CN107633960B - A kind of sheet iron reticulates the Ag-based electrical contact material and preparation method thereof of distribution reinforcing - Google Patents
A kind of sheet iron reticulates the Ag-based electrical contact material and preparation method thereof of distribution reinforcing Download PDFInfo
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- CN107633960B CN107633960B CN201710812040.XA CN201710812040A CN107633960B CN 107633960 B CN107633960 B CN 107633960B CN 201710812040 A CN201710812040 A CN 201710812040A CN 107633960 B CN107633960 B CN 107633960B
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
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Abstract
The present invention relates to a kind of sheet iron to reticulate the Ag-based electrical contact material and preparation method thereof that distribution is strengthened, and belongs to electrical contact material technical field.Main technical schemes are as follows: Ag-based electrical contact material includes silver: 80wt%-98wt%；Iron: 2wt%-20wt%；It is female salting liquid with silver nitrate and ferrous nitrate, oxalic acid precipitation agent solution is added dropwise, it is centrifuged after being stirred to react and washs acquisition sediment, after baking oven drying, silver-iron composite powder body that iron is sheet-like morphology is obtained through air calcination and hydrogen reducing, composite granule injection graphite jig is finally subjected to discharge plasma sintering and obtains silver-iron contact material.Since continuous sheet iron forms net distribution, silver enhances the load transmission effect of iron in plastic deformation, can be obtained the silver-based composite material of longer fibers iron reinforcing under lower true strain.
Description
Technical field
The present invention relates to a kind of sheet iron to reticulate the Ag-based electrical contact material and preparation method thereof that distribution is strengthened, and belongs to electricity
Contact material technical field.
Background technique
Electrical contact material is the base components of mechanical switch electric appliance, although under itself equilibrium state, silver and iron two are mutual
Immiscible, silver-ferroelectricity contact material contact resistance is stablized, and anti-scorching, resistance fusion welding and wearability are good.Relative to silver-
Nickel electric contact, silver-iron composite material not only have in price and have great advantage, and also show more in heavy load A.C. contactor
Good resistance fusion welding energy.Usual silver-iron composite electric contact material mostly uses coprecipitation method, and it is uniform to obtain two kinds of silver, iron elements
Mixed carbonate or hydroxide obtains the mixed uniformly silver-iron composite material of two-phase through air calcination and hydrogen reducing,
In the second phase iron be mostly tiny graininess.Under arcing, silver forms melt, and part iron, which dissolves in, forms solution in silver, change
The fluid and thermal property of kind melt alleviate contact failure to reduce melt splash.But the tiny granular iron in part is because of density
It is lower, it is easy to float to contact surface, and aoxidize, contact resistance is caused to rise, and accelerate contact electricity failure procedure.
The advantage of fibre strengthening Ag-based electrical contact material is verified extensively: on the one hand, the second phase of fiber (is especially hung down
When straight contact surface aligns) it is less to the scattering process of conduction electrons, advantageously ensure that the higher electric conductivity of contact；It is another
Aspect, dystectic fibrous second phase one end are pinned at matrix, and the second phase can be effectively suppressed to the stabilization of fiber in matrix
The effects of floating, the second phase fiber being stabilized passes through capillary absorption, improves molten bath viscosity etc., so that the electricity for improving contact connects
Touch the service life.It prepares fiber alignment reinforcing silver-ferroelectricity contact material by large plastometric set to be widely used, general side
Method is to carry out large plastometric set to silver-ferroelectricity contact material of the granular iron even dispersion of co-precipitation preparation, through excessive modeling
Property deformation after, the raw cooperative transformation of granular iron and silver hair, iron particle is elongated along plastic deformation direction, forms iron fiber.In electric arc
Under effect, compared with granular iron, fibrous iron can more preferable stabilised bath, to improve the working life of contact.Due to iron
Elasticity modulus and yield strength are all apparently higher than silver, thus in the initial stage of plastic deformation, the second phase iron is only along silver-colored crystal boundary stream
Dynamic or generation flexible deformation, only when true strain is higher, iron is just plastically deformed, and forms long fibre.Therefore, in order to obtain length
Fiber strengthened silver-ferroelectricity contact needs to carry out the plastic deformation of higher true strain, and this aspect improves processing intensity, another
Aspect also improves nickel because probability is replied in the heat etching occurred in processing, therefore limits the length of nickel fiber.
