CN108015276A - One kind enhancing phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof - Google Patents
One kind enhancing phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof Download PDFInfo
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- CN108015276A CN108015276A CN201711220515.2A CN201711220515A CN108015276A CN 108015276 A CN108015276 A CN 108015276A CN 201711220515 A CN201711220515 A CN 201711220515A CN 108015276 A CN108015276 A CN 108015276A
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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 enhancing phase gradient distribution infiltration class silver-based electric contact material and preparation method thereof, and step is：The first step, carries out high-energy ball milling by silver powder, enhancing phase powder, addition powder X, is prepared into composite granule；Second step, mixed powder, sieving are carried out by composite granule and silver powder, are added silver powder and are carried out wet-mixing, and add and be used for the colloid that powder is granulated；3rd step, the powder after wet-mixing is dried, be granulated, is molded；The shaping 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；4th step, degumming, infiltration are carried out by base substrate.Material prepared by the present invention is strengthened by working face to welding surface is mutually presented the distribution of a certain concentration gradient, material resistance changes with concentration, constantly reduces, and has ensured switch overall contact resistance stability in use, and temperature rise stabilization/relatively low, improve switch life.
Description
Technical field
The present invention relates to a kind of contact material and preparation method thereof, specifically, refers to a kind of enhancing phase gradient
The preparation method of distribution and the infiltration class silver-based electric contact material prepared by this method.
Background technology
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 retrieval, it is related to AgW or AgWC contact materials both at home and abroad, it is main that silver content is less than 70wt% (mass percent)
Based on being prepared with infiltration method, more than 70% mainly based on press-powder method.If Xue Bo spaces are by using ball-milling technology combination infiltration method,
Can effectively control and surface occurs during infiltration ooze silver-colored phenomenon, reduce product fraction defective (《Electrical material》Infiltration method AgW50 contacts
Ooze the technical study 2015No.4 of Ag problems in surface), its design principle：Not only meet conduction needs, and require light weight,
It is small, it is cheap.Such as patent CN 104480335A, silver powder and tungsten powder are mixed, then ball milling is placed in high purity nickel ball and water
Carry out ball milling in machine, the silver-colored tungsten mixed-powder after ball milling obtains silver tungsten contact material through drying, annealing, shaping, infiltration processing.
Improve wettability of the silver to tungsten, improve mixing uniformity, improve material compactness and electrical conductivity.
It is well known that in breaker is constantly run, since contact constantly consumes, can cause dynamic/static contact contact by
It is decrescence small.Contact resistance influence factor：A) sound contact pressure；B) contact self-resistance；C) contact surface situation.When after
In the case of both are constant, 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 and touches
Point material, its even tissue, physical property is consistent, and during slider material use, 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 stablize with it is consistent, then need contact
Material resistance constantly changes in use, reduces influence to offset contact, meets the contact resistance uniformity of switch.
The content of the invention
The present invention is in view of the deficiency of the prior art and defect, there is provided one kind enhancing 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.
To realize above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of first purpose according to the present invention, there is provided preparation for strengthening phase gradient distribution infiltration class silver-based electric contact material
Method, comprises the following steps：
The first step, carries out high-energy ball milling by silver powder, enhancing phase powder, additive X powders, is prepared into enhancing phase powder surface cladding
The composite granule of silver and additive X, wherein X can mutually infiltrate with enhancing for all and infinitely cannot mutually melt element with silver-colored；
Second step, mixed powder, sieving are carried out by the composite granule that the first step obtains and silver powder, are added silver powder progress wet method and are mixed
Close, and add and be used for the colloid that powder is granulated；
3rd step, the powder after wet-mixing is dried, be granulated, is molded, obtains base substrate；
The shaping 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；I.e.：First layer density is maximum, and second of density takes second place, successively decreases successively；
4th step, degumming, infiltration are carried out by base substrate, obtain enhancing phase gradient distribution infiltration class silver-based electric contact material.
Further, it is described to be compressed on every layer of formation zigzag fashion, when adding pressed by powder again, powder in the 3rd step
It will fill into sawtooth, and effectively increase molding blank and combine power between layers.
A kind of second purpose according to the present invention, there is provided enhancing phase gradient distribution infiltration class electrical contact prepared by above method
Material, its strengthen phase material by working face (on) to welding surface (under) gradually reduce, resistivity from top to bottom gradually reduces.
