CN107755711B - A kind of pros' micro-nano silver powder, preparation method thereof - Google Patents
A kind of pros' micro-nano silver powder, preparation method thereof Download PDFInfo
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- CN107755711B CN107755711B CN201710983970.1A CN201710983970A CN107755711B CN 107755711 B CN107755711 B CN 107755711B CN 201710983970 A CN201710983970 A CN 201710983970A CN 107755711 B CN107755711 B CN 107755711B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
Abstract
The present invention relates to a kind of square micro-nano silver powder, preparation method thereofs, belong to Technology of Preparing Superfine Silver Powders field.The silver nitrate solution for preparing low concentration first, is added dispersing agent, stirs evenly；0.01mol/L sodium chloride solution is added dropwise, is stirred to react and silver chlorate seed crystal is prepared；Then dispersing agent, silver chlorate seed crystal are added into the silver nitrate solution of high concentration, and the sodium chloride solution of 0.684mol/L is added dropwise for the silver nitrate solution of compounding high concentration, the reaction was continued 1 hour after dripping obtains silver chlorate crystal；It by silver chlorate crystal using sodium borohydride solution to silver powder is restored completely, is stirred to react after dripping 1~2 hour, is then aged 5~8 hours naturally, be finally filtered, washed, be dried in vacuo up to square bodily form micro/nano level silver powder.The present invention utilizes chemical reduction method principle, and silver powder is restored from silver nitride precipitation, prepares the silver powder of the square bodily form or nearly square pattern, and controls the granularity of silver powder between nanometer and micron order.
Description
Technical field
The present invention relates to a kind of square micro-nano silver powder, preparation method thereofs, belong to Technology of Preparing Superfine Silver Powders field.
Background technique
Super fine silver powder is a kind of function powder material, because it is with good electric conductivity, chemical stability, high-ductility, anti-
The advantages that oxidisability and higher surface energy and chemical activity, so that it is in optics, electromagnetic shielding material, biologic medical, light
The fields such as volt power generation and electronics industry have broad application prospects.With the rapid development of electronics industry and photovoltaic industry,
Development trend also increasing for the demand of super fine silver powder while increasingly high-grade, precision and advanced, integrated with electronics industry is right
It is also higher and higher in the requirement of super fine silver powder.
Generally speaking there are two types of preparation methods for the preparation method of super fine silver powder: physical method, chemical method.Solution phase chemical reduction
Technique is relatively easy, and operation is easy, lower production costs, is the common method for preparing super fine silver powder in batches at present.Electronation
Four factors of most critical in method: reducing agent, dispersing agent (protective agent), temperature, pH play key to the pattern and granularity of silver powder
Effect.Current used reducing agent has more than 40 kinds, and dispersing agent has more than more than 20 kinds.
It is conduction that super fine silver powder, which is used as electric slurry main purpose, such as circuit printing, solar battery anode, back electrode.
Production technology, product variety, quality level and the market scale of China's conductive silver paste and positive silver lag far behind developed country
Well-known manufacturer, such as Dupont (Dupond), German Digao husky (Degussa), Hayes power, Japanese Tanaka's noble metal
(TANAKA), same and three wells etc., they have monopolized the electric slurry market of 80% or more China.
Electric slurry silver powder mainly has ball shape silver powder and flake silver powder, and solution phase chemical reduction prepares ball shape silver powder
Main method, the preparation of flake silver powder are changed by high-energy ball milling normal direction chemical reduction method.The preparation of ball shape silver powder has had greatly
The document and patent report of amount, because when slurry prints, mobility is preferably the most common silver powder in current slurry to ball shape silver powder,
But the area that ball shape silver powder contacts with each other is small, theoretically increases contact resistance.Flake silver powder is applied in solar battery electricity
In the slurry of pole, facilitates the usage amount for reducing silver powder, reduce silver paste cost, and improve silver paste electric conductivity, but traditional
Mechanical attrition method high production cost, period are long, and the more performance of silver powder rough surface impurity is unstable.Find a kind of new pattern
Silver powder, makes that silver powder purity is higher, tap density is higher, contact resistance is smaller, partial size more preferably controls, to slurry developers' meaning
It is great.
