The preparation method of tin-oxygen-silver electric contact material
Technical field
The present invention relates to the opening and closing contact field of low-voltage electrical apparatus, particularly to a kind of preparation of tin-oxygen-silver electric contact material
Method.
Background technology
The silver-based composite material that siller tin oxide is is the second phase with granules of stannic oxide, extensively should currently as contact material
For in low-voltage electrical apparatus, such as relay, catalyst, chopper etc..Compared with general particles reiforced metal-base composition, silver-colored oxygen
Changing the granules of stannic oxide in tin material not only plays the role of to strengthen matrix, and strong influence contact material is made under electric arc
Performance, such as arc resistant, anti-melting welding and anti-material transfer ability etc..With conventional appliance field wide variety of Agcdo material
Material is compared, and silver tin oxide material outstanding advantage is under arcing not producing noxious substance, thus without to human body and environment
Constitute harm, and silver cadmium oxide material then occurs that Aska-Rid. decomposes under high arc temperature, form poisonous cd steam, to human body structure
Become to threaten, pollute environment simultaneously.Silver tin oxide material is due to having excellent anti electric arc corrosion, anti-melting welding and anti-material transitivity
Can, current silver tin oxide material is the material most possibly replacing Agcdo.
However, the stannum oxide in silver tin oxide material is due to having good heat stability, under it bears arcing
Do not decompose, add nonwetting with liquid silver, easily under the stirring of electromagnetic force, be enriched in contact surface, because stannum oxide is not led
Electricity, thus lead to contact resistance increase, have electric current by when lead to temperature rise excessive.Silver tin oxide material another one is asked
Topic is that hardness is high, and plasticity is poor, leads to cold working difficult, easily cracking phenomenon in rivet processing and riveting process.
At present in industrialization, siller tin oxide is prepared representational technique and is had powder mixing method and powder internal oxidation.Powder mixing method is
By argentum powder, putty powder and additive mix homogeneously, then by way of sintering, extruding, produce silk material, subsequently through drawing
Silk, the mode of heat treatment produce into the silk material of the specification of regulation, then are processed by cold pier, process rivet, are supplied to electrical apparatus factory
It is assembled into contact to be used.Although adopting the silver tin oxide material producing in this way there is preferable plasticity, oxidation
, easily the reunion of stannum oxide in stannum skewness in silver matrix, leads to the contact resistance of contact big, temperature rise too high
Phenomenon.Powder internal oxidation is Yin Xi and its additive is melted, afterwards by alloy powder internal oxidition, subsequently through pressure
System, sintering and the operation such as extruding, wire drawing, heat treatment are produced.The silver tin oxide material that powder internal oxidation produces has good
Good tissue distribution, granules of stannic oxide is tiny in silver matrix, uniform, is provided simultaneously with good electrical property.But adopt powder
The hardness of the silver tin oxide material that internal oxidation produces is high, plasticity is poor, is difficult to processing using common cold working, and rivet becomes simultaneously
Type performance is bad, the blocked up phenomenon of silver layer easily, leads to not apply in some relay fields.
Content of the invention
It is an object of the invention to provide a kind of preparation method of tin-oxygen-silver electric contact material, the material biography that the method obtains
System contact material compare, there is powder internal oxidition and powder mixing method, that is, improve silver tin oxide material hardness and
Plasticity, it is ensured that having good processability, can improve the distributional pattern of stannum oxide again, can reduce the gathering of stannum oxide, change
Kind structural homogenity, reduces slider material temperature rise, is conducive to improving the service life of slider material, can be widely applied to low tension
Device field.
Realization the technical scheme is that
The preparation method of tin-oxygen-silver electric contact material, comprises the steps of
1) each constituent mass percentage composition is taken to be: stannum 1.0~3.0%, the metal of balance of silver carries out melting, subsequently carries out
Alloy atomization, its atomizing pressure is 75~100mpa, and atomization post-drying becomes powder, screening, and the granularity of described powder is 15~5 μ
M, becomes closely spherical;
2) powder in step 1) is carried out internal oxidition and form siller tin oxide powder, the technique of its internal oxidition is: 100 DEG C
Under, temperature retention time, in 0.5h~2h, is subsequently rapidly heated to 400 DEG C, temperature retention time 0.5h~3h, then is rapidly heated to 700 DEG C,
Temperature retention time 5h~8h;
3) by step 2) described in siller tin oxide powder sieve, with putty powder and additives mixed, obtain mixed-powder,
The quality proportioning of its each component is: stannum oxide: 8~14%, additive: and 0.1~1%, silver is surplus, and incorporation time is 3h~6h;
4) mixed-powder that step 3) obtains carries out isostatic cool pressing and forms isostatic cool pressing ingot, and the pressure of isostatic cool pressing is 50~
80mpa, the dwell time >=100s;
5) step 4) obtains isostatic cool pressing ingot sintering formation sintered ingot, and sintering temperature is 850 DEG C~920 DEG C, sintering time
For 4h~5h;
6) pressing steps 5) sintered ingot that obtains obtains a base, its extrusion ratio >=1:150;
7) by the silk base in step 6), repeatedly cold drawn or hot-drawn and heat treatment, cold drawn pass deformation is less than 10%, heat
The pass deformation drawing be less than 30%, between passage heat treatment temperature be 550 DEG C~650 DEG C, heat treatment time be 30min~
60min, obtains tin-oxygen-silver electric contact material.
