CN104894421A - Preparation method of novel Ag-based lanthanum stannate composite electric contact material - Google Patents

Preparation method of novel Ag-based lanthanum stannate composite electric contact material Download PDF

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CN104894421A
CN104894421A CN201510222665.1A CN201510222665A CN104894421A CN 104894421 A CN104894421 A CN 104894421A CN 201510222665 A CN201510222665 A CN 201510222665A CN 104894421 A CN104894421 A CN 104894421A
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agla
preparation
powder
contact material
agla2sn2o7
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CN104894421B (en
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张玲洁
杨辉
沈涛
樊先平
申乾宏
陈乐生
张继
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention relates to preparation of an electric contact material and provides a preparation method of a novel Ag-based lanthanum stannate composite electric contact material. The preparation method comprises carrying out ball-mill mixing on Ag powder and lanthanum stannate nanometer powder to obtain AgLa2Sn2O7 composite powder, carrying out hot pressing sintering treatment to obtain an AgLa2Sn2O7 blank block, and carrying out hot extrusion treatment to obtain an AgLa2Sn2O7 wire rod. The preparation method utilizes a simple AgLa2Sn2O7 composite powder synthesis technology, utilizes a ball milling technology to realize synthesis and has a low cost. Compared with AgSnO2, the AgLa2Sn2O7 wire rod has lower specific resistance, higher elongation percentage after annealing fracture, good tensile strength, excellent mechanical properties and better welding resistance.