The present invention use method and conventional traditional material infiltration method or powder metallurgy press-powder sintering process preparation AgW or
The method of AgWC has dramatically different：
The circuit that the present invention uses is：The composite granule of WC or W powder coated with silver on surface and additive is prepared first, then is carried out
Mixed powder, wet mixing, drying are granulated, and are then molded, shaping can be suppressed with multistep；
In shaping, it is firstly added powder after part is granulated and is suppressed in die cavity, it is thick to adjust compacting by press power
Degree, makes first layer density maximum；Part powder is added, compacting thickness is adjusted, second layer density is taken second place, then add portion
Divide powder, adjust compacting thickness, make three layers of density minimum, operate repeatedly successively, operation repeatedly can be for twice or repeatedly.It is identical
Powder, pressing pressure gradually reduce 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 " for " sawtooth " shape suppressing above every layer
Shape, when adding pressed by powder again, powder will be filled into " sawtooth ", effectively be increased molding blank and be combined between layers
Power.
After base substrate carries out degumming after above-mentioned shaping, since each layer density is different, degumming back skeleton different levels, porosity is not
Together, when carrying out follow-up infiltration, ooze piece by placing equivalent fine silver or silver-based and carry out high temperature infiltration with base substrate bottom, through excessive
Temperature, oozes piece and starts to melt, under capillary action, into AgW or AgWC skeletons, since skeleton different levels porosity is different,
Fuse into silver also to differ, can be formed, such as：The various concentrations such as AgWC60/AgWC55/AgWC50 or AgW60/AgW55/AgW50 ladder
Degree distribution infiltration class silver-based electric contact material, can be that two layers or multilayer subgradient are distributed.
Compared with prior art, enhancing phase (WC or W) gradient distribution infiltration class silver-based electric contact material that 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 using process
In, constantly reduce, its electric life improves 10-20% than Dispersed precipitate infiltration method AgW or AgWC material, and overall temperature rise reduces 5-
15%；And process simply, suitable for large-scale production.
The method of the present invention is easy to operate, of low cost, to equipment without particular/special requirement, the silver prepared with material of the present invention
Base electric contact, is strengthened by working face to welding surface and the distribution of a certain concentration gradient is mutually presented, and material resistance changes with concentration, constantly
Reduce, ensured and switched overall contact resistance stability in use, and temperature rise stabilization/relatively low, switch life has larger
Raising.
Brief description of the drawings
Fig. 1 is that the W gradients prepared in one embodiment of the invention are distributed the metallographic of infiltration method AgW45/AgW35 contact materials
Microscopic structure, W is by working face to welding surface distribution gradient.
Fig. 2 is molding die upper mold core, the lower mold core outside drawing used in one embodiment of the invention.
Embodiment
Technical scheme is further described below, the following description is only to understand technical solution of the present invention
It is used, is not used in restriction the scope of the present invention, protection scope of the present invention is subject to claims.
Above-mentioned enhancing phase (WC or W) gradient provided by the invention is distributed infiltration class silver-based electric contact material preparation method, behaviour
Facilitate, it is of low 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, are molded, infiltration step, further,
It can include cleaning step.Step progress in detail below is referred to during specific implementation, wherein the concrete technology operation of each step
Parameter is alternatively, such as：
The first step, carries out high-energy ball milling by silver powder, W powder or WC powder, addition powder X, is prepared into WC powder coated with silver on surface
With the composite granule of additive；
In this step, parameter can use：
Ag contents are that 0.5%~5%, X contents are 0.5~5%, and surplus is W or WC, silver powder granularity：100nm≤D90
≤ 100 μm, W powder or wc grain size：50nm≤D90≤10μm.
High-energy ball milling rotating speed be 180 revs/min~300 revs/min between, Ball-milling Time for 2 it is small when~6 it is small when between；
Ratio of grinding media to material is 5:1~10:Between 1；
X can infiltrate for all with enhancing phase (WC and W), and cannot be with silver-colored unlimited mutually molten element, X granularities：100nm≤
D90≤100μm.Such as：Fe；Co；Ni etc..
