CN108015276B - A kind of reinforced phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof - Google Patents
A kind of reinforced phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof Download PDFInfo
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- CN108015276B CN108015276B CN201711220515.2A CN201711220515A CN108015276B CN 108015276 B CN108015276 B CN 108015276B CN 201711220515 A CN201711220515 A CN 201711220515A CN 108015276 B CN108015276 B CN 108015276B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- 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
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- 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
- B22F3/1035—Liquid phase sintering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/023—Composite material having a noble metal as the basic material
- H01H1/0233—Composite material having a noble metal as the basic material and containing carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The present invention discloses a kind of reinforced phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof, step are as follows: silver powder, reinforced phase powder, addition powder X are carried out high-energy ball milling, be prepared into composite granule by the first step；Composite granule and silver powder are carried out mixed powder, sieving by second step, are added silver powder and are carried out wet-mixing, and the colloid being granulated for powder is added；Powder after wet-mixing is dried, is granulated, is formed by third step；The molding is suppressed using at least two steps, and each step suppresses to form one layer, these layers arrange from big to small according to density；Green body is carried out degumming, infiltration by the 4th step.A certain concentration gradient distribution is presented by working face to welding surface reinforced phase in material prepared by the present invention, material resistance changes with concentration, constantly reduces, and has ensured switch whole contact resistance stability in use, and temperature rise is stable/lower, improves switch life.
Description
Technical field
The present invention relates to a kind of contact materials and preparation method thereof, specifically, what is involved is a kind of enhancing phase gradients
The preparation method of distribution and the infiltration class silver-based electric contact material prepared by this method.
Background technique
With the development of the social economy, the requirement of operation and the protection of supply network also increasing to the demand of electricity
It is higher and higher.Breaker is a kind of electrical power distribution apparatus for being widely used in low-voltage distribution terminal, undertakes supply network short circuit and overload point
The function of disconnected protection.AgWC or AgW has good electric conductivity, thermal conductivity, resistance fusion welding energy and resistance to arc erosion energy, wide
It is general to be applied in Low Voltage Circuit Breaker.
Through retrieving, it is related to AgW or AgWC contact material both at home and abroad, it is main that silver content is less than 70wt% (mass percent)
Based on preparing with infiltration method, it is greater than 70% mainly based on press-powder method.If Xue Boyu is by using ball-milling technology combination infiltration method,
Silver-colored phenomenon is seeped on generation surface during infiltration can be effectively controlled, and reduces product defect rate (" electrical material " infiltration method AgW50 contact
Surface infiltration Ag problem technical study 2015No.4), design principle: not only meeting conduction needs, and require light weight,
It is small in size, it is cheap.Such as patent CN 104480335A, silver powder and tungsten powder are mixed, then are placed in ball milling with high purity nickel ball and water
Ball milling is carried out in machine, the silver-colored tungsten mixed-powder after ball milling obtains silver tungsten contact material through drying, annealing, molding, infiltration processing.
Improve silver to the wettability of tungsten, improves mixing uniformity, improve material compactness and conductivity.
It is well known that in breaker is constantly run, since contact constantly consumes, will lead to dynamic/static contact contact pressure by
It is decrescence small.Contact resistance influence factor: a) sound contact contact pressure；B) contact self-resistance；C) contact surface situation.When after
In the constant situation of the two, as sound contact force reduces, contact resistance is increasing, makes its severe life time reduction；Due to electricity
Hinder it is larger, cause breaker fever it is more, plastic housing insulation performance reduce, personal safety may be endangered.The above method prepares AgW touching
Point material, even tissue, physical property is consistent, and in slider material use process, resistance does not change.But with contact
Pressure reduces, and circuit breaker contact persistence can constantly increase, in order to enable circuit breaker contact persistence it is stable with it is consistent, then need contact
Material resistance constantly changes in use, reduces influence to offset contact pressure, meets the contact resistance consistency of switch.
Summary of the invention
The present invention in view of the deficiency of the prior art and defect, provides a kind of reinforced phase gradient distribution infiltration class silver
Base electrical contact material and preparation method thereof, emphasis solves breaker in use, since contact is continuous in use
Consumption, contact resistance become larger problem.
