CN101462164A - High-tap density micro aluminum powder and method for producing the same - Google Patents
High-tap density micro aluminum powder and method for producing the same Download PDFInfo
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- CN101462164A CN101462164A CNA2009101024125A CN200910102412A CN101462164A CN 101462164 A CN101462164 A CN 101462164A CN A2009101024125 A CNA2009101024125 A CN A2009101024125A CN 200910102412 A CN200910102412 A CN 200910102412A CN 101462164 A CN101462164 A CN 101462164A
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Abstract
The invention discloses minute silver powder with high tap density and a method for producing the same. The silver powder has the following properties: the average particle diameter of the silver powder is between 0.3 and 1.5 mu m; the tap density of the silver powder is not less than 4.5g/cm<3>; and the contraction rate of the silver powder is less than or equal to 19 percent after the silver powder is sintered at the temperature of less than or equal to 900 DEG C. The production method comprises: (1) preparing a solution containing silver ions for standby; (2) preparing a reducer aqueous solution containing a dispersant for standby; (3) preparing a treatment solution containing a treating agent for standby; (4) mixing and reacting the solution containing the silver ions and the reducer solution containing the dispersant for reducing the silver ions to silver particles; (5) filtering out a reaction solution, and cleaning the silver particles by deionized water; (6) pumping and leaching the cleaned silver powder, putting the cleaned silver powder into the treatment solution for treatment; and subsequently, filtering out the treatment solution; and (7) drying the silver powder in a vacuum oven; and pulverizing the dried silver powder to obtain the minute silver powder with high tap density. Silver slurry prepared from the silver powder is printed on a magnet body or a substrate, is sintered at temperature of less than or equal to 900 DEG C and has good matching property with the magnet body or the substrate. The minute silver powder is suitable for a manufacturer for producing an electronic element.
Description
Technical field
The processing of the present invention and metal dust is relevant with the improvement of character, in particular to high-tap density micro aluminum powder and production method thereof.
Technical background
The chip electronic device, resistance for example, electric capacity, inductance, circuit board printed circuit adopt metal paste to form certain pattern by modes such as printing, dip-coatings more, form conductor then behind sintering.Conventional metal paste contains compositions such as metal powder, organic solvent, macromolecule resin, inorganic oxide, dispersant, glass.The production method of used silver powder mostly is chemical reduction method in traditional preparation slurry.But traditional chemical reduction method is difficult for making granularity＜1.5 μ m, tap density is not less than 4.5g/cm
3Silver powder.But along with the miniaturization of electronic product, require electronic component more and more littler, its internal circuit will inevitably be more and more thinner, and this just requires silver powder to want thin.Some Chinese patent application parts have appearred in super fine silver powder production, No. 200480020987.8 " manufacture method of particulate silver powder and particulate silver powder thereof " and No. 200480020988.2 " manufacture method of particulate silver powder and particulate silver powder thereof " of Mitsui metal mining industry Co., Ltd. application for example, No. 200410009079.0 " a kind of preparation of industrialization technology of nano-scale silver powder " of University of Science ﹠ Technology, Beijing's application, No. 200810047433.7 " industrialized process for preparing of the spherical porous silver powder of a kind " of Wuhan University of Technology's application, No. 200810097399.4 " preparation methods of high dispersed superfine spherical silver powder for conductive silver slurry " of Jinchuan Group Co.,Ltd's application etc.The silver powder granularity is all paid close attention in these inventions, but does not all pay attention to the tap density of silver powder; Yet the silver powder tap density is little, and the contraction of silver lines can not be mated with the contraction phase of magnet or substrate just greatly when burning till, and will cause metal wire to break, and forms open circuit.Up to now, do not see the patent application of high tap density silver powder.
Summary of the invention
The object of the present invention is to provide a kind of high-tap density micro aluminum powder, it has certain fineness, also has high-tap density and low-shrinkage.
Another purpose of the present invention provides the production method of this high-tap density micro aluminum powder.
The inventor finds after deliberation: average grain diameter 0.3～1.5 μ m, tap density is not less than 4.5g/cm
3Silver powder, do form slurry after, can well print out the silver-colored lines of wide 50 μ m when being made into slice component.Burning till the silver-colored lines in back can mate with magnet or substrate, does not occur rupturing and arching upward.Therefore, the high-tap density micro aluminum powder that the inventor provides is the silver powder with following characteristic: its average grain diameter is 0.3～1.5 μ m, and tap density is not less than 4.5g/cm
3, burn till back silver powder shrinkage factor≤19% at≤900 ℃.
