CN107598183A - A kind of magnanimity preparation method of nano-Ag particles - Google Patents
A kind of magnanimity preparation method of nano-Ag particles Download PDFInfo
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Abstract
The invention discloses a kind of magnanimity preparation method of nano-Ag particles, the described method comprises the following steps：S1, surface cleaning is carried out to Si powder, remove the oxide layer on Si powder surface；S2, by after surface cleaning Si powder dry；S3, the Si powder after drying added in the HF aqueous solution under normal temperature, ultrasound, stirring are to well mixed；Under S4, normal temperature and pressure, by AgNO3Solution is added dropwise in Si powder/HF aqueous solution, and ultrasound, stirring, Si powder are etched oxidation, Ag ion reductions generation Nano Silver, formation Nano silver solution；S5, after question response certain time, by Nano silver solution centrifugal treating, isolate nano-Ag particles；S6, nano-Ag particles are cleaned with ethanol solution, and nano-Ag particles are preserved in vacuum or ethanol solution.The present invention using micron order silica flour is raw material, cheap and can largely obtain；Reaction condition is simple, can be prepared under normal temperature and pressure；Prepared nano-Ag particles size is between 50~100nm, favorable dispersibility.
Description
Technical field
The present invention relates to nano-metal particle preparing technical field, is prepared more particularly to a kind of magnanimity of nano-Ag particles
Method.
Background technology
In modern industrial production, nano metal material has extensively in fields such as optics, electronics, biology, Industrial Catalysis
Application.In recent years, Nano Silver is due to good characteristic electron, optical characteristics, catalysis characteristics, mechanical property, Yi Jisheng
Excellent antibiotic property, bio-compatibility etc. in thing scientific domain, in microelectronic material, electrocondution slurry, optical element, sensory device
The fields such as material, bio-medical material, chemical catalyst, sewage disposal, high performance electrode material have a wide range of applications, its also into
For the study hotspot of new function material.
The preparation method of conventional nano-Ag particles is broadly divided into physics and the major class of chemical method two, and physical method mainly has
Physical crushing method, mechanical attrition method and magnetron sputtering method etc., chemical method mainly have chemical reduction method, photocatalytic method, electroreduction
Method, ultrasonic reducing process, gas-liquid two phase process, sol-gel process, microemulsion method etc., compared to physical method, chemical method pair is set
Standby less demanding, manipulation convenience, controllability are higher, therefore can be widely used, but existing chemical method still suffers from system
The shortcomings of causing this height, reaction condition whard to control.
Therefore, for above-mentioned technical problem, it is necessary to provide a kind of magnanimity preparation method of nano-Ag particles.
The content of the invention
In view of this, it is an object of the invention to provide a kind of magnanimity preparation method of nano-Ag particles, this method are practical
It is feasible, and condition is simple, is easy to control.
To achieve these goals, technical scheme provided in an embodiment of the present invention is as follows：
A kind of magnanimity preparation method of nano-Ag particles, the described method comprises the following steps：
S1, surface cleaning is carried out to Si powder, remove the oxide layer on Si powder surface；
S2, by after surface cleaning Si powder dry；
S3, the Si powder after drying added in the HF aqueous solution under normal temperature, ultrasound, stirring are to well mixed；
Under S4, normal temperature and pressure, by AgNO3Solution is added dropwise in Si powder/HF aqueous solution, and ultrasound, stirring, Si powder are etched
Oxidation, Ag ion reductions generation Nano Silver, forms Nano silver solution；
S5, after question response certain time, by Nano silver solution centrifugal treating, isolate nano-Ag particles.
As a further improvement on the present invention, " carrying out surface cleaning to Si powder " in the step S1 is specially：
Si powder is put into ionized water and dilute HF and carries out surface cleaning.
As a further improvement on the present invention, the step S1 is specially：
Si powder is put into ionized water and dilute HF of mass percent 0.1~10% and carries out surface cleaning, removes SiO2Oxygen
Change layer, cleaning time is 60s~1200s, and cleaning temp is 5 DEG C~90 DEG C.
As a further improvement on the present invention, the drying atmosphere in the step S2 is vacuum atmosphere or N2Protective atmosphere,
Drying temperature is 80 DEG C~200 DEG C.
As a further improvement on the present invention, the step S3 is specially：
Si powder after drying is added under normal temperature in the HF aqueous solution of mass percent 5%~50%, ultrasound, stirring 50s
~200s is to well mixed.
