CN103589897B - Preparation method of siluer metal oxide tungsten composite electric contact material and products thereof - Google Patents
Preparation method of siluer metal oxide tungsten composite electric contact material and products thereof Download PDFInfo
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- CN103589897B CN103589897B CN201310601397.5A CN201310601397A CN103589897B CN 103589897 B CN103589897 B CN 103589897B CN 201310601397 A CN201310601397 A CN 201310601397A CN 103589897 B CN103589897 B CN 103589897B
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Abstract
The invention discloses preparation method of a kind of siluer metal oxide wolfram varbide composite electric contact material and products thereof, its technical scheme includes contact body and welding silver layer, and this contact body comprises following component: metal oxide 1-25%, wolfram varbide 0.05 ~ 12%, additive≤5%, surplus is silver.The advantage that the present invention has and positively effect: 1, in AgMeO contact material, add WC, can significantly improve the resistance fusion welding of contact, improves the reliability of contactor; 2, select the AgMeOWC contact material of proper composition, AgMeO contact material can be substituted in miniature circuit breaker and protection switch, improve anti-electric-arc scaling loss ability and the resistance fusion welding energy of contact, reduce contact silver content simultaneously, play certain joint silver effect etc.
Description
Technical field
The present invention relates to a kind of production method of Contact Materials for Low Voltage Electric Apparatus, refer in particular to a kind of siluer metal oxide tungsten (
agMeOW) preparation method and products thereof of composite electric contact material.
Background technology
In current low voltage electrical apparatus industry large mainly with silver-based material as electrical contact material, and wherein siluer metal oxide (AgMeO, Me refers to metal) material has the comprehensive electrochemical properties of excellent anti electric arc corrosion, resistance fusion welding and low and stable contact resistance due to it, occupies an important position in whole electrical contact material system.In electrical contact contact process, the melting welding between contact is one of its main failure forms.The method of common raising material resistance fusion welding energy improves the content of refractory oxide composition in material, or make oxide particle be that needle-like separates out (needle-like direction is perpendicular to working face).But scheme reduces the conductivity of material for a moment, and the limitation that can improve; Scheme two can realize in internal oxidation process material, but is but difficult to realize in powder metallurgic method (comprising preoxidation and powder mixing method) technique.Because the wettability between MeO and solder and copper alloy is poor, AgMeO electrical contact material needs to increase one deck welding silver layer at face of weld in the course of processing, normally realizes AgMeO layer and the combination of welding between silver layer by method hot rolling mode.
AgW is also a kind of electrical contact material, because the fusing point of W is up to 3422 DEG C, has excellent resistance fusion welding, be generally used in isolating switch when disjunction big current.
Summary of the invention
The object of the invention is the shortcoming and defect existed to overcome prior art, and a kind of preparation method of siluer metal oxide tungsten composite electric contact material is provided, the siluer metal oxide tungsten composite electric contact material prepared by the method has fully utilized siluer metal oxide and tungsten (W) two kinds of contact materials advantage separately, improve the resistance fusion welding energy of electrical contact material, make it have and apply widely.
Another object of the present invention there is provided a kind of siluer metal oxide tungsten composite electric contact material utilizing aforesaid method to prepare.Compare siluer metal oxide electric contact material, improve resistance fusion welding, and adopt aforesaid method to be joined uniformly by W in AgMeO body material, W particle can not melt in electrical arc erosion process, when there is welding tendency in contact, equally distributed high-melting-point W particle can play the effect reducing melting welding power between contact, and the contact of melting welding is easily broken, thus improves the resistance fusion welding energy of contact.
