CN109500391A - A kind of preparation method of high ductility silver zinc oxide contact material - Google Patents

A kind of preparation method of high ductility silver zinc oxide contact material Download PDF

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Publication number
CN109500391A
CN109500391A CN201910009803.6A CN201910009803A CN109500391A CN 109500391 A CN109500391 A CN 109500391A CN 201910009803 A CN201910009803 A CN 201910009803A CN 109500391 A CN109500391 A CN 109500391A
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zno
silver
powder
preparation
zinc
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李波
黄锡文
陈光明
蒋义斌
肖光
李耀林
蒙建洲
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Guilin Electrical Equipment Scientific Research Institute Co Ltd
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Guilin Electrical Equipment Scientific Research Institute Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/048Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00Treatment under specific atmosphere
    • B22F2201/10Inert gases
    • B22F2201/11Argon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of preparation methods of high ductility silver zinc oxide contact material, the following steps are included: 1) material mixture ratio of the Ag-ZnO contact prepared as needed, the silver, zinc and additive of phase the application amount powder by atomization after melting are calculated and weighed, silver-colored zinc alloyed powder is obtained;2) silver-colored zinc alloyed powder is subjected to wet-milling under the conditions of protective atmosphere, the silver-colored zinc alloyed powder after obtaining ball milling;3) the silver-colored zinc alloyed powder after ball milling is aoxidized, obtains Ag-ZnO composite powder;4) Ag-ZnO composite powder is formed, obtains Ag-ZnO green body;5) gained Ag-ZnO green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is sintered under conditions of being 900~960 DEG C, obtains the Ag-ZnO ingot blank of high ductility;6) gained Ag-ZnO ingot blank obtains Ag-ZnO wire rod or band through hot extrusion.Silver zinc oxide contact material even tissue made from the method for the invention and high ductility of tool, the processing performance of material are effectively promoted.

Description

A kind of preparation method of high ductility silver zinc oxide contact material
Technical field
The present invention relates to the preparation methods of Ag-ZnO contact, and in particular to a kind of high ductility silver zinc oxide contact material Preparation method.
Background technique
Electrical contact is the core component of various high-low switch, electric appliance, instrument and meter, component, is widely used in space flight, boat The industrial circles such as sky, automobile and the large capacity AC/DC contactor of civilian industry, alternating current-direct current power relay, car electrics and in In small-capacity low-pressure breaker.Electrical contact is many kinds of, and there are commonly silver-base alloy and acid bronze alloy.In silver-base alloy, silver Cadmium oxide contact material has good resistance to arc wear, resistance fusion welding, electric conductivity and thermal conductivity, and contact resistance is small, steady Qualitative height, referred to as " omnipotent slider material ".But since silver cadmium oxide material all exists in production and application and removal process The harm of " cadmium poison ", therefore develop and develop popular class of the material of novel environment friendly and excellent electric contact performance as the field Topic.
Ag-ZnO (AgZnO) contact material has excellent interrupting performance, resistance fusion welding and resistance to arc erosion, and nontoxic Environmental protection is one of the contact material for substituting Agcdo.The preparation method of silver zinc oxide contact material is roughly divided into powder metallurgy Method, internal oxidation, chemical coprecipitation and atomization.These methods respectively have deficiency: density of material made of powder metallurgic method is low, Contact resistance is big, Wen Shenggao;The material surface and internal structure of internal oxidation preparation are uneven, and oxide particle aggregation is serious, There is poor oxide layer in centre;Chemical coprecipitation technique is more complex, and the problems such as can generate chemical contamination in preparation process.And it is atomized Method technique has merged the advantages of powder metallurgic method and internal oxidation, is suitble to produce in enormous quantities, have a good application prospect, but mist Change method also brings some shortcomings while improving Ag-ZnO production efficiency, is such as sintered difficulty, and poor processability etc. is asked Topic.
