CN110405223A - A kind of preparation method of the controllable nanon size gold particle of high-purity - Google Patents
A kind of preparation method of the controllable nanon size gold particle of high-purity Download PDFInfo
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- CN110405223A CN110405223A CN201910740031.3A CN201910740031A CN110405223A CN 110405223 A CN110405223 A CN 110405223A CN 201910740031 A CN201910740031 A CN 201910740031A CN 110405223 A CN110405223 A CN 110405223A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
- B23K26/062—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam
- B23K26/0622—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
- B23K26/064—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms
- B23K26/0648—Shaping the laser beam, e.g. by masks or multi-focusing by means of optical elements, e.g. lenses, mirrors or prisms comprising lenses
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- 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
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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Abstract
A kind of preparation method of the controllable nanon size gold particle of high-purity, belongs to metal material field.Preparation step is divided into target smelting, nanoparticles prepared by laser ablation seed, chemistry inoculation nanoparticle growth, four steps of centrifuge separation.Wherein chemistry inoculation nanoparticle growth is by using seed growth method with using sodium citrate to combine as the coreduction technology of reducing agent, it is ensured that the monodisperse of gold particle and control certain size gold nano grain formation；For large scale gold particle, it is necessary to use multi-step particle growth method.Centrifuge separation is the high speed rotation by rotor, generates centrifugal force field in internal rotor, weight component has differences in centrifugal force field along the radial pressure distribution of rotor, isolates the bronze of high-purity.The method of the present invention is ingenious in design, simple and reliable, durable, low in cost, and the high-purity bronze product of certain scale can be prepared with it.
Description
Technical field
The present invention is applied to the key technology area in the production of noble metal creamy material, more particularly to precision instrument surface
The production of golden plated film.
Background technique
A kind of optical coating product of the noble metal creamy material as specific use, after sintering can be in optical glass fibre
A kind of adhesion-tight, inviolateness, the surface golden film excellent in golden yellow, electric conductivity are formed on panel cylindrical surface.The gold paste applies
It is overlying on optical glass fibre panel cylindrical surface, after sintering, finish is applied to different field up to 12 grades or more.
Gold paste is in addition to being widely used in porcelain, fine pottery, decorates outer on the products such as glass, and coating is also widely used for building
It builds, optics and electric appliance etc. make conductive layer, reflection and protective film etc..With the development that electronics industry is maked rapid progress, metal has
Machine compound is applied to thick film production conductor and resistance slurry as a kind of new technology.Photosensitizer is added in cooperation in the slurry,
It can be used for making the hot showing head of arbitrary graphic, the products such as imaging sensor circuit using exposure technique.In common Gold conductor
It is middle that a small amount of base metal resinate is added, to form active novel structure, for improving adhesive force and improving film
The consistency of layer.
To prevent electrode from generating electric discharge phenomena, it is desirable that sintered gold film surface roughness Ra≤0.1 μm, on gold paste sintered membrane not
Allow to have a stain and stain, has good adhesive force to optical glass fibre panel, weak acid resistant weak base, therefore to nanogold particle
Preparation process require just be particularly important.
Summary of the invention
In order to solve high-purity nano gold particle preparation and gold paste in terms of application problem, the present invention
Purpose be by strictly control gold purity and nanogold particle size, utilize laser ablation and chemistry inoculation growth
The nanogold particle of necessary requirement is obtained, by being sufficiently stirred with organic solvent, gold paste is finally made, to meet military project to bronze
High-purity, the demand of high-compactness.
A kind of preparation method of the controllable nanon size gold particle of high-purity, it is characterised in that comprise the concrete steps that:
(1) target is smelted: carrying out vacuum metling to gold target material, Vacuum door is sealed together and is changed to two seals, Vacuum door
Liner heat-insulating and sealing material increases stainless steel cloth at the top of mist eliminator；
(2) nanoparticles prepared by laser ablation seed；
(3) chemistry inoculation nanoparticle growth: by seed growth method and sodium citrate will be used as reducing agent
Coreduction technology combines, it is ensured that the formation of the gold nano grain of the monodisperse and control certain size of gold particle；For big ruler
Very little gold particle, it is necessary to use multi-step particle growth method；
(4) it is centrifugated: by the high speed rotation of rotor, generating centrifugal force field in internal rotor, weight component is being centrifuged
Radial pressure distribution in the field of force along rotor has differences, and isolates the bronze of high-purity.
