CN100391662C - Low loose density sheet-like silver powder preparation method - Google Patents
Low loose density sheet-like silver powder preparation method Download PDFInfo
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- CN100391662C CN100391662C CNB2005100110110A CN200510011011A CN100391662C CN 100391662 C CN100391662 C CN 100391662C CN B2005100110110 A CNB2005100110110 A CN B2005100110110A CN 200510011011 A CN200510011011 A CN 200510011011A CN 100391662 C CN100391662 C CN 100391662C
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Abstract
The present invention relates to a method for producing sheet-shaped silver powder with low loose density, which comprises the five production procedure of material selection, ball milling, primarily surface modification, drying and secondary surface modification. The silver powder with the silver content of larger than 99.95% and the granularity of 0.1 to 1 um is used as a raw material, and the silver powder is milled into balls by a wetting method under the conditions that a ball milling medium, a ball milling auxiliary agent and a liquid lubricant exist; the silver powder balls are processed by the primary chemical modification and are processed by the ball milling modification in the primarily drying method; thereby, the silver powder with low loose density is obtained. The ball milling time by the wetting method is 2 to 8 hours, which is only 1/5 of a mechanical ball milling method. The loose density of the sheet-shaped silver powder of the present invention is only 1/2 of that of the mechanical ball milling method. The present invention solves the problem that the silver powder easily precipitates and agglomerates in conducting paint. The present invention adopts surface modification processes twice, and two layers of protective films are coated on the sliver powder, wherein the first layer of the protective film is a dispersal film, and the second layer of the protective film is a directional floating film; thus, the dispersibility and the flotation of the silver powder are improved. The sheet-shaped silver powder with low loose density is the raw material for producing electromagnetic shielding paint and conducting paint, and various indexes of the sheet-shaped silver powder can satisfy the requirements of the conducting paint and the shielding paint.
Description
One, technical field:
Belong to electronic powder materials chemistry preparation field.
Two, background technology:
Along with the high speed development of hyundai electronics industry, various commercializations and domestic electronic appliances quantity increase severely.The microminiaturization of electronic circuit and element, integrated, lightweight, digitlization cause electronic product easy electromagnetic wave interference used in everyday and malfunction, image obstacle occur.Meanwhile, these electronic products itself are also outwards launched electromagnetic wave, thereby form electromagnetic pollution problem.All there are electromagenetic wave radiation in our mobile phone used in everyday, computer, television set, micro-wave oven etc.When human body is in electromagnetic field for a long time, electromagenetic wave radiation can cause endocrine system disorder, microcirculation is unbalance, central nervous system, vision system, digestive system, reproductive system, immune system are also all had in various degree influence, cause various diseases thus.Irradiation of electromagnetic waves to the harm of human body head and shoulders above people's imagination degree, become the harm greatly in people's life.Having become the important subject that each manufacturer faces so how electromagnetic wave is protected and shields, also is one of enterprise's main contents of passing through 3 " C " authentication.Solve electronic product Electromagnetic Interference and shielding problem at present, all be to use the electromagnetic shielding conductive lacquer, low loose density sheet-like silver powder is the electromagnetic shielding conductive raw materials for varnish.
Known more about the flake silver powder preparation method, be divided into Mechanical Method and chemical method.Kunming Institute of Precious Metals just adopts the mechanical ball milling method to produce flake silver powder as far back as the seventies, and mechanical ball milling is a dry ball milling, and the ball milling time is 30~50 hours, and the production cycle is long, the energy consumption height.Jiangsu Teachers University of Technology adopts planetary ball mill to produce flake silver powder, but still is dry ball milling.The mechanical ball milling method is produced the flake silver powder apparent density all greater than 1 gram per centimeter
3, be the conductor paste raw material always.But because the method production flake silver powder apparent density is bigger, is used for conductive paint and easily precipitates, lump, cause composition inequality when spraying paint, constructional difficulties.Chemical method is produced flake silver powder three kinds of ammonium formate reducing process, ethylene glycol chemical reduction method and photo-induction inducing defecation by enema and suppository.Chemical method can directly prepare flake silver powder, because it is too thin to obtain powder, thickness only is that several nanometers are to tens nanometers.When silver powder and resin coupling, be rolled into slurry, be heating and curing, along with solidification temperature raises, silver strip shrinks, and forms particle and chap, loses metallic luster and is silver gray, causes zeropoint resistance to increase, and does not have big practical value.
