CN102407342A - Preparation method of nano silver powder with accurately controllable particle size - Google Patents
Preparation method of nano silver powder with accurately controllable particle size Download PDFInfo
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Abstract
The invention relates to a preparation method of nano silver powder with accurately controllable particle size. Silver nitrate is used as a starting raw material, and reacts with a precipitator to form uniform silver-containing precursor precipitate, and then a reducing agent is added to reduce the silver-containing precursor precipitate under the condition of adding silver seed crystals to obtain simple substance silver. The obtained silver powder particles are polyhedral or approximately spherical, the powder has good dispersibility and uniform particle size distribution, and the particle size of the silver powder can be accurately controlled within the range of 20-300 nm by controlling the size and the adding amount of the seed crystal. The invention is a method for preparing the aqueous solution system of the nano silver powder, which can accurately control the grain diameter of the silver powder under the reaction condition of normal temperature and pressure and is suitable for large-scale production. The preparation method has the advantages of mild reaction conditions, simplicity, convenience, low cost and stable quality.
Description
Technical field
The present invention relates to the preparation method of the nano-silver powder that a kind of particle diameter can accurately control, belong to field of inorganic chemical engineering.
Background technology
Argent has excellent physicochemical characteristics, like normal temperature electric conductivity, the thermal conductivity of optimum, and the strongest reflection characteristic, the photosensitive imaging characteristic, anti-inflammation characteristics etc. make it be widely used in the modern industry field.Silver also is the noble metal of the most cheap resistance to high temperature oxidation, utilizes its electrical and thermal conductivity performance, and silver powder is applied to electrocondution slurry, makes it become the indispensable functional material of electronics industry.Because the particle diameter of nano-silver powder is little, active high; Can effectively regulate and improve the parameters such as viscosity, rheological characteristic, thixotropy and sintering activity of conductive silver slurry; Light, little, thin trend along with electric continuous development makes nano-silver powder become one of main application direction in the microelectronics industry field; In addition, utilize the anti-inflammation characteristic of Nano Silver, use it for fields such as antibacterial fabric, plastics, pottery, coating, Medical dressing, also demonstrate tempting prospect.
The production method of silver powder can be divided into physics method and chemical method simply, and the physics method comprises plasma gas phase condensation method, atomization (water atomization, aerosolization) etc., and chemical method comprises thermal decomposition method, liquid phase reduction etc.The characteristics of physics method are that output is big, product degree of crystallinity is high; But still there is a difficult problem at aspects such as production equipment design, technology controlling and process; More crucial is that the silver powder that the physics method is produced basically all arrives tens of microns at several microns; And the particle diameter of silver powder distributes wide, and yield is low, has therefore limited its application (referring to CN1164452A).Chemical reduction method is to study more thorough, most widely used silver powder preparation method at present; Its production equipment is simple, technological process is simple and easy to control; Especially for the preparation of nano-silver powder; Utilize the solution nucleation of middle crystal and stablizing and dispersion theory of Growth Control and nano-colloid particle mutually, be expected to realize that the control of particle morphology and size is synthetic.Over past ten years; The liquid phase chemical reduction legal system is equipped with nano-silver powder and has obtained plentiful and substantial achievement in research; Add conditions such as speed, whipped form through regulator solution concentration, pH value, reaction temperature, reducing agent kind, reducing agent; Realized the size Control synthetic (referring to Angew.Chem.Int.Ed.2009,48,60) of silver nano material.But still there are some defectives in the silver-colored nano powder of the preparation of liquid phase control at present.At first, most methods need adopt control devices such as organic solvent, pyroreaction or microwave, ultraviolet lighting, and in water solution system, the nano-silver powder of normal temperature and pressure reaction control preparation different size is still a challenge (referring to Chem.Eur.J.2005,11,454); Secondly; Size Control for silver powder; Before obtaining experimental result, can only do qualitative estimation (become big or diminish) to the product size like size, can't design in advance and realize that through the regulation and control response parameter accurate and quantitative control synthesizes (referring to Acc.Chem.Res.2007 the product size; 40,1067); In addition, for obtaining nano-silver powder, control solution mutually in the growing up of silver-colored particle, often adopt the silver ion solution of low concentration, production efficiency obviously descend (referring to CN1653907A).Therefore, adopt the silver-colored nano powder of liquid-phase reduction technology preparation, countries in the world also are difficult to accomplish scale production at present.
Summary of the invention
To the deficiency of prior art, the present invention provides the preparation method of the nano-silver powder that a kind of particle diameter can accurately control.
The present invention is under the normal temperature and pressure reaction condition, can accurately control the water solution system preparation method of the nano-silver powder of silver powder particle diameter, suitable large-scale production.With the silver nitrate is initiation material, forms uniform argentiferous presoma deposition with the precipitating reagent reaction earlier, under the condition that adds silver-colored crystal seed, adds reducing agent reduction argentiferous presoma deposition and obtains simple substance silver then.Can in 20～300nm scope, accurately control the particle diameter of silver powder through control crystal seed size and addition.