For realizing first object of the present invention, technical scheme of the present invention is the siluer metal oxide tungsten composite electric contact material that this is prepared is small-size flaky contact material, comprises following operation:
(1) mixed powder configuration, adopts pre-oxidation process to prepare siluer metal oxide powder and additive powder, then siluer metal oxide powder, additive powder is mixed with tungsten powder; Or directly Ag powder, metal oxide powder, tungsten powder, additive powder are mixed; Each constituent mass ratio in this mixed powder is:
Metal oxide 1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver;
(2) in the rubber coating of a closed bottom, longitudinally dividing plate is inserted, the inner chamber of rubber coating is made to be separated into large room and cell, large room A controls at 7:1 ~ 10:1 with the radial height ratio of cell B, the mixed powder that step (1) configures is loaded large room, shaping for welding silver layer silver powder is loaded cell, extract dividing plate out, overall spindle is pressed in equal pressing equipment, spindle diameter control at 80 ~ 120mm, cut to lengthen at 200 ~ 500mm, hydrostatic pressure 50 ~ 300MPa;
(3) spindle is under atmosphere protection condition, and 600 ~ 900 DEG C sinter 1 ~ 6 hour, presses again in isostatic cool pressing equipment or hydropress, multiple pressure pressure 20 ~ 300MPa;
(4) spindle is under atmosphere protection condition, is squeezed into band, extrusion strip width 20 ~ 70mm, thickness 2 ~ 10mm 600 ~ 900 DEG C of heating after 1 ~ 6 hour;
(5) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, Process Annealing once or once more than, adopt atmosphere protection during annealing, temperature 300 ~ 800 DEG C, 0.5 ~ 8 hour time;
(6) itemize-dicing method is adopted to obtain finished product contact; Or adopt mould punching method to obtain finished product contact.
Technical scheme of the present invention can also be the siluer metal oxide tungsten composite electric contact material that this is prepared is large-scale sheet contact material, comprises following operation:
(1) mixed powder preparation, adopts pre-oxidation process to prepare siluer metal oxide powder and additive powder, then siluer metal oxide powder, additive powder and tungsten powder is mixed; Or directly Ag powder, metal oxide powder, tungsten powder, additive powder are mixed; Each constituent mass ratio in this mixed powder is:
Metal oxide 1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver;
(2) granulate, mixed powder prepared by step (1) is put into ball-grinding machine ball milling 2 ~ 24 hours;
(3) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 65% ~ 85%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 5% ~ 30% of contact total thickness;
(4) first pressing pressed compact sinters 2 ~ 5 hours in 600 ~ 900 DEG C under protective atmosphere condition;
(5) pressed compact after sintering is suppressed into finished product contact in multiple compression mould, multiple pressure pressure 6 ~ 14T/cm
2.
For realizing another object of the present invention, technical scheme of the present invention comprises following component, and include contact body and welding silver layer, this contact body comprises following component:
Metal oxide 1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver.
Concrete as this programme, comprises following several scheme,
Scheme 1 comprises following component, by percentage to the quality:
CdO1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver,
Wherein additive comprises following component, in mass fraction:
NiO0.1~0.5；SnO
20.05~2.0；ZnO0.01~2.5；
Bi
2O
30.01~2.5；TeO
20.1~2.5；Sb
2O
30.01~1.0；CuO0.01~2.5。Scheme 2 comprises following component, by percentage to the quality:
SnO
21-15%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver,
Wherein additive comprises following component, in mass fraction:
NiO0.1~0.5；WO
30.05~2.0；ZnO0.01~2.5；Bi
2O
30.01~2.5；TeO
20.1~2.5；Sb
2O
30.01~1.0；CuO0.01~2.5；In
2O
30.1~5.0；MoO
30.05~2.0。
Scheme 3 comprises following component, by percentage to the quality:
ZnO1-20%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver,
Wherein additive comprises following component, in mass fraction:
NiO0.1~0.5；WO
30.05~2.0；CuO0.01~2.5；Bi
2O
30.01~2.5；
TeO
20.1~2.5；Sb
2O
30.01~1.0；SnO
20.01~2.0；MoO
30.05~2.0。
Scheme 4 comprises following component, by percentage to the quality:
CuO1-20%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver,
Wherein additive comprises following component, in mass fraction:
NiO0.1~0.5；WO
30.05~2.0；ZnO0.01~2.5；Bi
2O
30.01~2.5；
TeO
20.1~2.5；Sb
2O
30.01~1.0；SnO
20.01~2.0；MoO
30.05~2.0。
The present invention adopts powder metallurgic method to be joined uniformly by W in AgMeO body material, W particle can not melt in electrical arc erosion process, when there is welding tendency in contact, equally distributed high-melting-point W particle can play the effect reducing melting welding power between contact, the contact of melting welding is easily broken, thus improves the resistance fusion welding energy of contact.
In addition, because AgMeOW electrical contact material needs to increase one deck welding silver layer at face of weld equally, due to containing a certain amount of W, this type material is poor with the AgMeO material phase specific plastic of same oxygen U content.When adopting preoxidation or powder mixing method to produce small dimension contact, because the plasticity of body material is poor, traditional hot rolling compounding method is adopted to carry out multiple silver, for ensureing that bonding strength deformation of one time needs to reach more than 50%, AgMeOW layer and can crack and affect material use efficiency and follow-up processing.The present invention adopts the mode of rubber coating to realize multiple silver, because between base layer and silver layer powder, contact area is large, by heating the crimp of rear aximal deformation value, making to realize atomic diffusion between body material and silver layer, achieving AgMeOW layer and the metallurgical binding of welding silver layer.
