or n-hexane thiol solution.
Preferably, monodisperse reduction liquid solution is sodium borohydride solution.
Preferably, a concentration of 0.5mol/L of monodisperse reduction liquid solution.
Beneficial effects of the present invention
The present invention provides a kind of method preparing gold nanoclusters based on micro-fluidic chip, and this method is to be based on micro-fluidic chip The small gold nanoclusters protected by alkyl carbon chain alkanethiol monolayer of single dispersing particle diameter are synthesized, by doing hydrophobic repair to chip channel inner wall Decorations, drop formation is stable, smooth, and droplet coalescence is accurate, and droplet size is uniform；The method droplet size of the present invention is small simultaneously, mixes Ignorant mixing mass transfer velocity is fast, and reactant is evenly distributed in channel, is conducive to nanoparticle nucleated, growth；The miniflow of the present invention It controls chip and uses transparent PDMS material, the formation of microscope on-line real time monitoring materials can be integrated and regulated and controled, chip is set Meter is simple, is easy to the multigroup parallel reaction channel of framework, carries out high-throughput synthesis, improves product yield.With traditional Brust- The gold nanoclusters of Schiffrin methods synthesis compare, the gold nanoclusters particle that this method synthesizes uniform, crystallinity with pattern Advantage good, grain size is small, and the preparation method period is short, easy to operate, yield is high.
Description of the drawings
Fig. 1 is the structural schematic diagram of the micro-fluidic PDMS chips of the present invention；
Fig. 2 is the photo figure in kind of the micro-fluidic PDMS chips of the present invention；
Fig. 3 is that the present invention is based on the method droplet coalescence process schematics that micro-fluidic chip prepares gold nanoclusters；
Fig. 4 is the transmission electron microscope picture for the gold nanoclusters that embodiment 2 is prepared；
Fig. 5 is the high-resolution transmission plot for the gold nanoclusters that embodiment 2 is prepared；
Fig. 6 is the afm scan figure that embodiment 3 is prepared.
Specific implementation mode
The present invention provides a kind of method preparing gold nanoclusters based on micro-fluidic chip, and this method includes：
Into the liquid storage tank A of micro-fluidic chip, liquid storage tank B and liquid storage tank C, aggressiveness is molten before Continuous Perfusion dispersed phase gold respectively Liquid, alkyl carbon chain thiol solution and monodisperse restore liquid solution, and continuous phase fluid flow velocity is 300nl/min in control liquid storage tank A The flow velocity of alkyl carbon chain mercaptan is 300nl/min in~800nl/min, liquid storage tank B, and monodisperse restores liquid solution in liquid storage tank C Flow velocity be 150nl/min~300nl/min, obtain gold nanoclusters；
The micro-fluidic chip is using transparent PDMS as base material, and the production method is according to well known to those skilled in the art Prepared by method, be not particularly limited, the present invention is to be combined making with method of molding using soft lithography, such as Fig. 1 and Fig. 2 institutes Show, the Y-Shaped channel unit 1 of level-one, integrated unit 2, the Y-Shaped channel unit 3 of two level and mixing are disposed on the chip Unit 4, the Y-Shaped channel unit 1 of level-one include liquid storage tank A and liquid storage tank B, and the Y-Shaped channel unit of two level includes liquid storage tank C, level-one Reaction-ure fluid interface is arranged in the port of Y-Shaped channel unit and the Y-Shaped channel unit of two level, and reaction-ure fluid interface passes through plastics Pipe is connected with syringe and by syringe pump control flow injecting flow velocity, for injecting oligomer solution before dispersed phase gold, alkyl carbon Chain thiol solution and monodisperse restore liquid solution；Collection of products interface is arranged in the port of mixed cell, for collecting product.
According to the present invention, the course of work of the micro-fluidic chip is：Use syringe pump with 300nl/min~800nl/ Injection dimethyldichlorosilane does hydrophobic modification to its inner wall in the liquid storage tank A of min, then under the perfusion of syringe pump, Xiang Wei Oligomer solution, alkyl carbon chain mercaptan are molten before Continuous Perfusion dispersed phase gold in liquid storage tank A, the liquid storage tank B and liquid storage tank C of fluidic chip Liquid and monodisperse restore liquid solution, and oligomer solution meets with alkyl carbon chain thiol solution in integrated unit before dispersed phase gold, and two Person is mixed into level-one drop under the shear action of continuous fluid, which moves to passages downstream, at the Y-Shaped channel of two level It meets with monodisperse reduction liquid solution, through the secondary mixing of mixed cell, realizes the mixing of reactive material, form drop after mixing and exist The growth ageing stage of reaction is realized in beeline channel, it is small by alkyl carbon chain alkanethiol monolayer that final reaction forms single dispersing particle diameter The gold nanoclusters of protection.
