CN104525968A - Flaky silver-tungsten electrical contact material preparation method - Google Patents
Flaky silver-tungsten electrical contact material preparation method Download PDFInfo
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- CN104525968A CN104525968A CN201410844385.XA CN201410844385A CN104525968A CN 104525968 A CN104525968 A CN 104525968A CN 201410844385 A CN201410844385 A CN 201410844385A CN 104525968 A CN104525968 A CN 104525968A
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Abstract
The invention discloses a flaky silver-tungsten electrical contact material preparation method. The method comprises the steps that according to the ratio of a silver-tungsten electrical contact material needing to be prepared, the required amount of tungsten trioxide powder and the required amount of silver nitrate are calculated respectively, the amount of sodium hydroxide is calculated, and the tungsten trioxide powder, the silver nitrate and the sodium hydroxide are weighed for use; the silver nitrate is taken and prepared into a silver nitrate solution with the weight-in-weight percent ranging from 20 to 40, and the tungsten trioxide powder and the silver nitrate solution are mixed evenly to obtain suspension liquid containing the silver nitrate and tungsten trioxide; the sodium hydroxide is taken and prepared into a sodium hydroxide solution with the weight-in-weight percent ranging from 10 to 30, the sodium hydroxide solution is added into the suspension liquid, the mixture is stirred for a reaction, sediment is generated and filtered out, and then composite powder containing silver oxide and the tungsten trioxide is obtained; the obtained composite powder is washed in water to be neutral, dried and calcined, obtained silver-tungsten oxide composite powder is subjected to oil pressure forming and restoring, obtained compacts are re-pressed and re-calcined, and then the flaky silver-tungsten electrical contact material is obtained. According to the method, the process is simple, and environmental protection is achieved; the contact material prepared through the method is more uniform in metallographic structure.
Description
Technical field
The present invention relates to the preparation method of a kind of sheet silver tungsten electrical contact material, belong to field of metal matrix composite.
Background technology
Silver tungsten electrical contact is widely used in various household electrical appliance owing to having the advantages such as good heat-conductivity conducting performance, resistance to electric abrasioning performance, resistance fusion welding energy and antioxygenic property.The preparation method of current silver-colored tungsten electrical contact mainly contains infiltration method and solid phase method two kinds, wherein: the silver-colored tungsten electrical contact density and hardness adopting infiltration method to prepare is high, metallographic structure is more even, but also there is good electrical property, but the technics comparing of this kind of method is complicated, operation is long, and production cost is relatively high; Though the method that solid phase method prepares silver-colored tungsten electrical contact has simple, the lower-cost advantage of production technology, the metallographic structure of gained contact material is even not, affects the resistance fusion welding energy of contact, thus affects the service life of electrical equipment.How raising the efficiency, under the prerequisite of not obvious increase cost, prepare electrical property and the excellent silver-colored tungsten material of structure property, become difficult point and the focus of research at present.
Publication number is that the patent of invention of CN102392170A discloses a kind of processing method manufacturing silver-colored tungsten composite contact material; the method tungsten powder is placed in reaction vessels to add water and after appropriate reducing agent (hydrazine hydrate or formaldehyde); spray into silver-colored ammonia complexing solution under agitation; reaction generates silver-colored tungsten coated composite powder; the silver-colored tungsten coated composite powder cleaned up is just molded after high-energy ball milling process and destressing process, then under restitutive protection's atmosphere through presintering, melting infiltration sintering, be pressed into silver-tungsten composite material again.In the described technical scheme of this invention, the very high (19.25g/cm of the density due to tungsten powder
3), with the density (10.5g/cm reacting the silver powder generated
3) difference is too large, is difficult to be stirred in course of reaction, thus there is tungsten powder and to unite the phenomenon of assembling, affect the metallographic structure uniformity of gained contact material; In addition, adopt hydrazine hydrate or formaldehyde to be reducing agent in technique scheme, not only have impact to the health of production operation personnel, also there is the problem of environmental pollution, be unfavorable for the sustainable development of society.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of technique is simple, preparation method to production operation personnel and the little sheet silver tungsten electrical contact material of ambient influnence, and sheet silver tungsten electrical contact material obtained by this method metallographic structure is more even.
