CN1109765C - Nickel-silver alloy and its preparing method - Google Patents
Nickel-silver alloy and its preparing method Download PDFInfo
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- MOFOBJHOKRNACT-UHFFFAOYSA-N nickel silver Chemical compound [Ni].[Ag] MOFOBJHOKRNACT-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000010956 nickel silver Substances 0.000 title claims abstract description 9
- 229910001316 Ag alloy Inorganic materials 0.000 title abstract description 9
- 238000000034 method Methods 0.000 title abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 238000000889 atomisation Methods 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 3
- 238000009849 vacuum degassing Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 2
- 238000005056 compaction Methods 0.000 claims 1
- 238000000280 densification Methods 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- 239000004332 silver Substances 0.000 abstract description 7
- 238000004663 powder metallurgy Methods 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000001125 extrusion Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 9
- 238000005242 forging Methods 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000009694 cold isostatic pressing Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001192 hot extrusion Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本发明属于用粉末冶金方法制造镍基合金领域。The invention belongs to the field of manufacturing nickel base alloy by powder metallurgy method.
电气设备中的导线，特别是接线柱，要求材料导电性能良好，强度高，耐磨性能好。在一般的情况下选用黄铜作为接线柱材料；在特殊的环境下，如电化学领域中，为满足抗腐蚀的需要，则选用纯镍捧或者镍网、带、片为导电极柱材料。但这些材料的电导率低。尤其是在卫星电源系统常用的CPV氢镍电池中，极柱材料还要和陶瓷绝缘子在700℃以上烧结成整体，纯镍的力学强度会因此大大下降，影响了接线的可靠性。The wires in electrical equipment, especially the terminals, require materials with good electrical conductivity, high strength, and good wear resistance. Under normal circumstances, brass is used as the terminal material; in special environments, such as in the field of electrochemistry, in order to meet the needs of corrosion resistance, pure nickel handles or nickel meshes, strips, and sheets are selected as the conductive electrode material. However, these materials have low electrical conductivity. Especially in the CPV nickel-hydrogen batteries commonly used in satellite power systems, the pole material has to be sintered with ceramic insulators at a temperature above 700°C to form a whole, which will greatly reduce the mechanical strength of pure nickel and affect the reliability of wiring.
本发明的目的是：制备一种镍银合金材料，其电阻率低于工业纯镍，耐700℃以上烧结，耐碱性(KOH)抗腐蚀能力不低于纯镍，有良好的加工性能，满足卫星电源系统CPV氢镍电池对特种极柱材料的需求。The purpose of the present invention is: prepare a kind of nickel-silver alloy material, its resistivity is lower than industrial pure nickel, sintering resistance above 700 ℃, alkali resistance (KOH) corrosion resistance is not lower than pure nickel, good processability is arranged, To meet the demand for special pole materials for CPV nickel-hydrogen batteries in satellite power systems.
本发明为达到上述目的，采用的技术方案是在纯镍中添加重量比为4-6％Ag用粉末冶金方法制造镍银合金。即：In order to achieve the above object, the present invention adopts the technical scheme of adding 4-6% Ag in pure nickel to produce nickel-silver alloy by powder metallurgy. Right now:
按重量比Ni-4～6％Ag配制合金在中频感应炉中熔化；待熔体到1600℃～1700℃后进行氮气雾化；然后在露点低于-20℃高纯氢中还原(800℃/2～3小时)；然后以250～300MPa压力冷等静压成型，再在氢气中高温烧结1130℃/4小时；将烧结坯封在钢质包套之中在真空度为5×10-2Pa时升温至350℃保温1～2小时，进行高温真空脱气，真空封口后，在电阻炉中加热至900℃保温2小时进行挤压，挤压面积比16，挤压压力8×106N，将热挤压坯剥离包套后进行锻、轧、拉、拔，进一步致密化，加工成相应的型材。According to the weight ratio of Ni-4~6%Ag, the alloy is melted in a medium frequency induction furnace; after the melt reaches 1600℃~1700℃, it is atomized with nitrogen gas; then it is reduced in high-purity hydrogen with a dew point lower than -20℃ (800℃/2 ~3 hours); then cold isostatic pressing at 250~300MPa pressure, and then sintered at 1130°C/4 hours in hydrogen at high temperature; the sintered billet is sealed in a steel sheath at a vacuum degree of 5×10 -2 Pa Heat it up to 350°C for 1 to 2 hours, carry out high-temperature vacuum degassing, after vacuum sealing, heat it in a resistance furnace to 900°C for 2 hours for extrusion, the extrusion area ratio is 16, and the extrusion pressure is 8×10 6 N , After the hot extrusion billet is stripped of the sheath, it is forged, rolled, drawn, drawn, further densified, and processed into corresponding profiles.
