CN101733410A - Preparation method of high dispersibility superfine silver powder with adjustable grain diameter - Google Patents
Preparation method of high dispersibility superfine silver powder with adjustable grain diameter Download PDFInfo
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- CN101733410A CN101733410A CN200910214605A CN200910214605A CN101733410A CN 101733410 A CN101733410 A CN 101733410A CN 200910214605 A CN200910214605 A CN 200910214605A CN 200910214605 A CN200910214605 A CN 200910214605A CN 101733410 A CN101733410 A CN 101733410A
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Abstract
The invention relates to a preparation method of high dispersibility superfine silver powder with adjustable grain diameter, comprising the following steps: 1. dissolving silver nitrate and surfactant in water to prepare silver solution A; 2. dissolving ascorbic acid, PH regulator and surfactant in water to prepare reducing liquid B; 3. preparing alkaline aqueous solution C by alkaline PH regulator; dropwise adding alkaline aqueous solution C and silver solution A to reducing liquid B at the set time. PH value of the reducing liquid B and flow velocity of alkaline aqueous solution C are adjusted, so that silver power particle size can be easily adjusted and the silver power particles can grow up uniformly. The silver powder obtained by the method of the invention has the characteristics of polyhedral microcosmic appearance, good dispersibility, narrow size distribution, high tap density and good sintering character.
Description
Technical field
The present invention relates to the liquid phase preparation process of super fine silver powder, relate in particular to a kind of preparation method who is applied to the particle size dispersibility superfine silver powder with adjustable of electric slurry.
Background technology
Silver powder is a kind of noble metal powder that is most widely used in the electronics industry with the consumption maximum, its pattern, particle size and uniformity, dispersiveness etc. are the key factors of influence silver slurry filming performance, can be used for making various low-temperature setting polymer silver slurries, conducting resinl in view of the above, or comprise the slug type silver paste of all kinds of ceramic components electrode slurrys.
At present the most frequently used method for preparing silver powder in enormous quantities belongs to liquid phase reduction, and liquid phase reduction production technology, equipment are simple, and production cost is low, and properties of product controllability, good reproducibility.The technology point that liquid phase reduction prepares silver powder is to control dispersiveness and the size and the uniformity of the silver-colored particle of reduction, because very easily producing in the aqueous solution, superfine powder reunites, cause dispersed bad, be difficult to satisfy the ordinary electronic slurry, the particularly printing of high-end silver paste, the sintering demand, for example application number is that 200510128715.6 patent needs subsequent heat treatment, and reactant concentration is low, the unit volume output is low, though be unfavorable for industrial production in enormous quantities. application number is 200710049490.4 patent silver nitrate concentration height, but do not relate to choosing of surfactant, the dispersiveness of reduction gained powder is difficult to controlled.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of silver powder decentralization height, the preparation method of the silver powder that silver powder particle size is evenly adjustable, tap density is high, can meet the demands the especially middle and high end silver slurry demand of high solids content, low-shrinkage, high printing precision of this silver powder;
The technical problem to be solved in the present invention is achieved through the following technical solutions: a kind of preparation method of particle size dispersibility superfine silver powder with adjustable, and step is: 1., silver nitrate, surfactant dissolves are configured to silver-colored solution A in water; 2., ascorbic acid, PH conditioning agent and surfactant dissolves are configured to reducing solution B in water; 3., with alkaline PH conditioning agent configuration alkaline aqueous solution C; 4., at the appointed time drip C liquid and A liquid in the B liquid, silver powder is evenly grown up;
Perhaps: 1., silver nitrate, surfactant dissolves are configured to silver-colored solution A in water; 2., ascorbic acid, surfactant dissolves are configured to reducing solution B1 in water; 3., with alkaline PH conditioning agent configuration alkaline aqueous solution C; 4., the aqueous solution that the PH conditioning agent is configured to certain pH value is made reaction end liquid D; 5., at the appointed time A liquid, B1 liquid and C drop are added to D liquid, silver powder is evenly grown up.
