CN1299861C - Preparation method of submicron silver copper alloy powder - Google Patents
Preparation method of submicron silver copper alloy powder Download PDFInfo
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- CN1299861C CN1299861C CNB2005100489127A CN200510048912A CN1299861C CN 1299861 C CN1299861 C CN 1299861C CN B2005100489127 A CNB2005100489127 A CN B2005100489127A CN 200510048912 A CN200510048912 A CN 200510048912A CN 1299861 C CN1299861 C CN 1299861C
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- 239000000843 powder Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 12
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 49
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011780 sodium chloride Substances 0.000 claims abstract description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000010930 yellow gold Substances 0.000 claims description 20
- 229910001097 yellow gold Inorganic materials 0.000 claims description 20
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 239000004332 silver Substances 0.000 abstract description 7
- 239000002002 slurry Substances 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011982 device technology Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000003053 toxin Substances 0.000 abstract 1
- 231100000765 toxin Toxicity 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 26
- 239000010935 stainless steel Substances 0.000 description 19
- 229910001220 stainless steel Inorganic materials 0.000 description 19
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 15
- 229910052786 argon Inorganic materials 0.000 description 13
- 229910052802 copper Inorganic materials 0.000 description 11
- 239000010949 copper Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000003701 mechanical milling Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The present invention discloses a preparation method of submicrometer silver-copper alloy powder. The method comprises steps: (1) ball milling operation is carried out on silver powder and copper powder for 18 to 72 hours, the mass ratio of ball materials ranges from 10: 1 to 40: 1, and the rotating speed of a ball milling machine ranges from 200 to 400 rpm; (2) sodium chloride is added, and the ratio of the sodium chloride to silver-copper alloy ranges from 0.1 to 10; the continuous ball milling time ranges from 12 to 120 hours, the mass ratio of ball materials ranges from 10: 1 to 40: 1, and the rotating speed of a ball milling machine ranges form 200 to 400 rpm; (3) obtained powder is washed by distilled water to remove the sodium chloride, and then filtration is carried out; (4) filtration products are dried in a vacuum drying oven to obtain the submicrometer silver-copper alloy powder, and the drying temperature ranges from 70 to 100 DEG C. The silver-copper alloy powder which is made by the present invention and satisfies the requirements of electrocondution slurry can replace silver powder, and thereby, the use amount of noble metal, namely silver, is reduced. The present invention has the advantages of few required chemical reagents, simple device technology and low production cost. The used chemical reagents have the advantages of no toxin, easy recovery and no damage to the environment.
Description
Technical field
The present invention relates to field of material preparation, relate in particular to a kind of preparation method of submicron silver copper alloy powder.
Background technology
Electronic product extensively is present in human lives's every field, but they generally relate to the electromagenetic wave radiation pollution problem, health is constituted a threat to, and for example the mobile phone in the daily life, television set, computer, micro-wave oven etc. all can produce electromagnetic radiation in use.The precautionary measures that extensively adopt are to be coated with the last layer electrocondution slurry on electronic product shell at present, with electromagnetic radiation shielding, thereby reach operable requirement.The general silver powder that uses is as conducting particles in this electrocondution slurry, but existing silver powder preparation method is generally chemical method, has used the bigger chemical reagent of toxicity in the preparation process, have in addition also adopted cyanide, environment is caused very big harm.Silver is a kind of noble metal simultaneously, uses the cost of silver higher.
In order to reduce cost, people propose to use the yellow gold powder to replace silver powder as the conductive compositions in the electrocondution slurry.Existing patent generally adopts reducing agent (as hydrazine hydrate, sodium borohydride, ascorbic acid etc.) reducing metal ion from soluble-salt (as nitrate etc.) mixed solution of argentiferous and copper to prepare the Kufil powder.Because what this method still adopted is chemical method, needs to use a large amount of chemical reagent in the preparation process, thereby also environment is worked the mischief inevitably.Its preparation process is complicated in addition, and cost also is difficult to reduce.