Description

The preparation method of new A g base stannic acid lanthanum composited contact material
Technical field
The present invention relates to the technology of preparing of contact material, particularly a kind of preparation of new A g base stannic acid lanthanum composited contact material and commercial application thereof, this materials application in low-voltage apparatus as in the equipment such as alternating current contactor, rly., air switch.
Background technology
Contact material and element, as the key foundation of electrical equipment industry, are responsible for the task of joint weldment electric current, and its performance is directly connected to the break-make capacity of whole set equipment, work-ing life and serviceability.AgCdO contact material was once used widely because of premium propertiess such as low, the anti-melting welding of its contact resistance, resistance to arc erosions, enjoyed the good reputation of " omnipotent contact ".But AgCdO contact material in use can discharge virose Cd steam, the RoSH instruction that European Union promulgates simultaneously limits the use of AgCdO contact material, need find corresponding substitute.AgSnO 2because it possesses steady the determining property ﹑ anti electric arc corrosion of high heat and the feature such as environmentally friendly, and become the conventional contact material of alternative AgCdO.But in the U.S. and China, Ag/SnO 2still there will be high arc erosion rate in process under arms, Welding Phenomena occurs, restriction Ag/SnO 2the further use of contact material.
In conjunction with current at Ag/SnO 2the surface arcing of contact material corrodes behavior and inefficacy mechanism aspect bibliographical information and experimental studies results thereof and shows: add rare earth element or its mixture and SnO 2surface modification will become and improve arc erosion, reduce melting welding power, improve one of effective way of electric life.The La of pyrochlore constitution is pointed out in correlative study 2sn 2o 7powder and SnO 2have similar physico-chemical property and higher oxygen ion vacancy conductive characteristic, simultaneously La 2sn 2o 7the experiment that the good mechanical property that powder plays in Ag base electrical contact material as the second wild phase and anti-fusion welding property have obtained this seminar confirms.The AgLa of experiment synthesis 2sn 2o 7contact material has minimum resistivity (≤2.2 μ Ω cm), and show through metal material stretching test result: annealed state elongation after fracture reaches to 24%, tensile strength is 230MPa.Compared to AgSnO 2, AgLa 2sn 2o 7contact material shows less melting welding power.
But the deficiency that existing technology exists is: Ag/SnO 2contact material is when hot extrude silk pressing material technique because hardness is excessive, and unit elongation is lower, causes a material course of processing to rupture, the major defects such as stripping, and occur high contact resistance in this external actual military service process, high melting welding power, reduces Ag/SnO 2the work-ing life of contact material.And AgLa of the present invention 2sn 2o 7the military service effect performance get Geng Jia of contact material in mechanical property and fusion welding property.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes Ag/SnO in prior art 2the defects such as the high erosion ratio of contact material and melting welding, provide a kind of preparation method of new A g base stannic acid lanthanum composited contact material.The product that the method obtains can be used in improving contact material resistance fusion welding energy, and Reactive Synthesis condition is simple and easy, with low cost.
For technical solution problem, solution of the present invention is:
A kind of preparation method of new A g base stannic acid lanthanum composited contact material is provided, comprises the following steps:
(1) Ag-La 2sn 2o 7the preparation of composite granule
Ag powder and stannic acid lanthanum nano-powder are weighed according to mass ratio 88: 12, ball milling mixes 4 hours, obtains AgLa 2sn 2o 7composite granule;
(2) by AgLa 2sn 2o 7composite granule carries out hot pressed sintering process, obtains AgLa 2sn 2o 7briquet; Then to AgLa 2sn 2o 7briquet carries out hot extrusion, and obtaining diameter is the AgLa of 1.5 ~ 3.5mm 2sn 2o 7wire rod;
During hot pressed sintering, control condition is: hot pressing pressure 450MPa, die temperature 500 DEG C; During hot extrusion, control condition is: extruding tonnage 50T, extrusion mould Heating temperature 500 DEG C.
In the present invention, also comprise AgLa 2sn 2o 7the further process of wire rod: by process and the wire drawing process of swaging, obtain the AgLa that diameter is 1.85 ~ 2.8mm 2sn 2o 7silk material.
In the present invention, also comprise AgLa 2sn 2o 7the further process of silk material: by AgLa 2sn 2o 7the rivet that rivet driver is processed into predetermined size specification sent into by silk material, at N 2the lower 400 DEG C of heating 6h of atmosphere, carry out annealing process process.
Stannic acid lanthanum nano powder system in the present invention prepares according to the step introduced in Chinese invention patent application " a kind of preparation method of high purity stannic acid lanthanum nano-powder " (application number 201410488560.6).
In the present invention, obtain AgLa 2sn 2o 7after briquet, the performance tests such as density, Vickers' hardness and resistivity can be carried out for it.Obtain AgLa 2sn 2o 7after wire rod, the process of employing post-treatment can also be carried out, namely by multiple tracks swage process and wire drawing process obtain AgLa 2sn 2o 7silk material, and carry out corresponding performance test.Recycling AgLa 2sn 2o 7silk material is processed into the rivet of different size and carries out annealing process process on rivet driver, is then mounted on electrical endurance test machine and carries out electric life test.
Compared with prior art, beneficial effect of the present invention is:
(1) AgLa 2sn 2o 7the synthesis technique of composite granule is simplified.Compared in the past conventional high-energy ball milling+mechanically mixing technique, this experiment only adopts ball-milling technology (Ball-milling Time is short, only needs 4h) just can realize AgLa 2sn 2o 7the synthesis of composite granule, cost is cheaper.
(2) AgLa 2sn 2o 7the excellent in mechanical performance of silk material.Compared to AgSnO 2, AgLa 2sn 2o 7silk material shows lower resistivity, higher annealed state elongation after fracture and preferably tensile strength.
(3) AgLa 2sn 2o 7the anti-fusion welding property of silk material is excellent.Compared to AgSnO 2, AgLa 2sn 2o 7show better anti-fusion welding property.
Embodiment
Below by embodiment, implementation of the present invention is described.
One, the preparation of stannic acid lanthanum nano-powder
(1) preparation of precursor solution A
Two oxalic acid hydrates are added in deionized water, with magnetic agitation to dissolving completely, then move constant volume in liquid to volumetric flask, being mixed with the colourless transparent solution that concentration is 0.03 ~ 0.6mol/L, i.e. precursor solution A;
(2) preparation of precursor solution B
By mol ratio be 1: 1 lanthanum nitrate and stannic chloride pentahydrate be added in deionized water, with magnetic agitation to dissolving completely, then constant volume in liquid to volumetric flask is moved, be mixed with the colourless transparent solution that total concn is 0.2 ~ 1.5mol/L (being the concentration that two kinds of solutes add up to), i.e. precursor solution B;
(3) preparation of stannic acid lanthanum nano-powder
Precursor solution B is imported in precursor solution A in dropping mode, forms homogeneous transparent solution; Then polyvinyl alcohol (PVA) and citric acid jelling agent is added, even with magnetic agitation; Polyvinyl alcohol (PVA) in mixing solutions and the mass concentration of citric acid jelling agent are respectively 1 ~ 5wt% and 2 ~ 10wt%;
Be the ammonia soln of 25% ~ 28% to mixed solution and dripping concentration, regulate pH to 7 ~ 9, and continue to stir 2h under room temperature; Then at room temperature sedimentation 24h, removes supernatant liquor, obtains powder 80 DEG C of oven dry;
Powder after drying is ground, after crossing 200 mesh sieves, at 900 ~ 1100 DEG C of sintering 2h ~ 5h, finally obtains the stannic acid lanthanum nano-powder be creamy white.
Two, the preparation of Ag base stannic acid lanthanum composited contact material
(1) Ag-La 2sn 2o 7the preparation of composite granule
Ag powder and stannic acid lanthanum nano-powder are weighed according to mass ratio 88:12, ball milling mixes 4 hours, obtains AgLa 2sn 2o 7composite granule;
(2) by AgLa 2sn 2o 7composite granule carries out hot pressed sintering process, obtains AgLa 2sn 2o 7briquet; Then to AgLa 2sn 2o 7briquet carries out hot extrusion, and obtaining mean diameter is the AgLa of 1.5 ~ 3.5mm 2sn 2o 7wire rod;
During hot pressed sintering, control condition is: hot pressing pressure 500MPa, die temperature 500 DEG C; During hot extrusion, control condition is: extruding tonnage 50T, extrusion mould Heating temperature 500 DEG C.
(3) to AgLa 2sn 2o 7wire rod carry out multiple tracks swage process and wire drawing process, obtain the AgLa that diameter is 1.85 ~ 2.8mm 2sn 2o 7silk material.
(4) by AgLa 2sn 2o 7the rivet that rivet driver is processed into predetermined dimension sent into by silk material, at N 2the lower 400 DEG C of heating 6h of atmosphere, carry out annealing process process.
By the AgLa of preparation 2sn 2o 7rivet is mounted on electrical endurance test machine and carries out electric life test, and test number (TN) is 20k time.Test-results shows AgLa 2sn 2o 7show better anti-fusion welding property.
Compared to the AgSnO of prior art 2material, AgLa in the present invention 2sn 2o 7the advantage of material in mechanical property and fusion welding property is as shown in table 1 below.
AgLa in table 1 the present invention 2sn 2o 7the AgSnO of material and prior art 2otherness between material