The production method of the high-tap density micro aluminum powder that the inventor provides comprises: 1. prepare the argentiferous ion solution, and standby; 2. preparation contains the reducing agent aqueous solution of dispersant, and is standby; 3. preparation contains the treatment fluid of inorganic agent, and is standby; 4. the argentiferous ion solution is mixed with the reductant solution that contains dispersant, it is reacted, the particulate of silver ion reduction Cheng Yin; 5. the elimination reactant liquor is used washings cleaning silver particulate; 6. after washed silver powder suction filtration being done, put into after the treatment fluid processing suction filtration elimination treatment fluid; 7. silver powder is dried in vacuum drying oven, the silver powder after the oven dry promptly obtains high-tap density micro aluminum powder through pulverizing.
In the first step of said method, described argentiferous ion solution is liquor argenti nitratis ophthalmicus or silver salt complex or the aqueous solution of silver-colored intermediate or slurry; Wherein the silver salt complex adds ammoniacal liquor, ammonia salt, chelate and makes in liquor argenti nitratis ophthalmicus; The silver intermediate adds NaOH, sodium carbonate, sodium acid carbonate and makes in liquor argenti nitratis ophthalmicus.
The inventor points out that preferred silver nitrate aqueous solution of argentiferous ion solution or silver nitrate add the solution of ammoniacal liquor, use this solution can obtain the silver particles of better granularity and particle shape.
In second step of said method, described reducing agent is at least a in formaldehyde, alkanolamine, sodium borohydride, hydrazine hydrate or ascorbic acid, the glucose; Described dispersant is at least a in aliphatic acid, soap, surfactant, the polymer substance.
In the 3rd step of said method, described inorganic agent is at least two kinds in acetone, cyclohexanone, hexane, ethanol, aliphatic acid, soap, surfactant, the polymer substance.
More than aliphatic acid in two steps comprise propionic acid, butyric acid, sad, laurate, myristic acid, palmitic acid, palmitic acid, stearic acid, leukotrienes, linoleic acid, oleic acid, arachidic acid, arachidonic acid, mountain Yu's acid; Soap comprises by aliphatic acid and lithium, sodium, potassium, calcium, magnesium, barium, zinc, copper, aluminium, iron, the formed salt of tin; Surfactant comprises that anion surfactant is odium stearate, dodecyl sodium sulfate, sldium lauryl sulfate, dioctyl sodium sulfosuccinate, triethanolamine soap, comprise that also cationic surfactant is dodecyl bromination ammonia, cetyl chloride ammonium, comprise that also zwitterionic surfactant is lecithin, sodium lauroyl glutamate, lauramide betaine, lauryl imidazoline; Comprise that also non-ionic surface active agent is glycerin monostearate, sucrose ester, T-80, T20; The polymer colloid material comprises gelatin, gelatine, xanthans, pectin, agar-agar, Arabic gum, tragacanth gum, locust bean gum, rubber made from soybean cake, polyvinyl alcohol, polyethylene glycol, polyethylene glycol oxide, HPMA, polyacrylic acid, polymethylacrylic acid, methylcellulose, ethyl cellulose, hydroxyethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, carboxymethyl hydroxyethyl cellulose, CMS, carboxyethyl starch, cyanoethyl starch, acetic starch, starch phosphate, cationic starch, polymerization starch, wheaten starch, potato starch, sweet potato starch, ground rice starch.
In the 4th step of said method, the concentration of described argentiferous ion solution is 7%～15%, and the concentration of described reductant solution is 4%～20%; The time of reduction reaction was controlled in 30～120 minutes.
In the 5th step of said method, described washings are deionized waters.
In the 6th step of said method, described to put into the time that treatment fluid handles be 30～120 minutes.
In the 7th step of said method, the temperature that described silver powder is dried in vacuum drying oven is 35 ℃～80 ℃, and vacuum is-0.08MPa.