As a further improvement on the present invention, the step S4 is specially：
Under normal temperature and pressure, by the AgNO that concentration is 0.0075mol/L~0.01mol/L3Si powder/HF water is added dropwise in solution
In solution, ultrasound, stirring, the reaction time is 5min~30min, the oxidation until Si powder is etched, Ag ion reductions generation nanometer
Silver, form Nano silver solution.
As a further improvement on the present invention, the step S5 is specially：
Nano silver solution is placed in a centrifuge, separation of solid and liquid is carried out with constant rotational speed, isolates nano-Ag particles.
As a further improvement on the present invention, also include after the step S5：
S6, nano-Ag particles are cleaned with ethanol solution, and nano-Ag particles are carried out in vacuum or ethanol solution
Preserve.
As a further improvement on the present invention, the Si powder be solar energy-level silicon wafer or electron level silicon chip warp cutting after
The micron-stage sheet-like Si powder arrived.
The beneficial effects of the invention are as follows：
The use of micron order silica flour is raw material, it is cheap and can largely obtain, reduce process costs；
Reaction condition is simple, can be prepared under normal temperature and pressure；
Prepared nano-Ag particles size is between 50~100nm, favorable dispersibility, not comprising other impurities.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments described in invention, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the particular flow sheet of the magnanimity preparation method of nano-Ag particles in the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of micron-stage sheet-like Si powder in the present invention；
Fig. 3 is the scanning electron microscope (SEM) photograph of nano-Ag particles prepared in the embodiment of the present invention 1；
Fig. 4 is the particle size distribution range block diagram of nano-Ag particles prepared in the embodiment of the present invention；
Fig. 5 is the X ray diffracting spectrum of nano-Ag particles prepared in the embodiment of the present invention.
Embodiment
In order that those skilled in the art more fully understand the technical scheme in the present invention, below in conjunction with of the invention real
The accompanying drawing in example is applied, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described implementation
Example only part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, should all belong to protection of the present invention
Scope.
Join shown in Fig. 1, the invention discloses a kind of magnanimity preparation method of nano-Ag particles, this method includes following step
Suddenly：
S1, surface cleaning is carried out to Si powder, remove the oxide layer on Si powder surface；
S2, by after surface cleaning Si powder dry；
S3, the Si powder after drying added in the HF aqueous solution under normal temperature, ultrasound, stirring are to well mixed；
Under S4, normal temperature and pressure, by AgNO3Solution is added dropwise in Si powder/HF aqueous solution, and ultrasound, stirring, Si powder are etched
Oxidation, Ag ion reductions generation Nano Silver, forms Nano silver solution；
S5, after question response certain time, by Nano silver solution centrifugal treating, isolate nano-Ag particles.
Further, step S5 also includes：
S6, nano-Ag particles are cleaned with ethanol solution, and nano-Ag particles are carried out in vacuum or ethanol solution
Preserve.
The present invention can at normal temperatures and pressures be carried out, operated using the technology of " silicon auxiliary etch reduction prepares Nano Silver "
Convenient, cost is relatively low.Each step in nano-Ag particles preparation method of the present invention is described in detail below.
First, Si powder is put into ionized water and dilute HF, surface cleaning is carried out to Si powder, removes the SiO on Si powder surface2Oxygen
Change layer.
Preferably, the Si powder in the present invention is obtained micron order after solar energy-level silicon wafer or the cutting of electron level silicon chip warp
Sheet Si powder, its configuration of surface is as shown in Fig. 2 HF mass percent 0.1~10%, cleaning time are 60s~1200s, clearly
Clean temperature is 5 DEG C~90 DEG C.
Then, Si powder is placed in vacuum atmosphere oven or N2Dried in special atmosphere oven, to avoid SiO2The generation of oxide layer.
Preferably, drying temperature is 80 DEG C~200 DEG C.
Then, the Si powder after drying is added in the HF aqueous solution under normal temperature, ultrasound, stirred to well mixed.Preferably,
The HF aqueous solution is the HF aqueous solution of mass percent 5%~50%, and ultrasound, mixing time are 50s~200s.
Afterwards, under normal temperature (20 DEG C ± 5 DEG C) normal pressure, by AgNO3Solution is added dropwise in Si powder/HF aqueous solution, ultrasound, is stirred
Mix, silver ion obtains electronics from Si powder surface and is reduced into silver-colored simple substance, and forms a large amount of galactic nucleus and be attached to Si powder surface, while Si
Powder is etched oxidation, and final Si powder is consumed, obtains nano-Ag particles and be suspended in solution.
Preferably, AgNO3The concentration of solution is 0.0075mol/L~0.01mol/L, and the oxidation of Si powder, Ag ion reductions are anti-
It is 5min~30min between seasonable.
