CN104505191B - A kind of preparation method of the siller tin oxide electric contact material containing stannic acid indium - Google Patents
A kind of preparation method of the siller tin oxide electric contact material containing stannic acid indium Download PDFInfo
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- CN104505191B CN104505191B CN201410844381.1A CN201410844381A CN104505191B CN 104505191 B CN104505191 B CN 104505191B CN 201410844381 A CN201410844381 A CN 201410844381A CN 104505191 B CN104505191 B CN 104505191B
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Abstract
The invention discloses the preparation method of a kind of siller tin oxide electric contact material containing stannic acid indium, particularly as follows: the consumption of putty powder, indium nitrate and the silver nitrate needed for calculating according to the material mixture ratio of the siller tin oxide electric contact containing stannic acid indium of required preparation, consumption according to indium nitrate calculates the consumption of sodium hydroxide, represents with sodium hydroxide A；Consumption according to silver nitrate calculates the consumption of sodium hydroxide, represents with sodium hydroxide B；Weigh standby；The material wiring solution-forming respectively that will weigh, is divided into two parts putty powder, putty powder A and putty powder B；Sodium hydroxide A is reacted with the indium nitrate suspension containing putty powder A and obtains indium hydroxide and stannum oxide composite powder, composite powder calcining, obtain stannic acid indium powder after ball milling, add it to putty powder B and suspension that silver nitrate solution is formed reacts with sodium hydroxide B and obtains silver oxide, stannum oxide and stannic acid indium composite powder；This composite powder is washed, be dried, after roasting through molding, sintering, multiple pressure, resintering, to obtain final product.
Description
Technical field
The present invention relates to the preparation method of a kind of siller tin oxide electric contact material containing stannic acid indium, belong to metal
Based composites field.
Background technology
In recent years, siller tin oxide contact extensively should as the optimal replacer of poisonous silver cadmium oxide contact
It is used in various low-voltage electrical apparatus.Sliver oxidized tin contactor materials has excellent wearability, resistance fusion welding and resistance to
Arc erosion, but there is the shortcomings such as contact resistance is big, temperature rise is high in it, has had a strong impact on the electrical resistance of electrical equipment
Energy.
Discovery is studied, one or more oxidations being added with in bismuth oxide, copper oxide and Indium sesquioxide. through forefathers
The siller tin oxide electric contact material of thing not only has good wearability, resistance fusion welding and resistance to arc erosion,
Improve the electric property of electrical equipment well.Have not yet to see the siller tin oxide electric contact of doping stannic acid indium
The relevant report of material.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of technique is simple, stannic acid indium is in matrix material point
Cloth contains the preparation method of the siller tin oxide electric contact material of stannic acid indium uniformly, obtained by this method stanniferous
The siller tin oxide electric contact metallographic structure of acid indium is uniform, have 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, including following step
Rapid:
1) needed for calculating according to the material mixture ratio of the siller tin oxide electric contact containing stannic acid indium of required preparation
The consumption of putty powder, indium nitrate and silver nitrate, calculates indium nitrate and hydroxide according to the consumption of indium nitrate
Sodium reaction generates the consumption of the sodium hydroxide needed for indium hydroxide, represents with sodium hydroxide A；According to nitric acid
The consumption of silver calculates the consumption of the sodium hydroxide needed for silver nitrate and sodium hydroxide reaction generation silver oxide, with
Sodium hydroxide B represents；Weigh above-mentioned substance, standby；Take silver nitrate water dissolution and be made into 20～40w/w%
Silver nitrate solution, take indium nitrate water dissolution and be made into indium nitrate solution；Take sodium hydroxide A water dissolution
Wiring solution-forming, obtains sodium hydroxide solution A；Take sodium hydroxide B water dissolution and be made into 10～30w/w%
Solution, obtains sodium hydroxide B solution；Being divided into two parts by the putty powder weighed, portion is putty powder
A, reacts completely in an amount of from reacting, with indium nitrate and sodium hydroxide, the indium hydroxide generated to generate stannic acid
The amount of indium, another part is putty powder B；
2) putty powder A and indium nitrate solution are placed in reactor, stir, obtain putty powder
A and the suspension of indium nitrate；In this suspension, add sodium hydroxide 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, are placed in after drying
Oxygen-containing atmosphere is calcined, then ball milling, obtains stannic acid indium powder；
4) putty powder B and silver nitrate solution are placed in another reactor, stir, obtain nitric acid
Silver and the suspension of putty powder B；It is added thereto to step 3) the stannic acid indium powder of gained, add hydrogen-oxygen
Change sodium B solution, stirring reaction, filter, obtain silver oxide, stannum oxide and stannic acid indium composite powder；
5) silver oxide of gained, stannum oxide and stannic acid indium composite powder are washed to neutrality, are dried, pulverize
After carry out roasting, then pulverize, obtain the siller tin oxide composite powder containing stannic acid indium；
6) gained siller tin oxide composite powder oil pressure molding containing stannic acid indium, is placed in oxygen-containing atmosphere burning the most again
Knot, obtains the siller tin oxide briquet containing stannic acid indium；
7) gained siller tin oxide briquet containing stannic acid indium carries out multiple pressure, resintering, i.e. obtains the silver containing stannic acid indium
Tin oxide electric contact material.