According to the present invention, oligomer solution is organic phase solution before the dispersed phase gold, oligomer solution before the gold Preferably include gold chloride and the mixed solution of ammonium bromide and tetraoctyl ammonium bromide；The concentration of gold chloride is preferably in oligomer solution before the gold The concentration of 0.01~0.4mmol/L, ammonium bromide and tetraoctyl ammonium bromide are preferably 0.011~0.05mol/L.Gold chloride and four in mixed solution The molar ratio of octyl ammonium bromide is preferably 1:(1.2-1.3)；The solvent of oligomer solution is preferably tetrahydrofuran, first before gold used Alcohol or acetone.
According to the present invention, the alkyl carbon chain mercaptan is CnHmAny one in SH (n=3~18), preferably positive 12 Alkyl hydrosulfide or n-hexane mercaptan.
According to the present invention, it is preferably sodium borohydride solution that the monodisperse, which restores liquid solution,.The monodisperse reduction The concentration of liquid solution is preferably 0.5mol/L.
According to the present invention, the molar ratio of gold and alkyl carbon chain mercaptan is preferably 1 in aggressiveness before the gold:5；The life of crystal Growth process is divided into 3 steps：Chemical reaction, nucleation and growth.In the process along with the mutual collision of crystal, mixed splitting or integrating From with reassociate.Alkyl carbon chain mercaptan is as surfactant, when molar ratio is more than 1:When 5, the amount of alkyl carbon chain is inadequate, causes Mutually assemble under crystal, particle is larger.When molar ratio is less than 1:When 5, amount of surfactant is larger, leads to the gold nano generated not It is the nano-cluster that 25 atoms are core.
According to the present invention, the monodisperse restores the body of oligomer solution and alkyl carbon chain thiol solution before liquid solution, gold Product ratio preferably 5:0.07:1.
According to the present invention, during the preparation method of the gold nanoclusters, reaction temperature is preferably room temperature.
Following embodiment will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
The progress of mixing and the reaction of differential responses object, using the chip of structure shown in Fig. 1, material object is shown in Fig. 2.Syringe pump With 600nl/min flow velocitys to liquid storage tank A Continuous Perfusion ethanol solutions, with 300nl/min flow velocitys to liquid storage tank B Continuous Perfusions go from Sub- water, to liquid storage tank C Continuous Perfusion 20mg/ml methyl blue dye solution in 100nl/min~900nl/min flow rates. At the Y-Shaped channel of level-one formed laminar flow fluid-mixing, under the driving of mineral oil along channel flow through at the second season Y-Shaped channel with Methyl blue solution is met, and realizes mixing after collision under the shear stress of fluid.Keep ethyl alcohol and deionized water flow velocity constant, Methyl blue solution flow velocity is increased into 900nl/min from 100nl/min, methyl blue solution can accurately be merged with prime solution, Fluid color after fusion is uniformly and color burn.As shown in Figure 3.As can be seen from Figure 3 dye molecule can promptly with Prime solution mixes, and forms homogeneous phase solution.
Embodiment 2
By gold chloride and ammonium bromide and tetraoctyl ammonium bromide (molar ratio 1:1.2) it is dissolved in tetrahydrofuran that be configured to 0.1mol/l molten Sodium borohydride is dissolved in ice water and is configured to 0.5mol/L solution by liquid, using syringe pump with 500nl/min flow velocitys to liquid storage tank The tetrahydrofuran solution of A Continuous Perfusions gold chloride/ammonium bromide and tetraoctyl ammonium bromide, using syringe pump with 300nl/min flow velocitys to liquid storage tank B Continuous Perfusion n-dodecyl mercaptan solution, with 300nl/min flow velocitys to the sodium borohydride of liquid storage tank C Continuous Perfusions 0.5mol/L Solution, tetrahydrofuran mixed liquor meets with n-dodecyl mercaptan at the Y-Shaped channel of level-one, and golden (III) is reduced in gold chloride Cheng Jin (I), the two are mixed into primary liquor under the shear action of continuous fluid, and the solution is under the impetus of fluid to logical Road downstream movement meets with monodisperse Reduction Body solution C at the Y-Shaped channel of two level, through secondary mixing, realizes reactive material Mixing, forms the growth ageing stage that homogeneous mixed solution realizes reaction in beeline channel after mixing, final reaction forms list The small gold nanoclusters protected by alkyl carbon chain alkanethiol monolayer of dispersion particle diameter.
The gold nanoclusters that embodiment 2 generates are collected, are aged, are washed, dry after carry out Electronic Speculum characterization, transmission electricity The nanotopography of mirror and high-resolution-ration transmission electric-lens difference is as shown in Figure 4 and Figure 5, and Fig. 4 and Fig. 5 show：It is closed with using conventional method At gold nanoclusters transmission electron microscope picture compare the gold nanoclusters grain size as can be seen that the alkanethiol monolayer protection of such method synthesis Small, pattern is uniform.
