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CN108149057A - A kind of AgCuNiV alloy materials and preparation method thereof - Google Patents

A kind of AgCuNiV alloy materials and preparation method thereof Download PDF

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Publication number
CN108149057A
CN108149057A CN201711431543.9A CN201711431543A CN108149057A CN 108149057 A CN108149057 A CN 108149057A CN 201711431543 A CN201711431543 A CN 201711431543A CN 108149057 A CN108149057 A CN 108149057A
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agcuniv
alloy materials
powder
agcuni
preparation
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CN108149057B (en
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蔡正旭
章明溪
黄小凯
金凯
姚映君
祁宇
付晓玄
王峰
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BEIJING NON-FERROUS METAL AND RARE-EARTH APPLICATION INST
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C5/00Alloys based on noble metals
    • C22C5/06Alloys based on silver
    • C22C5/08Alloys based on silver with copper as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0466Alloys based on noble metals

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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Abstract

The present invention relates to a kind of AgCuNiV alloy materials and preparation method thereof, belong to powder metallurgical technology.The weight percent of AgCuNiV alloy materials forms:Ag 66.5% 89.1%, Cu 9.5% 27.72%, Ni 0% 1.98%, V 1.0% 5.0%.By preparing AgCuNi alloyed powders, AgCuNiV alloy materials are prepared using discharge plasma sintering after then mixing AgCuNi alloyed powders and V powder.It is difficult to be added in alloy and generate in the alloy gross segregation that the present invention, which solves V, and uneven chemical components, surface have the problems such as blackspot and stomata.The present invention prepares AgCuNiV alloys using discharge plasma sintering technique, and fine microstructures are uniform, segregation-free, the reliability of contact material in radar electric device can be effectively ensured, acquisition ingredient is uniform, the flawless contact material in surface;Preparation process is simple simultaneously, and production procedure is short.

