CN102389981A - Method for continuously and homogeneously preparing silver tin oxide material - Google Patents
Method for continuously and homogeneously preparing silver tin oxide material Download PDFInfo
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- CN102389981A CN102389981A CN2011101888261A CN201110188826A CN102389981A CN 102389981 A CN102389981 A CN 102389981A CN 2011101888261 A CN2011101888261 A CN 2011101888261A CN 201110188826 A CN201110188826 A CN 201110188826A CN 102389981 A CN102389981 A CN 102389981A
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Abstract
The invention discloses a method for continuously and homogeneously preparing a silver tin oxide material, and the method comprises the following steps: firstly, homogenizing a tin oxide sizing agent; preparing a silver nitrate solution according to a content ratio of silver and tin oxide; mixing the silver nitrate solution with the tin oxide sizing agent; respectively injecting a sizing agent mixture and an ascorbic acid solution into a rotary type reaction kettle; reacting while splashing and rotating, and additionally utilizing an ultrasonic vibrator to homogenize, thereby acquiring uniformly distributed silver tin oxide powder; and molding and then preparing into an electrical contact. The method can be used for overcoming the difficulties that distribution of tin oxide grains in a silver substrate is not uniform enough, processing and electric properties are unstable, and the like. According to the method, the probability of powder conglobation is efficiently reduced, the distribution of the acquired silver tin oxide powder is more uniform, and the processing property and electric property of the prepared material are better and stable. The process of the method is simple. The method can be applied to continuous production, thereby acquiring products with stable property. The method is suitable for batch production and industrialization production. Preparing processes all meet the environmentally-friendly demand.
Description
Technical field
The present invention relates to the technical field of electrical contact material, particularly a kind of preparation of silver-tin oxide material.
Background technology
The silver oxide material is main used as electric contacts material, and domestic and international for a long time employed silver oxide contact is maximum with Agcdo.Silver cadmium oxide material once once had been that the mesolow device for switching is used topmost contact material, and it has good arc extinction performance, in the moderate duty switch, has the title of " omnipotent contact ".Yet; Harsh performance requirements such as the miniaturization that constantly electric contact is proposed along with electric switch, high reliability, long-life; Silver cadmium oxide material is not only resistance to wearing, is appearing obvious deficiency on the performance indications such as anti-melting welding, anti-electric arc etch; And the Cd steam that the Agcdo contact striking produces is poisonous, does not meet environmental requirement, and the silver cadmium oxide contact material has been forbidden in Europe indefinite duration.As the topmost substitute of present silver cadmium oxide material, the silver tin oxide material development in recent years is rapid, is widely used in low-voltage electrical apparatuses such as relay, contactor, breaker.At present, the preparation method of sliver oxidized tin contactor materials mainly contains alloy inner oxidation method and powder metallurgic method.Adopt the alloy inner oxidation legal system to be equipped with silver tin oxide material; Be about to silver, tin proportioning founding according to a certain percentage processing; The silver-colored ashbury metal base material of gained is processed product forms such as a material, sheet material through following process, through high temperature, high oxygen pressure, long-time in oxidation processes, obtain finished product.This technology is suitable for producing in batches, but in interior oxidizing process, because oxygen atom needs in the DB of alloy, spread, the Gradient distribution of its concentration will cause material internal oxygen-depleted zone or zoneofoxidation not to occur, and this electric property to material is unfavorable.Simultaneously, when tin content just is difficult to carry out oxidation greater than 5%, must be added with the element that helps oxidation, such as indium, bismuth etc. for this reason.Prepare sliver oxidized tin contactor materials with powder metallurgic method in recent years and obtain fast development, but the overall view As-Is prepares siller tin oxide electric contact with powder metallurgic method and remains in following deficiency: (1) tin ash powder distributes inadequately evenly, assembles; (2) tin ash and silver matrix material wellability are not enough, a little less than the intergranular adhesion, are prone to macroscopic view and micro-crack during use, poor processability; (3) criticize and batch between material property inconsistent.These all affect the processing characteristics and the electric property of electrical contact material.