Technical scheme of the present invention is following:
The preparation method of the silver powder that a kind of particle diameter can accurately be controlled may further comprise the steps:
(1) preparation of crystal seed
Polymer calculates with monomer; Earlier with dispersant I and silver nitrate in molar ratio 1～100: 1 is dissolved in the water; Forming silver nitrate concentration is 0.01～20.0mmol/L mixed solution I, stirs the solution that adds reducing agent I down then, continues stirring reaction and forms the Nano Silver crystal seed; Wherein, dispersant I is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination; Reducing agent is one of sodium borohydride, hydrazine hydrate, ascorbic acid or hydrogen peroxide solution or combination; The mol ratio of reducing agent I and silver nitrate is 0.2～3: 1.
(2) preparation of argentiferous presoma deposition
1. earlier complexing agent and silver nitrate are dissolved in the water, forming silver nitrate concentration is the mixed solution I I of 0.1～2.0mol/L; Wherein, described complexing agent is one of citric acid, trisodium citrate, enuatrol, ammoniacal liquor, polyvinylpyrrolidone, formamide, polyacrylic acid or combination; Wherein polymer calculates with monomer, and the mol ratio of complexing agent and silver nitrate is 0.1～10: 1;
2. the crystal seed that again dispersant II, precipitating reagent and step (1) is prepared is scattered in and forms mixed solution I II in the water;
Described dispersant II is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination; Described precipitating reagent is one of oxalic acid, sodium oxalate, carbonic hydroammonium, sodium carbonate, phosphoric acid, sodium phosphate, hydrochloric acid, sodium chloride, NaOH, sulfuric acid, ammonium sulfate or combination;
3. under agitation, mixed solution I I is added among the mixed solution I II, stirring reaction forms uniform argentiferous presoma deposition;
(3) redox of Nano Silver micelle preparation
1. polymer calculates with monomer, is to add that dissolving forms mixed solution I V in the entry at 0.1～10: 1 in molar ratio with dispersant III and reducing agent II; Said dispersant III is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination, and reducing agent II is sodium borohydride, hydrazine hydrate, ascorbic acid or hydrogen peroxide solution;
2. dispersant IV, reaction speed controlling agent are added dissolving formation mixed solution V in the entry; Said dispersant IV is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination; The reaction speed controlling agent is ammoniacal liquor, nitric acid or NaOH; Wherein polymer calculates with monomer, and the mol ratio of reducing agent II is 0.1～10: 1 among said dispersant IV consumption and the mixed solution I V; The mol ratio of reducing agent II is 0.1～10: 1 among reaction speed controlling agent consumption and the mixed solution I V; The concentration of reaction speed controlling agent is 0.05～3.0mol/L among the mixed solution V;
3. mixed solution I V and mixed solution V constant speed are added in the argentiferous presoma deposition that step (2) makes, stirring reaction generates the Nano Silver micelle.
(4) separation of Nano Silver micelle, washing, drying and pulverizing
The Nano Silver micelle that generates in the step (3) through Separation of Solid and Liquid, washing, drying and pulverizing, is obtained nano-silver powder.
According to the present invention, preferably as follows:
In the step (1), the concentration of silver nitrate is preferably 0.1～2.0mmol/L in the mixed solution I, and the concentration of reducing agent I solution is 0.1～200.0mmol/L, further is preferably 1～20.0mmol/L; Polymer calculates with monomer, and the mol ratio of dispersant I and silver nitrate is preferably 5～50: 1; Reducing agent I is 0.5～1.5: 1 to the preferred molar ratio of silver nitrate; Reaction temperature is room temperature～100 ℃, is preferably room temperature～60 ℃; The stirring reaction time is 1～120 minute, is preferably 5～30 minutes.
Step (2) 1. in, polymer calculates with monomer, complexing agent is preferably 0.1～3 to the mol ratio of silver nitrate: 1; The concentration of silver nitrate is preferably 0.2～1.0mol/L among the mixed solution I I.
Step (2) 2. among addition and the mixed solution I I of dispersant II the mol ratio of silver nitrate be 0.1～10: 1 (polymer calculates with monomer), be preferably 0.4～3: 1; The addition of precipitating reagent is 0.5～5: 1 to the mol ratio of silver nitrate among the mixed solution I I, is preferably 1～3: 1; The consumption of crystal seed is in silver nitrate, is 0.001～5% to the ratio of silver nitrate among the mixed solution I I, is preferably 0.002～2%; The amount ratio of water is 0～5: 1 among the consumption contrast mixed solution I I of water, is preferably 0～3: 1.
Step (2) 3. in, reaction temperature is room temperature～100 ℃, is preferably room temperature～60 ℃; Reaction time is 1～120 minute, is preferably 5～30 minutes; Mixing speed is 25～1200 rev/mins, is preferably 120～600 rev/mins.
Step (3) 1. in, polymer calculates with monomer, dispersant III is preferably 0.1～3 to the mol ratio of reducing agent II: 1; Reducing agent II consumption is 0.5～3: 1 to the mol ratio of silver nitrate among the mixed solution I I, is preferably 1～2: 1; The concentration of reducing agent is 0.05～3.0mol/L among the mixed solution I V, is preferably 0.1～1.0mol/L.
The 2. middle dispersant IV consumption of step (3) is preferably 0.1～3 to the mol ratio of reducing agent II among the mixed solution I V: 1 (polymer calculates with monomer); The concentration of reaction speed controlling agent is preferably 0.1～1.0mol/L among the mixed solution V; The mol ratio of reducing agent II is preferably 0.5～3 among reaction speed controlling agent consumption and the mixed solution I V: 1.