Three, summary of the invention
The object of the present invention is to provide a kind of low loose density sheet-like silver powder preparation method, silver content is carried out ball milling greater than 99.95% silver powder under ball milling circle matter, ball-milling additive, fluid lubricant existence condition, again through twice-modified processing, obtain low loose density sheet-like silver powder, this silver powder make a living electrogenesis magnetic screen lacquer and conductive paint needed raw material.Its every index can both satisfy conductive paint, the requirement of shielding lacquer.
The present invention realizes by the following technical solutions.
The production process of low loose density sheet-like silver powder by select materials, ball milling, one-time surface modification, drying and five parts of secondary surface modification form.
1, select materials: raw material be silver content greater than 99.95%, granularity is 0.1~1 micron a silver powder;
2, ball milling: in ball material weight ratio is that 10~50: 1 ratio adds medium ball and raw material silver powder in ball mill, medium ball adopts single sphere diameter, bulb diameter is 4~20 millimeters of φ, press the per kilogram raw material and add 5~30 gram ball-milling additives, 4~40 milliliters of liquid lubricants, 0.5~2 liter of absolute ethyl alcohol wet-milling abrasive media, rotating speed is 200~1000 rev/mins during ball milling, ball milling 2~8 hours adopts filter method that silver powder, medium ball and abrasive media are separated behind the ball milling, must ball milling after silver powder;
Described ball-milling additive is one or more in zinc stearate, calcium stearate, aluminum stearate, polyvinylpyrrolidone, molybdenum dioxide, silica, dodecoic acid, the hexadecanol.
Described fluid lubricant is a glycerine, polyethylene glycol, terpinol, one or more in the triethanolamine.
3, one-time surface modification: the preparation of one-time surface modifier is that polyvinyl alcohol, polyvinylpyrrolidone, triethanolamine metatitanic acid fat, one or more weight ratios by 1: 1 of containing in oxygen acetyl metatitanic acid fat and the stearoyl amino acid fat are taken by weighing, use deionized water dissolving, being mixed with concentration is the one-time surface modifier of 10~30g/L, silver powder behind the ball milling joins in 0.5~3 liter of one-time surface modifier by per kilogram, and the stirring time of staying is no less than 30 minutes;
4, the silver powder after modification filters, dries, and 60 ℃ of bake out temperatures get one-time surface modification silver powder;
5, secondary surface modification: the secondary surface modification adopts dry ball milling, the adding glass marble is a ball-milling medium, ratio of grinding media to material is 1~10: 1, sphere diameter is 2~6 millimeters of φ, press per kilogram one-time surface modification silver powder and add 2~15 gram secondary surface modifiers, rotating speed is 20~50 rev/mins during ball milling, 2~10 hours time, obtains low loose density sheet-like silver powder.Described secondary surface modifier is one or more in polyoxyethylene aliphatic alcohol ether, modified silicone, modified waxes powder, white carbon black, pyrophyllite, the polyene hydroxyl oligomer,
Compare advantage and the good effect that has with known technology:
1, the present invention is raw material with the super fine silver powder, the employing wet ball grinding, and 2~8 hours ball milling time only was the known mechanical ball milling method production time 1/5, and flake silver powder pine dress only is 1/2 of known technology production, and solution easily precipitates in conductive paint, agglomeration problems.
