CN109434130A - A kind of preparation method of spherical nano silver powder - Google Patents
A kind of preparation method of spherical nano silver powder Download PDFInfo
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- CN109434130A CN109434130A CN201811495475.7A CN201811495475A CN109434130A CN 109434130 A CN109434130 A CN 109434130A CN 201811495475 A CN201811495475 A CN 201811495475A CN 109434130 A CN109434130 A CN 109434130A
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- nano silver
- silver powder
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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
- 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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of preparation methods of spherical nano silver powder, include the following steps: (1) by 10ml concentration be 0.1mol/L silver nitrate, it is slowly dropped in the sodium bicarbonate solution that 30mL concentration is 0.05mol/L, generates the mixed solution containing silver carbonate sediment；(2) 1.7g surfactant polyvinylpyrrolidone is added in mixed liquor and sufficiently dissolves, reaction solution is transferred in hydrothermal reaction kettle, hydro-thermal reaction 5h, cooled to room temperature obtain nano silver colloidal sol under 180 DEG C of constant reaction temperatures；(3) nano silver colloidal sol deionized water, ethyl alcohol are sufficiently washed, is centrifugated, nano silver colloidal sol solution is evenly applied to clean glass substrate surface, spontaneously dries at room temperature, obtains nano silver powder.The preparation method no pollution to the environment, cost is relatively low, and nano silver powder particle obtained is spherical, particle size distribution narrow range, single dispersion, partial size 40nm.
Description
Technical field
The present invention relates to the technical field of powder body material preparation process more particularly to a kind of preparations of spherical nano silver powder
Method.
Background technique
Since nano silver particles are in microelectronics, photoelectron, catalysis, biosensor, data storage, magnetic device, medicine
Antibacterial, the potential application of Surface enhanced Raman spectroscopy etc., it has also become the hot fields of people's research.
There are many preparation methods of nano silver particles, can substantially be divided into physical method and chemical method two major classes, including
Microwave reduction method, ultrasonic wave added synthetic method, magnetron sputtering method, template, photoreduction met hod, crystal seed method, polyol process, microemulsion
Method, electrochemical process, biological reducing method etc., but all there are certain deficiencies to a certain extent, such as physical method preparation are received
The silver-colored the high requirements on the equipment of rice, thus preparation cost is relatively high, many reducing agents used in chemical method are toxic, need big
The surfactant of amount is protected, and the particle stability of generation is poor, easily reunites, and particle diameter distribution is uneven, to limit
The use of nano silver.
Summary of the invention
The purpose of the invention is to overcome the above-mentioned prior art, a kind of preparation of spherical nano silver powder is provided
The preparation method of method, the spherical nano silver powder uses hydro-thermal method, does not add any reducing agent, with silver nitrate and sodium bicarbonate
Solution reaction generates fresh silver carbonate precipitating, the isothermal reaction in hydrothermal reaction kettle, in point of polyvinylpyrrolidone (PVP)
It dissipates under effect, under surfactant polyvinylpyrrolidone (PVP) protection, nano silver colloidal sol is made in hydrothermal decomposition silver carbonate,
Nano silver colloidal sol is passed through into subsequent centrifuge separation, obtains nano silver powder after dry.The preparation method simple possible, to environment without
Pollution, cost is relatively low, is easy to industrialize, and the particle of nano silver powder obtained is spherical, particle size distribution narrow range, single
Dispersion, partial size 40nm or so.
The technical solution adopted by the present invention to solve the technical problems is: a kind of preparation method of spherical nano silver powder,
Include the following steps:
(1) it is 0.1mol/L silver nitrate by 10ml concentration, is slowly dropped to the sodium bicarbonate that 30mL concentration is 0.05mol/L
In solution, the mixed solution containing white silver carbonate sediment is generated；
(2) 1.7g surfactant polyvinylpyrrolidone is then added in above-mentioned mixed liquor and sufficiently dissolves, will
To reaction solution be transferred to teflon lined hydrothermal reaction kettle in, the hydro-thermal reaction 5h under 180 DEG C of constant reaction temperatures,
Cooled to room temperature obtains nano silver colloidal sol；
(3) nano silver colloidal sol deionized water, ethyl alcohol are sufficiently washed, is then centrifuged for separating, by nano silver colloidal sol solution
It is evenly applied to clean glass substrate surface, spontaneously dries at room temperature, obtains nano silver powder.
Further, the deionized water in the step (3) is secondary distilled water.
Further, the volume of the hydrothermal reaction kettle in the step (2) is 100mL.
In conclusion the preparation method of spherical nano silver powder of the invention uses hydro-thermal method, any reducing agent is not added,
It is reacted with silver nitrate with sodium bicarbonate solution and generates fresh silver carbonate precipitating, the isothermal reaction in hydrothermal reaction kettle, in poly- second
Under the peptizaiton of alkene pyrrolidone (PVP), under surfactant polyvinylpyrrolidone (PVP) protection, hydrothermal decomposition carbon
Sour silvery obtains nano silver colloidal sol, and nano silver colloidal sol is passed through subsequent centrifuge separation, obtains nano silver powder after dry.The preparation side
Method simple possible, no pollution to the environment, cost is relatively low, is easy to industrialize, and the particle of nano silver powder obtained is spherical, partial size
Size distribution narrow range, single dispersion, partial size 40nm or so.
