CN105458273A - Method for promoting oxidation of Ag-Sn alloy powder through high energy ball milling method - Google Patents
Method for promoting oxidation of Ag-Sn alloy powder through high energy ball milling method Download PDFInfo
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- CN105458273A CN105458273A CN201510844479.1A CN201510844479A CN105458273A CN 105458273 A CN105458273 A CN 105458273A CN 201510844479 A CN201510844479 A CN 201510844479A CN 105458273 A CN105458273 A CN 105458273A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1078—Alloys containing non-metals by internal oxidation of material in solid state
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention provides a method for promoting oxidation of Ag-Sn alloy powder through a high energy ball milling method. The method comprises the steps of 1, ball milling, wherein the Ag-Sn alloy powder and a ball are added into a ball milling tank, then the ball milling tank is put into a ball mill, protective gas is introduced, and ball milling is carried out for 5-20 h under the condition that the rotating speed is 170-250 rpm; and 2, oxidation, wherein the Ag-Sn alloy powder subjected to ball milling in the first step is put into an oxidizing furnace, oxidation is carried out for 20-110 h under the conditions that the oxygen pressure is 1-2 MPa, and the temperature is 500-700 DEG C, and an oxidation product, Ag-SnO2 composite powder, can be obtained. In the process of preparing the Ag-SnO2 powder, no In or other precious metal is added, and cost is low. The internal oxidation performance of the Ag-Sn alloy powder can be remarkably improved, and 96% of Sn in the Ag-Sn alloy powder with the weight percent of Sn reaching up to 12% can be oxidized into SnO2.
Description
(1) technical field
The present invention relates to field of metal matrix composite, be specifically related to a kind of by the oxidation of high-energy ball milling method promotion Ag-Sn alloyed powder, with the Ag-SnO of obtained high-load Sn
2the method of composite.
(2) background technology
Siller tin oxide (Ag-SnO
2) be with SnO
2particle is the Ag based composites of second-phase, there is asepsis environment-protecting, good anti-melting welding and resistance to electrical arc erosion performance, be the Novel electric contact material being hopeful alternative toxic material Agcdo (Ag-CdO) most, be widely applied in Large Copacity contactor, power relay, Small And Medium Capacity low-voltage circuit breaker and car electrics.
At present, widely used Ag-SnO
2contact material, main alloy inner oxidation method and the powder metallurgic method of adopting is produced.Internal oxidation is that Ag is smelt alloy with adding Metal Melting, then before or after machine-shaping, is heated to sufficiently high temperature in oxygen atmosphere, insulation a period of time, makes burning.But when Sn content is greater than 5wt%, Ag-Sn alloy is but difficult to oxidation, and this mainly defines the oxidation film of one deck densification due to Ag-Sn alloy surface, prevents oxygen atom to the diffusion of alloy inside; Powder metallurgic method prepares Ag-SnO
2material is by Ag and SnO
2and Addition ofelements puts into batch mixer, the rolling carrying out different time mixes powder, and material powder is fully mixed, then put into mould stamping, sintering, become the forming method using contact, this method has the advantage that technique is simple, cost is low, constituent content is controlled.But due to Ag powder and SnO
2the original grain border of powder self is difficult to eliminate, and causes material properties for follow sharply to worsen, and finished material rate declines.
Pre-oxidation alloyage be a kind of at alloy inner oxidation technique and powder metallurgical technique in conjunction with on basis, the manufacture Ag-SnO of new development
2the advanced technologies method of contact material.Its main contents, are first be oxidized by Ag-Sn alloyed powder, and then carry out powder metallurgy.The material obtained has the advantage of internal oxidation and powder metallurgic method, the Ag-SnO produced with alloy powder preoxidation
2material, SnO
2particle is high degree of dispersion in Ag matrix, even tissue, and wearability and the resistance fusion welding of material all improve a lot.But when not adding the elements such as prooxidant In, the silver-colored ashbury metal powder of high-load Sn is still difficult to be fully oxidized under hyperbaric oxygen, and In memory space is few, price is high, causes the increase of its production cost, limits further developing of pre-oxidation alloyage.Therefore, need to carry out further process modification to it.
(3) summary of the invention
The object of this invention is to provide a kind of method that high-energy ball milling method promotes the oxidation of Ag-Sn alloyed powder, the method environmental protection, cost is low, simple to operate, and in the raw material A g-Sn alloy adopted, the percetage by weight of Sn can up to 12%.
For achieving the above object, the present invention adopts following technical scheme.