Step (3) 3. in, reaction temperature is room temperature～100 ℃, is preferably room temperature～60 ℃; The reinforced time is 30～600 minutes, is preferably 120～300 minutes; Reaction time is 30～300 minutes, is preferably 60～180 minutes.
Preferably, the nanometer elargol described in the step (4) adopts the Separation of Solid and Liquid of suction filtration, press filtration or centrifugation, further is preferably the decanter type centrifugation.
Preferably, the Nano Silver micelle that Separation of Solid and Liquid obtains in the step (4) adopts water, absolute ethyl alcohol, washing with acetone, and further optimal way is used absolute ethanol washing again for spending deionised water earlier.
Preferably, the Nano Silver micelle in the step (4) after the washing adopts micro-wave oven, electric dry oven or vacuum drying chamber dry, and further optimal way is a vacuum drying chamber.Baking temperature described in the step (4) is 30～120 ℃, further is preferably 40～80 ℃.
Preferably, the pulverizing described in the step (4) adopts air-flow pulverizing, jaw formula to pulverize or hammer is pulverized, and further preferred grinding mode is the air-flow pulverizing.
Technical characterstic of the present invention and principle are explained as follows:
In step (1), silver nitrate is reduced the agent fast restore, forms silver-colored nanocrystal rapidly.Owing to adopt the stable and protective effect of low concentration of silver ions and dispersant, can avoid growing up and assembling of nucleus, obtain evenly, nanometer glue stable, dispersion is silver-colored, freshly prepd nanometer glue silver is as the crystal seed of next step reaction.In step (2), silver nitrate forms the presoma deposition of argentiferous with the precipitating reagent reaction and mixes with crystal seed.Adopt complexing agent can control the speed of micelle formation, adopt dispersant can stablize and protect newly-generated micelle, therefore, the argentiferous presoma that can obtain disperseing precipitates and forms uniform the mixing with crystal seed.In step (3), argentiferous presoma deposition is reduced and forms the Nano Silver micelle.The argentiferous presoma is precipitated as slightly soluble compound, through its dissolving ionization equilibrium, can control release and continue to provide silver ion, and can keep concentration of silver ions low in the reaction system, grows up rapidly to avoid nano-Ag particles; Dispersant can stablize with the protective reaction system in silver-colored particle, avoid particle aggregation growth Nano Silver micelle to obtain disperseing; The reaction speed controlling agent can be controlled the formation speed of redox reaction speed and simple substance silver, avoids homogeneous nucleation in the reaction system and forms new silver-colored nucleus, with the simple substance silver evenly growth on the crystal seed that provides in advance that impels reduction to form.Because the generation of having avoided new nucleus and agglomeration of particles growth, so the consumption of particle diameter, consumption and argentiferous presoma that can be through crystal seed is accurately controlled the particle diameter of product, the particle diameter of realization Nano Silver micelle is accurately controlled preparation.In step (4), under the situation of assurance powder recovery rate and silver powder dispersiveness, select the mode of the separation of Nano Silver micelle, washing, drying and pulverizing, obtain the nano-silver powder that particle diameter can accurately be controlled.
Compared with prior art, excellent results of the present invention is following:
1. the present invention is in 20～300nm scope, can accurately control the particle diameter of silver powder synthetic, the product good dispersion, particle diameter is evenly distributed;
2. the present invention adopts the slightly soluble compound of argentiferous to replace silver nitrate as the reaction precursor body, under the prerequisite of having controlled the concentration of silver ions that dissociates in the system, can effectively increase total concentration of silver ions, guarantees higher production efficiency;
3. water solution system of the present invention, the normal temperature and pressure reaction condition, process is easy, with low cost, steady quality, is suitable for industrial applications.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the embodiment of the invention 1 gained silver powder.
Fig. 2 is field emission scanning electron microscope (FE-SEM) photo of the embodiment of the invention 1 gained silver powder.
Fig. 3 is the FE-SEM photo of the embodiment of the invention 2 gained silver powder.
Fig. 4 is the FE-SEM photo of the embodiment of the invention 3 gained silver powder.
Fig. 5 is the FE-SEM photo of the embodiment of the invention 4 gained silver powder.
Fig. 6 is the FE-SEM photo of the embodiment of the invention 5 gained silver powder.
Fig. 7 is the FE-SEM photo of the embodiment of the invention 6 gained silver powder.
Fig. 8 is the FE-SEM photo of the embodiment of the invention 7 gained silver powder.
Fig. 9 is the FE-SEM photo of the embodiment of the invention 8 gained silver powder.
Figure 10 is the FE-SEM photo of the embodiment of the invention 9 gained silver powder.
Figure 11 is the FE-SEM photo of the embodiment of the invention 10 gained silver powder.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, further specify the present invention, but be not limited thereto.
Embodiment 1
(1) preparation of crystal seed
The component of dispersant I: 5.0g trisodium citrate (17.0mmol)+6.7g polyvinylpyrrolidone (PVP K-30 counts 60.4mmol with monomer)+18.0g enuatrol (59.1mmol);
Reducing agent I solution: be the fresh solution of 225mg sodium borohydride (5.9mmol) and the preparation of 330mL water, the about 17.9mmol/L of sodium borohydride concentration wherein, the mol ratio of silver nitrate is 1: 1 in sodium borohydride and the mixed solution I.