Detailed description of the invention
Fig. 1 is the SEM figure for the nano silver powder that reaction temperature is produced at 180 DEG C；
Fig. 2 is the SEM figure for the nano silver powder that reaction temperature is produced at 130 DEG C；
Fig. 3 is the SEM figure for the nano silver powder that reaction temperature is produced at 160 DEG C；
Fig. 4 is the SEM figure for the nano silver powder that reaction temperature is produced at 200 DEG C；
Fig. 5 is the SEM figure for the nano silver powder that reaction temperature is produced at 230 DEG C；
Fig. 6 is the SEM figure of the nano silver powder produced in 2h in the reaction time；
Fig. 7 is the SEM figure for the nano silver powder that reaction temperature is produced in 5h；
Fig. 8 is the SEM figure for the nano silver powder that reaction temperature is produced in 10h；
Fig. 9 is the SEM figure for the nano silver powder that reaction temperature is produced in 18h；
Figure 10 is that PVP schemes for the SEM of the nano silver powder produced when 0g；
Figure 11 is that PVP schemes for the SEM of the nano silver powder produced when 0.5g；
Figure 12 is that PVP schemes for the SEM of the nano silver powder produced when 1.2g；
Figure 13 is that PVP schemes for the SEM of the nano silver powder produced when 1.7g；
Figure 14 is that silver nitrate concentration is schemed for the SEM of the nano silver powder produced when 0.4mol/l；
Figure 15 is that silver nitrate concentration is schemed for the SEM of the nano silver powder produced when 0.025mol/l；
Figure 16 is that sodium bicarbonate concentration is schemed for the SEM of the nano silver powder produced when 0.1mol/l.
Specific embodiment
Embodiment 1
A kind of preparation method of spherical nano silver powder, includes the following steps: described in the present embodiment 1
(1) it is 0.1mol/L silver nitrate by 10ml concentration, is slowly dropped to the sodium bicarbonate that 30mL concentration is 0.05mol/L
In solution, the mixed solution containing white silver carbonate sediment is generated；
(2) 1.7g surfactant polyvinylpyrrolidone is then added in above-mentioned mixed liquor and sufficiently dissolves, will
To reaction solution be transferred to teflon lined hydrothermal reaction kettle in, the hydro-thermal reaction 5h under 180 DEG C of constant reaction temperatures,
Cooled to room temperature obtains nano silver colloidal sol；
(3) nano silver colloidal sol deionized water, ethyl alcohol are sufficiently washed, is then centrifuged for separating, by nano silver colloidal sol solution
It is evenly applied to clean glass substrate surface, spontaneously dries at room temperature, obtains nano silver powder.
In the present embodiment, the deionized water in the step (3) is secondary distilled water.
In the present embodiment, the volume of the hydrothermal reaction kettle in the step (2) is 100mL.
Make protective agent with surfactant PVP, is 0.1mol/L in silver nitrate concentration, sodium bicarbonate concentration is 0.05mol/
L, under conditions of the reaction time is 5h.In lower temperature, 130 DEG C, reaction is mostly in nucleation stage, and most of particle is also not
Complete regular morphology can be formed, the average grain diameter of particle is in 30nm or so, as shown in Figure 2；When temperature is increased to 160 DEG C, temperature
Degree is relatively still lower, and silver atoms are also not enough to provide enough anisotropic growth institutes to all nucleus while nucleation
The energy needed, i.e., in crystal growing process, the silver particles of small particle can along the biggish nucleating surface continued growth in part, from
And the irregular aggregate of pattern is formed, as shown in Figure 3；Temperature is increased to 180 degree, and at this temperature, atom is in forming core mistake
Saturated concentration is reached in journey, nucleation process carries out the surface accumulated growth along nucleus simultaneously, it is uniform to obtain particle diameter distribution
Ball shaped nano Argent grain, as shown in Figure 1；It is polyhedron pattern when reaction temperature is at 200 DEG C, average particle size increases fast
Speed, as shown in Figure 4；It is particle when reaction temperature is at 230 DEG C is irregular polyhedrons, particle diameter distribution is uneven, such as Fig. 5 institute
Show.Illustrate that properly increasing temperature is conducive to improve reaction speed, but when the temperature is excessively high, nucleation and growth course in rigid start
Occur simultaneously, particle increase cannot control and keep forming process complicated, to make the grain diameter to be formed and pattern all very not
Rule；Therefore, optimal reaction temperature is 180 DEG C.