Powder described in step 1) is closely spherical.
Step 2) described in Powder Oxidation during observe Powder Oxidation color change it is desirable to its color even is consistent.
The laser particle size d50 of the putty powder described in step 3) is 2~6 μm.
Additive described in step 3) is copper oxide or/and bismuth oxide.
Advantages of the present invention is:
1) adopt the inventive method it is ensured that a part of stannum oxide passes through internal oxidation process Dispersed precipitate in silver matrix
In, another partial oxidation stannum respectively in silver matrix, that is, is improved the hardness of silver tin oxide material and moulds by way of mixed powder
Property it is ensured that having good processability, the distributional pattern of stannum oxide can be improved again, the gathering of stannum oxide can be reduced, improve
Structural homogenity, reduces slider material temperature rise, is conducive to improving the service life of slider material.
2) present invention passes through to control the silver-colored granularity of glass putty and the granularity of putty powder and pattern it is ensured that the two has well
Mixed performance, is further improved the wettability of stannum oxide and silver matrix simultaneously by additive, and the material structure of formation is equal
Even, there is good electric property.
Specific embodiment
Embodiment 1:
Siller tin oxide 8 copper oxide 0.25 material (agsno2 (8) cuo(0.25)) preparation technology is as follows:
1. take each constituent mass percentage composition to be: stannum 1.0%, the metal of balance of silver carries out melting in intermediate frequency furnace, should
The weight of metal is 30kg, then passes through to carry out alloy atomization in water atomization equipment, wherein atomizing pressure is 75mpa, after atomization
It is dried into silver-colored tin powder, screening, at 13 μm, powder becomes closely spherical to the Task-size Controlling of powder;
2. the silver-colored tin powder in step 1 is carried out powder internal oxidition: the technique of internal oxidition is after 100 DEG C of insulation 1h
Be rapidly heated 400 DEG C of insulation 1h, is then rapidly heated 700 DEG C, is incubated 5h, notes observing powder during Powder Oxidation
The uniformity of oxidation color, prevents local from occurring aoxidizing insufficient phenomenon;
3. by the siller tin oxide powder of powder internal oxidition in step 2, after sieving, with laser particle size d50 in 3 μm of scope oxygen
Change glass putty and cupric oxide powder is mixed in mixed powder machine, described siller tin oxide, stannum oxide, the weight of cupric oxide powder are respectively as follows:
27.905kg, 2.02kg, 0.075kg, incorporation time 4h it is ensured that after the mixing of above-mentioned powder the weight/mass percentage composition of each component be:
Stannum oxide: 8%, copper oxide: 0.25%, silver is surplus;
4. above-mentioned mixed powder is carried out isostatic cool pressing and form isostatic cool pressing ingot, the Stress control of isostatic cool pressing exists
55mpa, dwell time 200s;
5. the isostatic cool pressing ingot in step 4 is sintered forming sintered ingot in atmosphere, and sintering temperature controls at 880 DEG C,
Sintering time is 4h;
6. the sintered ingot in step 5 is extruded, and carries out hot extrusion and forms silk base, the extrusion ratio >=1:150 of silk material, extruding
Become the silk material of 4.5mm specification;
7., by the silk base in step 6, hot-drawn is repeated and heat treatment reaches required specification 1.36mm of finished product, wherein
Hot drawn pass deformation is less than 30%, and between passage, heat treatment temperature controls at 550 DEG C, and passage heat treatment time is 30min.