Putty powder and sodium hydroxide powder are divided into two parts by the present invention, a portion sodium hydroxide with contain
The indium nitrate suspension reaction of a part of putty powder obtains indium hydroxide and stannum oxide composite powder, and this is multiple
Close after powder carries out high-temperature calcination, ball milling and obtain stannic acid indium powder, and gained stannic acid indium powder is joined another portion
The suspension dividing putty powder and silver nitrate solution to be formed is reacted to give again with another part sodium hydroxide
Silver oxide, stannum oxide and stannic acid indium composite powder.The silver oxide that the stannic acid indium powder density prepared generates with reaction
Being close with the density of stannum oxide, (density of the stannic acid indium wherein prepared is 7.07g/cm3, stannum oxide close
Degree is 6.95g/cm3, the density of silver oxide is 7.143g/cm3), thus silver oxide, stannum oxide can be made
Mix evenly with the stannic acid indium as additive so that stannic acid indium powder and stannum oxide divide with being more uniformly distributed
Cloth, in silver oxide, improves the problem pockety of additive in prior art so that gained electricity touches
Head material has uniform metallographic structure；Meanwhile, the present invention use sodium hydroxide as precipitant, permissible
Reduce human body and the harm of environment；On the other hand, owing to stannic acid indium is a kind of semi-conducting material, its electricity
Resistance rate only has 1 × 10-4Ω cm, and the resistivity of stannum oxide is 93 Ω cm, therefore, at siller tin oxide
Electrical contact adds appropriate stannic acid indium, resistivity and the temperature of siller tin oxide electric contact can be effectively reduced
Rise；Another further aspect, after adding stannic acid indium in siller tin oxide, gained contains the silver-colored oxygen of stannic acid indium compound
Change stannum electrical contact to be acted on by electric arc and Joule heat in the course of the work so that part stannic acid indium absorbs big
The energy of amount and be decomposed into stannum oxide and Indium sesquioxide., thus the arcing time can be shortened, reduce electrical contact
Electrical wear.
The step 1 of said method) in, need in the siller tin oxide electric contact material containing stannic acid indium of preparation,
Stannum oxide content is 8～15wt%, and the content of stannic acid indium is 0.1～4wt%, and surplus is silver；More excellent choosing
Being selected as stannum oxide content is 10～12wt%, and the content of stannic acid indium is 1～2wt%, and surplus is silver.This step
In, preferably silver nitrate is configured to the silver nitrate solution of 30～40w/w%, be more preferably configured to 30～
The silver nitrate solution of 35w/w%, for sodium hydroxide B solution, is more preferably joined
The solution becoming concentration to be 15～25w/w%, outside the silver oxide that so reaction can be made to generate has and is more uniformly distributed
See, and a step makes the metallographic structure of gained electrical contact material be more uniformly distributed；And for sodium hydroxide solution A
For stannic acid solution of indium, their concentration does not has the biggest being particular about, but preferably, is by hydroxide
Sodium A is made into the solution that concentration is 10～30w/w%, and 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 employ the powder that particle mean size is 1～10 μm
End.
The step 2 of said method) in, the addition speed of described sodium hydroxide solution A is not particular about, but excellent
Elect 0.1～1L/min as；Described stirring reaction is generally carried out under normal temperature condition, the time of stirring reaction
It is usually 0.3～1h.