The traditional process flow of atomization is substantially are as follows: melting, powder by atomization, alloy powder oxidation, isostatic pressing, burning Knot, hot extrusion, drawing, are eventually fabricated finished product.Wherein in alloy powder oxidation stage since the thermodynamic stability of ZnO is higher than Ag2O, therefore the oxidation of Zn is prior to the oxidation of Ag.In powder particle surface segregation occurs for ZnO, hinders in the subsequent sintering process The contact and diffusion of Ag between powder, leads to that blank sintering is difficult, poor processability.Such as Publication No. CN101202168 Patent of invention, a kind of technique for preparation of novel silver zinc oxide contact material is disclosed, specifically by silver, zinc, additive by certain Ratio is melted into silver-colored zinc alloy powder by fusing, water mist in mid-frequency melting furnace, is then dried, is aoxidized to atomized alloy powder Modifier treatment, etc. static pressure, sintering, extruding, wire drawing etc. be processed into silver zinc oxide electrical contact.As previously described, because ZnO under normal pressure Thermodynamic stability is higher than Ag2O, therefore oxidation of the oxidation prior to Ag of Zn is certainly existed, so as to cause ZnO in powder particle Segregation occurs for surface, and in the subsequent sintering process between obstruction powder the problem of the contact and diffusion of Ag, therefore same in the invention There are blank sintering difficulties, the deficiency of poor processability for sample.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation methods of high ductility silver zinc oxide contact material.The party Method first to wet-milling under the conditions of atmosphere protection of silver-colored zinc alloyed powder, is aoxidized later, is formed, then by molding Ag-ZnO green body It is placed under specific oxygen pressure, ultra-high temperature condition and is sintered, to obtain the Ag-ZnO ingot blank of even tissue and high ductility, improve silver-colored oxygen Change the processing performance of Zinc material.
In order to solve the above technical problems, the preparation method of high ductility silver zinc oxide contact material provided by the invention, including Following steps:
1) material mixture ratio of the Ag-ZnO contact prepared as needed, the dosage of silver needed for calculating, zinc and additive, claims The silver, zinc and additive of phase the application amount powder by atomization after melting are taken, silver-colored zinc alloyed powder is obtained;
2) silver-colored zinc alloyed powder is placed in ball mill, wet-milling is carried out under the conditions of protective atmosphere, to gained after the completion of wet-milling Powder is dried, the silver-colored zinc alloyed powder after obtaining ball milling;
3) the silver-colored zinc alloyed powder after ball milling is aoxidized, obtains Ag-ZnO composite powder;
4) Ag-ZnO composite powder is formed, obtains Ag-ZnO green body;
5) gained Ag-ZnO green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is sintered under conditions of being 900~960 DEG C, obtains To the Ag-ZnO ingot blank of high ductility;
6) gained Ag-ZnO ingot blank obtains Ag-ZnO wire rod or Ag-ZnO band through hot extrusion.
In the step 1) of above-mentioned preparation method, in resulting silver-colored zinc alloyed powder, by mass percentage, shared by additive Ratio be 0~2%, ratio shared by zinc is 1~20%, and surplus is silver.The selection of the additive is same as the prior art, It specifically can be the combination selected from one or more of Cu, Bi, Ni, Sb and Te.In the step, stock silver used, Zinc and additive can be the form of pure metal spindle, be also possible to the form of pure metal powder, if Ag can be pure Ag block, It can be pure Ag powder.
In the step 2) of above-mentioned preparation method, usually require that wet-milling to partial size≤5 μm of gained powder, preferably requires wet-milling To partial size≤2 μm of gained powder, further preferred wet-milling to partial size≤1 μm of gained powder.Ball-milling medium in wet-milling, When Ball-milling Time etc. is the same as those in the prior art ball material quality, it is preferred that ball material mass ratio is 3~10:1, and ball-milling medium is The mass ratio of dehydrated alcohol, medium and material is 0.5~2:1, and rotational speed of ball-mill is 250~500rmp, and Ball-milling Time is 6~15h.Institute The protective atmosphere stated is usually N2Or inert gas (such as Ar).The drying of gained powder is usually 80~100 after the completion of wet-milling DEG C condition carries out, and the time is usually 6~10h.
In the step 3) of above-mentioned preparation method, operation when oxidation is same as the prior art, specifically by the silver after ball milling Zinc alloy powder is placed in high-pressure oxidation furnace, and 4~8h is aoxidized under the conditions of partial pressure of oxygen is 0.5~2MPa, temperature is 600~800 DEG C. Resulting material obtains Ag-ZnO composite powder after crushing after oxidation.