In order to achieve the above object, the technical solution adopted by the present invention is that:
First purpose according to the present invention provides a kind of preparation of reinforced phase gradient distribution infiltration class silver-based electric contact material
Method, comprising the following steps:
Silver powder, reinforced phase powder, additive X powder are carried out high-energy ball milling, are prepared into reinforced phase powder surface cladding by the first step
Silver-colored and additive X composite granule, wherein X can infiltrate with reinforced phase for all and infinitely cannot mutually melt element with silver-colored；
Composite granule and silver powder that the first step obtains are carried out mixed powder, sieving by second step, and it is mixed to add silver powder progress wet process
It closes, and the colloid being granulated for powder is added；
Powder after wet-mixing is dried, is granulated, is formed, obtains green body by third step；
The molding is suppressed using at least two steps, and each step suppresses to form one layer, these layers according to density from big to small according to
Secondary arrangement；That is: first layer density is maximum, and second of density takes second place, successively successively decreases；
Green body is carried out degumming, infiltration, obtains reinforced phase gradient distribution infiltration class silver-based electric contact material by the 4th step.
Further, described to be compressed on every layer of formation zigzag fashion in third step, when pressed by powder being added again, powder
It will fill into sawtooth, and effectively increase molding blank binding force between layers.
Second purpose according to the present invention provides a kind of reinforced phase gradient distribution infiltration class electrical contact of above method preparation
Material, enhancing phase material by working face (on) to welding surface (under) gradually decrease, resistivity from top to bottom gradually decreases.
The infiltration method or powder metallurgy press-powder sintering process of use the method for the present invention and previous traditional material prepare AgW or
The method of AgWC has dramatically different:
The route that the present invention uses is: preparing the composite granule of WC or W powder coated with silver on surface and additive first, then carries out
Mixed powder, wet mixing, drying are granulated, and are then formed, molding can be suppressed with multistep；
At the time of molding, it is firstly added powder after part is granulated to be suppressed in die cavity, it is thick to adjust compacting by press power
Degree keeps first layer density maximum；Part powder is added, compacting thickness is adjusted, so that second layer density is taken second place, then add portion
Divide powder, adjust compacting thickness, make three layers of density minimum, successively operate repeatedly, operation can be for twice or repeatedly repeatedly.It is identical
Powder, pressing pressure gradually decrease, so that adjacent two layers density is gradually reduced.Two layers of adjacent layer at the middle and upper levels in pressing process not
Influence whether lower layer density.
Further, the shaping upper core that the present invention uses leaves " sawtooth " on every layer of compacting for " sawtooth " shape
Shape, when pressed by powder being added again, powder will be filled into " sawtooth ", effectively be increased molding blank and be combined between layers
Power.
After green body carries out degumming after above-mentioned molding, since each layer density is different, degumming back skeleton different levels, porosity is not
Together, when carrying out subsequent infiltration, piece and green body bottom progress high temperature infiltration are seeped by placing equivalent fine silver or silver-based, through excessively high
Temperature seeps piece and starts to melt, under capillary action, into AgW or AgWC skeleton, since skeleton different levels porosity is different,
It is also not identical to fuse into silver, can be formed, such as: AgWC60/AgWC55/AgWC50 or AgW60/AgW55/AgW50 various concentration ladder
Degree distribution infiltration class silver-based electric contact material, can be distributed for two or more layers subgradient.
Compared with prior art, reinforced phase (WC or W) gradient distribution infiltration class silver-based electric contact material prepared by the present invention,
Not only there is infiltration method AgW or AgWC high-compactness, high-wearing feature, high health heat sealability, but also its contact resistance is in use process
In, it constantly reduces, electric life improves 10-20% than Dispersed precipitate infiltration method AgW or AgWC material, and whole temperature rise reduces 5-
15%；And the processing is simple, is suitable for large-scale production.
The method of the present invention is easy to operate, low in cost, to equipment without particular/special requirement, the silver prepared with material of the present invention
A certain concentration gradient distribution is presented by working face to welding surface reinforced phase in base electric contact, and material resistance changes with concentration, constantly
It reduces, has ensured switch whole contact resistance stability in use, and temperature rise is stable/lower, switch life has larger
Raising.
Detailed description of the invention
Fig. 1 is the metallographic of the W gradient distribution infiltration method AgW45/AgW35 contact material prepared in one embodiment of the invention
Microscopic structure, W is by working face to welding surface distribution gradient.
Fig. 2 is the molding die upper mold core used in one embodiment of the invention, lower mold core outside drawing.