The step 3 of said method) in, it is dried and the operation of calcination is same as the prior art, in the application,
Preferably it is dried under the conditions of 100～150 DEG C until the composite powder of putty powder A and indium hydroxide is dried
, it usually needs the time of 12～18h；It is typically dried putty powder A and indium hydroxide
Composite powder be placed in oxygen-containing atmosphere under the conditions of 1450～1700 DEG C calcine 8～24h, ball after taking-up
Mill, crosses 100～200 eye mesh screens, obtains stannic acid indium powder.
The step 4 of said method) in, the addition speed of described sodium hydroxide B solution be preferably 0.1～
1L/min；Described stirring reaction generally carry out under normal temperature condition, stirring react time be usually 0.3～
1h。
The step 5 of said method) in, the operation of dry, pulverizing and roasting is same as the prior art, this Shen
In please, preferably it be dried under the conditions of 100～150 DEG C until by silver oxide, stannum oxide and stannic acid indium composite powder
End is dried, it usually needs the time of 12～18h；It is typically dried silver oxide, stannum oxide
Crossing 100～200 eye mesh screens with stannic acid indium composite powder after pulverizing, extracting screen underflow enters next process；Institute
The roasting stated is typically roasting 2～6h under 400～500 DEG C of temperature conditionss, then pulverizes and (at least crosses 100
Mesh sieve), obtain the siller tin oxide composite powder containing stannic acid indium.
The step 6 of said method) in, when oil pressure molding, briquetting pressure is usually 8～12T/cm2；Logical
Be often by molding after pressed compact be placed in oxygen-containing atmosphere under 880～920 DEG C of temperature conditionss sintering 4～8h,
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/cm2, described resintering is
Siller tin oxide oxide briquet after multiple pressure is placed in oxygen-containing atmosphere resintering under the conditions of 880～920 DEG C
4～8h.
Compared with prior art, present invention is characterized in that
1, putty powder and sodium hydroxide powder are divided into two parts by the present invention, a portion sodium hydroxide with
Indium nitrate suspension reaction containing a part of putty powder obtains indium hydroxide and stannum oxide composite powder, should
Composite powder obtains stannic acid indium powder after carrying out high-temperature calcination, ball milling, and gained stannic acid indium powder is joined another
The suspension that partial oxidation glass putty and silver nitrate solution are formed and another part sodium hydroxide secondary response again are to obtain
To silver oxide, stannum oxide and stannic acid indium composite powder.The oxidation that the stannic acid indium powder density prepared generates with reaction
The density of silver and stannum oxide is close, and (density of the stannic acid indium wherein prepared is 7.07g/cm3, stannum oxide
Density is 6.95g/cm3, the density of silver oxide is 7.143g/cm3), thus silver oxide, oxidation can be made
Stannum and the stannic acid indium as additive mix evenly so that stannic acid indium powder and stannum oxide are more uniformly distributed ground
It is distributed in silver oxide, improves the problem pockety of additive in prior art so that gained electricity
Contact material has uniform metallographic structure；Meanwhile, the present invention use sodium hydroxide as precipitant, can
To reduce human body and the harm of environment；On the other hand, owing to stannic acid indium is a kind of semi-conducting material, its
Resistivity only has 1 × 10-4Ω cm, and the resistivity of stannum oxide is 93 Ω cm, therefore, aoxidizes at silver
Stannum electrical contact adds appropriate stannic acid indium, can be effectively reduced siller tin oxide electric contact resistivity and
Temperature rise；Another further aspect, after adding stannic acid indium in siller tin oxide, gained contains the silver of stannic acid indium compound
Tin oxide electric contact is acted on by electric arc and Joule heat in the course of the work so that part stannic acid indium absorbs
Substantial amounts of energy and be decomposed into stannum oxide and Indium sesquioxide., thus the arcing time can be shortened, reduce electricity and touch
The electrical wear of head.
2, the method for the invention technique is simple, little to human body and environmental pollution, is suitable for industrialized production.