Said dispersant I and 1.0g silver nitrate (5.9mmol) be dissolved in form mixed solution I in the 25.0L water (wherein the mol ratio of dispersant I and silver nitrate is 23.1: 1; The concentration of silver nitrate is about 0.2mmol/L); Stir fast down; Add reducing agent I solution more rapidly, stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. complexing agent is 165g polyvinylpyrrolidone (PVP K-30 is in monomer 1.49mol) and 110g enuatrol (0.36mol);
Said complexing agent and 500g silver nitrate (2.94mol) are dissolved in formation mixed solution I I in the 10.0L water;
The mol ratio of complexing agent and silver nitrate is 0.63: 1; The concentration of silver nitrate is about 0.29mol/L among the mixed solution I I.
2. the composition of dispersant II: 330g polyvinylpyrrolidone (PVP K-30 counts 2.97mol with monomer)+220g enuatrol (0.72mol);
With said dispersant II and 500mL concentration is that 25% ammoniacal liquor (contains 6.5molNH approximately
3) add in the seed-solution of step (1) preparation, stirring and dissolving forms mixed solution I II;
Wherein the mol ratio of silver nitrate is 1.25: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 2.2: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.2% to the ratio of silver nitrate among the mixed solution I I;
3. under 500 rev/mins of stirrings, mixed solution I I is added among the mixed solution I II, stirring reaction is 10 minutes under the normal temperature, forms uniform argentiferous presoma deposition.
(3) preparation of Nano Silver micelle
1. the composition of dispersant III: identical with above-mentioned dispersant II.
With dispersant III and reducing agent II ascorbic acid 530g (3.0mol)) add and dissolve formation mixed solution I V in the 16.0L water;
Wherein dispersant III is 1.23: 1 to the mol ratio of reducing agent II; The mol ratio of silver nitrate is 1.02: 1 among ascorbic acid and the mixed solution I I; Ascorbic acid concentrations is 0.19mol/L among the mixed solution I V.
2. with the composition of dispersant IV: identical with above-mentioned dispersant II.
With dispersant IV and reaction speed controlling agent 300g NaOH (7.5mol)) add and dissolve formation mixed solution V in the 30.0L water; Wherein dispersant IV is 1.23: 1 to the mol ratio of reducing agent II among the mixed solution I V; The mol ratio of reducing agent II is 2.5: 1 among reaction speed controlling agent and the mixed solution I V; The concentration of reaction speed controlling agent is 0.25mol/L among the mixed solution V.
3. mixed solution I V and mixed solution V are added in the argentiferous presoma deposition that step (2) forms when reinforced shared (about 180 minutes) with the speed of 10.0L/h, stirring reaction is 120 minutes at normal temperatures, generates the Nano Silver micelle.
(4) separation of Nano Silver micelle, washing, drying and pulverizing
The Nano Silver micelle that generates in the step (3) is separated with high speed rotary drum sedimentation centrifuge, distinguish water and washing with alcohol 2 times again, then 50 ℃ of following vacuum drying, last air-flow is pulverized, and obtains about 300g nano-silver powder.The XRD diffracting spectrum of gained silver powder is a face-centred cubic structure simple substance silver (referring to Fig. 1), and particle is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 20nm of average grain diameter (referring to Fig. 2).
Embodiment 2
(1) preparation of crystal seed
The composition of dispersant I: 2.5g trisodium citrate (8.5mmol)+3.3g polyvinylpyrrolidone (PVP K-30 counts 29.7mmol with monomer)+9.0g enuatrol (29.6mmol);
Reducing agent I solution is: the fresh solution of 115mg sodium borohydride (3.0mmol) and 165mL water preparation, and the about 18.4mmol/L of sodium borohydride concentration wherein, the mol ratio of silver nitrate is about 1: 1 in sodium borohydride and the mixed solution I;
Said dispersant I and 500mg silver nitrate (2.94mmol) be dissolved in form mixed solution I in the 12.5L water (wherein the mol ratio of dispersant I and silver nitrate is 23: 1; The concentration of silver nitrate is about 0.2mmol/L); Stir fast down; Add reducing agent I solution more rapidly, stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 1.
2. dispersant II's consists of 330g polyvinylpyrrolidone (PVP K-30 counts 2.97mol with monomer) and 220g enuatrol (0.72mol); With dispersant II and 500mL concentration is that 25% ammoniacal liquor (contains 6.5molNH approximately
3) add in the seed-solution of step (1) preparation, adding 12.5L water again, stirring and dissolving forms mixed solution I II, and (wherein the mol ratio of silver nitrate is 1.25: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 2.2: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.1% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 1.25: 1 among the consumption contrast mixed solution I I of water).
3. form uniform argentiferous presoma deposition, with embodiment 1.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 1.The about 300g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 35nm of average grain diameter (referring to Fig. 3).
Embodiment 3
(1) preparation of crystal seed
The composition of dispersant I: 1.25g trisodium citrate (4.2mmol)+1.67g polyvinylpyrrolidone (PVP K-30 counts 15.0mmol with monomer)+4.5g enuatrol (14.8mmol);
Reducing agent I solution: the fresh solution of 56mg sodium borohydride (1.48mmol) and 82.0mL water preparation, the about 18.0mmol/L of sodium borohydride concentration wherein, the mol ratio of silver nitrate is about 1: 1 in sodium borohydride and the mixed solution I.
