CN103192203B - Process method for preparing silver solder - Google Patents
Process method for preparing silver solder Download PDFInfo
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- CN103192203B CN103192203B CN201310008917.1A CN201310008917A CN103192203B CN 103192203 B CN103192203 B CN 103192203B CN 201310008917 A CN201310008917 A CN 201310008917A CN 103192203 B CN103192203 B CN 103192203B
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 24
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 16
- 239000000956 alloy Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 14
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 16
- 239000010949 copper Substances 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229910052763 palladium Inorganic materials 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 239000011135 tin Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000005275 alloying Methods 0.000 abstract description 10
- 238000002490 spark plasma sintering Methods 0.000 abstract description 10
- 238000003723 Smelting Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract 2
- 230000004913 activation Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 238000005266 casting Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 238000005219 brazing Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000007499 fusion processing Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910000753 refractory alloy Inorganic materials 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Abstract
The invention relates to a method for preparing silver solder. The method comprises the following specific steps: applying pressure to raw material particles arranged in a graphite crucible by upper and lower graphite press heads in a spark plasma sintering system (SPS) under the vacuum condition; directly heating the raw material particles by using pulse current; and breaking through an oxidation film of each particle of metal powder at instant high temperature and enabling the oxidation film to be subjected to surface activation and quick liquefaction. The reaction speed of particles and the reaction speed among the particles are increased, the diffusion speed of alloy element atoms is increased and the aims of quickly alloying and densifying a sintering body are achieved. Compared with a traditional smelting method, the method disclosed by the invention has the advantages of simple and easily-controlled process, no loss of alloy elements, accurate components of silver-based solder components, low oxygen content, short sintering time, low energy consumption, safety, no pollution and favorable reproducibility. The ingot products prepared by the method are high in density; crystal particles are fine and are uniform in size; and the method is an economic and efficient green preparation process.
Description
Technical field
The present invention relates to a kind of method preparing silver solder, be different from the preparation method of traditional handicraft, with the silver-base solder recommended in GB/T 10046-2008 " silver solder " for manufacturing processing object, belonging to brazing material processing preparing technical field.
Background technology
Silver solder is current most widely used a kind of solder, and it has excellent processing performance, suitable fusing point, the good ability soaking and fill up gap.And the intensity of solder and fine seam is high, plasticity is good, electric conductivity and excellent corrosion resistance, be therefore widely used in all black of fine weldering except aluminium, magnesium and other low-melting-point metals and non-ferrous metal, as: mild steel, stainless steel, high temperature alloy, Copper and its alloy, kovar alloy and refractory alloy.Be widely used in the industry manufacture field such as refrigeration, lamp decoration, hardware appliance, instrument and meter, chemical industry, Aero-Space.
In recent years, the research of domestic and international silver solder mainly concentrates on design to silver solder chemical composition proportioning and trial, comprises 4 aspects: (1) cadmium-free silver brazing alloy; (2) low silver-colored silver-less solder; (3) impact of alloying element; (4) novel brazing filler metal alloy system develop the research etc. with solder for ceramic soldering.But preparation technology generally adopts melting mode, namely raw material is according to a certain ratio placed in intermediate frequency furnace and carries out melting and be cast into ingot, obtains a material, or obtain Strip by ingot formation, roughing, finish rolling by follow-up forging, extruding, drawing.Also adopt horizontal casting at present, and some other complexity, strict smelting technology ensure ingot quality, prevent component segregation, improve the mechanical property of silver-base solder, mechanical performance and welding performance with this simultaneously.