Then, after waiting solution fully to react, Nano silver solution is placed in a centrifuge, solid-liquid point is carried out with constant rotational speed
From isolating nano-Ag particles.
Finally, nano-Ag particles are cleaned repeatedly with ethanol solution, in order to avoid the nano-Ag particles and air of preparation
Contact, nano-Ag particles should be preserved in vacuum or ethanol solution.
Preferable AgNO in this present invention3Solution concentration is 0.0075mol/L~0.01mol/L, works as AgNO3Concentration is more than
During 0.01mol/L, AgNO can be caused3It can not completely react, cause solution waste, add process costs；Work as AgNO3Concentration
During less than 0.0075mol/L, Ag ions can not fall the complete etching reaction of silica flour in silicon Si powder/HF aqueous solution, cause to separate
Contain silica flour pollutant in nano-Ag particles out, the nano-Ag particles of preparation are not pure.
With reference to embodiment, the invention will be further described.
Embodiment 1：
A kind of magnanimity preparation method of nano-Ag particles, comprises the following steps：
S1, Si powder is put into ionized water and mass percent 5%HF solution, surface cleaning is carried out to Si powder, removes Si
The SiO on powder surface2Oxide layer, cleaning time 600s, cleaning temp are 50 DEG C；Then cleaned 4 times using deionized water；
S2, the wet Si powder after cleaning is put into vacuum atmosphere oven (or N2In special atmosphere oven), under the conditions of 150 DEG C
Dry stand-by；
S3, by after drying Si powder add normal temperature under mass percent 45% the HF aqueous solution in, ultrasound, stirring 200s extremely
It is well mixed；
S4, the AgNO by concentration for 0.009mol/L3Solution, with constant rate of addition, above-mentioned Si powder/HF is added dropwise
Reacted in the aqueous solution, reaction time 15min, ultrasound, stirring are needed in course of reaction；
After S5, question response terminate, Nano silver solution is placed in a centrifuge, carried out with 8000r/min rotating speeds centrifugation 5min
Separation of solid and liquid, isolate nano-Ag particles；
S6, with ethanol solution clean nano-Ag particles, be repeated 3 times, in order to avoid prepared nano-Ag particles with
Air contact, most nano-Ag particles are preserved in vacuum or ethanol solution at last.
Join shown in Fig. 3~Fig. 5, the scanning electron microscope (SEM) photograph of nano-Ag particles, particle size distribution range post respectively in the present embodiment
Shape figure and X ray diffracting spectrum, it is found that the size of nano-Ag particles is between 50~100nm, and purity is high, does not include
Other impurities.
Embodiment 2：
A kind of magnanimity preparation method of nano-Ag particles, comprises the following steps：
S1, Si powder is put into ionized water and mass percent 3%HF solution, surface cleaning is carried out to Si powder, removes Si
The SiO on powder surface2Oxide layer, cleaning time 60s, cleaning temp are 90 DEG C；Then cleaned 3 times using deionized water；
S2, the wet Si powder after cleaning is put into vacuum atmosphere oven (or N2In special atmosphere oven), under the conditions of 100 DEG C
Dry stand-by；
S3, by after drying Si powder add normal temperature under mass percent 20% the HF aqueous solution in, ultrasound, stirring 100s extremely
It is well mixed；
S4, the AgNO by concentration for 0.0075mol/L3Solution, with constant rate of addition, be added dropwise above-mentioned Si powder/
Reacted in the HF aqueous solution, reaction time 5min, ultrasound, stirring are needed in course of reaction；
After S5, question response terminate, Nano silver solution is placed in a centrifuge, carried out with 8000r/min rotating speeds centrifugation 10min
Separation of solid and liquid, isolate nano-Ag particles；
S6, with ethanol solution clean nano-Ag particles, be repeated 3 times, in order to avoid prepared nano-Ag particles with
Air contact, most nano-Ag particles are preserved in vacuum or ethanol solution at last.
In the present embodiment the scanning electron microscope (SEM) photograph of nano-Ag particles, particle size distribution range block diagram and X ray diffracting spectrum with
Embodiment 1 is essentially identical.
