CN104894421B - 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

Info

Publication number
CN104894421B
CN104894421B CN201510222665.1A CN201510222665A CN104894421B CN 104894421 B CN104894421 B CN 104894421B CN 201510222665 A CN201510222665 A CN 201510222665A CN 104894421 B CN104894421 B CN 104894421B
Authority
CN
China
Prior art keywords
agla
preparation
powder
agla2sn2o7
contact material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510222665.1A
Other languages
Chinese (zh)
Other versions
CN104894421A (en
Inventor
张玲洁
杨辉
沈涛
樊先平
申乾宏
陈乐生
张继
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang University ZJU
Original Assignee
Zhejiang University ZJU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang University ZJU filed Critical Zhejiang University ZJU
Priority to CN201510222665.1A priority Critical patent/CN104894421B/en
Publication of CN104894421A publication Critical patent/CN104894421A/en
Application granted granted Critical
Publication of CN104894421B publication Critical patent/CN104894421B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Powder Metallurgy (AREA)

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 new A g base stannic acid lanthanum composited contact material Preparation and commercial application, this materials application sets in low-voltage electrical apparatus such as A.C. contactor, relay, air switch etc. In Bei.
Background technology
Contact material and element, as the key foundation of electrical equipment industry, are responsible for connecting with breaking current of task, its property Break-make capacity, service life and the operational reliability of whole set equipment can be directly connected to.AgCdO contact material is because of it The premium properties such as contact resistance melting welding low, anti-, resistance to arc erosion were once used widely, and enjoyed the U.S. of " omnipotent contact " Reputation.But, AgCdO slider material in use can discharge virose Cd steam, and European Union promulgates simultaneously RoSH instruction limits the use of AgCdO slider material, need to find corresponding succedaneum.AgSnO2Because it possesses height Heat stability anti electric arc corrosion and the feature such as environmentally friendly, and become the conventional slider material substituting AgCdO. But at the U.S. and China, Ag/SnO2Still there will be high arc erosion rate during under arms, Welding Phenomena occur, Restriction Ag/SnO2The further use of contact material.
In conjunction with current at Ag/SnO2The surface arcing of slider material corrode behavior and inefficacy mechanism aspect document report thereof and Experimental studies results shows: add rare earth element or its complex and SnO2Surface modification will become and improve arc erosion, Reduce melting welding power, improve one of effective way of electric life.Correlational study points out the La of pyrochlore constitution2Sn2O7Powder body with SnO2Have similar physicochemical property and higher oxygen ion vacancy conductive characteristic, La simultaneously2Sn2O7Powder body is as second The good mechanical property of enhancing performance in Ag base electrical contact material and anti-fusion welding property have obtained the reality of this seminar Checking is real.The AgLa of experiment synthesis2Sn2O7Contact material has minimum resistivity (≤2.2 μ Ω cm), through metal Material tensile test result shows: annealed state elongation after fracture up to 24%, and tensile strength is 230MPa.Compared to AgSnO2, AgLa2Sn2O7Contact material shows less melting welding power.
But the deficiency that existing technology exists is: Ag/SnO2Slider material when hot extrusion silk pressing material technique due to hardness mistake The major defects such as greatly, elongation percentage is relatively low, causes a material course of processing to rupture, stripping, this external actual military service process In high contact resistance, high melting welding power occur, reduce Ag/SnO2The service life of slider material.And the present invention AgLa2Sn2O7Slider material military service effect in mechanical property and fusion welding property shows more preferably.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes Ag/SnO in prior art2The high erosion ratio of contact material is with molten The defects such as weldering, it is provided that the preparation method of a kind of new A g base stannic acid lanthanum composited contact material.The product that the method prepares Can be used in improving contact material resistance fusion welding energy, and the condition that is synthesized is simple, with low cost.
For solving technical problem, the solution of the present invention is:
The preparation method of a kind of new A g base stannic acid lanthanum composited contact material is provided, comprises the following steps:
(1)Ag-La2Sn2O7The preparation of composite granule
Ag powder and stannic acid lanthanum nano-powder being weighed according to mass ratio 88: 12, ball milling mixes 4 hours, obtains AgLa2Sn2O7Composite granule;
(2) by AgLa2Sn2O7Composite granule carries out hot pressed sintering process, it is thus achieved that AgLa2Sn2O7Briquet;The most right AgLa2Sn2O7Briquet carries out hot extrusion, it is thus achieved that a diameter of 1.5~the AgLa of 3.5mm2Sn2O7Wire rod;
During hot pressed sintering, control condition is: hot pressing pressure 450MPa, mold temperature 500 DEG C;Control condition during hot extrusion For: extruding tonnage 50T, extrusion die heating-up temperature 500 DEG C.