Embodiment 2:
Siller tin oxide 10 bismuth oxide 0.25 material (agsno2 (10) bi2o3(0.3)) preparation technology is as follows:
1. take each constituent mass percentage composition to be: stannum 2.0%, the metal of balance of silver carries out melting in intermediate frequency furnace, should
The weight of metal is 30kg, then passes through to carry out alloy atomization in water atomization equipment, wherein atomizing pressure is 80mpa, after atomization
It is dried into powder, screening, at 11 μm, powder becomes closely spherical to the Task-size Controlling of powder;
2. the silver-colored tin powder in step 1 is carried out powder internal oxidition: the technique of internal oxidition is after 100 DEG C of insulation 1h
Be rapidly heated 400 DEG C of insulation 1.5h, is then rapidly heated 700 DEG C, is incubated 5.5h, needs strict during Powder Oxidation
The uniformity of Powder Oxidation color, prevents local from occurring aoxidizing insufficient phenomenon;
3. by the siller tin oxide powder of powder internal oxidition in step 2, after sieving, with laser particle size d50 in 3.5 μm of scope
Putty powder and oxidation bismuth meal are mixed in mixed powder machine, described siller tin oxide, stannum oxide, the weight difference of oxidation bismuth meal
For 27.67kg, 2.24kg, 0.09kg, incorporation time 4h it is ensured that after the mixing of above-mentioned powder the weight/mass percentage composition of each component be:
Stannum oxide: 10%, bismuth oxide: 0.3%, silver is surplus;
4. above-mentioned mixed powder is carried out isostatic cool pressing and forms isostatic cool pressing ingot, the pressure of isostatic cool pressing is 65mpa,
Dwell time 250s;
5. the isostatic cool pressing ingot in step 4 is sintered forming sintered ingot in atmosphere, and sintering temperature controls at 900 DEG C,
Sintering time is 4.5h;
6. the sintered ingot in step 5 carries out hot extrusion, forms silk base, the extrusion ratio >=1:150 of silk material, is squeezed into 5.4mm
The silk material of specification;
7., by the silk base in step 6, cold drawn and heat treatment is repeated and reaches required specification 2.36mm of finished product, cold drawn
Pass deformation be less than 10%, between passage heat treatment temperature be 600 DEG C, passage heat treatment time be 30min.
Embodiment 3:
Siller tin oxide 13 bismuth oxide, 0.25 copper oxide 0.25 material (agsno2 (13) bi2o3(0.25) cuo(0.25)) system
Standby technique is as follows:
1. take each constituent mass percentage composition to be: stannum 3.0%, the metal of balance of silver carries out melting in intermediate frequency furnace, this gold
The weight belonging to is 30kg, then passes through to carry out alloy atomization in water atomization equipment, wherein atomizing pressure is 90mpa, is atomized after bake
Dry become powder, screening, the Task-size Controlling of powder at 8 μm, powder become closely spherical;
2. the silver-colored tin powder in step 1 is carried out powder internal oxidition: the technique of internal oxidition is to be incubated 1.5h at 100 DEG C
After be rapidly heated 400 DEG C insulation 2h, be then rapidly heated 700 DEG C, be incubated 7h, need strict powder during Powder Oxidation
The uniformity of last oxidation color, prevents local from occurring aoxidizing insufficient phenomenon;
3. by the siller tin oxide powder of powder internal oxidition in step 2, after sieving, with laser particle size d50 in 4 μm of scope oxygen
Change glass putty and bismuth oxide, cupric oxide powder are mixed in mixed powder machine, described siller tin oxide, stannum oxide, oxidation bismuth meal, copper oxide
The weight of powder is respectively as follows: 27.09kg, 2.76kg, 0.075kg, 0.075kg, incorporation time 4.5h it is ensured that above-mentioned powder mixing after
The weight/mass percentage composition of each component is: stannum oxide: 13%, bismuth oxide: and 0.25%, copper oxide: 0.25%, silver: surplus;
4. the powder of above-mentioned mixed siller tin oxide+copper oxide is carried out isostatic cool pressing and form isostatic cool pressing ingot, cold etc.
The pressure of static pressure is 75mpa, dwell time 300s;
5. the isostatic cool pressing ingot in step 4 is sintered forming sintered ingot in atmosphere, and sintering temperature controls at 920 DEG C,
Sintering time is 5h;
6. the sintered ingot in step 5 carries out hot extrusion, forms silk base, the extruding >=1:150 of silk material, is squeezed into 6.5mm rule
The silk material of lattice;
7th, by the silk base in step 6, cold drawn and heat treatment is repeated and reaches required specification 3.86mm of finished product, cold drawn
Pass deformation be less than 10%, between passage, heat treatment temperature controls at 650 DEG C, and passage heat treatment time controls in 60min.
