CN106086495A - Cupric oxide doped siller tin oxide composite and preparation method thereof - Google Patents

Cupric oxide doped siller tin oxide composite and preparation method thereof Download PDF

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CN106086495A
CN106086495A CN201610432717.2A CN201610432717A CN106086495A CN 106086495 A CN106086495 A CN 106086495A CN 201610432717 A CN201610432717 A CN 201610432717A CN 106086495 A CN106086495 A CN 106086495A
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silver
composite
oxide
copper
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CN106086495B (en
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李桂景
冯文杰
房学谦
刘金喜
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Shijiazhuang Tiedao University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver

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

The present invention relates to silver-base metal field of material technology, especially relate to a kind of low tension contact material, specifically disclosing a kind of cupric oxide doped siller tin oxide composite, the composition of described composite includes 4.9 18.5% stannum oxide and 0.1 1.5% copper oxide by weight percentage, and surplus is silver.Its preparation method, including: prepare silver-bearing copper complex, and silver-bearing copper complex is mixed with putty powder, re-compacted molding, sintering；Described silver-bearing copper complex includes argentum powder, and is coated on the copper oxide presoma on argentum powder surface.Composite of the present invention has the advantages such as microstructure is uniform, good processability, resistivity are low, it is adaptable to contact material, has good stability and longer service life.Its preparation method has simple and easy to do, the advantage such as production efficiency height, non-environmental-pollution.