Silver powder square-shaped can make silver powder stacking level finer and close, and the contact area between silver powder particles is bigger, have
Effect reduces the contact resistance of silver powder, makes electric conductivity more preferably, is the morphologies in ideal.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of micro-nano silver powder preparation side, pros
Method.The present invention utilizes chemical reduction method principle, and silver powder is restored from silver nitride precipitation, prepares the square bodily form or the nearly square bodily form
The silver powder of looks, and the granularity of silver powder is controlled between nanometer and micron order.The invention is realized by the following technical scheme.
A kind of pros' micro-nano silver powder, preparation method thereof, the specific steps of which are as follows:
Step 1, the silver nitrate solution for preparing low concentration first, are added the dispersing agent of total score powder dosage 5%, stir evenly；
Step 2, the silver nitrate solution that will be handled through step 1, with the speed of 2mL/min under the conditions of temperature is at 0~5 DEG C
0.01mol/L sodium chloride solution is added dropwise, is stirred to react and silver chlorate seed crystal is prepared, wherein silver ion and chlorine in silver nitrate solution
The molar ratio for changing chloride ion in sodium solution is 1:1；
Then the silver nitrate solution of step 3, compounding high concentration total score powder is added into the silver nitrate solution of high concentration and uses
The dispersing agent of amount 95% is simultaneously uniformly dispersed, silver chlorate seed crystal under the conditions of temperature is 30~45 DEG C in addition step 2, and with
The sodium chloride solution of 0.684mol/L is added dropwise in 2mL/min speed, and the reaction was continued 1 hour after dripping obtains silver chlorate crystal；Its
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in the silver nitrate solution of middle and high concentration；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 4~7,
Sodium borohydride solution is added dropwise to silver powder is restored completely with 1mL/min drop speed, is stirred to react 1~2 hour after dripping, then from
So ageing 5~8 hours are finally filtered, washed, are dried in vacuo up to square bodily form micro/nano level silver powder.
The silver nitrate solution concentration of low concentration is 0.005~0.01mol/L in the step 1.
Dispersing agent is Tween 80 or polyethylene pyrrole network alkanone in the step 1 and step 3, and total score powder dosage is used total
The 5~20% of silver nitrate solution quality.
The silver nitrate solution of step 3 middle and high concentration is 0.06~0.08mol/L.
The step 3 silver chlorate seed crystal is the 3~8% of total silver chlorate quality.
Sodium borohydride solution additional amount is 1.5~2.5 times for restoring silver powder theoretical amount completely, solution in the step 4
Concentration is 0.3~0.6mol/L.
The beneficial effects of the present invention are:
(1) silver powder with square pattern and nearly square pattern is prepared, the tap density of silver powder is effectively improved, subtracts
The contact resistance of small silver powder.
(2) silver powder is pure, and granularity can regulate and control between nanometer and micron order.
(3) simple production process, it is at low cost, it may extend to laboratory and industrialized production.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the micro-nano silver powder scanning electron microscope (SEM) photograph of pros that the embodiment of the present invention 4 is prepared；
Fig. 3 is the micro-nano silver powder X ray diffracting spectrum of pros that the embodiment of the present invention 4 is prepared；
Fig. 4 is the square micro-nano silver powder grain size distribution that the embodiment of the present invention 4 is prepared.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in Figure 1, pros' micro-nano silver powder, preparation method thereof, the specific steps of which are as follows:
Step 1 prepares 0.0036mol, 0.005mol/L low concentration silver nitrate solution first, and total score powder dosage 5% is added
Dispersing agent (dispersing agent be polyethylene pyrrole network alkanone, total score powder dosage be total silver nitrate solution quality used 5%), stirring
Uniformly；
Step 2, the silver nitrate solution that will be handled through step 1 are dripped under the conditions of temperature is at 0 DEG C with the speed of 2mL/min
Add 0.01mol/L sodium chloride solution, is stirred to react with 350r/min speed and silver chlorate seed crystal is prepared, wherein silver nitrate solution
The molar ratio of chloride ion is 1:1 in middle silver ion and sodium chloride solution；
Step 3, the silver nitrate solution for preparing 0.1164mol, 0.06mol/L high concentration, then to the silver nitrate of high concentration
The dispersing agent (dispersing agent is polyethylene pyrrole network alkanone) of total score powder dosage 95% is added in solution and is uniformly dispersed, is in temperature
The silver chlorate seed crystal (silver chlorate seed crystal is the 3% of total silver chlorate quality) being added under the conditions of 30 DEG C in step 2, and with 2mL/min speed
The sodium chloride solution of 0.684mol/L is added dropwise in degree, and the reaction was continued 1 hour after dripping obtains silver chlorate crystal；Its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in silver nitrate solution；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 4, with
1mL/min drop speed dropwise addition sodium borohydride solution (sodium borohydride solution additional amount is 1.5 times for restoring silver powder theoretical amount completely,
Solution concentration is 0.3mol/L) to silver powder is restored completely, it is stirred to react after dripping 2 hours, is then aged 8 hours naturally,
It is finally filtered, washed, is dried in vacuo (temperature is 60 DEG C, vacuum degree 0.05MPa) up to square bodily form micro/nano level silver powder.
