CN104493180B - A kind of lamellar or the preparation method of rivet type silver nickel electric contact material - Google Patents
A kind of lamellar or the preparation method of rivet type silver nickel electric contact material Download PDFInfo
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- CN104493180B CN104493180B CN201410840546.8A CN201410840546A CN104493180B CN 104493180 B CN104493180 B CN 104493180B CN 201410840546 A CN201410840546 A CN 201410840546A CN 104493180 B CN104493180 B CN 104493180B
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Abstract
The invention discloses a kind of lamellar or the preparation method of rivet type silver nickel electric contact material, particularly as follows: calculate the consumption of required nickel oxide powder and silver nitrate respectively according to the material mixture ratio of the silver-colored nickel electric contact of required preparation, and calculate the consumption of sodium hydroxide, weigh standby;Take silver nitrate and be made into the silver nitrate solution of 20~40w/w%, by nickel oxide powder and silver nitrate solution mix homogeneously, obtain the suspension containing silver nitrate and nickel oxide;Take sodium hydroxide and be made into the sodium hydroxide solution of 10~30w/w%, join stirring reaction in above-mentioned suspension, have precipitation to generate, filter, obtain the composite powder of silver oxide and nickel oxide;Gained composite powder is washed to neutrality; dry, roasting; gained silver nickel oxide composite powder isostatic pressing, then reducing, gained silver nickel billet is processed into band or wire rod through hot extrusion under protection of reducing atmosphere, again through plastic working, obtains lamellar or rivet type silver nickel electric contact material.
Description
Technical field
The present invention relates to a kind of lamellar or the preparation method of rivet type silver nickel electric contact material, belong to field of metal matrix composite.
Background technology
Silver nickel electric contact is widely used in various low-voltage electrical apparatus owing to having the advantages such as good heat-conductivity conducting performance, low and stable contact resistance, excellent processing characteristics.At present, the preparation method at silver nickel electric contact is mainly powder metallurgic method and Chemical coating method two kinds.The technique using powder metallurgic method preparation silver nickel electric contact is simple, is suitable for producing in enormous quantities, but owing to silver density is 10.53g/cm3, the density of nickel is 8.9g/cm3, both density difference are bigger so that material prepared by this kind of method exists the problem that nickel distribution of particles is uneven;The metallographic structure of silver-colored nickel electric contact prepared by employing Chemical coating method is relatively uniform, high comprehensive performance, but relatively big at the density difference of the two material own, and preparation process employs the noxious substance to human body and bad environmental, production cost is higher, is not suitable for commercial production.How on the premise of protection environment, prepare the silver-colored nickel contact material of high comprehensive performance and even tissue, become difficult point and the focus of research at present.
Through prior art is retrieved, the patent of invention of Publication No. CN102800513A discloses the preparation method of a kind of used as electric contacts silver nickel material, specifically the nikel powder after reduction is placed in the mixed solution of one or more of zinc salt, mantoquita, silver salt, lanthanum salt, chemical reaction is utilized to make one or more in simple substance zinc, elemental copper, elemental silver or simple substance lanthanum be coated on nikel powder surface, then the nikel powder being coated with is cleaned, dry after the metal-oxide that adds with argentum powder and trace carry out mixing, sieve, molding, finally obtain electrical contact material.This invention by include on nikel powder surface one layer as silver and the transition metal contacting bridge between nickel, improve the combination interface between silver and nickel, the silver-colored nickel material making the gained more conventional method of silver nickel material produce has more preferable performance.But the mode silver-colored in this patent, nickel by powder still uses mixed powder, owing to the density difference of argentum powder, nikel powder is relatively big, uses conventional Style of mixing powder can cause nickel granule skewness in silver Ni substrate material, thus affects the service life of contact material.
Summary of the invention
The technical problem to be solved in the present invention is to provide the lamellar or the preparation method of rivet type silver nickel electric contact material that a kind of technique is simple, nickel granule is evenly distributed in silver matrix, and silver obtained by this method nickel electric contact material metallographic structure is more uniformly distributed.
