CN113245548B - Infiltration processing technology and silver-tungsten contact material prepared by same - Google Patents
Infiltration processing technology and silver-tungsten contact material prepared by same Download PDFInfo
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- CN113245548B CN113245548B CN202110581153.XA CN202110581153A CN113245548B CN 113245548 B CN113245548 B CN 113245548B CN 202110581153 A CN202110581153 A CN 202110581153A CN 113245548 B CN113245548 B CN 113245548B
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
The invention provides an infiltration processing technology and a silver-tungsten contact material prepared by the technology, wherein the infiltration processing technology comprises the following steps: preparing tungsten and silver powder; pressing tungsten and silver powder to obtain a green compact of the powder, and controlling the density of the green compact at a specified pressure during pressing; carrying out primary silver infiltration processing on the pressed green body; machining the billet subjected to the primary silver infiltration processing; and finally inspecting and shipping the silver-tungsten contact material obtained by machining. According to the invention, the problems of long preparation time, unstable finished product quality and higher cost in the whole production process are effectively solved, and the process can realize the preparation of the silver-tungsten contact material by a one-step method, save the operation procedures, ensure and maintain the stable preparation process, realize stable and high-quality products, and reduce the overall cost.
Description
Technical Field
The invention relates to an infiltration processing technology and a silver-tungsten contact material prepared by the technology.
Background
The alloy contact belongs to a composite material product, and infiltration is a process method for filling pores in an unsintered or sintered product by using metal or alloy with a melting point lower than that of the product in a molten state.
Infiltration, also known as impregnation, refers to the infiltration of a molten second metal or alloy melt into the pores of a solid phase skeleton. The preparation is generally carried out in two steps. Firstly, the pressure forming and solid phase sintering are used to prepare a skeleton or rigid porous pressed compact. A preform made of the infiltrant is then placed over the skeleton. When the heating temperature exceeds the melting point of the infiltration agent, the infiltration agent is melted to generate a liquid phase, and the liquid phase infiltrates and fills the communicating pores under the action of capillary force between the infiltration agent and the matrix particles. The infiltration process can improve the density, strength, toughness, hardness, impact strength and thermal conductivity of the metal base material. Parts produced by the infiltration process are easy to electroplate, weld or braze and have high machinability. Steel parts produced by the infiltration process can be processed by normal heat treatment processes.
Vacuum brazing refers to heating of workpieces in a vacuum chamber, and is mainly used for welding products with high quality and easily-oxidized materials. And the silver-tungsten contact is easy to have welding performance failure during vacuum brazing.
In the prior art, a certain amount of copper material is added into a silver electric contact material, and then in the subsequent processing process, the added copper is tightly combined with the original silver through a copper sheet infiltration process, so that gaps between the copper and the silver can be fully filled by the infiltrated copper, so that the materials are tightly combined, but various components cannot be accurately controlled by adopting the process, and the process is divided into two sides by pressing, so that the effect of reducing the cost cannot be achieved.
In addition, in the prior art, there is also a method for preparing an AgMe contact material for a circuit breaker, which includes premixing Ag powder, Me powder and additive powder, performing wet ball milling at high and low speeds alternately, performing wet glue mixing granulation and drying on the powder subjected to wet ball milling, molding and pressing the granulated powder to obtain a green body, degumming and sintering the green body to obtain a skeleton, and finally infiltrating the degummed and sintered skeleton and Ag to obtain the AgMe electrical contact material.
The existing process for preparing silver-tungsten contact material using infiltration process as described above has the following disadvantages: the high-temperature sintering tungsten framework is adopted, and two times of pressing are needed, so that the preparation time is long, the content of silver in the high-temperature infiltration process is difficult to accurately control, the quality of a finished product is unstable, the welding performance is easy to lose efficacy in vacuum brazing, the infiltration time is long, and the cost is high.