The preparation method of sheet silver tungsten electrical contact material of the present invention, comprises the following steps:
1) calculate according to the material mixture ratio of the silver-colored tungsten electrical contact of required preparation needed for anhydrous wolframic acid powder and the consumption of silver nitrate, and the consumption of the NaOH needed for silver oxide is generated according to the Dosage calculation silver nitrate of silver nitrate and NaOH reaction, take for subsequent use; Get silver nitrate is made into 20 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, anhydrous wolframic acid powder and liquor argenti nitratis ophthalmicus are placed in reactor, stir, obtain the suspension containing silver nitrate and tungstic acid;
2) get the sodium hydroxide solution that NaOH is made into 10 ~ 30w/w%, join step 1) stirring reaction in the suspension of gained, there is precipitation to generate, filter, obtain the composite powder of silver oxide and tungstic acid;
3) silver oxide of gained and the composite powder of tungstic acid are washed to neutrality, carry out roasting after drying, pulverizing, then pulverize, obtain silver-colored tungsten oxide composite powder;
4) by shaping for the silver-colored tungsten oxide composite powder oil pressure of gained, and then be placed in reducing atmosphere and reduce, obtain silver-colored tungsten briquet;
5) gained silver tungsten briquet carries out multiple pressure, resintering, namely obtains sheet silver tungsten electrical contact material.
The present invention is obtained by reacting the composite powder of silver oxide and tungstic acid, due to the density (7.16g/cm of anhydrous wolframic acid powder with NaOH and the silver nitrate suspension containing anhydrous wolframic acid powder
3) and react the silver oxide (7.143g/cm generated
3) density be close, anhydrous wolframic acid powder and silver oxide thus can be made to be mixed to get evenly, make anhydrous wolframic acid powder more be evenly distributed in silver oxide matrix; On the other hand because the density of anhydrous wolframic acid powder and silver oxide is far smaller than the density of tungsten powder, which improve in prior art clustering phenomena (i.e. gained electrical contact material metallographic structure non-uniform phenomenon) of being united by the stirring tungsten powder that is uneven and then that produce that the silver powder of tungsten powder and formation causes because density variation is excessive, tungstic acid in the silver-colored tungsten oxide composite powder be obtained by reacting is distributed more disperse, evenly, and eliminate high-energy ball milling operation of the prior art, make preparation technology more simple.
The step 1 of above-mentioned preparation method) in, in the material of silver-colored tungsten electrical contact prepared by described needs, W content is 1 ~ 70wt%, and surplus is silver.In this step, described anhydrous wolframic acid powder adopts particle mean size to be the anhydrous wolframic acid powder of 1 ~ 10 μm usually, preferably adopts the powder of 2 ~ 3 μm; Preferably silver nitrate is mixed with the liquor argenti nitratis ophthalmicus of 30 ~ 40w/w%, is more preferably the liquor argenti nitratis ophthalmicus being mixed with 30 ~ 35w/w%, the metallographic structure of gained electrical contact material can be made so more even.In this step, the consumption of NaOH is generally 4/17 ~ 5/17 of silver nitrate consumption, is more preferably 4.4/17.
The step 2 of above-mentioned preparation method) in, described sodium hydroxide solution is sodium hydrate aqueous solution, and generally, the speed that adds of sodium hydroxide solution is preferably 0.1 ~ 1L/min; The concentration of described sodium hydroxide solution is preferably 15 ~ 25w/w%, and the metallographic structure of gained electrical contact material can be made so more even.In this step, stirring reaction carries out usually under normal temperature condition, and the time of stirring reaction is generally 0.3 ~ 1h.
The step 3 of above-mentioned preparation method) in, operation that is dry and that pulverize is same as the prior art, and in the application, preferably drying is until dry the composite powder of silver oxide and tungstic acid under 100 ~ 150 DEG C of conditions, usually needs the time of 12 ~ 18h; Normally the composite powder pulverizing of dried silver oxide and tungstic acid is crossed 100 ~ 200 eye mesh screens afterwards, extracting screen underflow enters next process.In this step, described roasting is roasting 2 ~ 6h under 400 ~ 500 DEG C of temperature conditions normally, then pulverizes (at least crossing 100 mesh sieves), obtains silver-colored tungsten oxide composite powder.