Description

Cupric oxide doped siller tin oxide composite and preparation method thereof
Technical field
The present invention relates to silver-base metal field of material technology, especially relate to a kind of low tension contact material.
Background technology
Silver-based electric contact material has preferably conduction, heat conduction and electrical contact performance, be low voltage switch, chopper, The core component of instrument and meter, is responsible for the break-make of electric current, and its performance directly influences the normal use of electric system.Traditional Silver-based electric contact material is Agcdo composite, generates due to it and use process can produce heavy metal cadmium and the most banned Only use.
Siller tin oxide composite be a kind of with Ag as matrix, SnO2It is the metal-base composites of the second phase, environment-friendly type Good, there is stronger anti-melting welding and resistance to arc erosion performance, it progressively obtains extensively should at appliance field as contact material With, it is expected to replace Agcdo.
But, in the preparation, nonwetting between silver and stannum oxide, interface belongs to mechanical bond, meeting to siller tin oxide composite Causing composite fragility big, processing difficulties, particularly electric conductivity are decreased obviously along with the increase of stannum oxide content, and Stannum oxide is easily caused to be enriched with in arc erosion process, temperature rise.For increasing the wettability between silver and tin ash, add oxidation Copper is a kind of effective means, but current technology is only limitted to direct mixed oxidization copper powders.
The ripe preparation method of tin-oxygen-silver electric contact material mainly has internal oxidation and powder metallurgic method, the most realizes Industrialized production.Powder metallurgic method is that component is made powder, after mixing, shapes sintering.Internal oxidation is first component It is smelted into alloy by proportioning, after processed molding, carries out internal oxidition process.All there is copper oxide and tin ash in two kinds of methods The content of problem the most pockety, especially copper oxide is relatively low, and can it the most uniformly divide Cloth, the performance boost to material is most important.In powder metallurgic method, cupric oxide powder consumption is few, and its mixed powder efficiency is low, uniformity Difference, easily causes microstructure uneven, makes material property be affected, such as poor processability, easily in composite edge Crackle occurs.And owing to oxygen is in alloy diffusion inside difficulty in internal oxidation, oxidation often can be caused uneven, produce lean oxidation Band, material inside organization is uneven, affects stability and the service life of product.The skewness of copper oxide and material internal group Knit uneven, cause cupric oxide doped tin-oxygen-silver electric contact material still suffer from uniformity and processing characteristics is poor, resistivity relatively High shortcoming.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of cupric oxide doped siller tin oxide composite and preparation side thereof Method, this composite has the advantages such as microstructure is uniform, good processability, resistivity are low, is suitable to contact material, has good Good stability and long service life.Its preparation method has simple and easy to do, and production efficiency is high, the advantage of non-environmental-pollution.
For solving above-mentioned technical problem, the technical solution used in the present invention is: cupric oxide doped siller tin oxide composite wood Material, described composite is the silver-based composite material containing stannum oxide and copper oxide, is made up of material powder sintering, described oxidation Copper is that copper oxide presoma generates at the sintering process situ of described composite.
Further, the composition of described composite includes 4.9-18.5% stannum oxide and 0.1-by weight percentage 1.5% copper oxide, surplus is silver.
The preparation method of aforementioned oxidation Copper-cladding Aluminum Bar siller tin oxide composite, including:
Prepare silver-bearing copper complex,
And silver-bearing copper complex is mixed with putty powder, re-compacted molding, sintering；
Described silver-bearing copper complex includes argentum powder, and is coated on the copper oxide presoma on argentum powder surface.
Described copper oxide presoma is the complex of copper ion and surfactant, and described surfactant contains sulfydryl, Described surfactant can form chemical bond by sulfydryl with silver so that described complex is coated on argentum powder surface.
As preferably, described surfactant is TGA or mercaptoethylmaine.
Further, the preparation method of silver-bearing copper complex is, by argentum powder and the solution of described surfactant, Cu2+Salt is molten Liquid hybrid reaction, obtains silver-bearing copper complex presoma, and it is cleaned after drying, anneals in vacuum environment, prepares silver-bearing copper complex, For powder.Cu2+Salt is the mantoquitas such as copper nitrate, copper chloride or copper sulfate.
As preferably, described surfactant and Cu2+Mol ratio be 10:1.
The particle size range of described argentum powder is that 50 nanometers are to 200 mesh.
Further, in 60 after described silver-bearing copper complex presoma cleansoC is dried, 250oC vacuum annealing.
Further, described sintering temperature controls at 750-850oC。