The advantage that the present invention has and positively effect: 1, in AgMeO contact material, add W, can significantly improve the resistance fusion welding of contact, improves the reliability of contactor, isolating switch; 2, substitute AgMeO material, there is certain joint silver effect; 3, adopt the multiple silver of pressed by powder-extrusion process, the bonding strength between welding silver layer and AgMeOW body material is firm, silver layer distribution uniform, solves the problem of the multiple silver difficulty of extrusion process AgMeOW contact material; 4, the operational path of the present invention's design is simple, and material use efficiency is high, with short production cycle, is applicable to producing in enormous quantities.
Below in conjunction with specification drawings and specific embodiments, the present invention is described further.
Accompanying drawing explanation
The rubber coating structure iron that Fig. 1 present invention process is used:
The cross-sectional figure of rubber coating that Fig. 2 present invention process is used;
In figure A be large room, B be cell, 1 for rubber coating, 2 is dividing plate.
Embodiment
Below by embodiment, the present invention is specifically described; only be used to further illustrate the present invention; can not be interpreted as limiting the scope of the present invention, the technician in this field can make some nonessential improvement and adjustment according to the content of foregoing invention to the present invention.
Embodiment one:
A) adopt pre-oxidation process to prepare AgCdO(12)+additive powder, then by AgCdO(12) the W powder of+additive powder and weight percent 1% altogether 25kg load to mix in powder machine and mix 6 hours.Wherein additive comprises the NiO powder of weight percent 0.15%, the SnO of 1.5%
2powder.
B) at isostatic cool pressing equipment rubber coating median septum dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 9:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 100mm, length 300mm, hydrostatic pressure 150MPa.
C) spindle is under argon shield condition, and 800 DEG C sinter 6 hours, multiple pressure in cold isostatic press, multiple pressure pressure 150MPa.
D) spindle is under argon shield condition, and 850 DEG C of heating were squeezed into band, extrusion strip width 70mm, thickness 3mm after 2 hours.
E) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to the annealing of 1.5mm thickness once, adopts argon shield, temperature 700 DEG C, 0.5 hour time during annealing.
F) itemize-dicing method is adopted to obtain 3.8 × 3.8 × 0.8mm specification finished product contact.
Embodiment two:
A) adopt pre-oxidation process to prepare AgCdO(22)+additive powder, then by AgCdO(22) the W powder of+additive powder and weight percent 0.5% altogether 25kg load to mix in powder machine and mix 8 hours.Wherein additive comprises the ZnO powder of weight percent 0.6%, the NiO powder of 0.1%, the CuO powder of 1.5%.
B) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 8:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 90mm, length 400mm, hydrostatic pressure 200MPa.
C) spindle is under argon shield condition, and 900 DEG C sinter 2 hours, multiple pressure in hydropress, multiple pressure pressure 30MPa.
D) spindle is under nitrogen protection condition, and 750 DEG C of heating were squeezed into band, extrusion strip width 60mm, thickness 8mm after 3 hours.
E) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts argon shield, temperature 300 DEG C, 4 hours time during annealing.
F) mould punching method is adopted to obtain Φ 6 × 1.2mm specification finished product contact.
Embodiment three:
A) directly by 21.625kgAg powder, 3.0kgCdO powder, 0.25kgW powder, 0.025kgNiO powder, 0.050kgTeO
2powder, 0.050kgSnO
2powder loads in mixed powder machine and mixes 10 hours.
B) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 7:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 95mm, length 350mm, hydrostatic pressure 220MPa.
C) spindle is under argon shield condition, and 850 DEG C sinter 4 hours, multiple pressure in hydropress, multiple pressure pressure 30MPa.
D) spindle is under argon shield condition, and 700 DEG C of heating were squeezed into band, extrusion strip width 70mm, thickness 8mm after 2 hours.
E) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2.5mm thickness, adopts nitrogen protection, temperature 450 DEG C, 1 hour time during annealing.
F) mould punching method is adopted to obtain Φ 10 × 2SR50mm specification finished product contact.
