CN107755711A - A kind of square micro-nano silver powder, preparation method thereof - Google Patents
A kind of square micro-nano silver powder, preparation method thereof Download PDFInfo
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- CN107755711A CN107755711A CN201710983970.1A CN201710983970A CN107755711A CN 107755711 A CN107755711 A CN 107755711A CN 201710983970 A CN201710983970 A CN 201710983970A CN 107755711 A CN107755711 A CN 107755711A
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- 239000000843 powder Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 110
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 75
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 60
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 55
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims abstract description 46
- 239000013078 crystal Substances 0.000 claims abstract description 38
- 239000011780 sodium chloride Substances 0.000 claims abstract description 30
- 239000002270 dispersing agent Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 3
- 238000013329 compounding Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 14
- 241000370738 Chlorion Species 0.000 claims description 12
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 8
- 229920000053 polysorbate 80 Polymers 0.000 claims description 8
- -1 polyethylene pyrrole Polymers 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 238000006197 hydroboration reaction Methods 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 6
- 239000004332 silver Substances 0.000 abstract description 6
- 238000006722 reduction reaction Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- XSNQEMWVLMRPFR-UHFFFAOYSA-N silver nitride Chemical compound [N-3].[Ag+].[Ag+].[Ag+] XSNQEMWVLMRPFR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 239000010946 fine silver Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to a kind of square micro-nano silver powder, preparation method thereof, belong to Technology of Preparing Superfine Silver Powders field.The silver nitrate solution of low concentration is prepared first, is added dispersant, is stirred；0.01mol/L sodium chloride solutions are added dropwise, silver chlorate seed crystal is prepared in stirring reaction；The silver nitrate solution of compounding high concentration, dispersant, silver chlorate seed crystal are then added into the silver nitrate solution of high concentration, and 0.684mol/L sodium chloride solution is added dropwise, continued reaction after dripping and obtain silver chlorate crystal in 1 hour；Silver chlorate crystal is dripped into rear stirring reaction 1~2 hour to silver powder is restored completely using sodium borohydride solution, then ageing 5~8 hours naturally, finally filter, wash, being dried in vacuo and produce square bodily form micro/nano level silver powder.The present invention utilizes chemical reduction method principle, and silver powder is reduced 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 thereof, belong to Technology of Preparing Superfine Silver Powders field.
Background technology
Super fine silver powder is a kind of function powder material, because it has good electric conductivity, chemical stability, high-ductility, anti-
The advantages that oxidisability and higher surface energy and chemism so that it is in optics, electromagnetic shielding material, biologic medical, light
Volt generates electricity to be had broad application prospects with fields such as electronics industries.With developing rapidly for electronics industry and photovoltaic industry,
It is also increasing for the demand of super fine silver powder, while with increasingly high-grade, precision and advanced, the integrated development trend of electronics industry, it is right
In the requirement also more and more higher of super fine silver powder.
The preparation method of super fine silver powder generally speaking has two kinds of preparation methods：Physical, chemical method.Solution phase chemical reduction
Technique is relatively easy, and operation is easy, and production cost is relatively low, is the common method for preparing super fine silver powder in batches at present.Electronation
Four factors of most critical in method：Reducing agent, dispersant（Protective agent）, temperature, pH, key is played to the pattern and granularity of silver powder
Effect.The reducing agent used at present has kind more than 40, and dispersant has more than kind more than 20.
It is conductive that super fine silver powder, which is used as electric slurry main purpose, such as circuit printing, solar cell positive pole, 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 Di Gaosha（Degussa）, Hayes power, Japanese Tanaka's noble metal
（TANAKA）, with and, three wells etc., they have monopolized the electric slurry market of China more than 80%.
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 of ball shape silver powder, when slurry prints, mobility is preferably most common silver powder in current slurry,
But the area that ball shape silver powder contacts with each other is small, increases contact resistance in theory.Flake silver powder is applied in solar cell electricity
In the slurry of pole, help to reduce the usage amount of silver powder, reduce silver paste cost, and improve silver paste electric conductivity, but it is traditional
Mechanical attrition method production cost is high, cycle length, 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, particle diameter more preferably controls, to slurry developers' meaning
It is great.