Accompanying drawing explanation
Fig. 1 is the metallographic structure figure of the contact material that the embodiment of the present invention 1 prepares；
Fig. 2 is the metallographic structure figure of the contact material that the embodiment of the present invention 2 prepares；
Fig. 3 is the metallographic structure figure of the contact material that the embodiment of the present invention 3 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, to be more fully understood that the present invention's
Content, but the present invention is not limited to following example.
Embodiment 1
1) it is first according to prepare 10kg Ag-SnO2(11.5)-In4Sn3O12(0.5) material mixture ratio calculates requisite oxygen
Change glass putty, indium nitrate silver nitrate consumption, weigh putty powder (particle mean size is 2～3 μm) 1.172kg,
Indium nitrate 0.06kg and silver nitrate 13.852kg, further according to consumption weighing sodium hydroxide A of indium nitrate
0.026kg, and according to the consumption weighing sodium hydroxide B 3.585kg of silver nitrate, standby；Take silver nitrate to use
Water dissolution is made into the silver nitrate solution of 30w/w%, and taking indium nitrate water dissolution, to be made into the indium nitrate of 30w/w% molten
Liquid；Take sodium hydroxide A water dissolution and be made into the solution of 20w/w%, obtain sodium hydroxide solution A；Take hydrogen-oxygen
Change sodium B water dissolution and be made into the solution of 20w/w%, obtain sodium hydroxide B solution；The putty powder that will weigh
Being divided into two parts, portion is putty powder A, and its quality is 0.022kg；Another part is putty powder B, its
Quality is 1.15kg；
2) putty powder A and indium nitrate solution are placed in reactor, stir and (be sufficiently stirred for
120min), the suspension of putty powder A and indium nitrate is obtained；Sodium hydroxide A is added in this suspension
Solution (drop rate is 0.1L/min), stirring reaction 0.3h, filters, obtains putty powder A and hydrogen-oxygen
Change indium (In (OH)3) composite powder；
3) after the putty powder A of gained and the composite powder deionized water of indium hydroxide being cleaned up
Dry 15h at a temperature of 120 DEG C, then the composite powder of drying is placed in air with 1550 DEG C of temperature calcination
12h, obtains stannic acid indium (In4Sn3O12) compound, and the stannic acid indium compound after calcining is loaded high energy ball
Grinding machine, with ratio of grinding media to material 4:1 ball milling 1h, is crossed 200 eye mesh screens, is obtained stannic acid indium powder after taking-up；
4) putty powder B and silver nitrate solution are placed in another reactor, stir and (be sufficiently stirred for
120min), silver nitrate and the suspension of putty powder B are obtained；It is added thereto to step 3) stannum of gained
Acid indium powder, adds sodium hydroxide B solution (drop rate is 0.1L/min), stirring reaction 1h, filters,
Obtain silver oxide, stannum oxide and stannic acid indium composite powder；
5) by the silver oxide of gained, stannum oxide and stannic acid indium composite powder deionized water at centrifugal swing dryer
Supernatant is washed till neutrality, dries 15h with 120 DEG C of temperature the most in an oven, is then put by the composite powder of drying
In bipyramid blender broken (rotating speed 25r/min, time 1h)；Gained powder is placed in air with 450
DEG C temperature calcination 4h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again after taking-up,
Cross 200 mesh sieves, obtain the siller tin oxide composite powder containing stannic acid indium；
6) (briquetting pressure is in gained siller tin oxide composite powder molding on hydraulic press containing stannic acid indium
10T/cm2), and the pressed compact after molding is placed in air with 880 DEG C of temperature sintering 4h, obtain containing stannic acid
The siller tin oxide briquet of indium；
7) gained carries out multiple pressure containing the siller tin oxide briquet of stannic acid indium (multiple pressure pressure is 15T/cm2), and will be multiple
The siller tin oxide briquet containing stannic acid indium after pressure is placed in air with 880 DEG C of temperature resintering 4h, obtains stanniferous
Siller tin oxide (the Ag-SnO of acid indium2(11.5)-In4Sn3O12(0.5)) electrical contact.
Gained contact material is carried out metallographic structure analysis, as it is shown in figure 1, present techniques as seen from the figure
The metallographic structure of contact product prepared by scheme is uniform, and tiny stannum oxide and stannic acid indium granule divide equably
Cloth is in silver matrix.
