CN109500392A - A kind of preparation method for the silver zinc oxide contact material improving ingot blank agglutinating property - Google Patents
A kind of preparation method for the silver zinc oxide contact material improving ingot blank agglutinating property Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B22F2201/00—Treatment under specific atmosphere
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- B22F2201/11—Argon
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Abstract
The invention discloses a kind of preparation methods of silver zinc oxide contact material for improving ingot blank agglutinating property, 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 aoxidized, obtains Ag-ZnO composite powder；3) Ag-ZnO composite powder is subjected to wet-milling under the conditions of protective atmosphere, the Ag-ZnO composite powder after obtaining ball milling；4) the Ag-ZnO composite powder after ball milling 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 Ag-ZnO ingot blank；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 processing performance is good.
Description
Technical field
The present invention relates to the preparation methods of Ag-ZnO contact, and in particular to a kind of silver oxidation for improving ingot blank agglutinating property
The preparation method of zinc contact material.
Background technique
Electrical contact is the core component of various high-low switch, electric appliance, instrument and meter, component, be widely used in space flight,
The industrial circles such as aviation, automobile and the large capacity AC/DC contactor of civilian industry, alternating current-direct current power relay, car electrics
And in Small And Medium Capacity low-voltage circuit breaker.Electrical contact is many kinds of, and there are commonly silver-base alloy and acid bronze alloy.In silver-base alloy
In, silver cadmium oxide contact material has good resistance to arc wear, resistance fusion welding, electric conductivity and thermal conductivity, and contact resistance
It is small, stability is high, referred to as " omnipotent slider material ".But since silver cadmium oxide material is in production and application and removal process
All there is the harm of " cadmium poison ", therefore the material for developing and developing novel environment friendly and excellent electric contact performance becomes the field
Heat subject.
Ag-ZnO (AgZnO) contact material has excellent interrupting performance, resistance fusion welding and resistance to arc erosion, and nothing
Poison ring is protected, and is one of the contact material for substituting Agcdo.The preparation method of silver zinc oxide contact material is roughly divided into powder smelting
Jin Fa, internal oxidation, chemical coprecipitation and atomization.These methods respectively have deficiency: density of material made of powder metallurgic method
Low, contact resistance is big, Wen Shenggao；The material surface and internal structure of internal oxidation preparation are uneven, and oxide particle aggregation is tight
Weight, 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
Atomization technique has merged the advantages of powder metallurgic method and internal oxidation, is suitble to produce in enormous quantities, before having good application
Scape, but atomization also brings some shortcomings while improving Ag-ZnO production efficiency, is such as sintered difficult, processability
Can be poor the problems such as.
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 high
In 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 for having hindered Ag between powder, lead to that blank sintering is difficult, poor processability.Such as Publication No.
The patent of invention of CN101202168 discloses a kind of technique for preparation of novel silver zinc oxide contact material, specifically by silver, zinc,
Additive is melted into silver-colored zinc alloy powder by fusing, water mist in mid-frequency melting furnace by a certain percentage, then to atomized alloy
Powder dried, aoxidize modifier treatment, etc. static pressure, sintering, extruding, wire drawing etc. be processed into silver zinc oxide electrical contact.Such as preceding institute
It states, since the thermodynamic stability of ZnO under normal pressure is higher than Ag2O, therefore oxidation of the oxidation prior to Ag of Zn is certainly existed, from
And cause ZnO that segregation occurs in powder particle surface, and the contact and diffusion of Ag between obstruction powder in the subsequent sintering process
Problem, therefore blank sintering difficulty, the deficiency of poor processability are equally existed in the invention.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of silver zinc oxide contact materials for improving ingot blank agglutinating property
Preparation method.This method forms the Ag-ZnO composite powder after oxidation under the conditions of atmosphere protection after wet-milling, gained green body
It is placed under specific oxygen pressure, ultra-high temperature condition and is sintered again, effectively improve the agglutinating property of ingot blank, to obtain even tissue and add
The good silver zinc oxide contact material of work performance.