Summary of the invention
The objective of the invention is to overcome the weak point of above-mentioned prior art; The method that a kind of continuous homogenising prepares silver tin oxide material is proposed; The electrical contact material of this method preparation has characteristics such as resistivity is low, even tissue is careful, processing characteristics is good; Its preparation technology is simple, can realize continuous batch production; The raw material that the present invention uses, the equal compliance with environmental protection requirements of preparation process is suitable for megatrend.
The objective of the invention is to realize through following technical scheme: a kind of continuous homogenising prepares the method for silver tin oxide material, and the chemical analysis of material is silver and tin oxide, wherein; The tin oxide percentage by weight is 8%～22%; Surplus is a silver, and it is characterized in that step is: (1) is selected particle diameter for use is 1～6um stannic oxide powder; Add water and be prepared into the tin oxide slurry, through ultrasonic vibrator the tin oxide slurry is carried out the ultrasonic wave homogenising and handle; (2) according to silver and tin oxide content ratio; The preparation liquor argenti nitratis ophthalmicus mixes being equipped with good liquor argenti nitratis ophthalmicus and tin oxide slurry, is prepared into mixed solution; Be contained in the storage tank, also mixed solution carried out the ultrasonic wave homogenising and handle through ultrasonic vibrator; (3) prepare ascorbic acid solution as reducing agent, and be contained in another storage tank; (4) extract silver nitrate and tin oxide mixed solution and ascorbic acid solution in the storage tank respectively through two pumps; Be transported to simultaneously in the rotary agitated reactor; Solution in the agitated reactor is carried out rotary type disperse, open ultrasonic vibrator simultaneously, let the reduction reaction of silver nitrate in sputter, carry out; Let the simple substance silver after reducing be compounded in equably on the surface of tin oxide, on powder catcher, collect the silver-tin oxider composite powder that is evenly distributed; (5) the siller tin oxide powder of collecting is carried out drying, screening, moulding, process electrical contact material.Further, the concentration of liquor argenti nitratis ophthalmicus is 3-25%, and the concentration of tin oxide slurry is 10-50%, and ascorbic acid solution concentration is 1-10%.The mixed solution of silver nitrate and tin oxide and ascorbic acid solution get into rotary agitated reactor according to even flow, and the by-pass valve control flow is 200-400L/h.The frequency of ultrasonic vibrator is 10-50KHz.The time that the tin oxide slurry carries out the processing of ultrasonic wave homogenising is 10-20 minute.
Major advantage of the present invention has: 1, the present invention proposes the ultrasonic wave homogenising first and prepares silver tin oxide material; Use rotary agitated reactor; Silver nitrate and tin oxide mixed solution and ascorbic acid solution carry out priming reaction in the splash in agitated reactor; The powder of reaction solution and generation is further evenly disperseed with rotary type by disperser, has reduced the chance that powder is reunited effectively; Because reaction is in flowing, to carry out, the time that reaction solution is stopped in agitated reactor is identical, thereby has guaranteed the uniformity of composite powder.2, can pass through the flow velocity and the concentration of control reaction solution, thereby reach the effect of control gained powder size.3, the silver composite tin oxide composite powder that generates owing to reaction does not rest in the agitated reactor, but flows away with water, needn't shut down, and realizes producing continuously, produces material property and stablizes.4, the silver tin oxide material plastic deformation ability prepared of the present invention is good, is prone to extruding, rolling or wire drawing, and electrical property can satisfy client's instructions for use.5, the present invention is raw materials used is easy to get, and simple for process, cost is lower, is applicable to mass, suitability for industrialized production.6, the raw material of the present invention's use, the equal compliance with environmental protection requirements of preparation process is suitable for megatrend.In addition, the present invention also can be applicable in the preparation of other composite, and is applied widely.
Description of drawings
Fig. 1 is a process route chart of the present invention.
The specific embodiment
Embodiment 1: preparation siller tin oxide (10) material
(1) taking by weighing particle diameter is 0.762 kilogram of 1～2um stannic oxide powder, is prepared into slurry, and adds activator, opens ultrasonic vibrator, carries out 10～20 minutes homogenising and handles.The concentration that is prepared into slurry at last is 30%.