Summary of the invention
To make up the deficiencies in the prior art, the present invention provides a kind of sheet iron and reticulates the Ag-based electrical contact material that distribution is strengthened
Material and preparation method thereof.Iron is sheet-like morphology in silver-ferroelectricity contact material of this method preparation, and is in net distribution.To we
When the electrical contact material of method preparation carries out large plastometric set, the silver that longer iron fiber is strengthened can be obtained under the conditions of lower true strain
Base electric contact material.
Technical scheme is as follows: a kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing, including such as
The material of lower mass percent:
Silver: 80wt%-98wt%；
Iron: 2wt%-20wt%；
The material is prepared as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in proportion, and are added to the water to obtain female salting liquid；
Step 2: configuration oxalic acid solution precipitating reagent；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, uniform stirring adjusts pH while reaction
It is worth appropriate section, filters and separate and wash to obtain sediment；
Step 4: putting the precipitate in dry in baking oven；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined, silver-iron oxide composite granule is obtained；
Step 6: silver-iron oxide composite granule being restored in hydrogen atmosphere to obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material.
Further, silver nitrate in the step 1, ferrous nitrate concentration be 0.001-1mol/L.
Further, the step 2 medium-height grass acid solutions are 0.001-1mol/L, the molar ratio of oxalic acid and metal ion
For (1:2)-(8:1), the metal ion includes silver ion and ferrous ion.
Further, precipitation reaction in the step 3, titration speed 1-100ml/min, reaction temperature are 20-80 DEG C,
Reaction time is 0.5-4h, pH value 0-4.
Further, step 4 drying temperature is 40-200 DEG C, time 4-48h.
Further, step 5 calcination temperature is 300-800 DEG C, time 1-4h.
Further, the step 6 hydrogen atmosphere reduction: calcination temperature is 300-700 DEG C, recovery time 15-
120min。
Further, step 7 discharge plasma sintering: sintering temperature is 400-800 DEG C, briquetting pressure 20-
120MPa, soaking time 5-60min.
The preparation method that a kind of sheet iron reticulates the Ag-based electrical contact material that distribution is strengthened is claimed in the present invention simultaneously,
Include the following steps:
Step 1: silver nitrate and ferrous nitrate being weighed in proportion, and are added to the water to obtain female salting liquid；The silver ion
Mass percent be 80wt%-98wt%；The mass percent of the ferrous ion are as follows: 2wt%-20wt%；
Step 2: configuration oxalic acid solution precipitating reagent；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, uniform stirring adjusts pH while reaction
It is worth appropriate section, filters and separate and wash to obtain sediment；
Step 4: putting the precipitate in dry in baking oven；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined, silver-iron oxide composite granule is obtained；
Step 6: silver-iron oxide composite granule being restored in hydrogen atmosphere to obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material.
Beneficial effects of the present invention are as follows: the present invention utilizes the heavy of silver oxalate and ferrous oxalate using positive titration method
Deposit difference carries out difference precipitating, successively obtains the silver oxalate of sheet and depends on the sheet ferrous oxalate grown on it, through air
Sheet iron pattern can be kept substantially with the calcining of two step of hydrogen.Using gained silver-iron composite powder body as raw material, can be obtained after hot pressed sintering
Continuous sheet iron is in silver-ferroelectricity contact material of net distribution, and the thickness of sheet iron is in 0.05-1 μ m.Due to serialgram
Shape iron forms net distribution, and silver enhances the load transmission effect of iron in plastic deformation, can be obtained under lower true strain
The silver-based composite material that longer fibers iron is strengthened.
