CN104505191A - Indium-tin-oxide-containing silver tin oxide electrical contact material preparation method - Google Patents
Indium-tin-oxide-containing silver tin oxide electrical contact material preparation method Download PDFInfo
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Abstract
The invention discloses an indium-tin-oxide-containing silver tin oxide electrical contact material preparation method. The preparation method specifically includes: calculating required dosage of tin oxide powder, indium nitrate and silver nitrate according to a material ratio required by preparing an indium-tin-oxide-containing silver tin oxide electrical contact, and calculating dosage of sodium hydroxide A according to the dosage of the indium nitrate; calculating dosage of sodium hydroxide B according to the dosage of the silver nitrate; weighing for standby; preparing solutions by the weighed substances, and dividing the tin oxide powder into two parts, namely the tin oxide powder A and the tin oxide powder B; enabling the sodium hydroxide A to react with indium nitrate suspension liquid containing the tin oxide powder A to obtain indium hydroxide and tin oxide composite powder, subjecting the composite powder to calcination and ball grinding to obtain indium tin oxide powder, adding the indium tin oxide powder into suspension liquid formed by the tin oxide powder B and the silver nitrate solution, and enabling the suspension liquid with the indium tin oxide powder to react with the sodium hydroxide B to obtain silver oxide, tin oxide and indium tin oxide powder composite powder; subjecting the composite powder to washing, drying, calcination, forming, sintering, re-pressing and resintering to obtain the indium-tin-oxide-containing silver tin oxide electrical contact material.
Description
Technical field
The present invention relates to a kind of preparation method of the siller tin oxide electric contact material containing stannic acid indium, belong to field of metal matrix composite.
Background technology
In recent years, siller tin oxide contact has been widely used in various low-voltage electrical apparatus as the best replacer of poisonous silver cadmium oxide contact.Sliver oxidized tin contactor materials has excellent resistance to wear, resistance fusion welding and resistance to arc erosion, but it exists the shortcomings such as contact resistance is large, temperature rise is high, has had a strong impact on the electric property of electrical equipment.
Study discovery through forefathers, the siller tin oxide electric contact material being added with one or more oxides in bismuth oxide, cupric oxide and indium oxide not only has good resistance to wear, resistance fusion welding and resistance to arc erosion, improves the electric property of electrical equipment well.Have not yet to see the relevant report of the siller tin oxide electric contact material of doping stannic acid indium.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of the siller tin oxide electric contact material containing stannic acid indium that a kind of technique is simple, stannic acid indium is evenly distributed in basis material, the siller tin oxide electric contact metallographic structure containing stannic acid indium obtained by this method evenly, there is excellent resistance to electric abrasioning performance.
The preparation method of the siller tin oxide electric contact material containing stannic acid indium of the present invention, comprises the following steps:
1) calculate according to the material mixture ratio of the siller tin oxide electric contact containing stannic acid indium of required preparation needed for the consumption of putty powder, indium nitrate and silver nitrate, generate the consumption of the NaOH needed for indium hydroxide according to the Dosage calculation indium nitrate of indium nitrate and NaOH reaction, represent with NaOH A; Generate the consumption of the NaOH needed for silver oxide according to the Dosage calculation silver nitrate of silver nitrate and NaOH reaction, represent with NaOH B; Take above-mentioned substance, for subsequent use; Get silver nitrate is made into 20 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, get the water-soluble solution of indium nitrate and be made into indium nitrate solution; Get the water-soluble solution wiring solution-forming of NaOH A, obtain NaOH solution A; Get NaOH B is made into 10 ~ 30w/w% solution by water-soluble solution, obtain NaOH B solution; The putty powder taken is divided into two parts, and portion is putty powder A, and its amount is for can react with indium nitrate and NaOH the amount that the indium hydroxide generated reacts completely to generate stannic acid indium, and another part is putty powder B;
2) putty powder A and indium nitrate solution are placed in reactor, stir, obtain the suspension of putty powder A and indium nitrate; In this suspension, add NaOH solution A, stirring reaction, filter, obtain the composite powder of putty powder A and indium hydroxide;
3) the putty powder A of gained and the composite powder of indium hydroxide are washed to neutrality, drying is placed on calcination in oxygen-containing atmosphere, then ball milling, obtains stannic acid indium powder;
4) putty powder B and liquor argenti nitratis ophthalmicus are placed in another reactor, stir, obtain the suspension of silver nitrate and putty powder B; Add step 3 wherein) the stannic acid indium powder of gained, then add NaOH B solution, stirring reaction, filter, obtain silver oxide, tin oxide and stannic acid indium composite powder;
5) silver oxide of gained, tin oxide and stannic acid indium composite powder are washed to neutrality, carry out roasting after drying, pulverizing, then pulverize, obtain the siller tin oxide composite powder containing stannic acid indium;
6) gained is shaping containing the siller tin oxide composite powder oil pressure of stannic acid indium, and then is placed in oxygen-containing atmosphere and sinters, and obtains the siller tin oxide briquet containing stannic acid indium;
7) gained carries out multiple pressure, resintering containing the siller tin oxide briquet of stannic acid indium, namely obtains the siller tin oxide electric contact material containing stannic acid indium.