Therefore, whether the improved infiltration processing technology and the silver-tungsten contact material prepared by the improved infiltration processing technology can be provided based on the defects in the prior art or not can be realized, the problems of long preparation time, unstable finished product quality, easy welding performance failure during vacuum brazing and high cost can be effectively solved, the cost of the whole production process is reduced, and a stable high-quality product can be ensured and maintained, so that the technical problem to be solved urgently by technical personnel in the field is solved.
Disclosure of Invention
Problems to be solved by the invention
The invention aims to overcome the defects of the prior art and provide an improved infiltration processing technology and a silver-tungsten contact material prepared by the technology. According to the improved infiltration processing technology and the silver-tungsten contact material prepared by the technology, the pressure is accurately controlled, only one-time infiltration is carried out after fixed green body density is manufactured, the component accuracy can be ensured, the infiltration time can be greatly shortened, the whole manufacturing cost is reduced, the stable quality is realized, the yield is high, and the cost is saved.
Means for solving the problems
The invention relates to an infiltration processing technology, which comprises the following steps:
preparing tungsten and silver powder;
pressing tungsten and silver powder to obtain a green compact of the powder, and controlling the density of the green compact at a specified pressure during pressing;
carrying out primary silver infiltration processing on the pressed green body without sintering;
machining the billet subjected to the primary silver infiltration processing;
carrying out final inspection and loading on the silver-tungsten contact material obtained by mechanical processing,
in the primary infiltration process, the infiltration temperature is adjusted as follows, the silver solution is firstly insulated for 15-50 minutes at 1010-1060 ℃ and then insulated for 25-60 minutes at 1070-1170 ℃.
Preferably, in the primary infiltration process, the infiltration temperature is adjusted as follows, the silver liquid is firstly preserved for 20-40 minutes at 1020-1050 ℃ and then preserved for 30-50 minutes at 1090-1150 ℃.
Preferably, in the primary infiltration process, the infiltration temperature is adjusted such that the silver solution is first incubated at 1030-1040 ℃ for about 28-32 minutes and then at 1105-1115 ℃ for about 38-42 minutes.
Preferably, the specified pressure is 20-350 KN.
Preferably, the specified pressure is 30-250 KN.
Preferably, the specified pressure is 50-200 KN.
Preferably, the density of the green body is controlled to be 9 to 16g/cm3。
Preferably, the density of the green body is controlled to be 10.2 to 14.5g/cm3。
Preferably, the primary silver impregnation process is performed using a continuous furnace.
Preferably, the mass percent of silver is 10% -30%.
The second aspect of the invention relates to a silver-tungsten contact material which is prepared by the infiltration processing technology of the first aspect of the invention.
Preferably, the silver tungsten contact material has a diameter of less than 40mm and a height of less than 5 mm.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the infiltration processing technology related to the first aspect of the invention, not only can the component accuracy be ensured, but also the infiltration time can be greatly shortened, the problems of long preparation time, unstable finished product quality and higher cost can be effectively solved, the cost of the whole production process is reduced, and the stable high-quality product can be ensured and maintained.
According to the silver-tungsten contact material related to the second aspect of the invention, stable product quality, high yield and cost saving are realized.
Drawings
Fig. 1 is a flowchart of an infiltration process according to a first embodiment of the present invention.
Fig. 2 is a schematic view of a silver tungsten contact resulting from the infiltration process of fig. 1.
Detailed Description
First, the infiltration process according to the present invention will be described in detail below.
