CN108436105A - A kind of overlength nano-silver thread dispersion liquid and preparation method thereof - Google Patents
A kind of overlength nano-silver thread dispersion liquid and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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- 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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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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Abstract
The invention discloses a kind of preparation methods of overlength nano-silver thread dispersion liquid, include the following steps：（1）Prepare solution A, B solution and C solution；（2）AB mixed solutions and ABC mixed solutions are prepared successively；（3）By step（2）The ABC mixed solutions of gained pour into autoclave, it is bubbled rear enclosed autoclave with high-purity gas, autoclave is heated to certain temperature, reaction is after a certain period of time up to overlength nano-silver thread dispersion liquid, with high-purity gas to autoclave pressurization during reaction so that pressure is certain value in autoclave.The present invention obtains better effect by mixing two kinds of polyalcohols, meanwhile, the introducing of deionized water reduces experimental implementation difficulty so that various drug dissolvings are quicker.By replacing a part of polyalcohol with deionized water, the cost of experiment is reduced under conditions of not changing experimental result, greatly reduces the viscosity of reagent, the collection for dispersion liquid later reduces difficulty.
Description
Technical field
The invention belongs to nano material technical field of producing, and in particular to a kind of overlength nano-silver thread dispersion liquid and its
Preparation method.
Background technology
With the fast development of electronic technology, electronic industry proposes more more towards development in pluralism, while to material
High performance requirement.In this background, nano material receives the extensive of all circles since it is unique to the performance of traditional material
Concern.Metal nano material is an important branch of nano material, and unique performance makes it be widely used in life
Every field.The powder such as iron cobalt are applied to military high-performance stealth material since it has electromagnetic wave special absorption
And shielding material etc.；Copper nano can be used as effective catalyst or be applied to electrocondution slurry；Nanometer ferromagnetic material is then since it is full
It is big with the intensity of magnetization, the capacity of various soft or hard disks is substantially increased, is had in medical instrument, magnetic conduction slurry, shielding material etc.
Extensive use；Also noble metal nanometer material has extensive use in efficient catalytic, biochemistry, dyeing etc..
With the appearance of the flexible transparent electrode material for substituting ITO glass, material supply section scholar, which has paid, largely to exert
Power is to find a kind of better conductive material while possess good electric conductivity and light transmittance.Nano silver wire material is with its superelevation
Electric conductivity and be easy prepare etc. characteristics and be concerned, become prepare flexible transparent electrode preferred material.
Overlength nano-silver thread reaches 100-300nm since its diameter is big, applies to when nano silver transparent conductive film mist degree very
Greatly, bad dispersibility not can operate with mobile phone etc. and require high touch panel to apparent, but due to its big diameter, high transmission
Rate, electric conductivity is fine, can operate with the transparent electrodes such as LED, solar cell.The generally long 100- of long nano-silver thread reported
200um, and preparation process is unstable, there is reunion, it is big by such environmental effects.
Invention content
The present invention provides a kind of overlength nano-silver thread dispersion liquids and preparation method thereof, solve the system of overlength nano-silver thread
Standby problem, and soilless sticking in preparation process, substantially not by such environmental effects, favorable repeatability, material is easy to get, at low cost
It is honest and clean.
The purpose of the present invention is what is realized in the following manner：
A kind of preparation method of overlength nano-silver thread dispersion liquid, includes the following steps：
（1）It is formulated as follows solution：
Solution A：Silver nitrate is dissolved in the mixed solution of polynary alcohol and water；
B solution：Polyethylene pyrrole network alkanone is dissolved in the mixed solution of polynary alcohol and water；
C solution：Copper chloride solution；
（2）Solution A is added in B solution under to stirring condition, obtains AB mixed solutions, after AB mixed solutions are stirred evenly, to
C solution is slowly added dropwise in AB mixed solutions, ABC mixed solutions are obtained after stirring evenly；
（3）By step（2）The ABC mixed solutions of gained pour into autoclave, rear enclosed autoclave are bubbled with high-purity gas, by high pressure
Kettle is heated to certain temperature, and reaction is after a certain period of time up to overlength nano-silver thread dispersion liquid, with high-purity gas to height during reaction
Press kettle pressurization so that pressure is certain value in autoclave.
The polyalcohol is the mixture of ethylene glycol and glycerine, and ethylene glycol and glycerine are mixed with arbitrary proportion.
In the mixed solution of the polynary alcohol and water, the mass ratio of polyalcohol and water is（1:0.5）-（0.5:1）.
The liquor capacity ratio A:B:C=70:70:（1-5）.
Silver nitrate concentration is 0.05mol/L-0.09mol/L in solution A.