Embodiment 3
It adopts gold chloride and ammonium bromide and tetraoctyl ammonium bromide (1:1.3) it is dissolved in methanol and is configured to 0.15mol/l solution, by boron hydrogen Change sodium, which is dissolved in ice water, is configured to 0.6mol/L solution.Using syringe pump with 600nl/min flow velocitys to liquid storage tank A Continuous Perfusions The methanol solution of gold chloride/ammonium bromide and tetraoctyl ammonium bromide, using syringe pump with 300nl/min flow velocitys to liquid storage tank B Continuous Perfusions just oneself Alkanethiol solution, with 150nl/min flow velocitys to the sodium borohydride solution of liquid storage tank C Continuous Perfusions 0.6mol/L, in first order Y- Tetrahydrofuran mixed liquor meets with n-hexane mercaptan at type channel, and golden (III) is reduced into golden (I) in gold chloride, and the two is continuous It is mixed into primary liquor under the shear action of fluid, which moves to passages downstream, at the Y-Shaped channel of two level and monodisperse Reduction Body solution C is met, and through secondary mixing, realizes the mixing of reactive material.It is logical in straight line that homogeneous mixed solution is formed after mixing Realize the growth ageing stage of reaction in road, final reaction forms that single dispersing particle diameter is small to be protected by alkyl carbon chain alkanethiol monolayer Gold nanoclusters.
The gold nanoclusters that embodiment 3 generates are collected, are aged, are washed, dry after carry out atomic force microscope characterization, The nanotopography of its atomic force microscope is as shown in Figure 6.Fig. 6 explanations：Electricity is transmitted with the gold nanoclusters using conventional method synthesis Mirror figure compares as can be seen that the gold nanoclusters grain size of the alkanethiol monolayer protection of such method synthesis is small, and pattern is uniform, reaction time Short, yield is high.
Embodiment 4
It adopts gold chloride and ammonium bromide and tetraoctyl ammonium bromide (1:1.2) it is dissolved in methanol and is configured to 0.15mol/l solution, by boron hydrogen Change sodium, which is dissolved in ice water, is configured to 0.6mol/L solution.Using syringe pump with 300nl/min flow velocitys to liquid storage tank A Continuous Perfusions The methanol solution of gold chloride/ammonium bromide and tetraoctyl ammonium bromide, using syringe pump with 300nl/min flow velocitys to liquid storage tank B Continuous Perfusions just oneself Alkanethiol solution, with 150nl/min flow velocitys to the sodium borohydride solution of liquid storage tank C Continuous Perfusions 0.6mol/L, in first order Y- Tetrahydrofuran mixed liquor meets with n-hexane mercaptan at type channel, and golden (III) is reduced into golden (I) in gold chloride, and the two is continuous It is mixed into primary liquor under the shear action of fluid, which moves to passages downstream, at the Y-Shaped channel of two level and monodisperse Reduction Body solution C is met, and through secondary mixing, realizes the mixing of reactive material.It is logical in straight line that homogeneous mixed solution is formed after mixing Realize the growth ageing stage of reaction in road, final reaction generates that single dispersing particle diameter is small to be protected by alkyl carbon chain alkanethiol monolayer Gold nanoclusters.
Embodiment 5
It adopts gold chloride and ammonium bromide and tetraoctyl ammonium bromide (1:1.2) it is dissolved in methanol and is configured to 0.15mol/l solution, by boron hydrogen Change sodium, which is dissolved in ice water, is configured to 0.6mol/L solution.Using syringe pump with 800nl/min flow velocitys to liquid storage tank A Continuous Perfusions The methanol solution of gold chloride/ammonium bromide and tetraoctyl ammonium bromide, using syringe pump with 300nl/min flow velocitys to liquid storage tank B Continuous Perfusions just oneself Alkanethiol solution, with 300nl/min flow velocitys to the sodium borohydride solution of liquid storage tank C Continuous Perfusions 0.6mol/L, in first order Y- Tetrahydrofuran mixed liquor meets with n-hexane mercaptan at type channel, and golden (III) is reduced into golden (I) in gold chloride, and the two is continuous It is mixed into primary liquor under the shear action of fluid, which moves to passages downstream, at the Y-Shaped channel of two level and monodisperse Reduction Body solution C is met, and through secondary mixing, realizes the mixing of reactive material.It is logical in straight line that homogeneous mixed solution is formed after mixing Realize the growth ageing stage of reaction in road, final reaction generates that single dispersing particle diameter is small to be protected by alkyl carbon chain alkanethiol monolayer Gold nanoclusters.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or It changes still within the protection scope of the invention.