(2) take by weighing 10 kilograms of silver nitrate crystals, be formulated as the liquor argenti nitratis ophthalmicus of concentration 5%, simultaneously the tin oxide slurry is added in the liquor argenti nitratis ophthalmicus, stirred 30 minutes, process uniform mixed liquor through ultrasonic vibrator.
(3) 2% an amount of ascorbic acid solution of preparation.
(4) extract silver nitrate and the mixed solution and the ascorbic acid solution of tin oxide in the storage tank simultaneously through two pumps, adopt valve controlling flow amount 300L/h, be transported to the agitated reactor the inside simultaneously from the left side of agitated reactor; And the solution that reacts is carried out rotary type disperse; Open ultrasonic vibrator simultaneously, frequency 20KHz lets the reduction reaction of silver nitrate in sputter, carry out; The siller tin oxide composite powder that reaction obtains flows to powder catcher with water; Through washing, temperature 100-200 ℃ of drying finally obtains silver-tin oxider composite powder.
(5) with silver-tin oxider composite powder through 200 mesh sieve branches, the diameter of packing into is in the punching block of Φ 120, carries out isostatic compaction.Pressure is 350MPa, and ingot blank is prepared in pressurize 1 minute.
(6) ingot blank after the moulding is carried out vacuum-sintering, 900 ℃ of sintering temperatures, vacuum 10
-3-10
-2Pa, 4 hours time.
(7) ingot blank behind the sintering is pushed 850 ℃ of extrusion temperatures.Extrusion ratio 120.
(8) wire rod that obtains of extruding is at 750 ℃ of annealing 1h.
(9) passing through wire drawing at last, is product with the wire-form, or makes into the electrical pickoff product again.
Product is made 100-500 times of metallographic observation of cross section and longitudinal section respectively, finds to be evenly distributed at silver-colored body at tin oxide, and the chemical composition of testing product, silver-colored average content is 89.5%.
Embodiment 2: preparation siller tin oxide (12) material
(1) taking by weighing particle diameter is 1.361 kilograms of 3～5um stannic oxide powders, is prepared into slurry, and adds activator, opens ultrasonic vibrator, carries out 10～20 minutes homogenising and handles.The concentration that is prepared into slurry at last is 25%.
(2) take by weighing 15 kilograms of silver nitrate crystals, be formulated as the liquor argenti nitratis ophthalmicus of concentration 4%, simultaneously the tin oxide slurry is added in the liquor argenti nitratis ophthalmicus, stirred 30 minutes, process uniform mixed liquor through ultrasonic vibrator.
(3) 5% an amount of ascorbic acid solution of preparation.
(4) remaining technology is identical with embodiment 1.
The chemical composition of testing product, silver-colored average content are 87.6%.Wire rod is done metallographic detect, the processing characteristics analysis, the result shows that prepared wire product has favorable tissue uniformity and processing characteristics equally.
Embodiment 3: preparation siller tin oxide (15) material
(1) taking by weighing particle diameter is 0.9 kilogram of 4～6um stannic oxide powder, is prepared into slurry, and adds activator, opens ultrasonic vibrator, carries out 10～20 minutes homogenising and handles.The concentration that is prepared into slurry at last is 20%.
(2) take by weighing 8 kilograms of silver nitrate crystals, be formulated as the liquor argenti nitratis ophthalmicus of concentration 4%, simultaneously the tin oxide slurry is added in the liquor argenti nitratis ophthalmicus, stirred 30 minutes, process uniform mixed liquor through ultrasonic vibrator.
(3) 5% an amount of ascorbic acid solution of preparation.
(4) remaining technology is identical with embodiment 1.
The chemical composition of testing product, silver-colored average content are 85.1%.Wire rod is done metallographic detect, with respect to example 1 and example 2, institute's oxycompound proportion is more in this material, and oxide has less clustering phenomena; Its processing characteristics is analyzed,, still had good processing properties though processing characteristics decreases with respect to example 1 and example 2 prepared materials.