Polyvinylpyrrolidoneconcentration concentration is 0.25mol/L-0.45mol/L in B solution, and the K values of polyvinylpyrrolidone are
120。
Copper chloride concentration is 0.025 mol/L -0.030mol/L in C solution.
The high-purity gas is helium, neon, argon gas or nitrogen, and when reaction, the pressure in autoclave is 0.5MP-15MP.
The heating rate of autoclave when heated is 10 DEG C -200 DEG C/h, and the reaction temperature in autoclave is 150 DEG C -250
DEG C, reaction time 5-24h.
A kind of overlength nano-silver thread dispersion liquid prepared by the preparation method of above-mentioned overlength nano-silver thread dispersion liquid.
Compared with the existing technology, beneficial effects of the present invention are：The present invention realizes overlength nano silver using the above scheme
The preparation of line, and preparation process soilless sticking, small by such environmental effects, preparation process is controllable.
The present invention obtains better effect by mixing two kinds of polyalcohols, meanwhile, the introducing of deionized water reduces reality
Test operation difficulty so that various drug dissolvings are quicker.By replacing a part of polyalcohol with deionized water, do not changing reality
Testing under conditions of result reduces the cost of experiment, greatly reduces the viscosity of reagent, for after the collection of dispersion liquid reduce
Difficulty.The present invention is tested using pressurization autoclave, can use higher reaction temperature, higher pressure so that reaction is molten
There is liquid lower surface tension and viscosity, better wellability, less reunion can thoroughly be prevented by controlling reaction condition
Reunite.The present invention is bubbled by rare gas, the most of air dissolved in solution has been discharged, then real by sealing reaction condition
Now to the isolation of external environment, so that experiment is not substantially by such environmental effects.
Specific implementation mode
In order to realize that the performance, the present invention provide two embodiments, the embodiment of the present invention is only the excellent of the present invention
Select embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
The concentration of polyvinylpyrrolidone is with the densimeter of polyvinylpyrrolidone monomer, polyvinylpyrrolidine in the present invention
The molecular weight of one monomers is 111.
A kind of preparation method of overlength nano-silver thread dispersion liquid, includes the following steps：
（1）It is formulated as follows solution：
Solution A：Silver nitrate is dissolved in the mixed solution of polynary alcohol and water；
B solution：Polyethylene pyrrole network alkanone is dissolved in the mixed solution of polynary alcohol and water；
C solution：Copper chloride solution；
（2）Solution A is added in B solution under to stirring condition, obtains AB mixed solutions, after AB mixed solutions are stirred evenly, to
C solution is slowly added dropwise in AB mixed solutions, ABC mixed solutions are obtained after stirring evenly；
（3）By step（2）The ABC mixed solutions of gained pour into autoclave, rear enclosed autoclave are bubbled with high-purity gas, by high pressure
Kettle is heated to certain temperature, and reaction is after a certain period of time up to overlength nano-silver thread dispersion liquid, with high-purity gas to height during reaction
Press kettle pressurization so that pressure is certain value in autoclave.
The polyalcohol is the mixture of ethylene glycol and glycerine, and ethylene glycol and glycerine are mixed with arbitrary proportion.
In the mixed solution of the polynary alcohol and water, the mass ratio of polyalcohol and water is（1:0.5）-（0.5:1）.
The liquor capacity ratio A:B:C=70:70:（1-5）.
Silver nitrate concentration is 0.05mol/L-0.09mol/L in solution A.
Polyvinylpyrrolidoneconcentration concentration is 0.25mol/L-0.45mol/L in B solution, and the K values of polyvinylpyrrolidone are
120。
Copper chloride concentration is 0.025 mol/L -0.030mol/L in C solution.
The high-purity gas is helium, neon, argon gas or nitrogen, and when reaction, the pressure in autoclave is 0.5MP-15MP.
The heating rate of autoclave when heated is 10 DEG C -200 DEG C/h, and the reaction temperature in autoclave is 150 DEG C -250
DEG C, reaction time 5-24h.
A kind of overlength nano-silver thread dispersion liquid prepared by the preparation method of above-mentioned overlength nano-silver thread dispersion liquid.
Embodiment 1：
Present embodiments provide a kind of method for the nano-silver thread preparing length 200um.
