CN1498707A - Micropowder method for producing copper based sheet with rare-noble metal contained - Google Patents
Micropowder method for producing copper based sheet with rare-noble metal contained Download PDFInfo
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- CN1498707A CN1498707A CNA02150170XA CN02150170A CN1498707A CN 1498707 A CN1498707 A CN 1498707A CN A02150170X A CNA02150170X A CN A02150170XA CN 02150170 A CN02150170 A CN 02150170A CN 1498707 A CN1498707 A CN 1498707A
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Abstract
A process for preparing the superfine flaky Cu-base particles containing noble metal includes loading flaky copper powder and ball grinding agent in the tubular ball grinder with hollow shaft, starting it for stirring, adding small alumina balls (1-3 mm in diameter) for grinding to make the flaky copper particles more fine and uniform, adding copper chelating agent of silver ions, stirring, flushing and discharging the liquid containing the particles.
Description
Technical field
The present invention relates to produce the ultra-fine grinding of metal in the production of electronic metal conductive powder material and generate the method for alloy simultaneously, it particularly is raw material with the flake copper, the abrasive media made from the material of special shape, size and unlike material, the mechanical energy that provides by the tubular ball mill of hollow shaft, through dry method and wet processing, produce the method that contains rare precious metal acid bronze alloy flake ultrafine powder.
Background technology
Ultrafine flake metal powder is a kind of important electron material, with polymer, additive allotment, in the mode of conduction connection, encapsulation and electromagnetic shielding, be applied to the production of electronic component such as integrated circuit, thin film switch and electrical instrumentation, in the communications electronics manufacturing industry purposes is widely arranged.The most frequently used electronic metal powder body material is a flake silver powder, has good conductivity, is difficult for the premium properties of oxidation, but cost an arm and a leg, and there is silver-colored migration problem in the application cost height under big electric current and high voltage situation.The copper price is low, and conduction is good, but there is the easy erosion problem of hot wet salt mist environment in easily oxidation, so has limited the product development application of conductive copper powder.
Summary of the invention
Technical problem to be solved by this invention is, sets up a kind of method of improving the conductive copper powder performance, produce can: save and part substitutes the product of flake silver powder.
The invention technical scheme be the invention principle be the powder that flake copper is converted into the rare precious metal acid bronze alloy, in order to obtain the premium properties of silver, niobium, nickel element and alloy thereof, strengthen the resistance to corrosion of powder granule, powder obtains even refinement simultaneously, satisfies technique for applying to carrying out under the requirement of particle shape granularity.
The present invention includes following steps: (1) is raw material with the flake copper, and the abrasive media of adapted rare precious metal niobium and nickel adopts the tubular ball mill of hollow shaft, under doing, wetting two process sections, utilize mill running, add ball-milling additive, to grind, to roll, produce and stir and stir; (2) use the alumina globule that diameter is 1～3mm instead, make sheet of copper alloy powder ultra-fine and homogenising fully, add the copper chelator of silver ion, mill running stirs, and powder liquid is discharged in flushing.
The corresponding process matched therewith condition of the present invention: in the dry process section, it is the flake copper of 1～40 μ m that raw material adopts granularity, consumption accounts for 10%～50% of whole charge weitghts, admission space accounts for 20%～50% of tube mill ball milling space, feed nitrogen or other inert gas by hollow shaft cast ball mill, mill speed exists
Scope (D is the tube mill diameter, unit: m).The abrasive media of described rare precious metal niobium and nickel is two kinds of ball-milling mediums, a kind of is to adopt bar-shaped metal niobium, diameter is 1.5～8mm, length is 10%～80% of tube mill length of straight pipe, another kind is the bead that adopts metallic nickel to make, diameter is 1.5～8mm, and two kinds of abrasive media weight ratios are 40: 60～60: 40, adds up to account for 50%～90% of charge weitght.The diameter of described bar-shaped metal niobium is 2～3mm, and use amount accounts for more than 50% of metallic nickel ball weight.In the wet processing section, use the alumina globule that diameter is 1～3mm instead, make sheet of copper alloy powder ultra-fine and homogenising fully, consumption accounts for powder and bead adds up to 5%～40% of weight.Can add ball-milling additive,, comprise that the accumulation addition that raw material is brought into is 0.1%～1% of a powder weight as stearic acid; As BTA, its accumulation addition is 0.05%～1%, in the wet processing section, is fed deionized water or is mixed use with alcohols solvent by hollow shaft cast ball mill 1～80 hour process time, and alcohols solvent is a monohydric alcohol, is preferably ethanol; Polyalcohol is preferably ethylene glycol, glycerine, triethylene-glycol, 1,4-butanediol etc., 4-60 hour process time.Add the copper chelator that contains silver ion subsequently, as alanine, glycine, serine, glycylglycine, trien, 1,2,3-triamido propane, triethanolamine, ethylenediamine etc., mill running stirred after 1～10 minute, end at hollow shaft cast ball mill feeds deionized water, keeps rotating, and washes 10-30 minute, powder liquid flows out from the other end, has arranged up to powder.
