CN104493171A - Preparation method of flakey silver and zinc oxide electrical contact material - Google Patents
Preparation method of flakey silver and zinc oxide electrical contact material Download PDFInfo
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- CN104493171A CN104493171A CN201410840408.XA CN201410840408A CN104493171A CN 104493171 A CN104493171 A CN 104493171A CN 201410840408 A CN201410840408 A CN 201410840408A CN 104493171 A CN104493171 A CN 104493171A
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Abstract
The invention discloses a preparation method of a flakey silver and zinc oxide electrical contact material. The preparation method specifically comprises the following steps of according to the proportion of to-be-prepared silver and zinc oxide electrical contact material, calculating the required usage amounts of zinc oxide powder and silver nitrate, calculating the usage amount of sodium carbonate, and weighing for preparing; preparing the silver nitrate into 20-40w/w% silver nitrate solution, and uniformly mixing the zinc oxide powder and the silver nitrate solution, so as to obtain a suspension liquid; preparing the sodium carbonate into 10-30w/w% sodium carbonate solution, adding into the suspension liquid, stirring and reacting, generating precipitates, and filtering, so as to obtain the silver nitrate and zinc oxide composite powder; washing the composite powder by water into the neutral property, drying, roasting, crushing, performing hydraulic pressing and sintering on the obtained silver and zinc oxide composite powder, and repeatedly pressing and sintering obtained silver and zinc oxide blanks, so as to obtain the flaky silver and zinc oxide electrical contact material. The preparation method has the advantage that the prepared contact has more uniform metallographic structure.
Description
Technical field
The present invention relates to a kind of preparation method of sheet silver zinc oxide electrical contact material, belong to field of metal matrix composite.
Background technology
Silver zinc oxide contact material has excellent interrupting performance, resistance fusion welding and resistance to arc erosion, and its heavy current impact capacity is not worse than silver tin oxide material, is one of common used material of breaker.As a rule, the preparation technology of silver zinc oxide electrical contact mainly contains three kinds: powder mixing method, internal oxidation and chemical method.Powder mixing method by mechanical mixture mode, silver powder, oxide powder and zinc is simply mixed, and then mixed powder carried out a series of processing such as isostatic pressed, sintering, extruding, finally obtain silver zinc oxide electrical contact.These class methods preparation technology is simple, the process-cycle is short, but easily occurs the problem that mixed powder is assembled.Internal oxidation first silver-colored kirsite is obtained silver zinc oxide composite material by oxidation modifier treatment, then carries out a series of processing such as isostatic pressed, sintering, extruding, finally obtain silver zinc oxide electrical contact.If publication number is the patent of invention etc. of CN101202168A, but easily there is poor oxide region when silver-colored kirsite oxidation in this method, affects the electrical property of material.Another kind of chemical method, but there is heavy-polluted deficiency.
The CN103710608A patent of invention of applying for before the applicant, disclose a kind of preparation method containing additive silver zinc oxide electrical contact material, first the method is joined in silver powder or oxide powder and zinc by the salt compounds solution containing Addition ofelements to make slurry, dried, broken, sieve after mix with oxide powder and zinc or silver powder, obtain Ag-ZnO mixed powder, afterwards it is processed into electrical contact through isostatic pressed, sintering, extruding etc.The method improves the phenomenon of traditional blending processes of powders additive segregation preferably, makes additive be no longer simple mechanical mixture, but is combined together with matrix well by coated, makes the Ag-ZnO material of gained have more outstanding performance.But composite mortar likely can cause the precipitation of Addition ofelements on silver matrix to produce the phenomenon of segregation in drying course because the speed that evaporates is uneven, in addition, silver powder containing additive (or the oxide powder and zinc containing additive) is comparatively large with the density difference of oxide powder and zinc (or silver powder), and two kinds of powders also there will be zinc oxide and to unite the phenomenon of assembling in mixed process.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of technique simply, substantially not to be existed zinc oxide and to unite the preparation method of sheet silver zinc oxide electrical contact material of clustering phenomena, silver zinc oxide electrical contact metallographic structure obtained by this method evenly, there is excellent processing characteristics.