Silver tin oxide material with resulting silver tin oxide material of above-mentioned process and the preparation of other method contrasts like following table 1:
With respect to other method, the silver tin oxide material of the present invention preparation has lower resistivity, higher percentage elongation, show that the present invention prepares silver tin oxide material have better electric conductivity and processing characteristics.
With siller tin oxide (12) and the siller tin oxide (12) of other method preparation and the rivet that Agcdo (12) is processed into specification of the same race of the present invention's preparation, the relay that is assemblied in specification of the same race carries out electric performance test respectively.The electric performance test condition is: coil voltage 12VDC; Environment temperature: 25 ℃; Contact load: 20A*250VAC, resistive; Operating frequency: 40 times/minute; Dutycycle: 1: 1; Require electric life 100,000 times more than the number, bond 5 times or continuous bond for 3 times be judged to be defective.The electrical endurance test result is as shown in table 2.
| The preparation method | Title material | Life-span number of times (ten thousand times) | Remarks |
| The present invention | Siller tin oxide (12) | 12-15 | There is not bonding |
| Chemical coprecipitation | Siller tin oxide (12) | 9-12 | The secondary bonding |
| The alloy inner oxidation method | Siller tin oxide (12) | 13-17 | The secondary bonding |
| Powder mixing method | Agcdo (12) | 8-12 | Once sticking dead |
Table 2
Above electrical performance test result shows that the sliver oxidized tin contactor materials of the present invention's preparation has good electrical properties.
Certainly, just list here and lifted several kinds of preferred implementation, the protection category that other is equal to, method roughly the same, technology all should belong to this patent repeats no more here.
Claims (5)
1. a continuous homogenising prepares the method for silver tin oxide material, and the chemical analysis of material is silver and tin oxide, and wherein, the tin oxide percentage by weight is 8%～22%, and surplus is a silver, it is characterized in that step is:
(1) selecting particle diameter for use is 1～6um stannic oxide powder, adds water and is prepared into the tin oxide slurry, through ultrasonic vibrator the tin oxide slurry is carried out the ultrasonic wave homogenising and handles;
(2) according to silver and tin oxide content ratio; The preparation liquor argenti nitratis ophthalmicus mixes being equipped with good liquor argenti nitratis ophthalmicus and tin oxide slurry, is prepared into mixed solution; Be contained in the storage tank, also mixed solution carried out the ultrasonic wave homogenising and handle through ultrasonic vibrator;
(3) prepare ascorbic acid solution as reducing agent, and be contained in another storage tank;
(4) extract silver nitrate and tin oxide mixed solution and ascorbic acid solution in the storage tank respectively through two pumps; Be transported to simultaneously in the rotary agitated reactor; Solution in the agitated reactor is carried out rotary type disperse, open ultrasonic vibrator simultaneously, let the reduction reaction of silver nitrate in sputter, carry out; Let the simple substance silver after reducing be compounded in equably on the surface of tin oxide, on powder catcher, collect the silver-tin oxider composite powder that is evenly distributed;
(5) the siller tin oxide powder of collecting is carried out drying, screening, moulding, process electrical contact material.
2. the method for silver tin oxide material according to claim 1 is characterized in that, the concentration of liquor argenti nitratis ophthalmicus is 3-25%, and the concentration of tin oxide slurry is 10-50%, and ascorbic acid solution concentration is 1-10%.
3. the method for silver tin oxide material according to claim 1 and 2 is characterized in that, the mixed solution of silver nitrate and tin oxide and ascorbic acid solution get into rotary agitated reactor according to even flow, and the by-pass valve control flow is 200-400L/h.
4. the method for silver tin oxide material according to claim 1 and 2 is characterized in that, the frequency of ultrasonic vibrator is 10-50KHz.
5. the method for silver tin oxide material according to claim 1 and 2 is characterized in that, the time that the tin oxide slurry carries out the processing of ultrasonic wave homogenising is 10-20 minute.