Dispersant I and 250mg silver nitrate (1.47mmol) be dissolved in form mixed solution I in the 6.25L water (wherein the mol ratio of dispersant I and silver nitrate is 23: 1; The concentration of silver nitrate is about 0.2mmol/L); Stir fast down; Add reducing agent I solution more rapidly, stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 1.
2. be that 25% ammoniacal liquor (contains 6.5molNH approximately with dispersant II (330g polyvinylpyrrolidone (PVP K-30 counts 2.97mol with monomer)+220g enuatrol (0.72mol)) and 500mL concentration
3) add in the seed-solution of step (1) preparation, adding 19.0L water again, stirring and dissolving forms mixed solution I II, and (wherein the mol ratio of silver nitrate is 1.25: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 2.2: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.05% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 1.9: 1 among the consumption contrast mixed solution I I of water).
3. form uniform argentiferous presoma deposition, with embodiment 1.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 1.The about 300g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 50nm of average grain diameter (referring to Fig. 4).
Embodiment 4
(1) preparation of crystal seed
The composition of dispersant I: 625mg trisodium citrate (2.1mmol)+837mg polyvinylpyrrolidone (PVP K-30 counts 7.5mmol with monomer)+2.25g enuatrol (7.4mmol);
Reducing agent I solution is: the fresh solution of 28mg sodium borohydride (0.74mmol) and 40mL water preparation, and the about 18.5mmol/L of sodium borohydride concentration wherein, the mol ratio of silver nitrate is 1: 1 in sodium borohydride and the mixed solution I;
Dispersant I and 125mg silver nitrate (0.74mmol) be dissolved in form mixed solution I in the 3.1L water (wherein the mol ratio of dispersant I and silver nitrate is 23: 1; The concentration of silver nitrate is about 0.2mmol/L); Stir fast down; Add reducing agent I solution more rapidly, stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 1.
2. the composition of dispersant II: 330g polyvinylpyrrolidone (PVP K-30 counts 2.97mol with monomer)+220g enuatrol (0.72mol); With dispersant II and 500mL concentration is that 25% ammoniacal liquor (contains 6.5molNH approximately
3) add in the seed-solution of step (1) preparation, adding 22.0L water again, stirring and dissolving forms mixed solution I II; Wherein the mol ratio of silver nitrate is 1.25: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 2.2: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.025% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 2.2: 1 among the consumption contrast mixed solution I I of water.
3. form uniform argentiferous presoma deposition, with embodiment 1.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 1.The about 300g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 65nm of average grain diameter (referring to Fig. 5).
Embodiment 5
(1) preparation of crystal seed
The composition of dispersant I: 250mg trisodium citrate (0.85mmol)+335mg polyvinylpyrrolidone (PVP K-30 counts 3.0mmol with monomer)+900mg enuatrol (3.0mmol);
Reducing agent I solution: the fresh solution of 11mg sodium borohydride (0.29mmol) and 20.0mL water preparation, the about 14.5mmol/L of sodium borohydride concentration wherein, the mol ratio of silver nitrate is 1.1: 1 in sodium borohydride and the mixed solution I.
Said dispersant I and 50mg silver nitrate (0.29mmol) be dissolved in form mixed solution I in the 1.25L water (wherein the mol ratio of dispersant I and silver nitrate is 23: 1; The concentration of silver nitrate is about 0.2mmol/L); Stir fast down; Add said reducing agent I solution more rapidly, stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 1.
2. the composition of dispersant II: 330g polyvinylpyrrolidone (PVP K-30 counts 2.97mol with monomer)+220g enuatrol (0.72mol); With dispersant II and 500mL concentration is that 25% ammoniacal liquor (contains 6.5molNH approximately
3) add in the seed-solution of step (1) preparation, adding 24L water again, stirring and dissolving forms mixed solution I II; Wherein the mol ratio of silver nitrate is 1.25: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 2.2: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.01% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 2.4: 1 among the consumption contrast mixed solution I I of water.
3. form uniform argentiferous presoma deposition, with embodiment 1.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 1.The about 300g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 80nm of average grain diameter (referring to Fig. 6).
Embodiment 6
(1) preparation of crystal seed
With dispersant I (5.0g trisodium citrate (17.0mmol)+6.7g polyvinylpyrrolidone (PVP K-30; In monomer 60.4mmol)) and 560mg silver nitrate (3.3mmol) be dissolved in and form mixed solution I in the 13.5.0L water (wherein the mol ratio of dispersant I and silver nitrate is 23.5: 1; The concentration of silver nitrate is about 0.24mmol/L), stir down fast, (reducing agent I solution is the fresh solution of 580mg ascorbic acid (3.3mmol) and the preparation of 330mL water to add reducing agent I solution more rapidly; The about 10mmol/L of ascorbic acid concentrations wherein; The mol ratio of silver nitrate is 1: 1 in ascorbic acid and the mixed solution I), stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. with complexing agent 165g polyvinylpyrrolidone (PVP K-30 is in monomer 1.49mol)) and 1000g silver nitrate (5.9mol) be dissolved in the 10.0L water and form mixed solution I I (wherein the mol ratio of complexing agent and silver nitrate is 0.25: 1; The concentration of silver nitrate is about 0.59mol/L among the mixed solution I I).
