CN109482899A - A kind of surface modifying method of nano silver fibre - Google Patents
A kind of surface modifying method of nano silver fibre Download PDFInfo
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- CN109482899A CN109482899A CN201811497044.4A CN201811497044A CN109482899A CN 109482899 A CN109482899 A CN 109482899A CN 201811497044 A CN201811497044 A CN 201811497044A CN 109482899 A CN109482899 A CN 109482899A
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- nano silver
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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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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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
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Abstract
The present invention discloses a kind of surface modifying method of nano silver fibre, includes the following steps: that 10ml concentration is that be added drop-wise to 20mL concentration of ordinary dissolution be in the ascorbic acid of 0.1mol/L to 0.15mol/L AgNO3 by (1)；(2) addition 20mL concentration is 0.015mol/L Fe2 (SO4) 3 into above-mentioned solution；(3) surface active agent polyvinyl alcohol is then added in above-mentioned mixed liquor and sufficiently dissolves, obtained reaction solution is transferred in the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE) lining, hydro-thermal reaction 3h, cooled to room temperature at 180 DEG C；(4) products therefrom is sufficiently washed with ethyl alcohol, nano silver colloidal sol solution is obtained after high speed tabletop centrifuge is centrifuged, then it is dried in electric heating constant temperature ancient customs drying box, nano silver fibre is obtained after carrying out vibrating dispersion finally by ultrasonator, each crystal face of nano silver is coated by the molecule of surfactant.The surface modifying method prepares nano silver fibre using hydro-thermal method, is the nano silver fibre of dispersing agent synthesis high-purity using ascorbic acid as reducing agent, polyvinyl alcohol.
Description
Technical field
The present invention relates to the technical field of the surface modification technology of nano silver more particularly to a kind of surfaces of nano silver fibre
Method of modifying.
Background technique
Nano silver material is due to its special physics and chemical property, in catalysis, optics, electronics, areal stretch enhancing, life
The numerous areas such as object medicine and biosensor are all with a wide range of applications.These special performances of nano material and its ruler
It is very little, shape is closely related, thus morphology controllable to prepare nano material extremely important.Although the preparation method of nano material is increasingly
Diversification, but acquired achievement in terms of the controllable preparation of nano material is still very limited, therefore finds new synthetic method
Preparation size and shape is adjustable silver nanostructured to be had a very important significance and broad application prospect.
Since nanoparticle surface atomicity increases, crystalline field environment and combination can be different from inside, surface atom week
It encloses and lacks adjacent atom, there are many dangling bonds, have unsaturation, surface atom ligancy deficiency and high surface energy, make
These atoms are easily combined with other atoms and are settled out, therefore have very strong chemical activity.In the prior art, nano silver
Surface modifying method generally use be added surfactant come formed with certain pattern and guidance growth nanoparticle；And
All there are certain deficiencies to a certain extent to the method that nano silver is modified in the prior art, such as physical method preparation
Nano silver the high requirements on the equipment, thus preparation cost is relatively high, many reducing agents used in chemical method are toxic, need
A large amount of surfactant protection, 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, the surface for providing a kind of nano silver fibre is modified
The surface modifying method of method, the nano silver fibre prepares nano silver fibre using hydro-thermal method, using ascorbic acid as reducing agent, gathers
Vinyl alcohol is dispersing agent, and the nano silver that the nano silver fibre of formation in patterns such as nano wire or nanometer rods, can synthesize high-purity is fine
Dimension, with biggish reactant concentration, the reaction time is short, and low in cost, pattern is easy to regulate and control, excellent to reaction reagent environment
Change, surface modification is excellent, has widened application range.
The technical solution adopted by the present invention to solve the technical problems is: a kind of surface modifying method of nano silver fibre,
Include the following steps:
It (1) is ascorbic acid that 0.15mol/L AgNO3 is added drop-wise to that 20mL concentration of ordinary dissolution is 0.1mol/L by 10ml concentration
In；
(2) addition 20mL concentration is 0.015mol/L Fe2 (SO4) 3 into above-mentioned solution；
(3) surface active agent polyvinyl alcohol is then added in above-mentioned mixed liquor and sufficiently dissolves, the reaction solution that will be obtained
It is transferred in the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE) lining, hydro-thermal reaction 3h, cooled to room temperature at 180 DEG C；
(4) products therefrom is sufficiently washed with ethyl alcohol, obtains nanometer after high speed tabletop centrifuge is centrifuged
Then silver sol solution is dried in electric heating constant temperature ancient customs drying box, carry out vibrating dispersion finally by ultrasonator
After obtain nano silver fibre, each crystal face of nano silver is coated by the molecule of surfactant.
Further, the volume of the hydrothermal reaction kettle is 100mL.
Further, the additional amount of the surface active agent polyvinyl alcohol is 2.25g.