The preparation method of the controllable nanon size gold particle of high-purity as described above, specific preparation step is:
(1), target is smelted
Before smelting, first have to update pump oil in vacuum pump, it is secondary that metal auxiliary material is toasted in 380-420 DEG C of oven
25-35min, to remove moisture removal；Vacuum degree reading < 0.01Pa, 1150-1250 DEG C of smelting temperature, duration of heat 10-12h；It smelts
Number is 5-7 times, finally obtains the proof gold target that purity is 99.999%；
(2), nanoparticles prepared by laser ablation seed
Firstly, with the target surface of 500 grit carborundum paper processing Au to remove surface defect；By target be placed on acetone and
It cleans 18-12 minutes, is then rinsed with deionized water to eliminate any existing pollutant in the ultrasonic bath of ethyl alcohol；It will cleaning
Target be placed on the bottom of the Pyrex glass container filled with 70vol% ethyl alcohol, pulse Nd is used in ablation procedure:
YAG laser is as radiation source, fundamental wavelength: 1064nm；Pulse duration 8ns；Repetitive rate: 10Hz；Laser beam is by focal length
The lens focus of 90-110mm obtains the laser energy density of 20J/cm2 on the surface of Au target；Ablation process at room temperature into
Row 218-22min obtains pure Au colloidal solution, average grain diameter 20nm；
(3), chemistry inoculation nanoparticle growth
By carrying out chemistry inoculation growth to the gold particle after laser ablation, reach the requirement of its size；Going back based on metal
Metal ion is converted neutral atom by original, and it is small metal cluster that the low solubility of these free atoms, which induces their fast nucleations,
Then remaining neutral atom is grown on existing particle；Gold particle growth is by using reduction of sodium citrate gold chloride in water
And it is formed；The size of gold particle is controlled by changing the ratio of Au and citrate during synthesis；It is raw by using seed
Long method has been realized in pure Au particle, wherein be initially formed small dispersed nano particle, then use them as growth compared with
The seed of big gold particle；During growth step, by precise controlling growth conditions and select suitable reducing agent new to prevent
The formation of seed.
(4), it is centrifugated
Using centrifuge, turn up 1800-2200 per minute is set and is turned, is run 13-17 minutes, high speed centrifugation filters out most
High-purity bronze made from end.
Further, step (3) the precise controlling growth conditions is: during the growth process using the short time, low concentration,
Multifrequency time, control method stage by stage will be rocked time control every time and be no more than 1 minute, and time of repose is no more than 10 minutes,
Chlorauric acid solution and reducing agent solution control are being no more than 0.02mol/L, and solution when adding pays attention to that low concentration is wanted repeatedly to add
Grow nanogold particle stage by stage；In this preparation process, reducing agent is chosen are as follows: ascorbic acid, sodium bromide, citric acid
Sodium.
Explanation about specific steps:
(1) target is smelted: being carried out vacuum metling to gold target material, is only done some local improvement to vacuum drying oven: improving vacuum valve peace
Dress mode, Vacuum door seal together is changed to two seals, transformation vacuum door lining heat-insulating and sealing material, transformation graphite rod conductive seat
Material etc..Since smelting room space is larger, uniform heat distribution, temperature are easily adjusted, therefore continuous still, collecting and the taking-up of gold are all
Very smoothly.Metallurgical slag is also relatively more smooth in the auto-ignition combustion of volatilization cooling chamber and volatilization, and absorption tower assimilation effect is relatively good, multiple shelves
Mist eliminator initial performances are poor, after increase stainless steel cloth at the top of mist eliminator, reached extraordinary effect, periodically rushed with water
It washes.By repeatedly smelting, so that the gold target material purity smelted out reaches 99.999%.