But no matter adopt which kind of smelting technology in actual production, alloying element loss in fusion process is larger, especially active metallic element (as: zinc, lithium, magnesium etc.) is easy to oxidation, alloying component is difficult to control, simultaneously because argent is easy to air-breathing, reported in literature in the molten state, in the molten state, silver can dissolve the oxygen exceeding himself volume 21 times, and this character of silver brings problem to melting and casting.It makes alloy at high temperature easily volatilize or cause a large amount of loss because producing splash from High-temperature cooling process.And the generation of inside ingot defect can be caused in ingot casting subsequently and temperature-fall period, or directly have influence on the follow-up mechanical performance of silver-base solder and welding performance.Although adopt the mode such as deoxidier or vacuum melting at present, or introduce other impurity elements, or increase vacuum equipment, the continuity that impact is produced.
Summary of the invention
The object of this invention is to provide a kind of economic, efficient discharge plasma sintering process and prepare silver-base solder, to reduce the loss of alloying element in fusion process, guarantee alloying component is accurate, improve ingot quality, reduce ingot casting oxygen content and internal flaw, improve mechanical mechanics property and the welding performance of silver-base solder.
The method that the present invention prepares silver solder comprises: by silver powder, with other simple metal element powders or intermediate alloy powder, according to selected formula, be placed in the ball grinder of inner liner polytetrafluoroethylene and carry out ball milling, the powder mixed by ball milling is inserted in SPS system graphite crucible, be evacuated to 2 ~ 10Pa, with 5 ~ 50
owithin C/ minute, be warming up to 900 ~ 1100
oc, pressure is 5MPa ~ 40MPa, 10 minutes ~ 60 minutes dwell time, and cold feeding of going of lowering the temperature subsequently is come out of the stove, and the ingot bar precision after sintering is swaged, be drawn to a material subsequently, or rolling is sheet material.
Described silver powder purity >=99%, particle size range is 100 order ~ 500 orders.
Described simple metal element powders is: one of copper, nickel, zinc, tin, palladium, purity >=99%, and particle size range is 100 order ~ 500 orders.
Described intermediate alloy powder is M
xn
y, M is: one of copper, nickel, palladium; N is one of zinc, indium, lithium, and x scope is: 0.50 ~ 0.99, y scope is 0.05 ~ 0.5.Purity >=99%, particle size range is 100 order ~ 500 orders.
The technology of the present invention principle is (spark plasma sintering in discharge plasma sintering system, be called for short SPS), under vacuum condition, the feed particles being placed in graphite crucible is exerted pressure by push-down head on graphite, utilize the direct heating raw particle of pulse current, the oxide-film breaking through each particle of metal dust under transient high temperature makes its surface active, and fast liquefying.Improve particle/intergranular reaction rate, increase the diffusion rate of alloying element atom, reach the rapid alloying of sintered body and densified object.
Compare with traditional smelting process, present invention process is simple and easy to control, and the loss of alloy-free element, silver-base solder composition is accurate, oxygen content is low, and sintering time is short, and energy consumption is low, safety non-pollution, favorable reproducibility.Prepared ingot density is high, and crystal grain fine size is even, and band, the silk material mechanical mechanics property of silver-base solder are excellent, and weldability is good, are that a kind of technique is terse, cost is low, free of contamination green preparation process.
Detailed description of the invention
The method step preparing silver solder of the present invention comprises: by silver powder, with other simple metal element powders or intermediate alloy powder, according to selected formula, be placed in the ball grinder of inner liner polytetrafluoroethylene and carry out ball milling, the powder mixed by ball milling is inserted in SPS system graphite crucible, be evacuated to 2 ~ 10Pa, with 5 ~ 50
owithin C/ minute, be warming up to 900 ~ 1100
oc, pressure is 5MPa ~ 40MPa, 10 minutes ~ 60 minutes dwell time, and cold feeding of going of lowering the temperature subsequently is come out of the stove, and the ingot bar precision after sintering is swaged, be drawn to a material subsequently, or rolling is sheet material.
Described silver powder purity >=99%, particle size range is 100 order ~ 500 orders.
Described simple metal element powders is: one of copper, nickel, zinc, tin, palladium, purity >=99%, and particle size range is 100 order ~ 500 orders.