Fig. 1 is a flowchart of an infiltration process according to a first embodiment of the present invention. As shown in fig. 1, the infiltration process is specifically performed by preparing tungsten and silver powder, weighing the tungsten and silver powder at a predetermined ratio, for example (step S101), pressing the tungsten and silver powder to obtain a green compact of the powder, controlling the density of the green compact at a predetermined pressure during pressing (step S102), controlling and determining the content of the infiltrated silver by the pressure of the powder, and controlling the mass percentage of silver to 10% to 30%, preferably 15% to 25%, or 18% to 22%. The pressure is controlled by a control device (such as a computer), is very easy to measure and control, and the green density is accurately controlled by using the pressure of 30-250KN and is controlled to be 10-16g/cm3And the green density of the silver-tungsten contact material can be precisely controlled and adjusted by a control device (e.g., a computer), such as a press force curve calculated and adjusted by the control device. Then carrying out primary silver infiltration processing on the pressed powder without sintering (step S103), wherein in the primary silver infiltration processing step, the temperature is regulated in two stages in a manner similar to climbing in the same step, preferably in the primary silver infiltration processing, the infiltration temperature is adjusted in such a way that the silver liquid is firstly preserved at 1010-1050 ℃ for 15-50 minutes, preferably at 1020-1050 ℃ for 20-40 minutes, and more preferably at 1030-1040 ℃ for about 28-32 minutes; further, the temperature is maintained at 1070-1170 ℃ for 25-60 minutes, preferably at 1090-1150 ℃ for 30-50 minutes, more preferably at 1105-1115 ℃ for 38-42 minutes, but the temperature is not limited thereto, and may be adjusted to other temperatures and times, preferably, the tungsten-silver infiltration process is performed by using a continuous furnace, but is not limited thereto, and the tungsten-silver infiltration process may be performed by using batch equipment or other suitable devices. The once-silver-infiltrated block is machined again (step S104), and finally the machined silver-tungsten contact is finally inspected and shipped (step S105), for example, by observing the metallographic microstructure by a conventional apparatus.
The traditional processing technology generally adopts a batch furnace, all products are sintered at one time, the batch furnace and all the products are fixed in a hot zone, the continuous furnace is modern newly developed continuous sintering equipment, a conveying belt conveying device passes through the whole hot zone, the products are heated very uniformly by adopting the continuous furnace, a thermal field experienced by each sample is the same, large-scale and continuous production can be realized, and the lowest cost and the largest large-scale production can be realized.
Compared with the existing infiltration processing technology, the infiltration processing technology of the invention accurately controls the density of the green body through pressure, the existing sintering and infiltration processes are included in one-time infiltration silver processing, which is equivalent to reducing the two-step technology of the prior art into one step, so that high-temperature framework sintering is not needed any more, and the infiltration time is very short by adopting a continuous furnace, only one-time pressing is needed, and two-time pressing is not needed like the prior art, so that the processing time is saved. In the prior art, two steps of sintering and infiltration are needed, the common method is to sinter in a sintering furnace firstly and then infiltrate in an infiltration furnace, and the temperature is regulated in two stages in a climbing-like manner during infiltration. By accurately controlling and adjusting the proportion of tungsten and silver and the density of the green body, stable quality is realized, the cost of the whole production process is reduced, and stable high quality can be ensured and maintained.
The invention provides a silver-tungsten contact, which is characterized in that a silver-tungsten contact is subjected to vacuum brazing, and welding performance failure is easy to occur when a double-pressing process in the prior art is adopted.
Originally, in the whole production and manufacturing process of the silver-tungsten contact material, because the sintering time of the high-temperature framework is longer and the temperature is higher, the sintering process of the high-temperature framework accounts for 24% -30% of the whole cost according to the electricity cost, the labor cost, the equipment depreciation cost and other costs, and the time of high-temperature sintering is multiplied, the infiltration processing technology of the invention omits the step, and compared with the prior art, the cost is substantially saved by 24% -30%.
Hereinafter, suitable examples of the present invention will be described, but the embodiments of the present invention are not limited thereto.