Second step, mixed powder is carried out by the composite granule that the first step obtains and silver powder；
Parameter can use in this step：Rotating speed is at 10 revs/min~150 revs/min, and when the time is 2~30 small, silver contains
Measure as 15%~50%, silver powder granularity is 100nm≤D90≤100 μm.
3rd step, the powder after mixed powder is sieved；
Parameter can use in this step：Sieving is between the mesh of 30 mesh~200.
4th step, by the powder after sieving, adds silver powder and carries out wet-mixing, and add colloid；
In this step, silver content is 15%~50%, and silver powder granularity is 100nm≤D90≤100 μm；
Wet mixing solution medium can select acetone, alcohol or deionized water any of which, and ratio is powder gross weight
Measure (Kg)/liquor capacity (L)=2:1~1:Between 5；Powder gross weight/steel ball gross weight=1:5~1:Between 10；Rotating speed is
100 revs/min~300 revs/min；Time for 2 it is small when~12 it is small when；
Added colloid reaches the Polymer Solution for being granulated function to may be such that powder during follow-up stirring and drying.
5th step, the powder after wet mixing is dried and is granulated；
In this step, parameter can use：
Drying temperature is between 50 DEG C -110 DEG C；Between time is when 0.2~2 is small；
Sieve selected by granulation is between the mesh of 30 mesh~80.
6th step, powder after granulation is molded, and shaping is in two steps or multistep is suppressed；
The shaping 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 operated successively, last layer of density minimum；
The lower mold core of compacting can be plane or cambered surface, and upper mold core press face is " sawtooth " shape patterned surface.
In this step, shaping plus powder weight, by requiring that layer (such as AgW55, AgW50, or other) reason after infiltration
By density, acquisition is calculated with reference to 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 2 between layer:1~1:Between 1, between 0.05mm~0.4mm, groove bottom angle is " sawtooth " pattern depth
Between 30 degree~120 degree.
Specific formula for calculation is as follows：
Setting：Product size is length L1, width L2；It is W percent mass that single layer component AgW (t1), t1 are required after infiltration
Fraction；AgW (t1) solid densities ρ；Powder W content is t2 after wet mixing；Wet mixing glue mixing amount mass percent is t3；Individual layer requires thick
Spend for h, then, it is necessary to which it is G to add powder weight when being molded：
G=(L1 × L2 × h × ρ × t1%)/t2%/(1-t3) %；
Being calculated by formula to obtain, and every layer needs to add powder amount.
7th step, degumming is carried out by base substrate after shaping；
In this step, parameter can use：Temperature is between 300 DEG C -650 DEG C；Time for 2 it is small when~10 it is small when；Protection
Atmosphere is H2 or hydrogen-nitrogen mixture gas or vacuum.
8th step, infiltration is carried out by base substrate after degumming；
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.
Sheet weight is wherein oozed for every layer of volume V × every shelf theory density=every shelf theory substance, it is total per shelf theory substance
With-every layer weight the summation of shaping, draw and ooze piece aggregate demand.
9th step, product after infiltration is cleaned.Obtain enhancing phase gradient distribution infiltration class silver-based electric contact material.
Illustrate come the technical operation detailed to the present invention below by way of the preferred embodiment of concrete application, implement below
It is pressed in example using the mould shown in Fig. 2.
Embodiment one
Exemplified by preparing AgW40/AgW35 electrical contact materials
The first step, high-energy ball milling：Take 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 rotating speed is 180 revs/min after mixing, ball
Consume time 6 it is small when, ratio of grinding media to material 10:1, obtain being prepared into W powder coated with silver on surface and the composite granule of Ni.
Second step, carries out mixed powder, total silver content is 50% (D90=100nm by the composite granule that the first step obtains and silver powder
Silver powder 10%；D90=100 μm of silver powder 40%)；150 revs/min of rotating speed, time 2 h.
3rd step, the powder after mixing is sieved, and is sieved in 30 mesh.
4th step, by the powder after sieving, adds silver powder and carries out wet-mixing, and add 0.5% polyethylene glycol colloid；It is wet
Miscible fluid vehicle acetone, ratio are powder gross weight (Kg)/liquor capacity (L)=2:1；Powder gross weight/steel ball gross weight=
1:5；Rotating speed is 100 revs/min；When time is 2 small.
5th step, the powder after wet mixing is dried and is granulated, drying temperature is at 50 DEG C；Time is when 0.2 is small；It is granulated
Selected sieve is in 30 mesh.