Description

A kind of AgCuNiV alloy materials and preparation method thereof
Technical field
The present invention relates to a kind of AgCuNiV alloy materials and preparation method thereof, more particularly to a kind of high intensity, high V content AgCuNiV contact materials and preparation method thereof, the material are a kind of contact materials for being mainly used for radar electric device, are belonged to In powder metallurgical technology.
Background technology
With the development of science and technology, automatic control system, remote control telemetering system and communication system become more and more multiple It is miscellaneous, caused by system jam lose and endanger also just it is increasing, therefore to the component including relay can It is required by property also higher and higher.In the high-tech areas such as military and aerospace, height is required to the overall reliability of relay, Contact in especially crucial occasion cannot break down at crucial moment.
At present, have the highly reliable contact material of many scientific research institution's R and D, silver-based electric contact both at home and abroad Material have higher reliability, good electric conductivity, processing performance, oxidation resistance, be widely used in moderate duty or In the electric appliance of big load, wherein AgCuNiV alloys have higher mechanical property, anti-scorching performance, stable contact resistance etc. Performance, alloy surface is still kept bright and clean in ammonia, moist atmosphere, be widely used in making wear-resisting and erosion-resisting relay, The elements such as make and break contact and commutator segment, commutator segment, brush and conducting ring.
The preparation of AgCuNiV alloy sheet materials is generally using traditional founding+milling method, the conjunction that this method prepares Gold exists apparent insufficient:1) V is difficult to be added in alloy, causes V content in alloy that cannot control;2) macroscopic views of V in the alloy Segregation is serious, uneven chemical components;3) alloy surface has blackspot, it is difficult to remove;4) easily occur hole, bubble in process Phenomena such as.Due to more than, mechanical and physical character, electric property, processing performance and the product of the material have been seriously affected Yield rate, so as to affect the reliability of integral device.Chen Yongtai et al. is using extremely cold powder by atomization, isostatic cool pressing, vacuum Sintering, the technique squeezed prepare AgCu10V0.3Alloy.But this method prepares AgCuV alloy sheet materials, complex process, preparation Period is long, and materials microstructure is coarse after vacuum-sintering, and consistency is not high, is unfavorable for following process, and low strength, with When corresponding conduction pair is matched, it is impossible to meet the requirements.The discharge plasma sintering compared with ordinary powder metallurgical technology Technology has that sintering heating rate is fast, sintering time is short, sintering is efficient, sintering process is simple, can obtain fine microstructures, equal Even, high-compactness product.Directly preparing AgCuNV alloys using discharge plasma sintering technique becomes the hot spot of research.
Invention content
It is insufficient existing for the AgCuNiV alloys that the present invention is prepared for traditional casting method and ordinary sinter method, it carries For a kind of AgCuNiV alloy materials and preparation method with highly reliable, high V content, the present invention is burnt using plasma discharging Highly reliable, high V content AgCuNiV contact materials are prepared in knot technology.
It is difficult to be added in alloy and generate in the alloy gross segregation present invention mainly solves V, chemical composition is not Uniformly, there is the problems such as blackspot and stomata on surface, and so as to obtain, ingredient is uniform, the flawless contact material in surface.
The main object of the present invention is to provide a kind of prepares highly reliable, high V content using discharge plasma sintering technique AgCuNiV alloy materials.
Another object of the present invention is to provide a kind of preparation method of AgCuNiV alloy materials, this method is simple, prepares Alloy structure it is tiny, uniform, consistency is high, and the reliability for material provides guarantee.
The purpose of the present invention is achieved through the following technical solutions:
A kind of AgCuNiV alloy materials, weight percent composition are:Ag is 66.5%-89.1%, Cu 9.5%- 27.72%, Ni 0%-1.98%, V 1.0%-5.0%.
In above-mentioned AgCuNiV alloy materials, the mass percent of Ni is preferably 0.475%-1.98%, more preferably 0.95%-1.98%.
A kind of preparation method of AgCuNiV alloy materials, prepares AgCuNi alloyed powders first, then by AgCuNi alloyed powders AgCuNiV alloy materials are prepared using discharge plasma sintering after being mixed with V powder;Wherein AgCuNi alloyed powders are in the material Shared mass percent is 95%-99%, and shared mass percent is 1.0%-5.0% to V powder in the material;AgCuNi is closed In bronze, the mass percent of Ag is 70%-90%;The mass percent of Cu is 10%-28%;The mass percent of Ni is 0- 2%, preferably 0.5%-2%, more preferably 1%-2%.
The preparation method of above-mentioned AgCuNiV alloy materials, comprises the following specific steps that:
(1) prepared by AgCuNi alloyed powders:AgCuNi alloyed powders are prepared using vacuum gas atomization, wherein, the quality hundred of Ag Score is 70%-90%;The mass percent of Cu is 10%-28%;The mass percent of Ni is 0%-2%;
(2) powder is sieved:AgCuNi alloyed powders made from step (1) are sieved;