The preparation method of sheet silver zinc oxide electrical contact material of the present invention, comprises the following steps:
1) calculate according to the material mixture ratio of the silver zinc oxide electrical contact of required preparation needed for oxide powder and zinc and the consumption of silver nitrate, and generate the consumption of the sodium carbonate needed for silver carbonate according to the Dosage calculation silver nitrate of silver nitrate and sodium carbonate reaction, take for subsequent use; Get silver nitrate is made into 20 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, oxide powder and zinc and liquor argenti nitratis ophthalmicus are placed in reactor, stir, obtain the suspension containing silver nitrate and zinc oxide;
2) get sodium carbonate is made into 10 ~ 30w/w% sodium carbonate liquor by water-soluble solution, join step 1) stirring reaction in the suspension of gained, there is precipitation to generate, filter, obtain the composite powder of silver carbonate and zinc oxide;
3) silver carbonate of gained and the composite powder of zinc oxide are washed to neutrality, carry out roasting after drying, pulverizing, then pulverize, obtain Ag-ZnO composite powder;
4) by shaping for the Ag-ZnO composite powder oil pressure of gained, and then be placed in oxygen-containing atmosphere and sinter, obtain Ag-ZnO briquet;
5) gained Ag-ZnO briquet carries out multiple pressure, resintering, namely obtains sheet silver zinc oxide electrical contact material.
The present invention is obtained by reacting the composite powder of silver carbonate and zinc oxide, due to the density (5.606g/cm of oxide powder and zinc with sodium carbonate and the silver nitrate suspension containing oxide powder and zinc
3) and react the silver carbonate (6.077g/cm generated
3) density be close; thus oxide powder and zinc and silver carbonate particle can be made to be mixed to get evenly; oxide powder and zinc is made more to be evenly distributed in silver carbonate matrix; effectively improve oxide powder and zinc in prior art to unite the phenomenon of assembling, thus make gained silver zinc oxide electrical contact material have uniform metallographic structure.
The step 1 of said method) in, in the silver zinc oxide electrical contact material of described needs preparation, zinc oxide content is 1 ~ 30wt%, and surplus is silver; The preferred zinc oxide content that is chosen as is 8 ~ 12wt%, and surplus is silver.In this step, described oxide powder and zinc adopts particle mean size to be the oxide powder and zinc of 1 ~ 20 μm usually, preferably adopts particle mean size to be 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 sodium carbonate is generally 53/170 ~ 63/170 of silver nitrate consumption, is more preferably 58/170.
The step 2 of said method) in, the speed that adds of described sodium carbonate liquor is preferably 0.1 ~ 1L/min; The concentration of described sodium carbonate liquor 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 said 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 carbonate and zinc oxide under 100 ~ 150 DEG C of conditions, usually needs the time of 12 ~ 18h; Normally the composite powder pulverizing of dried silver carbonate and zinc oxide 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 Ag-ZnO composite powder.
The step 4 of said method) in, when oil pressure is shaping, briquetting pressure is generally 8 ~ 12T/cm
2; Normally the briquet after shaping is placed in oxygen-containing atmosphere and under 880 ~ 920 DEG C of temperature conditions, sinters 4 ~ 8h, to obtain Ag-ZnO briquet.
The step 5 of said method) in, the pressure of described multiple pressure is 12 ~ 18T/cm
2, described resintering be by multiple pressure after Ag-ZnO briquet be placed in vacuum or oxygen-containing atmosphere resintering 4 ~ 8h under 880 ~ 920 DEG C of conditions.
Compared with prior art, feature of the present invention is:
1, the present invention is obtained by reacting the composite powder of silver carbonate and zinc oxide, due to the density (5.606g/cm of oxide powder and zinc with sodium carbonate and the silver nitrate suspension containing oxide powder and zinc
3) and react the silver carbonate (6.077g/cm generated
3) density be close; thus oxide powder and zinc and silver carbonate particle can be made to be mixed to get evenly; oxide powder and zinc is made more to be evenly distributed in silver carbonate matrix; effectively improve oxide powder and zinc in prior art to unite the phenomenon of assembling, thus make gained silver zinc oxide electrical contact material have uniform metallographic structure.