Putty powder and NaOH powder are divided into two parts by the present invention, wherein a part of NaOH is obtained by reacting indium hydroxide and tin oxide composite powder with the indium nitrate suspension containing a part of putty powder, obtain stannic acid indium powder after this composite powder is carried out high-temperature calcination, ball milling, and gained stannic acid indium powder is joined suspension that another part putty powder and liquor argenti nitratis ophthalmicus formed and another part NaOH again secondary response to obtain silver oxide, tin oxide and stannic acid indium composite powder.Obtained stannic acid indium powder density and the density of reacting silver oxide and the tin oxide generated are close, and (density of wherein obtained stannic acid indium is 7.07g/cm
3, the density of tin oxide is 6.95g/cm
3, the density of silver oxide is 7.143g/cm
3), thus silver oxide, tin oxide and the stannic acid indium as additive can be made to be mixed to get evenly, stannic acid indium powder and tin oxide are more evenly distributed in silver oxide, improve the problem pockety of additive in prior art, make gained electrical contact material have uniform metallographic structure; Meanwhile, the present invention adopts NaOH as precipitation reagent, can reduce the harm to human body and environment; On the other hand, because stannic acid indium is a kind of semi-conducting material, its resistivity only has 1 × 10
-4Ω cm, and the resistivity of tin oxide is 93 Ω cm, therefore, adds appropriate stannic acid indium in siller tin oxide electric contact, effectively can reduce resistivity and the temperature rise of siller tin oxide electric contact; Again on the one hand, add stannic acid indium in siller tin oxide after, the siller tin oxide electric contact that gained contains stannic acid indium compound is subject to the effect of electric arc and Joule heat in the course of the work, part stannic acid indium is made to absorb a large amount of energy and be decomposed into tin oxide and indium oxide, thus can the arcing time be shortened, reduce the electrical wear of electrical contact.
The step 1 of said method) in, need containing in the siller tin oxide electric contact material of stannic acid indium of preparation, tin oxide content is 8 ~ 15wt%, and the content of stannic acid indium is 0.1 ~ 4wt%, and surplus is silver; The more excellent tin oxide content that is chosen as is 10 ~ 12wt%, and the content of stannic acid indium is 1 ~ 2wt%, and surplus is silver.In this step, preferably silver nitrate is mixed with the liquor argenti nitratis ophthalmicus of 30 ~ 40w/w%, be more preferably the liquor argenti nitratis ophthalmicus being mixed with 30 ~ 35w/w%, correspondingly, for NaOH B solution, be more preferably and be made into the solution that concentration is 15 ~ 25w/w%, the silver oxide that reaction can be made to generate like this has more uniform outer appearance, and a step makes the metallographic structure of gained electrical contact material more even; And for NaOH solution A and stannic acid solution of indium, their too not large being particular about of concentration, but preferably, be NaOH A is made into the solution that concentration is 10 ~ 30w/w%, indium nitrate is made into the solution that concentration is 30 ~ 40w/w%.In this step, described oxidate powder and stannic acid indium powder all preferably adopt particle mean size to be the powder of 1 ~ 10 μm.