(3) mechanical alloying:It is 95%-99% by AgCuNi alloyed powders mass percent, V powder mass percent is 1%- 5.0%, the mixed-powder of AgCuNi alloyed powders and V powder is subjected to mechanical alloying in the ball mill;
(4) reduction treatment:Mixed-powder obtained in step (3) is subjected to reduction treatment, furnace cooling;
(5) discharge plasma sintering:Obtained mixed-powder will be restored in step (4) in discharge plasma sintering furnace mould It is sintered in tool, then cools to room temperature with the furnace, obtain AgCuNiV alloy blanks.
After step (5), cold working step is may also include, i.e., obtained AgCuNiV alloy preforms will be sintered in step (5) Material surface is handled, and removes the graphite flake on surface layer, then carries out cold rolling processing, obtains AgCuNiV sheet materials.
In step (1), AgCuNi alloyed powders are prepared using vacuum gas atomization:Silver, copper and mickel are put into vacuum aerosolization It in graphite crucible in legal system powder stove, vacuumizes, heating fusing keeps the temperature 5-15min at 950-1050 DEG C, is sufficiently stirred, casts It dusts;Wherein silver-colored purity is more than 99.99wt%, and the purity of copper is more than 99.99wt%, and the purity of nickel is more than 99.99wt%, vanadium Purity be more than 99.99wt%.
In step (2), the AgCuNi alloyed powders granularity is 50-150 μm, and V Powder Particle Sizes are 30-50 μm.
In step (3), alloyed powder is subjected to ball-milling treatment, rotational speed of ball-mill 50-100r/min, the mechanical alloying time is 120 minutes or more.
In step (4), the reduction treatment is in hydrogen shield atmosphere, is heated to 300 DEG C -500 DEG C, keeps the temperature 1-5 Hour.
In step (5), sintering parameter is:Pressure is 30-50MPa, and temperature is 700-750 DEG C, heating rate 100-150 DEG C/min, sintering time 1-60min, atmosphere is vacuum.The mold is graphite jig.
Advantages of the present invention:
1st, AgCuNiV alloy sheet material hardness prepared by the present invention is can be controlled between 140-225HV, and the thickness of sheet material is most thin 0.5mm can be worked into, meets the requirement of contact material in radar electric device.
2nd, the present invention prepares AgCuNiV alloys using discharge plasma sintering technique for the first time, and V content can be in alloy Reach 5.0%, alloy may finally be processed into sheet material.
3rd, AgCuNiV alloys are prepared using discharge plasma sintering technique, during discharge plasma sintering, passes through point Discharge effect is held, the oxidation film of powder particle surface is abolished, and particle surface is activated, and intergranular diffusion is added By force, the process of densification is accelerated, thus the consistency of material can reach more than 99% after sintering.
4th, AgCuNiV alloys are prepared using discharge plasma sintering technique, sintering temperature is low, and sintering time is short, can be notable Inhibit grain coarsening, tiny, uniform tissue can be obtained, convenient for subsequent cold working.
5th, AgCuNiV alloys are prepared using discharge plasma sintering technique, fine microstructures are uniform, segregation-free, can be effective Ensure the reliability of contact material in radar electric device.
6th, AgCuNiV alloys are prepared using discharge plasma sintering technique, preparation process is simple, and production procedure is short.
Description of the drawings
Fig. 1 is the AgCuNiV that the embodiment of the present invention 1 obtains3.0The photo of alloy finished product.
Specific embodiment
The present invention prepares highly reliable, high V content AgCuNiV contact materials using discharge plasma sintering technique, passes through AgCuNi alloyed powders are prepared, are prepared after then mixing AgCuNi alloyed powders and V powder using discharge plasma sintering technique. AgCuNi alloyed powders are prepared using vacuum gas-atomized powder stove first, and filter out the alloyed powder that grain size is 50 μm -150 μm;So Afterwards by the way of powder mixing machine by the AgCuNi alloyed powders of preparation and V powder according to mass percent 95%-99% and 1%- 5.0% carries out mechanical mixture aurification 120 minutes or more in the ball mill;The mixed powder of preparation is carried out to also original place in hydrogen furnace Reason is subsequently placed into and waits preparation AgCuNiV alloy blanks in discharge plasma sinterings stove, and material combines preferable, consistency after sintering It is high;Finally the AgCuNiV alloy blanks of preparation are cold worked, obtain required AgCuNiV finished products.
(1) dispensing:Raw material is selected, wherein the purity of silver is more than 99.99wt%, the purity of copper is more than 99.99wt%, nickel Purity is more than 99.99wt%, and the purity of V is more than 99.99wt%, raw material is weighed according to the mass percent of each component.
(2) prepared by AgCuNi alloyed powders:AgCuNi alloyed powders, the wherein quality of Ag are prepared using vacuum gas-atomized powder stove Percentage is 70%-90%;The mass percent of Cu is 10%-28%;The mass percent of Ni is 0%-2%;It will match and can be compared to Fine silver, the fine copper of example are put into the graphite crucible in vacuum aerosolization legal system powder stove, are vacuumized, heating fusing, in 950-1050 DEG C heat preservation 5-15min, be sufficiently stirred, casting is dusted.
(3) powder is sieved:AgCuNi alloyed powders obtained are sieved, obtain the alloyed powder that grain size is 50 μm -150 μm Grain.
(4) mechanical alloying:By the AgCuNi alloyed powders of preparation and V powder according to quality percentage by the way of powder mixing machine Mechanical alloying is carried out in the ball mill than 95%-99% and 1%-5.0%, when rotational speed of ball-mill is 50-100r/min alloyings Between 120 minutes or more, V Powder Particle Sizes be 30-50 μm.