High-energy ball milling method promotes a method for Ag-Sn alloyed powder oxidation, and described method is carried out as follows:
(1) ball milling: Ag-Sn alloy powder and spheroid are added in ball grinder, then spheroidal graphite tank is placed in ball mill, pass into protective gas, under rotating speed is 170 ~ 250rpm condition, carries out ball milling 5 ~ 20h; In described Ag-Sn alloy powder, the percetage by weight of Ag is 88% ~ 99%; The percetage by weight of Sn is 1% ~ 12%;
(2) be oxidized: the Ag-Sn alloy powder through step (1) ball milling is put into oxidation furnace, be 1 ~ 2MPa in oxygen pressure, temperature is carry out oxidation 20 ~ 110h (preferably 70 ~ 110h) under the condition of 500 ~ 700 DEG C, obtains oxidation product Ag-SnO
2composite powder.
Further, the present invention, by step (2) gained oxidation product being repeated again ball milling, the oxidation of step (1) and step (2), obtains oxidation product Ag-SnO after repeating 1 ~ 10 time
2composite powder, makes the Sn in alloy be oxidized fully, and preferred number of repetition is 1 ~ 3 time.
In the present invention, raw material A g-Sn alloy powder can adopt the powder by atomization method of this area routine to obtain, and is specially: metal A g and metal Sn are heated to melting, obtain metal bath, then adopt high-voltage high-speed airflow to be smashed by metal bath, after cooling, namely obtain Ag-Sn alloy powder.
In step of the present invention (1), the ball mill described in recommendation adopts agate spheroid, agate jar and planetary ball mill, and adopts the mode that positive and negative 15min alternately rotates in mechanical milling process.
In step (1), the ball material mass ratio of preferred described spheroid and Ag-Sn alloy powder is 10 ~ 15:1.
In step (1), described protective gas can be: the inert gas such as nitrogen, argon gas.
Concrete, recommend the method for the invention to carry out as follows:
(1) ball milling: Ag-Sn alloy powder and spheroid are added in ball grinder, then spheroidal graphite tank is placed in ball mill, pass into protective gas, under rotating speed is 170 ~ 250rpm condition, carries out ball milling 5 ~ 20h; In described Ag-Sn alloy powder, the percetage by weight of Ag is 88% ~ 99%; The percetage by weight of Sn is 1% ~ 12%; The ball material mass ratio of described spheroid and Ag-Sn alloy powder is 10 ~ 15:1;
(2) be oxidized: the Ag-Sn alloy powder through step (1) ball milling is put into oxidation furnace, is 1 ~ 2MPa in oxygen pressure, and temperature is carry out oxidation 70 ~ 110h under the condition of 500 ~ 700 DEG C, obtains oxidation product;
(3) ball milling, oxidation step is repeated: get step (2) gained oxidation product and carry out a ball milling again according to the process of step (1), oxidation furnace is put into after ball milling, be warming up to 500 ~ 700 DEG C, insulation 20 ~ 30h, be carry out once oxidation again under the condition of 1 ~ 2MPa in oxygen pressure, obtain Ag-SnO
2composite powder.
Compared with prior art, beneficial effect of the present invention shows:
(1) the present invention is at preparation Ag-SnO
2do not add the noble metals such as In in the middle of powder process, cost is low;
(2) in raw material Ag-Sn alloy of the present invention, the percetage by weight of Sn reaches as high as 12%, the Ag-SnO that Sn content is so high so far
2material has no and makes by the method;
(3) the present invention can significantly improve the internal oxidition performance of Ag-Sn alloy powder, and containing Sn percetage by weight up in the Ag-Sn alloy powder of 12%, the Sn of 96% can be oxidized to SnO
2.
(4) accompanying drawing explanation
Fig. 1 is Ag-SnO obtained in embodiment 1
2composite metallographic microscope photo, multiplication factor 200;
Fig. 2 is Ag-SnO obtained in embodiment 2
2composite metallographic microscope photo, multiplication factor 200;
Fig. 3 is Ag-SnO obtained in embodiment 3
2composite metallographic microscope photo, multiplication factor 200;
Fig. 4 is Ag-SnO obtained in embodiment 4
2composite metallographic microscope photo, multiplication factor 200;
Fig. 5 is undressed Ag-Sn alloy XRD photo;
Fig. 6 is Ag-SnO obtained in embodiment 4
2composite XRD photo.
(5) detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this.
Embodiment 1
(1) alloy will prepared is by the composition designed than batching, and this tests Ag content 88wt%, Sn content 12wt% in Ag-Sn alloy.Adopt powder by atomization legal system for Ag-Sn alloy powder.
(2) 30gAg-Sn alloy powder is taken.It on average joined in 2 tank agate jars, every tank 15g, selects agate ball, and wherein ball material mass ratio is 10:1, and adopts planetary ball mill, rotating speed 170 revs/min, within clockwise 15 minutes counterclockwise 15 minutes, alternately rotates, it is carried out to the ball milling of 10 hours.Pass into nitrogen in the process of ball milling, prevent in process of lapping oxidized.