Specific embodiment
Further description of the technical solution of the present invention below, and the following description is only to understand technical solution of the present invention
It is used, is not used in and limits the scope of the invention, protection scope of the present invention is subject to claims.
Above-mentioned reinforced phase (WC or W) gradient distribution infiltration class silver-based electric contact material preparation method provided by the invention, behaviour
Facilitate, it is low in cost, to equipment without particular/special requirement, and stablize for temperature rise after switching, the service life is higher.
In the present invention, the high-energy ball milling of design, mixed powder, wet mixing, drying are granulated, form, infiltration step, further,
It may include cleaning step.Step progress in detail below is referred to when specific implementation, wherein the concrete technology of each step operates
Parameter is alternatively, such as:
Silver powder, W powder or WC powder, addition powder X are carried out high-energy ball milling, are prepared into WC powder coated with silver on surface by the first step
With the composite granule of additive；
In this step, parameter can be used:
Ag content is that 0.5%~5%, X content is 0.5~5%, and surplus is W or WC, silver powder granularity: 100nm≤D90
≤ 100 μm, W powder or wc grain size: 50nm≤D90≤10 μm.
High-energy ball milling revolving speed is between 180 revs/min~300 revs/min, and Ball-milling Time is between 2 hours~6 hours；
Ratio of grinding media to material is between 5:1~10:1；
X is that all can be infiltrated with reinforced phase (WC and W), and infinitely cannot mutually melt element with silver-colored, X granularity: 100nm≤
D90≤100μm.Such as: Fe；Co；Ni etc..
Composite granule and silver powder that the first step obtains are carried out mixed powder by second step；
Parameter can use in this step: revolving speed is at 10 revs/min~150 revs/min, and the time is 2~30 hours, and silver contains
Amount is 15%~50%, and silver powder granularity is 100nm≤D90≤100 μm.
Powder after mixed powder is sieved by third step；
Parameter can use in this step: sieving is between 30 mesh~200 mesh.
Powder after sieving is added silver powder and carries out wet-mixing by the 4th step, and colloid is added；
In this step, silver content is 15%~50%, and silver powder granularity is 100nm≤D90≤100 μm；
Wet mixing solution medium can choose acetone, alcohol or deionized water any of them, and ratio is powder gross weight
It measures between (Kg)/liquor capacity (L)=2:1~1:5；Between powder total weight/steel ball total weight=1:5~1:10；Revolving speed is
100 revs/min~300 revs/min；Time is 2 hours~12 hours；
Colloid be added is that may make powder during subsequent stirring and drying, reaches the Polymer Solution for being granulated function.
Powder after wet mixing is dried and is granulated by the 5th step；
In this step, parameter can be used:
Drying temperature is between 50 DEG C -110 DEG C；Time is between 0.2~2 hour；
Selected sieve is granulated between 30 mesh~80 mesh.
6th step forms powder after granulation, and molding is in two steps or multistep is suppressed；
The molding is suppressed using at least two steps, and each step suppresses to form one layer, and wherein first layer density is maximum, the second layer
Density is taken second place, and is successively operated, and the last layer density is minimum；
The lower mold core of compacting can be a plane or an arc surface, and upper mold core press face is " sawtooth " shape patterned surface.
In this step, molding plus powder weight, by requiring that layer (such as AgW55, AgW50 or other) to manage after infiltration
By density, acquisition is calculated in conjunction with the silver content of skeleton powder to be pressed after degumming, by pressed density, matrix porosity rate is controlled, makes
After infiltration between first layer silver content 25wt%~60wt%；Between adjacent two layers silver content difference 5%~15%.Any two
Thickness proportion is between 2:1~1:1 between layer, and between 0.05mm~0.4mm, groove bottom angle is " sawtooth " pattern depth
Between 30 degree~120 degree.
Specific formula for calculation is as follows:
Set: product size is length L1, width L2；It is required after infiltration single layer component AgW (t1), t1 is W percent mass
Score；AgW (t1) theoretical density ρ；Powder W content is t2 after wet mixing；Wet mixing glue mixing amount mass percent is t3；Single layer requires thick
Degree is h, then when forming, needing to be added powder weight is G:
G=(L1 × L2 × h × ρ × t1%)/t2%/(1-t3) %；
It can be obtained by formula calculating, every layer needs to add powder amount.
Green body after molding is carried out degumming by the 7th step；
In this step, parameter can be used: temperature is between 300 DEG C -650 DEG C；Time is 2 hours~10 hours；Protection
Atmosphere is H2 or hydrogen-nitrogen mixture gas or vacuum.