The invention has the beneficial effects as follows: flake copper is processed through method of the present invention, the mechanical energy that provides by the tubular ball mill of hollow shaft, carry out the alloying of metal and the processing of sheet ultra-fine grinding, especially use the abrasive media of the material making of special shape, size and unlike material, doing, wetting the corresponding process conditions of process section adapted, the reinforcement process effect.Produce have the rare precious metal elemental silver, the alloying sheet superfine powder of niobium, nickel premium properties, strengthened the non-oxidizability of conductive copper powder and the application reliability of high temperature hygrothermal environment, the powder granule refinement is even, particle mean size can reach 1～3.5 μ m.Can be used as printing electric slurry, bonding, brushing shielding material, partly substitute flake silver powder and use, niobium, nickel price are relatively cheap in addition, thus reduced the production cost of electronic product, thus obtain favorable economic benefit.
The specific embodiment
Embodiment 1
With particle mean size is the copper powder of 8.5 μ m, stearic acid content 0.7%; φ 3mm nickel ball, niobium rod 6kg, replenish φ 3 stainless steel bars, bead 8kg, four fluorine ethylene spinning joints lead to nitrogen, processed 8 hours with rpm=40, φ 300 * 1000 tube mills: φ 3 alumina balls that change 95% content, with proportioning 30: 100 13 liters of ethanol, deionized water mixed liquors, process after 16 hours, the alanine addition product that adds argentiferous 150g, turned round 10 minutes, feed deionization washing 20 minutes, the centrifuge that powder liquid flow into to rotate dries, and ethanol dehydration makes the ultrafine flake copper powder 3kg of rare precious metal alloy strengthening.
Embodiment 2
Adopting granularity is the flake copper of 24 μ m, and consumption accounts for 15% of whole charge weitghts, and admission space accounts for 25% of tube mill ball milling space.Feed nitrogen by the grinding machine hollow shaft, mill speed exists
Scope, (D is the tube mill diameter, unit: m).Add ball-milling additive,, comprise that the accumulation addition that raw material is brought into is 0.7% of a powder weight as stearic acid; BTA, ethanol melts, and addition is 0.05%, 32 hours process times,, feed deionized water and mix use with alcohols solvent by the grinding machine hollow shaft in the wet processing section, alcohols solvent is an ethanol, and glycerine, the triethylene-glycol of trace, 16 hours process times.Adding subsequently contains the copper chelator triethanolamine of silver ion etc., and mill running stirred after 10 minutes, and the end feeding deionized water at the grinding machine hollow shaft keeps rotating, and washes 10～30 minutes, and powder liquid flows out from the other end, obtains the fine powder of 3.5 μ m through sedimentation.
Embodiment 3
Adopting granularity is the flake copper of 10 μ m, and consumption accounts for 25% of whole charge weitghts, and admission space accounts for 35% of tube mill ball milling space.Feed nitrogen by the grinding machine hollow shaft, mill speed is in the scope of 25 √ D, and (D is the tube mill diameter, unit: m).Add ball-milling additive,, comprise that the accumulation addition that raw material is brought into is 0.5% of a powder weight as stearic acid; BTA, ethanol melts, and addition is 0.08%, 22 hours process times,, feed deionized water and mix use with alcohols solvent by the grinding machine hollow shaft in the wet processing section, alcohols solvent is an ethanol, and glycerine, the triethylene-glycol of trace, 16 hours process times.Adding subsequently contains the copper chelator triethanolamine of silver ion etc., and mill running stirred after 5 minutes, and the end feeding deionized water at the grinding machine hollow shaft keeps rotating, and washes 10～30 minutes, and powder liquid flows out from the other end, obtains the fine powder of about 3.5 μ m through sedimentation.