2. with dispersant II 330g polyvinylpyrrolidone (PVP K-30 is in monomer 2.97mol)) and precipitating reagent (1.0L hydrochloric acid, concentration are 36.5%, contain 6.0molHCl approximately) add in the seed-solution of step (1) preparation, stirring and dissolving forms mixed solution I II;
Wherein the mol ratio of silver nitrate is 0.5: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 1.02: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.056% to the ratio of silver nitrate among the mixed solution I I.
3. under 500 rev/mins of stirrings, mixed solution I I is added among the mixed solution I II, stirring reaction is 10 minutes under the normal temperature, forms uniform argentiferous presoma deposition.
(3) preparation of Nano Silver micelle
1. with dispersant III polyvinylpyrrolidone (PVP K-30) 330g (in monomer 2.97mol)) and reducing agent II ascorbic acid 1065g (6.05mo1) add in the 16.5L water dissolving and form mixed solution I V (wherein dispersant III is 0.49: 1 to the mol ratio of reducing agent II; The mol ratio of silver nitrate is 1.02: 1 among ascorbic acid and the mixed solution I I; Ascorbic acid concentrations is 0.36mol/L among the mixed solution I V).
2. (wherein dispersant IV is 1.23: 1 to the mol ratio of reducing agent II among the mixed solution I V dissolving in dispersant IV polyvinylpyrrolidone (PVP K-30) 330g and reaction speed controlling agent (440g NaOH (11.0mol)) the adding 30.0L water to be formed mixed solution V; The mol ratio of reducing agent II is 2.5: 1 among reaction speed controlling agent and the mixed solution I V; The concentration of reaction speed controlling agent is 0.36mol/L among the mixed solution V).
3. mixed solution I V and mixed solution V are added in the argentiferous presoma deposition that step (2) forms when reinforced shared (about 180 minutes) with the speed of 10.0L/h, stirring reaction is 120 minutes at normal temperatures, generates the Nano Silver micelle.
(4) separation of Nano Silver micelle, washing, drying and pulverizing
The Nano Silver micelle that generates in the step (3) is separated with high speed rotary drum sedimentation centrifuge, distinguish water and washing with alcohol 2 times again,, pulverize with air-flow at last, obtain about 600g nano-silver powder then 50 ℃ of following vacuum drying.The gained silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 100nm of average grain diameter (referring to Fig. 7).
Embodiment 7
(1) preparation of crystal seed
With dispersant I (1.5g trisodium citrate (5.1mmol)+2.0g polyvinylpyrrolidone (PVP K-30; In monomer 18mmol)) and 166mg silver nitrate (0.98mmol) be dissolved in and form mixed solution I in the 4.0L water (wherein the mol ratio of dispersant I and silver nitrate is 21.5: 1; The concentration of silver nitrate is about 0.24mmol/L), stir down fast, (reducing agent I solution is the fresh solution of 170mg ascorbic acid (0.97mmol) and the preparation of 100.0mL water to add reducing agent I solution more rapidly; The about 9.7mmol/L of ascorbic acid concentrations wherein; The mol ratio of silver nitrate is 1: 1 in ascorbic acid and the mixed solution I), stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 6.
2. with dispersant II (330g polyvinylpyrrolidone (PVP K-30; In monomer 2.97mol)) and precipitating reagent (1.0L hydrochloric acid; Concentration is 36.5%; Contain 6.0molHCl approximately) add in the seed-solution of step (1) preparation, add 10.0L water again, stirring and dissolving forms mixed solution I II, and (wherein the mol ratio of silver nitrate is 0.5: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 1.02: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.017% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 1: 1 among the consumption contrast mixed solution I I of water).
3. form uniform argentiferous presoma deposition, with embodiment 6.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 6.The about 600g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 150nm of average grain diameter (referring to Fig. 8).
Embodiment 8
(1) preparation of crystal seed
With dispersant I (625mg trisodium citrate (2.1mmol)+840mg polyvinylpyrrolidone (PVP K-30; In monomer 7.6mmol)) and 70mg silver nitrate (0.41mmol) be dissolved in and form mixed solution I in the 1.7L water (wherein the mol ratio of dispersant I and silver nitrate is 23.6: 1; The concentration of silver nitrate is about 0.24mmol/L), stir down fast, (reducing agent I solution is the fresh solution of 72mg ascorbic acid (0.41mmol) and the preparation of 42.0mL water to add reducing agent I solution more rapidly; The about 9.8mmol/L of ascorbic acid concentrations wherein; The mol ratio of silver nitrate is 1: 1 in ascorbic acid and the mixed solution I), stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 6.
2. with dispersant II (330g polyvinylpyrrolidone (PVP K-30; In monomer 2.97mol)) and precipitating reagent (1.0L hydrochloric acid; Concentration is 36.5%; Contain 6.0molHCl approximately) add in the seed-solution of step (1) preparation, add 12.0L water again, stirring and dissolving forms mixed solution I II, and (wherein the mol ratio of silver nitrate is 0.5: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 1.02: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.007% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 1.2: 1 among the consumption contrast mixed solution I I of water).
3. form uniform argentiferous presoma deposition, with embodiment 6.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 6.The about 600g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 200nm of average grain diameter (referring to Fig. 9).