Green body after degumming is carried out infiltration by the 8th step；
In this step, the infiltration is continuous oven infiltration, and temperature is between 980 DEG C -1200 DEG C；Time 2 h~7 are small
When；H2 or hydrogen-nitrogen mixture gas protection.
Wherein seeping sheet weight is every layer of volume V × every shelf theory density=every shelf theory substance, and every shelf theory substance is total
With-every layer weight the summation of molding, obtains and seep piece aggregate demand.
9th step cleans product after infiltration.Obtain reinforced phase gradient distribution infiltration class silver-based electric contact material.
The detailed technical operation of the present invention is illustrated below by way of the preferred embodiment of concrete application, is implemented below
It is pressed in example using mold shown in Fig. 2.
Embodiment one
For preparing AgW40/AgW35 electrical contact material
High-energy ball milling: the first step takes silver powder (D90=100nm) 0.5% (wt), W powder (D90=50nm) 10% (wt)；W
Powder (D90=10 μm) 84.5%, Ni powder (D90=100nm) 5% (wt), high-energy ball milling revolving speed is 180 revs/min after mixing, ball
Time consuming 6 hours, ratio of grinding media to material 10:1, obtains the composite granule for being prepared into W powder coated with silver on surface and Ni.
Composite granule and silver powder that the first step obtains are carried out mixed powder by second step, and total silver content is 50% (D90=100nm
Silver powder 10%；D90=100 μm of silver powder 40%)；150 revs/min of revolving speed, time 2 h.
Powder after mixing is sieved by third step, is sieved in 30 mesh.
Powder after sieving is added silver powder and carries out wet-mixing by the 4th step, and 0.5% polyethylene glycol colloid is added；It is wet
Miscible fluid vehicle acetone, ratio are powder total weight (Kg)/liquor capacity (L)=2:1；Powder total weight/steel ball total weight=
1:5；Revolving speed is 100 revs/min；Time is 2 hours.
Powder after wet mixing is dried and is granulated by the 5th step, and drying temperature is at 50 DEG C；Time was at 0.2 hour；It is granulated
Selected sieve is in 30 mesh.
6th step forms powder after granulation；
It forms described in the present embodiment in two steps, is required according to finished size after infiltration: length 8mm, width 6mm, thickness
2mm；It in conjunction with powder silver content 50% (wt), is calculated: it is required that being 1mmAgW40 after first layer infiltration, after the second sublevel infiltration
1mmAgW35, then when forming, first layer is with a thickness of 1mm；Second layer thickness 2mm, product size are length L1:8mm, width L2:
6mm；The first composition of layer AgW (40), t1=40 are required after infiltration；AgW (40) theoretical density ρ=12.4g/cm3；Powder after wet mixing
W content is t2=50；Wet mixing glue mixing amount mass percent is t3=0.5%；
Single layer requires with a thickness of h=1mm, then when forming, needing to be added first layer powder weight is G1:
G1=(L1 × L2 × h × ρ × t1%)/t2%/(1-t3)=8 × 6 × 1 ÷ 100 × 12.4 × 40%/50%/
99.5%=0.478g；
Calculating second layer addition powder amount according to this is 0.406g.
Lower mold core can be plane, and upper mold core press face is " sawtooth " shape patterned surface, pattern depth 0.05mm, groove bottom
Angle is 120 degree.
Green body after molding is carried out degumming by the 7th step, and temperature is at 300 DEG C；Time 10 hours；Protective atmosphere is H2.
Green body after degumming is carried out infiltration and is computed acquisition using continuous oven infiltration by the 8th step, and it is total to need to add infiltration piece
Weight is 0.29g, and temperature is at 980 DEG C, the time 7 hours, H2Protection.
9th step cleans product after infiltration.Obtain two layers of infiltration class silver-based electric contact material of reinforced phase gradient distribution
Material.
The present embodiment finally obtains W gradient distribution AgW40/AgW35 infiltration class electrical contact material, wherein this material resistance
Rate has under, is reduced to 2.2 μ Ω cm by 2.5 μ Ω cm；Electric life improves 10%, and temperature rise reduces by 5%.