In the step 4) of above-mentioned preparation method, existing conventional techniques is used to form to obtain Ag-ZnO composite powder Ag-ZnO composite powder is usually placed on isostatic pressing machine and forms by Ag-ZnO green body, control isostatic pressure be 50~ 200MPa, dwell time are 10s~200s,
In the step 5) of above-mentioned preparation method, the time of sintering is normally controlled in 4~10h.In order to further increase gained The processing performance of ingot blank, more preferably sintering carry out under conditions of partial pressure of oxygen is 1~2Mpa, temperature is 950~960 DEG C, at this time The time of sintering is preferably controlled in 6~8h.
In the step 6) of above-mentioned preparation method, the operation of the hot extrusion is same as the prior art, specifically, hot extrusion Temperature is 830~900 DEG C, and extrusion ratio is 190~270.After obtaining Ag-ZnO wire rod or Ag-ZnO band, by existing Required Ag-ZnO contact is made in common process.As wire rod or band are carried out multiple drawing (or Rolling compund), annealing again It is machined to required size, then again with rivet machining (or punching machine punching press) at rivet type (or sheet) contact.
Compared with prior art, present invention is characterized in that
1, molding Ag-ZnO green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is burnt under conditions of being 900~960 DEG C Knot, be especially sintered under conditions of partial pressure of oxygen is 1~2Mpa, temperature is 950~960 DEG C, using silver point with The increase of pressure and the characteristics of increase so that in technical solution of the present invention (at normal atmospheric pressure, silver point is greater than 962 DEG C Silver point be 962 DEG C), therefore ingot blank be not in during super high sintering temperature melting phenomenon (at normal atmospheric pressure, when The sintering temperature of Ag-ZnO ingot blank will appear melting phenomenon when reaching 960 DEG C, or even just will appear melting at 950 DEG C or more Phenomenon);On the other hand, it is sintered under the conditions of superhigh-temperature and-pressure, moreover it is possible to enhance the mutual sintering diffusion between Ag-ZnO particle It acts on, (according to conventional sintering theory, sintering temperature is sintered closer to the fusing point of substance for the formation of sintering neck between promotion particle The substance arrived has more superior sintering character), to improve the processing performance of material, and then the Ag-ZnO ingot of high ductility Base.
2, silver-colored zinc alloy powder obtained will be atomized and is placed in ball mill the progress high energy wet-milling under the conditions of atmosphere protection, Particle size will not both generate caking phenomenon while obtaining refining broken, and powder particle surface problem of oxidation will not occur, And particle can generate a large amount of micro-crack during wet-milling, increase the diffusion admittance of oxygen for subsequent oxidation process, so that Oxygen atom of the grain in subsequent high-voltage high-speed oxidation process is greater than zinc atom out of particle to the diffusion rate inside powder particle Portion reduces zinc oxide in the enrichment of particle surface, improves the uniformity of material structure toward the diffusion rate on boundary.
3, the method for the invention is simple and easy to control, is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the picture of step 5) sintering gained Ag-ZnO ingot blank material object in the embodiment of the present invention 1;
Fig. 2 is the picture of step 5) sintering gained Ag-ZnO ingot blank material object in comparative example 1 of the present invention;
Fig. 3 is the picture of step 5) sintering gained Ag-ZnO ingot blank material object in comparative example 2 of the present invention;
Fig. 4 is the resulting Ag-ZnO ingot blank of 1 step 5) of the embodiment of the present invention and the resulting silver oxidation of 2 step 5) of comparative example Zinc ingot metal base carries out appearance analysis and Metallographic Analysis respectively;Wherein, (a) is the resulting Ag-ZnO ingot of 2 step 5) of comparative example The fracture apperance of base is (b) metallographic structure of the resulting Ag-ZnO ingot blank of 2 step 5) of comparative example, (c) is 1 step of embodiment 5) fracture apperance of resulting Ag-ZnO ingot blank is (d) the metallographic group of the resulting Ag-ZnO ingot blank of 1 step 5) of embodiment It knits.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below, content to better understand the invention, but The present invention is not limited to following embodiments.