In the present invention, also include AgLa2Sn2O7The further process of wire rod: by process and the wire drawing process of swaging, Obtain the AgLa of a diameter of 1.85~2.8mm2Sn2O7Silk material.
In the present invention, also include AgLa2Sn2O7The further process of silk material: by AgLa2Sn2O7Rivet sent into by silk material It is machined to the rivet of preliminary dimension specification, at N2The lower 400 DEG C of heating 6h of atmosphere, carry out annealing process process.
Stannic acid lanthanum nano powder system in the present invention is according to Chinese invention patent application " a kind of high-purity stannic acid lanthanum nano-powder Preparation method " step described in (application number 201410488560.6) prepares.
In the present invention, it is thus achieved that AgLa2Sn2O7After briquet, density, Vickers hardness and resistivity etc. can be carried out for it Performance test.Obtain AgLa2Sn2O7After wire rod, it is also possible to carry out using post-treatment to process, i.e. swaged place by multiple tracks Reason and wire drawing process and obtain AgLa2Sn2O7Silk material, and carry out corresponding performance test.Recycling AgLa2Sn2O7Silk material Rivet driver it is processed into the rivet of different size and carries out annealing process process, then installing to electrical endurance test machine Carry out electric life test.
Compared with prior art, the beneficial effects of the present invention is:
(1)AgLa2Sn2O7The synthesis technique of composite granule is simplified.Mix compared to the most conventional high-energy ball milling+machinery For closing technique, this experiment only can be achieved with AgLa only with ball-milling technology (Ball-milling Time is short, it is only necessary to 4h)2Sn2O7 The synthesis of composite granule, cost is less expensive.
(2)AgLa2Sn2O7The excellent in mechanical performance of silk material.Compared to AgSnO2For, AgLa2Sn2O7Silk material table Reveal lower resistivity, higher annealed state elongation after fracture and preferably tensile strength.
(3)AgLa2Sn2O7The anti-fusion welding property of silk material is excellent.Compared to AgSnO2For, AgLa2Sn2O7Performance Go out more preferable anti-fusion welding property.
Detailed description of the invention
Below by detailed description of the invention, the 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 to deionized water, with magnetic agitation to being completely dissolved, then moves liquid to fixed in volumetric flask Hold, be configured to the colourless transparent solution that concentration is 0.03~0.6mol/L, i.e. precursor solution A;
(2) preparation of precursor solution B
Lanthanum (III) nitrate and stannic chloride pentahydrate that mol ratio is 1: 1 are added to deionized water, with magnetic agitation to completely Dissolve, then move liquid to constant volume in volumetric flask, be configured to total concentration be 0.2~1.5mol/L (be two kinds of solutes add up to dense Degree) colourless transparent solution, 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;It is subsequently adding Polyvinyl alcohol (PVA) and citric acid gellant, uniform with magnetic agitation;Polyvinyl alcohol (PVA) in mixed solution It is respectively 1~5wt% and 2~10wt% with the mass concentration of citric acid gellant;
To the ammonia spirit that mixed solution and dripping concentration is 25%~28%, regulate pH to 7~9, and continue at room temperature Stirring 2h;The most at room temperature settle 24h, remove supernatant, obtain powder body 80 DEG C of drying;
Powder body after drying is ground, and crosses after 200 mesh sieves, sinters 2h~5h at 900~1100 DEG C, final obtain in Milky stannic acid lanthanum nano-powder.
Two, the preparation of Ag base stannic acid lanthanum composited contact material
(1)Ag-La2Sn2O7The preparation of composite granule
Ag powder and stannic acid lanthanum nano-powder being weighed according to mass ratio 88:12, ball milling mixes 4 hours, obtains AgLa2Sn2O7Composite granule;
(2) by AgLa2Sn2O7Composite granule carries out hot pressed sintering process, it is thus achieved that AgLa2Sn2O7Briquet;The most right AgLa2Sn2O7Briquet carries out hot extrusion, it is thus achieved that average diameter is the AgLa of 1.5~3.5mm2Sn2O7Wire rod;
During hot pressed sintering, control condition is: hot pressing pressure 500MPa, mold temperature 500 DEG C;Control condition during hot extrusion For: extruding tonnage 50T, extrusion die heating-up temperature 500 DEG C.
(3) to AgLa2Sn2O7Wire rod carry out multiple tracks swage process and wire drawing process, obtain a diameter of 1.85~2.8mm AgLa2Sn2O7Silk material.
(4) by AgLa2Sn2O7Silk material is sent into rivet driver and is processed into the rivet of predetermined dimension, at N2Lower 400 DEG C of atmosphere Heating 6h, carries out annealing process process.
AgLa by preparation2Sn2O7Rivet is installed and is carried out electric life test to electrical endurance test machine, and test number (TN) is 20k time.Result of the test shows AgLa2Sn2O7Show the most anti-fusion welding property.
AgSnO compared to prior art2Material, AgLa in the present invention2Sn2O7Material is at mechanical property and fusion welding property The advantage of aspect is as shown in table 1 below.
AgLa in table 1 present invention2Sn2O7Material and the AgSnO of prior art2Diversity between material