Embodiment two
For preparing AgW75/AgW60/Ag45 electrical contact material
High-energy ball milling: the first step takes silver powder (D90=100 μm) 5% (wt), W powder (D90=50nm) 94.5% (wt), Co
Powder (D90=100 μm) 0.5% (wt), carry out high-energy ball milling, revolving speed be 300 revs/min, Ball-milling Time 2 hours, ratio of grinding media to material 5:
1, obtain the composite granule for being prepared into W powder coated with silver on surface and Co.
Composite granule and silver powder that the first step obtains are carried out mixed powder by second step, and total silver content is 15% (D90=20 μ
M), 10 revs/min of revolving speed, the time 30 hours.
Powder after mixing is sieved by third step, and be sieved 200 mesh.
Powder after sieving is added silver powder and carries out wet-mixing by the 4th step, and 0.5% polyvinylpyrrolidone is added
Colloid；Revolving speed is 300 revs/min；Time is 12 hours.
In this step, for the medium that wet-mixing uses for alcohol, the ratio that is used to of alcohol is powder total weight (Kg)/solution
Volume (L)=1:5；
In this step, powder total weight/steel ball total weight=1:10.
Powder after wet mixing is dried and is granulated by the 5th step, and drying temperature is at 80 DEG C；Time was at 1 hour；It is granulated institute
Select sieve in 60 mesh.
6th step forms powder after granulation；
Molding described in the present embodiment is carried out in three steps, wherein being required according to finished size after infiltration: length 12mm, width
6mm, thickness 2.25mm；In conjunction with powder silver content 15% (wt), it is calculated: it is required that be 1mmAgW75 after first layer infiltration, the
0.25mmAgW60 after quadratic-layer infiltration, 0.25mmAgW45 after third sublevel infiltration.Then molding parameter: first layer is with a thickness of 1mm；
Second layer thickness 0.25mm, third layer thickness 1mm；Product size is length L1:12mm, width L2:6mm；Is required after infiltration
One composition of layer AgW (75), t1=75；AgW (75) theoretical density ρ=15.36g/cm3；Powder W content is t2=85 after wet mixing；
Wet mixing glue mixing amount mass percent is t3=0.5%；
First layer requires with a thickness of h=1mm, then when forming, needing to be added first layer powder weight is G1:
G1=(L1 × L2 × h × ρ × t1%)/t2%/(1-t3)=12 × 6 × 1 ÷ 1000 × 15.36 × 75%/
85%/99.5%=0.98g；
Calculating second layer addition powder amount according to this is 0.176g；It is 0.488g that third layer, which adds powder amount,；Lower mold core can be with
For spherical surface, upper mold core press face is " sawtooth " shape patterned surface, and pattern depth 0.2mm, groove bottom angle is 30 degree.
Green body after molding is carried out degumming by the 7th step, and wherein for temperature at 650 DEG C, time 2 h, protective atmosphere is hydrogen nitrogen
Mixed gas.
Green body after degumming is carried out infiltration and is computed acquisition using continuous oven infiltration by the 8th step, and it is total to need to add infiltration piece
Weight is 0.629g, and temperature at 1200 DEG C, protect by time 2 h, hydrogen-nitrogen mixture gas.
9th step cleans product after infiltration, obtains enhancing three layers of distribution infiltration class silver-based electric contact material of phase gradient
Material.
The present embodiment finally obtains W gradient distribution AgW75/AgW60/AgW45 infiltration class electrical contact material, wherein this material
Material resistivity has under, by 4.0 μ Ω cm to 3.5 μ Ω cm to 2.6 μ Ω cm；Electric life improves 20%, and temperature rise reduces
15%.
Embodiment three
For preparing AgWC65/AgWC60/AgWC55 electrical contact material
High-energy ball milling: the first step takes silver powder (D90=100nm) 2% (wt), WC powder (D90=10 μm) 93% (wt)；Add
Add object Co powder (D90=100 μm) 0.5% (wt), additive Ni powder (D90=100nm) 4.5% (wt) carries out high-energy ball milling, turns
Speed is 300 revs/min, Ball-milling Time 2 hours, ratio of grinding media to material 10:1, obtains being prepared into the compound of WC powder coated with silver on surface and Co, Ni
Powder.
Composite granule and silver powder that the first step obtains are carried out mixed powder by second step, and total silver content is 30% (D90=100 μ
m)；100 revs/min of its revolving speed, the time 15 hours.
Powder after mixing is sieved by third step, and be sieved 100 mesh.