0.64g silver nitrates are dissolved in 25ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly
2.08gPVPK120 is dissolved in 25ml water by solution A, and 25ml ethylene glycol and 25ml glycerine is added, stir evenly B is molten
3.38g copper chlorides are dissolved in 1L deionized waters, obtain C solution by liquid；70ml B solutions are slowly added under the premise of being vigorously stirred
Enter into 70ml solution As, 1ml C solutions are added dropwise after stirring evenly, the process of dropwise addition continues 15min, then shifts gained liquid
Into autoclave, bubbling argon 15min is first used, autoclave is then closed, it is high with high-purity argon gas to autoclave pressurization to 0.5MP
Pressure kettle heating rate is 10 DEG C/h, and isothermal reaction 5h after being warming up to 150 DEG C, natural cooling is up to the nano silver that length is 200um
Line dispersion liquid, reaction overall process keep constant pressure.
Embodiment 2：
Present embodiments provide a kind of method for the nano-silver thread preparing length 300um.
0.79g silver nitrates are dissolved in 27.8ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly
Solution A is obtained, 2.59gPVPK120 is dissolved in 27.8ml water, 25ml ethylene glycol and 25ml glycerine is added, stirs evenly to obtain B
3.51g copper chlorides are dissolved in 1L deionized waters, obtain C solution by solution；It is under the premise of being vigorously stirred that 70ml B solutions is slow
It is added in 70ml solution As, 2ml C solutions is added dropwise after stirring evenly, the process of dropwise addition continues 16min, then turns gained liquid
It moves on in autoclave, first uses bubbling argon 12min, then close autoclave, it is high with high-purity argon gas to autoclave pressurization to 5MP
Pressure kettle heating rate is 40 DEG C/h, and isothermal reaction 10h after being warming up to 180 DEG C, natural cooling is up to the nano silver that length is 300um
Line dispersion liquid, reaction overall process keep constant pressure.
Embodiment 3：
Present embodiments provide a kind of method for the nano-silver thread preparing length 350um.
0.99g silver nitrates are dissolved in 33.3ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly
Solution A is obtained, 3.24gPVPK120 is dissolved in 33.3ml water, 25ml ethylene glycol and 25ml glycerine is added, stirs evenly to obtain B
3.65g copper chlorides are dissolved in 1L deionized waters, obtain C solution by solution；It is under the premise of being vigorously stirred that 70ml B solutions is slow
It is added in 70ml solution As, 3ml C solutions is added dropwise after stirring evenly, the process of dropwise addition continues 17min, then turns gained liquid
It moves on in autoclave, first uses bubbling argon 10min, then close autoclave, it is high with high-purity argon gas to autoclave pressurization to 10MP
Pressure kettle heating rate is 100 DEG C/h, and isothermal reaction 15h after being warming up to 200 DEG C, natural cooling is up to the nanometer that length is 350um
Silver wire dispersion liquid, reaction overall process keep constant pressure.
Embodiment 4：
Present embodiments provide a kind of method for the nano-silver thread preparing length 400um.
1.36g silver nitrates are dissolved in 50ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly
4.44gPVPK120 is dissolved in 50ml water by solution A, and 25ml ethylene glycol and 25ml glycerine is added, stir evenly B is molten
3.92g copper chlorides are dissolved in 1L deionized waters, obtain C solution by liquid；70ml B solutions are slowly added under the premise of being vigorously stirred
Enter into 70ml solution As, 4ml C solutions are added dropwise after stirring evenly, the process of dropwise addition continues 18min, then shifts gained liquid
Into autoclave, bubbling argon 18min is first used, autoclave is then closed, with high-purity argon gas to autoclave pressurization to 12MP, high pressure
Kettle heating rate is 150 DEG C/h, and isothermal reaction 20h after being warming up to 220 DEG C, natural cooling is up to the nano silver that length is 400um
Line dispersion liquid, reaction overall process keep constant pressure.
Embodiment 5：
Present embodiments provide a kind of method for the nano-silver thread preparing length 500um.
2.30g silver nitrates are dissolved in 100ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly
Solution A is obtained, 7.49gPVPK120 is dissolved in 100ml water, 25ml ethylene glycol and 25ml glycerine is added, stirs evenly to obtain B
4.05g copper chlorides are dissolved in 1L deionized waters, obtain C solution by solution；It is under the premise of being vigorously stirred that 70ml B solutions is slow
It is added in 70ml solution As, 5ml C solutions is added dropwise after stirring evenly, the process of dropwise addition continues 15min, then turns gained liquid
It moves on in autoclave, first uses bubbling argon 20min, then close autoclave, it is high with high-purity argon gas to autoclave pressurization to 15MP
Pressure kettle heating rate is 200 DEG C/h, and for 24 hours, natural cooling is up to the nanometer that length is 500um for isothermal reaction after being warming up to 250 DEG C
Silver wire dispersion liquid, reaction overall process keep constant pressure.
Embodiment 6：
Present embodiments provide a kind of method for the nano-silver thread preparing length 200um.