< example 1 >
The infiltration process of example 1 first prepares tungsten and silver powders, weighs the tungsten and silver powders in a predetermined ratio of 2 to 1, then compacts the tungsten and silver powders, controls the density of the green compact at a prescribed pressure during compaction, controls and determines the silver content by the pressure, specifically, controls the silver content to 18-22% by mass, and controls the tungsten skeleton density to 10.2-14.5 g/cm3The pressure is controlled by a computer, the green density is accurately controlled within the range by adopting the accurate pressure control of 50-200KN, and the green density of the silver-tungsten contact material can be accurately controlled and adjusted by the computer, and the pressing force curve is calculated and adjusted by the computer. The final silver content and pressure are determined by the following formula:
Y= K1•X + K2
where X is the pressure, Y is the silver content, K1 and K2 are constants depending on the equipment and the raw materials, K1 being 0.0182 and K2 being 11.425 in this example.
And then carrying out primary silver infiltration processing on the pressed powder, wherein in the primary silver infiltration processing, the infiltration temperature is adjusted as follows, the silver liquid is firstly kept at 1030 ℃ for about 30 min, then kept at 1130 ℃ for about 40min, and a continuous furnace is used for carrying out primary tungsten silver infiltration process. And then machining the powder after the continuous furnace processing, and finally carrying out final inspection and shipment on the silver-tungsten contact obtained by machining, wherein the diameter of the finally obtained product is about 25mm, and the height of the finally obtained product is less than 4.4 mm.
< example 2 >
The infiltration process of example 2 begins with the preparation of tungsten and silver powders according to a predetermined scheduleWeighing tungsten and silver at a ratio of 3: 1, pressing the tungsten and silver powder, controlling the density of the green body at a specified pressure during pressing, wherein the content of silver is controlled and determined by the pressure, specifically, the mass percent of silver is controlled to be 10-30%, and the density of the tungsten skeleton is controlled to be 9.0-13.0g/cm3The pressure is controlled by a computer, the green density is accurately controlled within the range by adopting the accurate pressure control of 20-180KN, the green density of the silver-tungsten contact material can be accurately controlled and adjusted by the computer, and the pressing force curve is calculated and adjusted by the computer. The final silver content and pressure are determined by the following formula:
Y= K1•X + K2
where X is the pressure, Y is the silver content, K1 and K2 are constants depending on the equipment and the raw materials, K1 being 0.0185 and K2 being 11.427 in this example.
And then carrying out primary infiltration processing on the pressed powder, wherein in the primary infiltration processing, the infiltration temperature is adjusted as follows, the silver liquid is firstly preserved for 30 min at 1010-1050 ℃, then preserved for 35min at 1110-1150 ℃, and a continuous furnace is used for carrying out primary infiltration tungsten-silver process. And then, machining the powder processed by the continuous furnace, and finally, carrying out final inspection and shipment on the silver-tungsten contact obtained by machining, wherein the diameter of the finally obtained product is 20mm, and the height of the finally obtained product is less than 5 mm.
< example 3 >
The infiltration process of example 3 first prepares tungsten and silver powders, weighs the tungsten and silver powders in a predetermined 4 to 1 ratio, then compacts the tungsten and silver powders, controls the density of the green compact at a prescribed pressure during compaction, controls and determines the silver content by the pressure, specifically, controls the silver content to 15-25% by mass, and controls the density of the tungsten skeleton to 12.0-16.0g/cm3The pressure is controlled by a computer, the green density is accurately controlled within the range by adopting the accurate pressure control of 40-350KN, and the green density of the silver-tungsten contact material can be accurately controlled and adjusted by the computer, and the pressing force curve is calculated and adjusted by the computer. The final silver content and pressure are determined by the following formula:
Y= K1•X + K2
where X is the pressure, Y is the silver content, K1 and K2 are constants depending on the equipment and the raw materials, K1 being 0.0189 and K2 being 11.429 in this example.
And then carrying out primary silver infiltration processing on the pressed powder, wherein in the primary silver infiltration processing, the infiltration temperature is adjusted as follows, the silver liquid is firstly kept at 1050 ℃ for 30 min, then kept at 1110 ℃ for 45min, and a continuous furnace is used for carrying out primary tungsten silver infiltration process. And then machining the powder after the continuous furnace processing, and finally carrying out final inspection and shipment on the silver-tungsten contact obtained by machining, wherein the diameter of the finally obtained product is about 23mm, and the height of the finally obtained product is less than about 4 mm.