Lamellar of the present invention or the preparation method of rivet type silver nickel electric contact material, it is characterised in that comprise the following steps:
1) nickel oxide powder needed for calculating according to the material mixture ratio of the silver-colored nickel electric contact of required preparation and the consumption of silver nitrate, and calculate silver nitrate according to the consumption of silver nitrate and sodium hydroxide reaction generates the consumption of the sodium hydroxide needed for silver oxide, weigh standby;Take silver nitrate water dissolution and be made into the silver nitrate solution of 20~40w/w%, nickel oxide powder and silver nitrate solution are placed in reactor, stir, obtain the suspension containing silver nitrate and nickel oxide;
2) take sodium hydroxide and be made into the sodium hydroxide solution of 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 nickel oxide;
3) silver oxide of gained and the composite powder of nickel oxide are washed to neutrality, be dried, pulverize after carry out roasting, then pulverize, obtain silver-nickel oxide composite powder;
4) by the silver of gained-nickel oxide composite powder isostatic pressing, it is placed in reducing atmosphere the most again and reduces, obtain silver nickel billet;
5) gained silver nickel billet under protection of reducing atmosphere through hot extrusion be processed into band or wire rod, after through rolling or drawing, more stamped processing or rivet driver processing, i.e. obtain lamellar or rivet type silver nickel electric contact material.
The present invention reacts the composite powder obtaining silver oxide and nickel oxide with sodium hydroxide and the silver nitrate suspension containing nickel oxide powder, due to the density (6.67g/cm of nickel oxide3) and the silver oxide (7.143g/cm of reaction generation3) density be close, thus nickel oxide powder and silver oxide can be made to mix evenly so that nickel oxide powder is more uniformly distributed in silver oxide matrix;Silver oxide, nickel oxide obtain fine silver and pure nickel after hydrogen reducing, thus obtain the silver-colored nickel contact material that nickel granule is uniform, be distributed to disperse, and then make resulting materials have excellent electrical property.
The step 1 of said method) in, in the material of the described silver-colored nickel electric contact needing preparation, nickel content is 5~40wt%, and surplus is silver;Preferably nickel content is 10~30wt%, and surplus is silver.In this step, the nickel oxide powder that described nickel oxide powder generally uses particle mean size to be 1~10 μm, it is preferred to use particle mean size is the powder of 2~8 μm;Preferably silver nitrate is configured to the silver nitrate solution of 30~40w/w%, is more preferably configured to the silver nitrate solution of 30~35w/w%, the metallographic structure of gained electrical contact material so can be made to be more uniformly distributed.In this step, the consumption of sodium hydroxide is usually the 4/17~5/17 of silver nitrate consumption, and more preferably 4.4/17.
The step 2 of said method) in, described sodium hydroxide solution is sodium hydrate aqueous solution, and generally, the addition speed of sodium hydroxide solution is preferably 0.1~1L/min;The concentration of described sodium hydroxide solution is preferably 15~25w/w%, and the silver oxide that so reaction can be made to generate has and is more uniformly distributed outward appearance, and makes the metallographic structure of gained electrical contact material be more uniformly distributed further.In this step, stirring reaction is generally carried out under normal temperature condition, and the time of stirring reaction is usually 0.3~1h.
The step 3 of said method) in, the operation being dried and pulverizing is same as the prior art, in the application, is preferably dried and is dried by the composite powder of silver oxide and nickel oxide under the conditions of 100~150 DEG C, it usually needs the time of 12~18h;Crossing 100~200 eye mesh screens after being typically to pulverize the composite powder of dried silver oxide and nickel oxide, extracting screen underflow enters next process.In this step, described roasting is typically roasting 2~6h under 400~500 DEG C of temperature conditionss, then pulverizes (at least crossing 100 mesh sieves), obtains silver-nickel oxide composite powder.
The step 4 of said method) in, described isostatic pressing is identical with existing routine operation with restoring operation, and specifically, the briquetting pressure of isostatic pressing is usually 100~150MPa;Described reducing atmosphere is usually hydrogen atmosphere, it is common that the silver-colored nickel oxide billet after isostatic pressing is placed in hydrogen atmosphere under 600~900 DEG C of temperature conditionss reduction 15~25h, to obtain silver nickel billet.
The step 5 of said method) in, described reducing atmosphere is usually hydrogen atmosphere.Described hot extrusion operation is identical with existing routine operation, and specifically, the temperature of hot extrusion is usually 750~900 DEG C, and extrusion ratio is 10:1~600:1.When band is processed in silver nickel billet hot extrusion, gained band in reducing atmosphere after repeatedly rolling, being annealed to required size through punch press punching press, obtain lamellar silver nickel electric contact material.When silver nickel billet hot extrusion is processed into wire rod, gained wire rod is processed through rivet driver in reducing atmosphere after repeatedly drawing and annealing to required size, obtains rivet type silver nickel electric contact material.