2, the method for the invention technique is simple, to human body and environmental pollution little, be applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure (200 ×) of the contact material that the embodiment of the present invention 1 obtains;
Fig. 2 is the metallographic structure figure (200 ×) of the contact material that the embodiment of the present invention 2 obtains.
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 oxide powder and zinc and silver nitrate consumption is calculated according to preparation 10kgAg-ZnO (10) material mixture ratio, take oxide powder and zinc 1kg, silver nitrate 14.167kg, weighing sodium carbonate 4.833kg again, for subsequent use, wherein oxide powder and zinc 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, the liquor argenti nitratis ophthalmicus of the oxide powder and zinc taken and preparation is placed in reactor, stir (stirring 120min), obtains the suspension containing silver nitrate and zinc oxide;
2) sodium carbonate liquor that sodium carbonate water is made into 30w/w% is got, under stirring condition, the sodium carbonate liquor (drop rate is 0.5L/min) adding 30w/w% in the suspension of silver nitrate and zinc oxide is contained to above-mentioned, reaction 0.5h, obtains the composite powder of silver carbonate and zinc oxide after filtration;
3) by the above-mentioned silver carbonate that is obtained by reacting and zinc oxide compound powder end washed with de-ionized water to neutral, 15h is dried in an oven subsequently with 120 DEG C of temperature, then the silver carbonate of oven dry and zinc oxide compound powder end are placed in bipyramid blender broken (rotating speed 25r/min, time 1h); Gained powder is placed in potoven in 450 DEG C of temperature calcination 4h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again, then crosses 200 eye mesh screens, obtain Ag-ZnO composite powder after taking-up;
4) shaping on hydraulic press (briquetting pressure is 10T/cm to gained composite powder
2), and the pressed compact after shaping is placed in air with 880 DEG C of temperature sintering 4h, obtain Ag-ZnO briquet;
5) gained Ag-ZnO briquet carries out multiple pressure (multiple pressure pressure is 15T/cm
2), and the Ag-ZnO briquet after multiple pressure is placed in air with 880 DEG C of temperature resintering 4h, obtain sheet Ag-ZnO (Ag-ZnO (10)) electrical contact material.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 1, the metallographic structure of contact product prepared of technical scheme is even as seen from the figure, and tiny Zinc oxide particles is evenly distributed in silver matrix.
Embodiment 2
1) first required oxide powder and zinc and silver nitrate consumption is calculated according to preparation 10kg Ag-ZnO (30) material mixture ratio, take oxide powder and zinc 3kg, silver nitrate 11.019kg, weighing sodium carbonate 3.759kg again, for subsequent use, wherein oxide powder and zinc employing particle mean size is the powder of 10 ~ 20 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 oxide powder and zinc taken and preparation is placed in reactor, stir (stirring 80min), obtains the suspension containing silver nitrate and zinc oxide;
2) sodium carbonate liquor that sodium carbonate water is made into 10w/w% is got, under stirring condition, contain to above-mentioned the sodium carbonate liquor (drop rate is 1L/min) adding 10w/w% in the suspension of silver nitrate and zinc oxide, reaction 1h, obtains the composite powder of silver carbonate and zinc oxide after filtration;
3) by the above-mentioned silver carbonate that is obtained by reacting and zinc oxide compound powder end washed with de-ionized water to neutral, 18h is dried in an oven subsequently with 100 DEG C of temperature, then the silver carbonate of oven dry and zinc oxide compound powder end are placed in bipyramid blender broken (rotating speed 25r/min, time 1h); Gained powder is placed in potoven in 500 DEG C of temperature calcination 6h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again, then crosses 200 eye mesh screens, obtain Ag-ZnO composite powder after taking-up;
4) shaping on hydraulic press (briquetting pressure is 8T/cm to gained composite powder
2), and the pressed compact after shaping is placed in air with 900 DEG C of temperature sintering 8h, obtain Ag-ZnO briquet;
5) gained Ag-ZnO briquet carries out multiple pressure (multiple pressure pressure is 18T/cm
2), and the Ag-ZnO briquet after multiple pressure is placed in air with 920 DEG C of temperature resintering 6h, obtain sheet Ag-ZnO (Ag-ZnO (30)) electrical contact material.