The silver powder of the square bodily form can make that silver powder stacking level is finer and close, and the contact area between silver powder particles is bigger, has
Effect reduces the contact resistance of silver powder, makes electric conductivity more preferably, is the morphologies in ideal.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of square micro-nano silver powder preparation side
Method.The present invention utilizes chemical reduction method principle, and silver powder is reduced 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 present invention is achieved through the following technical solutions.
A kind of square micro-nano silver powder, preparation method thereof, it is comprised the following steps that：
Step 1, the silver nitrate solution for preparing low concentration first, add the dispersant of total score powder dosage 5%, stir；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 0~5 DEG C with 2mL/min speed in temperature
Silver chlorate seed crystal is prepared in 0.01mol/L sodium chloride solutions, stirring reaction, silver ion and sodium chloride wherein in silver nitrate solution
The mol ratio of Chlorine in Solution ion is 1:1；
The silver nitrate solution of step 3, compounding high concentration, total score powder dosage is then added into the silver nitrate solution of high concentration
95% dispersant is simultaneously uniformly dispersed, and the silver chlorate seed crystal in step 2 is added under the conditions of being 30~45 DEG C in temperature, and with 2mL/
0.684mol/L sodium chloride solution is added dropwise in min speed, continues reaction after dripping and obtains silver chlorate crystal in 1 hour；It is wherein high
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in the silver nitrate solution of concentration:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 4~7, with
Sodium borohydride solution is added dropwise to silver powder is restored completely in 1mL/min drops speed, drips rear stirring reaction 1~2 hour, then natural
Ageing 5~8 hours, finally filter, wash, being dried in vacuo and produce 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.
Dispersant 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 addition is restores 1.5~2.5 times of silver powder theoretical amount completely in the step 4, solution
Concentration is 0.3~0.6mol/L.
The beneficial effects of the invention are as follows：
（1）The silver powder with square pattern and nearly square pattern is prepared, effectively improves the tap density of silver powder, reduces silver
The contact resistance of powder.
（2）Silver powder is pure, and granularity can regulate and control between nanometer and micron order.
（3）Simple production process, cost is low, may extend to laboratory and industrialized production.
Brief description of the drawings
Fig. 1 is present invention process flow chart；
Fig. 2 is the square micro-nano silver powder scanning electron microscope (SEM) photograph that the embodiment of the present invention 4 is prepared；
Fig. 3 is the square micro-nano silver powder X ray diffracting spectrum 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.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in figure 1, the square micro-nano silver powder, preparation method thereof, it is comprised the following steps that：
Step 1,0.0036mol, 0.005mol/L low concentration silver nitrate solution are prepared first, add point of total score powder dosage 5%
Powder（Dispersant is polyethylene pyrrole network alkanone, and total score powder dosage is the 5% of total silver nitrate solution quality used）, stir；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 0 DEG C with 2mL/min speed in temperature
0.01mol/L sodium chloride solutions, silver chlorate seed crystal is prepared with 350r/min speed stirring reactions, wherein in silver nitrate solution
The mol ratio of silver ion and chlorion in sodium chloride solution is 1:1；
Step 3, the silver nitrate solution for preparing 0.1164mol, 0.06mol/L high concentration, then to the silver nitrate solution of high concentration
The middle dispersant for adding total score powder dosage 95%（Dispersant is polyethylene pyrrole network alkanone）And be uniformly dispersed, it is 30 DEG C in temperature
Under the conditions of add step 2 in silver chlorate seed crystal（Silver chlorate seed crystal is the 3% of total silver chlorate quality）, and dripped with 2mL/min speed
Add 0.684mol/L sodium chloride solution, continue reaction after dripping and obtain silver chlorate crystal in 1 hour；The nitric acid of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in silver-colored solution:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 4, with 1mL/
Sodium borohydride solution is added dropwise in min drops speed（Sodium borohydride solution addition is restores 1.5 times of silver powder theoretical amount completely, solution
Concentration is 0.3mol/L）To silver powder is restored completely, drip rear stirring reaction 2 hours, then naturally be aged 8 hours, finally
Filtering, washing, vacuum drying（Temperature is 60 DEG C, vacuum 0.05MPa）Produce square bodily form micro/nano level silver powder.