The powder that adopts the inventive method to make is surveyed its particle diameter under Electronic Speculum, the diameter of silver-colored particle is many between 0.3～1.5 μ m as can be known.The tap density of measuring silver powder on multi-functional powder tester is〉4.5g/cm
3Weigh up 1g silver powder, be pressed into silver and buckle in mould, the speed that puts it in the sintering furnace with 10 ℃/min rises to 900 ℃ and constant temperature 2h, measure the silver-colored diameter of detaining after allowing it cool off naturally to be punctured into＜19%, high shrinkage is＜19%.Organic solvent (terpinol) with 80 weight portion silver powder, 4 weight portion macromolecule resins, 16 weight portions mixes again, is kneaded into the silver slurry on three-roller.The 400 order stainless steel cloths of silver slurry with special pattern are imprinted on magnet or the substrate, after the oven dry, examine under a microscope full, the non-cracking of wide 50 μ m lines that prints off.Electric property is no abnormal after being used for making slice component, and magnet or substrate and the no cracking phenomena of silver-colored wire bonds branch.
High-tap density micro aluminum powder provided by the invention and production method thereof can make the silver powder with following characteristic: its average grain diameter is 0.3～1.5 μ m, and density (tap density) is not less than 4.5g/cm
3, burn till back silver powder shrinkage factor≤19% at≤900 ℃; The silver slurry made from this silver powder is printed in the slice component, and burning till the back at≤900 ℃ has good matching with magnet or substrate.Be applicable to the producer that produces electronic element.
The specific embodiment
Following examples can illustrate the present invention better:
Embodiment 1 at first adds the 10mL concentrated ammonia liquor in the 200mL liquor argenti nitratis ophthalmicus that contains the 23.6g silver nitrate, stir, and is standby.Then in the 400mL reductant solution that contains the 20g hydrazine hydrate, add 1.0g dodecyl sodium sulfate and 0.2g polyvinylpyrrolidone K
30, stir and make its dissolving, standby.In stirring, above-mentioned liquor argenti nitratis ophthalmicus is joined in 30min in the above-mentioned reductant solution, can restore silver-colored particle.Afterwards reactant liquor is filtered, with deionized water cleaning silver particle.After washed silver powder suction filtration done, put into inorganic agent solution and handle 60min.The treatment fluid suction filtration is fallen, silver powder is dried in vacuum drying oven, the silver powder after the oven dry is pulverized and is got final product.
Embodiment 2 at first adds the 10mL concentrated ammonia liquor in the 200mL liquor argenti nitratis ophthalmicus that contains the 23.6g silver nitrate, stir, and is standby; In the 400mL reductant solution that contains the 24g ascorbic acid, add 2.0g NaOH and 2g Tween 80, stir and make its dissolving.Liquor argenti nitratis ophthalmicus is joined in 50min in the reductant solution, can restore silver-colored particle.Reactant liquor is filtered, with deionized water cleaning silver particle.After washed silver powder suction filtration done, put into inorganic agent solution and handle 60min; The treatment fluid suction filtration is fallen, silver powder is dried in vacuum drying oven, the silver powder after the oven dry is pulverized and is got final product.
The silver powder that the foregoing description is made is surveyed its particle diameter under Electronic Speculum, can find out that the diameter of silver-colored particle is many between 0.3～0.9 μ m.The tap density embodiment 1 that measures silver powder on multi-functional powder tester is 4.76g/cm
3, embodiment 2 is 4.64g/cm
3Weigh up 1g silver powder, being pressed into silver in mould buckles, the speed that puts it in the sintering furnace with 10 ℃/min rises to 900 ℃ and constant temperature 2h, the diameter of measuring the silver powder silver button of embodiment 1 after allowing it cool off naturally is punctured into 15.4%, high shrinkage is 17.1%, the diameter of the silver powder silver button of embodiment 2 is punctured into 17.5%, and high shrinkage is 16.4%.Organic solvent (terpinol) with 80 weight portion silver powder, 4 weight portion macromolecule resins, 16 weight portions mixes respectively, is kneaded into the silver slurry on three-roller.The 400 order stainless steel cloths of silver slurry with special pattern are imprinted on magnet or the substrate, after the oven dry, examine under a microscope the 50 μ m lines that print off, full, the non-cracking of lines.Electric property is no abnormal after sending producer to make element, and magnet or substrate and the no cracking phenomena of silver-colored wire bonds branch.
Claims (10)
1 one kinds of high-tap density micro aluminum powders are the silver-colored particulates that obtain by the reducing agent reduction with the argentiferous ion solution, and it is characterized in that this silver powder has following characteristic: average grain diameter is 0.3～1.5 μ m, and tap density is not less than 4.5g/cm
3, burn till back silver powder shrinkage factor≤19% at≤900 ℃.