(5) reduction treatment:Obtained mixed-powder is subjected to reduction treatment in hydrogen furnace, in hydrogen shield atmosphere 300 DEG C -500 DEG C are heated to, keeps the temperature 1-5 hours, furnace cooling.
(6) discharge plasma sintering:Obtained mixed-powder loading discharge plasma sintering furnace graphite jig will be restored In, it is put into SPS stoves, quickly heating up to 700 DEG C -750 DEG C with the rate of heat addition of 100-150 DEG C/min is sintered, sintering pressure Power is 30-50MPa, and sintering time 1-60min, atmosphere is vacuum;Then it cools to room temperature with the furnace, obtains AgCuNiV alloy preforms Material.
(7) it is cold worked:The AgCuV alloy blanks surface that sintering obtains is handled, removes the graphite flake on surface layer, then Cold rolling processing is carried out, obtains required AgCuNiV alloy finished products, the thickness of finished product is most thin can be worked into 0.5mm.
Technical solution of the present invention is further described, but do not limit the present invention below with reference to embodiment and attached drawing.
Embodiment 1
(1) AgCuNi alloyed powders are prepared using vacuum gas atomization, the wherein specific ingredient of AgCuNi alloys is Ag contents For 70wt%;Cu contents are 28wt%;Ni contents are 2wt%.Filter out particle of the granularity between 50 μm -100 μm, V powders Degree selects 30 μm.(2) mixing and ball milling, ball milling are carried out according to the AgCuNi alloyed powders and 3.0% V powder that mass percent is 97% Rotating speed is 80r/min, and Ball-milling Time is 120 minutes.(3) alloyed powder after mixing and ball milling is heated in hydrogen shield atmosphere 500 DEG C, 2 hours are kept the temperature, reduction treatment is carried out to alloyed powder.(4) mixed powder is put into discharge plasma sintering stove and carried out very AgCuNiV is made in sky sintering3.0Alloy blank, wherein sintering temperature are 750 DEG C, sintering pressure 50MPa, heating rate 100 DEG C/min, 5min is kept the temperature, atmosphere is vacuum.Using AgCuNiV made from this technique3.0Alloy blank consistency can reach 99.9%.(5) to sintered AgCuNiV3.0Alloy blank surface is handled, using milling machine that the graphite of blank surface is clear Reason is clean, until blank surface is metal surface entirely, until graphite.(6) to AgCuNiV3.0Alloy blank carries out cold rolling and adds Work, is worked into 0.5mm, surface-brightening zero defect, and finished product hardness is 225HV.As shown in Figure 1, obtained for the present embodiment AgCuNiV3.0The photo of alloy finished product, it can be seen that ingredient is uniform, the smooth zero defect in surface, can be used as contact material.
Embodiment 2
The process conditions of the present embodiment are same as Example 1, are only changed to the mass percent of V powder in alloyed powder 5.0%, obtained AgCuNiV5.0The consistency of alloy blank reaches 99.8%, is worked into 1.0mm, surface-brightening zero defect, Finished product hardness is 207HV.
Embodiment 3
The process conditions of the present embodiment are same as Example 1, are only changed to the mass percent of V powder in alloyed powder 1.0%, obtained AgCuNiV1.0The consistency of alloy blank reaches 99.9%, is worked into 0.5mm, surface-brightening zero defect, Finished product hardness is 195HV.
Embodiment 4
The process conditions of the present embodiment are same as Example 1, and finished product only is processed as thickness 2.5mm finished products, finished surface Bright zero defect, finished product hardness are 218HV.
Embodiment 5
The process conditions of the present embodiment are same as Example 1, only change AgCuNi alloying components, and specific ingredient is Ag contents For 72wt%;Cu contents are 27wt%;Ni contents are 1wt%.AgCuNi alloyed powders granularity is 50-100 μm;V content is 3wt%, V Powder Particle Size are 30 μm.Obtained AgCuNiV3.0The consistency of alloy blank reaches 99.9%, is worked into 1.0mm, Surface-brightening zero defect, finished product hardness are 220HV.
Embodiment 6
The process conditions of the present embodiment are same as Example 1, and V Powder Particle Sizes only are changed to 50 μm, obtained AgCuNiV3.0The consistency of alloy blank reaches 99.8%, is worked into 1.0mm, surface-brightening zero defect, and finished product hardness is 152HV。
Embodiment 7
The process conditions of the present embodiment are same as Example 1, sintering temperature only are changed to 700 DEG C, sintering pressure change For 30MPa, obtained AgCuNiV3.0The consistency of alloy blank reaches 99.2%, is worked into 1.0mm, and surface-brightening is intact It falls into, finished product hardness is 147HV.
The present invention prepares AgCuNiV alloys using discharge plasma sintering technique, and fine microstructures are uniform, segregation-free, can be with The reliability of contact material in radar electric device is effectively ensured, acquisition ingredient is uniform, the flawless contact material in surface; Preparation process is simple simultaneously, and production procedure is short.
The embodiment of AgCuNiV alloy materials of the present invention and preparation method thereof part is only enumerated in above-described embodiment, In the technical solution of the invention described above:The AgCuNi alloyed powders particle size and percentage, V powder particles size and percentage Ratio, sintering temperature, sintering pressure, sintering rate etc. in prescribed limit can unrestricted choice, will not enumerate herein, thus with On illustrate that included technical solution should be regarded as protection domain illustrative rather than to limit the present patent application patent.