In order to solve the above technical problems, the system of the silver zinc oxide contact material provided by the invention for improving ingot blank agglutinating property
Preparation Method, 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,
The silver, zinc and additive of phase the application amount powder by atomization after melting are weighed, silver-colored zinc alloyed powder is obtained；
2) silver-colored zinc alloyed powder is aoxidized, obtains Ag-ZnO composite powder；
3) Ag-ZnO 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 Ag-ZnO composite powder after obtaining ball milling；
4) the Ag-ZnO composite powder after ball milling 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 Ag-ZnO ingot blank；
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, additive institute
The ratio accounted for is 0~2%, and ratio shared by zinc is 1~20%, and surplus is silver.The selection of the additive and prior art phase
Together, it specifically can be the combination selected from one or more of Cu, Bi, Ni, Sb and Te.In the step, raw material used
Silver, zinc and additive, can be the form of pure metal spindle, are also possible to the form of pure metal powder, as Ag can be pure Ag
Block is also possible to pure Ag powder.
In the step 2) of above-mentioned preparation method, operation when oxidation is same as the prior art, specifically by silver-colored zinc alloyed 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.After oxidation
Resulting material obtains Ag-ZnO composite powder after crushing.
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
It is milled to partial size≤2 μm of gained powder, further preferred wet-milling to partial size≤1 μm of gained powder.Ball milling in wet-milling is situated between
When Ball-milling Time etc. is the same as those in the prior art for matter, ball material quality, it is preferred that ball material mass ratio is 3~10:1, and ball milling is situated between
Matter is dehydrated alcohol, and the mass ratio of medium and material is 0.5~2:1, and rotational speed of ball-mill is 250~500rmp, Ball-milling Time is 6~
15h.The protective atmosphere is usually N2Or inert gas (such as Ar).The drying of gained powder usually exists after the completion of wet-milling
80~100 DEG C of conditions carry out, and the time is usually 6~10h.
In the step 4) of above-mentioned preparation method, the Ag-ZnO composite powder after ball milling is carried out using existing conventional techniques
Ag-ZnO composite powder after ball milling is usually placed on isostatic pressing machine and forms to obtain Ag-ZnO green body by molding, controls
Isostatic 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 be 830~900 DEG C, extrusion ratio be 190~270.After obtaining Ag-ZnO wire rod or Ag-ZnO band, press
Required Ag-ZnO contact is made in existing common process.As again by wire rod or band carry out multiple drawing (or Rolling compund),
Annealing 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,
It will appear melting phenomenon when the sintering temperature of Ag-ZnO ingot blank reaches 960 DEG C, or even just will appear at 950 DEG C or more
Melting phenomenon)；On the other hand, it is sintered under the conditions of superhigh-temperature and-pressure, moreover it is possible to enhance the mutual burning between Ag-ZnO particle
Tie diffusion, promote particle between be sintered neck formation (according to conventional sintering theory, sintering temperature closer to substance fusing point,
Being sintered obtained substance has more superior sintering character), to improve the processing performance of material, and then the silver-colored oxygen of high ductility
Change zinc ingot metal base.
2, it is placed in ball mill under the conditions of atmosphere protection and carries out again after silver-colored zinc alloy powder initial oxidation made from being atomized
High energy wet-milling smashes the hard shell that segregation formation occurs in powder particle surface for the ZnO in oxidation operation, 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 zinc atom inside particle toward side to the diffusion rate inside powder particle
The diffusion rate on boundary reduces zinc 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 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-colored oxygen of 2 step 5) of comparative example
Change zinc ingot metal base and carries out appearance analysis and Metallographic Analysis respectively；Wherein, (a) is the resulting Ag-ZnO of 2 step 5) of comparative example
The fracture apperance of ingot blank is (b) metallographic structure of the resulting Ag-ZnO ingot blank of 2 step 5) of comparative example, (c) is 1 step of embodiment
The fracture apperance of rapid 5) resulting Ag-ZnO ingot blank is (d) metallographic of the resulting Ag-ZnO ingot blank of 1 step 5) of embodiment
Tissue.
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:12%；
Additive: Cu 1%, Ni 1%；
Surplus is Ag；
2) silver-colored zinc alloyed 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 Ag-ZnO composite powder；
3) Ag-ZnO 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, and the powder after wet-milling is placed in baking oven under the conditions of 80 DEG C dry 10h, obtains ball milling
Ag-ZnO composite powder afterwards；In wet-milling, ball material mass ratio is 8:1, and ball-milling medium is dehydrated alcohol, the matter of medium and material
Amount is than being 0.8:1, rotational speed of ball-mill 500rmp, Ball-milling Time 15h；
4) the Ag-ZnO composite powder after ball milling is placed on isostatic pressing machine and is formed, control isostatic pressure is 50MPa, is protected
The pressure time is 200s, obtains Ag-ZnO green body；
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, under the conditions of partial pressure of oxygen is 0.8MPa, temperature is 960 DEG C
It is sintered 6h, obtains Ag-ZnO ingot blank, material object is as shown in Figure 1, as seen from the figure, be sintered resulting Ag-ZnO surface of ingot blank
With metallic luster, illustrate 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 is warming up under standard atmosphere condition
6h.As a result: silver-based has melted (since 1 normal atmosphere pressure silver point is 961 DEG C, at 960 DEG C in gained ingot blank
Sintering 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.?