Prepare comparative example metal:
Comparative example 1 siller tin oxide, 8 copper oxide 0.25 material [agsno2 (8) cuo(0.25)] powder mixing method preparation technology:
1. take 30kg fine silver metal melting in intermediate frequency furnace, then pass through to carry out alloy atomization, wherein in water atomization equipment
Atomizing pressure be 75mpa, atomization post-drying become silver powder, screening, the Task-size Controlling of powder below 15 μm, powder Cheng Jinqiu
Shape;
2., by the silver powder in step 1, after sieving, the putty powder being 3 μm with laser particle size d50 and cupric oxide powder are altogether
30kg is mixed in mixed powder machine, incorporation time 4h it is ensured that after the mixing of above-mentioned powder the weight/mass percentage composition of each component be: oxygen
Change stannum: 8%, copper oxide: 0.25%, silver is surplus, obtains the powder of siller tin oxide+copper oxide;
3. the powder of above-mentioned mixed siller tin oxide+copper oxide is carried out isostatic cool pressing and form isostatic cool pressing ingot, cold etc.
The pressure of static pressure is 55mpa, dwell time 250s;
4. the isostatic cool pressing ingot in step 3 sinters formation sintered ingot in atmosphere, and sintering temperature is 880 DEG C, sintering time
For 3.5h;
5. the sintered ingot in step 4 carries out hot extrusion, forms silk base, the extrusion ratio >=1:150 of silk material, is squeezed into 5.4mm
The silk material of specification;
6., by the silk base in step 6, hot-drawn is repeated and heat treatment reaches required specification 1.36mm of finished product, hot-drawn
Pass deformation be less than 30%, between passage, heat treatment temperature controls at 550 DEG C, passage heat treatment time be 30min.
Comparative example 2 siller tin oxide, 8 copper oxide 0.25 material [agsno2 (8) cuo(0.25)] powder internal oxidition preparation work
Skill:
1. by silver plate, stannum and the common 30kg of three kinds of raw materials of copper, by mass percentage: sn:6.3%, cu:0.2%, ag: surplus
Carry out proportioning, melting in intermediate frequency furnace, then pass through to carry out alloy atomization in water atomization equipment, wherein atomizing pressure is 85mpa,
Atomization post-drying becomes silver-colored gun-metal powder, screening, and below 12 μm, powder becomes closely spherical to the Task-size Controlling of powder;
2. the silver-colored gun-metal powder in step 1 is carried out powder internal oxidition, the technique of internal oxidition aoxidizes 8h at 750 DEG C,
Form siller tin oxide 8 copper oxide 0.25(after internal oxidition and contain siller tin oxide 8%, copper oxide 0.25%, similarly hereinafter) alloy powder;
3. above-mentioned mixed powder is carried out isostatic cool pressing and forms isostatic cool pressing ingot, the pressure of isostatic cool pressing is 60mpa,
Dwell time 250s;
4. the isostatic cool pressing ingot in step 3 is sintered forming sintered ingot in atmosphere, and sintering temperature is 900 DEG C, sintering
Time is 4h;
5. the sintered ingot in step 4 carries out hot extrusion, forms silk base, the extrusion ratio >=1:150 of silk material, is squeezed into 5.4mm
The silk material of specification;
6., by the silk base in step 5, hot-drawn is repeated and heat treatment reaches required specification 1.36mm of finished product, hot-drawn
Pass deformation be less than 30%, between passage, heat treatment temperature controls at 550 DEG C, and passage heat treatment time controls in 30min.
Comparative example 3: the method using comparative example 1 produces siller tin oxide 10 bismuth oxide 0.25 material, and trimmed size is drawn to
2.36mm.
Comparative example 4: the method using comparative example 2 produces siller tin oxide 10 bismuth oxide 0.25 material, and trimmed size is drawn to
2.36mm.
Comparative example 5: the method using comparative example 1 produces siller tin oxide 13 bismuth oxide, 0.25 copper oxide 0.25 material, finished product
Specification is drawn to 3.86mm.
Comparative example 6: the method using comparative example 2 produces siller tin oxide 13 bismuth oxide, 0.25 copper oxide 0.25 material, finished product
Specification is drawn to 3.86mm.
The contrast of correlated performance is as follows:
Embodiment |
Tensile strength (mpa) |
Elongation percentage (%) |
Hv hardness |
Embodiment 1 |
255 |
12 |
85 |
Embodiment 2 |
270 |
8 |
90 |
Embodiment 3 |
315 |
6 |
98 |
Comparative example 1 |
230 |
15 |
73 |
Comparative example 2 |
280 |
5 |
95 |
Comparative example 3 |
245 |
12 |
78 |
Comparative example 4 |
295 |
4 |
100 |
Comparative example 5 |
255 |
8 |
85 |
Comparative example 6 |
330 |
3 |
105 |
From the point of view of embodiment with the contrast of comparative example, silver tin oxide material that method of the present invention produces both had had good
Good tensile strength and plasticity, hv hardness is also more moderate, and the material of the present invention has good rivet processing characteristics, simultaneously group
Knit distribution relatively good, the demand of various Contacts can be met.