Silver powder obtained by the present embodiment is positive cube shape, and without other miscellaneous peaks, peak shape is sharp at X-ray diffraction peak, shows that silver powder is pure
Net advantages of good crystallization, median are 0.34 μm, and partial size is concentrated, apparent density 1.54g/cm3。
Embodiment 2
As shown in Figure 1, pros' micro-nano silver powder, preparation method thereof, the specific steps of which are as follows:
Step 1 prepares 0.0096mol, 0.01mol/L low concentration silver nitrate solution first, and total score powder dosage 5% is added
Dispersing agent (dispersing agent is Tween 80, and total score powder dosage is the 20% of total silver nitrate solution quality used), stir evenly；
Step 2, the silver nitrate solution that will be handled through step 1 are dripped under the conditions of temperature is at 5 DEG C with the speed of 2mL/min
Add 0.01mol/L sodium chloride solution, is stirred to react with 650r/min speed and silver chlorate seed crystal is prepared, wherein silver nitrate solution
The molar ratio of chloride ion is 1:1 in middle silver ion and sodium chloride solution；
Step 3, the silver nitrate solution for preparing 0.1164mol, 0.06mol/L high concentration, then to the silver nitrate of high concentration
The dispersing agent (dispersing agent is Tween 80) of total score powder dosage 95% is added in solution and is uniformly dispersed, is 45 DEG C of conditions in temperature
The lower silver chlorate seed crystal (silver chlorate seed crystal is the 8% of total silver chlorate quality) being added in step 2, and with the dropwise addition of 2mL/min speed
The sodium chloride solution of 0.684mol/L, the reaction was continued 1 hour after dripping obtains silver chlorate crystal；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in solution；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 7, with
1mL/min drop speed dropwise addition sodium borohydride solution (sodium borohydride solution additional amount is 2.5 times for restoring silver powder theoretical amount completely,
Solution concentration is 0.6mol/L) to silver powder is restored completely, it is stirred to react after dripping 2 hours, is then aged 8 hours naturally,
It is finally filtered, washed, is dried in vacuo (temperature is 60 DEG C, vacuum degree 0.05MPa) up to square bodily form micro/nano level silver powder.