Described intermediate alloy powder is M
xn
y, M is: one of copper, nickel, palladium; N is one of zinc, indium, lithium, and x scope is: 0.50 ~ 0.99, y scope is 0.05 ~ 0.5.Purity >=99%, particle size range is 100 order ~ 500 orders.
The present invention is specifically implemented by following steps:
1, by particle size range 100 order ~ 300 order silver powder, purity >=99%.With other particle size range 100 order ~ 500 order alloying element powders, one of copper, nickel, zinc, tin, palladium, purity >=99%, particle size range is 100 order ~ 500 orders.Or intermediate alloy powder, M
xn
y, M is: one of copper, nickel, palladium; N is one of zinc, indium, lithium, and x scope is: 0.50 ~ 0.99, y scope is 0.05 ~ 0.5, purity>=99%, and particle size range is 100 order ~ 500 orders.According to selected formula, be placed in the ball grinder of inner liner polytetrafluoroethylene, ratio of grinding media to material 1:3 ~ 5, rotating speed 100 ~ 300 rpm/min, even batch mixing 0.5 ~ 3 hour.
2, the powder that ball milling mixes is inserted in SPS system graphite crucible, be evacuated to 2 ~ 10Pa, with 5 ~ 50
owithin C/ minute, be warming up to 900 ~ 1100
oc, pressure is 5MPa ~ 40MPa, 10 minutes ~ 60 minutes dwell time.Cold feeding of going of lowering the temperature subsequently is come out of the stove.
3, the ingot bar precision after sintering swaged, be drawn to a material subsequently, or rolling is sheet material, dimensional tolerance is determined according to actual conditions.
The present invention adopts discharge plasma sintering technique, utilize the transient high temperature under plasmoid, by controlling programming rate, sintering temperature, pressing pressure, make the different material particle surface fast activating liquefaction also rapid alloying of silver-base solder, form fine and close ingot bar material, the silver-base solder ingot bar crystal grain obtained is tiny, size uniform.Because sintering time is short, compare with traditional smelting technology, Volatile Elements loss is little, and formulated component is accurate, and oxygen content is low.Make silver-base solder ingot bar be provided with good plastic working ability, ensure that silk material or band had mechanical mechanics property and welding performance.It is simple and easy to control that this invention has technique, the loss of alloy-free element, and silver-colored Composition Control is accurate, and sintering time is short, and energy consumption is low, safety non-pollution, the features such as favorable reproducibility.
Below describe several embodiments of the present invention in detail, but the present invention is not only limited to this.
Purity is 99.5% by embodiment 1,72 grams, particle size range 100 order silver powder, and with purity 99%, particle size range 100 object copper powder 28 grams, is placed in the ball grinder of inner liner polytetrafluoroethylene, ratio of grinding media to material 1:3, rotating speed 100rpm/min, even batch mixing 1 hour.The powder mixed by ball milling is inserted in SPS system graphite crucible, and graphite crucible is of a size of × and 10, be evacuated to 5Pa, with 5
owithin C/ minute, be warming up to 900
oc, pressure is 5MPa, 15 minutes dwell times, and cold feeding of going of lowering the temperature subsequently is come out of the stove.Ingot bar precision after sintering is swaged to Φ 6, is drawn to a material Φ 1 ± 0.05 subsequently.
Purity is 99.5% by embodiment 2, and particle size range is 80 grams, 200 order silver powder, is 99% with purity, and particle size range is 200 object copper nickel intermediate alloy powder Cu
0.9ni
0.120 grams, be placed in the ball grinder of inner liner polytetrafluoroethylene, ratio of grinding media to material 1:5, rotating speed 200rpm/min, even batch mixing 2 hours.The powder mixed by ball milling is inserted in SPS system graphite crucible, and graphite crucible is of a size of Φ 20 × 10, is evacuated to 5Pa, with 25
owithin C/ minute, be warming up to 1100
oc, pressure is 20MPa, 20 minutes dwell times, and cold feeding of going of lowering the temperature subsequently is come out of the stove.Swage to Φ 6 by the ingot bar precision after sintering, rolling is subsequently sheet material 6 × 0.5 ± 0.01.