Silver powder obtained by the present embodiment is the square bodily form, and without other miscellaneous peaks, peak shape is sharp, shows that silver powder is pure at X-ray diffraction peak
Net advantages of good crystallization, median are 0.34 μm, and particle diameter is concentrated, apparent density 1.54g/cm3。
Embodiment 2
As shown in figure 1, the square micro-nano silver powder, preparation method thereof, it is comprised the following steps that：
Step 1,0.0096mol, 0.01mol/L low concentration silver nitrate solution are prepared first, add point of total score powder dosage 5%
Powder（Dispersant is Tween 80, and total score powder dosage is the 20% of total silver nitrate solution quality used）, stir；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 5 DEG C with 2mL/min speed in temperature
0.01mol/L sodium chloride solutions, silver chlorate seed crystal is prepared with 650r/min speed stirring reactions, wherein in silver nitrate solution
The mol ratio of silver ion and chlorion in sodium chloride solution is 1:1；
Step 3, the silver nitrate solution for preparing 0.1164mol, 0.06mol/L high concentration, then to the silver nitrate solution of high concentration
The middle dispersant for adding total score powder dosage 95%（Dispersant is Tween 80）And be uniformly dispersed, add under the conditions of being 45 DEG C in temperature
Enter the silver chlorate seed crystal in step 2（Silver chlorate seed crystal is the 8% of total silver chlorate quality）, and be added dropwise with 2mL/min speed
0.684mol/L sodium chloride solution, continue reaction after dripping and obtain silver chlorate crystal in 1 hour；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in solution:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 7, with 1mL/
Sodium borohydride solution is added dropwise in min drops speed（Sodium borohydride solution addition is restores 2.5 times of silver powder theoretical amount completely, solution
Concentration is 0.6mol/L）To silver powder is restored completely, drip rear stirring reaction 2 hours, then naturally be aged 8 hours, finally
Filtering, washing, vacuum drying（Temperature is 60 DEG C, vacuum 0.05MPa）Produce 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, shows silver powder at X-ray diffraction peak
Pure crystalline is good, and median is 0.24 μm, and particle diameter is concentrated, apparent density 1.68g/cm3。
Embodiment 3
As shown in figure 1, the square micro-nano silver powder, preparation method thereof, it is comprised the following steps that：
Step 1,0.006mol, 0.0075mol/L low concentration silver nitrate solution are prepared first, add point of total score powder dosage 5%
Powder（Dispersant is polyethylene pyrrole network alkanone, and total score powder dosage is the 15% of total silver nitrate solution quality used）, stirring is
It is even；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 3 DEG C with 2mL/min speed in temperature
0.01mol/L sodium chloride solutions, silver chlorate seed crystal is prepared with 500r/min speed stirring reactions, wherein in silver nitrate solution
The mol ratio of silver ion and chlorion in sodium chloride solution is 1:1；
Step 3, the silver nitrate solution for preparing 0.114mol, 0.07mol/L high concentration, then into the silver nitrate solution of high concentration
Add the dispersant of total score powder dosage 95%（Dispersant is polyethylene pyrrole network alkanone）And be uniformly dispersed, it is 35 DEG C of bars in temperature
The silver chlorate seed crystal added under part in step 2（Silver chlorate seed crystal is the 5% of total silver chlorate quality）, and be added dropwise with 2mL/min speed
0.684mol/L sodium chloride solution, continue reaction after dripping and obtain silver chlorate crystal in 1 hour；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in solution:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 7, with 1mL/
Sodium borohydride solution is added dropwise in min drops speed（Sodium borohydride solution addition is restore silver powder theoretical amount completely 2 times, and solution is dense
Spend for 0.375mol/L）To silver powder is restored completely, drip rear stirring reaction 2 hours, then naturally be aged 6 hours, finally
Filtering, washing, vacuum drying（Temperature is 60 DEG C, vacuum 0.05MPa）Produce square bodily form micro/nano level silver powder.