After described sintering completes, also include sintered product is carried out multiple pressure and resintering；The pressure of described multiple pressure is higher than previous Compressing pressure, the temperature of described resintering is less than the temperature of previous sintering.
Use and have the beneficial effects that produced by technique scheme: the present invention cupric oxide doped siller tin oxide composite Preparation method use surfactant, in the solution copper ion is self-assembled to argentum powder surface and forms copper oxide presoma, logical Later continue and clean, be dried and after heat treatment, uniformly mix with a certain amount of tin dioxide powder, repressed and high temperature sintering, oxidation Copper presoma decomposes, and is formed in situ copper oxide in silver and stannum oxide interface so that the wettability between silver and tin ash is good, Being obtained in that novel oxidized Copper-cladding Aluminum Bar tin-oxygen-silver electric contact material, this composite has good Microstructure Uniformity, Its machinability and electric conductivity are significantly improved compared to prior art, and utilize what composite of the present invention made to touch Head, its surface good dispersion to electric arc, hence it is evident that reduce the enrichment of stannum oxide.
Preparation method of the present invention makes argentum powder surface attachment uniform copper oxide presoma, according to silver-bearing copper complex of the present invention Preparation method, prepare size about 5 nanometer of copper oxide presoma, see Fig. 1, it is thus possible to increase mixed powder efficiency and uniformity.
Preparation method of the present invention utilizes the surfactant containing sulfydryl, the sulfur hydrogen bond of surfactant in aqueous Chemical bond, the other functional group (such as carboxyl or amido) of surfactant and copper ion complexation is formed, finally with argentum powder surface Realize copper ion and be coated on silver surface, it is possible to obtain uniform silver-copper nano complex, there is the highest production efficiency, operation letter Single feasible, it is suitable for large-scale production.Simultaneously as copper oxide presoma loads at argentum powder surface trace, activating agent consumption is few, raw Product process will not cause environmental pollution.
Cupric oxide doped siller tin oxide composite prepared by the inventive method, in the range of aforesaid ingredients, through testing it Conductivity is 89%IACS(International Annealed Copper Standard to the maximum), improve 11% than silver tin oxide material, hardness is 58.28, declines 6%, When forced compression, composite edge does not has crackle, has the strongest resistance to arc erosion performance simultaneously.
Accompanying drawing explanation
Fig. 1 is the inventive method SEM photograph after argentum powder area load copper oxide presoma；
Fig. 2 is Ag-SnO2Composite (a) and Ag-CuO/SnO of the present invention2Composite (b) electric arc under 5 kilovoltages is invaded Lose the electron scanning micrograph after 50 times.
Detailed description of the invention
The present invention provides a kind of cupric oxide doped siller tin oxide composite and preparation method thereof, concrete: by copper nitrate Or the salt such as copper sulfate is configured to certain density aqueous solution, whipping process adds the surfactants such as TGA, its with copper from The mol ratio of son is 10:1；After reaction 24h, clean, be dried, 250oC heat treatment, forms silver-bearing copper complex, sees Fig. 1；Use again Ripe powder metallurgic method sinter molding, i.e. mixes with tin ash powder, and being formed with weight proportion is 75-95% silver, 4.9- 18.5% stannum oxide, the composite powder of 0.1-1.5% copper oxide, 200MPa forming under the pressure in mould, at 750-850oC calcines 2h.Follow-up 800MPa presses and again 600oC heat treatment, it is also possible to carry out cold working, prepares contact material of good performance.
Prepared composition ratio is different as stated above cupric oxide doped siller tin oxide composite and nano composite material.
Embodiment 1
Cupric oxide doped siller tin oxide composite, it is containing 5wt% stannum oxide, the silver-based composite material of 0.1wt% copper oxide.
By this composition proportion, 1mM TGA is configured to aqueous solution, under the conditions of magnetic agitation, adds argentum powder (200 mesh), Copper nitrate solution complex reaction 24h with 0.1mM.After cleaning 60oC is dried, 250oC vacuum annealing, the silver-bearing copper complex obtained After powder mixes with nano oxidized glass putty, 200MPa is compressing, 750oC sinters 2h, prepares the cupric oxide doped silver of the present embodiment Stannum oxide composite.
In various embodiments of the present invention, mM is mmol/L, mM every liter.
Embodiment 2
Cupric oxide doped siller tin oxide composite, it is containing 15wt% stannum oxide, the money base composite wood of 0.5wt% copper oxide Material.
By this composition proportion, 1mM TGA is configured to aqueous solution, under the conditions of magnetic agitation, adds argentum powder (200 mesh), Copper-bath complex reaction 24h with 0.2mM.After cleaning 60oC is dried, 250oC vacuum annealing, the silver-bearing copper complex obtained After powder mixes with nano oxidized glass putty, 200MPa is compressing, 750oC sinters 2h, prepares the cupric oxide doped silver of the present embodiment Stannum oxide composite.
Embodiment 3