In conclusion the surface modifying method of nano silver fibre of the invention prepares nano silver fibre using hydro-thermal method, with
Ascorbic acid is reducing agent, and polyvinyl alcohol is dispersing agent, and the nano silver fibre of formation can be closed in patterns such as nano wire or nanometer rods
At the nano silver fibre of high-purity, with biggish reactant concentration, the reaction time is short, low in cost, and pattern is easy to regulate and control,
To reaction reagent environment optimization, surface modification is excellent, has widened application range.
Detailed description of the invention
Fig. 1 is the scanning electron microscope enlarged drawing of nano silver fibre low range；
Fig. 2 is the powerful scanning electron microscope enlarged drawing of nano silver fibre；
Fig. 3 is Fe3+The scanning electron microscope enlarged drawing of nano silver fibre is generated when concentration is 0；
Fig. 4 is Fe3+The scanning electron microscope enlarged drawing of nano silver fibre is generated when concentration is 0.006mol/L；
Fig. 5 is Fe3+The scanning electron microscope enlarged drawing of nano silver fibre is generated when concentration is 0.03mol/L；
The scanning electron microscope enlarged drawing of nano silver fibre is generated when Fig. 6 is 140 DEG C of reaction temperature；
The scanning electron microscope enlarged drawing of nano silver fibre is generated when Fig. 7 is 160 DEG C of reaction temperature；
The scanning electron microscope enlarged drawing of nano silver fibre is generated when Fig. 8 is 200 DEG C of reaction temperature；
Fig. 9 is the scanning electron microscope enlarged drawing for being 1h generation nano silver fibre the reaction time；
Figure 10 is the scanning electron microscope enlarged drawing for being 2h generation nano silver fibre the reaction time；
Figure 11 is the scanning electron microscope enlarged drawing for being 4h generation nano silver fibre the reaction time.
Specific embodiment
Embodiment 1
A kind of surface modifying method of nano silver fibre, includes the following steps: described in the present embodiment 1
It (1) is ascorbic acid that 0.15mol/L AgNO3 is added drop-wise to that 20mL concentration of ordinary dissolution is 0.1mol/L by 10ml concentration
In；
(2) addition 20mL concentration is 0.015mol/L Fe2 (SO4) 3 into above-mentioned solution；
(3) surface active agent polyvinyl alcohol is then added in above-mentioned mixed liquor and sufficiently dissolves, the reaction solution that will be obtained
It is transferred in the hydrothermal reaction kettle of polytetrafluoroethylene (PTFE) lining, hydro-thermal reaction 3h, cooled to room temperature at 180 DEG C；
(4) products therefrom is sufficiently washed with ethyl alcohol, obtains nanometer after high speed tabletop centrifuge is centrifuged
Then silver sol solution is dried in electric heating constant temperature ancient customs drying box, carry out vibrating dispersion finally by ultrasonator
After obtain nano silver fibre, each crystal face of nano silver is coated by the molecule of surfactant.
In the present embodiment, the volume of the hydrothermal reaction kettle is 100mL.
In the present embodiment, the additional amount of the surface active agent polyvinyl alcohol is 2.25g.
As shown in Figure 1, the length of nano silver fibre is up to several hundred um；As shown in Figure 2, the pattern of nano silver fibre is single,
Purity is higher, and for diameter probably in 150nm or so, particle diameter distribution is more uniform.
As shown in figure 3, in Fe3+When concentration is 0, reaction product is mainly nano-Ag particles, there is triangle, rodlike, more
Face body shape, spheric granules cannot form complete regular morphology, not the formation of nano silver fibre, and nano silver particles are averaged
Partial size is in 100-300nm or so；As shown in figure 4, in Fe3+When concentration is 0.006mol/L, there are a large amount of silver nanowiress and nano silver
Particle generates, and the diameter of nano silver fibre is about the silver nanowires of 90nm；As shown in Fig. 2, when concentration continues to rise to
When 0.015mol/L, product is mainly the single nano silver fibre of rule of 150nm or so；As shown in figure 5, working as Fe3+Concentration reaches
When 0.03mol/L, nano silver fibre and silver nanoparticle rectangular tab that diameter is 200-400nm or so are obtained.Fe3+Concentration can be adjusted
The nano silver particles pattern main cause that control generates is: due to Fe3+Oxide etch effect, i.e., silver due to itself characteristic and
The stability of its twin structure, twin seed is etched into monocrystalline seed by oxide etch by iron ion, with iron concentration
Increase, oxide etch effect reinforces to a large amount of twin seed easy to form, and twin seed is gradually etched to monocrystalline
Seed, along the longitudinal constantly growth of crystal face, forms nano silver fibre under the action of PVA.The reason of changes of diameter is: iron from
There is a large amount of etch areas in etching in son, relatively high in surface free energy here, although due to PVA being suction-operated,
But a large amount of twin seeds are very fast in longitudinal growth, and nucleus growth is accelerated, thus radial dimension increases.Thus we are it can be concluded that knot
By: increase Fe3+Concentration nano silver fibre diameter may be implemented change within the scope of 90-300nm.The size wave of nano silver fibre
Dynamic range increases, while also the properties such as its photoelectricity can be allowed to change, to pass through Fe3+The regulation of concentration, to obtain
The nano silver fibre needed.Therefore, work as Fe3+Concentration be 0.015mol/L advantageously form high-purity nano silver fibre it is raw
At.