Embodiment 9
(1) preparation of crystal seed
With dispersant I (320mg trisodium citrate (1.1mmol)+430mg polyvinylpyrrolidone (PVP K-30; Count 3.9mmol with monomer)) and 36mg silver nitrate (0.21mmol) be dissolved in and form mixed solution I in the 860mL water (wherein the mol ratio of dispersant I and silver nitrate is 23.8: 1; The concentration of silver nitrate is about 0.24mmol/L), stir down fast, (reducing agent I solution is the fresh solution of 37mg ascorbic acid (0.2lmmol) and the preparation of 22.0mL water to add reducing agent I solution more rapidly; The about 9.5mmol/L of ascorbic acid concentrations wherein; The mol ratio of silver nitrate is 1: 1 in ascorbic acid and the mixed solution I), stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) 1. the preparation of argentiferous presoma prepares mixed solution I I, with embodiment 6.
2. with dispersant II (330g polyvinylpyrrolidone (PVP K-30; Count 2.97mol with monomer)) and precipitating reagent (1.0L hydrochloric acid; Concentration is 36.5%; Contain 6.0molHCl approximately) add in the seed-solution of step (1) preparation, add 12.5L water again, stirring and dissolving forms mixed solution I II, and (wherein the mol ratio of silver nitrate is 0.5: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 1.02: 1 to the mol ratio of silver nitrate among the mixed solution I I; The consumption of crystal seed is in silver nitrate, is 0.0036% to the ratio of silver nitrate among the mixed solution I I; The consumption of water is 1.25: 1 among the consumption contrast mixed solution I I of water).
3. form uniform argentiferous presoma deposition, with embodiment 6.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 6.The about 600g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 250nm of average grain diameter (referring to Figure 10).
Embodiment 10
(1) preparation of crystal seed
With dispersant I (185mg trisodium citrate (0.63mmol)+250mg polyvinylpyrrolidone (PVP K-30; Count 2.25mmol with monomer)) and 20mg silver nitrate (0.12mmol) be dissolved in and form mixed solution I in the 500mL water (wherein the mol ratio of dispersant I and silver nitrate is 24: 1; The concentration of silver nitrate is about 0.24mmol/L), stir down fast, (reducing agent I solution is the fresh solution of 22mg ascorbic acid (0.12mmol) and the preparation of 12mL water to add reducing agent I solution more rapidly; The about 10mmol/L of ascorbic acid concentrations wherein; The mol ratio of silver nitrate is 1: 1 in ascorbic acid and the mixed solution I), stirring reaction is 10 minutes under the normal temperature, and is subsequent use as crystal seed.
(2) preparation of argentiferous presoma
1. prepare mixed solution I I, with embodiment 6.
2. with dispersant II (330g polyvinylpyrrolidone (PVP K-30; Count 2.97mol with monomer)) and precipitating reagent (1.0L hydrochloric acid; Concentration is 36.5%; Contain 6.0molHCl approximately) add in the seed-solution of step (1) preparation, add 13.0L water again, stirring and dissolving forms mixed solution I II, and (wherein the mol ratio of silver nitrate is 0.5: 1 among dispersant II and the mixed solution I I; Precipitating reagent is 1.02: 1 to the mol ratio of silver nitrate among the mixed solution I I; The ratio of silver nitrate is 0.002% among consumption of crystal seed (in silver nitrate) and the mixed solution I I; The consumption of water is 1.3: 1 among the consumption of water and the mixed solution I I).
3. form uniform argentiferous presoma deposition, with embodiment 6.
The preparation of step (3) Nano Silver micelle is with the separation of (4) Nano Silver micelle, washing, drying and pulverize all identical with embodiment 6.The about 600g of gained nano-silver powder, silver powder particles is polyhedron or almost spherical, and powder dispersity is good, particle diameter is evenly distributed, the about 300nm of average grain diameter (referring to Figure 11).
Those skilled in the art can do other and change in the present invention enlightens, change crystal seed size and type like the preparation condition through the change crystal seed, thereby change the size and the pattern of silver powder; Through the chemical composition of change crystal seed and presoma deposition, thus the chemical composition of change product; Through the temperature of change crystal seed preparation feedback or silver powder reduction reaction, thus the size of change silver powder and pattern or the like.Certainly, these all should be included within the present invention's scope required for protection according to the variation that the present invention's spirit is done.