It is 180 DEG C, silver nitrate concentration 0.1mol/l in reaction temperature, sodium bicarbonate concentration is 0.05mol/l, with surface
Activating agent PVP makees under conditions of protective agent.As shown in fig. 6, the reaction time is 2h, Ag particle is mostly with nucleation stage fine granularity
State exists, and pattern is irregular, mostly in 15~50nm or so；As shown in fig. 7, reaction 5h, the pattern of spherical nano silver are more advised
Then, particle diameter distribution is more uniform；As shown in figure 8, reaction 10h, the silver particles of small particle continue along the biggish seed surface in part
Growth, thus the nano-Ag particles size formed is extremely uneven；As shown in figure 9, little particle partial size increases, partial size after reaction 18h
It redistributes more uniform.It is possible thereby to infer the continuity with the reaction time during the reaction, small particles tachyauxesis is at big
Particle continues to extend to 18h or more with the reaction time, and particle can constantly increase, and finally obtained particle size will tend to
Unanimously.Therefore, optimum reacting time 5h.
PVP is a kind of common nonionic surface active agent, has special light based structures, is highly soluble in water, is receiving
It is widely used in the preparation process of rice silver particles, surfactant PVP is added can play the work of dispersion and protection in the reaction
With can inhibit the unconfined diffusion of nano silver particles and attachment, control each to different of particle in particle formation and growth course
Property growth, thus have larger impact for the formation and form of nanoparticle.It is 0.1mol/l, sodium bicarbonate in silver nitrate concentration
Concentration is 0.05mol/l, and reaction temperature is 180 DEG C, under conditions of the reaction time is 5h.As shown in Figure 10, when PVP is 0g,
The silver particles of generation will reunite, and the aggregate pattern of formation is irregular；As shown in figure 11,0.5gPVP is added, generation
Nanoscale silver is not single, and particle diameter distribution is uneven；As shown in figure 12,1.2gPVP is added and forms spherical nano silver particles, grain
Diameter is unevenly distributed；As shown in figure 13, particle diameter distribution is uniform when 1.7gPVP is added, and is single dispersing ball nano silver.It illustrates
With PVP increasing concentrations, dispersion effect is better, and closer to spherical, particle diameter distribution obtains more evenly pattern, thus 1.7gPVP compared with
Properly.
It is 180 DEG C, reaction time 5h in reaction temperature, the concentration of silver nitrate has very the formation of nano silver and its pattern
It is big to influence.As shown in figure 14, when the more a height of 0.4mol/l of AgNO3 concentration, nucleation rate and growth course occur simultaneously, and gained is received
There is triangle in meter Yin, rodlike, the various patterns such as spherical shape.As shown in figure 15, nanometer silver granuel when AgNO3 concentration is 0.025mol/l
Son is in irregular roundness plate-like, has part reunion, particle diameter distribution is uneven.As shown in figure 16, when sodium bicarbonate concentration is crossed greatly
When 0.1mol/l, it be easy to cause a large amount of reunions of particle.Therefore, select silver nitrate concentration for 0.1mol/l, sodium bicarbonate concentration
When for 0.05mol/l, the spherical nano-Ag particles of create-rule.
The above described is only a preferred embodiment of the present invention, not making any form to technical solution of the present invention
On limitation.According to the technical essence of the invention any simple modification to the above embodiments, equivalent variations and repair
Decorations, in the range of still falling within technical solution of the present invention.
Claims (3)
1. a kind of preparation method of spherical nano silver powder, which comprises the steps of:
(1) it is 0.1mol/L silver nitrate by 10ml concentration, is slowly dropped to the sodium bicarbonate solution that 30mL concentration is 0.05mol/L
In, generate the mixed solution containing white silver carbonate sediment；
(2) 1.7g surfactant polyvinylpyrrolidone is then added in above-mentioned mixed liquor and sufficiently dissolves, by what is obtained
Reaction solution is transferred in the hydrothermal reaction kettle of teflon lined, the hydro-thermal reaction 5h under 180 DEG C of constant reaction temperatures, natural
It is cooled to room temperature, obtains nano silver colloidal sol；
(3) nano silver colloidal sol deionized water, ethyl alcohol are sufficiently washed, is then centrifuged for separating, nano silver colloidal sol solution is uniform
Coated on clean glass substrate surface, spontaneously dries at room temperature, obtain nano silver powder.
2. a kind of preparation method of spherical nano silver powder according to claim 1, which is characterized in that the step (3)
In deionized water be secondary distilled water.
3. a kind of preparation method of spherical nano silver powder according to claim 2, which is characterized in that the step (2)
In hydrothermal reaction kettle volume be 100mL.
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| CN201811495475.7A CN109434130A (en) | 2018-12-07 | 2018-12-07 | A kind of preparation method of spherical nano silver powder |
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| CN201811495475.7A CN109434130A (en) | 2018-12-07 | 2018-12-07 | A kind of preparation method of spherical nano silver powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111663148A (en) * | 2020-06-11 | 2020-09-15 | 中南大学 | Method for preventing elemental sulfur from adhering to electrode surface in process of electrocatalytic reduction of sulfur dioxide |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111663148A (en) * | 2020-06-11 | 2020-09-15 | 中南大学 | Method for preventing elemental sulfur from adhering to electrode surface in process of electrocatalytic reduction of sulfur dioxide |
| CN111663148B (en) * | 2020-06-11 | 2021-06-25 | 中南大学 | Method for preventing elemental sulfur from adhering to electrode surface in process of electrocatalytic reduction of sulfur dioxide |
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Application publication date: 20190308 |