Claims (3)

1. the preparation method of new A g base stannic acid lanthanum composited contact material, it is characterised in that comprise the following steps:
(1)Ag-La2Sn2O7The preparation of composite granule
Ag powder and stannic acid lanthanum nano-powder being weighed according to mass ratio 88: 12, ball milling mixes 4 hours, obtains AgLa2Sn2O7Composite granule;
(2) by AgLa2Sn2O7Composite granule carries out hot pressed sintering process, it is thus achieved that AgLa2Sn2O7Briquet;The most right AgLa2Sn2O7Briquet carries out hot extrusion, it is thus achieved that a diameter of 1.5~the AgLa of 3.5mm2Sn2O7Wire rod;
During hot pressed sintering, control condition is: hot pressing pressure 450MPa, mold temperature 500 DEG C;Control condition during hot extrusion For: extruding tonnage 50T, extrusion die heating-up temperature 500 DEG C.
Method the most according to claim 1, it is characterised in that also include AgLa2Sn2O7Wire rod further Process: by process and the wire drawing process of swaging, obtain the AgLa of a diameter of 1.85~2.8mm2Sn2O7Silk material.
Method the most according to claim 2, it is characterised in that also include AgLa2Sn2O7Silk material further Process: by AgLa2Sn2O7Silk material is sent into rivet driver and is processed into the rivet of predetermined dimension, at N2Lower 400 DEG C of atmosphere adds Hot 6h, carries out annealing process process.
CN201510222665.1A 2015-05-04 2015-05-04 Preparation method of novel Ag-based lanthanum stannate composite electric contact material Active CN104894421B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510222665.1A CN104894421B (en) 2015-05-04 2015-05-04 Preparation method of novel Ag-based lanthanum stannate composite electric contact material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510222665.1A CN104894421B (en) 2015-05-04 2015-05-04 Preparation method of novel Ag-based lanthanum stannate composite electric contact material

Publications (2)

Publication Number Publication Date
CN104894421A CN104894421A (en) 2015-09-09
CN104894421B true CN104894421B (en) 2017-01-11

Family

ID=54027371

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510222665.1A Active CN104894421B (en) 2015-05-04 2015-05-04 Preparation method of novel Ag-based lanthanum stannate composite electric contact material

Country Status (1)