Ball milling is a kind of simple lower cost materials preparation method.Existing bibliographical information adopts the method for ball milling to prepare the yellow gold powder, and its granular size is a micron order.Fig. 1 is the X ray diffracting spectrum of 2.524 gram copper powders and 0.476 gram silver powder ball milling 48 hours products, and this collection of illustrative plates shows ball milling silver-bearing copper mixed-powder alloying preferably after 48 hours.But because silver and copper all belong to face-centred cubic structure, have good ductility, its particle of yellow gold powder that adopts ball milling directly to prepare is bigger, is difficult to satisfy the requirement of electrocondution slurry to grain graininess.Fig. 2 is the optical microscope photograph of 2.524 gram copper powders and 48 hours products of 0.476 gram silver powder ball milling, and as can be seen from the figure particle is about 100 microns.Simultaneously, after yellow gold forms, continue ball milling and then can cause the yellow gold powder particle to be grown up.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of submicron silver copper alloy powder.
The step of method is:
1) silver powder and copper powder are carried out ball milling, the ball milling time is 18～72 hours, and ball material mass ratio is 10～40: 1, and drum's speed of rotation is 200～400rpm;
2) add sodium chloride subsequently, the mass ratio of sodium chloride and yellow gold is 0.1～1.5; Continuing the ball milling time is 12～120 hours, and ball material mass ratio is 10～40: 1, and drum's speed of rotation is 200～400rpm;
3) powder with gained washs with distilled water, removes sodium chloride, filters then;
4) filtration product drying in vacuum drying chamber is obtained submicron silver copper alloy powder, baking temperature is 70～100 ℃.
Compare with additive method, the present invention has following advantage: (1) makes satisfies the yellow gold powder that electrocondution slurry requires and can replace silver powder, reduces the consumption of noble metal silver.(2) means of employing ball milling, required chemical reagent is less, and apparatus and process is simple, and production cost is low.(3) chemical reagent of Shi Yonging is nontoxic and be easy to reclaim, and environment is not had harm.(4) its composition of yellow gold powder that makes and granular size are convenient to control.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of ball milling powder after 48 hours in the embodiment of the invention 3;
Fig. 2 is the optical microscope photograph of ball milling powder after 48 hours in the embodiment of the invention 3;
Fig. 3 is the X ray diffracting spectrum of final yellow gold powder in the embodiment of the invention 1;
Fig. 4 is the electron scanning micrograph of final yellow gold powder in the embodiment of the invention 1.
The specific embodiment
The present invention can reduce the particle size of alloy powder effectively by add dispersant sodium chloride in mechanical milling process, can make the yellow gold powder that can satisfy as the electrocondution slurry requirement.
Concrete steps of the present invention are as follows:
1) a certain proportion of silver powder and copper powder are carried out ball milling.Its time is 18～72 hours, and ball material mass ratio is 10～40: 1, and drum's speed of rotation is 200～400rpm.Make the abundant alloying of raw material, make the yellow gold powder of certain granules size;
2) after above-mentioned mechanical milling process is finished, add sodium chloride subsequently, the sodium chloride of adding and the ratio of yellow gold are 0.1～10.Continued ball milling 12～120 hours, ball material mass ratio is 10～40: 1, and drum's speed of rotation is 200～400rpm;
3) powder with gained washs with distilled water, removes sodium chloride, filters then;
4) filtration product is drying to obtain submicron silver copper alloy powder in vacuum drying chamber.Baking temperature is 70～100 ℃.
The present invention's amount of sodium chloride under the same ball time consuming has a direct impact yellow gold particles of powder size.What preparation yellow gold powder adopted is ball grinding method, and the content from 0.1% to 99.9% of copper can be regulated arbitrarily in its raw material proportioning, is convenient to control the composition of alloy powder.
Abrading-ball and ball grinder that ball milling uses are stainless steel material.The diameter of abrading-ball is 4～18mm, adopts the ball of different-diameter to be used during ball milling.
