CN109593981A - A kind of preparation method for the sliver oxidized tin contactor materials improving ingot blank agglutinating property - Google Patents

A kind of preparation method for the sliver oxidized tin contactor materials improving ingot blank agglutinating property Download PDF

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CN109593981A
CN109593981A CN201811590827.7A CN201811590827A CN109593981A CN 109593981 A CN109593981 A CN 109593981A CN 201811590827 A CN201811590827 A CN 201811590827A CN 109593981 A CN109593981 A CN 109593981A
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tin oxide
powder
siller
siller tin
silver
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CN109593981B (en
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李波
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Guilin Jinge Electrotechnical Electronic Material Science & Technology Co Ltd
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Guilin Jinge Electrotechnical Electronic Material Science & Technology Co Ltd
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    • 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
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • C22C1/053Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
    • C22C1/056Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using gas
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/12Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • H01H1/023Composite material having a noble metal as the basic material
    • H01H1/0237Composite material having a noble metal as the basic material and containing oxides
    • H01H1/02372Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te
    • H01H1/02376Composite material having a noble metal as the basic material and containing oxides containing as major components one or more oxides of the following elements only: Cd, Sn, Zn, In, Bi, Sb or Te containing as major component SnO2

Abstract

The invention discloses a kind of preparation methods of sliver oxidized tin contactor materials for improving ingot blank agglutinating property, the following steps are included: 1) material mixture ratio of the siller tin oxide contact prepared as needed, the silver, tin and additive of phase the application amount powder by atomization after melting are calculated and weighed, silver-tin alloy powder is obtained;2) silver-tin alloy powder is aoxidized, obtains siller tin oxide composite powder;3) siller tin oxide composite powder is subjected to wet-milling under the conditions of protective atmosphere, the siller tin oxide composite powder after obtaining ball milling;4) the siller tin oxide composite powder after ball milling is formed, obtains siller tin oxide green body;5) gained siller tin oxide green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is sintered under conditions of being 900~960 DEG C, obtains siller tin oxide ingot blank;6) gained siller tin oxide ingot blank obtains AgSnO2 wire or band through hot extrusion.Sliver oxidized tin contactor materials even tissue made from the method for the invention and processing performance is good.