The step 2 of said method) in, the speed that adds of described NaOH solution A is not particular about, but is preferably 0.1 ~ 1L/min; Described 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 calcination is same as the prior art, and in the application, preferably drying is until dry the composite powder of putty powder A and indium hydroxide under 100 ~ 150 DEG C of conditions, usually needs the time of 12 ~ 18h; Normally the composite powder of dried putty powder A and indium hydroxide is placed in oxygen-containing atmosphere and calcines 8 ~ 24h under 1450 ~ 1700 DEG C of conditions, ball milling after taking out, cross 100 ~ 200 eye mesh screens, obtain stannic acid indium powder.
The step 4 of said method) in, the speed that adds of described NaOH B solution is preferably 0.1 ~ 1L/min; Described stirring reaction carries out usually under normal temperature condition, and the time of stirring reaction is generally 0.3 ~ 1h.
The step 5 of said method) in, dry, pulverize and the operation of roasting same as the prior art, in the application, preferably drying is until dry silver oxide, tin oxide and stannic acid indium composite powder under 100 ~ 150 DEG C of conditions, usually needs the time of 12 ~ 18h; Cross 100 ~ 200 eye mesh screens after normally dried silver oxide, tin oxide and stannic acid indium composite powder being pulverized, extracting screen underflow enters next process; Described roasting is roasting 2 ~ 6h under 400 ~ 500 DEG C of temperature conditions normally, then pulverizes (at least crossing 100 mesh sieves), obtains the siller tin oxide composite powder containing stannic acid indium.
The step 6 of said method) in, when oil pressure is shaping, briquetting pressure is generally 8 ~ 12T/cm
2; Normally the pressed compact after shaping is placed in oxygen-containing atmosphere and sinters 4 ~ 8h under 880 ~ 920 DEG C of temperature conditions, to obtain the siller tin oxide briquet containing stannic acid indium.
The step 7 of said method) in, the pressure of described multiple pressure is 12 ~ 18T/cm
2, described resintering be by multiple pressure after siller tin oxide oxide briquet be placed in oxygen-containing atmosphere resintering 4 ~ 8h under 880 ~ 920 DEG C of conditions.
Compared with prior art, feature of the present invention is:
1, putty powder and NaOH powder are divided into two parts by the present invention, wherein a part of NaOH is obtained by reacting indium hydroxide and tin oxide composite powder with the indium nitrate suspension containing a part of putty powder, obtain stannic acid indium powder after this composite powder is carried out high-temperature calcination, ball milling, and gained stannic acid indium powder is joined suspension that another part putty powder and liquor argenti nitratis ophthalmicus formed and another part NaOH again secondary response to obtain silver oxide, tin oxide and stannic acid indium composite powder.Obtained stannic acid indium powder density and the density of reacting silver oxide and the tin oxide generated are close, and (density of wherein obtained stannic acid indium is 7.07g/cm
3, the density of tin oxide is 6.95g/cm
3, the density of silver oxide is 7.143g/cm
3), thus silver oxide, tin oxide and the stannic acid indium as additive can be made to be mixed to get evenly, stannic acid indium powder and tin oxide are more evenly distributed in silver oxide, improve the problem pockety of additive in prior art, make gained electrical contact material have uniform metallographic structure; Meanwhile, the present invention adopts NaOH as precipitation reagent, can reduce the harm to human body and environment; On the other hand, because stannic acid indium is a kind of semi-conducting material, its resistivity only has 1 × 10
-4Ω cm, and the resistivity of tin oxide is 93 Ω cm, therefore, adds appropriate stannic acid indium in siller tin oxide electric contact, effectively can reduce resistivity and the temperature rise of siller tin oxide electric contact; Again on the one hand, add stannic acid indium in siller tin oxide after, the siller tin oxide electric contact that gained contains stannic acid indium compound is subject to the effect of electric arc and Joule heat in the course of the work, part stannic acid indium is made to absorb a large amount of energy and be decomposed into tin oxide and indium oxide, thus can the arcing time be shortened, reduce the electrical wear of electrical contact.
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 of the contact material that the embodiment of the present invention 1 obtains;
Fig. 2 is the metallographic structure figure of the contact material that the embodiment of the present invention 2 obtains;
Fig. 3 is the metallographic structure figure of the contact material that the embodiment of the present invention 3 obtains.