As shown in fig. 6, reduction rate is slower when compared with 140 DEG C of low reaction temperatures, the monocrystalline seed amount of generation is less,
It is slower to continue longitudinal generation nano silver fibre speed.The product of generation has silver nano-grain, a small amount of nano silver fibre and Yin Na
Rice stick, nano-Ag particles partial size is larger, and nano silver fibre diameter is in 100nm or so, and nanorod diameter is 500 or so；Such as Fig. 7
Shown, when reaction temperature is increased to 160 DEG C, primary product is a large amount of nano silver fibres and a small amount of particles, and diameter is unevenly distributed,
Substantially between 100-400nm, length is in 20u or more；As shown in Fig. 2, reaction temperature is increased to 180 DEG C, in this temperature
Under, the monocrystalline seed of generation has reached saturated concentration, and it is raw along the surface longitudinal of seed to generate the progress simultaneously of monocrystalline sub-processes
Long, obtaining diameter is 150nm or so and distribution uniform, and length reaches the silver nanowires of several hundred um；As shown in figure 8, when reaction temperature
It is that nano silver fibre and more nanoparticle agglomerates body, average particle size are larger when spending 200 DEG C.So as to analyze to obtain,
At a lower temperature, the energy that system provides is not enough to provide more monocrystalline seed along longitudinal growth, thus, it properly increases
Temperature is conducive to improve reduction reaction speed, promotes to make twin seed along longitudinal growth with appropriate speed, but when the temperature is excessively high,
Initial reaction stage with regard to when generate a large amount of twin seed, while twin seed occurs simultaneously along crystal face longitudinal growth process, instead
Answer rate excessive, to make product morphology that cannot control and keep pattern irregular, thus the nano silver fibre partial size formed point
Cloth is uneven, shows that temperature is the synthesis of 180 DEG C or so the control for being conducive to pattern and nano silver fibre.
As shown in figure 9, the reaction time is 1h, nano silver shows to go back unreacted complete in particulate and unintelligible；Such as
Shown in Figure 10, reaction time 2h, predominantly nano silver fibre and silver nanoparticle molecule, nano silver fibre diameter are 70nm left
The right side, length are 5um or so；As shown in Fig. 2, the reaction time is 3h, the nano silver fibre of formation is of uniform size, diameter 150nm
Left and right and distribution uniform, length reach the nano silver fibre of several hundred um；As shown in figure 11, reaction time 4h, nano silver are average
Partial size is about 250nm or so.It is possible thereby to infer during the reaction, twin seed is generated before this, with prolonging for reaction time
Long, the twin seed constantly restored is along crystal face longitudinal growth, so that it be made to generate nano silver fibre.Show to select the reaction time
It is preferable for 3h.
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 surface modifying method of nano silver fibre, which comprises the steps of:
It (1) is that be added drop-wise to 20mL concentration of ordinary dissolution be in the ascorbic acid of 0.1mol/L to 0.15mol/L AgNO3 by 10ml concentration；
(2) addition 20mL concentration is 0.015mol/L Fe2 (SO4) 3 into above-mentioned solution；
(3) surface active agent polyvinyl alcohol is then added in above-mentioned mixed liquor and sufficiently dissolves, obtained reaction solution is shifted
In the hydrothermal reaction kettle served as a contrast to polytetrafluoroethylene (PTFE), hydro-thermal reaction 3h, cooled to room temperature at 180 DEG C；
(4) products therefrom is sufficiently washed with ethyl alcohol, it is molten to obtain nano silver after high speed tabletop centrifuge is centrifuged
Then sol solution is dried in electric heating constant temperature ancient customs drying box, obtain after carrying out vibrating dispersion finally by ultrasonator
To nano silver fibre, each crystal face of nano silver is coated by the molecule of surfactant.
2. a kind of surface modifying method of nano silver fibre according to claim 1, which is characterized in that the hydro-thermal reaction
The volume of kettle is 100mL.
3. a kind of surface modifying method of nano silver fibre according to claim 2, which is characterized in that the surface is living
Property agent polyvinyl alcohol additional amount be 2.25g.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811497044.4A CN109482899A (en) | 2018-12-07 | 2018-12-07 | A kind of surface modifying method of nano silver fibre |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811497044.4A CN109482899A (en) | 2018-12-07 | 2018-12-07 | A kind of surface modifying method of nano silver fibre |
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| CN109482899A true CN109482899A (en) | 2019-03-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116372181A (en) * | 2023-06-07 | 2023-07-04 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116372181A (en) * | 2023-06-07 | 2023-07-04 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
| CN116372181B (en) * | 2023-06-07 | 2023-09-05 | 长春黄金研究院有限公司 | Rod-shaped silver powder and preparation method thereof |
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