6th step, powder after granulation is molded；
It is molded described in the present embodiment in two steps, is required according to finished size after infiltration：Length 8mm, width 6mm, thickness
2mm；With reference to powder silver content 50% (wt), it is calculated：It is required that it is 1mmAgW40 after first layer infiltration, after the second sublevel infiltration
1mmAgW35, then when being molded, the first layer thickness is 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) solid 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%；
It is h=1mm that individual layer, which requires thickness, then, it is necessary to which it is G1 to add first layer powder weight when being molded：
G1=(L1 × L2 × h × ρ × t1%)/t2%/÷ of (1-t3)=8 × 6 × 1 100 × 12.4 × 40%/50%/
99.5%=0.478g；
It is 0.406g to calculate second layer addition powder amount according to this.
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.
7th step, carries out degumming, temperature is at 300 DEG C by base substrate after shaping；When time 10 is small；Protective atmosphere is H2.
8th step, infiltration is carried out by base substrate after degumming, using continuous oven infiltration, is computed obtaining, it is necessary to add that to ooze piece total
Weight is 0.29g, and temperature is at 980 DEG C, when the time 7 is small, H2Protection.
9th step, product after infiltration is cleaned.Obtain enhancing phase gradient and be distributed two layers of infiltration class silver-based electric contact material
Material.
The present embodiment finally obtains W gradients distribution AgW40/AgW35 infiltration class electrical contact materials, wherein, this material resistance
Rate has under, and 2.2 μ Ω cm are reduced to by 2.5 μ Ω cm；Electric life improves 10%, and temperature rise reduces by 5%.
Embodiment two
Exemplified by preparing AgW75/AgW60/Ag45 electrical contact materials
The first step, high-energy ball milling：Take silver powder (D90=100 μm) 5% (wt), W powder (D90=50nm) 94.5% (wt), Co
Powder (D90=100 μm) 0.5% (wt), carries out high-energy ball milling, and rotating speed is 300 revs/min, when Ball-milling Time 2 is small, ratio of grinding media to material 5:
1, obtain being prepared into W powder coated with silver on surface and the composite granule of Co.
Second step, carries out mixed powder, total silver content is 15% (D90=20 μ by the composite granule that the first step obtains and silver powder
M), 10 revs/min of rotating speed, when the time 30 is small.
3rd step, the powder after mixing is sieved, and sieve 200 mesh.
4th step, by the powder after sieving, adds silver powder and carries out wet-mixing, and add 0.5% polyvinylpyrrolidone
Colloid；Rotating speed is 300 revs/min；When time is 12 small.
In this step, for the medium that wet-mixing uses for alcohol, alcohol is powder gross weight (Kg)/solution for ratio
Volume (L)=1:5；
In this step, powder gross weight/steel ball gross weight=1:10.
5th step, the powder after wet mixing is dried and is granulated, drying temperature is at 80 DEG C；Time is when 1 is small；It is granulated institute
Sieve is selected in 60 mesh.
6th step, powder after granulation is molded；
Shaping is carried out in three steps described in the present embodiment, wherein being required according to finished size after infiltration：Length 12mm, width
6mm, thickness 2.25mm；With reference to 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 time layer infiltration.Then molding parameter：First layer thickness is 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) solid 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%；
It is h=1mm that first layer, which requires thickness, then, it is necessary to which it is G1 to add first layer powder weight when being molded：
G1=(L1 × L2 × h × ρ × t1%)/t2%/÷ of (1-t3)=12 × 6 × 1 1000 × 15.36 × 75%/
85%/99.5%=0.98g；
It is 0.176g to calculate second layer addition powder amount according to this；Third layer addition powder amount is 0.488g；Lower mold core can be with
For sphere, upper mold core press face is " sawtooth " shape patterned surface, and pattern depth 0.2mm, groove bottom angle is 30 degree.
7th step, carries out degumming, wherein for temperature at 650 DEG C, time 2 h, protective atmosphere is hydrogen nitrogen by base substrate after shaping
Mixed gas.
8th step, infiltration is carried out by base substrate after degumming, using continuous oven infiltration, is computed obtaining, it is necessary to add that to ooze piece total
Weight is 0.629g, and temperature at 1200 DEG C, protect by time 2 h, hydrogen-nitrogen mixture gas.
