CN101651050B - Submicron particle reinforced Ag-based electrical contact material and preparation method thereof - Google Patents
Submicron particle reinforced Ag-based electrical contact material and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a submicron particle reinforced Ag-based electrical contact material and a preparation method thereof. The method comprises the following steps: adopting chemical plating method to coat silver on the surface of submicron W particles or WC particles, and then adopting pressing infiltration method to prepare dense micron particle reinforced Ag-based composite material. The material comprises the following components by weight percent: 0.1%<=Ni<=2%, 0.1%<=Cu<=2%, 30%<=W(or WC)<=80% and the balance Ag, wherein the grain size of W or WC powder is 0.01-1mu. The material of the present invention has good mechanical and physical properties and the reinforced phase particles are dispersed evenly. Compared with the traditional Ag-W material or Ag-WC material, the material has better fusion welding resistance, lower electric arc burning loss resistance and longer electrical life as the tiny high melting point reinforced phase is distributed evenly in the material substrate in dispersion manner.
Description
Technical field
The present invention relates to a kind of electrical contact material and preparation method thereof, specifically, what relate to is a kind of submicron particle reinforced Ag-based electrical contact material and preparation method thereof.
Background technology
Characteristics such as Ag-W or Ag-WC contact material be owing to have favorable conductive, heat conductivility, and erosion-resisting characteristics is good and be widely used in circuit breaker.In recent years, constantly release the novel mold cased circuit breaker and the small-sized high score circuit breaker of various series both at home and abroad, these novel circuit breaker volumes are littler, and breaking capacity but increases substantially.Novel breaker is except adopting a series of new current limiting techniques to improve the breaking capacity, and to the anti-melting welding of all electric contacts, anti-electrical arc erosion and electric life are all had higher requirement.At above growing instructions for use, concentrate on aspects such as improving material preparation method and component prescription both at home and abroad.Result of study is as follows:
1) model is beautiful; The research of silver tungsten series contact infiltration process; Suzhou Silk Polytechnic College journal 21 (5) 2001
2) Meng Fanqi; The preparation technology of silver tungsten contact material and serviceability; Material Leader V20 2006
3) the preparation method CN1651590A of a kind of tungsten copper or tungsten silver
From above document result as can be known the main preparation methods of Ag-W or Ag-WC material have: 1) powder metallurgic method; 2) infiltration method; 3) chemical coprecipitation.And discover that by above method powder metallurgy process has easy and simple to handle, characteristics such as Composition Control is flexible, but be difficult to obtain densified composite.Chemical coprecipitation obtains material even dispersion, easy sintering, but this method can only be applied to certain material system such as Ag-W material, and the Ag-WC material just can't use coprecipitation production.And coprecipitation can be brought unavoidable impurities into, thereby influences material property.Infiltration method is preparation method commonly used, has the advantage that technological operation is simple, density of material is high, but for the Ag sill that the preparation submicron particles strengthens, need carry out necessary early stage to powder and handle, otherwise can occur can not infiltration or clustering phenomena produce.The lot of domestic and foreign result of study shows: the anti-arc erosion performance of contact material and resistance fusion welding can be along with W particle or reducing of WC particle granularity and strengthen.Its subject matter that need solve is the too much problem of skewness, hole that fine particle is reunited and caused.
Summary of the invention
The present invention is directed to deficiency and defective that above-mentioned prior art exists, adopt chemical plating and infiltration technique process combined route, at the tiny characteristics of grain graininess, chemical plating adopts the liquid phase spraying and stirs the preparation method that the excusing from death concussion combines, a kind of submicron particle reinforced Ag-based electrical contact material and preparation method thereof is provided, and this material has the institutional framework of even dispersion, the material density height, arc ablation resistance and resistance fusion welding can be good, have good electric life.
For achieving the above object, the technical solution used in the present invention is:
A kind of submicron particle reinforced Ag-based electrical contact material provided by the present invention, component that comprises and weight percent content thereof are: 0.1%≤nickel (Ni)≤2%, 0.1%≤copper (Cu)≤2%, 30%≤tungsten (W) or tungsten carbide (WC)≤80%, surplus are silver; Described tungsten carbide (WC) or tungsten (W) particle size are between 0.1～1um.
The present invention also provides the preparation method of above-mentioned submicron particle reinforced Ag-based electrical contact material; at first adopt chemical plating method at sub-micron W particle or WC particle coated with silver on surface, suppress infiltrating method then and prepare fine and close sub-micron hard-phase particles enhancing silver-based composite material.Specific procedure has the surface treatment of employing, chemical plating, vacuum drying, ball milling, compacting, infiltration, the multiple pressure.