2, adopt twice surface modifying method, apply two layers of diaphragm.Ground floor is a dispersion membrane, and the second layer is directed floating film, improves the dispersiveness and the floatability of low loose density sheet-like silver powder;
3, low loose density sheet-like silver powder and existing GB GB/T1774-1995 flake silver powder product compare, and the average-size of product and density are different fully, and the low loose density sheet-like silver powder that the present invention produces is a kind of new product.The average-size of product and density contrast are as follows:
The average-size of GB product and density
The trade mark | Average-size um | Apparent density g/cm 3 | Tap density g/cm 3 |
FAgL-1 | ≤6.0 | 1.2~1.7 | 2.5~3.5 |
FAgL-2 | ≤5.0 | 1.4~1.9 | 2.7~3.8 |
FAgL-3 | ≤4.0 | 1.6~2.2 | 3.0~4.0 |
Low loose density sheet-like silver powder average-size of the present invention and density
The trade mark | Average-size um | Apparent density g/cm 3 | Tap density g/cm 3 |
PA-1D | ≤10 | 0.45~0.60 | 1.0~2.0 |
PA-2D | ≤15 | 0.50~0.65 | 1.4~2.0 |
Four, the specific embodiment:
Embodiment 1:
1, raw material: requiring the super fine silver powder granularity is 0.1~1um, and silver content is 99.96-99.98%;
2, ball milling: the stainless cylinder of steel of planetary ball mill is spent ionized water clean up, the ball grinder volume is 3 liters, the ball-milling medium diameter is 10 kilograms of the agate balls of 4 millimeters of φ, add 1 kilogram of raw material super fine silver powder, 1 liter of wet-milling abrasive media absolute ethyl alcohol, 4 milliliters of fluid lubricant glycerine, ball-milling additive zinc stearate 5 grams, 200 rev/mins of rotating speeds, 8 hours ball milling time, afterwards slip in the ball grinder is taken out, isolated by filtration, to be bonded at absolute ethyl alcohol that silver powder washes down on the ball, the gained flake silver powder cleans 3 times with absolute ethyl alcohol, treats a modification after the filtration;
3, one-time surface modification: take by weighing 10 gram polyvinyl alcohol, use deionized water dissolving, add ionized water to 1 liter, being mixed with concentration is 10 grams per liter one-time surface modifier, with silver powder behind 1 kilogram of ball milling, join in 1 liter of one-time surface modifier solution stirring at normal temperature 32 minutes; Flake silver powder after the one-time surface modification filters with filter cloth, sends into the air dry oven oven dry, 60 ℃ of bake out temperatures.Oven dry back powder disperses with powder beater;
4, secondary surface modification: the secondary surface modification adopts dry ball milling, and the adding glass marble is a ball-milling medium, and sphere diameter is 2 millimeters of φ.Add 1 kilogram of one-time surface modification silver powder; 2 kilograms of glass marbles; Secondary surface modifier modified waxes powder 2 grams; Rotational speed of ball-mill is 25 rev/mins; 6 hours time, twice-modified flake silver powder is taken out, carry out ball, powder separation, gained low loose density sheet-like silver powder average-size is 10 microns, apparent density 0.52 gram per centimeter
3, tap density 1.20 gram per centimeters
3
Embodiment 2: raw material is identical with example 1;
The stainless cylinder of steel of planetary ball mill is spent ionized water to be cleaned up, the ball grinder volume is 10 liters, the ball-milling medium diameter is 80 kilograms of the stainless steel balls of 10 millimeters of φ, 3.5 kilograms in adding raw material silver powder, 5 liters of wet-milling abrasive media absolute ethyl alcohols, 35 milliliters of fluid lubricant terpinols, ball-milling additive polyethylene are given a tongue-lashing pyrrolidone 70 grams, 400 rev/mins of rotating speeds, 4 hours ball milling time, slip in the ball grinder is taken out, isolated by filtration, to be bonded at absolute ethyl alcohol that silver powder washes down on the ball, the gained flake silver powder cleans 3 times with absolute ethyl alcohol, treats a modification after the filtration; Take by weighing 30 gram polyvinyl alcohol and 30 gram polyvinylpyrrolidone deionized water dissolvings, add ionized water to 3 liter, being mixed with concentration is 20 grams per liter one-time surface modifier, with silver powder behind 3.5 kilograms of ball millings, join in 3 liters of one-time surface modifier solutions stirring at normal temperature 35 minutes; Flake silver powder after the one-time surface modification filters with filter cloth, sends into the air dry oven oven dry, 60 ℃ of bake out temperatures, and oven dry back powder disperses with powder beater; The secondary surface modification adopts the dry ball milling mode, the adding glass marble is an abrasive media, sphere diameter is 4 millimeters of φ, add 3.5 kilograms of one-time surface modification silver powder, 25 kilograms of glass marbles, secondary surface modifier wax powder 8 grams, silicone 10 grams, rotational speed of ball-mill is 35 rev/mins, 4 hours time, twice-modified flake silver powder is taken out, carry out ball, powder separation.Gained low loose density sheet-like silver powder average-size is 15 microns, apparent density 0.61 gram per centimeter