The step 4 of above-mentioned preparation method) in, when oil pressure is shaping, briquetting pressure is generally 8 ~ 12T/cm
2; Described reducing atmosphere is generally hydrogen atmosphere, normally the silver-colored tungsten oxide pressed compact after shaping is placed in hydrogen atmosphere under 600 ~ 900 DEG C of temperature conditions, reduces (reduction, sintering are carried out simultaneously) 8 ~ 15h, to obtain silver-colored tungsten briquet.
The step 5 of above-mentioned preparation method) in, the pressure of described multiple pressure is 12 ~ 18T/cm
2, described resintering be by multiple pressure after silver-colored tungsten briquet be placed in hydrogen atmosphere sinter 4 ~ 8h under 880 ~ 920 DEG C of condition.
Compared with prior art, feature of the present invention is:
1, the composite powder of silver oxide and tungstic acid is obtained by reacting with NaOH and the silver nitrate suspension containing anhydrous wolframic acid powder, due to the density (7.16g/cm of anhydrous wolframic acid powder
3) and react the silver oxide (7.143g/cm generated
3) density be close, anhydrous wolframic acid powder and silver oxide thus can be made to be mixed to get evenly, make anhydrous wolframic acid powder more be evenly distributed in silver oxide matrix; On the other hand because the density of anhydrous wolframic acid powder and silver oxide is far smaller than the density of tungsten powder, which improve in prior art clustering phenomena (i.e. gained electrical contact material metallographic structure non-uniform phenomenon) of being united by the stirring tungsten powder that is uneven and then that produce that the silver powder of tungsten powder and formation causes because density variation is excessive, tungstic acid in the silver-colored tungsten oxide composite powder be obtained by reacting is distributed more disperse, evenly, and eliminate high-energy ball milling operation of the prior art, make preparation technology more simple, production cost is lower;
2, do not use hydrazine hydrate or formaldehyde, decrease the impact of producing operating personnel's health dramatically, and effectively reduce the pollution to environment.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure (200 ×) of the electrical contact product that the embodiment of the present invention 1 obtains;
Fig. 2 is the metallographic structure figure (200 ×) of the electrical contact product that the embodiment of the present invention 2 obtains;
Fig. 3 is the metallographic structure figure (200 ×) of the electrical contact product that the embodiment of the present invention 3 obtains;
Fig. 4 is the metallographic structure figure (200 ×) of Ag-W (30) product adopting conventional solid sintering process to prepare.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and to understand content of the present invention better, but the present invention is not limited to following examples.
Embodiment 1
1) first required anhydrous wolframic acid powder and silver nitrate consumption is calculated according to preparation 10kg Ag-W (5) material mixture ratio, take anhydrous wolframic acid powder 0.63kg and silver nitrate 14.954kg, weighing sodium hydroxide 3.87kg again, for subsequent use, wherein anhydrous wolframic acid powder employing particle mean size is the powder of 2 ~ 3 μm; The silver nitrate taken is made into the liquor argenti nitratis ophthalmicus of 33w/w% by water-soluble solution, the liquor argenti nitratis ophthalmicus of the anhydrous wolframic acid powder taken and preparation is placed in reactor, stir (stirring 120min), obtains the suspension containing silver nitrate and tungstic acid;
2) sodium hydroxide solution that NaOH is made into 20w/w% is got, under stirring condition, the sodium hydroxide solution (rate of addition is 0.5L/min) adding 20w/w% in the suspension of silver nitrate and tungstic acid is contained to above-mentioned, reaction 0.5h, filters the composite powder obtaining silver oxide and tungstic acid;
3) the composite powder deionized water of the above-mentioned silver oxide that is obtained by reacting and tungstic acid is washed till neutrality at centrigugal swing dryer supernatant, under 120 DEG C of temperature conditions, 15h is dried with being placed in baking oven, take out, the silver oxide of oven dry and tungstic acid composite powder are placed in broken (the rotating speed 25r/min of bipyramid blender, time 1h), gained powder is placed in potoven roasting 4h under 450 DEG C of temperature conditions, taking-up is placed on broken (rotating speed 25r/min in bipyramid blender, time 1h), then powder crosses 200 eye mesh screens, obtains silver-colored tungsten oxide composite powder;
4) (briquetting pressure is 10T/cm by shaping on hydraulic press for the silver-colored tungsten oxide composite powder of above-mentioned gained
2), and the pressed compact after shaping is placed in hydrogen atmosphere with 800 DEG C of temperature reduction 10h, obtain silver-colored tungsten briquet;
5) (multiple pressure pressure is 15T/cm gained silver tungsten briquet to be carried out multiple pressure
2), and the silver-colored tungsten briquet after multiple pressure is placed in hydrogen atmosphere in 880 DEG C of temperature sintering 6h, obtain silver-colored tungsten (Ag-W (the 5)) electrical contact material of sheet.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 1, in Ag-W (5) product prepared of technical scheme, tungsten particle is evenly distributed in silver matrix as seen from the figure.