(2) nanoparticles prepared by laser ablation seed: currently, the preparation method of gold nano-material has very much, such as solwution method, photochemical
Method, electrolysis method, chemical vapour deposition technique, DC sputtering, particle beam bombardment method etc. can substantially be attributed to chemistry according to principle
Method and physical method.In chemical method, gold nano crystal grain is present in solution or colloid environment more, in order to prevent crystal grain
Cluster increases its stability, generally requires that the chemical substances such as dispersing agent, passivator, stabilizer are added, and these substances not only can
Nanocrystal purity is caused to decline, impaired performance also will cause a degree of environmental pollution；Meanwhile it is thin forming gold nano
During film, thickness and uniformity are difficult control.Using laser ablation technology, prepares gold nano-material and belongs to physical method,
It is possible to prevente effectively from the above problem.Relative to the d.c. sputtering and particle beam bombardment in physical method, laser ablation technology due to
High and fast and high-efficient with the heating speed advantage of laser energy, can be used for metal, the preparation of the infusibilities substance such as ceramics；This
Outside, laser ablation technology can also by change optical maser wavelength, pulse width and frequency, laser energy, environmental gas type and
The experiment conditions such as pressure, target lining spacing, environment temperature, study nanocrystal pattern, structure and its growth power from different perspectives
Process.
(3) chemistry inoculation nanoparticle growth: by seed growth method and sodium citrate will be used as reducing agent
Coreduction technology combines, it can be ensured that the formation of the gold nano grain of the monodisperse and control certain size of gold particle.Due to
Reduction can cause undesirable nucleation at high temperature, it is therefore necessary to very carefully control the ratio of seed Au- citrate.Such as
Fruit seed concentration is high, then metallic monomer is more likely to grow on existing seed rather than forms new core.It is therefore preferable that using high
Seed is to concentration of metal ions.But which has limited the final sizes of particle.For large scale gold particle, it is necessary to use multistep
Rapid particle growth method.
(4) it is centrifugated: by the high speed rotation of rotor, generating centrifugal force field in internal rotor, weight component is being centrifuged
Radial pressure distribution in the field of force along rotor has differences, and isolates the bronze of high-purity.
Our method is depended in small Au seed continued growth, generates the monodispersed gold nano for reaching size requirement
Grain.Gold is used as seed, they are more stable, it is easier to produce, there are small Au seeds at center, for diameter greater than 50nm's
The optical property of particle does not have significant impact.Even if theoretical plasma peak position only slightly deviates, but peak value at 30nm
It is wider.Obtained nanogold particle may be used as the seed of then gold growth, and repeat the process until reaching required ruler
It is very little.
The method that the present invention designs is ingenious in design, simple and reliable, durable, low in cost, and a set pattern can be prepared with it
The high-purity bronze product of mould
Specific embodiment
Example one:
1, target is smelted
Before smelting, first have to update pump oil in vacuum pump, because old pump oil will affect degasifying effect, diffusion pump needs to preheat
50min, it is secondary that the auxiliary materials such as metal are toasted 30min in 400 DEG C of ovens, to remove moisture removal.Every furnace feeds 0.5kg, very
Reciprocal of duty cycle reading < 0.01Pa, 1200 DEG C of smelting temperature or so, duration of heat 12h；Smelting number is 6 times, and finally obtaining purity is
99.999% proof gold target.
2, nanoparticles prepared by laser ablation seed
Firstly, with the target surface of emery paper (with 500 granularities) processing Au to remove surface defect.Target is placed on
It cleans 10 minutes, is then rinsed with deionized water to eliminate any existing pollutant in the ultrasonic bath of acetone and ethyl alcohol.It will
Clean target is placed on the bottom of the Pyrex glass container (volume 15mL) filled with 70vol% ethyl alcohol, in ablation procedure
It is middle to use pulse Nd:YAG laser (fundamental wavelength: 1064nm；Pulse duration 8ns；Repetitive rate: 10Hz) it is used as radiation source.
Laser beam is obtained the laser energy density of about 20J/cm2 by the lens focus that focal length is 100mm on the surface of Au target.Ablation
Journey carries out 20min at room temperature, obtains pure Au colloidal solution, average grain diameter 20nm.