Embodiment 3：
A kind of magnanimity preparation method of nano-Ag particles, comprises the following steps：
S1, Si powder is put into ionized water and mass percent 10%HF solution, surface cleaning is carried out to Si powder, removes Si
The SiO on powder surface2Oxide layer, cleaning time 1200s, cleaning temp are 5 DEG C；Then cleaned 5 times using deionized water；
S2, the wet Si powder after cleaning is put into vacuum atmosphere oven (or N2In special atmosphere oven), under the conditions of 200 DEG C
Dry stand-by；
S3, by after drying Si powder add normal temperature under mass percent 50% the HF aqueous solution in, ultrasound, stirring 200s extremely
It is well mixed；
S4, the AgNO by concentration for 0.01mol/L3Solution, with constant rate of addition, above-mentioned Si powder/HF is added dropwise
Reacted in the aqueous solution, reaction time 30min, ultrasound, stirring are needed in course of reaction；
After S5, question response terminate, Nano silver solution is placed in a centrifuge, carried out with 8000r/min rotating speeds centrifugation 20min
Separation of solid and liquid, isolate nano-Ag particles；
S6, with ethanol solution clean nano-Ag particles, be repeated 5 times, in order to avoid prepared nano-Ag particles with
Air contact, most nano-Ag particles are preserved in vacuum or ethanol solution at last.
In the present embodiment the scanning electron microscope (SEM) photograph of nano-Ag particles, particle size distribution range block diagram and X ray diffracting spectrum with
Embodiment 1 is essentially identical.
As can be seen from the above technical solutions, the invention has the advantages that：
The use of micron order silica flour is raw material, it is cheap and can largely obtain, reduce process costs；
Reaction condition is simple, can be prepared under normal temperature and pressure；
Prepared nano-Ag particles size is between 50~100nm, favorable dispersibility, not comprising other impurities.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Any reference in claim should not be considered as to the involved claim of limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (9)
1. the magnanimity preparation method of a kind of nano-Ag particles, it is characterised in that the described method comprises the following steps：
S1, surface cleaning is carried out to Si powder, remove the oxide layer on Si powder surface；
S2, by after surface cleaning Si powder dry；
S3, the Si powder after drying added in the HF aqueous solution under normal temperature, ultrasound, stirring are to well mixed；
Under S4, normal temperature and pressure, by AgNO3Solution is added dropwise in Si powder/HF aqueous solution, and ultrasound, stirring, Si powder are etched oxidation,
Ag ion reductions generate Nano Silver, form Nano silver solution；
S5, after question response certain time, by Nano silver solution centrifugal treating, isolate nano-Ag particles.
2. the magnanimity preparation method of a kind of nano-Ag particles according to claim 1, it is characterised in that in the step S1
" carrying out surface cleaning to Si powder " is specially：
Si powder is put into ionized water and dilute HF and carries out surface cleaning.
A kind of 3. magnanimity preparation method of nano-Ag particles according to claim 2, it is characterised in that the step S1 tools
Body is：
Si powder is put into ionized water and dilute HF of mass percent 0.1~10% and carries out surface cleaning, removes SiO2Oxide layer,
Cleaning time is 60s~1200s, and cleaning temp is 5 DEG C~90 DEG C.
4. the magnanimity preparation method of a kind of nano-Ag particles according to claim 1, it is characterised in that in the step S2
Drying atmosphere be vacuum atmosphere or N2Protective atmosphere, drying temperature are 80 DEG C~200 DEG C.
A kind of 5. magnanimity preparation method of nano-Ag particles according to claim 1, it is characterised in that the step S3 tools
Body is：
Si powder after drying is added under normal temperature in the HF aqueous solution of mass percent 5%~50%, ultrasound, stirring 50s~
200s is to well mixed.
A kind of 6. magnanimity preparation method of nano-Ag particles according to claim 5, it is characterised in that the step S4 tools
Body is：
Under normal temperature and pressure, by the AgNO that concentration is 0.0075mol/L~0.01mol/L3Si powder/HF aqueous solution is added dropwise in solution
In, ultrasound, stirring, the reaction time is 5min~30min, the oxidation until Si powder is etched, Ag ion reductions generation Nano Silver, shape
Into Nano silver solution.
A kind of 7. magnanimity preparation method of nano-Ag particles according to claim 1, it is characterised in that the step S5 tools
Body is：
Nano silver solution is placed in a centrifuge, separation of solid and liquid is carried out with constant rotational speed, isolates nano-Ag particles.
8. the magnanimity preparation method of a kind of nano-Ag particles according to claim 1, it is characterised in that after the step S5
Also include：
S6, nano-Ag particles are cleaned with ethanol solution, and nano-Ag particles are preserved in vacuum or ethanol solution.
9. the magnanimity preparation method of a kind of nano-Ag particles according to claim 1, it is characterised in that the Si powder is too
The micron-stage sheet-like Si powder obtained after positive energy level silicon wafer or electron level silicon chip warp cutting.
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Cited By (2)
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| CN113118450A (en) * | 2019-12-31 | 2021-07-16 | 拓米(成都)应用技术研究院有限公司 | Preparation method of nano-scale and submicron-scale metal powder |
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