Comparative example 1
According to preparation Ag-SnO2(11.5)-In4Sn3O12(0.5) material mixture ratio calculates and weighs required oxidation
Glass putty (particle mean size is 2～3 μm), stannic acid indium, argentum powder (particle mean size is 2～3 μm), by existing often
The powder mixing method of rule prepares contact product.
Embodiment 2
1) it is first according to prepare 10kg Ag-SnO2(8)-In4Sn3O12(4) material mixture ratio calculates required stannum oxide
Powder, indium nitrate and silver nitrate consumption, weigh putty powder (particle mean size is 2～3 μm) 0.98kg, nitre
Acid indium 0.477kg and silver nitrate 13.852kg, further according to consumption weighing sodium hydroxide A of indium nitrate
0.209kg, and according to the consumption weighing sodium hydroxide B 3.585kg of silver nitrate, standby；Take silver nitrate to use
Water dissolution is made into the silver nitrate solution of 40w/w%, and taking indium nitrate water dissolution, to be made into the indium nitrate of 20w/w% molten
Liquid；Take sodium hydroxide A water dissolution and be made into the solution of 10w/w%, obtain sodium hydroxide solution A；Take hydrogen-oxygen
Change sodium B water dissolution and be made into the solution of 30w/w%, obtain sodium hydroxide B solution；The putty powder that will weigh
Being divided into two parts, portion is putty powder A, and its quality is 0.18kg；Another part is putty powder B, its matter
Amount is 0.8kg；
2) putty powder A and indium nitrate solution are placed in reactor, stir and (be sufficiently stirred for
80min), the suspension of putty powder A and indium nitrate is obtained；Sodium hydroxide A is added in this suspension
Solution (drop rate is 0.5L/min), stirring reaction 0.5h, filters, obtains putty powder A and hydrogen-oxygen
Change the composite powder of indium；
3) after the putty powder A of gained and the composite powder deionized water of indium hydroxide being cleaned up
Dry 18h at a temperature of 100 DEG C, then the composite powder of drying is placed in air with 1650 DEG C of temperature calcination
24h, obtains stannic acid indium compound, and the stannic acid indium compound after calcining is loaded high energy ball mill with ball material
Ratio 6:1 ball milling 2h, crosses 200 eye mesh screens, obtains stannic acid indium powder after taking-up；
4) putty powder B and silver nitrate solution are placed in another reactor, stir and (be sufficiently stirred for
120min), silver nitrate and the suspension of putty powder B are obtained；It is added thereto to step 3) stannum of gained
Acid indium powder, adds sodium hydroxide B solution (drop rate is 0.8L/min), stirring reaction 0.5h, mistake
Filter, obtains silver oxide, stannum oxide and stannic acid indium composite powder；
5) by the silver oxide of gained, stannum oxide and stannic acid indium composite powder deionized water at centrifugal swing dryer
Supernatant is washed till neutrality, dries 12h with 150 DEG C of temperature the most in an oven, is then put by the composite powder of drying
In bipyramid blender broken (rotating speed 25r/min, time 1h)；Gained powder is placed in air with 500
DEG C temperature calcination 6h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again after taking-up,
Cross 200 mesh sieves, obtain the siller tin oxide composite powder containing stannic acid indium；
6) (briquetting pressure is in gained siller tin oxide composite powder molding on hydraulic press containing stannic acid indium
12T/cm2), and the pressed compact after molding is placed in air with 920 DEG C of temperature sintering 6h, obtain containing stannic acid
The siller tin oxide briquet of indium；
7) gained carries out multiple pressure containing the siller tin oxide briquet of stannic acid indium (multiple pressure pressure is 12T/cm2), and will be multiple
The siller tin oxide briquet containing stannic acid indium after pressure is placed in air with 900 DEG C of temperature resintering 8h, obtains stanniferous
Siller tin oxide (the Ag-SnO of acid indium2(8)-In4Sn3O12(4)) electrical contact.
Gained contact material is carried out metallographic structure analysis, as in figure 2 it is shown, present techniques as seen from the figure
The metallographic structure of contact product prepared by scheme is uniform, and tiny stannum oxide and stannic acid indium granule divide equably
Cloth is in silver matrix.