Embodiment four:
A) directly by mixing in 21.125kgAg powder, 3.75kgCdO powder, the mixed powder machine of 0.125kgW powder loading 6 hours.
B) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 10:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 110mm, length 400mm, hydrostatic pressure 300MPa.
C) spindle is under nitrogen protection condition, and 600 DEG C sinter 6 hours, multiple pressure in isostatic pressing machine, multiple pressure pressure 250MPa.
D) spindle is under nitrogen protection condition, and 800 DEG C of heating were squeezed into band, extrusion strip width 50mm, thickness 4mm after 1.5 hours.
E) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, anneals once, adopt argon shield, temperature 500 DEG C, 1 hour time during annealing when being cold-rolled to 2mm thickness.
F) itemize-dicing method is adopted to obtain 3.5 × 3.5 × 1.0mm specification finished product contact.
Embodiment five:
A) directly by mixing in 20.875kgAg powder, 3.75kgCdO powder, 0.25kgW powder, 0.025kgNiO powder, the mixed powder machine of 0.100kgZnO powder loading 2 hours.
B) mixed powder puts into ball-grinding machine ball milling 3 hours, granulates.
C) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 75%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 15% of contact total thickness.
D) first pressing pressed compact sinters 2 hours in 800 DEG C under argon shield condition.
A) pressed compact after sintering is suppressed into Φ 10 × 2mm finished product contact in multiple compression mould, multiple pressure pressure 8T/cm
2.
Embodiment six:
A) adopt pre-oxidation process to prepare AgCdO(15)+additive powder, then by AgCdO(15) the W powder of+additive powder and weight percent 0.1% altogether 25kg load to mix in powder machine and mix 6 hours.Wherein additive comprises the CuO powder of weight percent 0.5%, the SnO of 2.0%
2powder.
B) mixed powder puts into ball-grinding machine ball milling 6 hours, granulates.
C) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 80%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 14% of contact total thickness.
D) first pressing pressed compact sinters 4 hours in 850 DEG C under nitrogen protection condition.
E) pressed compact after sintering is suppressed into 20 × 15 × 4mm finished product contact in multiple compression mould, multiple pressure pressure 10T/cm
2.
Embodiment seven:
G) pre-oxidation process is adopted to prepare AgSnO
2(10)+additive powder, then by AgSnO
2(10) the common 25kg of W powder of+additive powder and weight percent 0.5% loads in mixed powder machine and mixes 4 hours.
H) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 9:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 100mm, length 300mm, hydrostatic pressure 150MPa.
I) spindle is under argon shield condition, and 800 DEG C sinter 6 hours, multiple pressure in cold isostatic press, multiple pressure pressure 150MPa.
J) spindle is under argon shield condition, and 850 DEG C of heating were squeezed into band, extrusion strip width 60mm, thickness 4mm after 2 hours.
K) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to the annealing of 2.0mm thickness once, adopts nitrogen protection, temperature 700 DEG C, 1 hour time during annealing.
L) itemize-dicing method is adopted to obtain 3.8x3.8x0.9mm specification finished product contact.
Embodiment eight:
G) pre-oxidation process is adopted to prepare AgSnO
2(15)+additive powder, then by AgSnO
2(15) the common 25kg of W powder of+additive powder and weight percent 0.3% loads in mixed powder machine and mixes 8 hours.
H) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 8:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 90mm, length 400mm, hydrostatic pressure 200MPa.
I) spindle is under argon shield condition, and 900 DEG C sinter 2 hours, multiple pressure in hydropress, multiple pressure pressure 20MPa.
J) spindle is under nitrogen protection condition, and 750 DEG C of heating were squeezed into band, extrusion strip width 50mm, thickness 10mm after 3 hours.
K) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 7mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts argon shield, temperature 300 DEG C, 4 hours time during annealing.
L) mould punching method is adopted to obtain Φ 4x1.2mm specification finished product contact.
Embodiment nine:
G) directly by 21.625kgAg powder, 3.0kgSnO
2powder, 0.25kgW powder, 0.125kg additive powder load in mixed powder machine and mix 12 hours
H) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 7:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 95mm, length 350mm, hydrostatic pressure 220MPa.
I) spindle is under nitrogen protection condition, and 850 DEG C sinter 4 hours, multiple pressure in hydropress, multiple pressure pressure 30MPa.
J) spindle is under argon shield condition, and 600 DEG C of heating were squeezed into band, extrusion strip width 70mm, thickness 8mm after 5 hours.
K) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts nitrogen protection, temperature 500 DEG C, time 2 h during annealing.
L) mould punching method is adopted to obtain Φ 3x0.8mm specification finished product contact.
Embodiment ten:
G) directly by 21.125kgAg powder, 3.75kgSnO
2powder, 0.125kgW powder load in mixed powder machine and mix 6 hours.
H) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 10:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 110mm, length 400mm, hydrostatic pressure 300MPa.
I) spindle is under nitrogen protection condition, and 600 DEG C sinter 6 hours, multiple pressure in isostatic pressing machine, multiple pressure pressure 250MPa.
J) spindle is under nitrogen protection condition, and 800 DEG C of heating were squeezed into band, extrusion strip width 50mm, thickness 4mm after 1.5 hours.
K) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, anneals once, adopt argon shield, temperature 800 DEG C, 1 hour time during annealing when being cold-rolled to 2mm thickness.
L) itemize-dicing method is adopted to obtain 3.5x3.5x0.5mm specification finished product contact.
Embodiment 11:
B) directly by 22.25kgAg powder, 2.0kgSnO
2powder, 0.5kgW powder, 0.250kg additive powder load in mixed powder machine and mix 10 hours.
C) mixed powder puts into ball-grinding machine ball milling 12 hours, granulates.
D) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 75%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 10% of contact total thickness.
E) first pressing pressed compact sinters 5 hours in 900 DEG C under nitrogen protection condition.
A) pressed compact after sintering is suppressed into 25x10x2mm finished product contact in multiple compression mould, multiple pressure pressure 10T/cm
2.
Embodiment 12:
A) pre-oxidation process is adopted to prepare AgSnO
2(12)+additive powder, then by AgSnO
2(12) the common 25kg of W powder of+additive powder and weight percent 1% loads in mixed powder machine and mixes 1 hour.
B) mixed powder puts into ball-grinding machine ball milling 8 hours, granulates.
C) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 85%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 10% of contact total thickness.
D) first pressing pressed compact sinters 2 hours in 650 DEG C under argon shield condition.
A) pressed compact after sintering is suppressed into 30x20x4mm finished product contact in multiple compression mould, multiple pressure pressure 14T/cm
2.
Embodiment 13:
M) adopt pre-oxidation process to prepare AgZnO(10)+additive powder, then by AgZnO(10) the W powder of+additive powder and weight percent 0.5% altogether 25kg load to mix in powder machine and mix 4 hours.
N) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 9:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 100mm, length 300mm, hydrostatic pressure 150MPa.
O) spindle is under argon shield condition, and 800 DEG C sinter 6 hours, multiple pressure in cold isostatic press, multiple pressure pressure 150MPa.
P) spindle is under argon shield condition, and 850 DEG C of heating were squeezed into band, extrusion strip width 60mm, thickness 3mm after 2 hours.
Q) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to the annealing of 1.5mm thickness once, adopts argon shield, temperature 700 DEG C, 1.5 hours time during annealing.
R) itemize-dicing method is adopted to obtain 3x2x0.8mm specification finished product contact.
Embodiment 14:
M) adopt pre-oxidation process to prepare AgZnO(20)+additive powder, then by AgZnO(20) the W powder of+additive powder and weight percent 0.3% altogether 25kg load to mix in powder machine and mix 8 hours.
N) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 8:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 90mm, length 400mm, hydrostatic pressure 200MPa.
O) spindle is under argon shield condition, and 900 DEG C sinter 2 hours, multiple pressure in hydropress, multiple pressure pressure 20MPa.
P) spindle is under nitrogen protection condition, and 750 DEG C of heating were squeezed into band, extrusion strip width 45mm, thickness 8mm after 3 hours.
Q) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts nitrogen protection, temperature 300 DEG C, 4 hours time during annealing.
R) mould punching method is adopted to obtain Φ 8x1SR30mm specification finished product contact.
Embodiment 15:
M) directly by mixing in 21.625kgAg powder, 3.0kgZnO powder, 0.25kgW powder, the mixed powder machine of 0.125kg additive powder loading 12 hours
N) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 7:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 95mm, length 450mm, hydrostatic pressure 220MPa.
O) spindle is under nitrogen protection condition, and 850 DEG C sinter 4 hours, multiple pressure in hydropress, multiple pressure pressure 30MPa.
P) spindle is under argon shield condition, and 700 DEG C of heating were squeezed into band, extrusion strip width 60mm, thickness 8mm after 2 hours.