Embodiment 1
1) each component is weighed by following mass percents, is placed in medium frequency induction melting furnace that be smelted into uniform alloy molten Then liquid is atomized through hydraulic atomized equipment, obtained powder slurries are dried, and is crossed 200 meshes, is arrived very much silver-colored zinc alloy Powder;
Zn:9.5%;
Additive: Bi 0.27%, Cu 0.33%, Ni 0.15%;
Surplus is Ag;
2) silver-colored zinc alloyed powder is placed in high energy ball mill, wet ground is carried out under atmosphere (Ar) protection, until gained The partial size of powder is 1~5 μm, the powder after wet-milling is placed in baking oven under the conditions of 80 DEG C dry 10h, the silver after obtaining ball milling Zinc alloy powder;In wet-milling, ball material mass ratio is 3:1, and ball-milling medium is dehydrated alcohol, and the mass ratio of medium and material is 0.5:1, Rotational speed of ball-mill is 500rmp, Ball-milling Time 15h;
3) the silver-colored zinc alloyed powder after ball milling is placed in high-pressure oxidation furnace, partial pressure of oxygen is 2MPa, temperature is 600 DEG C of conditions Lower oxidation 8h takes out, is crushed, sieves with 100 mesh sieve, obtain Ag-ZnO composite powder;
4) Ag-ZnO composite powder is placed on isostatic pressing machine and is formed, control isostatic pressure is 50MPa, and the dwell time is 200s obtains Ag-ZnO green body;
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, is burnt under the conditions of partial pressure of oxygen is 0.8MPa, temperature is 960 DEG C 6h is tied, obtains Ag-ZnO ingot blank, material object is as shown in Figure 1, as seen from the figure, being sintered resulting Ag-ZnO surface of ingot blank has had Metallic luster illustrates that blank sintering densification effect is fine;
6) wire rod is processed into Ag-ZnO ingot blank hot extrusion, wire rod is used after multiple drawing and annealing to the size needed Rivet is machined to rivet type contact.
Comparative example 1
Embodiment 1 is repeated, unlike:
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, 960 DEG C of sintering 6h is warming up under standard atmosphere condition. As a result: silver-based has melted in gained ingot blank (since 1 normal atmosphere pressure silver point is 961 DEG C, is sintered at 960 DEG C Billet is certain to melt, and then can not obtain qualified Ag-ZnO ingot blank), gained ingot blank is in kind as shown in Figure 2.Namely It says, this example does not obtain the qualified Ag-ZnO ingot blank for subsequent handling.
Comparative example 2
Embodiment 1 is repeated, unlike:
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, 930 DEG C of sintering 6h is warming up under standard atmosphere condition. As a result: obtain Ag-ZnO ingot blank, it is in kind as shown in figure 3, but gained surface of ingot blank is still dark gray, illustrate at 930 DEG C It is very undesirable that blank sintering densifies effect.
Embodiment 2
1) each component is weighed by following mass percents, is placed in medium frequency induction melting furnace that be smelted into uniform alloy molten Then liquid is atomized through hydraulic atomized equipment, obtained powder slurries are dried, and is crossed 200 meshes, is arrived very much silver-colored zinc alloy Powder;
Zn:8%;
Additive: Cu 0.3%, Ni 0.2%;
Surplus is Ag;
2) silver-colored zinc alloyed powder is placed in high energy ball mill, wet ground is carried out under atmosphere (Ar) protection, until gained The partial size of powder is 1~2 μm, the powder after wet-milling is placed in baking oven under the conditions of 100 DEG C dry 6h, the silver after obtaining ball milling Zinc alloy powder;In wet-milling, ball material mass ratio is 10:1, and ball-milling medium is dehydrated alcohol, and the mass ratio of medium and material is 2:1, Rotational speed of ball-mill is 250rmp, Ball-milling Time 6h;
3) the silver-colored zinc alloyed powder after ball milling is placed in high-pressure oxidation furnace, partial pressure of oxygen is 0.5MPa, temperature is 800 DEG C of items 4h is aoxidized under part, is taken out, is crushed, sieves with 100 mesh sieve, obtain Ag-ZnO composite powder;
4) Ag-ZnO composite powder is placed on isostatic pressing machine and is formed, control isostatic pressure is 100MPa, and the dwell time is 10s obtains Ag-ZnO green body;
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, is sintered under the conditions of partial pressure of oxygen is 2MPa, temperature is 960 DEG C 6h obtains Ag-ZnO ingot blank;
6) plate is processed into Ag-ZnO ingot blank hot extrusion, plate is used after repeatedly being rolled, being annealed to the sizes of needs Punching machine is processed into blade contact.
