CN1416986A - High temperature antioxidant base metal composition and its production process - Google Patents
High temperature antioxidant base metal composition and its production process Download PDFInfo
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- CN1416986A CN1416986A CN02145520A CN02145520A CN1416986A CN 1416986 A CN1416986 A CN 1416986A CN 02145520 A CN02145520 A CN 02145520A CN 02145520 A CN02145520 A CN 02145520A CN 1416986 A CN1416986 A CN 1416986A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a high temperature antioxidant base metal composition and its production process. The composition includes Ni in 30-54 pts.wt. and Ag in 46-70 pts.wt, and the Ag alloy forms thin antioxidant layer on the surface of Ni grains. The production process includes preparing sensitizing liquid, activating liquid, ammonia solution of silver and reductant; dipping, stirring, pickling, sensitizing, cleaning, activating, reduction, heating, and other steps. The said process can produce electrode with the conducting performance similar to that of noble metal but only one tench in cost. The application of the present invention can reduce the cost of MPT, MLCC and other electronic elements and product. The present invention has the features of simple process, low production cost and capacity of co-sintering with ceramic in atmosphere.
Description
One, technical field
The present invention relates to fire-resistant oxidation resistant base metal composition and production method thereof, be specially adapted to produce multi-layer piezoelectric transformer (MPT), the electrode materials in multi-layer capacitor (MLCC) and the multiclass thick-film resistor.
Two, background technology
(1) U.S. Pat-4122232
[1], adopt base metal and boron powder etc. to make agglomerating base metal electrocondution slurry under the atmospheric condition.It is bigger that but subject matter is sheet resistance, so use range is restricted, and can not use in MLCC and MPT product.
(2) domestic high tender and the Liu Zhicheng etc. of protecting
[2-5]Study silver-colored copper-clad technology, their purpose is the anti-oxidant problem of preparation in ultrafine powder, mainly is general experimental research, does not relate to the experimental study of application facet.
(3) scientific and technological result project of Kunming Institute of Precious Metals, it adopts the method for electroless plating, at lowpriced metal surfaces such as nickel plating silver layer equably, the mean particle size of the powder of producing can be less than 1 μ m, this composite powder replaces fine silver to prepare conductive resin, can save silver 70%, prepare silver-colored nickel electric contact material with this composite powder, because Ni is coated by Ag, realized contacting of Ag and Ag, physicals such as electroconductibility, processing characteristics makes obviously to be improved, but the environment of its experiment condition, production technique, purposes, use and the present invention have in essence different.
(4) document [7] is a U.S. US5045349 patent documentation, is the preparation technology of a kind of silver at the nickel surface coated with silver-nickel combined electrode, and kind electrode is used for alkaline cell.
In sum, pertinent literature does not see that utilizing the nickel particulate material to carry out coated with silver on surface forms the high-temperature oxidation resistant layer, and it can be burnt with porcelain body under atmospheric condition altogether, becomes the report of the electrode slurry that replaces precious metal.
Three, summary of the invention
Goal of the invention of the present invention provides a kind of silver alloys that adopts and forms very thin anti oxidation layer at the nickel particle surface, protects it at high temperature not oxidized, is applicable to the fire-resistant oxidation resistant base metal composition of the electronic component products of burning till at atmosphere.
Another goal of the invention of the present invention provides a kind of preparation base metal composition manufacturing method.
The technical scheme that realizes goal of the invention is to solve like this: its contribution is that the base metal composition contains nickel powder 30-54 part of weight ratio, silver-colored 70-46 part, and said nickel powder particle diameter is 0.5-6 μ m.
The production method of fire-resistant oxidation resistant base metal powder composition, comprise technology and preparation sensitizing solution, activation solution, silver ammino solution, reductive agent, following each component all by weight or the volume ratio meter, said sensitizing solution contains tin protochloride 10-25 part, hydrogenchloride 20-50 part, deionized water 900-1100 part; Said activation solution contains Palladous chloride 0.5-2.5 part, hydrogenchloride 10-100 part, deionized water 900-1000 part; Said silver ammino solution contains Silver Nitrate 46-70 part, ammoniacal liquor 167-110 part, deionized water 900-1000 part; Said reductive agent contains ethanol 100-800 part, formaldehyde 3-15 part, deionized water 200-500 part or glucose 5-20 part, distilled water 220-280 part, alcohol 10-60 part.