3, chemistry inoculation nanoparticle growth
By carrying out chemistry inoculation growth to the gold particle after laser ablation, reach the requirement of its size.Going back based on metal
Metal ion is converted neutral atom by original.It is small metal cluster that the low solubility of these free atoms, which induces their fast nucleations,
Then remaining neutral atom is grown on existing particle.Gold particle growth is by using reduction of sodium citrate gold chloride in water
And it is formed.In this method, the size of gold particle can be controlled by changing the ratio of Au and citrate during synthesis.
For small size, this method may be generated with the coefficient of variation (being defined as the standard deviation of size distribution divided by average-size)
Gold particle, but its content be lower than 10%, this correspond to excellent monodispersity.However, when producing big (> 40nm) gold particle
When, the dispersion of size and shape is worse.
It is to be nucleated in forming process and the time of growth step point in terms of synthesizing monodispersed gold nano grain most critical
From.Pure Au particle is had been realized in by using seed growth method, wherein being initially formed small dispersed nano particle, then
Use them as growing the seed of larger gold particle.It is important that preventing the formation of new seed during growth step.This is logical
Precise controlling growth conditions and the suitable reducing agent of selection is crossed to realize.At low temperature there is reduction ion in metal surface for selection
Reducing agent prevent new nucleation, this seed growth method has been successfully used to the Au of synthesis large scale and size Control
Particle.
4, it is centrifugated
Using centrifuge, it is arranged 2000 turns per minute of turn up, runs 15 minutes, high speed centrifugation, filters out final obtained
High-purity bronze.
Example two:
1, target is smelted
Before smelting, first have to update pump oil in vacuum pump, because old pump oil will affect degasifying effect, diffusion pump needs to preheat
50min, it is secondary that the auxiliary materials such as metal are toasted 25min in 380 DEG C of ovens, to remove moisture removal.Every furnace feeds 0.2kg, very
Reciprocal of duty cycle reading < 0.01Pa, 1200 DEG C of smelting temperature or so, duration of heat 10h；Smelting number is 5 times, and finally obtaining purity is
99.999% proof gold target.
2, nanoparticles prepared by laser ablation seed
Firstly, with the target surface of emery paper (with 500 granularities) processing Au to remove surface defect.Target is placed on
It cleans 15 minutes, is then rinsed with deionized water to eliminate any existing pollutant in the ultrasonic bath of acetone and ethyl alcohol.It will
Clean target is placed on the bottom of the Pyrex glass container (volume 15mL) filled with 70vol% ethyl alcohol, in ablation procedure
It is middle to use pulse Nd:YAG laser (fundamental wavelength: 1064nm；Pulse duration 8ns；Repetitive rate: 10Hz) it is used as radiation source.
Laser beam is obtained the laser energy density of about 20J/cm2 by the lens focus that focal length is 100mm on the surface of Au target.Ablation
Journey carries out 18min at room temperature, obtains pure Au colloidal solution, average grain diameter 25nm.
3, chemistry inoculation nanoparticle growth
By carrying out chemistry inoculation growth to the gold particle after laser ablation, reach the requirement of its size.Going back based on metal
Metal ion is converted neutral atom by original.It is small metal cluster that the low solubility of these free atoms, which induces their fast nucleations,
Then remaining neutral atom is grown on existing particle.Gold particle growth be by water use bromination sodium reduction gold chloride and
It is formed.In this method, the size of gold particle can be controlled by changing the ratio of Au and sodium bromide during synthesis.For
Small size, this method may generate the gold with the coefficient of variation (being defined as the standard deviation of size distribution divided by average-size)
Particle, but its content is lower than 10%, and this corresponds to excellent monodispersity.However, when producing big (> 40nm) gold particle, ruler
Very little and shape dispersion is worse.