Cupric oxide doped siller tin oxide composite, it is containing 10wt% stannum oxide, the money base composite wood of 0.3wt% copper oxide Material.
By this composition proportion, 2mM TGA is configured to aqueous solution, under the conditions of magnetic agitation, adds the argentum powder of 200 mesh, Copper chloride solution complex reaction 24h with 0.2mM.After cleaning 60oC is dried, 250oC vacuum annealing, the silver-bearing copper complex obtained After powder mixes with nano oxidized glass putty, 200MPa is compressing, 750oC sinters 2h, prepares the cupric oxide doped silver of the present embodiment Stannum oxide composite.
Embodiment 4
Cupric oxide doped siller tin oxide composite, it is containing 10wt% stannum oxide, the money base composite wood of 1.20wt% copper oxide Material.
By this composition proportion, 3mM mercaptoethylmaine is configured to aqueous solution, under the conditions of magnetic agitation, adds the argentum powder of 200 mesh, Copper nitrate solution complex reaction 24h with 0.3mM.After cleaning 60oC is dried, 250oC vacuum annealing, the silver-bearing copper complex obtained After powder mixes with nano oxidized glass putty, 200MPa is compressing, 750oC sinters 2h, after 800MPa presses again, 600oC resintering, system Obtain the present embodiment cupric oxide doped siller tin oxide composite.
Embodiment 5
Cupric oxide doped siller tin oxide composite, it is containing 10wt% stannum oxide, the money base composite wood of 1.5wt% copper oxide Material.
By this composition proportion, 4mM mercaptoethylmaine is configured to aqueous solution, under the conditions of magnetic agitation, adds the argentum powder of 200 mesh, Copper nitrate solution complex reaction 24h with 0.4mM.After cleaning 60oC is dried, 250oC vacuum annealing, the silver-bearing copper complex obtained After powder mixes with nano oxidized glass putty, 200MPa is compressing, 850oC sinters after 2h, 800MPa press again 600oC resintering, system Obtain the present embodiment cupric oxide doped siller tin oxide composite.
Embodiment 6
Cupric oxide doped siller tin oxide composite, it is containing 15wt% stannum oxide, the money base composite wood of 1.4wt% copper oxide Material.
By this composition proportion, 3mM mercaptoethylmaine being configured to aqueous solution, the average diameter added under the conditions of magnetic agitation is The argentum powder of 10 microns, with the copper nitrate solution complex reaction 24h of 0.3mM.After cleaning 60oC is dried, 250oC vacuum annealing, After the silver-bearing copper complex powder arrived mixes with nano oxidized glass putty, 200MPa is compressing, 850oC sinters 2h, 800MPa and presses again Rear 600oC resintering, prepares the present embodiment cupric oxide doped siller tin oxide composite.
Embodiment 7
Cupric oxide doped siller tin oxide composite, it is that the money base containing 10wt% stannum oxide, 0.6wt% copper oxide is nano combined Material.
By this composition proportion, 1mM TGA and 1mM mercaptoethylmaine are configured to aqueous solution, add under the conditions of magnetic agitation Enter the argentum powder that average diameter is 100 nanometers, with the copper nitrate solution complex reaction 24h of 0.2mM.After cleaning 60oDo for C degree Celsius Dry, 250oC vacuum annealing, after the silver-bearing copper complex powder obtained mixes with nano oxidized glass putty, 200MPa is compressing, 800oC sinters after 2h, 800MPa press again 600oC resintering, prepares the present embodiment cupric oxide doped siller tin oxide composite.
Embodiment 8
Cupric oxide doped siller tin oxide composite, it is that the money base containing 15wt% stannum oxide, 1.0wt% copper oxide is nano combined Material.
By this composition proportion, 2mM TGA is configured to aqueous solution, under the conditions of magnetic agitation, adds a certain amount of 50 nanometers Argentum powder, with the copper chloride solution complex reaction 24h of 0.2mM.After cleaning 60oC is dried, 250oC vacuum annealing, the silver obtained After copper complex powder mixes with nano oxidized glass putty, 200MPa is compressing, 850oC sinters after 2h, 800MPa press again 600oC Resintering, prepares the present embodiment cupric oxide doped siller tin oxide composite.
Cupric oxide doped siller tin oxide composite prepared by various embodiments of the present invention, due to content and the silver of copper oxide The granularity of powder is different, and conductivity and mechanical property are the most different, but, the doping of copper oxide can significantly improve moulding of composite Property and conductivity, simultaneously also be able to strengthen arc ablation resistance performance, reduce the arc time, see Fig. 2 and following table.
Ag-CuO/SnO in table 12Composite is the silver that composition quality ratio is 95% prepared by the inventive method, 5% Stannum oxide and copper oxide composite, 200MPa is compressing, 750oC sinters 2h, and under 800MPa pressure multiple pressure with 600oC resintering, its conductivity and hardness are better than congruent commercial product.
Above the present invention is described in detail, the present invention applies specific case embodiments of the present invention are carried out Illustrating, the explanation of above example is only intended to help and understands the present invention, it is noted that for the technology people of the art For Yuan, under the premise without departing from the principles of the invention, also the present invention can be carried out some improvement, these improvement also fall into this In bright scope of the claims.