Said technology is in two steps:
The first step, nickel powder particle surface chemical silvering: at first nickel powder be impregnated in the gelatin solution of 5～20g/L, stir and made suspension in 9-12 minute; In suspension, add 20～60ml/L dilute sulphuric acid, removing oxide compound at 40～50 ℃ of following pickling 8-12 minutes; The nickel powder of washing is poured in the sensitizing solution, at room temperature, sensitization 9-13 minute, taken out and clean 2-3 time; Join in the activation solution, at room temperature, stirred 9-12 minute, take out and clean 2-3 time; Nickel powder is joined in the gelatin solution of 5～20g/L, stir and make suspension, pour the silver ammino solution for preparing into,, can make silver-plated nickel powder with the fast reductive agent that drips of dripping of 0.5～2ml/min.
In second step, vacuum heat treatment: silver-colored nickel powder is 200～600 ℃ in Heating temperature, and vacuum tightness is: 10Pa, heated 2～3 hours, and promptly get nickeline solid solution alloy powder.
The present invention is to adopt chemical method to make Ni fine powder surface directly be formed protective membrane by Ag molecule affinity in the liquid compared with prior art.Be applicable to the electronic component products of burning till at atmosphere, this electrode conductivity reaches the conductivity of noble metal electrode, and cost is 1/10th of a precious metal.Its application can reduce the cost of electronic components such as MPT and MLCC and other electronic product significantly, to the development of electronic devices and components and product bigger pushing effect will be arranged.It is simple that the present invention has technology, and production cost is low, can be total to the characteristics of baked under atmosphere with porcelain body, and better economic and social benefit are arranged.
Four, description of drawings
Fig. 1 is a clad structure model synoptic diagram of the present invention;
Fig. 2 forges the model synoptic diagram that forms the alloy protecting layer behind the baked for the present invention.
Five, embodiment
Accompanying drawing is the specific embodiment of the present composition.
Below in conjunction with accompanying drawing and technical process content of the present invention is described further:
With reference to Fig. 1, shown in Figure 2, composition contains nickel powder 30-54 part of weight ratio, silver-colored 70-46 part, and said nickel powder particle diameter is 0.5-6 μ m.
The base metal composition contains nickel powder 36-52 part or 48-54 part of weight ratio, silver-colored 64-48 part or 52-46 part, and said nickel powder particle diameter is 2-3 μ m or 4-6 μ m.
The production method of fire-resistant oxidation resistant base metal powder composition, comprise technology and preparation sensitizing solution, activation solution, silver ammino solution, reductive agent, following each component all by weight or the volume ratio meter, said sensitizing solution contains tin protochloride 10-25 part, hydrogenchloride 20-50 part, deionized water 900-1100 part, it is the divalent tin ion that surface adsorption one deck has reductibility that sensitization is handled; Said activation solution contains Palladous chloride 0.5-2.5 part, hydrogenchloride 10-100 part, and deionized water 900-1000 part, activation treatment is that the divalence palladium ion is reduced into the palladium particle with katalysis by surperficial divalent tin ion; Said silver ammino solution contains Silver Nitrate 111-73 part, ammoniacal liquor 167-110 part, deionized water 900-1000 part, Silver Nitrate (AgNO
3Ammoniacal liquor (the NH of)+1000 part deionized water+167-110 part
3H
2O) Silver Nitrate is dissolved in the deionized water, slowly adds ammoniacal liquor and stir 10 fens up to just disappearance of precipitation.Said reductive agent contains ethanol 100-800 part, formaldehyde 3-15 part, deionized water 200-500 part or glucose 5-20 part, distilled water 220-280 part, alcohol 10-60 part.Its reductive agent prescription (1) is: 100～800 parts of ethanol (CH
3CH
2OH)+3～15 part formaldehyde (HCHO)+200～500 part deionized water (H
2O); Reductive agent prescription (2) is: 5～20 parts of glucose, tartrate are dissolved in 250 parts of distilled water for 1～5 part successively; Boil the 10min postcooling to normal temperature; Add 10～60 parts of alcohol.Speed of response when adopting reductive agent 1 than the summary height that adopts reductive agent 2 a bit, its effect is the same, reacted difference as a result is also little.Both adopted two kinds of reductive agents all can.