During the inventive method specific implementation, can carry out according to following steps:
The first step is carried out chemical plating with tungsten carbide after the surface treatment or tungsten powder;
Described chemical plating, its basic procedure are at first disposing reducing solution, and the powder that the first step is obtained is poured into and stirred ultrasonic dispersion in the reducing solution again, main salt liquor argenti nitratis ophthalmicus is added in the reducing solution carry out plating then.The plating mode adopts ultrasonic concussion to combine with stirring.The chemical plating reducing solution is a hydrazine hydrate solution, and volumetric concentration is 3～6ml/L, adopts ammoniacal liquor to regulate acidity-basicity ph value between 8～10.Main salt silver nitrate solution quality concentration is 10～30g/L, and addition manner adopts spraying to add, and mixing speed is at 20～200 rev/mins, and ultrasonic concussion frequency is 15～50KHz.The chemical plating useful load is 10～30g/L.
In second step, tungsten powder behind the chemical plating or tungsten-carbide powder are dried in a vacuum;
Described vacuum drying, its temperature are at 100～150 ℃, and the time is 24h;
In the 3rd step, will dry the back powder and proportionally carry out mixing and ball milling with copper powder or nickel powder;
Described mixing and ball milling, its ratio of grinding media to material are 2: 1～10: 1, and the ball milling time is 2h～20h, and rotational speed of ball-mill is 20 rev/mins～150 rev/mins.
In the 4th step, the powder compaction behind the ball milling is become blank;
Described powder compaction behind the ball milling is become blank, be meant under 100MPa～500MPa pressure the powder compaction behind the ball milling is become blank.
In the 5th step, will suppress the back blank with corresponding weight silver strip infiltration;
Described infiltration, wherein infiltrating temperature is 1000～1250 ℃, the infiltration time is determined by product thickness, thickness and time relationship: time=infiltration speed * thickness, infiltration speed is 2～5min/mm, hydrogen atmosphere or inert atmosphere protection.
The silver that the gross weight of silver-chemical plating produces in described corresponding weight=required preparation material is heavy.
The present invention can carry out surface treatment to tungsten carbide or tungsten powder earlier before carrying out above-mentioned steps, be about to tungsten carbide or tungsten powder and be soaked in rare nitric acid stirring and washing 10～30 minutes, filtered the back with washed with de-ionized water three times.
Described rare nitric acid, its mass concentration are 5%～20%.
The present invention can further carry out multiple pressure to the material behind the infiltration after above-mentioned steps five finishes.
Described multiple the pressure wherein answered pressure pressure between 200～1000MPa.
The present invention adopts liquid phase spraying addition manner to realize submicron particles surface chemistry plating Ag, and in conjunction with follow-up infiltrating method, preparation compact block composite material.Adopt liquid phase spray pattern chemical plating, can be at the even in advance coated with silver of particle surface, surface coated silver can play guiding function in follow-up infiltration process, help silvering solution evenly to enter between each submicron particles, thereby obtains the uniform tissue structure.The sub-micron WC or the W particle of small and dispersed can disperse electric arc greatly in electrically contacting use simultaneously, prevent that electric arc is concentrated, thereby make the resistance fusion welding of material to be greatly improved with the arc resistant ablation property.
Above-mentioned submicron particle reinforced Ag-based contact material provided by the invention has good mechanical and physical property, the disperse of wild phase uniform particles.Compare traditional Ag-W or Ag-WC material, because tiny high-melting-point wild phase even dispersion is distributed in the material matrix, therefore in use can keep good resistance fusion welding and lower spillage of material, thereby have longer electric life, better arc ablation resistance ability.The content of submicron particles is during greater than 80wt%, will make the material conductance descend and can not satisfy instructions for use; When submicron particles content during less than 30wt%, the resistance fusion welding energy and the arc ablation resistance performance of material are not enough to satisfy instructions for use.Therefore submicron particles content is best between 30～80wt%.Compare micron WC of conventional method preparation or the silver-based material that the W particle strengthens, the sub-micron WC of employing the present invention preparation or W particle strengthen Ag based composites resistance fusion welding energy and the arc ablation resistance rate improves more than 50%, and intensity and hardness raising are more than 50%.
Description of drawings
Fig. 1 is one embodiment of the invention preparation method flow chart
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are done one and describe in detail, following embodiment as the usefulness of understanding technical solution of the present invention, is not to be used to limit scope of the present invention just.
Submicron particle reinforced Ag-based electrical contact material described in the present embodiment, component that comprises and weight percent content thereof are: nickel (Ni)+copper (Cu)≤2%, 30%≤tungsten (W) or tungsten carbide (WC)≤80%, surplus are silver; Described tungsten carbide (WC) or tungsten (W) particle size are between 0.1～1um.