Embodiment 2
1) first required anhydrous wolframic acid powder and silver nitrate consumption is calculated according to preparation 10kg Ag-W (70) material mixture ratio, take anhydrous wolframic acid powder 8.826kg and silver nitrate 4.722kg, weighing sodium hydroxide 0.323kg again, for subsequent use, wherein anhydrous wolframic acid powder employing particle mean size is the powder of 2 ~ 3 μm; The silver nitrate taken is made into the liquor argenti nitratis ophthalmicus of 20w/w% by water-soluble solution, the liquor argenti nitratis ophthalmicus of the anhydrous wolframic acid powder taken and preparation is placed in reactor, stir (stirring 80min), obtains the suspension containing silver nitrate and tungstic acid;
2) sodium hydroxide solution that NaOH is made into 30w/w% is got, under stirring condition, the sodium hydroxide solution (rate of addition is 1L/min) adding 30w/w% in the suspension of silver nitrate and tungstic acid is contained to above-mentioned, reaction 0.3h, obtains the composite powder of silver oxide and tungstic acid after filtration;
3) the composite powder deionized water of the above-mentioned silver oxide that is obtained by reacting and tungstic acid is washed till neutrality at centrigugal swing dryer supernatant, under 100 DEG C of temperature conditions, 18h is dried with being placed in baking oven, take out, the silver oxide of oven dry and tungstic acid composite powder are placed in broken (the rotating speed 25r/min of bipyramid blender, time 1h), gained powder is placed in potoven roasting 6h under 400 DEG C of temperature conditions, taking-up is placed on broken (rotating speed 25r/min in bipyramid blender, time 1h), then powder crosses 200 eye mesh screens, obtains silver-colored tungsten oxide composite powder;
4) (briquetting pressure is 10T/cm by shaping on hydraulic press for the silver-colored tungsten oxide composite powder of above-mentioned gained
2), and the pressed compact after shaping is placed in hydrogen atmosphere with 900 DEG C of temperature reduction 15h, obtain silver-colored tungsten briquet;
5) (multiple pressure pressure is 18T/cm gained silver tungsten briquet to be carried out multiple pressure
2), and the silver-colored tungsten briquet after multiple pressure is placed in hydrogen atmosphere in 920 DEG C of temperature sintering 8h, obtain silver-colored tungsten (Ag-W (the 70)) electrical contact material of sheet.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 2, in Ag-W (70) product prepared of technical scheme, tungsten particle is evenly distributed in silver matrix as seen from the figure.
Embodiment 3
Repeat the method for embodiment 1, unlike:
Step 1) in, calculate required anhydrous wolframic acid powder and silver nitrate consumption according to preparation 10kg Ag-W (30) material mixture ratio and take for subsequent use, take appropriate NaOH for subsequent use simultaneously, wherein anhydrous wolframic acid powder employing particle mean size is the powder of 6 ~ 10 μm, the silver nitrate taken is made into the liquor argenti nitratis ophthalmicus of 40w/w% by water-soluble solution;
Step 2) in, the concentration of sodium hydroxide solution is 15w/w%, and consumption is 19.01L (rate of addition is 0.1L/min);
Step 3) in, the temperature of roasting is 500 DEG C, and the time is 5h;
Step 4) in, the temperature of reduction is 850 DEG C, and the time is 8h.