Description

A kind of preparation method for the sliver oxidized tin contactor materials improving ingot blank agglutinating property
Technical field
The present invention relates to the preparation methods of siller tin oxide contact, and in particular to a kind of siller tin oxide for improving ingot blank agglutinating property The preparation method of contact material.
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.
Siller tin oxide (AgSnO2) due to good anti-melting welding and arc ablation resistance performance, and asepsis environment-protecting, it is most It is hopeful to substitute the contact material of Agcdo.The preparation method of sliver oxidized tin contactor materials is roughly divided into powder metallurgic method (such as The patent of invention of Publication No. CN101202169A and CN101649399A), internal oxidation (such as Publication No. The patent of invention of CN1042010208A and CN103700544A), chemical coprecipitation is (such as Publication No. CN102528055A Patent of invention) and atomization.Wherein powder metallurgic method and internal oxidation are the mainstream preparation methods of sliver oxidized tin contactor materials.But These methods respectively have deficiency: density of material made of powder metallurgic method is low, contact resistance is big, Wen Shenggao;Internal oxidation preparation Material surface and internal structure are uneven, and oxide particle aggregation is serious, and there is poor oxide layer in centre;Chemical coprecipitation technique compared with Complexity, and the problems such as chemical contamination can be generated in preparation process.And atomization technique has merged powder metallurgic method and internal oxidation The advantages of, it is suitble to produce in enormous quantities, has a good application prospect, but atomization is improving the same of siller tin oxide production efficiency When also bring some shortcomings, if Powder Oxidation and sintering are difficult, the problems such as poor processability.
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 due to SnO2Thermodynamic stability it is high In Ag2O, therefore the oxidation of Sn is prior to the oxidation of Ag.SnO2Segregation occurs in powder particle surface, hinders in the subsequent sintering process The contact and diffusion for having hindered Ag between powder, lead to that blank sintering is difficult, poor processability.
Through retrieving to the prior art, the patent of invention of Publication No. CN101707153A discloses a kind of fine grained oxygen Change the preparation method of tin enhancing Ag-based electrical contact material.AgSn alloyed powder and additive sieving are placed on high energy first by this method Ball milling is carried out in the case where oxygen calms the anger atmosphere in ball mill, is carried out so that the pre-oxidation of AgSn alloy powder is synchronous with ball milling dispersion process, so The powder after ball milling is subjected to annealing afterwards and isostatic pressing, the green body of acquisition are sintered under oxygen atmosphere, will finally be burnt Green body after knot carries out hot pressing, resintering and hot extrusion, obtains band or wire rod.The invention points out, by by mechanical alloying with High normal pressure and temperature method for pre-oxidizing combines, so that constantly there is fresh AgSn alloyed powder surface sudden and violent in ma process Dew, so that AgSn alloyed powder is promoted constantly to combine with oxygen, the realization of accelerated oxidation process under huge high energy impact;And So that the SnO that oxidation obtains2Particle Dispersed precipitate in Ag matrix.But it is well known to those skilled in the art, it depresses and carries out in oxygen High-energy ball milling is easy that AgSn alloyed powder and additive is made to agglomerate, to influence the uniformity of material structure.
The patent of invention of Publication No. CN101202169A discloses a kind of novel silver tin oxide silk electrical contact material system Make method.Raw material after this method matches silver, tin, additive by a certain percentage melts in mid-frequency melting furnace, passes through Hydraulic atomized equipment carries out high pressure alloy atomization, atomized alloy powder is dried and aoxidized modifier treatment, after waiting static pressure Static pressure ingot blank, the ingot blanks such as formation are sintered in heating furnace, and sintering ingot blank send extruder to squeeze out silk material, are used to silk material is squeezed Hot pull mode carries out being worked into finished product.As previously mentioned, in alloy powder oxidation stage due to SnO2Thermodynamic stability Higher than Ag2O, therefore the oxidation of Sn is prior to the oxidation of Ag, SnO2Segregation occurs in powder particle surface, in the subsequent sintering process The contact and diffusion of Ag between powder are hindered, thus the problems such as that there are blank sinterings is difficult, poor processability.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of systems of sliver oxidized tin contactor materials for improving ingot blank agglutinating property Preparation Method.This method forms the siller tin oxide composite powder after oxidation under the conditions of atmosphere protection after wet-milling, gained green body is set again It is sintered under specific oxygen pressure, ultra-high temperature condition, the agglutinating property of gained ingot blank is effectively improved, to obtain even tissue and processing The good sliver oxidized tin contactor materials of performance.
In order to solve the above technical problems, provided by the invention
Improve the preparation method of the sliver oxidized tin contactor materials of ingot blank agglutinating property, comprising the following steps:
1) material mixture ratio of the siller tin oxide contact prepared as needed, the dosage of silver needed for calculating, tin and additive, claims The silver, tin and additive of phase the application amount powder by atomization after melting are taken, silver-tin alloy powder is obtained;
2) silver-tin alloy powder is aoxidized, obtains siller tin oxide composite powder;