That is 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 is warming up under standard atmosphere condition
6h.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 930
Blank sintering densification effect is very undesirable at DEG C.
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-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 Ag-ZnO composite powder；
3) Ag-ZnO 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, and the powder after wet-milling is placed in baking oven under the conditions of 100 DEG C dry 6h, obtains ball milling
Ag-ZnO composite powder afterwards；In wet-milling, ball material mass ratio is 3:1, and ball-milling medium is dehydrated alcohol, the matter of medium and material
Amount is than being 1:1, rotational speed of ball-mill 250rmp, Ball-milling Time 10h；
4) the Ag-ZnO 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 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 2MPa, temperature is 960 DEG C
6h is tied, Ag-ZnO ingot blank is obtained；
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；
Zn:10%；
Additive: Sb 0.1%；
Surplus is Ag；
2) silver-colored zinc alloyed powder is placed in high-pressure oxidation furnace, oxygen under the conditions of partial pressure of oxygen is 0.5MPa, temperature is 800 DEG C
Change 8h, takes out, be crushed, sieve with 100 mesh sieve, obtain Ag-ZnO composite powder；
3) Ag-ZnO 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
Ag-ZnO composite powder powder；In wet-milling, ball material mass ratio is 5:1, and ball-milling medium is dehydrated alcohol, the matter of medium and material
Amount is than being 10:1, rotational speed of ball-mill 400rmp, Ball-milling Time 10h；
4) the Ag-ZnO composite powder after ball milling is placed on isostatic pressing machine and is formed, control isostatic pressure is 80MPa, is protected
The pressure time is 100s, obtains Ag-ZnO green body；
5) Ag-ZnO green body is placed in high-pressure oxidation furnace, is sintered 4h under the conditions of partial pressure of oxygen is 1MPa, temperature is DEG C,
Obtain 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；
Zn:20%；
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 burnt under the conditions of partial pressure of oxygen is 1MPa, temperature is 950 DEG C
6h is tied, Ag-ZnO ingot blank is obtained；
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 made from Ag-ZnO ingot blank made from step 5) to Examples 1 to 4 and comparative example 2 respectively
The performances such as the bending strength of base are 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) is the resulting silver-colored oxygen of 2 step 5) of comparative example
Change the fracture apperance of zinc ingot metal base, (b) be the metallographic structure of the resulting Ag-ZnO ingot blank of 2 step 5) of comparative example, is (c) implementation
The fracture apperance of the resulting Ag-ZnO ingot blank of 1 step 5) of example is (d) the resulting Ag-ZnO ingot blank of 1 step 5) of embodiment
Metallographic structure.As shown in Figure 4, for the sintered blank of comparison example, powder has been 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 particle
Surface is dispersed with a large amount of ZnO particle, and to bulky grain crystal grain (or particle), internal constituent analysis shows internal Theil indices
Extremely low, the overwhelming majority has been enriched to powder particle surface (as shown in Fig. 4 a, Fig. 4 b).However the sintering of present invention process preparation
The powder of base is fully sintered together, forms fine and close tissue, and the fracture of blank shows as the modeling with a large amount of dimples
Property fracture characteristic can not offer an explanation original powder particle on section at all (as shown in Fig. 4 c, Fig. 4 d).ZnO particle is not only distributed
It is also largely distributed on crystal boundary, and in the inside of crystal grain, this improves the distribution of second phase particles significantly, has
Beneficial to the raising of material processing performance, plasticity and electrical property.
Claims (7)
1. a kind of preparation method for the silver zinc oxide contact material for improving ingot blank agglutinating property, 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 aoxidized, obtains Ag-ZnO composite powder；
3) Ag-ZnO 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 Ag-ZnO composite powder after obtaining ball milling；
4) the Ag-ZnO composite powder after ball milling 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 silver
Zinc oxide ingot blank；
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 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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| CN109500392B (en) | 2021-03-16 |
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