Embodiment one
With the thick Ag-WC30-1Cu-1Ni material of preparation 5mm is example
As shown in Figure 1, at first 10kg WC powder (granularity is 1 μ m) is placed 5% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.
Implement chemical plating then, powder behind the suction filtration is poured in the hydrazine hydrate solution of 500L, its concentration is 3ml/L, regulating pH value with ammoniacal liquor is 8, stir ultrasonic concussion, be that 10g/L liquor argenti nitratis ophthalmicus 500L adds with Sprayable simultaneously with concentration, mixing speed is 20 rev/mins, and ultrasonic concussion frequency is 15KHz.After treating that chemical plating is fully, suction filtration obtains the good WC powder of plating, and with deionized water rinsing three times.
Vacuumize afterwards, the WC powder that plating is good places vacuum, 100 ℃ of dryings 24 hours.
Get dry good silver-plated WC powder and 300gCu powder and 300g Ni sphere of powder mill 20h, ratio of grinding media to material 2: 1, rotational speed of ball-mill is 20 rev/mins.
Every part get 13 the gram ball millings after powder under 100MPa, suppress the acquisition pressed compact.
Carry out infiltration with the heavy Ag sheet of 17g under hydrogen atmosphere afterwards, infiltrating temperature is 1000 ℃, infiltration time=2min/mm * 5mm=10 minute.
The material that infiltration is finished is pressed under 200MPa again at last.Can obtain the Ag-WC30 material like this, material property: hardness (HB): 120; Resistivity: 2.2 μ Ω .cm; Density 11.5g/cm
3Strengthen silver-based material with traditional tungsten carbide and compare, material resistance fusion welding and arc ablation resistance raising 80%, electric life improves 50%.
Embodiment two
With preparation 10mm Ag-WC80-1Ni material is example
As shown in Figure 1, at first 30kg WC powder (granularity is 0.1 μ m) is placed 20% salpeter solution, stirring and washing 30 minutes adopts suction filtration after the washed with de-ionized water three times then.
Implement chemical plating then, powder behind the suction filtration is poured in the 500L hydrazine hydrate solution, its concentration is 6ml/L, regulating pH value with ammoniacal liquor is 10, stir ultrasonic concussion, the 500L liquor argenti nitratis ophthalmicus that with concentration is 30g/L simultaneously adds with Sprayable, and mixing speed is 200 rev/mins, and ultrasonic concussion frequency is 50KHz.After treating that chemical plating is fully, suction filtration obtains the good WC powder of plating, and with deionized water rinsing three times.
Vacuumize afterwards, the WC powder that plating is good places vacuum, 150 ℃ of dryings 24 hours.
Powder that drying is good and 375gNi sphere of powder mill 2h, ratio of grinding media to material 10: 1, rotational speed of ball-mill is 150 commentaries on classics.
Getting behind the ball milling powder 20g for every part suppresses under 500MPa and obtains pressed compact.
Carry out infiltration with 0.5 gram Ag sheet under hydrogen atmosphere afterwards, infiltrating temperature is 1250 ℃, infiltration time=5min/mm * 10mm=50 minute.
The material that infiltration is finished is pressed under 1000MPa again at last.Can obtain the Ag-WC80 material like this, material property: hardness (HB): 230; Resistivity: 4.0 μ Ω .cm; Density 15.2g/cm
3Strengthen silver-based material with traditional tungsten carbide and compare, material resistance fusion welding and arc ablation resistance raising 200%, electric life improves 180%.
Embodiment three
With preparation 20mm Ag-WC50-0.1Cu material is example
At first 15kg WC powder (granularity is 0.5 μ m) is placed 10% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.
Implement chemical plating then, the powder behind the suction filtration is poured in the 500L hydrazine hydrate solution, its concentration is 4.5ml/L, and regulating pH value with ammoniacal liquor is 9, stirs ultrasonic concussion.Be that the 15g/L liquor argenti nitratis ophthalmicus adds with Sprayable simultaneously with 500L concentration, mixing speed is 100 rev/mins, and ultrasonic concussion frequency is 30KHz.After treating that chemical plating is fully, suction filtration obtains the good WC powder of plating, and with deionized water rinsing three times.
Vacuumize afterwards, the WC powder that plating is good places vacuum, 100 ℃ of dryings 24 hours.
Powder that drying is good and 30gCu sphere of powder mill 20h, ratio of grinding media to material 2: 1, rotational speed of ball-mill is 20 commentaries on classics.