(3) the Ag-Sn alloy powder through step (2) ball milling is put into oxidation furnace, be warming up to 500 DEG C, be incubated 70 hours, oxygen pressure 1.5MPa, (in Ag-Sn alloy, 63%Sn is converted into SnO to obtain oxidation product
2).
(4) get step (3) gained oxidation product and carry out a ball milling again according to the process of step (2).After ball milling, direct room temperature enters stove, is warming up to 700 DEG C, is incubated 20 hours, carries out once oxidation again when oxygen pressure 1.5MPa.Products therefrom is Ag-SnO
2(in Ag-Sn alloy, 72%Sn is converted into SnO to composite powder
2).
Embodiment 2
(1) alloy will prepared is by the composition designed than batching, and this tests Ag content 88wt%, Sn content 12wt% in Ag-Sn alloy.Adopt powder by atomization legal system for Ag-Sn alloy powder.
(2) 30gAg-Sn alloy powder is taken.It on average joined in 2 tank agate jars, every tank 15g, selects agate ball, and wherein ball material mass ratio is 10:1, and adopts planetary ball mill, rotating speed 250 revs/min, within clockwise 15 minutes counterclockwise 15 minutes, alternately rotates, it is carried out to the ball milling of 15 hours.Pass into nitrogen in the process of ball milling, prevent in process of lapping oxidized.
(3) the Ag-Sn alloy powder through step (2) ball milling is put into oxidation furnace, be warming up to 600 DEG C, be incubated 90 hours, oxygen pressure 1.5MPa, (in Ag-Sn alloy, 61%Sn is converted into SnO to obtain oxidation product
2).
(4) get step (3) gained oxidation product and carry out a ball milling again according to the process of step (2).After ball milling, direct room temperature enters stove, is warming up to 500 DEG C, is incubated 30 hours, carries out once oxidation again when oxygen pressure 1.5MPa.Products therefrom is Ag-SnO
2(in Ag-Sn alloy, 78%Sn is converted into SnO to composite powder
2).
Embodiment 3
(1) alloy will prepared is by the composition designed than batching, and this tests Ag content 88wt%, Sn content 12wt% in Ag-Sn alloy.Adopt powder by atomization legal system for Ag-Sn alloy powder.
(2) 30gAg-Sn alloy powder is taken.It on average joined in 2 tank agate jars, every tank 15g, selects agate ball, and wherein ball material mass ratio is 10:1, and adopts planetary ball mill, rotating speed 200 revs/min, within clockwise 15 minutes counterclockwise 15 minutes, alternately rotates, it is carried out to the ball milling of 5 hours.Pass into nitrogen in the process of ball milling, prevent in process of lapping oxidized.
(3) the Ag-Sn alloy powder through step (2) ball milling is put into oxidation furnace, be warming up to 600 DEG C, be incubated 110 hours, oxygen pressure 1.5MPa, (in Ag-Sn alloy, 66%Sn is converted into SnO to obtain oxidation product
2).
(4) get step (3) gained oxidation product and carry out a ball milling again according to the process of step (2).After ball milling, direct room temperature enters stove, is warming up to 700 DEG C, is incubated 24 hours, carries out once oxidation again when oxygen pressure 1.5MPa.Products therefrom is Ag-SnO
2(in Ag-Sn alloy, 81%Sn is converted into SnO to composite powder
2).
Embodiment 4
(1) alloy will prepared is by the composition designed than batching, and this tests Ag content 88wt%, Sn content 12wt% in Ag-Sn alloy.Adopt powder by atomization legal system for Ag-Sn alloy powder.
(2) 30gAg-Sn alloy powder is taken.It on average joined in 2 tank agate jars, every tank 15g, selects agate ball, and wherein ball material mass ratio is 15:1, and adopts planetary ball mill, rotating speed 200 revs/min, within clockwise 15 minutes counterclockwise 15 minutes, alternately rotates, it is carried out to the ball milling of 5 hours.Pass into nitrogen in the process of ball milling, prevent in process of lapping oxidized.
(3) the Ag-Sn alloy powder through step (2) ball milling is put into oxidation furnace, be warming up to 600 DEG C, be incubated 90 hours, oxygen pressure 1.5MPa, (in Ag-Sn alloy, 78%Sn is converted into SnO to obtain oxidation product
2).
(4) get step (3) gained oxidation product and carry out a ball milling again according to the process of step (2).After ball milling, direct room temperature enters stove, is warming up to 700 DEG C, is incubated 24 hours, carries out once oxidation again when oxygen pressure 1.5MPa.Products therefrom is Ag-SnO
2(in Ag-Sn alloy, 96%Sn is converted into SnO to composite powder
2).