Embodiment
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 according to preparation 10kg Ag-SnO
2(11.5)-In
4sn
3o
12(0.5) material mixture ratio calculates required putty powder, indium nitrate silver nitrate consumption, take putty powder (particle mean size is 2 ~ 3 μm) 1.172kg, indium nitrate 0.06kg and silver nitrate 13.852kg, again according to the consumption weighing sodium hydroxide A0.026kg of indium nitrate, and according to the consumption weighing sodium hydroxide B 3.585kg of silver nitrate, for subsequent use; Get silver nitrate is made into 30w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, get the indium nitrate solution that the water-soluble solution of indium nitrate is made into 30w/w%; Get NaOH A is made into 20w/w% solution by water-soluble solution, obtain NaOH solution A; Get NaOH B is made into 20w/w% solution by water-soluble solution, obtain NaOH B solution; The putty powder taken is divided into two parts, and portion is putty powder A, and its quality is 0.022kg; Another part is putty powder B, and its quality is 1.15kg;
2) putty powder A and indium nitrate solution are placed in reactor, stir (fully stirring 120min), obtains the suspension of putty powder A and indium nitrate; In this suspension, add NaOH solution A (drop rate is 0.1L/min), stirring reaction 0.3h, filter, obtain putty powder A and indium hydroxide (In (OH)
3) composite powder;
3) at 120 DEG C of temperature, dry 15h after the composite powder washed with de-ionized water of the putty powder A of gained and indium hydroxide is clean, then the composite powder of oven dry is placed in air with 1550 DEG C of temperature calcination 12h, obtains stannic acid indium (In
4sn
3o
12) compound, and the stannic acid indium compound after calcining is loaded high energy ball mill with ratio of grinding media to material 4:1 ball milling 1h, cross 200 eye mesh screens after taking out, obtain stannic acid indium powder;
4) putty powder B and liquor argenti nitratis ophthalmicus are placed in another reactor, stir (fully stirring 120min), obtains the suspension of silver nitrate and putty powder B; Add step 3 wherein) the stannic acid indium powder of gained, then add NaOH B solution (drop rate is 0.1L/min), stirring reaction 1h, filter, obtain silver oxide, tin oxide and stannic acid indium composite powder;
5) silver oxide of gained, tin oxide and stannic acid indium composite powder deionized water are washed till neutrality at centrigugal swing dryer supernatant, 15h is dried in an oven subsequently with 120 DEG C of temperature, then the composite powder of oven dry is placed in bipyramid blender broken (rotating speed 25r/min, time 1h); Gained powder is placed in air with 450 DEG C of temperature calcination 4h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again, crosses 200 mesh sieves, obtain the siller tin oxide composite powder containing stannic acid indium after taking-up;
6) containing the siller tin oxide composite powder of stannic acid indium, shaping on hydraulic press (briquetting pressure is 10T/cm to gained
2), and the pressed compact after shaping is placed in air with 880 DEG C of temperature sintering 4h, obtain the siller tin oxide briquet containing stannic acid indium;
7) gained carries out multiple pressure containing the siller tin oxide briquet of stannic acid indium (multiple pressure pressure is 15T/cm
2), and the siller tin oxide briquet containing stannic acid indium after multiple pressure is placed in air with 880 DEG C of temperature resintering 4h, obtain the siller tin oxide (Ag-SnO containing stannic acid indium
2(11.5)-In
4sn
3o
12(0.5)) electrical contact.
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, is distributed in silver matrix to tiny tin oxide and stannic acid indium uniform particles.
Comparative example 1
According to preparation Ag-SnO
2(11.5)-In
4sn
3o
12(0.5) material mixture ratio calculates and takes required putty powder (particle mean size is 2 ~ 3 μm), stannic acid indium, silver powder (particle mean size is 2 ~ 3 μm), prepares contact product by the powder mixing method of existing routine.