3, tap density 1.50 gram per centimeters
3
Embodiment 3: raw material is identical with example 1; Adopt stirring ball mill, the ball grinder volume is 30 liters, the ball-milling medium diameter is 200 kilograms of the stainless steel balls of 20 millimeters of φ, 5 kilograms of raw materials of adding, 10 liters of wet-milling abrasive media absolute ethyl alcohols, 80 milliliters of fluid lubricant terpinols, 50 milliliters of glycerine, ball-milling additive polyethylene are given a tongue-lashing pyrrolidone 50 grams, zinc stearate 60 grams, 600 rev/mins of rotating speeds, 2 hours ball milling time, slip in the ball grinder is taken out, isolated by filtration, to be bonded at absolute ethyl alcohol that silver powder washes down on the ball, the gained flake silver powder cleans 3 times with absolute ethyl alcohol, treats a modification after the filtration; Take by weighing 100 gram polyvinyl alcohol, 100 gram triethanolamine metatitanic acid fat and 100 gram polyvinylpyrrolidone deionized water dissolvings, add ionized water to 10 liter, being mixed with concentration is 30 grams per liter one-time surface modifier, with silver powder behind 5 kilograms of ball millings, join in 10 liters of one-time surface modifier solutions stirring at normal temperature 35 minutes; Flake silver powder after the one-time surface modification filters with filter cloth, sends into the air dry oven oven dry, 60 ℃ of bake out temperatures, and oven dry back powder disperses with powder beater; The secondary surface modification adopts the dry ball milling mode, and adding sphere diameter is 6 millimeters glass marbles of φ, adds 5 kilograms of one-time surface modification silver powder, 50 kilograms of glass marbles, secondary surface modifier wax powder 10 grams, pyrophyllites 40 restrain, and rotational speed of ball-mill is 50 rev/mins, 10 hours time; Twice-modified flake silver powder is taken out, carry out ball, powder separation, gained low loose density sheet-like silver powder average-size is 15 microns, apparent density 0.42 gram per centimeter
3, tap density 1.20 gram per centimeters
3
Claims (1)
1. the preparation method of a low loose density sheet-like silver powder, with raw material is that silver content is greater than 99.95%, granularity is 0.1~1 micron a silver powder, in ball material weight ratio is that 10~50: 1 ratio adds in the ball mill, medium ball adopts single sphere diameter, bulb diameter is 4~20 millimeters of φ, press the per kilogram raw material and add 5~30 gram ball-milling additives, 4~40 milliliters of liquid lubricants, 0.5~2 liters of absolute ethyl alcohol wet-milling abrasive medias, rotating speed is 200~1000 rev/mins during ball milling, ball milling 2~8 hours, adopt filter method with silver powder behind the ball milling, medium ball separates with abrasive media, silver powder behind the ball milling, after one-time surface modification and secondary surface modification, obtain low loose density sheet-like silver powder, it is characterized in that:
Described one-time surface modification is that polyvinyl alcohol, polyvinylpyrrolidone, triethanolamine metatitanic acid fat, one or more modifier of containing in oxygen acetyl metatitanic acid fat and the stearoyl amino acid fat are taken by weighing by 1: 1 weight ratio, use deionized water dissolving, being mixed with concentration is the one-time surface modifier of 10~30g/L, silver powder behind the ball milling joins in 0.5~3 liter of one-time surface modifier by per kilogram, the stirring time of staying is no less than 30 minutes, silver powder after modification filters, oven dry, 60 ℃ of bake out temperatures get one-time surface modification silver powder;
Described secondary surface modification is to adopt dry ball milling, the adding glass marble is a ball-milling medium, ratio of grinding media to material is 1~10: 1, the glass sphere diameter is 2~6 millimeters of φ, press per kilogram one-time surface modification silver powder and add 2~15 gram secondary surface modifiers, rotating speed is 20~50 rev/mins during ball milling, 2~10 hours time, obtain low loose density sheet-like silver powder, described secondary surface modifier is one or more in polyoxyethylene aliphatic alcohol ether, modified silicone, modified waxes powder, white carbon black, pyrophyllite, the polyene hydroxyl oligomer.
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