Claims (8)
1. high-energy ball milling method promotes a method for Ag-Sn alloyed powder oxidation, and described method is carried out as follows:
(1) ball milling: Ag-Sn alloy powder and spheroid are added in ball grinder, then spheroidal graphite tank is placed in ball mill, pass into protective gas, under rotating speed is 170 ~ 250rpm condition, carries out ball milling 5 ~ 20h; In described Ag-Sn alloy powder, the percetage by weight of Ag is 88% ~ 99%; The percetage by weight of Sn is 1% ~ 12%;
(2) be oxidized: the Ag-Sn alloy powder through step (1) ball milling is put into oxidation furnace, is 1 ~ 2MPa in oxygen pressure, and temperature is carry out oxidation 20 ~ 110h under the condition of 500 ~ 700 DEG C, obtains oxidation product Ag-SnO
2composite powder.
2. the method for claim 1, is characterized in that, step (2) gained oxidation product is repeated again ball milling, the oxidation of step (1) and step (2), obtains oxidation product Ag-SnO after repeating 1 ~ 10 time
2composite powder.
3. method as claimed in claim 2, it is characterized in that, the number of times of described repetition is 1 ~ 3 time.
4. the method for claim 1, is characterized in that, in step (1), described ball mill adopts agate spheroid, agate jar and planetary ball mill.
5. the method for claim 1, is characterized in that, in step (1) mechanical milling process, adopts the mode that positive and negative 15min alternately rotates.
6. the method for claim 1, is characterized in that, in step (1), the ball material mass ratio of described spheroid and Ag-Sn alloy powder is 10 ~ 15:1.
7. the method for claim 1, is characterized in that, in step (1), described protective gas is: nitrogen or argon gas.
8. the method for claim 1, is characterized in that, described method is carried out as follows:
(1) ball milling: Ag-Sn alloy powder and spheroid are added in ball grinder, then spheroidal graphite tank is placed in ball mill, pass into protective gas, under rotating speed is 170 ~ 250rpm condition, carries out ball milling 5 ~ 20h; In described Ag-Sn alloy powder, the percetage by weight of Ag is 88% ~ 99%; The percetage by weight of Sn is 1% ~ 12%; The ball material mass ratio of described spheroid and Ag-Sn alloy powder is 10 ~ 15:1;
(2) be oxidized: the Ag-Sn alloy powder through step (1) ball milling is put into oxidation furnace, is 1 ~ 2MPa in oxygen pressure, and temperature is carry out oxidation 70 ~ 110h under the condition of 500 ~ 700 DEG C, obtains oxidation product;
(3) ball milling, oxidation step is repeated: get step (2) gained oxidation product and carry out a ball milling again according to the process of step (1), oxidation furnace is put into after ball milling, be warming up to 500 ~ 700 DEG C, insulation 20 ~ 30h, be carry out once oxidation again under the condition of 1 ~ 2MPa in oxygen pressure, obtain product A g-SnO
2composite powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510844479.1A CN105458273A (en) | 2015-11-26 | 2015-11-26 | Method for promoting oxidation of Ag-Sn alloy powder through high energy ball milling method |
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|---|---|---|---|
| CN201510844479.1A CN105458273A (en) | 2015-11-26 | 2015-11-26 | Method for promoting oxidation of Ag-Sn alloy powder through high energy ball milling method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609794A (en) * | 2018-12-25 | 2019-04-12 | 桂林金格电工电子材料科技有限公司 | A kind of preparation method of high ductility sliver oxidized tin contactor materials |
| WO2019205231A1 (en) * | 2018-04-28 | 2019-10-31 | 中国科学院深圳先进技术研究院 | Method for preparing nanometer oxide particle reinforced metal composite material |
| CN111334694A (en) * | 2020-04-14 | 2020-06-26 | 燕山大学 | Method for modifying LPSO structure in magnesium alloy through primary nano disperse phase |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019205231A1 (en) * | 2018-04-28 | 2019-10-31 | 中国科学院深圳先进技术研究院 | Method for preparing nanometer oxide particle reinforced metal composite material |
| CN109609794A (en) * | 2018-12-25 | 2019-04-12 | 桂林金格电工电子材料科技有限公司 | A kind of preparation method of high ductility sliver oxidized tin contactor materials |
| CN111334694A (en) * | 2020-04-14 | 2020-06-26 | 燕山大学 | Method for modifying LPSO structure in magnesium alloy through primary nano disperse phase |
| CN111334694B (en) * | 2020-04-14 | 2021-10-15 | 燕山大学 | Method for modifying LPSO structure in magnesium alloy through primary nano disperse phase |
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