Q) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts nitrogen protection, temperature 700 DEG C, time 2 h during annealing.
R) mould punching method is adopted to obtain Φ 7x1mm specification finished product contact.
Embodiment 16:
M) directly by mixing in 20.375kgAg powder, 4.50kgZnO powder, the mixed powder machine of 0.125kgW powder loading 8 hours.
N) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 10:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 100mm, length 400mm, hydrostatic pressure 200MPa.
O) spindle is under nitrogen protection condition, and 780 DEG C sinter 6 hours, multiple pressure in isostatic pressing machine, multiple pressure pressure 200MPa.
P) spindle is under nitrogen protection condition, and 800 DEG C of heating were squeezed into band, extrusion strip width 60mm, thickness 3mm after 2 hours.
Q) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, anneals once, adopt nitrogen protection, temperature 800 DEG C, time 2 h during annealing when being cold-rolled to 1.5mm thickness.
A) itemize-dicing method is adopted to obtain 6x6x1mm specification finished product contact.
Embodiment 17:
E) directly by mixing in 23.5kgAg powder, 0.125kgZnO powder, 1.25kgW powder, the mixed powder machine of 0.125kg additive powder loading 2 hours.
F) mixed powder puts into ball-grinding machine ball milling 3 hours, granulates.
G) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 85%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 15% of contact total thickness.
H) first pressing pressed compact sinters 2 hours in 800 DEG C under argon shield condition.
I) pressed compact after sintering is suppressed into 20x20x3mm finished product contact in multiple compression mould, multiple pressure pressure 12T/cm
2.
Embodiment 18:
F) adopt pre-oxidation process to prepare AgZnO(8)+additive powder, then by AgZnO(8) the W powder of+additive powder and weight percent 1.5% altogether 25kg load to mix in powder machine and mix 8 hours.
G) mixed powder puts into ball-grinding machine ball milling 6 hours, granulates.
H) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 80%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 15% of contact total thickness.
I) first pressing pressed compact sinters 4 hours in 850 DEG C under argon shield condition.
A) pressed compact after sintering is suppressed into 25x10x2mm finished product contact in multiple compression mould, multiple pressure pressure 8T/cm
2.
Embodiment 19:
S) adopt pre-oxidation process to prepare AgCuO(10)+additive powder, then by AgCuO(10) the W powder of+additive powder and weight percent 0.5% altogether 25kg load to mix in powder machine and mix 4 hours.Wherein additive comprises the NiO powder of weight percent 0.15%, the ZnO powder of 1.2%.
T) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 9:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 100mm, length 300mm, hydrostatic pressure 150MPa.
U) spindle is under argon shield condition, and 800 DEG C sinter 6 hours, multiple pressure in cold isostatic press, multiple pressure pressure 150MPa.
V) spindle is under argon shield condition, and 850 DEG C of heating were squeezed into band, extrusion strip width 60mm, thickness 4mm after 2 hours.
W) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to the annealing of 2.0mm thickness once, adopts nitrogen protection, temperature 700 DEG C, 1 hour time during annealing.
X) itemize-dicing method is adopted to obtain 3.8 × 3.8 × 0.9mm specification finished product contact.
Embodiment 20:
S) adopt pre-oxidation process to prepare AgCuO(20)+additive powder, then by AgCuO(20) the W powder of+additive powder and weight percent 0.3% altogether 25kg load to mix in powder machine and mix 8 hours.Wherein additive comprises the Sb of weight percent 0.3%
2o
3powder, the MoO of 0.1%
3powder.
T) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 8:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 90mm, length 400mm, hydrostatic pressure 200MPa.
U) spindle is under argon shield condition, and 900 DEG C sinter 2 hours, multiple pressure in hydropress, multiple pressure pressure 20MPa.
V) spindle is under nitrogen protection condition, and 750 DEG C of heating were squeezed into band, extrusion strip width 45mm, thickness 8mm after 3 hours.
W) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts nitrogen protection, temperature 300 DEG C, 4 hours time during annealing.
X) mould punching method is adopted to obtain Φ 8 × 0.9SR30mm specification finished product contact.
Embodiment 21:
S) directly by 21.625kgAg powder, 3.0kgCuO powder, 0.25kgW powder, 0.025kgNiO powder, 0.050kgBi
2o
3powder, 0.050kgSb
2o
3powder loads in mixed powder machine and mixes 12 hours.
T) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 7:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 95mm, length 350mm, hydrostatic pressure 220MPa.