Claims (10)

  1. The most cupric oxide doped siller tin oxide composite, it is characterised in that: described composite is containing stannum oxide and copper oxide Silver-based composite material, by material powder sintering make, described copper oxide is the copper oxide presoma burning at described composite Knot technique situ generates.
  2. Cupric oxide doped siller tin oxide composite the most according to claim 1, it is characterised in that described composite Composition includes 4.9-18.5% stannum oxide and 0.1-1.5% copper oxide by weight percentage, and surplus is silver.
  3. The preparation method of the most cupric oxide doped siller tin oxide composite, it is characterised in that including:
    Prepare silver-bearing copper complex, and silver-bearing copper complex is mixed with putty powder, re-compacted molding, sintering；
    Described silver-bearing copper complex includes argentum powder, and is coated on the copper oxide presoma on argentum powder surface.
  4. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 3, it is characterised in that described Copper oxide presoma is the complex of copper ion and surfactant, and described surfactant contains sulfydryl, described surface activity Agent can form chemical bond by sulfydryl with silver so that described complex is coated on argentum powder surface.
  5. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 4, it is characterised in that described Surfactant is TGA or mercaptoethylmaine.
  6. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 4, it is characterised in that silver-bearing copper The preparation method of complex is, by argentum powder and the solution of described surfactant, Cu2+Saline solution hybrid reaction, obtains silver-bearing copper multiple Fit presoma, it is cleaned after drying, anneals in vacuum environment, prepares silver-bearing copper complex, for powder.
  7. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 6, it is characterised in that described Surfactant and Cu2+Mol ratio be 10:1.
  8. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 6, it is characterised in that described The particle size range of argentum powder is that 50 nanometers are to 200 mesh.
  9. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 6, it is characterised in that described In 60 after the cleaning of silver-bearing copper complex presomaoC is dried, 250oC vacuum annealing.
  10. The preparation method of cupric oxide doped siller tin oxide composite the most according to claim 3, it is characterised in that institute State sintering temperature to control at 750-850oC；After described sintering completes, also include sintered product is carried out multiple pressure and resintering；Described The pressure of multiple pressure is higher than previous compressing pressure, and the temperature of described resintering is less than the temperature of previous sintering.
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Publication number Priority date Publication date Assignee Title
CN108493024A (en) * 2018-05-22 2018-09-04 东北大学 A kind of silver-tin electrical contact material and preparation method thereof
CN109880572A (en) * 2019-01-29 2019-06-14 安徽天光传感器有限公司 A kind of preparation method of sensor high-conductive heat-resistant conducting resinl
CN110468295A (en) * 2019-08-05 2019-11-19 李忠勇 A kind of strong―binding interface type Ag/SnO2The preparation method of contact material
CN112831683A (en) * 2020-12-31 2021-05-25 东莞正丰科技有限公司 Electric contact material and preparation method thereof
CN113699402A (en) * 2021-08-25 2021-11-26 石家庄铁道大学 Preparation method of silver tin oxide electrical contact material containing copper oxide nano additive

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108493024A (en) * 2018-05-22 2018-09-04 东北大学 A kind of silver-tin electrical contact material and preparation method thereof
CN109880572A (en) * 2019-01-29 2019-06-14 安徽天光传感器有限公司 A kind of preparation method of sensor high-conductive heat-resistant conducting resinl
CN110468295A (en) * 2019-08-05 2019-11-19 李忠勇 A kind of strong―binding interface type Ag/SnO2The preparation method of contact material
CN112831683A (en) * 2020-12-31 2021-05-25 东莞正丰科技有限公司 Electric contact material and preparation method thereof
CN113699402A (en) * 2021-08-25 2021-11-26 石家庄铁道大学 Preparation method of silver tin oxide electrical contact material containing copper oxide nano additive

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