Embodiment 2
1) first according to preparation 10kg Ag-SnO
2(8)-In
4sn
3o
12(4) material mixture ratio calculates required putty powder, indium nitrate and silver nitrate consumption, take putty powder (particle mean size is 2 ~ 3 μm) 0.98kg, indium nitrate 0.477kg and silver nitrate 13.852kg, again according to the consumption weighing sodium hydroxide A0.209kg of indium nitrate, and according to the consumption weighing sodium hydroxide B 3.585kg of silver nitrate, for subsequent use; Get silver nitrate is made into 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, get the indium nitrate solution that the water-soluble solution of indium nitrate is made into 20w/w%; Get NaOH A is made into 10w/w% solution by water-soluble solution, obtain NaOH solution A; Get NaOH B is made into 30w/w% solution by water-soluble solution, obtain NaOH B solution; The putty powder taken is divided into two parts, and portion is putty powder A, and its quality is 0.18kg; Another part is putty powder B, and its quality is 0.8kg;
2) putty powder A and indium nitrate solution are placed in reactor, stir (fully stirring 80min), obtains the suspension of putty powder A and indium nitrate; In this suspension, add NaOH solution A (drop rate is 0.5L/min), stirring reaction 0.5h, filter, obtain the composite powder of putty powder A and indium hydroxide;
3) at 100 DEG C of temperature, 18h is dried after the composite powder washed with de-ionized water of the putty powder A of gained and indium hydroxide is clean, then the composite powder of oven dry is placed in air with 1650 DEG C of temperature calcination 24h, obtain stannic acid indium compound, and the stannic acid indium compound after calcining is loaded high energy ball mill with ratio of grinding media to material 6:1 ball milling 2h, cross 200 eye mesh screens after taking out, obtain stannic acid indium powder;
4) putty powder B and liquor argenti nitratis ophthalmicus are placed in another reactor, stir (fully stirring 120min), obtains the suspension of silver nitrate and putty powder B; Add step 3 wherein) the stannic acid indium powder of gained, then add NaOH B solution (drop rate is 0.8L/min), stirring reaction 0.5h, filter, obtain silver oxide, tin oxide and stannic acid indium composite powder;
5) silver oxide of gained, tin oxide and stannic acid indium composite powder deionized water are washed till neutrality at centrigugal swing dryer supernatant, 12h is dried in an oven subsequently with 150 DEG C of temperature, then the composite powder of oven dry is placed in bipyramid blender broken (rotating speed 25r/min, time 1h); Gained powder is placed in air with 500 DEG C of temperature calcination 6h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again, crosses 200 mesh sieves, obtain the siller tin oxide composite powder containing stannic acid indium after taking-up;
6) containing the siller tin oxide composite powder of stannic acid indium, shaping on hydraulic press (briquetting pressure is 12T/cm to gained
2), and the pressed compact after shaping is placed in air with 920 DEG C of temperature sintering 6h, obtain the siller tin oxide briquet containing stannic acid indium;
7) gained carries out multiple pressure containing the siller tin oxide briquet of stannic acid indium (multiple pressure pressure is 12T/cm
2), and the siller tin oxide briquet containing stannic acid indium after multiple pressure is placed in air with 900 DEG C of temperature resintering 8h, obtain the siller tin oxide (Ag-SnO containing stannic acid indium
2(8)-In
4sn
3o
12(4)) electrical contact.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 2, the metallographic structure of contact product prepared of technical scheme is even as seen from the figure, is distributed in silver matrix to tiny tin oxide and stannic acid indium uniform particles.
Embodiment 3
1) first according to preparation 10kg Ag-SnO
2(15)-In
4sn
3o
12(2) material mixture ratio calculates required putty powder, indium nitrate and silver nitrate consumption, take putty powder (particle mean size is 2 ~ 3 μm) 1.59kg, indium nitrate 0.238kg and silver nitrate 13.065kg, again according to the consumption weighing sodium hydroxide A0.105kg of indium nitrate, and according to the consumption weighing sodium hydroxide B 3.382kg of silver nitrate, for subsequent use; Get silver nitrate is made into 30w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, get the indium nitrate solution that the water-soluble solution of indium nitrate is made into 25w/w%; Get NaOH A is made into 20w/w% solution by water-soluble solution, obtain NaOH solution A; Get NaOH B is made into 25w/w% solution by water-soluble solution, obtain NaOH B solution; The putty powder taken is divided into two parts, and portion is putty powder A, and its quality is 0.09kg; Another part is putty powder B, and its quality is 1.5kg;
2) putty powder A and indium nitrate solution are placed in reactor, stir (fully stirring 100min), obtains the suspension of putty powder A and indium nitrate; In this suspension, add NaOH solution A (drop rate is 0.3L/min), stirring reaction 0.6h, filter, obtain putty powder A and indium hydroxide (In (OH)
3) composite powder;
3) at 120 DEG C of temperature, 15h is dried after the composite powder washed with de-ionized water of the putty powder A of gained and indium hydroxide is clean, then the composite powder of oven dry is placed in air with 1550 DEG C of temperature calcination 20h, obtain stannic acid indium compound, and the stannic acid indium compound after calcining is loaded high energy ball mill with ratio of grinding media to material 5:1 ball milling 1h, cross 200 eye mesh screens after taking out, obtain stannic acid indium powder;