本发明的优点和积极效果“从性能指标对比表”可见：Advantage of the present invention and positive effect " can be seen from performance index comparison table ":
以电解纯镍和高纯银(重量比＞99.99％)为原料制备的镍银合金，与按相同的粉末冶金工艺方法制备的未添加银的纯镍进行性能对比，可以看出，加银后，电阻率明显降低，在加工状态下由79nΩm；在退火状态下进一步降为63；热扩散系数有所提高，提高到0.255；热处理后的样品晶粒细小，为15μm；力学强度成倍提高，屈服强度σs从120MPa提高到200MPa，抗拉强度从181MPa提高382MPa，延伸率大，达42％；耐碱性腐蚀能力未降低。在实际应用中，由于导电性能与加工性能良好，满足了卫星电源系统CPV氢镍电池对极柱材料的要求。The nickel-silver alloy prepared with electrolytic pure nickel and high-purity silver (weight ratio > 99.99%) is compared with the pure nickel without silver added by the same powder metallurgy process. It can be seen that after adding silver, the resistance The ratio is significantly reduced, from 79nΩm in the processed state; it is further reduced to 63 in the annealed state; the thermal diffusivity is increased to 0.255; the grain size of the sample after heat treatment is fine, 15 μm; the mechanical strength doubles, and the yield strength The σ s increased from 120MPa to 200MPa, the tensile strength increased from 181MPa to 382MPa, and the elongation rate was large, reaching 42%; the alkaline corrosion resistance did not decrease. In practical applications, due to its good electrical conductivity and processing performance, it meets the requirements of the pole material for the CPV nickel-hydrogen battery of the satellite power system.
性能指标对比表
实施例：Example:
实施例1：Example 1:
①配料：按Ni∶Ag＝96∶4重量比配料。①Batching: According to the weight ratio of Ni:Ag=96:4.
②熔炼雾化：②Smelting atomization:
采用中频感应加热，镁砂坩埚，用1#电解镍洗炉一次。Use medium frequency induction heating, magnesia crucible, and wash the furnace once with 1 # electrolytic nickel.
先将电解镍熔化，待温度升到1650℃以上时加银条，继续升温保温10分钟进行高压氮气雾化水冷收集粉末离心脱水，烘箱烘干。First melt the electrolytic nickel, add silver bars when the temperature rises above 1650°C, continue to heat up and keep warm for 10 minutes, carry out high-pressure nitrogen atomization water cooling to collect powder, centrifuge dehydration, and oven dry.
③过筛还原：③Sieve reduction:
粉末过200目筛后，在露点低于-20℃的电解氢气中还原(800℃/2小时)，氧含量从重量比0.43％降到重量比0.20％。After the powder passes through a 200-mesh sieve, it is reduced in electrolytic hydrogen with a dew point lower than -20°C (800°C/2 hours), and the oxygen content is reduced from 0.43% by weight to 0.20% by weight.
④冷压烧结：④Cold press sintering:
用内径～100mm的软胶模将粉末密封后进行冷等静压成型，压力为300MPa保压5分钟，压坯相对密度达80％，将压坯放在露点低于-20℃的氢气中烧结，烧结条件为1130℃/4小时，烧结坯氢含量从重量比0.20％降到重量比0.09％，相对密度从80％升到95％。Use a soft rubber mold with an inner diameter of ~100mm to seal the powder and carry out cold isostatic pressing. The pressure is 300MPa for 5 minutes, and the relative density of the compact reaches 80%. The compact is sintered in hydrogen with a dew point lower than -20°C. , the sintering condition is 1130°C/4 hours, the hydrogen content of the sintered compact is reduced from 0.20% by weight to 0.09% by weight, and the relative density is increased from 80% to 95%.
⑤真空脱气包套：⑤ Vacuum degassing bag:
将烧结坯放入钢包套之中逐步升温在350℃保温1小时真空度为5×10-2Pa，抽气管用酒精喷灯加热，用铁锤砸扁封口。Put the sintered billet into the ladle and gradually raise the temperature at 350°C for 1 hour. The vacuum degree is 5×10 -2 Pa. The exhaust pipe is heated with an alcohol blowtorch, and the seal is flattened with a hammer.