Specific embodiment
The present invention is further described combined with specific embodiments below, if material of the present invention is without specified otherwise, equal city
Selling can obtain.
Embodiment 1
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 88wt%；Iron
Mass percent is 12wt%.The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.001mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.01mol/L, oxalic acid and metal ion
Molar ratio is 1:1；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 1ml/min adjusts pH
It is worth 1, reacts 0.5h in 20 DEG C of uniform stirrings, filter and separate and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 80 DEG C of dry 48h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 400 DEG C, it is multiple to obtain silver-iron oxide by time 2h
Close powder；
Step 6: in hydrogen atmosphere, 300 DEG C of recovery time 60min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 400 DEG C, briquetting pressure 30MPa, soaking time 40min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.1 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 2
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 90wt%；Iron
Mass percent is 10wt%.The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.005mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.005mol/L, oxalic acid and metal ion
Molar ratio be 2:1；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 5ml/min adjusts pH
It is worth 2, reacts 1h in 50 DEG C of uniform stirrings, filter and separate and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 40 DEG C of dry 38h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 600 DEG C, it is multiple to obtain silver-iron oxide by time 3h
Close powder；
Step 6: in hydrogen atmosphere, 400 DEG C of recovery time 15min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 500 DEG C, briquetting pressure 40MPa, soaking time 30min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.5 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 3
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 95wt%；Iron
Mass percent is 5wt%.The preparation method comprises the following steps:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.1mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.1mol/L, oxalic acid and metal ion
Molar ratio is 4:1；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 10ml/min is adjusted
PH value reacts 3h to 2.5, in 40 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 60 DEG C of dry 44h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 800 DEG C, it is multiple to obtain silver-iron oxide by time 1h
Close powder；
Step 6: in hydrogen atmosphere, 300 DEG C of recovery time 90min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 600 DEG C, briquetting pressure 70MPa, soaking time 60min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 1 micron, and in silver
It is formed in matrix continuous net-shaped.
Embodiment 4
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 98wt%；Iron
Mass percent is 2wt%.The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.5mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.3mol/L, oxalic acid and metal ion
Molar ratio is 1:2；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 100ml/min is adjusted
PH value reacts 1h to 1.5, in 80 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven and dried for 24 hours at 80 DEG C；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 600 DEG C, it is multiple to obtain silver-iron oxide by time 4h
Close powder；
Step 6: in hydrogen atmosphere, 400 DEG C of recovery time 30min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 700 DEG C, briquetting pressure 20MPa, soaking time 60min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.05 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 5
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 94%；The matter of iron
Measuring percentage is 6%；The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.02mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.02mol/L, oxalic acid and metal ion
Molar ratio is 7:1；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 50ml/min is adjusted
PH value reacts 4h to 4, in 50 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 120 DEG C of dry 8h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 700 DEG C, it is multiple to obtain silver-iron oxide by time 2h
Close powder；
Step 6: in hydrogen atmosphere, 600 DEG C of recovery time 70min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 450 DEG C, briquetting pressure 90MPa, soaking time 60min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.2 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 6
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 84wt%；Iron
Mass percent is 16wt%；The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.05mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.05mol/L, oxalic acid and metal ion
Molar ratio is 7:2；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 20ml/min is adjusted