Since contain copper in the alloy, oxidized easily.In order to prevent oxidation, when carrying out ball milling, after abrading-ball and raw material were put into ball grinder, the reply ball grinder vacuumized, and general vacuum is 0.1～2Pa.After vacuumizing, also should charge into inert gas shielding.The inert gas that charges into is generally argon gas or nitrogen, and the pressure that charges into gas is 0.1～2MPa.
Embodiment 1
Take by weighing 1.112 gram copper powders and 1.888 gram silver powder are put into stainless steel jar mill, add 60 gram stainless steel abrading-balls.Seal charging door, be evacuated to 0.4Pa, pour argon shield, pressure is 0.2MPa, places ball milling on the ball mill, and drum's speed of rotation is 300rpm.Behind the ball milling 48 hours, open ball grinder fast, add 3 gram sodium chloride and 60 gram stainless steel abrading-balls, be evacuated to 0.6Pa, pour argon shield, pressure is 0.18MPa, continues ball milling 36 hours with the rotating speed of 300rpm.The product of ball milling is washed with distilled water, in vacuum drying chamber, dry down then in 75 ℃.Fig. 3 shows in the product that silver and copper have formed alloy.Fig. 4 shows that this yellow gold particles of powder is generally below 500 nanometers.
Embodiment 2
Take by weighing 0.184 gram copper powder and 2.816 gram silver powder are put into stainless steel jar mill, add 60 gram stainless steel abrading-balls.Seal charging door, be evacuated to 0.6Pa, pour argon shield, pressure is 0.18MPa, places ball milling on the ball mill, and drum's speed of rotation is 300rpm.Behind the ball milling 36 hours, open ball grinder fast, add 3 gram sodium chloride and 60 gram stainless steel abrading-balls, be evacuated to 0.4Pa, pour argon shield, pressure is 0.18MPa, continues ball milling 50 hours with the rotating speed of 300rpm.The product of ball milling is washed with distilled water, in vacuum drying chamber, dry down then in 80 ℃.
Embodiment 3
Take by weighing 2.524 gram copper powders and 0.476 gram silver powder is put into stainless steel jar mill, add 90 gram stainless steel abrading-balls.Seal charging door, be evacuated to 0.5Pa, pour argon shield, pressure is 0.18MPa, places ball milling on the ball mill, and drum's speed of rotation is 300rpm.Behind the ball milling 48 hours, open ball grinder fast, add 2 gram sodium chloride and 60 gram stainless steel abrading-balls, be evacuated to 0.6Pa, pour argon shield, pressure is 0.18MPa, continues ball milling 48 hours with the rotating speed of 300rpm.The product of ball milling is washed with distilled water, in vacuum drying chamber, dry down then in 80 ℃.
Embodiment 4
Take by weighing 0.385 gram copper powder and 2.615 gram silver powder are put into stainless steel jar mill, add 75 gram stainless steel abrading-balls.Seal charging door, be evacuated to 0.5Pa, pour argon shield, pressure is 0.18MPa, places ball milling on the ball mill, and drum's speed of rotation is 300rpm.Behind the ball milling 24 hours, open ball grinder fast, add 6 gram sodium chloride and 150 gram stainless steel abrading-balls, be evacuated to 0.4Pa, pour argon shield, pressure is 0.18MPa, continues ball milling 48 hours with the rotating speed of 300rpm.The product of ball milling is washed with distilled water, in vacuum drying chamber, dry down then in 80 ℃.Product is the yellow gold powder, and granular size is generally the hundreds of nanometer.