⑥热挤压：⑥Hot extrusion:
将有钢包套的烧结坯于电阻炉中加热到900℃，保温2小时放入挤压模筒中进行热挤压，压力机压力为8×106N，挤压面积比达16，采用钙基脂油+鳞片石墨的润滑剂。Heat the sintered billet with a steel ladle to 900°C in a resistance furnace, keep it warm for 2 hours, put it into the extrusion mold for hot extrusion, the pressure of the press is 8×10 6 N, the extrusion area ratio is 16, and the calcium-based Lubricant of grease + flake graphite.
采用车削方法剥离钢包套，挤压后Ni-Ag合金相对密度达100％。The ladle cover is peeled off by turning method, and the relative density of Ni-Ag alloy reaches 100% after extrusion.
⑦压力加工：⑦Pressure processing:
热锻：电阻炉加热850℃～600℃间模锻至Φ20mmHot forging: Die forging to Φ20mm by heating in resistance furnace at 850℃～600℃
轧制：将模锻坯表面机加在后进行多次轧制—退火，成为薄带。Rolling: After the surface of the die forging billet is machined, it is rolled and annealed several times to become a thin strip.
拉拔：将模锻坯进行旋锻，再多次冷拉—退火，成为丝材。Drawing: Swivel forging the die forging billet, and then cold drawing and annealing several times to become wire.
实施例2：Example 2:
①配料：按Ni∶Ag＝95∶5重量比配料。①Batching: According to the weight ratio of Ni:Ag=95:5.
②熔炼雾化：②Smelting atomization:
熔炼设备与坩埚预处理与实施例1相同，待温度升高1650℃时加银条，继续升温保温8分钟进行高压氮气雾化，粉末后处理过程与实施例1相同。The smelting equipment and crucible pretreatment are the same as in Example 1. When the temperature rises to 1650°C, silver bars are added, and the temperature is continued to rise for 8 minutes to carry out high-pressure nitrogen atomization. The powder post-treatment process is the same as in Example 1.
③过筛还原：③Sieve reduction:
粉末过200目筛后，在露点低于-20℃的电解氢气中还原(780℃/2小时)，氧含量从重量比0.40％降到重量比0.20％。After the powder passes through a 200-mesh sieve, it is reduced in electrolytic hydrogen with a dew point lower than -20°C (780°C/2 hours), and the oxygen content is reduced from 0.40% by weight to 0.20% by weight.
④冷压烧结：④Cold press sintering:
用内径为～110mm的软胶模将粉末密封成圆柱状后进行冷等静压成型，压力为250MPa保压5分钟。压坯相对密度达78％，将压坯去模套后放在露点低于-20℃的氢气中烧结，烧结条件为1120℃/4小时烧结坯氧含量从重量比0.2％降到重量比0.08％，相对密度从78％上升到94％。Seal the powder into a cylindrical shape with a soft rubber mold with an inner diameter of ~110mm, and then perform cold isostatic pressing at a pressure of 250MPa for 5 minutes. The relative density of the green compact reaches 78%. After the green compact is removed from the mold cover, it is sintered in hydrogen with a dew point lower than -20°C. The sintering condition is 1120°C/4 hours. The oxygen content of the sintered compact is reduced from 0.2% by weight to 0.08 by weight. %, the relative density rose from 78% to 94%.
⑤真空包套脱气：⑤Degassing with vacuum bag:
将烧结坯放入钢包套之中逐步升温在350℃保温1小时真空度为5×10-2Pa，抽气管用酒精喷灯加热，用铁锤砸扁封口。Put the sintered billet into the ladle and gradually raise the temperature at 350°C for 1 hour. The vacuum degree is 5×10 -2 Pa. The exhaust pipe is heated with an alcohol blowtorch, and the seal is flattened with a hammer.
⑥热挤压：⑥Hot extrusion:
将有钢包套的烧结坯于电阻炉中加热到920℃，保温2小时，放入挤压框筒中进行热挤压。压力机压力为8×102N，挤压面积比为16，采用钙基脂油+鳞片石墨的润滑剂。Heat the sintered billet with a steel ladle to 920°C in a resistance furnace, keep it warm for 2 hours, and put it into the extrusion frame for hot extrusion. The pressure of the press is 8×10 2 N, the extrusion area ratio is 16, and the lubricant of calcium-based grease + flake graphite is used.
挤压后Ni-Ag合金相对密度达100％。After extrusion, the relative density of Ni-Ag alloy reaches 100%.
⑦压力加工：⑦Pressure processing:
热锻：电阻炉加热，830～600℃间模锻。Hot forging: heating in resistance furnace, die forging at 830～600℃.