The method of the described high-tap density micro aluminum powder of 2 production claims 1 is characterized in that comprising: 1. prepare the argentiferous ion solution, and standby; 2. preparation contains the reducing agent aqueous solution of dispersant, and is standby; 3. preparation contains the treatment fluid of inorganic agent, and is standby; 4. the argentiferous ion solution is mixed with the reductant solution that contains dispersant, make its reaction, silver ion reduction is become silver-colored particulate; 5. the elimination reactant liquor is used washings cleaning silver particulate; 6. after washed silver powder suction filtration being done, put into treatment fluid and handle, afterwards the elimination treatment fluid; 7. silver powder is dried in vacuum drying oven, the silver powder of oven dry promptly obtains high-tap density micro aluminum powder through pulverizing.
3 in accordance with the method for claim 2, it is characterized in that in the first step of described method, and the argentiferous ion solution is liquor argenti nitratis ophthalmicus or silver salt complex or the aqueous solution of silver-colored intermediate or slurry; Wherein the silver salt complex adds ammoniacal liquor, ammonia salt, chelate and makes in liquor argenti nitratis ophthalmicus; The silver intermediate adds NaOH, sodium carbonate, sodium acid carbonate and makes in liquor argenti nitratis ophthalmicus.
4 in accordance with the method for claim 2, it is characterized in that in second step of described method, described reducing agent be formaldehyde, alkanolamine, sodium borohydride, hydrazine hydrate or ascorbic acid,, at least a in the glucose; Described dispersant is at least a in aliphatic acid, soap, surfactant, the polymer substance.
5 in accordance with the method for claim 2, it is characterized in that described inorganic agent is at least two kinds in acetone, cyclohexanone, hexane, ethanol, aliphatic acid, soap, surfactant, the polymer substance in the 3rd step of described method.
6 according to the described method in one of claim 4 or 5, it is characterized in that described aliphatic acid comprises propionic acid, butyric acid, sad, laurate, myristic acid, palmitic acid, palmitic acid, stearic acid, leukotrienes, linoleic acid, oleic acid, arachidic acid, arachidonic acid, mountain Yu's acid; Soap comprises by aliphatic acid and lithium, sodium, potassium, calcium, magnesium, barium, zinc, copper, aluminium, iron, the formed salt of tin; Surfactant comprises that anion surfactant is odium stearate, dodecyl sodium sulfate, sldium lauryl sulfate, dioctyl sodium sulfosuccinate, triethanolamine soap, comprise that also cationic surfactant is dodecyl bromination ammonia, cetyl chloride ammonium, comprise that also zwitterionic surfactant is lecithin, sodium lauroyl glutamate, lauramide betaine, lauryl imidazoline; Comprise that also non-ionic surface active agent is glycerin monostearate, sucrose ester, T-80, T20; The polymer colloid material comprises gelatin, gelatine, xanthans, pectin, agar-agar, Arabic gum, tragacanth gum, locust bean gum, rubber made from soybean cake, polyvinyl alcohol, polyethylene glycol, polyethylene glycol oxide, HPMA, polyacrylic acid, polymethylacrylic acid, methylcellulose, ethyl cellulose, hydroxyethylcellulose, hydroxypropyl cellulose, hydroxypropyl methylcellulose, carboxymethyl hydroxyethyl cellulose, CMS, carboxyethyl starch, cyanoethyl starch, acetic starch, starch phosphate, cationic starch, polymerization starch, wheaten starch, potato starch, sweet potato starch, ground rice starch.
7 in accordance with the method for claim 2, it is characterized in that the concentration of described argentiferous ion solution is 7%～15% in the 4th step of described method, and the concentration of described reductant solution is 4%～15%; The time of reduction reaction was controlled in 30～120 minutes.
8 in accordance with the method for claim 2, it is characterized in that described washings are deionized waters in the 5th step of described method.
9 in accordance with the method for claim 2, it is characterized in that in the 6th step of described method, and described to put into the time that treatment fluid handles be 60 minutes.
10 in accordance with the method for claim 2, it is characterized in that the temperature that described silver powder is dried in vacuum drying oven is 35 ℃～80 ℃ in the 7th step of described method, and vacuum is-0.08MPa.
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