Claims (3)

1. the preparation method of new A g base stannic acid lanthanum composited contact material, is characterized in that, comprise the following steps:
(1) Ag-La 2sn 2o 7the preparation of composite granule
Ag powder and stannic acid lanthanum nano-powder are weighed according to mass ratio 88: 12, ball milling mixes 4 hours, obtains AgLa 2sn 2o 7composite granule;
(2) by AgLa 2sn 2o 7composite granule carries out hot pressed sintering process, obtains AgLa 2sn 2o 7briquet; Then to AgLa 2sn 2o 7briquet carries out hot extrusion, and obtaining diameter is the AgLa of 1.5 ~ 3.5mm 2sn 2o 7wire rod;
During hot pressed sintering, control condition is: hot pressing pressure 450MPa, die temperature 500 DEG C; During hot extrusion, control condition is: extruding tonnage 50T, extrusion mould Heating temperature 500 DEG C.
2. method according to claim 1, is characterized in that, also comprises AgLa 2sn 2o 7the further process of wire rod: by process and the wire drawing process of swaging, obtain the AgLa that diameter is 1.85 ~ 2.8mm 2sn 2o 7silk material.
3. method according to claim 1, is characterized in that, also comprises AgLa 2sn 2o 7the further process of silk material: by AgLa 2sn 2o 7the rivet that rivet driver is processed into predetermined dimension sent into by silk material, at N 2the lower 400 DEG C of heating 6h of atmosphere, carry out annealing process process.
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Cited By (7)

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CN105970015A (en) * 2016-06-26 2016-09-28 浙江大学 Method for preparing silver carbon nanotube and lanthanum zirconate composite electric contact material
CN106048288A (en) * 2016-05-30 2016-10-26 浙江大学 Raw material formula and preparation method of high-conductivity silver-based composite material
CN106636723A (en) * 2016-12-30 2017-05-10 衢州学院 Preparation method of Ag-based electric contact material with La1-xSrxInO3 microspheres as strengthening phase
CN107052075A (en) * 2017-05-31 2017-08-18 浙江大学 Multimode is cold to swage and cold drawn processing AgSnO2The method of wire rod
CN107574333A (en) * 2017-08-10 2018-01-12 浙江大学 A kind of preparation method of Ag YAG contact materials
CN107695360A (en) * 2017-09-01 2018-02-16 浙江大学 Graphene is modified the preparation method of silver-colored stannic acid lanthanum electric contact composite material
CN108408763A (en) * 2018-02-13 2018-08-17 浙江大学 It is a kind of be co-doped with niobium, indium nano tin-oxide powder preparation and application process

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106048288A (en) * 2016-05-30 2016-10-26 浙江大学 Raw material formula and preparation method of high-conductivity silver-based composite material
CN106048288B (en) * 2016-05-30 2017-11-28 浙江大学 The composition of raw materials and preparation method of highly conductive silver-based composite material
CN105970015A (en) * 2016-06-26 2016-09-28 浙江大学 Method for preparing silver carbon nanotube and lanthanum zirconate composite electric contact material
CN105970015B (en) * 2016-06-26 2017-08-25 浙江大学 The preparation method of silver-colored CNT zirconic acid lanthanum composited contact material
CN106636723A (en) * 2016-12-30 2017-05-10 衢州学院 Preparation method of Ag-based electric contact material with La1-xSrxInO3 microspheres as strengthening phase
CN107052075A (en) * 2017-05-31 2017-08-18 浙江大学 Multimode is cold to swage and cold drawn processing AgSnO2The method of wire rod
CN107052075B (en) * 2017-05-31 2019-01-08 浙江大学 Multimode is cold to swage and cold drawing processing AgSnO2The method of wire rod
CN107574333A (en) * 2017-08-10 2018-01-12 浙江大学 A kind of preparation method of Ag YAG contact materials
CN107695360A (en) * 2017-09-01 2018-02-16 浙江大学 Graphene is modified the preparation method of silver-colored stannic acid lanthanum electric contact composite material
CN107695360B (en) * 2017-09-01 2019-05-03 浙江大学 The preparation method of the modified silver-colored stannic acid lanthanum electric contact composite material of graphene
CN108408763A (en) * 2018-02-13 2018-08-17 浙江大学 It is a kind of be co-doped with niobium, indium nano tin-oxide powder preparation and application process
CN108408763B (en) * 2018-02-13 2019-12-06 浙江大学 preparation and application method of niobium and indium co-doped nano tin oxide powder

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Application publication date: 20150909

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