Said technical process is in two steps:
The first step, nickel powder particle surface chemical silvering: at first nickel powder be impregnated in the gelatin solution of 5～20g/L, stir and made suspension in 10 minutes; In suspension, adding 20～60ml/L dilute sulphuric acid, removing oxide compound in 10 minutes 40～50 ℃ of following pickling; The nickel powder of washing is poured in the sensitizing solution, and at room temperature, sensitization 10 minutes is taken out and is cleaned 3 times; Join in the activation solution, at room temperature, stirred 10 minutes, take out and clean 3 times; Nickel powder is joined in the gelatin solution of 5～20g/L, stir and make suspension, pour the silver ammino solution for preparing into,, can make silver-plated nickel powder with the fast reductive agent that drips of dripping of 0.5～2ml/min; In second step, vacuum heat treatment: silver-colored nickel powder is 200～600 ℃ in Heating temperature, and vacuum tightness is: 10Pa, heated 2～3 hours, and promptly get nickeline solid solution alloy powder.
Embodiment 1
At first, impregnated among the gelatin solution 250ml of 10g/L, stir and made suspension in 10 minutes the 25g nickel powder; In suspension, add 25ml/L dilute sulphuric acid 100ml again, removed oxide compound, washing in 10 minutes 45 ℃ of following pickling; Pour the nickel powder of washing the stannous chloride solution 50ml of 10 parts/L into, at room temperature, sensitization 10 minutes is cleaned 3 times; The PdCl that adds 1g/L
2Solution 50ml at room temperature, stirred 10 minutes, cleaned 3 times; Nickel powder is added the gelatin solution 250ml of 10g/L, stir and make suspension, add the silver ammino solution 500ml that the Silver Nitrate of 50g/L is made; With the fast reductive agent 1000ml (with 4ml/L formaldehyde and 100ml/L ethanol) that drips of dripping of 0.5ml/min, stirring causes and records till the no silver ions, filters the cleaning powder and promptly gets silver-plated nickel powder.Is 450 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is: 10Pa, heated 2.5 hours, and promptly obtain nickeline solid solution alloy powder.
Embodiment 2
At first the 20g nickel powder be impregnated among the gelatin solution 200ml of 15/L, stir and made suspension in 10 minutes; In suspension, add 35ml/L dilute sulphuric acid 80ml again, removed oxide compound in 13 minutes, take out washing 48 ℃ of following pickling; Pour the nickel powder of washing the stannous chloride solution 40ml of 10g/L into, at room temperature, sensitization 12 minutes is cleaned 3 times; The PdCl that adds 1g/L
2Solution 40ml at room temperature, stirred 10 minutes, cleaned 3 times; Nickel powder is added the gelatin solution 200ml of 10g/L, stir and make suspension, add the silver ammino solution 400ml that the Silver Nitrate of 50g/L is made; The speed of dripping with 0.8ml/min drips reductive agent (in 11.25 parts of glucose, 250 parts of distilled water of 1.8 parts dissolvings of tartrate, boil the 10min postcooling to normal temperature, add 35 parts of alcohol); Stirring causes and records till the no silver ions, filters the cleaning powder and promptly gets silver-plated nickel powder; Is 450 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is 10Pa, heats 3 hours, promptly obtains nickeline solid solution alloy powder.
Embodiment 3
At first 25 gram nickel powders be impregnated among the gelatin solution 250ml of 10g/L, stir and made suspension in 10 minutes; In suspension, add 25ml/L dilute sulphuric acid 100ml again, removed oxide compound in 10 minutes, wash 3 times 45 ℃ of following pickling; With the nickel powder of washing pour into 10g/L stannous chloride solution 150ml, at room temperature, sensitization 10 minutes is cleaned 3 times; The PdCl that adds 1g/L
2Solution 150ml at room temperature, stirred 10 minutes, cleaned 3 times; Nickel powder is added the gelatin solution 250ml of 10g/L, stir and make suspension, add the silver ammino solution 1500ml that the Silver Nitrate of 50g/L is made; The speed of dripping with 5ml/min drips reductive agent 1500ml (with 7.5ml formaldehyde+600ml ethanol+900ml deionized water), and filtration is cleaned powder and promptly got silver-plated nickel powder.Is 450 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is: 10Pa, heated 3 hours, and promptly obtain nickeline solid solution alloy powder.