9th step, product after infiltration is cleaned, and obtains three layers of distribution infiltration class silver-based electric contact material of enhancing phase gradient
Material.
The present embodiment finally obtains W gradients distribution AgW75/AgW60/AgW45 infiltration class electrical contact materials, 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
Exemplified by preparing AgWC65/AgWC60/AgWC55 electrical contact materials
The first step, high-energy ball milling：Take silver powder (D90=100nm) 2% (wt), WC powder (D90=10 μm) 93% (wt)；Add
Add thing 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, when Ball-milling Time 2 is small, ratio of grinding media to material 10:1, obtain being prepared into the compound of WC powder coated with silver on surface and Co, Ni
Powder.
Second step, carries out mixed powder, total silver content is 30% (D90=100 μ by the composite granule that the first step obtains and silver powder
m)；100 revs/min of its rotating speed, when the time 15 is small.
3rd step, the powder after mixing is sieved, and sieve 100 mesh.
4th step, by the powder after sieving, adds silver powder and carries out wet-mixing, and add 0.5% polyvinylpyrrolidone
Colloid；Rotating speed is 300 revs/min, when the time is 8 small.
Wet mixing solution medium deionized water, deionized water usage ratio are powder gross weight (Kg)/liquor capacity (L)=1:
5；Powder gross weight/steel ball gross weight=1:10.
5th step, the powder after wet mixing is dried and is granulated, and wherein drying temperature is at 110 DEG C, and the time is when 2 is small；
80 mesh of sieve selected by granulation.
6th step, powder after granulation is molded；
Shaping is carried out in three steps described in the present embodiment, wherein being required according to finished size after infiltration：Length 10mm, width
5mm, thickness 3mm；With reference to 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 time layer infiltration.Parameter when being then molded：First layer thickness is 1mm；Second
Layer thickness 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) solid 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%；
It is h=1mm that first layer, which requires thickness, then, it is necessary to which it is G1 to add first layer powder weight when being molded：
G1=(L1 × L2 × h × ρ × t1%)/t2%/÷ of (1-t3)=10 × 5 × 1 1000 × 13.28 × 65%/
70%/99.5%=0.619g；
It is 0.559g to calculate second layer addition powder amount according to this；Second layer addition powder amount is 0.503g；
Lower mold core can be sphere, and upper mold core press face is " sawtooth " shape patterned surface, pattern depth 0.4mm, groove bottom
Angle is 60 degree.
7th step, carries out degumming, wherein for temperature at 650 DEG C, time 2 h, protective atmosphere is hydrogen nitrogen by base substrate after shaping
Mixed gas.
8th step, infiltration is carried out by base substrate after degumming, using continuous oven infiltration, is computed obtaining, it is necessary to add that to ooze piece total
Weight is 0.278g, and temperature is at 1200 DEG C, time 2 h；Hydrogen-nitrogen mixture gas is protected.
9th step, product after infiltration is cleaned, and obtains three layers of distribution infiltration class silver-based electric contact material of enhancing phase gradient
Material.
The present embodiment finally obtains WC gradients distribution AgWC65/AgWC60/AgWC55 infiltration class electrical contact materials, 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, the W gradients to be prepared in one embodiment of the invention, which are distributed infiltration method AgW45/AgW35, makes electrical contact with material
The metallographic microstructure of material, W is by working face to welding surface distribution gradient.
To sum up, the distribution of a certain concentration gradient, material is mutually presented by working face to welding surface enhancing in the material that prepared by the present invention
Resistance changes with concentration, constantly reduces, and has ensured switch overall contact resistance stability, and temperature rise is steady in use
It is fixed/relatively low, improve switch life.It is easy to operate, it is of low cost, to equipment without particular/special requirement, and it is steady for temperature rise after switching
Fixed, the service life is higher.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or change within the scope of the claims, this not shadow
Ring the substantive content of the present invention.In the case where there is no conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (10)
- A kind of 1. preparation method for strengthening phase gradient distribution infiltration class silver-based electric contact material, it is characterised in that：Including following step Suddenly：The first step, high-energy ball milling is carried out by silver powder, enhancing phase powder, additive X powders, be prepared into enhancing phase powder coated with silver on surface and The composite granule of additive X, wherein X can mutually infiltrate with enhancing for all and infinitely cannot mutually melt element with silver-colored；Second step, carries out mixed powder, sieving by the composite granule that the first step obtains and silver powder, adds silver powder and carry out wet-mixing, And add and be used for the colloid that powder is granulated；3rd step, the powder after wet-mixing is dried, be granulated, is molded, obtains base substrate；The shaping 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；4th step, degumming, infiltration are carried out by base substrate, obtain enhancing phase gradient distribution infiltration class silver-based electric contact material.