Silver powder obtained by the present embodiment is the nearly square bodily form, and without other miscellaneous peaks, peak shape is sharp at X-ray diffraction peak, shows silver powder
Pure crystalline is good, and median is 0.24 μm, and partial size is concentrated, apparent density 1.68g/cm3。
Embodiment 3
As shown in Figure 1, pros' micro-nano silver powder, preparation method thereof, the specific steps of which are as follows:
Step 1 prepares 0.006mol, 0.0075mol/L low concentration silver nitrate solution first, and total score powder dosage 5% is added
Dispersing agent (dispersing agent be polyethylene pyrrole network alkanone, total score powder dosage be total silver nitrate solution quality used 15%), stirring
Uniformly；
Step 2, the silver nitrate solution that will be handled through step 1 are dripped under the conditions of temperature is at 3 DEG C with the speed of 2mL/min
Add 0.01mol/L sodium chloride solution, is stirred to react with 500r/min speed and silver chlorate seed crystal is prepared, wherein silver nitrate solution
The molar ratio of chloride ion is 1:1 in middle silver ion and sodium chloride solution；
Step 3, the silver nitrate solution for preparing 0.114mol, 0.07mol/L high concentration, it is then molten to the silver nitrate of high concentration
The dispersing agent (dispersing agent is polyethylene pyrrole network alkanone) of total score powder dosage 95% is added in liquid and is uniformly dispersed, is 35 in temperature
The silver chlorate seed crystal (silver chlorate seed crystal is the 5% of total silver chlorate quality) being added under the conditions of DEG C in step 2, and with 2mL/min speed
The sodium chloride solution of 0.684mol/L is added dropwise, the reaction was continued 1 hour after dripping obtains silver chlorate crystal；The nitre of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in sour silver solution；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 7, with
Sodium borohydride solution is added dropwise in 1mL/min drop speed, and (sodium borohydride solution additional amount is 2 times for restoring silver powder theoretical amount completely, molten
Liquid concentration is 0.375mol/L) to silver powder is restored completely, it is stirred to react after dripping 2 hours, is then aged 6 hours naturally,
It is finally filtered, washed, is dried in vacuo (temperature is 60 DEG C, vacuum degree 0.05MPa) up to square bodily form micro/nano level silver powder.
Silver powder obtained by the present embodiment is positive cube shape, and without other miscellaneous peaks, peak shape is sharp at X-ray diffraction peak, shows that silver powder is pure
Net advantages of good crystallization, median are 0.17 μm, and partial size is concentrated, apparent density 1.37g/cm3。
Embodiment 4
As shown in Figure 1, pros' micro-nano silver powder, preparation method thereof, the specific steps of which are as follows:
Step 1 prepares 0.066mol, 0.009mol/L low concentration silver nitrate solution first, and total score powder dosage 5% is added
Dispersing agent (dispersing agent is Tween 80, and total score powder dosage is the 15% of total silver nitrate solution quality used), stir evenly；
Step 2, the silver nitrate solution that will be handled through step 1 are dripped under the conditions of temperature is at 2 DEG C with the speed of 2mL/min
Add 0.01mol/L sodium chloride solution, is stirred to react with 500r/min speed and silver chlorate seed crystal is prepared, wherein silver nitrate solution
The molar ratio of chloride ion is 1:1 in middle silver ion and sodium chloride solution；
Step 3, the silver nitrate solution for preparing 0.862mol, 0.08mol/L high concentration, it is then molten to the silver nitrate of high concentration
The dispersing agent (dispersing agent is Tween 80) of total score powder dosage 95% is added in liquid and is uniformly dispersed, under the conditions of temperature is 45 DEG C
The silver chlorate seed crystal (silver chlorate seed crystal is the 7% of total silver chlorate quality) being added in step 2, and with the dropwise addition of 2mL/min speed
The sodium chloride solution of 0.684mol/L, the reaction was continued 1 hour after dripping obtains silver chlorate crystal；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in solution；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 7, with
Sodium borohydride solution is added dropwise in 1mL/min drop speed, and (sodium borohydride solution additional amount is 2 times for restoring silver powder theoretical amount completely, molten
Liquid concentration is 0.6mol/L) to silver powder is restored completely, it is stirred to react after dripping 1.5 hours, is then aged 8 hours naturally,
It is finally filtered, washed, is dried in vacuo (temperature is 60 DEG C, vacuum degree 0.05MPa) up to square bodily form micro/nano level silver powder.
The present embodiment is to expand experiment, and gained silver powder is positive cube shape, and the scanning electron microscope (SEM) photograph that the present embodiment is prepared is such as
Shown in Fig. 2, X ray diffracting spectrum as shown in figure 3, square micro-nano silver powder grain size distribution as shown in figure 4, in from Fig. 2 to Fig. 4
The cube shape it can be seen that silver powder is positive, X-ray diffraction peak type show that silver powder pure crystalline is good sharply without other miscellaneous peaks, middle position grain
Diameter is 0.69 μm, apparent density 1.79g/cm3, tap density 5.13g/cm3。
Embodiment 1 to 4 obtains that the results are shown in Table 1, a kind of preparation of the micro-nano silver powder of pros as can be seen from Table 1
Method, prepared morphologies are positive cube shape, a small amount of the nearly square bodily form occur, partial size between nanoscale and micron order,
And centralized particle diameter, silver powder pure crystalline is good, expands the stabilization that experiment is also able to maintain performance.