In the preparation method of above-mentioned particle size dispersibility superfine silver powder with adjustable, described PH conditioning agent is acetic acid, nitric acid or alkaline PH conditioning agent; Alkalescence PH conditioning agent is one or more in sodium carbonate, NaOH, the ammoniacal liquor; Surfactant is one or more in gelatin, polyvinyl alcohol, natural gum, the hydroxyethylcellulose.Concentration of silver ions 50～the 150g/L of described silver-colored solution A; Ascorbic acid concentrations 100～200g/L.Described ph value of reaction scope is 2～7; Reaction temperature is 30～50 ℃.Described reaction mechanism is:
C
6H
8O
6+2AgNO
3＝2Ag↓+C
6H
6O
6+2HNO
3
Compared with the prior art, among the preparation method of above-mentioned particle size dispersibility superfine silver powder with adjustable, the silver powder particle size can be regulated easily, widen application by conditioned reaction liquid pH value; Adopt alkaline matter neutralization reaction accessory substance nitric acid, stopping reaction system pH value, the control reaction temperature makes the silver powder particle size uniformity good.This liquid phase chemical reduction method, need not post processing, direct step preparation high dispersibility superfine silver powder, this silver powder microscopic appearance is polyhedron, have good dispersion, narrow particle size distribution, tap density height, characteristics that sintering character is good, be suitable for preparing solid content height, printing lines precision height, the low silver paste of shrinkage factor requirement, be specially adapted to sheet sense electrode size, LTCC silver paste, solar cell and PDP silver slurry etc., have the low characteristics of high conductivity, densification and shrinkage factor after the sintering film forming, the end product excellent performance.
Description of drawings
Fig. 1 is the SEM figure of embodiment 1 gained silver powder;
Fig. 2 is the SEM figure of embodiment 3 gained silver powder;
Fig. 3 is the SEM figure of embodiment 5 gained silver powder.
The specific embodiment
Purport of the present invention is by control temperature, reinforced time and selects suitable surfactant for use, and the conditioned reaction pH value makes that the silver powder particle size can be regulated easily, good uniformity.Below in conjunction with embodiment content of the present invention is described in further detail, mentioned content is not a limitation of the invention among the embodiment, and the selection of temperature, time and material can be suited measures to local conditions and the result be there is no substantial effect among the preparation method.
At first, summary preparation method's of the present invention basic scheme: a kind of preparation method of particle size dispersibility superfine silver powder with adjustable, step is: 1., silver nitrate, surfactant dissolves are configured to silver-colored solution A in water; 2., ascorbic acid, PH conditioning agent and surfactant dissolves are configured to reducing solution B in water; 3., with alkaline PH conditioning agent configuration alkaline aqueous solution C; 4., at the appointed time drip C liquid and A liquid in the B liquid, silver powder is evenly grown up;
Perhaps: 1., silver nitrate, surfactant dissolves are configured to silver-colored solution A in water; 2., ascorbic acid, surfactant dissolves are configured to reducing solution B1 in water; 3., with alkaline PH conditioning agent configuration alkaline aqueous solution C; 4., the aqueous solution that the PH conditioning agent is configured to certain pH value is made reaction end liquid D; 5., at the appointed time A liquid, B1 liquid and C drop are added to D liquid, silver powder is evenly grown up.
Embodiment 1
With 157gAgNO
3Be dissolved in 1L deionized water (hereinafter to be referred as water) with 1g natural gum, stirring and dissolving gets silver-colored solution.120g ascorbic acid and 2g natural gum are joined in the 1L water, and adding PH conditioning agent adjustment PH is 3, gets reducing solution.The control reaction temperature is in (30～35) ℃, in 30min, Ag-containing solution is added drop-wise in the reducing solution, the ph value of reaction of dropping sodium solution control simultaneously is 3 ± 0.5, stir 15min after adding again, staticly settle, wash with water powder to the filtrate electrical conductivity less than 100 μ s/cm, filter is done the back in 60 ℃ of dryings, after the screening silver powder.The powder testing result: the SEM picture of powder is seen accompanying drawing 1, average grain diameter 4.0 μ m; Tap density 5.1g/ml; Size distribution S.D./D50 is 0.425.
Embodiment 2
It is consistent with embodiment one that embodiment 1 material usage is enlarged 200 times, other technical process.Powder testing result: powder average grain diameter 3.8 μ m; Tap density 4.9g/ml; Size distribution S.D./D50 is 0.451.