Claims (10)

1. a kind of method preparing gold nanoclusters based on micro-fluidic chip, which is characterized in that this method includes：
Oligomer solution, alkane before Continuous Perfusion dispersed phase gold into the liquid storage tank A of micro-fluidic chip, liquid storage tank B and liquid storage tank C respectively Base carbochain thiol solution and monodisperse restore liquid solution, in control liquid storage tank A continuous phase fluid flow velocity be 300nl/min~ The flow velocity of alkyl carbon chain mercaptan is 300nl/min in 800nl/min, liquid storage tank B, monodisperse reduction liquid solution in liquid storage tank C Flow velocity is 150nl/min~300nl/min, obtains gold nanoclusters；
The micro-fluidic chip is that it is single that the Y-Shaped channel of level-one is disposed on the chip using transparent PDMS as base material The Y-Shaped channel unit of member, integrated unit, two level and mixed cell, the Y-Shaped channel unit of level-one include liquid storage tank A and liquid storage tank B, The Y-Shaped channel unit of two level includes liquid storage tank C, the port setting reaction of the Y-Shaped channel unit of level-one and the Y-Shaped channel unit of two level Object fluid interface, for injecting oligomer solution before dispersed phase gold, alkyl carbon chain thiol solution and monodisperse restore liquid solution；Mixing Collection of products interface is arranged in the port of unit, for collecting product.
2. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that described Gold before in aggressiveness the molar ratio of gold and alkyl carbon chain mercaptan be 1:5.
3. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that described Monodisperse reduction liquid solution, gold before the volume ratio of oligomer solution and alkyl carbon chain thiol solution be 5:0.07:1.
4. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that described Gold before oligomer solution include gold chloride and the mixed solution of ammonium bromide and tetraoctyl ammonium bromide.
5. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 4, which is characterized in that described Gold chloride and ammonium bromide and tetraoctyl ammonium bromide molar ratio be 1：(1.2-1.3).
6. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 4, which is characterized in that described Gold before in oligomer solution gold chloride a concentration of 0.01~0.4mmol/L, ammonium bromide and tetraoctyl ammonium bromide a concentration of 0.011~ 0.05mol/L。
7. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that used Gold before oligomer solution solvent be tetrahydrofuran, methanol or acetone.
8. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that described Alkyl carbon chain mercaptan be n-dodecyl mercaptan solution or n-hexane thiol solution.
9. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that described Monodisperse reduction liquid solution be sodium borohydride solution.
10. a kind of method preparing gold nanoclusters based on micro-fluidic chip according to claim 1, which is characterized in that institute A concentration of 0.5mol/L for the monodisperse reduction liquid solution stated.
CN201710036454.8A 2017-01-18 2017-01-18 A method of gold nanoclusters are prepared based on micro-fluidic chip Active CN106825605B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710036454.8A CN106825605B (en) 2017-01-18 2017-01-18 A method of gold nanoclusters are prepared based on micro-fluidic chip