3) siller tin oxide composite powder is placed in ball mill, wet-milling is carried out under the conditions of protective atmosphere, it is right after the completion of wet-milling Gained powder is dried, the siller tin oxide composite powder after obtaining ball milling;
4) the siller tin oxide composite powder after ball milling is formed, obtains siller tin oxide green body;
5) gained siller tin oxide green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is sintered under conditions of being 900~960 DEG C, obtains To siller tin oxide ingot blank;
6) gained siller tin oxide ingot blank obtains AgSnO2 wire or siller tin oxide band through hot extrusion.
In the step 1) of above-mentioned preparation method, in resulting silver-tin alloy powder, by mass percentage, shared by additive Ratio be 0~5%, ratio shared by tin is 1~20%, and surplus is silver.Preferably, ratio shared by additive be 0.1~ 2%, ratio shared by tin is 1~20%, and surplus is silver.The selection of the additive is same as the prior art, specifically can be Combination selected from one or more of Cu, Bi, In, Ni, Zn, Sb and Te.In the step, stock silver used, tin and Additive can be the form of pure metal spindle, be also possible to the form of pure metal powder, can also be with if Ag can be pure Ag block It is pure Ag powder.
In the step 2) of above-mentioned preparation method, operation when oxidation is same as the prior art, specifically by silver-tin alloy powder It is placed in high-pressure oxidation furnace, 4~8h is aoxidized under the conditions of partial pressure of oxygen is 0.5~2MPa, temperature is 600~800 DEG C.Institute after oxidation Siller tin oxide composite powder is obtained after obtaining crushing material.
In the step 3) 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 4) of above-mentioned preparation method, using existing conventional techniques to after ball milling siller tin oxide composite powder carry out at Siller tin oxide composite powder after ball milling is usually placed on isostatic pressing machine and forms to obtain siller tin oxide green body by type, control etc. Static pressure is 50~200MPa, and the dwell time is 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 AgSnO2 wire or siller tin oxide band, by existing Required siller tin oxide 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 siller tin oxide 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 siller tin oxide 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 siller tin oxide 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 siller tin oxide ingot of high ductility Base.
2, it is placed in ball mill under the conditions of atmosphere protection and carries out again after silver-tin alloy powder initial oxidation made from being atomized The SnO in oxidation operation is smashed in high energy wet-milling2The hard shell that segregation is formed occurs in powder particle surface, makes Metal Substrate therein Constantly it is exposed, plays the role of acceleration of sintering, further increases the processing performance of ingot blank;On the other hand, particle size Caking phenomenon will not be both generated while obtaining refining broken, and powder particle surface problem of oxidation, and particle will not occur A large amount of micro-crack can be generated during wet-milling, increase the diffusion admittance of oxygen for subsequent oxidation process, so that particle is rear Oxygen atom in continuous high-voltage high-speed oxidation process is greater than tin atom inside particle toward side to the diffusion rate inside powder particle The diffusion rate on boundary reduces tin oxide in the enrichment of particle surface, improves the uniformity of material structure.
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 siller tin oxide ingot blank material object in the embodiment of the present invention 1;
Fig. 2 is the fracture apperance figure of step 5) sintering gained siller tin oxide ingot blank and metallographic structure in the embodiment of the present invention 1, Wherein (a) is fracture apperance figure, (b) is metallographic structure;
Fig. 3 is the picture of step 5) sintering gained siller tin oxide ingot blank material object in comparative example 1 of the present invention;
Fig. 4 is the picture of step 5) sintering gained siller tin oxide ingot blank material object in comparative example 2 of the present invention;
Fig. 5 is the fracture apperance figure of step 5) sintering gained siller tin oxide ingot blank and metallographic structure in comparative example 2 of the present invention, Wherein (a) is fracture apperance figure, (b) is metallographic structure;
Fig. 6 is the fracture apperance figure and metallographic group of step 5) sintering gained siller tin oxide ingot blank in the embodiment of the present invention 2 and 3 It knits, wherein (a) is the fracture apperance figure of embodiment 2, it (b) is the fracture apperance figure of embodiment 3.
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-tin alloy Powder;
Sn:9.5%;
Additive: Bi 0.1%;
Surplus is Ag;
2) silver-tin alloy powder is placed in high-pressure oxidation furnace, is aoxidized under the conditions of partial pressure of oxygen is 1MPa, temperature is 700 DEG C 6h takes out, is crushed, sieves with 100 mesh sieve, obtain siller tin oxide composite powder;
3) siller tin oxide composite powder is placed in high energy ball mill, carries out wet ground under atmosphere (Ar) protection, until The partial size of gained powder is 1~2 μm, the powder after wet-milling is placed in baking oven under the conditions of 80 DEG C dry 10h, after obtaining ball milling Siller tin oxide composite powder;In wet-milling, ball material mass ratio is 8:1, and ball-milling medium is dehydrated alcohol, the mass ratio of medium and material For 0.8:1, rotational speed of ball-mill 500rmp, Ball-milling Time 15h;
4) the siller tin oxide composite powder after ball milling is placed on isostatic pressing machine and is formed, control isostatic pressure is 50MPa, pressure maintaining Time is 200s, obtains siller tin oxide green body;