轧制与拉拔与实施例1相同。Rolling and drawing are the same as in Example 1.
实施例3：Example 3:
①配料：按Ni∶Ag＝94∶6重量比配料。①Batching: According to the weight ratio of Ni:Ag=94:6.
②熔炼雾化：②Smelting atomization:
熔炼设备与坩埚预处理与实施例1相同，待温度升高到1650℃时加银条继续升温使保持在1700℃稳定10分钟，进行高压氮气雾化。粉末收集烘干与实施例1相同。The smelting equipment and crucible pretreatment are the same as in Example 1. When the temperature rises to 1650°C, add silver bars and continue to raise the temperature to keep it stable at 1700°C for 10 minutes, and carry out high-pressure nitrogen atomization. Powder collection and drying are the same as in Example 1.
③过筛还原：③Sieve reduction:
粉末过200目筛后在露点低于-20℃的电解氢气中还原(780℃/3小时)，氧含量从重量比0.44％降到重量比0.20％。After passing through a 200-mesh sieve, the powder is reduced in electrolytic hydrogen with a dew point lower than -20°C (780°C/3 hours), and the oxygen content is reduced from 0.44% by weight to 0.20% by weight.
④冷压烧结：④Cold press sintering:
用内径为～110mm的软胶模将粉末密封成圆柱状后进行冷等静压成型，压力为300MPa，保压5分钟，压坯相对密度达81％，将压坯去胶模套后放在露点低于-20℃的电解氢气中烧结，烧结条件为1120℃/4小时，烧结坯氧含量从重量比0.2％降到重量比0.09％相对密度从81％上升到95％。Use a soft rubber mold with an inner diameter of ~110mm to seal the powder into a cylindrical shape and then carry out cold isostatic pressing. The pressure is 300MPa, and the pressure is kept for 5 minutes. The relative density of the green compact reaches 81%. Sintering in electrolytic hydrogen with a dew point lower than -20°C, the sintering condition is 1120°C/4 hours, the oxygen content of the sintered body decreases from 0.2% by weight to 0.09% by weight, and the relative density increases from 81% to 95%.
⑤真空包套脱气：⑤Degassing with vacuum bag:
将烧结坯放入钢包套之中逐步升温在400℃保温1小时真空度为5×10-2Pa，抽气管用酒精喷灯加热，用铁锤砸扁封口。Put the sintered billet into the ladle and gradually raise the temperature at 400°C for 1 hour. The vacuum degree is 5×10 -2 Pa. The exhaust pipe is heated with an alcohol blowtorch, and the seal is flattened with a hammer.
⑥热挤压：与实施例2相同。6. hot extrusion: same as embodiment 2.
⑦压力加工：与实施例2相同。⑦Pressure processing: Same as Example 2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100523239C (en) * | 2005-03-16 | 2009-08-05 | 德累斯顿协会莱布尼茨固体材料研究所 | Method for producing a nickel-based semifinished product having a recrystallized three-dimensional texture and use of such a nickel-based semifinished product |
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| DE10342965A1 (en) * | 2003-09-10 | 2005-06-02 | Leibniz-Institut Für Festkörper- Und Werkstoffforschung Dresden E.V. | Nickel-based semifinished product with a recrystallization cube texture and process for its production |
| CN101169985B (en) * | 2007-11-22 | 2010-11-24 | 昆明贵金属研究所 | Special nickel-based composite conductive powder material and preparation method thereof |
| EP4332259A3 (en) * | 2013-12-27 | 2024-05-22 | Raytheon Technologies Corporation | High-strength high-thermal-conductivity wrought nickel alloy |
| CN108550414A (en) * | 2018-04-12 | 2018-09-18 | 江苏通鼎光电科技有限公司 | A kind of high-performance answering machine data transmission cable |
| CN110629135B (en) * | 2019-10-21 | 2021-07-06 | 常德力元新材料有限责任公司 | Preparation method of nickel-silver alloy material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5386622A (en) * | 1977-01-11 | 1978-07-31 | Toshiba Corp | Silver-nickel electrical contact point material |
-
2000
- 2000-02-29 CN CN00103911A patent/CN1109765C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5386622A (en) * | 1977-01-11 | 1978-07-31 | Toshiba Corp | Silver-nickel electrical contact point material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100523239C (en) * | 2005-03-16 | 2009-08-05 | 德累斯顿协会莱布尼茨固体材料研究所 | Method for producing a nickel-based semifinished product having a recrystallized three-dimensional texture and use of such a nickel-based semifinished product |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1311344A (en) | 2001-09-05 |
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