Silver powder obtained by the present embodiment is the square bodily form, and without other miscellaneous peaks, peak shape is sharp, shows that silver powder is pure at X-ray diffraction peak
Net advantages of good crystallization, median are 0.17 μm, and particle diameter is concentrated, apparent density 1.37g/cm3。
Embodiment 4
As shown in figure 1, the square micro-nano silver powder, preparation method thereof, it is comprised the following steps that：
Step 1,0.066mol, 0.009mol/L low concentration silver nitrate solution are prepared first, add point of total score powder dosage 5%
Powder（Dispersant is Tween 80, and total score powder dosage is the 15% of total silver nitrate solution quality used）, stir；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 2 DEG C with 2mL/min speed in temperature
0.01mol/L sodium chloride solutions, silver chlorate seed crystal is prepared with 500r/min speed stirring reactions, wherein in silver nitrate solution
The mol ratio of silver ion and chlorion in sodium chloride solution is 1:1；
Step 3, the silver nitrate solution for preparing 0.862mol, 0.08mol/L high concentration, then into the silver nitrate solution of high concentration
Add the dispersant of total score powder dosage 95%（Dispersant is Tween 80）And be uniformly dispersed, added under the conditions of being 45 DEG C in temperature
Silver chlorate seed crystal in step 2（Silver chlorate seed crystal is the 7% of total silver chlorate quality）, and be added dropwise with 2mL/min speed
0.684mol/L sodium chloride solution, continue reaction after dripping and obtain silver chlorate crystal in 1 hour；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in solution:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 7, with 1mL/
Sodium borohydride solution is added dropwise in min drops speed（Sodium borohydride solution addition is restore silver powder theoretical amount completely 2 times, and solution is dense
Spend for 0.6mol/L）To silver powder is restored completely, drip rear stirring reaction 1.5 hours, then naturally be aged 8 hours, finally
Filtering, washing, vacuum drying（Temperature is 60 DEG C, vacuum 0.05MPa）Produce square bodily form micro/nano level silver powder.
The present embodiment is tested to expand, and gained silver powder is the square bodily form, 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
It can be seen that silver powder is the square bodily form, X-ray diffraction peak type sharply without other miscellaneous peaks, shows that silver powder pure crystalline is good, middle position grain
Footpath is 0.69 μm, apparent density 1.79g/cm3, tap density 5.13g/cm3。
The result that embodiment 1 to 4 obtains is as shown in table 1, as can be seen from Table 1 a kind of preparation of the micro-nano silver powder of pros
Method, prepared morphologies are the square bodily form, a small amount of the nearly square bodily form occur, particle diameter between nanoscale and micron order,
And centralized particle diameter, silver powder pure crystalline is good, expand experiment also can retention property stabilization.