It is to be nucleated in forming process and the time of growth step point in terms of synthesizing monodispersed gold nano grain most critical
From.Pure Au particle is had been realized in by using seed growth method, wherein being initially formed small dispersed nano particle, then
Use them as growing the seed of larger gold particle.It is important that preventing the formation of new seed during growth step.This is logical
Precise controlling growth conditions and the suitable reducing agent of selection is crossed to realize.At low temperature there is reduction ion in metal surface for selection
Reducing agent prevent new nucleation, this seed growth method has been successfully used to the Au of synthesis large scale and size Control
Particle.
4, it is centrifugated
Using centrifuge, it is arranged 1800 turns per minute of turn up, runs 17 minutes, high speed centrifugation, filters out final obtained
High-purity bronze.
Example three:
1, target is smelted
Before smelting, first have to update pump oil in vacuum pump, because old pump oil will affect degasifying effect, diffusion pump needs to preheat
50min, it is secondary that the auxiliary materials such as metal are toasted 35min in 420 DEG C of ovens, to remove moisture removal.Every furnace feeds 0.7kg, very
Reciprocal of duty cycle reading < 0.01Pa, 1200 DEG C of smelting temperature or so, duration of heat 12h；Smelting number is 7 times, and finally obtaining purity is
99.999% proof gold target.
2, nanoparticles prepared by laser ablation seed
Firstly, with the target surface of emery paper (with 500 granularities) processing Au to remove surface defect.Target is placed on
It cleans 20 minutes, is then rinsed with deionized water to eliminate any existing pollutant in the ultrasonic bath of acetone and ethyl alcohol.It will
Clean target is placed on the bottom of the Pyrex glass container (volume 15mL) filled with 70vol% ethyl alcohol, in ablation procedure
It is middle to use pulse Nd:YAG laser (fundamental wavelength: 1064nm；Pulse duration 8ns；Repetitive rate: 10Hz) it is used as radiation source.
Laser beam is obtained the laser energy density of about 20J/cm2 by the lens focus that focal length is 100mm on the surface of Au target.Ablation
Journey carries out 202min at room temperature, obtains pure Au colloidal solution, average grain diameter 15nm.
3, chemistry inoculation nanoparticle growth
By carrying out chemistry inoculation growth to the gold particle after laser ablation, reach the requirement of its size.Going back based on metal
Metal ion is converted neutral atom by original.It is small metal cluster that the low solubility of these free atoms, which induces their fast nucleations,
Then remaining neutral atom is grown on existing particle.Gold particle growth is by restoring gold chloride with ascorbic acid in water
And it is formed.In this method, the size of gold particle can be controlled by changing the ratio of Au and ascorbic acid during synthesis.
For small size, this method may be generated with the coefficient of variation (being defined as the standard deviation of size distribution divided by average-size)
Gold particle, but its content be lower than 10%, this correspond to excellent monodispersity.However, when producing big (> 40nm) gold particle
When, the dispersion of size and shape is worse.
It is to be nucleated in forming process and the time of growth step point in terms of synthesizing monodispersed gold nano grain most critical
From.Pure Au particle is had been realized in by using seed growth method, wherein being initially formed small dispersed nano particle, then
Use them as growing the seed of larger gold particle.It is important that preventing the formation of new seed during growth step.This is logical
Precise controlling growth conditions and the suitable reducing agent of selection is crossed to realize.At low temperature there is reduction ion in metal surface for selection
Reducing agent prevent new nucleation, this seed growth method has been successfully used to the Au of synthesis large scale and size Control
Particle.
4, it is centrifugated
Using centrifuge, it is arranged 2500 turns per minute of turn up, runs 15 minutes, high speed centrifugation, filters out final obtained
High-purity bronze.
Claims (3)
1. a kind of preparation method of the controllable nanon size gold particle of high-purity, it is characterised in that preparation step is:
(1) target is smelted: carrying out vacuum metling to gold target material, Vacuum door is sealed together and is changed to two seals, vacuum door lining
Heat-insulating and sealing material increases stainless steel cloth at the top of mist eliminator；
(2) nanoparticles prepared by laser ablation seed；
(3) chemistry inoculation nanoparticle growth: by going back seed growth method as the total of reducing agent with sodium citrate is used
Former technology combines, it is ensured that the formation of the gold nano grain of the monodisperse and control certain size of gold particle；For large scale gold
Particle, it is necessary to use multi-step particle growth method；
(4) it is centrifugated: by the high speed rotation of rotor, generating centrifugal force field in internal rotor, weight component is in centrifugal force field
The middle radial pressure distribution along rotor has differences, and isolates the bronze of high-purity.