Embodiment 3
1) it is first according to prepare 10kg Ag-SnO2(15)-In4Sn3O12(2) material mixture ratio calculates required stannum oxide
Powder, indium nitrate and silver nitrate consumption, weigh putty powder (particle mean size is 2～3 μm) 1.59kg, nitre
Acid indium 0.238kg and silver nitrate 13.065kg, further according to consumption weighing sodium hydroxide A of indium nitrate
0.105kg, and according to the consumption weighing sodium hydroxide B 3.382kg of silver nitrate, standby；Take silver nitrate to use
Water dissolution is made into the silver nitrate solution of 30w/w%, and taking indium nitrate water dissolution, to be made into the indium nitrate of 25w/w% molten
Liquid；Take sodium hydroxide A water dissolution and be made into the solution of 20w/w%, obtain sodium hydroxide solution A；Take hydrogen-oxygen
Change sodium B water dissolution and be made into the solution of 25w/w%, obtain sodium hydroxide B solution；The putty powder that will weigh
Being divided into two parts, portion is putty powder A, and its quality is 0.09kg；Another part is putty powder B, its matter
Amount is 1.5kg；
2) putty powder A and indium nitrate solution are placed in reactor, stir and (be sufficiently stirred for
100min), the suspension of putty powder A and indium nitrate is obtained；Sodium hydroxide A is added in this suspension
Solution (drop rate is 0.3L/min), stirring reaction 0.6h, filters, obtains putty powder A and hydrogen-oxygen
Change indium (In (OH)3) composite powder；
3) after the putty powder A of gained and the composite powder deionized water of indium hydroxide being cleaned up
Dry 15h at a temperature of 120 DEG C, then the composite powder of drying is placed in air with 1550 DEG C of temperature calcination
20h, obtains stannic acid indium compound, and the stannic acid indium compound after calcining is loaded high energy ball mill with ball material
Ratio 5:1 ball milling 1h, crosses 200 eye mesh screens, obtains stannic acid indium powder after taking-up；
4) putty powder B and silver nitrate solution are placed in another reactor, stir and (be sufficiently stirred for
100min), silver nitrate and the suspension of putty powder B are obtained；It is added thereto to step 3) stannum of gained
Acid indium powder, adds sodium hydroxide B solution (drop rate is 0.5L/min), stirring reaction 0.5h, mistake
Filter, obtains silver oxide, stannum oxide and stannic acid indium composite powder；
5) by the silver oxide of gained, stannum oxide and stannic acid indium composite powder deionized water at centrifugal swing dryer
Supernatant is washed till neutrality, dries 18h with 120 DEG C of temperature the most in an oven, is then put by the composite powder of drying
In bipyramid blender broken (rotating speed 25r/min, time 1h)；Gained powder is placed in air with 450
DEG C temperature calcination 6h, is placed in bipyramid blender broken (rotating speed 25r/min, time 1h) again after taking-up,
Cross 200 mesh sieves, obtain the siller tin oxide composite powder containing stannic acid indium；
6) (briquetting pressure is in gained siller tin oxide composite powder molding on hydraulic press containing stannic acid indium
12T/cm2), and the pressed compact after molding is placed in air with 920 DEG C of temperature sintering 6h, obtain containing stannic acid
The siller tin oxide briquet of indium；
7) gained carries out multiple pressure containing the siller tin oxide briquet of stannic acid indium (multiple pressure pressure is 18T/cm2), and will be multiple
The siller tin oxide briquet containing stannic acid indium after pressure is placed in air with 920 DEG C of temperature resintering 8h, obtains stanniferous
Siller tin oxide (the Ag-SnO of acid indium2(15)-In4Sn3O12(2)) electrical contact.
Gained contact material is carried out metallographic structure analysis, as it is shown on figure 3, present techniques as seen from the figure
The metallographic structure of contact product prepared by scheme is uniform, and tiny stannum oxide and stannic acid indium granule divide equably
Cloth is in silver matrix.
The contact material that embodiment 1 and comparative example 1 prepare is carried out performance detection, and mixes with existing routine
The contact product of the siller tin oxide adding Indium sesquioxide. that powder-monolithic pressing prepares compares, and result is as follows
State shown in table 1:
Table 1 embodiment 1 and comparative example 1 mix articles of sheet material performance prepared by powder-monolithic pressing with existing routine
As shown in Table 1, the property of the sliver oxidized tin contactor materials containing stannic acid indium that prepared by technical scheme
Can be better than comparative example 1 and existing routine is mixed the siller tin oxide containing Indium sesquioxide. prepared by powder-monolithic pressing and touched
Head material performance.