Embodiment 3
1) each component is weighed by following mass percents, is placed in medium frequency induction melting furnace that be smelted into uniform alloy molten Then liquid is atomized through hydraulic atomized equipment, obtained powder slurries are dried, and is crossed 200 meshes, is arrived very much silver-colored zinc alloy Powder;
Sn:10%;
Additive: Te 1%;
Surplus is Ag;
2) silver-colored zinc alloyed powder is placed in high energy ball mill, wet ground is carried out under atmosphere (Ar) protection, until gained The partial size of powder is 3~5 μm, the powder after wet-milling is placed in baking oven under the conditions of 90 DEG C dry 9h, the silver after obtaining ball milling Zinc alloy powder;In wet-milling, ball material mass ratio is 5:1, and ball-milling medium is dehydrated alcohol, and the mass ratio of medium and material is 1:1, ball Mill revolving speed is 400rmp, Ball-milling Time 10h;
3) the silver-colored zinc alloyed powder after ball milling is placed in high-pressure oxidation furnace, partial pressure of oxygen is 1MPa, temperature is 700 DEG C of conditions Lower oxidation 7h takes out, is crushed, sieves with 100 mesh sieve, obtain Ag-ZnO composite powder;
4) Ag-ZnO composite powder is placed on isostatic pressing machine and is formed, control isostatic pressure is 80MPa, and the dwell time is 100s obtains Ag-ZnO green body;
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, is sintered under the conditions of partial pressure of oxygen is 1MPa, temperature is 960 DEG C 4h obtains Ag-ZnO ingot blank;
6) wire rod is processed into Ag-ZnO ingot blank hot extrusion, wire rod is used after multiple drawing and annealing to the size needed Rivet is machined to rivet type contact.
Embodiment 4
1) each component is weighed by following mass percents, is placed in medium frequency induction melting furnace that be smelted into uniform alloy molten Then liquid is atomized through hydraulic atomized equipment, obtained powder slurries are dried, and is crossed 200 meshes, is arrived very much silver-colored zinc alloy Powder;
Sn:12%;
Additive: 0%;
Surplus is Ag;
Step 2), 3), 4) with embodiment 3;
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, is sintered under the conditions of partial pressure of oxygen is 1MPa, temperature is 900 DEG C 10h obtains Ag-ZnO ingot blank;
6) wire rod is processed into Ag-ZnO ingot blank hot extrusion, wire rod is used after multiple drawing and annealing to the size needed Rivet is machined to rivet type contact.
Ag-ZnO ingot blank made from Ag-ZnO ingot blank made from step 5) to Examples 1 to 4 and comparative example 2 respectively The performances such as bending strength be measured, as a result as described in Table 1:
Table 1:
To the resulting Ag-ZnO ingot blank of 1 step 5) of embodiment and the resulting Ag-ZnO ingot blank of 2 step 5) of comparative example point Not carry out appearance analysis and Metallographic Analysis, as a result as shown in figure 4, wherein (a) be 2 step 5) of comparative example it is resulting silver oxidation The fracture apperance of zinc ingot metal base is (b) metallographic structure of the resulting Ag-ZnO ingot blank of 2 step 5) of comparative example, (c) is embodiment 1 The fracture apperance of the resulting Ag-ZnO ingot blank of step 5) is (d) metallographic of the resulting Ag-ZnO ingot blank of 1 step 5) of embodiment Tissue.As shown in Figure 4, the resulting Ag-ZnO ingot blank of 2 step 5) of comparative example, powder are broken almost without being sintered together Be entirely it is brittle come along powder particle boundary separation, fracture surface remains the feature of starting powder particle, and Grain surface is dispersed with a large amount of ZnO particle, and to bulky grain crystal grain (or particle), internal constituent analysis shows internal Zn content Extremely low, the overwhelming majority has been enriched to powder particle surface.Powder in the resulting Ag-ZnO ingot blank of 1 step 5) of embodiment is Fully sintered to form fine and close tissue together, the fracture of blank shows as the ductile fracture feature with a large amount of dimples, breaks Original powder particle almost can not be offered an explanation on face.ZnO particle is not distributed only on crystal boundary, and also a large amount of in the inside of crystal grain Distribution, this improves the distribution of second phase particles significantly, is beneficial to material processing performance, plasticity and electrical property It improves.