5) siller tin oxide 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 siller tin oxide ingot blank, material object is as shown in Figure 1, as seen from the figure, being sintered resulting siller tin oxide surface of ingot blank has had Metallic luster illustrates that blank sintering densification effect is fine;The fracture apperance of gained siller tin oxide ingot blank and metallographic structure difference As shown in Fig. 2 (a) and 2 (b);
6) wire rod is processed into siller tin oxide 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) siller tin oxide 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 siller tin oxide ingot blank), gained ingot blank is in kind as shown in Figure 3.Namely It says, this example does not obtain the qualified siller tin oxide ingot blank for subsequent handling.
Comparative example 2
Embodiment 1 is repeated, unlike:
5) siller tin oxide 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 siller tin oxide ingot blank, it is in kind as shown in figure 4, but gained surface of ingot blank is still dark gray, illustrate at 930 DEG C It is very undesirable that blank sintering densifies effect.The fracture apperance of gained siller tin oxide ingot blank and metallographic structure are respectively such as Fig. 5 (a) With shown in 5 (b).
Comparison diagram 5 and Fig. 2 are it is found that the resulting siller tin oxide ingot blank of 2 step 5) of comparative example, powder exist almost without sintering Together, fracture be entirely it is brittle come along powder particle boundary separation, fracture surface remains the spy of starting powder particle Sign, and particle surface is dispersed with a large amount of SnO2Particle, to bulky grain crystal grain (or particle), internal constituent analysis shows interior The Theil indices in portion are extremely low, and the overwhelming majority has been enriched to powder particle surface.In the resulting siller tin oxide ingot blank of 1 step 5) of embodiment Powder it is fully sintered together, form fine and close tissue, the fracture of blank shows as the plasticity with a large amount of dimples Fracture characteristic almost can not offer an explanation original powder particle on section.SnO2Particle is not distributed only on crystal boundary, and in crystal grain Inside be also largely distributed, this improves the distribution of second phase particles significantly, is beneficial to material processing performance, plasticity And the raising of electrical property.
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-tin alloy Powder;
Sn:8%;
Additive: In 1%, Cu 1%, Ni 1%;
Surplus is Ag;
2) silver-tin alloy powder is placed in high-pressure oxidation furnace, is aoxidized under the conditions of partial pressure of oxygen is 2MPa, temperature is 800 DEG C 4h takes out, is crushed, sieves with 100 mesh sieve, obtain siller tin oxide composite powder;
3) siller tin oxide composite powder is placed in high energy ball mill, carries out wet ground under atmosphere (Ar) protection, until The partial size of gained powder is 2~4 μm, the powder after wet-milling is placed in baking oven under the conditions of 100 DEG C dry 6h, after obtaining ball milling Siller tin oxide composite powder;In wet-milling, ball material mass ratio is 3:1, and ball-milling medium is dehydrated alcohol, the mass ratio of medium and material For 1:1, rotational speed of ball-mill 250rmp, Ball-milling Time 10h;
4) the siller tin oxide composite powder after ball milling is placed on isostatic pressing machine and is formed, control isostatic pressure is 100MPa, is protected The pressure time is 10s, obtains siller tin oxide green body;
5) siller tin oxide 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 siller tin oxide ingot blank;Shown in its fracture apperance figure such as Fig. 6 (a);
6) plate is processed into siller tin oxide 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-tin alloy Powder;
Sn:10%;
Additive: Zn2%;
Surplus is Ag;
2) silver-tin alloy powder is placed in high-pressure oxidation furnace, is aoxidized under the conditions of partial pressure of oxygen is 0.5MPa, temperature is 800 DEG C 8h takes out, is crushed, sieves with 100 mesh sieve, obtain siller tin oxide composite powder;
3) siller tin oxide composite powder is placed in high energy ball mill, carries out wet ground under atmosphere (Ar) protection, until The partial size of gained powder is 3~5 μm, the powder after wet-milling is placed in baking oven under the conditions of 90 DEG C dry 9h, after obtaining ball milling Siller tin oxide composite powder powder;In wet-milling, ball material mass ratio is 5:1, and ball-milling medium is dehydrated alcohol, the quality of medium and material Than for 10:1, rotational speed of ball-mill 400rmp, Ball-milling Time 10h;
4) the siller tin oxide composite powder after ball milling is placed on isostatic pressing machine and is formed, control isostatic pressure is 80MPa, pressure maintaining Time is 100s, obtains siller tin oxide green body;
5) siller tin oxide 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 siller tin oxide ingot blank;Shown in its fracture apperance figure such as Fig. 6 (b);
6) wire rod is processed into siller tin oxide 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-tin alloy Powder;
Sn:20%;
Additive: Sb3%, Te 2%;
Surplus is Ag;
Step 2), 3), 4) with embodiment 3;
5) siller tin oxide 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 siller tin oxide ingot blank;
6) wire rod is processed into siller tin oxide 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 5
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-tin alloy Powder;
Sn:12%;
Additive: 0%;
Surplus is Ag;
Step 2), 3), 4) with embodiment 3;
5) siller tin oxide green body is placed in high-pressure oxidation furnace, is sintered under the conditions of partial pressure of oxygen is 1MPa, temperature is 950 DEG C 6h obtains siller tin oxide ingot blank;
6) wire rod is processed into siller tin oxide ingot blank hot extrusion, wire rod is used after multiple drawing and annealing to the size needed Rivet is machined to rivet type contact.
Siller tin oxide ingot blank made from siller tin oxide ingot blank made from step 5) to Examples 1 to 5 and comparative example 2 respectively The performances such as bending strength be measured, as a result as described in Table 1:
Table 1:

Claims (7)

1. a kind of preparation method for the sliver oxidized tin contactor materials for improving ingot blank agglutinating property, comprising the following steps:
1) material mixture ratio of the siller tin oxide contact prepared as needed, the dosage of silver needed for calculating, tin and additive, weighs phase Silver, tin and the additive of application amount powder by atomization after melting, obtain silver-tin alloy powder;
2) silver-tin alloy powder is aoxidized, obtains siller tin oxide composite powder;
3) siller tin oxide composite 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 siller tin oxide composite powder after obtaining ball milling;
4) the siller tin oxide composite powder after ball milling is formed, obtains siller tin oxide green body;
5) gained siller tin oxide green body is placed in partial pressure of oxygen >=0.8Mpa, temperature is sintered under conditions of being 900~960 DEG C, obtains silver Tin oxide ingot blank;
6) gained siller tin oxide ingot blank obtains AgSnO2 wire or siller tin oxide band through hot extrusion.
2. preparation method according to claim 1, it is characterised in that: in step 1), in resulting silver-tin alloy powder, press Mass percent meter, ratio shared by additive are 0~5%, and ratio shared by tin 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, In, Ni, Zn, Sb and Te.
4. preparation method according to claim 1, it is characterised in that: in step 3), 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.
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* Cited by examiner, † Cited by third party
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CN114334503A (en) * 2021-12-24 2022-04-12 佛山市诺普材料科技有限公司 Method for preparing silver tin oxide electrical contact material by low-temperature homogenization and material thereof
CN115570139A (en) * 2022-10-12 2023-01-06 浙江福达合金材料科技有限公司 Preparation method of silver tin oxide electric contact material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07173555A (en) * 1993-12-17 1995-07-11 Higashifuji Seisakusho:Kk Silver-tin oxide sintered electrical contact material excellent in melt sticking and wear resistance
CN1443864A (en) * 2003-04-17 2003-09-24 章景兴 Silver tin-oxide zinc-oxide alloy electric contact and its production process
JP2012003885A (en) * 2010-06-15 2012-01-05 Tanaka Kikinzoku Kogyo Kk Ag-OXIDE-BASED ELECTRICAL CONTACT MATERIAL AND RELAY FOR VEHICLE USING IT
CN103639232A (en) * 2013-12-06 2014-03-19 桂林电器科学研究院有限公司 Method for preparing AgSnO2 wire
CN104498762A (en) * 2014-12-30 2015-04-08 桂林电器科学研究院有限公司 Processing method of silver tin oxide electrical contact material containing additives

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07173555A (en) * 1993-12-17 1995-07-11 Higashifuji Seisakusho:Kk Silver-tin oxide sintered electrical contact material excellent in melt sticking and wear resistance
CN1443864A (en) * 2003-04-17 2003-09-24 章景兴 Silver tin-oxide zinc-oxide alloy electric contact and its production process
JP2012003885A (en) * 2010-06-15 2012-01-05 Tanaka Kikinzoku Kogyo Kk Ag-OXIDE-BASED ELECTRICAL CONTACT MATERIAL AND RELAY FOR VEHICLE USING IT
CN103639232A (en) * 2013-12-06 2014-03-19 桂林电器科学研究院有限公司 Method for preparing AgSnO2 wire
CN104498762A (en) * 2014-12-30 2015-04-08 桂林电器科学研究院有限公司 Processing method of silver tin oxide electrical contact material containing additives

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张琪: "AgSnO2CuBi电触头材料制备工艺改善研究", 《硕士学位论文》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114334503A (en) * 2021-12-24 2022-04-12 佛山市诺普材料科技有限公司 Method for preparing silver tin oxide electrical contact material by low-temperature homogenization and material thereof
CN115570139A (en) * 2022-10-12 2023-01-06 浙江福达合金材料科技有限公司 Preparation method of silver tin oxide electric contact material
CN115570139B (en) * 2022-10-12 2023-08-15 浙江福达合金材料科技有限公司 Preparation method of silver tin oxide electric contact material

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