Claims (6)
1. the preparation method of the siller tin oxide electric contact material containing stannic acid indium, it is characterised in that bag
Include following steps:
1) institute is calculated according to the material mixture ratio of the siller tin oxide electric contact containing stannic acid indium of required preparation
The consumption of putty powder, indium nitrate and silver nitrate needed, according to the consumption of indium nitrate calculate indium nitrate and
Sodium hydroxide reaction generates the consumption of the sodium hydroxide needed for indium hydroxide, represents with sodium hydroxide A；
Consumption according to silver nitrate calculates silver nitrate and sodium hydroxide reaction generates the hydroxide needed for silver oxide
The consumption of sodium, represents with sodium hydroxide B；Weigh above-mentioned substance, standby；Take silver nitrate water dissolution
It is made into the silver nitrate solution of 20～40w/w%, takes indium nitrate water dissolution and be made into indium nitrate solution；Take hydrogen
Sodium oxide A water dissolution wiring solution-forming, obtains sodium hydroxide solution A；Take sodium hydroxide B with water-soluble
Solution is made into the solution of 10～30w/w%, obtains sodium hydroxide B solution；The putty powder weighed is divided into
Two parts, portion is putty powder A, in an amount of from reacting, with indium nitrate and sodium hydroxide, the hydrogen generated
Indium sesquioxide. reaction is completely to generate the amount of stannic acid indium, and another part is putty powder B；
2) putty powder A and indium nitrate solution are placed in reactor, stir, obtain stannum oxide
Powder A and the suspension of indium nitrate；Adding sodium hydroxide solution A in this suspension, stirring is reacted,
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, are dried rearmounted
It is calcined in oxygen-containing atmosphere, then ball milling, obtains stannic acid indium powder；
4) putty powder B and silver nitrate solution are placed in another reactor, stir, obtain nitre
Acid silver and the suspension of putty powder B；It is added thereto to step 3) the stannic acid indium powder of gained, add
Sodium hydroxide B solution, stirring reaction, filter, obtain silver oxide, stannum oxide and stannic acid indium composite powder
End；
5) silver oxide of gained, stannum oxide and stannic acid indium composite powder are washed to neutrality, dry, powder
Carry out roasting after broken, then pulverize, obtain the siller tin oxide composite powder containing stannic acid indium；
6) gained siller tin oxide composite powder oil pressure molding containing stannic acid indium, is placed in oxygen-containing atmosphere the most again
Sintering, obtains the siller tin oxide briquet containing stannic acid indium；
7) gained siller tin oxide briquet containing stannic acid indium carries out multiple pressure, resintering, i.e. obtains containing stannic acid indium
Siller tin oxide electric contact material.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, need
In the siller tin oxide electric contact material containing stannic acid indium of preparation, stannum oxide content is 8～15wt%, stannic acid
The content of indium is 0.1～4wt%, and surplus is silver.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, nitric acid
The concentration of silver solution is 30～40w/w%.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, take nitre
Acid indium water is made into the solution that concentration is 30～40w/w%.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, take hydrogen
Sodium oxide A water is made into the solution that concentration is 10～30w/w%.
Preparation method the most according to claim 1, it is characterised in that: step 1) in, hydrogen-oxygen
The concentration changing sodium B solution is 15～25w/w%.
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| JP3838615B2 (en) * | 2000-02-10 | 2006-10-25 | 同和鉱業株式会社 | Tin-doped indium oxide powder and method for producing the same |
| US7201888B2 (en) * | 2003-10-07 | 2007-04-10 | Ferro Corporation | Nanosized silver oxide powder |
| DE102005038235A1 (en) * | 2005-08-12 | 2007-02-15 | Umicore Ag & Co. Kg | Use of indium-tin mixed oxide for silver-based materials |
| US7842274B2 (en) * | 2006-03-31 | 2010-11-30 | Umicore, S.A. | Process for manufacture of silver-based particles and electrical contact materials |
| CN102142325B (en) * | 2010-12-30 | 2013-04-03 | 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 |
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