Table 1
。
Embodiment 5
As shown in Figure 1, pros' micro-nano silver powder, preparation method thereof, the specific steps of which are as follows:
Step 1 prepares 0.066mol, 0.009mol/L low concentration silver nitrate solution first, and total score powder dosage 18% is added
Dispersing agent (dispersing agent is Tween 80, and total score powder dosage is the 15% of total silver nitrate solution quality used), stir evenly；
Step 2, the silver nitrate solution that will be handled through step 1 are dripped under the conditions of temperature is at 4 DEG C with the speed of 2mL/min
Add 0.01mol/L sodium chloride solution, is stirred to react with 500r/min speed and silver chlorate seed crystal is prepared, wherein silver nitrate solution
The molar ratio of chloride ion is 1:1 in middle silver ion and sodium chloride solution；
Step 3, the silver nitrate solution for preparing 0.862mol, 0.08mol/L high concentration, it is then molten to the silver nitrate of high concentration
The dispersing agent (dispersing agent is Tween 80) of total score powder dosage 95% is added in liquid and is uniformly dispersed, under the conditions of temperature is 35 DEG C
The silver chlorate seed crystal (silver chlorate seed crystal is the 7% of total silver chlorate quality) being added in step 2, and with the dropwise addition of 2mL/min speed
The sodium chloride solution of 0.684mol/L, the reaction was continued 1 hour after dripping obtains silver chlorate crystal；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in solution；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 6, with
Sodium borohydride solution is added dropwise in 1mL/min drop speed, and (sodium borohydride solution additional amount is 2 times for restoring silver powder theoretical amount completely, molten
Liquid concentration is 0.6mol/L) to silver powder is restored completely, it is stirred to react 1 hour after dripping, then ageing 5 hours naturally, most
After be filtered, washed, be dried in vacuo (temperature is 60 DEG C, vacuum degree 0.05MPa) up to square bodily form micro/nano level silver powder.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (6)
1. a kind of pros' micro-nano silver powder, preparation method thereof, it is characterised in that specific step is as follows:
Step 1, the silver nitrate solution for preparing low concentration first, are added the dispersing agent of total score powder dosage 5%, stir evenly；
Step 2, the silver nitrate solution that will be handled through step 1 are added dropwise under the conditions of temperature is at 0~5 DEG C with the speed of 2mL/min
0.01mol/L sodium chloride solution is stirred to react and silver chlorate seed crystal is prepared, wherein silver ion and sodium chloride in silver nitrate solution
The molar ratio of Chlorine in Solution ion is 1:1；
Then total score powder dosage is added in the silver nitrate solution of step 3, compounding high concentration into the silver nitrate solution of high concentration
95% dispersing agent is simultaneously uniformly dispersed, and the silver chlorate seed crystal in step 2 is added, and under the conditions of temperature is 30~45 DEG C with 2mL/
The sodium chloride solution of 0.684mol/L is added dropwise in min speed, and the reaction was continued 1 hour after dripping obtains silver chlorate crystal；It is wherein high
Silver ion and 0.684mol/L sodium chloride solution chloride ion molar ratio are 1:1 in the silver nitrate solution of concentration；
Step 4 uses the silver chlorate crystal that step 3 obtains dilute hydrochloric acid or sodium hydroxide solution to adjust pH value as 4~7, with
Sodium borohydride solution is added dropwise to silver powder is restored completely in 1mL/min drop speed, is stirred to react after dripping 1~2 hour, then natural
Ageing 5~8 hours is finally filtered, washed, is dried in vacuo up to square bodily form micro/nano level silver powder.
2. pros' micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that: low concentration in the step 1
Silver nitrate solution concentration be 0.005~0.01mol/L.
3. pros' micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that: in the step 1 and step 3
Dispersing agent is Tween 80 or polyvinylpyrrolidone, and total score powder dosage is the 5~20% of total silver nitrate solution quality used.