Compared with prior art, present invention is characterized in that
1, the present invention reacts the composite powder obtaining silver oxide and nickel oxide with sodium hydroxide and the silver nitrate suspension containing nickel oxide powder, due to the density (6.67g/cm of nickel oxide3) and the silver oxide (7.143g/cm of reaction generation3) density be close, thus nickel oxide powder and silver oxide can be made to mix evenly so that nickel oxide powder is more uniformly distributed in silver oxide matrix;Silver oxide, nickel oxide obtain fine silver and pure nickel after hydrogen reducing, thus obtain the silver-colored nickel contact material that nickel granule is uniform, be distributed to disperse, and then make resulting materials have excellent electrical property.
2, the method for the invention technique is simple, little to human body and environmental pollution, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure (200 ×) of the electrical contact product that the embodiment of the present invention 1 prepares;
Fig. 2 is the metallographic structure figure (200 ×) of the electrical contact product that the embodiment of the present invention 2 prepares;
Fig. 3 is the metallographic structure figure (200 ×) of the electrical contact product that the embodiment of the present invention 3 prepares;
Fig. 4 is the metallographic structure (200 ×) of Ag-Ni (10) product using 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 be more fully understood that present disclosure, but the present invention is not limited to following example.
Embodiment 1
1) it is first according to prepare 10kg Ag-Ni (5) material mixture ratio and calculates required nickel oxide (NiO) powder and silver nitrate (AgNO3) consumption, weigh nickel oxide powder 0.64kg and silver nitrate 14.96kg, then weighing sodium hydroxide 16.46kg, standby, wherein nickel oxide powder employing particle mean size is the powder of 3~5 μm;The silver nitrate water dissolution weighed being made into the silver nitrate solution of 30w/w%, is placed in reactor by the silver nitrate solution of the nickel oxide powder weighed and preparation, stir (stirring 120min), obtains the suspension containing silver nitrate and nickel oxide;
2) take sodium hydroxide and be made into the sodium hydroxide solution of 20w/w%, under stirring condition, the sodium hydroxide solution (rate of addition is 0.5L/min) of 20w/w% is added in the above-mentioned suspension containing silver nitrate and nickel oxide, reaction 0.5h, obtains the composite powder of silver oxide and nickel oxide after filtration;
3) silver oxide above-mentioned reaction obtained and the composite powder deionized water of nickel oxide are washed till neutrality at centrifugal swing dryer supernatant, it is subsequently placed in baking oven under 150 DEG C of temperature conditionss drying 12h, take out, silver oxide and the nickel oxide composite powder end of drying are placed in bipyramid blender broken (rotating speed 25r/min, time 1h), gained powder is placed in potoven roasting 4h under 500 DEG C of temperature conditionss, taking-up is placed in bipyramid blender broken (rotating speed 25r/min, time 1h), then powder crosses 200 eye mesh screens, obtains silver-nickel oxide composite powder;
4) by silver-nickel oxide composite powder molding on isostatic pressing machine (briquetting pressure is 100MPa) of above-mentioned gained, and the silver after molding-nickel oxide billet is placed in hydrogen atmosphere with 880 DEG C of temperature reduction, sintering 15h, obtains silver nickel billet;
5) hot extrusion under hydrogen atmosphere is protected of the silver-colored nickel billet of gained being processed into wire rod, extrusion temperature is 850 DEG C, and mold preheating temperature is 150 DEG C, and extrusion ratio is 500:1;Gained wire rod in hydrogen shield atmosphere repeatedly drawing and annealing after required size, be processed into rivet type silver nickel (Ag-Ni (5)) electrical contact with rivet driver.
Gained contact material is carried out metallographic structure analysis, as it is shown in figure 1, result shows that in Ag-Ni (5) product prepared by technical scheme, nickel granule is evenly distributed in silver matrix.