Embodiment 4
Adopting granularity is the flake copper of 20 μ m, and consumption accounts for 30% of whole charge weitghts, and admission space accounts for 35% of tube mill ball milling space.Feed nitrogen by the grinding machine hollow shaft, mill speed is in the scope of 30 √ D, and (D is the tube mill diameter, unit: m).Add ball-milling additive,, comprise that the accumulation addition that raw material is brought into is 0.5% of a powder weight as stearic acid; BTA, ethanol melts, and addition is 1%, 20 hours process times,, feed deionized water and mix use with alcohols solvent by the grinding machine hollow shaft in the wet processing section, alcohols solvent is an ethanol, and glycerine, the triethylene-glycol of trace, 50 hours process times.Adding subsequently contains the copper chelator triethanolamine of silver ion etc., and mill running stirred after 8 minutes, and the end feeding deionized water at the grinding machine hollow shaft keeps rotating, and washes 10～30 minutes, and powder liquid flows out from the other end, obtains the fine powder of about 3.5 μ m through sedimentation.
Claims (8)
1, a kind of production contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that may further comprise the steps: (1) is raw material with the flake copper, the abrasive media of adapted rare precious metal niobium and nickel, adopt the tubular ball mill of hollow shaft, under doing, wetting two process sections, utilize mill running, add ball-milling additive, to grind, to roll, produce and stir and stir; (2) use the alumina globule that diameter is 1～3mm instead, make sheet of copper alloy powder ultra-fine and homogenising fully, add the copper chelator of silver ion, mill running stirs, and powder liquid is discharged in flushing.
2, production according to claim 1 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that: the granularity of described flake copper is 1～40 μ m's, consumption accounts for 10%～50% of whole charge weitghts, and admission space accounts for 20%～50% of tube mill ball milling space.
3, production according to claim 1 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that: the abrasive media of described rare precious metal niobium and nickel is two kinds of ball-milling mediums, a kind of is to adopt bar-shaped metal niobium, diameter is 1.5～8mm, length is 10%～80% of tube mill length of straight pipe, and another kind is the bead that adopts metallic nickel to make, and diameter is 1.5～8mm, two kinds of abrasive media weight ratios are 40: 60～60: 40, add up to account for 50%～90% of charge weitght.
4, production according to claim 3 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that: the diameter of described bar-shaped metal niobium is 2～3mm, and use amount accounts for more than 50% of metallic nickel ball weight.
5, production according to claim 1 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that: the hollow feeding nitrogen of described hollow shaft cast ball mill or other inert gas, mill speed is in the scope of 20/ √ Dm～32/ √ Dm, and D is the tube mill diameter.
6, production according to claim 1 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, and it is characterized in that: described ball-milling additive is a stearic acid, comprises that the accumulation addition that raw material is brought into is 0.1%～1% of a powder weight.
7, production according to claim 1 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that: the tubular ball mill of described hollow shaft feeds deionized water or mixes use with alcohols solvent, and alcohols solvent is monohydric alcohol, ethanol, polyalcohol or ethylene glycol etc.
8, production according to claim 1 contains the method for rare precious metal acid bronze alloy flake ultrafine powder, it is characterized in that: described dry process process time is 1～80 hour, described is that wet processing process time is 4～60 hours, and mill running stirred 1～10 minute.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA02150170XA CN1498707A (en) | 2002-11-09 | 2002-11-09 | Micropowder method for producing copper based sheet with rare-noble metal contained |
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| CNA02150170XA CN1498707A (en) | 2002-11-09 | 2002-11-09 | Micropowder method for producing copper based sheet with rare-noble metal contained |
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| CN1498707A true CN1498707A (en) | 2004-05-26 |
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| CNA02150170XA Pending CN1498707A (en) | 2002-11-09 | 2002-11-09 | Micropowder method for producing copper based sheet with rare-noble metal contained |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106825589A (en) * | 2016-12-30 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of mechanical alloying preparation method of niobium silica flour |
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2002
- 2002-11-09 CN CNA02150170XA patent/CN1498707A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106825589A (en) * | 2016-12-30 | 2017-06-13 | 西安交通大学青岛研究院 | A kind of mechanical alloying preparation method of niobium silica flour |
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