Embodiment 5
Take by weighing 0.846 gram copper powder and 2.154 gram silver powder are put into stainless steel jar mill, add 90 gram stainless steel abrading-balls.Seal charging door, be evacuated to 0.7Pa, pour argon shield, pressure is 0.20MPa, places ball milling on the ball mill, and drum's speed of rotation is 300rpm.Behind the ball milling 40 hours, open ball grinder fast, add 5 gram sodium chloride and 150 gram stainless steel abrading-balls, be evacuated to 0.5Pa, pour argon shield, pressure is 0.18MPa, continues ball milling 72 hours with the rotating speed of 300rpm.The product of ball milling is washed with distilled water, in vacuum drying chamber, dry down then in 80 ℃.Product is the yellow gold powder, the general hundreds of nanometer of granular size.
Embodiment 6
Take by weighing 2.106 gram copper powders and 0.894 gram silver powder is put into stainless steel jar mill, add 75 gram stainless steel abrading-balls.Seal charging door, be evacuated to 0.7Pa, pour argon shield, pressure is 0.18MPa, places ball milling on the ball mill, and drum's speed of rotation is 300rpm.Behind the ball milling 36 hours, open ball grinder fast, add 8 gram sodium chloride and 200 gram stainless steel abrading-balls, be evacuated to 0.5Pa, pour argon shield, pressure is 0.18MPa, continues ball milling 60 hours with the rotating speed of 300rpm.The product of ball milling is washed with distilled water, in vacuum drying chamber, dry down then in 80 ℃.Product is the yellow gold powder, the general hundreds of nanometer of granular size.
Claims (1)
1. the preparation method of a submicron silver copper alloy powder is characterized in that, the step of method is:
1) silver powder and copper powder are carried out ball milling, the ball milling time is 18～72 hours, and ball material mass ratio is 10～40: 1, and drum's speed of rotation is 200～400rpm;
2) add sodium chloride, the ratio of sodium chloride and yellow gold is 0.1～1.5; Continuing the ball milling time is 12～120 hours, and ball material mass ratio is 10～40: 1, and drum's speed of rotation is 200～400rpm;
3) powder with gained washs with distilled water, removes sodium chloride, filters then;
4) filtration product drying in vacuum drying chamber is obtained submicron silver copper alloy powder, baking temperature is 70～100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100489127A CN1299861C (en) | 2005-01-14 | 2005-01-14 | Preparation method of submicron silver copper alloy powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100489127A CN1299861C (en) | 2005-01-14 | 2005-01-14 | Preparation method of submicron silver copper alloy powder |
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| CN1657202A CN1657202A (en) | 2005-08-24 |
| CN1299861C true CN1299861C (en) | 2007-02-14 |
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| CNB2005100489127A Expired - Fee Related CN1299861C (en) | 2005-01-14 | 2005-01-14 | Preparation method of submicron silver copper alloy powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100411157C (en) * | 2006-06-30 | 2008-08-13 | 中南大学 | Process for preparing silumin electronic package materials |
| CN117620161B (en) * | 2023-12-04 | 2024-08-16 | 扬州虹运电子材料有限公司 | Antioxidant copper-silver composite powder for conductive paste and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06128609A (en) * | 1992-10-15 | 1994-05-10 | Daido Steel Co Ltd | Production of ag-cu alloy powder |
| JPH1192805A (en) * | 1997-09-17 | 1999-04-06 | Sumitomo Metal Mining Co Ltd | Copper alloy powder and its production |
| US20040142816A1 (en) * | 2001-12-11 | 2004-07-22 | Baker R. Terry K. | Method for producing powdered metal catalysts |
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2005
- 2005-01-14 CN CNB2005100489127A patent/CN1299861C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06128609A (en) * | 1992-10-15 | 1994-05-10 | Daido Steel Co Ltd | Production of ag-cu alloy powder |
| JPH1192805A (en) * | 1997-09-17 | 1999-04-06 | Sumitomo Metal Mining Co Ltd | Copper alloy powder and its production |
| US20040142816A1 (en) * | 2001-12-11 | 2004-07-22 | Baker R. Terry K. | Method for producing powdered metal catalysts |
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| CN1657202A (en) | 2005-08-24 |
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