Embodiment 2
1) it is first according to prepare 10kg Ag-Ni (40) material mixture ratio and calculates required nickel oxide powder and silver nitrate consumption, weigh nickel oxide powder 5.08kg and silver nitrate 9.45kg, weighing sodium hydroxide 10.40kg again, standby, wherein nickel oxide powder employing particle mean size is the powder of 2~3 μm;The silver nitrate water dissolution weighed being made into the silver nitrate solution of 20w/w%, is placed in reactor by the silver nitrate solution of the nickel oxide powder weighed and preparation, stir (stirring 100min), obtains the suspension containing silver nitrate and nickel oxide;
2) take sodium hydroxide and be made into the sodium hydroxide solution of 10w/w%, under stirring condition, the sodium hydroxide solution (rate of addition is 1L/min) of 10w/w% is added in the above-mentioned suspension containing silver nitrate and nickel oxide, reaction 0.4h (addition speed is 1L/min), obtains the composite powder of silver oxide and nickel oxide after filtration;
3) silver oxide above-mentioned reaction obtained and the composite powder deionized water of nickel oxide are washed till neutrality at centrifugal swing dryer supernatant, it is subsequently placed in baking oven under 120 DEG C of temperature conditionss drying 15h, take out, silver oxide and the nickel oxide composite powder end of drying are placed in bipyramid blender broken (rotating speed 25r/min, time 1h), gained powder is placed in potoven roasting 4h under 450 DEG C of temperature conditionss, taking-up is placed in bipyramid blender broken (rotating speed 25r/min, time 1h), then powder crosses 200 eye mesh screens, obtains silver-nickel oxide composite powder;
4) by silver-nickel oxide composite powder molding on isostatic pressing machine (briquetting pressure is 150MPa) of above-mentioned gained, and the silver after molding-nickel oxide billet is placed in hydrogen atmosphere with 900 DEG C of temperature reduction, sintering 25h, obtains silver nickel billet;
5) hot extrusion under hydrogen atmosphere is protected of the silver-colored nickel billet of gained being processed into sheet material, extrusion temperature is 750 DEG C, and mold preheating temperature is 150 DEG C, and extrusion ratio is 10:1;Gained sheet material is processed into lamellar silver nickel (Ag-Ni (40)) electrical contact with punch press punching press in hydrogen shield atmosphere after rolling, being annealed to required size.
Gained contact material is carried out metallographic structure analysis, as in figure 2 it is shown, result shows that in Ag-Ni (40) product prepared by technical scheme, nickel granule is evenly distributed in silver matrix.
Embodiment 3
1) it is first according to prepare 10kg Ag-Ni (10) material mixture ratio and calculates required nickel oxide powder and silver nitrate consumption, weigh nickel oxide powder 1.27kg and silver nitrate 14.17kg, weighing sodium hydroxide 15.59kg again, standby, wherein nickel oxide powder employing particle mean size is the powder of 3~5 μm;The silver nitrate water dissolution weighed being made into the silver nitrate solution of 40w/w%, is placed in reactor by the silver nitrate solution of the nickel oxide powder weighed and preparation, stir (stirring 120min), obtains the suspension containing silver nitrate and nickel oxide;
2) take sodium hydroxide and be made into the sodium hydroxide solution of 30w/w%, under stirring condition, the sodium hydroxide solution (rate of addition is 0.5L/min) of 30w/w% is added in the above-mentioned suspension containing silver nitrate and nickel oxide, reaction 0.5h, obtains the composite powder of silver oxide and nickel oxide after filtration;
3) silver oxide above-mentioned reaction obtained and the composite powder deionized water of nickel oxide are washed till neutrality at centrifugal swing dryer supernatant, it is subsequently placed in baking oven under 150 DEG C of temperature conditionss drying 12h, take out, silver oxide and the nickel oxide composite powder end of drying are placed in bipyramid blender broken (rotating speed 25r/min, time 1h), gained powder is placed in potoven roasting 6h under 500 DEG C of temperature conditionss, taking-up is placed in bipyramid blender broken (rotating speed 25r/min, time 1h), then powder crosses 200 eye mesh screens, obtains silver-nickel oxide composite powder;
4) by silver-nickel oxide composite powder molding on isostatic pressing machine (briquetting pressure is 100MPa) of above-mentioned gained, and the silver after molding-nickel oxide billet is placed in hydrogen atmosphere with 650 DEG C of temperature reduction, sintering 20h, obtains silver nickel billet;
5) hot extrusion under hydrogen atmosphere is protected of the silver-colored nickel billet of gained being processed into wire rod, extrusion temperature is 850 DEG C, and mold preheating temperature is 150 DEG C, and extrusion ratio is 500;Gained wire rod in hydrogen shield atmosphere repeatedly drawing and annealing after required size, be processed into, with rivet driver, integral rivet type silver nickel (Ag-Ni (the 10)) electrical contact that specification is 2.5 × 1.2+1.5 × 1.5 (unit: mm).
Gained contact material is carried out metallographic structure analysis, as it is shown on figure 3, result shows that in Ag-Ni (10) product prepared by technical scheme, nickel granule is evenly distributed in silver matrix.