2. the preparation method of the controllable nanon size gold particle of high-purity as described in claim 1, it is characterised in that specific preparation
Step is:
(1), target is smelted
Before smelting, first have to update pump oil in vacuum pump, it is secondary that metal auxiliary material is toasted 25- in 380-420 DEG C of oven
35min, to remove moisture removal；Vacuum degree reading < 0.01Pa, 1150-1250 DEG C of smelting temperature, duration of heat 10-12h；It smelts secondary
Number is 5-7 times, finally obtains the proof gold target that purity is 99.999%；
(2), nanoparticles prepared by laser ablation seed
Firstly, with the target surface of 500 grit carborundum paper processing Au to remove surface defect；Target is placed on acetone and ethyl alcohol
Ultrasonic bath in clean 15-20 minutes, then rinsed with deionized water to eliminate any existing pollutant；By clean target
It is placed on the bottom of the Pyrex glass container filled with 70vol% ethyl alcohol, is swashed in ablation procedure using pulse Nd:YAG
Light is as radiation source, fundamental wavelength: 1064nm；Pulse duration 8ns；Repetitive rate: 10Hz；Laser beam is 90- by focal length
The lens focus of 110mm obtains 20 J/cm on the surface of Au target2Laser energy density；Ablation process carries out at room temperature
18-22min obtains pure Au colloidal solution, average grain diameter 20nm；
(3), chemistry inoculation nanoparticle growth
By carrying out chemistry inoculation growth to the gold particle after laser ablation, reach the requirement of its size；Reduction based on metal will
Metal ion is converted into neutral atom, and it is small metal cluster that the low solubility of these free atoms, which induces their fast nucleations, then
Remaining neutral atom is grown on existing particle；Gold particle growth be by water use reduction of sodium citrate gold chloride and shape
At；The size of gold particle is controlled by changing the ratio of Au and citrate during synthesis；By using seed growth side
Method has been realized in pure Au particle, wherein being initially formed small dispersed nano particle, then uses them as growing larger gold
The seed of particle；During growth step, new seed is prevented by precise controlling growth conditions and the suitable reducing agent of selection
Formation；
(4), it is centrifugated
Using centrifuge, turn up 1800-2500 per minute is set and is turned, is run 13-17 minutes, high speed centrifugation filters out final system
The high-purity bronze obtained.
3. the preparation method of the controllable nanon size gold particle of high-purity as claimed in claim 2, it is characterised in that step (3) institute
Stating precise controlling growth conditions is:, will during the growth process using short time, low concentration, multifrequency time, control method stage by stage
It rocks time control every time be no more than 1 minute, time of repose is no more than 10 minutes, chlorauric acid solution and reducing agent solution control
System is being no more than 0.02mol/L, and solution notices that wanting low concentration repeatedly to add grows nanogold particle stage by stage when adding；At this
In a preparation process, reducing agent is chosen are as follows: ascorbic acid, sodium bromide, sodium citrate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111702186A (en) * | 2020-07-23 | 2020-09-25 | 苏州大学 | Preparation method of gold nanoparticles with adjustable size |
| CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
| CN116443858A (en) * | 2023-04-27 | 2023-07-18 | 安徽工业大学 | Method for synthesizing nano biomass charcoal by seed induction under nano biomass charcoal and acid hydrolysis |
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| CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
| CN116443858A (en) * | 2023-04-27 | 2023-07-18 | 安徽工业大学 | Method for synthesizing nano biomass charcoal by seed induction under nano biomass charcoal and acid hydrolysis |
| CN116443858B (en) * | 2023-04-27 | 2024-03-12 | 安徽工业大学 | Method for synthesizing nano biomass charcoal by seed induction under nano biomass charcoal and acid hydrolysis |
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