4. pros' micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that: step 3 middle and high concentration
Silver nitrate solution be 0.06~0.08mol/L.
5. pros' micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that: the step 3 silver chlorate seed
Brilliant additional amount is the 3~8% of total silver chlorate quality.
6. pros' micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that: hydroboration in the step 4
Sodium solution additional amount is 1.5~2.5 times for restoring silver powder theoretical amount completely, and solution concentration is 0.3~0.6mol/L.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994631A (en) * | 2005-12-28 | 2007-07-11 | 中国科学院理化技术研究所 | Method for preparing redispersible Ag nanoparticle by using silver halide precrystallization reduction process |
| CN101076572A (en) * | 2004-12-11 | 2007-11-21 | 伊斯曼柯达公司 | Conductive silver dispersions and uses thereof |
| CN101626856A (en) * | 2007-03-30 | 2010-01-13 | 三菱麻铁里亚尔株式会社 | The manufacture method of fine silver particle, fine silver particle and the manufacturing installation of fine silver particle |
| JP2011089143A (en) * | 2009-10-20 | 2011-05-06 | Japan Advanced Institute Of Science & Technology Hokuriku | Method for producing mono-component system and bi-component system cubic type metal nanoparticle |
| CN103658678A (en) * | 2014-01-06 | 2014-03-26 | 景德镇陶瓷学院 | Preparation method for silver nanocubes |
| CN104308172A (en) * | 2014-08-11 | 2015-01-28 | 常州大学 | Method for preparing hollow cubic micro-nano metal |
| CN104923801A (en) * | 2014-03-17 | 2015-09-23 | 北京中科纳通电子技术有限公司 | Method for preparing nanosilver powder in batches |
| CN104985191A (en) * | 2015-07-08 | 2015-10-21 | Tcl集团股份有限公司 | Silver nano cube with monodispersity and preparation method and conductive ink thereof |
| CN105665748A (en) * | 2016-04-25 | 2016-06-15 | 辽宁石化职业技术学院 | Method for preparing high-purity superfine silver powder |
| CN106001607A (en) * | 2016-07-06 | 2016-10-12 | 济宁利特纳米技术有限责任公司 | Method for preparing silver nanocubes in hydrophobic phase |
-
2017
- 2017-10-20 CN CN201710983970.1A patent/CN107755711B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101076572A (en) * | 2004-12-11 | 2007-11-21 | 伊斯曼柯达公司 | Conductive silver dispersions and uses thereof |
| CN1994631A (en) * | 2005-12-28 | 2007-07-11 | 中国科学院理化技术研究所 | Method for preparing redispersible Ag nanoparticle by using silver halide precrystallization reduction process |
| CN101626856A (en) * | 2007-03-30 | 2010-01-13 | 三菱麻铁里亚尔株式会社 | The manufacture method of fine silver particle, fine silver particle and the manufacturing installation of fine silver particle |
| JP2011089143A (en) * | 2009-10-20 | 2011-05-06 | Japan Advanced Institute Of Science & Technology Hokuriku | Method for producing mono-component system and bi-component system cubic type metal nanoparticle |
| CN103658678A (en) * | 2014-01-06 | 2014-03-26 | 景德镇陶瓷学院 | Preparation method for silver nanocubes |
| CN104923801A (en) * | 2014-03-17 | 2015-09-23 | 北京中科纳通电子技术有限公司 | Method for preparing nanosilver powder in batches |
| CN104308172A (en) * | 2014-08-11 | 2015-01-28 | 常州大学 | Method for preparing hollow cubic micro-nano metal |
| CN104985191A (en) * | 2015-07-08 | 2015-10-21 | Tcl集团股份有限公司 | Silver nano cube with monodispersity and preparation method and conductive ink thereof |
| CN105665748A (en) * | 2016-04-25 | 2016-06-15 | 辽宁石化职业技术学院 | Method for preparing high-purity superfine silver powder |
| CN106001607A (en) * | 2016-07-06 | 2016-10-12 | 济宁利特纳米技术有限责任公司 | Method for preparing silver nanocubes in hydrophobic phase |
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