Comparative example 1
1) contrast test condition is to ensure that the contact silver content prepared with embodiment 3 is consistent, weighs 9.0kg fine silver powder and 1.0kg nikel powder, carries out mixed powder with three-dimensional blender device, controls rotating speed 40r/min, and the mixed powder time is 3h, obtains mixed powder;
2) remaining steps is by 4 in above example 3), 5) same process is prepared as wire rod, and is processed into integral rivet type silver nickel (Ag-Ni (the 10)) electrical contact that specification is 3.0 × 0.8+1.5 × 1.5 (unit: mm).
Gained contact material is carried out metallographic structure analysis, as shown in Figure 4.
Integral rivet type contact embodiment 3, comparative example 1 prepared, is assemblied on contact simulation of electrical performance testing machine, carries out electrical contact endurance contrast test under the conditions of 220VAC, 30A, resistive load, and every kind of material is tested three simultaneously and contact, result of the test are shown in Table 1.
Table 1:
Result of the test and Fig. 3 and Fig. 4 by table 1 can be seen that, under the same test conditions, silver content composition is identical, compared with the material of comparative example 1 preparation, Ag-Ni (10) the material not only metallographic structure of embodiment 3 preparation is evenly, and electric life fluctuation is less, the life-span is higher, shows that the AgNi contact material using the method for the present invention to prepare has better and stable electric property.
Claims (5)
1. a lamellar or the preparation method of rivet type silver nickel electric contact material, it is characterised in that comprise the following steps:
1) nickel oxide powder needed for calculating according to the material mixture ratio of the silver-colored nickel electric contact of required preparation and the consumption of silver nitrate, and calculate silver nitrate according to the consumption of silver nitrate and sodium hydroxide reaction generates the consumption of the sodium hydroxide needed for silver oxide, weigh standby;Take silver nitrate water dissolution and be made into the silver nitrate solution of 20~40w/w%, nickel oxide powder and silver nitrate solution are placed in reactor, stir, obtain the suspension containing silver nitrate and nickel oxide;
2) take sodium hydroxide and be made into the sodium hydroxide solution of 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 nickel oxide;
3) silver oxide of gained and the composite powder of nickel oxide are washed to neutrality, be dried, pulverize after carry out roasting, then pulverize, obtain silver-nickel oxide composite powder;
4) by the silver of gained-nickel oxide composite powder isostatic pressing, it is placed in reducing atmosphere the most again and reduces, obtain silver nickel billet;
5) gained silver nickel billet under protection of reducing atmosphere through hot extrusion be processed into band or wire rod, after through rolling or drawing, more stamped processing or rivet driver processing, i.e. obtain lamellar or rivet type silver nickel electric contact material.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, needing in the silver-colored nickel electric contact material of preparation, nickel content is 5~40wt%, and surplus is silver.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, take silver nitrate water dissolution and be made into the silver nitrate solution of 30~40w/w%.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, the consumption of sodium hydroxide is the 4/17~5/17 of silver nitrate consumption.
Preparation method the most according to claim 1, it is characterised in that: step 2) in, the concentration of sodium hydroxide solution is 15~25w/w%.
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US4370395A (en) * | 1980-06-04 | 1983-01-25 | Union Carbide Corporation | Alkaline cell |
CN1841819A (en) * | 2005-03-31 | 2006-10-04 | 同和矿业株式会社 | Battery positive electrode material |
CN101139663A (en) * | 2007-10-19 | 2008-03-12 | 厦门大学 | Preparation method of silver nickel composite material |
CN101403105A (en) * | 2008-11-19 | 2009-04-08 | 河北工业大学 | Preparation method for carbon-coating nickel nano-particle reinforced silver-based composite material |
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Publication number | Priority date | Publication date | Assignee | Title |
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US4370395A (en) * | 1980-06-04 | 1983-01-25 | Union Carbide Corporation | Alkaline cell |
CN1841819A (en) * | 2005-03-31 | 2006-10-04 | 同和矿业株式会社 | Battery positive electrode material |
CN101139663A (en) * | 2007-10-19 | 2008-03-12 | 厦门大学 | Preparation method of silver nickel composite material |
CN101403105A (en) * | 2008-11-19 | 2009-04-08 | 河北工业大学 | Preparation method for carbon-coating nickel nano-particle reinforced silver-based composite material |
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Effective date of registration: 20180115 Address after: 541004 the Guangxi Zhuang Autonomous Region Dongcheng Qixing District, Guilin City Road No. 8 Patentee after: Guilin Jinge Electrotechnical Electronic Material Science & Technology Co., Ltd. Address before: 541004 the Guangxi Zhuang Autonomous Region Dongcheng Qixing District, Guilin City Road No. 8 Patentee before: Guilin Electrical Equipment Scientific Research Institute Co., Ltd. |