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710036454.8A CN106825605B (en) 2017-01-18 2017-01-18 A method of gold nanoclusters are prepared based on micro-fluidic chip

Publications (2)

Publication Number Publication Date
CN106825605A CN106825605A (en) 2017-06-13
CN106825605B true CN106825605B (en) 2018-07-13

Family

ID=59124616

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710036454.8A Active CN106825605B (en) 2017-01-18 2017-01-18 A method of gold nanoclusters are prepared based on micro-fluidic chip

Country Status (1)

Country Link
CN (1) CN106825605B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108405875A (en) * 2018-03-15 2018-08-17 山东豪迈化工技术有限公司 It is used to prepare the method and device of gold nanoparticle
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
CN111618313B (en) * 2020-05-14 2022-12-13 西安石油大学 Method for preparing silver nanoparticles based on microfluidic technology
CN115582552B (en) * 2022-10-10 2023-10-27 武汉理工大学 Preparation method for improving gold cluster based on solvent-assisted two-phase synthesis strategy

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102745660A (en) * 2011-04-18 2012-10-24 中国科学院大连化学物理研究所 Microfluidic chip based method for synthesizing needle-like hydroxyapatite nanoparticle
CN103737018A (en) * 2014-01-17 2014-04-23 昆明理工大学 Method for continuous and rapid preparation of nano nickel by microfluidics technology
CN105033278A (en) * 2015-08-18 2015-11-11 深圳前海桓硕芯嘉纳微科技有限公司 Preparation method for silver nanowire
CN204912776U (en) * 2015-08-18 2015-12-30 深圳前海桓硕芯嘉纳微科技有限公司 Micro -fluidic preparation facilities of nanometer gold solution

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040124085A1 (en) * 2002-06-26 2004-07-01 California Institute Of Technology Microfluidic devices and methods with electrochemically actuated sample processing
KR101356933B1 (en) * 2012-12-28 2014-01-29 고려대학교 산학협력단 Apparatus and method for separating micro-nano scale particles using surface acoustic wave-based microfluidic chromatography

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102745660A (en) * 2011-04-18 2012-10-24 中国科学院大连化学物理研究所 Microfluidic chip based method for synthesizing needle-like hydroxyapatite nanoparticle
CN103737018A (en) * 2014-01-17 2014-04-23 昆明理工大学 Method for continuous and rapid preparation of nano nickel by microfluidics technology
CN105033278A (en) * 2015-08-18 2015-11-11 深圳前海桓硕芯嘉纳微科技有限公司 Preparation method for silver nanowire
CN204912776U (en) * 2015-08-18 2015-12-30 深圳前海桓硕芯嘉纳微科技有限公司 Micro -fluidic preparation facilities of nanometer gold solution

Also Published As

Publication number Publication date
CN106825605A (en) 2017-06-13

Similar Documents

Publication Publication Date Title
CN106825605B (en) A method of gold nanoclusters are prepared based on micro-fluidic chip
CN106270543B (en) The method for continuously preparing the controllable Triangular nanoplates of arrangement mode
Mello et al. FocusMicroscale reactors: nanoscale products
CN101343778B (en) Process for producing golden nano stick with short length-diameter ratio
CN103386333A (en) Micro-fluidic liquid drop production chip
CN103273083B (en) A kind of preparation method of gold nano grain
Su et al. Ideal micromixing performance in packed microchannels
CN101072991B (en) Method and installation for determining rheological characteristics of a fluid, and corresponding identifying method
CN102745660B (en) Microfluidic chip based method for synthesizing needle-like hydroxyapatite nanoparticle
CN102826585B (en) Method for producing ultra-small water soluble near-infrared Ag2S quantum dots
CN101565175A (en) Device of fast synthetizing CdSe quantum dots and method thereof
CN103386336A (en) Microfluidic chip for producing droplets with concentration gradients
CN107617750B (en) The method for preparing Ag/ redox graphene composite nano materials
CN106563811A (en) Method for continuously preparing urchin-like Ag-ZnO nano particles by using microchannel reactor
CN103754837A (en) Method for preparation of bismuth-containing nano-hollow ball by using porous bismuth oxide as template
CN106109440A (en) A kind of micro-fluidic chip and the preparation method of alginate magnetic microsphere
CN104150537B (en) A kind of six side phase WO3Nanotube and preparation method thereof
CN103386337A (en) Microfluidic chip for producing multicomponent droplets
CN103737018A (en) Method for continuous and rapid preparation of nano nickel by microfluidics technology
CN208340745U (en) A kind of microballoon quickly prepares collection micro-fluidic chip
Li et al. Synthesis of quantum dots based on microfluidic technology
CN112630407A (en) Microcosmic visual simulation experiment device and method for seepage and sand production of hydrate reservoir
CN108726554A (en) One kind efficiently preparing evengranular nano barium sulfate method
He et al. Screening the Ion compositions on crystal morphology transitions by a microfluidic chip with a well-defined concentration gradient
CN106634923A (en) Surface-modified nano-silica and nano fluid for crude oil recovery

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
GR01 Patent grant
GR01 Patent grant