PH value reacts 4h to 3, in 70 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 150 DEG C of dry 14h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 500 DEG C, it is multiple to obtain silver-iron oxide by time 4h
Close powder；
Step 6: in hydrogen atmosphere, 600 DEG C of recovery time 50min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 400 DEG C, briquetting pressure 70MPa, soaking time 20min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.15 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 7
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 80wt%；Iron
Mass percent is 20wt%；The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.8mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.3mol/L, oxalic acid and metal ion
Molar ratio is 5:2；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 5ml/min adjusts pH
It is worth 3.5, reacts 2h in 60 DEG C of uniform stirrings, filter and separate and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 180 DEG C of dry 12h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 600 DEG C, it is multiple to obtain silver-iron oxide by time 3h
Close powder；
Step 6: in hydrogen atmosphere, 300 DEG C of recovery time 100min obtain silver-iron composite powder body；Step 7: by gained
Silver-iron composite powder body injects graphite jig, obtains blocky silver-ferroelectricity contact material, sintering temperature 800 by plasma discharging
DEG C, briquetting pressure 20MPa, soaking time 5min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.3 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 8
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 86wt%；Iron
Mass percent is 14wt%.The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.12mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 1mol/L, and oxalic acid and metal ion rub
You are than being 3:2；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 70ml/min is adjusted
PH value reacts 2.5h to 3.5, in 50 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 120 DEG C of dry 28h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 450 DEG C, it is multiple to obtain silver-iron oxide by time 4h
Close powder；
Step 6: in hydrogen atmosphere, 500 DEG C of recovery time 40min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 600 DEG C, briquetting pressure 30MPa, soaking time 5min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.5 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 9
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 92wt%；Iron
Mass percent is 8wt%.The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and are added to the water
Female salting liquid is obtained, wherein silver nitrate concentration is 0.002mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.001mol/L, oxalic acid and metal ion
Molar ratio be 8:1；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 90ml/min is adjusted
PH value reacts 1.5h to 0, in 30 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 200 DEG C of dry 4h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 300 DEG C, it is multiple to obtain silver-iron oxide by time 4h
Close powder；
Step 6: in hydrogen atmosphere, 700 DEG C of recovery time 20min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 650 DEG C, briquetting pressure 120MPa, soaking time 50min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.7 micron, and
It is formed in silver matrix continuous net-shaped.
Embodiment 10
A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing: silver-colored mass percent is 82wt%；Iron
Mass percent is 18wt%.The preparation method is as follows:
Step 1: silver nitrate and ferrous nitrate being weighed in the ratio of silver and iron in silver-iron contact material, and solution is added
In obtain female salting liquid, wherein silver nitrate concentration be 0.02mol/L；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.5mol/L, oxalic acid and metal ion
Molar ratio is 6:1；
Step 3: oxalic acid solution titration being added in female salting liquid and is precipitated, titration speed 30ml/min is adjusted
PH value reacts 0.5h to 0.5, in 80 DEG C of uniform stirrings, filters and separates and wash to obtain sediment；
Step 4: putting the precipitate in baking oven in 100 DEG C of dry 20h；
Step 5: the sediment after drying being transferred to Muffle furnace and is calcined at 550 DEG C, time 2.5h obtains silver-iron oxide
Composite granule；
Step 6: in hydrogen atmosphere, 300 DEG C of recovery time 120min obtain silver-iron composite powder body；
Step 7: gained silver-iron composite powder body being injected into graphite jig, blocky silver-ferroelectricity is obtained by plasma discharging and is touched
Head material, sintering temperature are 750 DEG C, briquetting pressure 50MPa, soaking time 25min.
Iron is sheet-like morphology in silver-tin electrical contact material manufactured in the present embodiment, and thickness is about 0.9 micron, and
It is formed in silver matrix continuous net-shaped.