0.8g silver nitrates are dissolved in 20ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly
2.6gPVPK120 is dissolved in 20ml water by solution A, and 25ml ethylene glycol and 25ml glycerine is added, stirs evenly to obtain solution B,
5g copper chlorides are dissolved in 1L deionized waters, solution C is obtained；B liquid is slowly added into A liquid under the premise of being vigorously stirred, is stirred
1ml solution Cs are added dropwise after mixing uniformly, the process of dropwise addition continues 15min, and then gained liquid is transferred in autoclave, first uses argon gas
It is bubbled 15min, then closes autoclave, with high-purity argon gas to autoclave pressurization to 1MP, autoclave heating rate is 60 DEG C/h,
Isothermal reaction 5h after being warming up to 180 DEG C, natural cooling are protected up to the nano-silver thread dispersion liquid that length is 200um, reaction overall process
Hold constant pressure.
Embodiment 7：
Present embodiments provide a kind of method for the nano-silver thread preparing length 500um.
1g silver nitrates are dissolved in 20ml water, 25ml ethylene glycol and 25ml glycerine is then added, stirs evenly molten
3.2gPVPK120 is dissolved in 20ml water by liquid A, and 25ml ethylene glycol and 25ml glycerine is added, stirs evenly to obtain solution B, will
5g copper chlorides are dissolved in 1L deionized waters, obtain solution C；B liquid is slowly added into A liquid under the premise of being vigorously stirred, is stirred
3ml solution Cs are added dropwise after uniformly, the process of dropwise addition continues 15min, and then gained liquid is transferred in autoclave, is first roused with argon gas
15min is steeped, autoclave is then closed, with high-purity argon gas to autoclave pressurization to 5MP, autoclave heating rate is 100 DEG C/h, is risen
Temperature is to isothermal reaction 5h after 220 DEG C, and natural cooling is up to the nano-silver thread dispersion liquid that length is 500um, reaction overall process holding
Constant pressure.
The method of synthesis overlength nano-silver thread provided by the present invention increases polyethylene pyrrole by increasing silver nitrate concentration
The dosage and molecular weight of pyrrolidone, by promoting reaction temperature and changing heating rate, by giving autoclave pressurization, to improve
The length of nano-silver thread.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those skilled in the art,
Under the premise of not departing from general idea of the present invention, several changes and improvements can also be made, these should also be considered as the present invention's
Protection domain.
Claims (10)
1. a kind of preparation method of overlength nano-silver thread dispersion liquid, it is characterised in that：Include the following steps：
（1）It is formulated as follows solution：
Solution A：Silver nitrate is dissolved in the mixed solution of polynary alcohol and water；
B solution：Polyethylene pyrrole network alkanone is dissolved in the mixed solution of polynary alcohol and water；
C solution：Copper chloride solution；
（2）Solution A is added in B solution under to stirring condition, obtains AB mixed solutions, after AB mixed solutions are stirred evenly, to
C solution is slowly added dropwise in AB mixed solutions, ABC mixed solutions are obtained after stirring evenly；
（3）By step（2）The ABC mixed solutions of gained pour into autoclave, rear enclosed autoclave are bubbled with high-purity gas, by high pressure
Kettle is heated to certain temperature, and reaction is after a certain period of time up to overlength nano-silver thread dispersion liquid, with high-purity gas to height during reaction
Press kettle pressurization so that pressure is certain value in autoclave.
2. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：The polyalcohol is
The mixture of ethylene glycol and glycerine, ethylene glycol and glycerine are mixed with arbitrary proportion.
3. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：The polyalcohol and
In the mixed solution of water, the mass ratio of polyalcohol and water is（1:0.5）-（0.5:1）.
4. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：The liquor capacity
Compare A:B:C=70:70:（1-5）.
5. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：Nitric acid in solution A
Silver concentration is 0.05mol/L-0.09mol/L.
6. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：Poly- second in B solution
The K values of a concentration of 0.25mol/L-0.45mol/L of alkene pyrrolidone, polyvinylpyrrolidone are 120.
7. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：Chlorination in B solution
Copper concentration is 0.025 mol/L -0.030mol/L.
8. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：The high-purity gas
For helium, neon, argon gas or nitrogen, when reaction, the pressure in autoclave is 0.5MP-15MP.
9. the preparation method of overlength nano-silver thread dispersion liquid according to claim 1, it is characterised in that：Autoclave is heating
When heating rate be 10 DEG C -200 DEG C/h, the reaction temperature in autoclave is 150 DEG C -250 DEG C, reaction time 5-24h.
10. overlength nanometer prepared by a kind of preparation method of overlength nano-silver thread dispersion liquid as described in claim 1-9 is any
Silver wire dispersion liquid.
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