Embodiment 4
At first 25 gram nickel powders be impregnated among the gelatin solution 250ml of 10g/L, stir and made suspension in 10 minutes; In suspension, add 25ml/L dilute sulphuric acid 100ml again, removed oxide compound in 10 minutes, take out washing 40～50 ℃ of following pickling; Pour the nickel powder of washing the stannous chloride solution 150ml of 10g/L into, at room temperature, sensitization 10 minutes is cleaned 3 times; The PdCl that adds 1g/L
2Solution 150ml at room temperature, stirred 10 minutes, cleaned 3 times; Nickel powder is added the gelatin solution 250ml of 10g/L, stir and make suspension, add the silver ammino solution 1500ml that the Silver Nitrate of 50g/L is made; The speed of dripping with 5ml/min drips reductive agent 1500ml (in glucose 56.25g, 5g dissolving of tartrate 1250ml distilled water, boil the 10min postcooling to normal temperature, add 125ml alcohol); Stirring causes and records till the no silver ions, filters the cleaning powder and promptly gets silver-plated nickel powder; Is 450 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is 10Pa, heats 3 hours, promptly obtains nickeline solid solution alloy powder
Embodiment 5
At first 25 gram nickel powders be impregnated among the gelatin solution 250ml of 10g/L, stir and made suspension in 10 minutes; In suspension, add 25ml/L dilute sulphuric acid 100ml again, removed oxide compound in 10 minutes, wash 3 times 45 ℃ of following pickling; With the nickel powder of washing pour into 10g/L stannous chloride solution 150ml, at room temperature, sensitization 10 minutes is cleaned 3 times; The PdCl that adds 1g/L
2Solution 150ml at room temperature, stirred 10 minutes, cleaned 3 times; Nickel powder is added the gelatin solution 250ml of 10g/L, stir and make suspension, add the silver ammino solution 750ml that the Silver Nitrate of 50g/L is made; The speed of dripping with 5ml/min drips reductive agent 750ml (with 3.75ml formaldehyde+200ml ethanol+300ml deionized water), and filtration is cleaned powder and promptly got silver-plated nickel powder.Is 450 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is: 10Pa, heated 3 hours, and promptly obtain nickeline solid solution alloy powder.
Embodiment 6:
At first 25 gram nickel powders be impregnated among the gelatin solution 250ml of 10g/L, stir and made suspension in 10 minutes; In suspension, add 25ml/L dilute sulphuric acid 100ml again, removed oxide compound in 10 minutes, take out washing 40～50 ℃ of following pickling; Pour the nickel powder of washing the stannous chloride solution 150ml of 10g/L into, at room temperature, sensitization 10 minutes is cleaned for several times; The PdCl that adds 1g/L
2Solution 150ml at room temperature, stirred 10 minutes, cleaned for several times; Nickel powder is added the gelatin solution 250ml of 10g/L, stir and make suspension, add the silver ammino solution 750ml that the Silver Nitrate of 50g/L is made; The speed of dripping with 5ml/min drips reductive agent 750ml (in glucose 28.13g, 2.5g dissolving of tartrate 625ml distilled water, boil the 10min postcooling to normal temperature, add 62.5ml alcohol); Stirring causes and records till the no silver ions, filters the cleaning powder and promptly gets silver-plated nickel powder; Is 450 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is 10Pa, heats 3 hours, promptly obtains nickeline solid solution alloy powder.
Claims (6)
1, a kind of fire-resistant oxidation resistant base metal powder composition is characterized in that silver-colored nickel powder 30-54 part that coats nickel and contain weight ratio, silver-colored 70-46 part, and said nickel powder particle diameter is 0.5-6 μ m.
2, fire-resistant oxidation resistant base metal powder composition according to claim 1 is characterized in that containing nickel powder 36-52 part of weight ratio, silver-colored 64-48 part, and said nickel powder particle diameter is 2-3 μ m.
3, fire-resistant oxidation resistant base metal powder composition according to claim 1 and 2 is characterized in that containing nickel powder 48-54 part of weight ratio, silver-colored 52-46 part, and said nickel powder particle diameter is 4-6 μ m.