Table 1
。
Embodiment 5
As shown in figure 1, the square micro-nano silver powder, preparation method thereof, it is comprised the following steps that：
Step 1,0.066mol, 0.009mol/L low concentration silver nitrate solution are prepared first, add point of total score powder dosage 18%
Powder（Dispersant is Tween 80, and total score powder dosage is the 15% of total silver nitrate solution quality used）, stir；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 4 DEG C with 2mL/min speed in temperature
0.01mol/L sodium chloride solutions, silver chlorate seed crystal is prepared with 500r/min speed stirring reactions, wherein in silver nitrate solution
The mol ratio of silver ion and chlorion in sodium chloride solution is 1:1；
Step 3, the silver nitrate solution for preparing 0.862mol, 0.08mol/L high concentration, then into the silver nitrate solution of high concentration
Add the dispersant of total score powder dosage 95%（Dispersant is Tween 80）And be uniformly dispersed, added under the conditions of being 35 DEG C in temperature
Silver chlorate seed crystal in step 2（Silver chlorate seed crystal is the 7% of total silver chlorate quality）, and be added dropwise with 2mL/min speed
0.684mol/L sodium chloride solution, continue reaction after dripping and obtain silver chlorate crystal in 1 hour；The silver nitrate of its middle and high concentration
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in solution:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 6, with 1mL/
Sodium borohydride solution is added dropwise in min drops speed（Sodium borohydride solution addition is restore silver powder theoretical amount completely 2 times, and solution is dense
Spend for 0.6mol/L）To silver powder is restored completely, rear stirring reaction is dripped 1 hour, be then aged 5 hours naturally, last mistake
Filter, washing, vacuum drying（Temperature is 60 DEG C, vacuum 0.05MPa）Produce square bodily form micro/nano level silver powder.
Above in association with accompanying drawing to the present invention embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, can also be before present inventive concept not be departed from those of ordinary skill in the art's possessed knowledge
Put that various changes can be made.
Claims (6)
1. a kind of square micro-nano silver powder, preparation method thereof, it is characterised in that comprise the following steps that：
Step 1, the silver nitrate solution for preparing low concentration first, add the dispersant of total score powder dosage 5%, stir；
Step 2, the silver nitrate solution that will be handled through step 1, it is to be added dropwise under the conditions of 0~5 DEG C with 2mL/min speed in temperature
Silver chlorate seed crystal is prepared in 0.01mol/L sodium chloride solutions, stirring reaction, silver ion and sodium chloride wherein in silver nitrate solution
The mol ratio of Chlorine in Solution ion is 1:1；
The silver nitrate solution of step 3, compounding high concentration, total score powder dosage is then added into the silver nitrate solution of high concentration
95% dispersant is simultaneously uniformly dispersed, and the silver chlorate seed crystal in step 2 is added under the conditions of being 30~45 DEG C in temperature, and with 2mL/
0.684mol/L sodium chloride solution is added dropwise in min speed, continues reaction after dripping and obtains silver chlorate crystal in 1 hour；It is wherein high
Silver ion and 0.684mol/L sodium chloride solution chlorions mol ratio are 1 in the silver nitrate solution of concentration:1；
Step 4, the silver chlorate crystal that step 3 obtains used watery hydrochloric acid or sodium hydroxide solution adjust pH value as 4~7, with
Sodium borohydride solution is added dropwise to silver powder is restored completely in 1mL/min drops speed, drips rear stirring reaction 1~2 hour, then natural
Ageing 5~8 hours, finally filter, wash, being dried in vacuo and produce square bodily form micro/nano level silver powder.
2. square 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. square micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that：In the step 1 and step 3
Dispersant is Tween 80 or polyethylene pyrrole network alkanone, and total score powder dosage is the 5~20% of total silver nitrate solution quality used.
4. square 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. square micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that：The step 3 silver chlorate seed
Crystalline substance is the 3~8% of total silver chlorate quality.
6. square micro-nano silver powder, preparation method thereof according to claim 1, it is characterised in that：Hydroboration in the step 4
Sodium solution addition is restore silver powder theoretical amount completely 1.5~2.5 times, and solution concentration is 0.3~0.6mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710983970.1A CN107755711B (en) | 2017-10-20 | 2017-10-20 | A kind of pros' micro-nano silver powder, preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710983970.1A CN107755711B (en) | 2017-10-20 | 2017-10-20 | A kind of pros' micro-nano silver powder, preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
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| CN107755711A true CN107755711A (en) | 2018-03-06 |
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| CN108714699A (en) * | 2018-06-07 | 2018-10-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | It is a kind of to prepare the method for Active silver powder and its silver powder obtained using silver sulfide induction |
| CN109019661A (en) * | 2018-07-16 | 2018-12-18 | 天津大学 | A kind of synthetic method of silver chlorate nano-powder |
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