Carry out metallographic structure analysis to gained contact material, as Fig. 2 shows, the metallographic structure of contact product prepared of technical scheme is even as seen from the figure, and tiny Zinc oxide particles is evenly distributed in silver matrix.
Embodiment 3
Repeat the method for embodiment 1, unlike:
Step 1) in, calculate required oxide powder and zinc and silver nitrate consumption according to preparation Ag-ZnO (1) material mixture ratio and take for subsequent use, take appropriate sodium carbonate more for subsequent use simultaneously, wherein oxide powder and zinc employing particle mean size is the powder of 5 ~ 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 carbonate liquor is 25w/w%;
Step 5) in, the temperature of reduction is 900 DEG C, and the time is 6h.
Embodiment 4
Repeat the method for embodiment 2, unlike:
Step 1) in, calculate required oxide powder and zinc and silver nitrate consumption according to preparation Ag-ZnO (20) material mixture ratio and take for subsequent use, take appropriate sodium carbonate more for subsequent use simultaneously, wherein oxide powder and zinc employing particle mean size is the powder of 5 ~ 8 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 carbonate liquor is 15w/w%.
The contact material that embodiment 1 is obtained carries out Performance Detection, and compares with the contact product that existing routine mixes the Ag-ZnO that powder-monolithic pressing obtains, result as described in Table 1:
Table 1:
As shown in Table 1, the performance of silver zinc oxide contact material that prepared by technical scheme is better than existing routine and mixes powder-monolithic pressing silver zinc oxide contact material performance.
Claims (5)
1. a preparation method for sheet silver zinc oxide electrical contact material, is characterized in that comprising the following steps:
1) calculate according to the material mixture ratio of the silver zinc oxide electrical contact of required preparation needed for oxide powder and zinc and the consumption of silver nitrate, and generate the consumption of the sodium carbonate needed for silver carbonate according to the Dosage calculation silver nitrate of silver nitrate and sodium carbonate reaction, take for subsequent use; Get silver nitrate is made into 20 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, oxide powder and zinc and liquor argenti nitratis ophthalmicus are placed in reactor, stir, obtain the suspension containing silver nitrate and zinc oxide;
2) get sodium carbonate is made into 10 ~ 30w/w% sodium carbonate liquor by water-soluble solution, join step 1) stirring reaction in the suspension of gained, there is precipitation to generate, filter, obtain the composite powder of silver carbonate and zinc oxide;
3) silver carbonate of gained and the composite powder of zinc oxide are washed to neutrality, carry out roasting after drying, pulverizing, then pulverize, obtain Ag-ZnO composite powder;
4) by shaping for the Ag-ZnO composite powder oil pressure of gained, and then be placed in oxygen-containing atmosphere and sinter, obtain Ag-ZnO briquet;
5) gained Ag-ZnO briquet carries out multiple pressure, resintering, namely obtains sheet silver zinc oxide electrical contact material.
2. preparation method according to claim 1, is characterized in that: step 1) in, need in the silver zinc oxide electrical contact material of preparation, zinc oxide content is 1 ~ 30wt%, 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 consumption of sodium carbonate is 53/170 ~ 63/170 of silver nitrate consumption.
5. preparation method according to claim 1, is characterized in that: step 2) in, the concentration of sodium carbonate liquor is 15 ~ 25w/w%.
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Cited By (2)
| 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 |
| CN108179297A (en) * | 2018-01-20 | 2018-06-19 | 云南大学 | A kind of new A g-ZnO electrical contact materials and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105965022B (en) * | 2015-12-29 | 2018-04-10 | 桂林电器科学研究院有限公司 | A kind of processing method of sheet silver-graphite electrical contact material |
| CN108179297A (en) * | 2018-01-20 | 2018-06-19 | 云南大学 | A kind of new A g-ZnO electrical contact materials and preparation method thereof |
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Application publication date: 20150408 |