Embodiment 3
With 157gAgNO
3Be dissolved in 1L water with the 0.5g gelatin, stirring and dissolving gets silver-colored solution.120g ascorbic acid and 2g gelatin are joined in the 0.8L water, adjusting PH is 6, reducing solution, the control reaction temperature is added to silver-colored drips of solution in the reducing solution in 90min in (40～45) ℃, dripping sodium carbonate liquor control ph value of reaction simultaneously is 6 ± 0.5, stir 15min after adding again, staticly settle, wash with water powder to the filtrate electrical conductivity less than 100 μ s/cm, filter is done the back in 70 ℃ of dryings, gets silver powder after the screening.The powder testing result: the SEM picture of powder is seen accompanying drawing 2, average grain diameter 2.2 μ m; Tap density 4.6g/ml; Size distribution S.D./D50 is 0.462.
Embodiment 4
Reaction temperature is changed into (36～40) ℃, other materials, consumption and technology are consistent with embodiment 3.Powder testing result: powder average grain diameter 2.5 μ m; Tap density 4.5g/ml; Size distribution S.D./D50 is 0.438.
Embodiment 5
With 157gAgNO
3Be dissolved in 500ml water with 2g starch, stirring and dissolving gets silver-colored solution.120g ascorbic acid and 0.5g starch are joined 500ml water, and stirring and dissolving gets reducing solution.200ml water is added to the 2L beaker, dropping ammonia to pH value is 8, stir reaction end liquid, the control reaction temperature is in (40～45) ℃, stir, drip silver-colored solution and reducing solution in 60min, the ph value of reaction of dropping ammonia solution control simultaneously is 8 ± 0.5, stirs 15min after adding again, staticly settle, wash with water powder to the filtrate electrical conductivity less than 100 μ s/cm, filter is done the back in 60 ℃ of dryings, after the screening silver powder.The powder testing result: the SEM picture of powder is seen accompanying drawing 3, average grain diameter 1.1 μ m; Tap density 4.2g/ml; Size distribution S.D./D50 is 0.447.
Embodiment 6
Material usage is enlarged 200 times, and the reinforced time changes 100min into, and other process conditions are consistent with embodiment 5.Powder testing result: powder average grain diameter 1.3 μ m; Tap density 4.0g/ml; Size distribution S.D./D50 is 0.469.
Claims (5)
1. the preparation method of a particle size dispersibility superfine silver powder with adjustable, step is:
1., silver nitrate, surfactant dissolves are configured to silver-colored solution A in water;
2., ascorbic acid, PH conditioning agent and surfactant dissolves are configured to reducing solution B in water;
3., with alkaline PH conditioning agent configuration alkaline aqueous solution C;
4., at the appointed time drip A liquid and C liquid in the B liquid, silver powder is evenly grown up;
Perhaps:
1., silver nitrate, surfactant dissolves are configured to silver-colored solution A in water;
2., ascorbic acid, surfactant dissolves are configured to reducing solution B1 in water;
3., with alkaline PH conditioning agent configuration alkaline aqueous solution C;
4., the aqueous solution that the PH conditioning agent is configured to certain pH value is made reaction end liquid D;
5., at the appointed time A liquid, B1 liquid and C drop are added to D liquid, silver powder is evenly grown up.
2. the preparation method of particle size dispersibility superfine silver powder with adjustable according to claim 1 is characterized in that: described PH conditioning agent is acetic acid, nitric acid or alkaline PH conditioning agent; Alkalescence PH conditioning agent is one or more in sodium carbonate, NaOH, the ammoniacal liquor; Surfactant be a kind of or several in gelatin, polyvinyl alcohol, hydroxyethylcellulose, pectin, the polyvinylpyrrolidone and.
3. the preparation method of particle size dispersibility superfine silver powder with adjustable according to claim 2 is characterized in that: the concentration of silver ions 50～150g/L of described silver-colored solution A; Ascorbic acid concentrations 100～200g/L.
4. the preparation method of particle size dispersibility superfine silver powder with adjustable according to claim 3 is characterized in that: described ph value of reaction scope is 2～9,30～50 ℃ of reaction temperatures.
5. the preparation method of particle size dispersibility superfine silver powder with adjustable according to claim 3 is characterized in that: described reaction mechanism is
C
6H
8O
6+2AgNO
3＝2Ag↓+C
6H
6O
6+2HNO
3
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