Powder after sieving is added silver powder and carries out wet-mixing by the 4th step, and 0.5% polyvinylpyrrolidone is added
Colloid；Revolving speed is 300 revs/min, and the time is 8 hours.
Wet mixing solution medium deionized water, deionized water usage ratio are powder total weight (Kg)/liquor capacity (L)=1:
5；Powder total weight/steel ball total weight=1:10.
Powder after wet mixing is dried and is granulated by the 5th step, and wherein drying temperature is at 110 DEG C, and the time was at 2 hours；
It is granulated 80 mesh of selected sieve.
6th step forms powder after granulation；
Molding described in the present embodiment is carried out in three steps, wherein being required according to finished size after infiltration: length 10mm, width
5mm, thickness 3mm；In conjunction with powder silver content 30% (wt), it is calculated: it is required that be 1mmAgWC65 after first layer infiltration, second
1mmAgWC60 after sublevel infiltration, 1mmAgWC55 after third sublevel infiltration.Parameter when then forming: first layer is with a thickness of 1mm；Second
Thickness degree 1mm, third layer thickness 1mm；Product size is length L1:10mm, width L2:5mm；The first composition of layer is required after infiltration
AgWC (65), t1=65；AgWC (65) theoretical density ρ=13.28g/cm3；Powder WC content is t2=70 after wet mixing；Wet mixing is mixed
Glue amount mass percent is t3=0.5%；
First layer requires with a thickness of h=1mm, then when forming, needing to be added first layer powder weight is G1:
G1=(L1 × L2 × h × ρ × t1%)/t2%/(1-t3)=10 × 5 × 1 ÷ 1000 × 13.28 × 65%/
70%/99.5%=0.619g；
Calculating second layer addition powder amount according to this is 0.559g；It is 0.503g that the second layer, which adds powder amount,；
Lower mold core can be spherical surface, and upper mold core press face is " sawtooth " shape patterned surface, pattern depth 0.4mm, groove bottom
Angle is 60 degree.
Green body after molding is carried out degumming by the 7th step, and wherein for temperature at 650 DEG C, time 2 h, protective atmosphere is hydrogen nitrogen
Mixed gas.
Green body after degumming is carried out infiltration and is computed acquisition using continuous oven infiltration by the 8th step, and it is total to need to add infiltration piece
Weight is 0.278g, and temperature is at 1200 DEG C, time 2 h；Hydrogen-nitrogen mixture gas protection.
9th step cleans product after infiltration, obtains enhancing three layers of distribution infiltration class silver-based electric contact material of phase gradient
Material.
The present embodiment finally obtains WC gradient distribution AgWC65/AgWC60/AgWC55 infiltration class electrical contact material, wherein
This resistivity of material has under, by 5.0 μ Ω cm to 4.5 μ Ω cm to 4.0 μ Ω cm；Electric life improves 10%, temperature rise
Reduce by 10%.
As shown in Figure 1, being in electrical contact material for the W gradient distribution infiltration method AgW45/AgW35 prepared in one embodiment of the invention
The metallographic microstructure of material, W is by working face to welding surface distribution gradient.
To sum up, a certain concentration gradient distribution, material is presented by working face to welding surface reinforced phase in material prepared by the present invention
Resistance changes with concentration, constantly reduces, and has ensured switch whole contact resistance stability in use, and temperature rise is steady
It is fixed/lower, improve switch life.It is easy to operate, it is low in cost, to equipment without particular/special requirement, and it is steady for temperature rise after switching
Fixed, the service life is higher.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (10)
1. a kind of preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material, it is characterised in that: including following step
It is rapid:
The first step, by silver powder, reinforced phase powder, additive X powder carry out high-energy ball milling, be prepared into reinforced phase powder coated with silver on surface and
The composite granule of additive X, wherein X can infiltrate with reinforced phase for all and infinitely cannot mutually melt element with silver-colored；The enhancing
It is mutually that WC, W are one or two kinds of；
Composite granule and silver powder that the first step obtains are carried out mixed powder, sieving, add silver powder and carry out wet-mixing by second step,
And the colloid being granulated for powder is added；
Powder after wet-mixing is dried, is granulated, is formed, obtains green body by third step；
The molding is suppressed using at least two steps, and each step suppresses to form one layer, these layers arrange from big to small according to density；
Green body is carried out degumming, infiltration, obtains reinforced phase gradient distribution infiltration class silver-based electric contact material by the 4th step.
2. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material according to claim 1, feature
It is: in the first step, there is one or more of selection:
In the composite granule: Ag weight content is 0.5%~5%, and additive X weight content is 0.5~5%, and surplus is to increase
Qiang Xiang；
The silver powder granularity is 100nm≤D90≤100 μm；
The W powder or wc grain size are 50nm≤D90≤10 μm；
The additive X granularity is 100nm≤D90≤100 μm；
The high-energy ball milling revolving speed be 180 revs/min~300 revs/min between, Ball-milling Time be 2 hours~6 hours between,
Ratio of grinding media to material is between 5:1~10:1.
3. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material according to claim 1, feature
It is: in the second step, there is one or more of selection:
The mixed powder, for revolving speed between 10 revs/min~150 revs/min, the time is between 2 hours~30 hours；
The sieving, between 30 mesh~200 mesh；
The colloid is that all can to reach the Polymer Solution for being granulated function in powder drying course.
4. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material as described in claim 1, feature exist
In in second step, the wet-mixing has one or more of selection:
The silver weight content is 15%~50%, and silver powder granularity is 100nm≤D90≤100 μm；
The wet-mixing, for the medium used to be a kind of in acetone, alcohol or deionized water, which is powder
Between body total weight (Kg)/liquor capacity (L)=2:1~1:5；
The wet-mixing, the wherein powder total weight of wet mixing solution/steel ball total weight=1:5~1:10, revolving speed is 100 turns/
Minute~300 revs/min, the time is 2 hours~12 hours.
5. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material as described in claim 1, feature exist
In in third step, with one or more of selection:
The drying, temperature is between 50 DEG C -110 DEG C, and the time is between 0.2~2 hour；
The granulation, selected sieve is between 30 mesh~80 mesh.
6. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material as described in claim 1, feature exist
In in third step, with one or more of selection:
Described to be compressed on every layer of formation zigzag fashion, when pressed by powder being added again, powder will be filled into sawtooth, effectively be increased
Big molding blank binding force between layers；
The molding adjusts compacting thickness by control press power, keeps first layer density maximum；Part powder is added, is adjusted
Thickness is suppressed, so that second layer density is taken second place, the pressing pressure of identical powder gradually decreases, so that adjacent two layers density gradually subtracts
It is small；It successively operates, the last layer density is minimum.
7. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material as claimed in claim 6, feature exist
In in third step, the compacting, wherein lower mold core is a plane or an arc surface, and upper mold core press face is sawtooth pattern face, is being suppressed
Every layer leaves zigzag fashion above.
8. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material as described in claim 1, feature exist
In in the 4th step, the degumming, temperature is between 300 DEG C -650 DEG C, and the time is 2 hours~10 hours, protective atmosphere H2Or
Hydrogen-nitrogen mixture gas or vacuum.
9. the preparation method of reinforced phase gradient distribution infiltration class silver-based electric contact material as described in claim 1, feature exist
In in the 4th step, with one or more of selection:
The infiltration, using continuous oven infiltration, temperature is between 980 DEG C -1200 DEG C, time 2 h~7 hour, H2Or hydrogen nitrogen
It is mixed gas protected；
The first layer silver content of green body is between 25wt%~60wt% after the infiltration；Adjacent two layers silver content difference is 3%
Between~15%；
For the sawtooth pattern depth of green body between 0.05mm~0.4mm, groove bottom angle is 30 degree~120 after the infiltration
Between degree.
10. a kind of reinforced phase gradient distribution infiltration class silver-based electricity being prepared such as any one of claim 1-9 the method connects
Material is touched, the concentration of the reinforced phase of the material is gradually decreased by working face to welding surface, and resistivity is gradually lowered.
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| CN108807020A (en) * | 2018-05-29 | 2018-11-13 | 德力西电气有限公司 | A kind of contact system of breaker of plastic casing |
| CN110373566B (en) * | 2019-08-23 | 2020-06-30 | 浙江大学 | AgWCC electric contact material with special tissue structure and preparation method |
| CN111054927A (en) * | 2019-12-03 | 2020-04-24 | 同济大学 | Aluminum/magnesium/aluminum composite board with interface structure design and powder hot-pressing preparation method thereof |
| CN111411280A (en) * | 2020-03-03 | 2020-07-14 | 福达合金材料股份有限公司 | Copper tungsten carbide diamond composite electrical contact material and preparation method thereof |
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