U) spindle is under nitrogen protection condition, and 850 DEG C sinter 4 hours, multiple pressure in hydropress, multiple pressure pressure 30MPa.
V) spindle is under argon shield condition, and 600 DEG C of heating were squeezed into band, extrusion strip width 55mm, thickness 8mm after 5 hours.
W) extrusion strip is removed end to end, cold-rolling mill is cold-rolled to finished product thickness, is cold-rolled to 6mm thickness, is cold-rolled to 4mm thickness, respectively anneals once when being cold-rolled to 2mm thickness, adopts nitrogen protection, temperature 500 DEG C, time 2 h during annealing.
X) mould punching method is adopted to obtain Φ 8 × 0.9mm specification finished product contact.
Embodiment 22:
R) directly by mixing in 20.375kgAg powder, 4.50kgCuO powder, the mixed powder machine of 0.125kgW powder loading 6 hours.
S) in isostatic cool pressing equipment rubber coating, put into dividing plate, make it form size two Room, the aspect ratio of large room A and cell B controls at 10:1; Mixed powder is loaded in large room A, silver powder is loaded in cell B, extract dividing plate out, in equal pressing equipment, be pressed into overall spindle, spindle diameter 110mm, length 400mm, hydrostatic pressure 300MPa.
T) spindle is under nitrogen protection condition, and 600 DEG C sinter 6 hours, multiple pressure in isostatic pressing machine, multiple pressure pressure 250MPa.
U) spindle is under nitrogen protection condition, and 800 DEG C of heating were squeezed into band, extrusion strip width 50mm, thickness 4mm after 1.5 hours.
V) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, anneals once, adopt argon shield, temperature 800 DEG C, 1 hour time during annealing when being cold-rolled to 2mm thickness.
W) itemize-dicing method is adopted to obtain 3.5 × 3.5 × 0.5mm specification finished product contact.
Embodiment 23:
F) directly by 22.25kgAg powder, 2.0kgCuO powder, 0.5kgW powder, 0.050kgNiO powder, 0.025kgTeO
2powder, 0.025kgSb
2o
3powder, 0.025kgZnO powder, 0.050kgMoO
3powder, 0.075kgSnO
2powder loads in mixed powder machine and mixes 10 hours.
G) mixed powder puts into ball-grinding machine ball milling 12 hours, granulates.
H) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 75%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 10% of contact total thickness.
I) first pressing pressed compact sinters 5 hours in 900 DEG C under nitrogen protection condition.
A) pressed compact after sintering is suppressed into Φ 17.5x2mm finished product contact in multiple compression mould, multiple pressure pressure 10T/cm
2.
Embodiment 24:
A) adopt pre-oxidation process to prepare AgCuO(15)+additive powder, then by AgCuO(15) the W powder of+additive powder and weight percent 0.1% altogether 25kg load to mix in powder machine and mix 1 hour.Wherein additive comprises the NiO powder of weight percent 0.2%, the ZnO powder of 0.3%, the TeO of 0.8%
2powder.
B) mixed powder puts into ball-grinding machine ball milling 8 hours, granulates.
C) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 85%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 10% of contact total thickness.
D) first pressing pressed compact sinters 2 hours in 650 DEG C under argon shield condition.
Pressed compact after sintering is suppressed into Φ 20 × 2mm finished product contact in multiple compression mould, multiple pressure pressure 14T/cm
2.
Claims (3)
1. a preparation method for siluer metal oxide tungsten composite electric contact material, is characterized in that: this siluer metal oxide tungsten composite electric contact material prepared is small-size flaky contact material, comprises following operation:
(1) mixed powder configuration, adopts pre-oxidation process to prepare siluer metal oxide powder and additive powder, then siluer metal oxide powder, additive powder is mixed with tungsten powder; Or directly Ag powder, metal oxide powder, tungsten powder, additive powder are mixed; Each constituent mass ratio in this mixed powder is:
Metal oxide 1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver;
(2) in the rubber coating of a closed bottom, longitudinally dividing plate is inserted, the inner chamber of rubber coating is made to be separated into large room and cell, large room (A) controls at 7:1 ~ 10:1 with the radial height ratio of cell (B), the mixed powder that step (1) configures is loaded large room, shaping for welding silver layer silver powder is loaded cell, extract dividing plate out, overall spindle is pressed in equal pressing equipment, spindle diameter control at 80 ~ 120mm, cut to lengthen at 200 ~ 500mm, hydrostatic pressure 50 ~ 300MPa;
(3) spindle is under argon gas or nitrogen protection condition, and 600 ~ 900 DEG C sinter 1 ~ 6 hour, presses again in isostatic cool pressing equipment or hydropress, multiple pressure pressure 20 ~ 300MPa;
(4) spindle is under argon gas or nitrogen protection condition, is squeezed into band, extrusion strip width 20 ~ 70mm, thickness 2 ~ 10mm 600 ~ 900 DEG C of heating after 1 ~ 6 hour;
(5) extrusion strip is removed end to end, and cold-rolling mill is cold-rolled to finished product thickness, Process Annealing once more than, adopt argon gas or nitrogen protection during annealing, temperature 300 ~ 800 DEG C, 0.5 ~ 8 hour time;
(6) itemize-dicing method is adopted to obtain finished product contact; Or adopt mould punching method to obtain finished product contact.