- 2. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material according to claim 1, its feature It is：In the first step, there is one or more of technical characteristic：- the enhancing is mutually one or two kinds of for WC, W；In-the composite granule：Ag weight contents are that 0.5%~5%, X enhancing phase contents are 0.5~5%, and surplus is enhancing Phase；- silver powder the granularity is 100nm≤D90≤100 μm；- W the powder or wc grain size are 50nm≤D90≤10 μm；- X the granularities are 100nm≤D90≤100 μm；Between-high-energy ball milling the rotating speed is 180 revs/min~300 revs/min, Ball-milling Time for 2 it is small when~6 it is small when between, Ratio of grinding media to material is 5:1~10:Between 1.
- 3. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material according to claim 1, its feature It is：In the second step, there is one or more of technical characteristic：- mixed the powder, rotating speed between 10 revs/min~150 revs/min, the time for 2 it is small when~30 it is small when between；- the sieving, between the mesh of 30 mesh~200；- the colloid can to reach the Polymer Solution for being granulated function in powder drying course for all.
- 4. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material, its feature exist as claimed in claim 1 In in second step, the wet-mixing, has one or more of technical characteristic：- silver-colored the weight content is 15%~50%, and silver powder granularity is 100nm≤D90≤100 μm；- the wet-mixing, the medium used for acetone, alcohol or deionized water in it is a kind of, which is powder Body gross weight (Kg)/liquor capacity (L)=2:1~1:Between 5；- wet mixing the solution, wherein powder gross weight/steel ball gross weight=1:5~1:10, rotating speed is 100 revs/min~300 Rev/min, the time for 2 it is small when~12 it is small when.
- 5. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material, its feature exist as claimed in claim 1 In in the 3rd step, there is one or more of technical characteristic：- the drying, temperature is between 50 DEG C -110 DEG C, between the time is when 0.2~2 is small；- the granulation, selected sieve is between the mesh of 30 mesh~80.
- 6. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material, its feature exist as claimed in claim 1 In in the 3rd step, there is one or more of technical characteristic：- it is described be compressed on every layer formation zigzag fashion, again add pressed by powder when, powder will fill into sawtooth, effectively increase Big molding blank combines power between layers；- the shaping, by controlling press power to adjust compacting thickness, makes first layer density maximum；Part powder is added, is adjusted Thickness is suppressed, second layer density is taken second place, the pressing pressure of identical powder gradually reduces so that adjacent two layers density gradually subtracts It is small；Operate successively, last layer of density minimum.
- 7. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material, its feature exist as claimed in claim 6 In in the 3rd step, the compacting, wherein lower mold core are plane or cambered 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 enhancing phase gradient distribution infiltration class silver-based electric contact material, its feature exist as claimed in claim 1 In, in the 4th step, the degumming, temperature between 300 DEG C -650 DEG C, the time for 2 it is small when~10 it is small when, protective atmosphere for H2 or Hydrogen-nitrogen mixture gas or vacuum.
- 9. the preparation method of enhancing phase gradient distribution infiltration class silver-based electric contact material, its feature exist as claimed in claim 1 In in the 4th step, there is one or more of feature：- the infiltration, using continuous oven infiltration, temperature is between 980 DEG C -1200 DEG C, when time 2 h~7 are small, H2Or hydrogen nitrogen It is mixed gas protected；The first layer silver content of base substrate is between 25wt%~60wt% after the-infiltration；Adjacent two layers silver content difference is 3% Between~15%；For the sawtooth pattern depth of base substrate between 0.05mm~0.4mm, groove bottom angle is 30 degree~120 after the-infiltration Between degree.
- 10. a kind of enhancing 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 enhancing of the material is mutually gradually reduced by working to welding surface, and resistivity is gradually lowered.
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| 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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