4) putty powder B and liquor argenti nitratis ophthalmicus are placed in another reactor, stir (fully stirring 100min), obtains the suspension of silver nitrate and putty powder B; Add step 3 wherein) the stannic acid indium powder of gained, then add NaOH B solution (drop rate is 0.5L/min), stirring reaction 0.5h, filter, obtain silver oxide, tin oxide and stannic acid indium composite powder;
5) silver oxide of gained, tin oxide and stannic acid indium composite powder deionized water are washed till neutrality at centrigugal swing dryer supernatant, 18h is dried in an oven subsequently with 120 DEG C of temperature, then the composite powder of oven dry is placed in bipyramid blender broken (rotating speed 25r/min, time 1h); Gained powder is placed in air with 450 DEG C of temperature calcination 6h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again, crosses 200 mesh sieves, obtain the siller tin oxide composite powder containing stannic acid indium after taking-up;
6) containing the siller tin oxide composite powder of stannic acid indium, shaping on hydraulic press (briquetting pressure is 12T/cm to gained
2), and the pressed compact after shaping is placed in air with 920 DEG C of temperature sintering 6h, obtain the siller tin oxide briquet containing stannic acid indium;
7) gained carries out multiple pressure containing the siller tin oxide briquet of stannic acid indium (multiple pressure pressure is 18T/cm
2), and the siller tin oxide briquet containing stannic acid indium after multiple pressure is placed in air with 920 DEG C of temperature resintering 8h, obtain the siller tin oxide (Ag-SnO containing stannic acid indium
2(15)-In
4sn
3o
12(2)) electrical contact.
Carry out metallographic structure analysis to gained contact material, as shown in Figure 3, the metallographic structure of contact product prepared of technical scheme is even as seen from the figure, is distributed in silver matrix to tiny tin oxide and stannic acid indium uniform particles.
Embodiment 1 and the obtained contact material of comparative example 1 are carried out Performance Detection, and compare with the contact product that existing routine mixes the siller tin oxide of the interpolation indium oxide that powder-monolithic pressing obtains, result as described in Table 1:
Table 1 embodiment 1 and comparative example 1 and existing routine mix articles of sheet material performance prepared by powder-monolithic pressing
As shown in Table 1, the performance of sliver oxidized tin contactor materials containing stannic acid indium that prepared by technical scheme is better than comparative example 1 and existing routine and mixes the sliver oxidized tin contactor materials performance containing indium oxide prepared by powder-monolithic pressing.
Claims (6)
1., containing a preparation method for the siller tin oxide electric contact material of stannic acid indium, it is characterized in that comprising the following steps:
1) calculate according to the material mixture ratio of the siller tin oxide electric contact containing stannic acid indium of required preparation needed for the consumption of putty powder, indium nitrate and silver nitrate, generate the consumption of the NaOH needed for indium hydroxide according to the Dosage calculation indium nitrate of indium nitrate and NaOH reaction, represent with NaOH A; Generate the consumption of the NaOH needed for silver oxide according to the Dosage calculation silver nitrate of silver nitrate and NaOH reaction, represent with NaOH B; Take above-mentioned substance, for subsequent use; Get silver nitrate is made into 20 ~ 40w/w% liquor argenti nitratis ophthalmicus by water-soluble solution, get the water-soluble solution of indium nitrate and be made into indium nitrate solution; Get the water-soluble solution wiring solution-forming of NaOH A, obtain NaOH solution A; Get NaOH B is made into 10 ~ 30w/w% solution by water-soluble solution, obtain NaOH B solution; The putty powder taken is divided into two parts, and portion is putty powder A, and its amount is for can react with indium nitrate and NaOH the amount that the indium hydroxide generated reacts completely to generate stannic acid indium, and another part is putty powder B;
2) putty powder A and indium nitrate solution are placed in reactor, stir, obtain the suspension of putty powder A and indium nitrate; In this suspension, add NaOH solution A, stirring reaction, filter, obtain the composite powder of putty powder A and indium hydroxide;
3) the putty powder A of gained and the composite powder of indium hydroxide are washed to neutrality, drying is placed on containing calcination in oxygen atmosphere, then ball milling, obtains stannic acid indium powder;
4) putty powder B and liquor argenti nitratis ophthalmicus are placed in another reactor, stir, obtain the suspension of silver nitrate and putty powder B; Add step 3 wherein) the stannic acid indium powder of gained, then add NaOH B solution, stirring reaction, filter, obtain silver oxide, tin oxide and stannic acid indium composite powder;
5) silver oxide of gained, tin oxide and stannic acid indium composite powder are washed to neutrality, carry out roasting after drying, pulverizing, then pulverize, obtain the siller tin oxide composite powder containing stannic acid indium;
6) gained is shaping containing the siller tin oxide composite powder oil pressure of stannic acid indium, and then is placed in oxygen-containing atmosphere and sinters, and obtains the siller tin oxide briquet containing stannic acid indium;
7) gained carries out multiple pressure, resintering containing the siller tin oxide briquet of stannic acid indium, namely obtains the siller tin oxide electric contact material containing stannic acid indium.