Claims (7)

1. a kind of preparation method of high ductility silver zinc oxide contact material, comprising the following steps:
1) material mixture ratio of the Ag-ZnO contact prepared as needed, the dosage of silver needed for calculating, zinc and additive, weighs phase Silver, zinc and the additive of application amount powder by atomization after melting, obtain silver-colored zinc alloyed powder;
2) silver-colored zinc alloyed powder is placed in ball mill, wet-milling is carried out under the conditions of protective atmosphere, to gained powder after the completion of wet-milling It is dried, the silver-colored zinc alloyed powder after obtaining ball milling;
3) the silver-colored zinc alloyed powder after ball milling is aoxidized, obtains Ag-ZnO composite powder;
4) Ag-ZnO composite powder is formed, obtains Ag-ZnO green body;
5) gained Ag-ZnO green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is sintered under conditions of being 900~960 DEG C, obtains height The Ag-ZnO ingot blank of ductility;
6) gained Ag-ZnO ingot blank obtains Ag-ZnO wire rod or Ag-ZnO band through hot extrusion.
2. preparation method according to claim 1, it is characterised in that: in step 1), in resulting silver-colored zinc alloyed powder, press Mass percent meter, ratio shared by additive are 0~2%, and ratio shared by zinc is 1~20%, and surplus is silver.
3. preparation method according to claim 1, it is characterised in that: in step 1), the additive be selected from Cu, The combination of one or more of Bi, Ni, Sb and Te.
4. preparation method according to claim 1, it is characterised in that: in step 2), wet-milling to partial size≤5 of gained powder μm。
5. preparation method according to any one of claims 1 to 4, it is characterised in that: in step 5), the time of sintering is 4 ~10h.
6. preparation method according to claim 5, it is characterised in that: in step 5), sintering partial pressure of oxygen be 1~2Mpa, Temperature carries out under conditions of being 950~960 DEG C.
7. preparation method according to claim 6, it is characterised in that: in step 5), the time of sintering is 6~8h.
CN201910009803.6A 2019-01-05 2019-01-05 A kind of preparation method of high ductility silver zinc oxide contact material Pending CN109500391A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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CN110465671A (en) * 2019-08-08 2019-11-19 湖南诺尔得材料科技有限公司 A kind of preparation method of flake silver powder
CN112095057A (en) * 2020-08-08 2020-12-18 福达合金材料股份有限公司 Nano silver wire modified silver-nickel electric contact material and preparation method thereof
CN114182222A (en) * 2021-11-03 2022-03-15 梭莱镀膜工业(江阴)有限公司 Preparation process of conductive metal oxide target
CN115740465A (en) * 2022-12-13 2023-03-07 温州中希电工合金有限公司 Silver tin oxide contact material and preparation method thereof

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CN110465671A (en) * 2019-08-08 2019-11-19 湖南诺尔得材料科技有限公司 A kind of preparation method of flake silver powder
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CN112095057A (en) * 2020-08-08 2020-12-18 福达合金材料股份有限公司 Nano silver wire modified silver-nickel electric contact material and preparation method thereof
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CN115740465A (en) * 2022-12-13 2023-03-07 温州中希电工合金有限公司 Silver tin oxide contact material and preparation method thereof
CN115740465B (en) * 2022-12-13 2023-08-18 温州中希电工合金有限公司 Silver tin oxide contact material and preparation method thereof

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