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| CN2011101888261A CN102389981A (en) | 2011-06-21 | 2011-06-21 | Method for continuously and homogeneously preparing silver tin oxide material |
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Cited By (13)
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| CN104073666A (en) * | 2014-07-21 | 2014-10-01 | 温州宏丰电工合金股份有限公司 | Preparation method for particle dispersion strengthening metal basal composite material |
| CN104087777A (en) * | 2014-07-21 | 2014-10-08 | 温州宏丰电工合金股份有限公司 | Method for preparing particle dispersion reinforced metal matrix composite material |
| CN104117684A (en) * | 2014-08-11 | 2014-10-29 | 郴州市金贵银业股份有限公司 | Preparation method of silver tin oxide electric contact materials |
| CN104493170A (en) * | 2014-12-30 | 2015-04-08 | 桂林电器科学研究院有限公司 | Preparation method of flakey or rivet-shaped silver and tungsten electrical contact material |
| CN104907581A (en) * | 2015-06-20 | 2015-09-16 | 浙江大学 | Preparation method of material in which globular micron stannic oxide is loaded with micron and nano silver particles |
| CN105039767A (en) * | 2015-08-07 | 2015-11-11 | 西安工程大学 | Method for preparing silver tin oxide electrical contact alloy |
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| CN104073666B (en) * | 2014-07-21 | 2016-09-14 | 温州宏丰电工合金股份有限公司 | A kind of preparation method of particle dispersion-strengthened metal based composites |
| CN104087777A (en) * | 2014-07-21 | 2014-10-08 | 温州宏丰电工合金股份有限公司 | Method for preparing particle dispersion reinforced metal matrix composite material |
| CN104073666A (en) * | 2014-07-21 | 2014-10-01 | 温州宏丰电工合金股份有限公司 | Preparation method for particle dispersion strengthening metal basal composite material |
| CN104117684A (en) * | 2014-08-11 | 2014-10-29 | 郴州市金贵银业股份有限公司 | Preparation method of silver tin oxide electric contact materials |
| CN104117684B (en) * | 2014-08-11 | 2016-06-22 | 郴州市金贵银业股份有限公司 | A kind of preparation method of tin-oxygen-silver electric contact material |
| US10639722B2 (en) | 2014-12-12 | 2020-05-05 | Schneider Electric Industries Sas | Preparation method and preparation device for silver-metal oxide electrical contact material and application of the material |
| WO2016091216A1 (en) * | 2014-12-12 | 2016-06-16 | 施耐德电气工业公司 | Silver-metal oxide electrical contact tip material preparation method, device and application |
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| CN104907581A (en) * | 2015-06-20 | 2015-09-16 | 浙江大学 | Preparation method of material in which globular micron stannic oxide is loaded with micron and nano silver particles |
| CN105039767A (en) * | 2015-08-07 | 2015-11-11 | 西安工程大学 | Method for preparing silver tin oxide electrical contact alloy |
| CN105112706A (en) * | 2015-08-07 | 2015-12-02 | 西安工程大学 | Preparation method of silver zinc oxide contact alloy |
| CN105695791A (en) * | 2016-02-25 | 2016-06-22 | 昆明贵金属研究所 | Novel silver rare earth oxide alloy and preparing method thereof |
| CN105695791B (en) * | 2016-02-25 | 2017-12-15 | 昆明贵金属研究所 | A kind of new silver rare earth oxide alloy and preparation method thereof |
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| CN106807953A (en) * | 2017-01-23 | 2017-06-09 | 西安工程大学 | A kind of tin oxide disperse strengthens the preparation method of silver-based electric contact alloy |
| CN106807953B (en) * | 2017-01-23 | 2018-07-10 | 西安工程大学 | A kind of preparation method of tin oxide disperse enhancing silver-based electric contact alloy |
| CN107502774A (en) * | 2017-09-25 | 2017-12-22 | 常州市沃兰特电子有限公司 | A kind of preparation method of silver tin oxide material |
| CN113637866A (en) * | 2021-08-09 | 2021-11-12 | 江西蓝微电子科技有限公司 | Graphene bonded silver wire and preparation method thereof |
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Application publication date: 20120328 |