2. preparation method according to claim 1, is characterized in that: step 1) in, need containing in the siller tin oxide electric contact material of stannic acid indium of preparation, tin oxide content is 8 ~ 15wt%, and the content of stannic acid indium is 0.1 ~ 4wt%, and surplus is silver.
3. preparation method according to claim 1, is characterized in that: step 1) in, step 1) in, the concentration of liquor argenti nitratis ophthalmicus is 30 ~ 40w/w%.
4. preparation method according to claim 1, is characterized in that: step 1) in, get indium nitrate water and be made into the solution that concentration is 30 ~ 40w/w%.
5. preparation method according to claim 1, is characterized in that: step 1) in, get NaOH A water and be made into the solution that concentration is 10 ~ 30w/w%.
6. preparation method according to claim 1, is characterized in that: step 1) in, the concentration of NaOH B solution is 15 ~ 25w/w%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001220137A (en) * | 2000-02-10 | 2001-08-14 | Dowa Mining Co Ltd | Tin-doped indium oxide powder and its manufacturing method |
| US20050074394A1 (en) * | 2003-10-07 | 2005-04-07 | Ferro Corporation | Nanosized silver oxide power |
| WO2007020006A1 (en) * | 2005-08-12 | 2007-02-22 | Umicore Ag & Co. Kg | Use of indium-tin mixed oxide for silver-based materials |
| CN101415644A (en) * | 2006-03-31 | 2009-04-22 | 尤米科尔股份有限公司 | Process for manufacture of silver-based particles and electrical contact materials |
| CN102142325A (en) * | 2010-12-30 | 2011-08-03 | 温州宏丰电工合金股份有限公司 | Preparation method of particle direction-arrangement enhanced silver-based oxide electrical contact material |
-
2014
- 2014-12-30 CN CN201410844381.1A patent/CN104505191B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001220137A (en) * | 2000-02-10 | 2001-08-14 | Dowa Mining Co Ltd | Tin-doped indium oxide powder and its manufacturing method |
| US20050074394A1 (en) * | 2003-10-07 | 2005-04-07 | Ferro Corporation | Nanosized silver oxide power |
| WO2007020006A1 (en) * | 2005-08-12 | 2007-02-22 | Umicore Ag & Co. Kg | Use of indium-tin mixed oxide for silver-based materials |
| CN101415644A (en) * | 2006-03-31 | 2009-04-22 | 尤米科尔股份有限公司 | Process for manufacture of silver-based particles and electrical contact materials |
| CN102142325A (en) * | 2010-12-30 | 2011-08-03 | 温州宏丰电工合金股份有限公司 | Preparation method of particle direction-arrangement enhanced silver-based oxide electrical contact material |
Non-Patent Citations (2)
| Title |
|---|
| Y.S. JUNG ET AL.: "Effects of thermal treatment on the electrical and optical properties of silver-based indium tin oxide metal indium tin oxide structures", 《THIN SOLID FILMS》 * |
| 李波，刘心宇等: "微量添加In对Ag-Sn合金粉末氧化机理的影响", 《稀有金属材料与工程》 * |
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