2. a preparation method for siluer metal oxide tungsten composite electric contact material, is characterized in that: this siluer metal oxide tungsten composite electric contact material prepared is large-scale sheet contact material, comprises following operation:
(1) mixed powder preparation, adopts pre-oxidation process to prepare siluer metal oxide powder and additive powder, then siluer metal oxide powder, additive powder and tungsten powder is mixed; Or directly Ag powder, metal oxide powder, tungsten powder, additive powder are mixed; Each constituent mass ratio in this mixed powder is:
Metal oxide 1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver;
(2) granulate, mixed powder prepared by step (1) is put into ball-grinding machine ball milling 2 ~ 24 hours;
(3) adopt compression-moulding methods to obtain first pressing pressed compact, relative density controls 65% ~ 85%; Spread one deck silver powder as welding silver layer at powder mix surface uniform during first pressing, silver thickness controls in 5% ~ 30% of contact total thickness;
(4) first pressing pressed compact sinters 2 ~ 5 hours in 600 ~ 900 DEG C under argon gas or nitrogen protection condition;
(5) pressed compact after sintering is suppressed into finished product contact in multiple compression mould, multiple pressure pressure 6 ~ 14T/cm
2.
3. the siluer metal oxide tungsten composite electric contact material prepared by the method for claim 1 or 2, is characterized in that: include contact body and welding silver layer, this contact body comprises following component:
Metal oxide 1-25%, tungsten 0.05 ~ 10%, additive≤5%, surplus is silver.
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| CN105886813A (en) * | 2016-04-23 | 2016-08-24 | 东莞市华诺合金有限公司 | Silver tin oxide-wolfram electrical contact material and preparation method thereof |
| CN107385267A (en) * | 2017-07-07 | 2017-11-24 | 福达合金材料股份有限公司 | Siluer metal oxide titanium nitride composite electric contact material and preparation method thereof |
| CN110802224A (en) * | 2018-08-06 | 2020-02-18 | 三菱电机株式会社 | Preparation method of silver-nickel-tin oxide composite powder and silver-nickel-tin oxide electrical contact material |
| CN111468718B (en) * | 2020-03-07 | 2022-03-25 | 浙江福达合金材料科技有限公司 | Silver copper oxide sheet-shaped electric contact and preparation method thereof |
| CN111468719B (en) * | 2020-03-07 | 2022-03-25 | 浙江福达合金材料科技有限公司 | Silver tin oxide sheet-shaped electrical contact and preparation method thereof |
| CN113245547B (en) * | 2021-04-23 | 2022-06-10 | 浙江福达合金材料科技有限公司 | Preparation method of silver-nickel graphite electrical contact with continuous decarburized layer on side surface |
| CN115491539B (en) * | 2022-08-30 | 2023-04-18 | 昆明理工大学 | Enhanced AgSnO 2 Electric contact material and preparation method thereof |
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| CN102763183A (en) * | 2009-12-18 | 2012-10-31 | 美泰乐技术国际公司 | Methods for manufacturing an electrical contact pad and electrical contact |
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| CN1477219A (en) * | 2002-08-21 | 2004-02-25 | 中国科学院金属研究所 | Preparation method of siluer metal oxide electric contact material |
| CN1425782A (en) * | 2003-01-14 | 2003-06-25 | 天津大学 | Metal oxide blended silver-tin dioxide electric contactor material and its preparing method |
| CN102763183A (en) * | 2009-12-18 | 2012-10-31 | 美泰乐技术国际公司 | Methods for manufacturing an electrical contact pad and electrical contact |
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