Powder is got 10g for every part and suppress the acquisition pressed compact under 100MPa behind the ball milling.
Carry out infiltration with 13 gram Ag sheets under hydrogen atmosphere afterwards, infiltrating temperature is 1100 ℃, infiltration time=2min/mm * 20mm=40 minute.
The material that infiltration is finished is pressed under 200MPa again at last.Can obtain the Ag-WC50 material like this, material property is hardness (HB): 160; Resistivity: 3.3 μ Ω .cm; Density 13.3g/cm
3Strengthen silver-based material with traditional tungsten carbide and compare, material resistance fusion welding and arc ablation resistance raising 200%, electric life improves 150%.
Embodiment four
With preparation 15mm Ag-W30-1Cu-1Ni material is example
At first 10kg W powder (granularity is 1 μ m) is placed 5% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.
Implement chemical plating then, powder behind the suction filtration is poured in the hydrazine hydrate solution of 500L, its concentration is 3ml/L, regulating pH value with ammoniacal liquor is 8, stir ultrasonic concussion, be that 10g/L liquor argenti nitratis ophthalmicus 500ml adds with Sprayable simultaneously with concentration, mixing speed is 20 rev/mins, and ultrasonic concussion frequency is 15KHz.After treating that chemical plating is fully, suction filtration obtains the good WC powder of plating, and with deionized water rinsing three times.
Vacuumize afterwards, the WC powder that plating is good places vacuum, 100 ℃ of dryings 24 hours.
Powder that drying is good and 300gCu powder and 300g Ni sphere of powder mill 20h, ratio of grinding media to material 2: 1, rotational speed of ball-mill is 20 commentaries on classics.
Powder is got the compacting under 100MPa of 13 grams for every part and is obtained pressed compact behind the ball milling.
Carry out infiltration with 17 gram Ag sheets under hydrogen atmosphere afterwards, infiltrating temperature is 1000 ℃, infiltration time=3min/mm * 15mm=45 minute.
The material that infiltration is finished is pressed under 200MPa again at last.Can obtain the Ag-W30 material like this, material property: hardness (HB): 120; Resistivity: 2.2 μ Ω .cm; Density 11.8g/cm
3Strengthen silver-based material with traditional tungsten carbide and compare, material resistance fusion welding and arc ablation resistance raising 150%, electric life improves 100%.
Embodiment five
With preparation 30mm Ag-W80-1Ni material is example
At first 30kg W powder (granularity is 0.1 μ m) is placed 20% salpeter solution, stirring and washing 30 minutes adopts suction filtration after the washed with de-ionized water three times then.
Implement chemical plating then, powder behind the suction filtration is poured in the 500L hydration callosity solution, its concentration is 6ml/L, regulating pH value with ammoniacal liquor is 10, stir ultrasonic concussion, the 500ml liquor argenti nitratis ophthalmicus that with concentration is 30g/L simultaneously adds with Sprayable, and mixing speed is 200 rev/mins, and ultrasonic concussion frequency is 50KHz.After treating that chemical plating is fully, suction filtration obtains the good WC powder of plating, and with deionized water rinsing three times.
Vacuumize afterwards, the WC powder that plating is good places vacuum, 150 ℃ of dryings 24 hours.
Powder that drying is good and 375g Ni sphere of powder mill 2h, ratio of grinding media to material 10: 1, rotational speed of ball-mill is 150 commentaries on classics.
Powder is got 20g for every part and suppress the acquisition pressed compact under 500MPa behind the ball milling.
Carry out infiltration with corresponding weight 0.5g Ag sheet under hydrogen atmosphere afterwards, infiltrating temperature is 1250 ℃, infiltration time=3min/mm * 30mm=90 minute.
The material that infiltration is finished is pressed under 1000MPa again at last.Can obtain the Ag-W80 material like this, material property: hardness (HB): 220; Resistivity: 3.8 μ Ω .cm; Density 15.5g/cm
3Strengthen silver-based material with traditional tungsten carbide and compare, material resistance fusion welding and arc ablation resistance raising 100%, electric life improves 80%.
Embodiment six
With the thick Ag-W50-0.1Cu material of preparation 25mm is example
At first 15kg WC powder (granularity is 0.5 μ m) is placed 10% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.
Implement chemical plating then, the powder behind the suction filtration is poured in the 500L hydrazine hydrate solution, its concentration is 4.5ml/L, and regulating pH value with ammoniacal liquor is 9, stirs ultrasonic concussion.Be that the 15g/L liquor argenti nitratis ophthalmicus adds with Sprayable simultaneously with 500L concentration, mixing speed is 100 rev/mins, and ultrasonic concussion frequency is 30KHz.After treating that chemical plating is fully, suction filtration obtains the good WC powder of plating, and with deionized water rinsing three times.