4, a kind of production method for preparing the described fire-resistant oxidation resistant base metal of claim 1 powder composition, comprise technology and preparation sensitizing solution, activation solution, silver ammino solution, reductive agent, following each component all by weight or the volume ratio meter, it is characterized in that said sensitizing solution contains tin protochloride 10-25 part, hydrogenchloride 20-50 part, deionized water 900-1100 part; Said activation solution contains Palladous chloride 0.5-2.5 part, hydrogenchloride 10-100 part, deionized water 900-1000 part; Said silver ammino solution contains Silver Nitrate 111-73 part, ammoniacal liquor 167-110 part, deionized water 900-1000 part; Said reductive agent contains ethanol 100-800 part, formaldehyde 3-15 part, deionized water 200-500 part or glucose 5-20 part, distilled water 220-280 part, alcohol 10-60 part; Said technology is in two steps:
The first step, nickel powder particle surface chemical silvering: at first nickel powder be impregnated in the gelatin solution of 5～20g/L, stir and made suspension in 9-12 minute; In suspension, add 20～60ml/L dilute sulphuric acid, removing oxide compound at 40～50 ℃ of following pickling 8-12 minutes; The nickel powder of washing is poured in the sensitizing solution, at room temperature, sensitization 9-13 minute, taken out and clean 2-3 time; Join in the activation solution, at room temperature, stirred 9-12 minute, take out and clean 2-3 time; Nickel powder is joined in the gelatin solution of 5～20g/L, stir and make suspension, pour the silver ammino solution for preparing into,, can make silver-plated nickel powder with the fast reductive agent that drips of dripping of 0.5～2ml/min;
In second step, vacuum heat treatment: is 200～600 ℃ with silver-plated nickel powder in Heating temperature, and vacuum tightness is: 10Pa, heated 2～3 hours, and promptly get nickeline solid solution alloy powder.
5, the production method of fire-resistant oxidation resistant base metal powder composition according to claim 4, comprise technology and preparation sensitizing solution, activation solution, silver ammino solution, reductive agent, following each component all by weight or the volume ratio meter, it is characterized in that said sensitizing solution contains tin protochloride 15-20 part, hydrogenchloride 25-40 part, deionized water 900-1000 part; Said activation solution contains Palladous chloride 0.8-2.2 part, hydrogenchloride 20-80 part, deionized water 900-1000 part; Said silver ammino solution contains Silver Nitrate 102-76 part, ammoniacal liquor 153-114 part, deionized water 900-1000 part; Said reductive agent contains ethanol 200-600 part, formaldehyde 5-10 part, and deionized water 200-500 part or glucose 8-15 part, distilled water 220-280 part, alcohol 20-40 part, technology is with claim 4.
6, according to the production method of claim 4 or 5 described fire-resistant oxidation resistant base metal powder compositions, comprise technology and preparation sensitizing solution, activation solution, silver ammino solution, reductive agent, following each component all by weight or the volume ratio meter, it is characterized in that said sensitizing solution contains tin protochloride 17-23 part, hydrogenchloride 30-40 part, deionized water 900-1000 part; Said activation solution contains Palladous chloride 1.0-1.8. part, hydrogenchloride 20-80 part, deionized water 900-1000 part; Said silver ammino solution contains Silver Nitrate 83-73 part, ammoniacal liquor 125-110 part, deionized water 900-1000 part; Said reductive agent contains ethanol 200-600 part, formaldehyde 6-8 part, and deionized water 200-500 part or glucose 10-13 part, distilled water 220-280 part, alcohol 20-40 part, technology is with claim 4.
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| EP1777287A1 (en) * | 2005-10-21 | 2007-04-25 | Symrise GmbH & Co. KG | Reducing allergy in perfume oils and fragrances |
| CN101065204B (en) * | 2004-09-29 | 2010-06-16 | Tdk株式会社 | Conductive particle manufacturing method, conductive paste, and electronic component manufacturing method |
| CN1898813B (en) * | 2003-12-26 | 2010-11-24 | 株式会社村田制作所 | Thick-film electrode and multilayer ceramic electronic component |
| CN101717928B (en) * | 2008-10-09 | 2011-05-18 | 北京有色金属研究总院 | Method for preparing compound powder used for abrasion-resistant self-lubricating coating |
| CN102218533A (en) * | 2011-05-17 | 2011-10-19 | 陈钢强 | Silver-coated nickel alloy powder |
| CN102800513A (en) * | 2012-08-10 | 2012-11-28 | 佛山通宝精密合金股份有限公司 | Preparation method for preparing silver nickel materials by means of electrical contacts |
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| JP2017186661A (en) * | 2016-03-31 | 2017-10-12 | Ｄｏｗａエレクトロニクス株式会社 | Silver coated nickel powder and manufacturing method therefor |
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