Claims (10)
1. the preparation method of the silver powder that can accurately control of a particle diameter may further comprise the steps:
(1) preparation of crystal seed
Polymer calculates with monomer; Earlier with dispersant I and silver nitrate in molar ratio 1～100: 1 is dissolved in the water; Forming silver nitrate concentration is 0.01～20.0mmol/L mixed solution I, stirs the solution that adds reducing agent I down then, continues stirring reaction and forms the Nano Silver crystal seed;
Wherein, dispersant I is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination; Reducing agent is one of sodium borohydride, hydrazine hydrate, ascorbic acid or hydrogen peroxide solution or combination; The mol ratio of reducing agent I and silver nitrate is 0.2～3: 1;
(2) preparation of argentiferous presoma deposition
1. earlier complexing agent and silver nitrate are dissolved in the water, forming silver nitrate concentration is the mixed solution I I of 0.1～2.0mol/L; Wherein, described complexing agent is one of citric acid, trisodium citrate, enuatrol, ammoniacal liquor, polyvinylpyrrolidone, formamide, polyacrylic acid or combination; Wherein polymer calculates with monomer, and the mol ratio of complexing agent and silver nitrate is 0.1～10: 1;
2. the crystal seed that again dispersant II, precipitating reagent and step (1) is prepared forms mixed solution I II in water;
Described dispersant II is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination; Described precipitating reagent is one of oxalic acid, sodium oxalate, carbonic hydroammonium, sodium carbonate, phosphoric acid, sodium phosphate, hydrochloric acid, sodium chloride, NaOH, sulfuric acid, ammonium sulfate or combination;
3. under agitation, mixed solution I I is added among the mixed solution I II, stirring reaction forms uniform argentiferous presoma deposition;
(3) redox of Nano Silver micelle preparation
1. polymer calculates with monomer, is to add that dissolving forms mixed solution I V in the entry at 0.1～10: 1 in molar ratio with dispersant III and reducing agent II; Said dispersant III is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination, and reducing agent II is sodium borohydride, hydrazine hydrate, ascorbic acid or hydrogen peroxide solution;
2. dispersant IV, reaction speed controlling agent are added dissolving formation mixed solution V in the entry; Said dispersant IV is one of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, citric acid, trisodium citrate, enuatrol, neopelex or combination; The reaction speed controlling agent is ammoniacal liquor, nitric acid or NaOH; Wherein polymer calculates with monomer, and the mol ratio of reducing agent II is 0.1～10: 1 among said dispersant IV consumption and the mixed solution I V; The mol ratio of reducing agent II is 0.1～10: 1 among reaction speed controlling agent consumption and the mixed solution I V; The concentration of reaction speed controlling agent is 0.05～3.0mol/L among the mixed solution V;
3. mixed solution I V and mixed solution V constant speed are added in the argentiferous presoma deposition that step (2) makes, stirring reaction generates the Nano Silver micelle;
(4) separation of Nano Silver micelle, washing, drying and pulverizing
The Nano Silver micelle that generates in the step (3) through Separation of Solid and Liquid, washing, drying and pulverizing, is obtained nano-silver powder.
2. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled; It is characterized in that in the step (1), the concentration of silver nitrate is 0.1～2.0mmol/L in the mixed solution I; The concentration of reducing agent I solution is 0.1～200.0mmol/L, is preferably 1～20.0mmol/L; Polymer calculates with monomer, and the mol ratio of dispersant I and silver nitrate is 5～50: 1; Reducing agent I is 0.5～1.5: 1 to the mol ratio of silver nitrate; Reaction temperature is room temperature～100 ℃, is preferably room temperature～60 ℃; The stirring reaction time is 1～120 minute, is preferably 5～30 minutes.
3. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, step (2) 1. in, polymer calculates with monomer, complexing agent is 0.1～3: 1 to the mol ratio of silver nitrate; The concentration of silver nitrate is 0.2～1.0mol/L among the mixed solution I I.
4. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled; It is characterized in that; Step (2) 2. among addition and the mixed solution I I of dispersant II the mol ratio of silver nitrate be 0.1～10: 1 (polymer calculates with monomer), be preferably 0.4～3: 1; The addition of precipitating reagent is 0.5～5: 1 to the mol ratio of silver nitrate among the mixed solution I I, is preferably 1～3: 1; The consumption of crystal seed is in silver nitrate, is 0.001～5% to the ratio of silver nitrate among the mixed solution I I, is preferably 0.002～2%; The amount ratio of water is 0～5: 1 among the consumption contrast mixed solution I I of water, is preferably 0～3: 1.
5. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, step (2) 3. in, reaction temperature is room temperature～100 ℃, is preferably room temperature～60 ℃; Reaction time is 1～120 minute, is preferably 5～30 minutes; Mixing speed is 25～1200 rev/mins, is preferably 120～600 rev/mins.
6. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, step (3) 1. in, polymer calculates with monomer, dispersant III is 0.1～3: 1 to the mol ratio of reducing agent II; Reducing agent II consumption is 0.5～3: 1 to the mol ratio of silver nitrate among the mixed solution I I, is preferably 1～2: 1; The concentration of reducing agent is 0.05～3.0mol/L among the mixed solution I V, is preferably 0.1～1.0mol/L.
7. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, the 2. middle dispersant IV consumption of step (3) is 0.1～3: 1 (polymer calculates with monomer) to the mol ratio of reducing agent II among the mixed solution I V; The concentration of reaction speed controlling agent is 0.1～1.0mol/L among the mixed solution V; The mol ratio of reducing agent II is preferably 0.5～3 among reaction speed controlling agent consumption and the mixed solution I V: 1.
8. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, step (3) 3. in, reaction temperature is room temperature～100 ℃, is preferably room temperature～60 ℃; The reinforced time is 30～600 minutes, is preferably 120～300 minutes; Reaction time is 30～300 minutes, is preferably 60～180 minutes.
9. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, the nanometer elargol described in the step (4) adopts the Separation of Solid and Liquid of suction filtration, press filtration or centrifugation; Preferred decanter type centrifugation.
10. the preparation method of the silver powder that particle diameter as claimed in claim 1 can accurately be controlled is characterized in that, the Nano Silver micelle that Separation of Solid and Liquid obtains in the step (4) adopts water, absolute ethyl alcohol, washing with acetone; Be preferably and spend deionised water earlier, use absolute ethanol washing again; Baking temperature described in the step (4) is 30～120 ℃, is preferably 40～80 ℃; Pulverizing described in the step (4) adopts air-flow pulverizing, jaw formula to pulverize or hammer is pulverized, and preferred grinding mode is that air-flow is pulverized.
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