Metallographic structure analysis is carried out to gained contact material, as shown in Figure 3, contrast with the metallographic structure (as shown in Figure 4) of Ag-W (30) product adopting conventional solid sintering process to prepare, more disperse is even in the metallographic structure of known Ag-W (30) product prepared by technical scheme.
Embodiment 4
Repeat the method for embodiment 1, unlike:
Step 1) in, calculate required anhydrous wolframic acid powder and silver nitrate consumption according to preparation 10kg Ag-W (55) material mixture ratio and take for subsequent use, take appropriate NaOH for subsequent use simultaneously, wherein anhydrous wolframic acid powder employing particle mean size is the powder of 1 ~ 5 μm, the silver nitrate taken is made into the liquor argenti nitratis ophthalmicus of 30w/w% by water-soluble solution;
Step 2) in, the concentration of sodium hydroxide solution is 10w/w%, and consumption is 18.33L (rate of addition is 0.5L/min).
Embodiment 5
Repeat the method for embodiment 1, unlike:
Step 1) in, calculate required anhydrous wolframic acid powder and silver nitrate consumption according to preparation 10kg Ag-W (10) material mixture ratio and take for subsequent use, take appropriate NaOH for subsequent use simultaneously, wherein anhydrous wolframic acid powder employing particle mean size is the powder of 1 ~ 3 μm, the silver nitrate taken is made into the liquor argenti nitratis ophthalmicus of 35w/w% by water-soluble solution;
Step 2) in, the concentration of sodium hydroxide solution is 25w/w%, and consumption is 14.67L (rate of addition is 1L/min).
The contact material that embodiment 3 is obtained carries out Performance Detection, and the silver tungsten contact product obtained with existing conventional solid sintering process compares, result as described in Table 1:
Articles of sheet material performance prepared by table 1 embodiment 3 and existing conventional solid sintering process
As shown in Table 1, the performance of silver tungsten contact material that prepared by technical scheme is better than silver tungsten contact material property prepared by existing conventional solid sintering process.
Claims (5)
1. a preparation method for sheet silver tungsten electrical contact material, is characterized in that comprising the following steps:
1) calculate according to the material mixture ratio of the silver-colored tungsten electrical contact of required preparation needed for anhydrous wolframic acid powder and the consumption of silver nitrate, and the consumption of the NaOH needed for silver oxide is generated according to the Dosage calculation silver nitrate of silver nitrate and NaOH reaction, take for subsequent use; Get silver nitrate is made into 20 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, anhydrous wolframic acid powder and liquor argenti nitratis ophthalmicus are placed in reactor, stir, obtain the suspension containing silver nitrate and tungstic acid;
2) get the sodium hydroxide solution that NaOH is made into 10 ~ 30w/w%, join step 1) stirring reaction in the suspension of gained, there is precipitation to generate, filter, obtain the composite powder of silver oxide and tungstic acid;
3) silver oxide of gained and the composite powder of tungstic acid are washed to neutrality, carry out roasting after drying, pulverizing, then pulverize, obtain silver-colored tungsten oxide composite powder;
4) by shaping for the silver-colored tungsten oxide composite powder oil pressure of gained, and then be placed in reducing atmosphere and reduce, obtain silver-colored tungsten briquet;
5) gained silver tungsten briquet carries out multiple pressure, resintering, namely obtains sheet silver tungsten electrical contact material.
2. preparation method according to claim 1, is characterized in that: step 1) in, need in the silver-colored tungsten electrical contact material of preparation, W content is 1 ~ 70wt%, and surplus is silver.
3. preparation method according to claim 1, is characterized in that: step 1) in, get silver nitrate is made into 30 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution.
4. preparation method according to claim 1, is characterized in that: step 1) in, the addition of NaOH is 4/17 ~ 5/17 of silver nitrate consumption.
5. preparation method according to claim 1, is characterized in that: step 2) in, the concentration of sodium hydroxide solution is 15 ~ 25w/w%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105965022A (en) * | 2015-12-29 | 2016-09-28 | 桂林电器科学研究院有限公司 | Processing method for slice-shaped silver graphite electrical contact material |
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