Claims (10)

1. a kind of AgCuNiV alloy materials, it is characterised in that:Its weight percent forms:Ag 66.5%-89.1%, Cu 9.5%-27.72%, Ni 0%-1.98%, V 1.0%-5.0%.
2. AgCuNiV alloy materials according to claim 1, it is characterised in that:In the AgCuNiV alloy materials, The mass percent of Ni is 0.475%-1.98%.
3. a kind of preparation method of AgCuNiV alloy materials, it is characterised in that:AgCuNi alloyed powders are prepared first, then will AgCuNiV alloy materials are prepared using discharge plasma sintering after AgCuNi alloyed powders and the mixing of V powder.
4. the preparation method of AgCuNiV alloy materials according to claim 3, it is characterised in that:This method includes as follows Step:
(1) prepared by AgCuNi alloyed powders:AgCuNi alloyed powders are prepared using vacuum gas atomization, wherein, the mass percent of Ag For 70%-90%;The mass percent of Cu is 10%-28%;The mass percent of Ni is 0%-2%;
(2) powder is sieved:AgCuNi alloyed powders obtained are sieved;
(3) mechanical alloying:It is 95%-99% by AgCuNi alloyed powders mass percent, V powder mass percent is 1%- 5.0%, the mixed-powder of AgCuNi alloyed powders and V powder is subjected to mechanical alloying in the ball mill;
(4) reduction treatment:Mixed-powder obtained is subjected to reduction treatment, furnace cooling;
(5) discharge plasma sintering:The mixed-powder that reduction obtains is sintered in discharge plasma sintering furnace mold, then It cools to room temperature with the furnace, obtains AgCuNiV alloy blanks.
5. the preparation method of AgCuNiV alloy materials according to claim 4, it is characterised in that:After step (5), Further include cold working step.
6. the preparation method of AgCuNiV alloy materials according to claim 5, it is characterised in that:The cold working is The AgCuNiV alloy blanks surface that sintering obtains is handled, removes the graphite flake on surface layer, cold rolling processing is then carried out, obtains Obtain AgCuNiV sheet materials.
7. the preparation method of AgCuNiV alloy materials according to claim 4, it is characterised in that:It is described in step (2) AgCuNi alloyed powders granularity for 50-150 μm, V Powder Particle Sizes are 30-50 μm.
8. the preparation method of AgCuNiV alloy materials according to claim 4, it is characterised in that:During mechanical alloying, ball Mill rotating speed is 50-100r/min, and the time is 120 minutes or more.
9. the preparation method of AgCuNiV alloy materials according to claim 4, it is characterised in that:The reduction treatment In hydrogen shield atmosphere, to be heated to 300 DEG C -500 DEG C, 1-5 hours are kept the temperature.
10. the preparation method of AgCuNiV alloy materials according to claim 4, it is characterised in that:During sintering, pressure is 30-50MPa, temperature are 700-750 DEG C, and heating rate is 100-150 DEG C/min, and sintering time 1-60min, atmosphere is true It is empty.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109686630A (en) * 2018-12-14 2019-04-26 郑州机械研究所有限公司 A kind of fuse silver strip
CN114974645A (en) * 2022-05-18 2022-08-30 武汉数字化设计与制造创新中心有限公司 Silver-based multi-element alloy powder material and preparation method and application thereof
WO2022208031A1 (en) * 2021-03-31 2022-10-06 Sintermat Method for manufacturing a precious metal part based on sps sintering and precious metal part thus produced

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1073292A (en) * 1991-12-12 1993-06-16 中国有色金属工业总公司昆明贵金属研究所 Silver based alloy electric contact material
CN1413794A (en) * 2001-10-09 2003-04-30 株式会社微笑智能 Brazing filler metal and diamond soldering method
CN101418393A (en) * 2008-12-01 2009-04-29 昆明贵金属研究所 Novel method for preparing AgCuV alloy material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1073292A (en) * 1991-12-12 1993-06-16 中国有色金属工业总公司昆明贵金属研究所 Silver based alloy electric contact material
CN1413794A (en) * 2001-10-09 2003-04-30 株式会社微笑智能 Brazing filler metal and diamond soldering method
CN101418393A (en) * 2008-12-01 2009-04-29 昆明贵金属研究所 Novel method for preparing AgCuV alloy material

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109686630A (en) * 2018-12-14 2019-04-26 郑州机械研究所有限公司 A kind of fuse silver strip
CN109686630B (en) * 2018-12-14 2020-08-28 郑州机械研究所有限公司 Preparation method of silver sheet for fuse
WO2022208031A1 (en) * 2021-03-31 2022-10-06 Sintermat Method for manufacturing a precious metal part based on sps sintering and precious metal part thus produced
FR3121375A1 (en) * 2021-03-31 2022-10-07 Sintermat Process for manufacturing precious metal parts based on SPS sintering and precious metal part thus obtained
CN114974645A (en) * 2022-05-18 2022-08-30 武汉数字化设计与制造创新中心有限公司 Silver-based multi-element alloy powder material and preparation method and application thereof

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