Country Link
CN (1) CN104894421B (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
CN106636723B (en) * 2016-12-30 2018-04-20 衢州学院 One kind is with La1‑xSrxInO3Microballoon is the Ag base electrical contact material preparation methods of enhancing phase
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
CN107574333B (en) * 2017-08-10 2019-05-21 浙江大学 A kind of preparation method of Ag-YAG contact 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
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

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5855546A (en) * 1981-09-28 1983-04-01 Fuji Electric Co Ltd Electric contact material
CN1252757C (en) * 2004-07-02 2006-04-19 天津大学 Method for preparing submicron silver-tin dioxide electrical contact material
JP5071840B2 (en) * 2005-10-26 2012-11-14 三井金属鉱業株式会社 Exhaust gas purification catalyst
CN101407868B (en) * 2008-10-09 2011-06-22 西安工程大学 Preparation of copper-based surface nano composite AgSnO2 electrical contact alloy
CN101608279B (en) * 2009-07-20 2012-10-03 温州宏丰电工合金股份有限公司 Silver oxide electrical contact material and preparation method thereof
CN102618773B (en) * 2012-04-05 2013-06-19 浙江大学 Method for preparing Ag/La1-xSrxCoO3 electric contact composite material
CN103276235B (en) * 2013-06-25 2015-04-29 西安工程大学 Method for preparing superfine AgSnO2 doped electrical contact material by high energy ball milling method

Also Published As

Publication number Publication date
CN104894421A (en) 2015-09-09

Similar Documents

Publication Publication Date Title
CN104894421B (en) Preparation method of novel Ag-based lanthanum stannate composite electric contact material
CN107794389B (en) Silver tin oxide indium oxide electric contact material and preparation method thereof
CN102176336B (en) Preparation method of silver-based oxide electrical contact material with filamentary structure
CN112126838B (en) Copper-tungsten alloy material and preparation method and application thereof
CN106498209A (en) A kind of preparation method of doped graphene tungsten-copper alloy
CN106636776A (en) Rare earth graphene aluminum alloy type conductive wire material and preparation method thereof
CN101127253B (en) Silver nickel electricity-conductive ceramic electrical contact material and its production method
CN104505287B (en) A kind of Ag-based electrical contact material preparation method of bar-shaped tin oxide reinforcing
US7754280B2 (en) Silver/carbon-based material and method for producing the same for contact material
CN102737863B (en) Silver nickel graphite composite contact terminal material and processing method thereof
CN104480335B (en) A kind of preparation method of silver tungsten contact material
CN105895418A (en) Preparation method of silver based electric contact material
CN103794391B (en) A kind for the treatment of process strengthening Ag matrix phase in AgNi composite material and Ni wild phase wetability
CN105695792B (en) A kind of preparation method of graphene/silver nickel electric contact material
CN102864325A (en) Multielement rare earth silver electric contact as well as preparation method and application thereof
CN101794636B (en) Preparation method of silver ferric oxide electrical contact material
CN1323179C (en) High-strength, High-conductivity copper-base alloy material and preparing method thereof
CN101982558B (en) Grain refinement technology of silver-nickel electrical contact material and grain refinement technology of silver tin oxide electrical contact material
CN102044347A (en) Preparation method and products of silver-copper-nickel-ceramic alloy contact material with high welding resistance
CN105551861B (en) A kind of preparation method of graphene enhancing Ag-based electrical contact material
CN107695360B (en) The preparation method of the modified silver-colored stannic acid lanthanum electric contact composite material of graphene
CN103667767A (en) Preparation method of silver-nickel contact material containing additives capable of enhancing substrate performance and product prepared with method
CN115667169A (en) Preparation method of glass powder, silver paste and preparation method
CN101736178B (en) Manufacturing method of alloy material mixing silver with rare soil for electrical contact
CN1100886C (en) Silver heavy rake earth metal oxide electric contact material and its preparation process

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20150909

Assignee: Wenzhou Hongfeng Electrical Alloy Co., Ltd.

Assignor: Zhejiang University

Contract record no.: 2018330000029

Denomination of invention: Preparation method of novel Ag-based lanthanum stannate composite electric contact material

Granted publication date: 20170111

License type: Common License

Record date: 20180328