Claims (1)
1. the preparation method that a kind of sheet iron reticulates the Ag-based electrical contact material that distribution is strengthened, which is characterized in that including as follows
Step:
Step 1: being that the silver nitrate of 0.001-1mol/L and ferrous nitrate weigh in proportion, and are added to the water to obtain mother by concentration
Salting liquid, the mass percent of the silver ion are 80wt%-98wt%；The mass percent of the ferrous ion are as follows: 2wt%-
20wt%；
Step 2: configuration oxalic acid solution precipitating reagent, wherein oxalic acid solution concentration is 0.001-1mol/L, oxalic acid and metal ion
Molar ratio is (1:2)-(8:1), and the metal ion includes silver ion and ferrous ion；
Step 3: oxalic acid solution being added to mother with 1-100 ml/min titration speed under conditions of reaction temperature is 40-80 DEG C
It is adjusted after salting liquid after pH value reacts 0.5-4h to 0-4 and filters separation, carried out using the precipitating product moment of silver oxalate and ferrous oxalate
Difference precipitating successively obtains the silver oxalate of sheet and depends on the sheet ferrous oxalate sediment grown on it, and to sediment
It is washed；
Step 4: putting the precipitate in drying in baking oven, drying temperature is 40-200 DEG C, time 4-48h；
Step 5: the sediment after drying being transferred at Muffle furnace is 300-500 DEG C in calcination temperature and calcines 1-4h, obtains silver-oxygen
Change iron composite powder body；
Step 6: silver-iron oxide composite granule being restored in hydrogen atmosphere to obtain silver-iron composite powder body, calcination temperature is
300-700 DEG C, recovery time 15-120min；
Step 7: gained silver-iron composite powder body being injected into graphite jig, is 400-800 DEG C in temperature, pressure is 20-120MPa's
Under the conditions of reaction 5-60min obtain blocky silver-ferroelectricity contact material.
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| CN201710812040.XA CN107633960B (en) | 2017-09-11 | 2017-09-11 | A kind of sheet iron reticulates the Ag-based electrical contact material and preparation method thereof of distribution reinforcing |
| CN201711358070.4A CN108054031B (en) | 2017-09-11 | 2017-09-11 | A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing |
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| CN201710812040.XA CN107633960B (en) | 2017-09-11 | 2017-09-11 | A kind of sheet iron reticulates the Ag-based electrical contact material and preparation method thereof of distribution reinforcing |
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| CN201711358070.4A Active CN108054031B (en) | 2017-09-11 | 2017-09-11 | A kind of sheet iron reticulates the Ag-based electrical contact material of distribution reinforcing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1058289A (en) * | 1990-07-20 | 1992-01-29 | 安徽省机械科学研究所 | A kind of manufacture method of Ag-based electrical contact material |
| DE19607183C1 (en) * | 1996-02-27 | 1997-04-10 | Degussa | Sintered silver@-iron@ alloy for making electrical contacts |
| CN100452259C (en) * | 2006-03-17 | 2009-01-14 | 乐百令 | Silver-nickel electric contact producing technology |
| CN101823153A (en) * | 2009-03-06 | 2010-09-08 | 五邑大学 | Technology for preparing flake nano silver with overlarge area |
| CN102737863B (en) * | 2012-07-03 | 2015-01-28 | 扬州乐银合金科技有限公司 | Silver nickel graphite composite contact terminal material and processing method thereof |
| CN103996426B (en) * | 2014-05-28 | 2016-05-11 | 东北大学 | Silver-colored nickel composite electric contact material of a kind of nickel net distribution and preparation method thereof |
| CN104505287B (en) * | 2014-12-22 | 2017-10-24 | 东北大学 | A kind of Ag-based electrical contact material preparation method of bar-shaped tin oxide reinforcing |
| CN104439249A (en) * | 2014-12-30 | 2015-03-25 | 桂林电器科学研究院有限公司 | Method for processing sheet silver nickel electric contact material |
| CN104493177A (en) * | 2014-12-30 | 2015-04-08 | 桂林电器科学研究院有限公司 | Preparation method of flakey silver and tungsten electrical contact material |
| CN104475733A (en) * | 2014-12-30 | 2015-04-01 | 桂林电器科学研究院有限公司 | Preparation method of flake-like silver-nickel-tungsten electrical contact material |
| CN105268992B (en) * | 2015-11-20 | 2018-07-31 | 浙江海洋学院 | A kind of netted two-dimensional sheet silver powder and its liquid-phase synthesis process |
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| CN108054031A (en) | 2018-05-18 |
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