Vacuumize afterwards, the WC powder that plating is good places vacuum, 100 ℃ of dryings 24 hours.
Powder that drying is good and 30g Cu sphere of powder mill 20h, ratio of grinding media to material 2: 1, rotational speed of ball-mill is 20 commentaries on classics.
Powder is got 10g for every part and suppress the acquisition pressed compact under 100MPa behind the ball milling.
Carry out infiltration with 13g Ag sheet under hydrogen atmosphere afterwards, infiltrating temperature is 1000 ℃, infiltration time=3min/mm * 25mm=75 minute.
The material that infiltration is finished is pressed under 200MPa again at last.Can obtain the Ag-W50 material like this, material property is hardness (HB): 150; Resistivity: 3.0 μ Ω .cm; Density 13.5g/cm
3, strengthen silver-based material with traditional tungsten carbide and compare, material resistance fusion welding and arc ablation resistance raising 100%, electric life improves 80%.
Claims (9)
1. a submicron particle reinforced Ag-based electrical contact material is characterized in that, component that comprises and weight percent content thereof are: 0.1%≤nickel≤2%, 0.1%≤copper≤2%, 30%≤tungsten or tungsten carbide≤80%, surplus are silver; This material adopts liquid phase spraying addition manner to realize submicron particles surface chemistry plating Ag, prepares through follow-up infiltrating method again.
2. submicron particle reinforced Ag-based electrical contact material as claimed in claim 1 is characterized in that, described tungsten carbide or tungsten powder granularity are between 0.1～1um.
3. the preparation method of a submicron particle reinforced Ag-based electrical contact material as claimed in claim 1, it is characterized in that, at first adopt chemical plating method at sub-micron tungsten or tungsten carbide W particle surface coated with silver, suppress infiltrating method then and prepare fine and close sub-micron hard-phase particles enhancing silver-based composite material, wherein:
Described chemical plating method, its plating mode adopts ultrasonic concussion to combine with stirring; The chemical plating reducing solution is a hydrazine hydrate solution, and volumetric concentration is 3～6ml/L, adopts ammoniacal liquor to regulate acidity-basicity ph value between 8～10; Main salt silver nitrate solution quality concentration is 10～30g/L, and addition manner adopts spraying to add, and the chemical plating useful load is 10-30g/L;
Described compacting infiltrating method is under 100MPa～500MPa pressure the powder compaction behind the ball milling to be become blank; Infiltrating temperature is 1000～1250 ℃, and infiltration speed is 2～5min/mm, hydrogen atmosphere or inert atmosphere protection.
4. the preparation method of submicron particle reinforced Ag-based electrical contact material as claimed in claim 3 is characterized in that, carries out according to following steps:
The first step is carried out chemical plating with tungsten carbide or tungsten powder;
In second step, tungsten powder behind the chemical plating or tungsten-carbide powder are dried in a vacuum;
In the 3rd step, will dry the back powder and proportionally carry out mixing and ball milling with copper powder or nickel powder;
In the 4th step, the powder compaction behind the ball milling is become blank;
In the 5th step, will suppress the back blank with corresponding weight silver strip infiltration; The silver that the gross weight of silver-chemical plating produces in described corresponding weight=required preparation material is heavy.
5. the preparation method of submicron particle reinforced Ag-based electrical contact material as claimed in claim 4 is characterized in that, in the first step, mixing speed is at 20～200 rev/mins, and ultrasonic concussion frequency is 15～50KHz.
6. the preparation method of submicron particle reinforced Ag-based electrical contact material as claimed in claim 4 is characterized in that, in second step, and described vacuum drying, its temperature is at 100～150 ℃, and the time is 24h.
7. the preparation method of submicron particle reinforced Ag-based electrical contact material as claimed in claim 4 is characterized in that, in the 3rd step, described mixing and ball milling, its ratio of grinding media to material is 2: 1～10: 1, and the ball milling time is 2h～20h, and rotational speed of ball-mill is 20 rev/mins～150 rev/mins.
8. the preparation method of submicron particle reinforced Ag-based electrical contact material as claimed in claim 4, it is characterized in that, before carrying out described step 1, earlier tungsten carbide or tungsten powder were soaked in rare nitric acid stirring and washing 10～30 minutes, filter the back with washed with de-ionized water three times.
9. the preparation method of submicron particle reinforced Ag-based electrical contact material as claimed in claim 4 is characterized in that, after above-mentioned steps five finishes, further the material behind the infiltration is carried out multiple pressure, and described multiple pressure pressure is between 200～1000MPa.
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