Purity is 99.5% by embodiment 3, and particle size range is 70 grams, 300 order silver powder, is 99% with purity, and particle size range is 300 object copper indium intermediate alloy powder Cu
0.95in
0.0530 grams, be placed in the ball grinder of inner liner polytetrafluoroethylene, ratio of grinding media to material 1:4, rotating speed 300rpm/min, even batch mixing 0.5 hour.The powder mixed by ball milling is inserted in SPS system graphite crucible, and graphite crucible is of a size of Φ 20 × 10, is evacuated to 3Pa, with 50
owithin C/ minute, be warming up to 950
oc, pressure is 30MPa, 10 minutes dwell times, and cold feeding of going of lowering the temperature subsequently is come out of the stove.Swage to Φ 10 by the ingot bar precision after sintering, rolling is subsequently sheet material 10 × 0.2 ± 0.01.
Claims (1)
1. prepare the method for silver solder for one kind, its feature comprises: by silver powder, with other simple metal element powders or intermediate alloy powder, according to selected formula, be placed in the ball grinder of inner liner polytetrafluoroethylene and carry out ball milling, the powder mixed by ball milling is inserted in SPS system graphite crucible, is evacuated to 2 ~ 10Pa, with 5 ~ 50
owithin C/ minute, be warming up to 900 ~ 1100
oc, pressure is 5MPa ~ 40MPa, and 10 minutes ~ 60 minutes dwell time, cooling down feeding is come out of the stove subsequently, the ingot bar precision after sintering is swaged, be drawn to a material subsequently, or rolling is sheet material;
Described simple metal element powders is: one of copper, nickel, zinc, tin, palladium, purity >=99%, and particle size range is 100 order ~ 500 orders;
Described intermediate alloy powder is M
xn
y, M is: one of copper, nickel, palladium; N is one of zinc, indium, lithium, and x scope is: 0.50 ~ 0.99, y scope is 0.05 ~ 0.5, purity>=99%, and particle size range is 100 order ~ 500 orders.
2. a kind of method preparing silver solder according to claim 1, is characterized in that described silver powder purity >=99%, and particle size range is 100 order ~ 500 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310008917.1A CN103192203B (en) | 2013-01-10 | 2013-01-10 | Process method for preparing silver solder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310008917.1A CN103192203B (en) | 2013-01-10 | 2013-01-10 | Process method for preparing silver solder |
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| CN103192203A CN103192203A (en) | 2013-07-10 |
| CN103192203B true CN103192203B (en) | 2015-06-17 |
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| CN201310008917.1A Active CN103192203B (en) | 2013-01-10 | 2013-01-10 | Process method for preparing silver solder |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103659059B (en) * | 2013-12-12 | 2016-08-17 | 北京科技大学 | A kind of method preparing annular Ag-Cu-Sn intermediate temperature solder sheet |
| CN105921908A (en) * | 2016-06-23 | 2016-09-07 | 国网江苏省电力公司宿迁供电公司 | Silver solder and preparation method thereof |
| CN106001989A (en) * | 2016-06-23 | 2016-10-12 | 国网江苏省电力公司宿迁供电公司 | Silver brazing flux and preparation method thereof |
| CN108907500A (en) * | 2018-08-03 | 2018-11-30 | 北京有色金属与稀土应用研究所 | A kind of high temperature auri active solder and preparation method thereof |
| CN111015017B (en) * | 2019-12-20 | 2021-09-14 | 西南交通大学 | Mn-Cu-based welding wire and preparation method and application thereof |
| CN114029651B (en) * | 2021-11-18 | 2022-07-01 | 东北大学 | Titanium-containing active solder and preparation method and application thereof |
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| CN103192203A (en) | 2013-07-10 |
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