Through the infiltration processing technology applied to the embodiments 1-3, the existing sintering and infiltration processes are included in one-time silver infiltration processing, which is equivalent to reducing the two-step technology of the prior art into one step, so that high-temperature framework sintering is not needed any more, and the infiltration time is very short due to the adoption of a continuous furnace, and only one-time pressing is needed instead of two-time pressing as in the prior art, so that the processing time is saved. The proportion of tungsten and silver and the density of the tungsten skeleton are accurately controlled and adjusted, the quality is stable, the cost of the whole production process is reduced, and the stable high quality can be ensured and maintained.
Next, the silver-tungsten contact material according to the present invention will be described in detail.
The silver-tungsten contact material of the second embodiment of the present invention is the silver-tungsten contact material prepared by the infiltration process of the first embodiment of the present invention, and is preferably a small-sized silver-tungsten contact material, and more preferably has a diameter of less than 40mm and a height of less than 5 mm. The representative embodiment is shown in figure 2, which is a sheet with a circular section, the diameter is 20-30mm, the height is less than 5mm and preferably 2-4mm, and the device is suitable for equipment such as medium and high voltage vacuum switches, circuit breakers, electrical switches, instruments and meters. The silver-tungsten contact material prepared by the existing infiltration processing technology and the infiltration processing technology of the first embodiment of the invention are compared. Specifically, the silver-tungsten contact material was prepared by the conventional infiltration process in which the pressing was performed twice, and the pressing-sintering-skeleton-infiltration process was performed in each of the comparative examples i and ii shown in the table.
Robert Grill, etc. WC / Ag Contact Materials with Improved Homogeneity. RM 20，
In the above documents, a plurality of examples are described, and in the following tables, comparative example one and comparative example two are both examples when the mass percentage of silver is 35%. The invention in the following table uses the product made in example 1 above. According to the ASTM B663-94 standard issued by the American society for testing and materials, silver-tungsten contact materials are largely used in medium-voltage vacuum switches, and the three indexes of density, hardness and conductivity directly influence the electroerosion, the cut-off current and the service life of the contact materials. The silver-tungsten contact materials prepared in these comparative examples were compared with the silver-tungsten contact material of the present invention in terms of density, hardness, and electrical conductivity as shown in the following table.
In the above table, density measurement was performed using a gravimetric method or a buoyancy method, a displacement method, a specific gravity method, and a digital density method, hardness measurement was performed using HV10 or HV30 in vickers hardness measurement, and conductivity measurement was performed using a conductivity meter.
As shown in the above table, the infiltration process of the first embodiment is used to prepare the silver-tungsten contact material of the second embodiment, which reduces the production time and the production cost, but compared with the conventional process with long production time and high cost, the prepared silver-tungsten contact material has stable quality and high yield.
Specifically, the yield of the contact material with a height of 3.9mm can reach 99.9%, the yield of the contact material with a height of 4mm is about 99%, and the yield of the contact material with a height of about 5mm is about 97%. In the prior art, if the yield close to the present invention is obtained, the infiltration time needs to be increased to about 16 hours or more, and the corresponding cost is greatly increased.
The silver-tungsten contact material of the second embodiment of the present invention is an embodiment corresponding to the infiltration process of the first embodiment. Therefore, various implementation points in the first embodiment are also applicable to the second embodiment, and are not described herein.
According to the silver-tungsten contact material provided by the second embodiment of the invention, the problems of long preparation time, unstable finished product quality and high cost are effectively solved, the cost of the whole production process is reduced, stable high-quality products can be ensured and maintained, the stable quality and high yield are realized, and the cost is saved.
Industrial applicability
According to the infiltration processing technology and the silver-tungsten contact material, the problems of long preparation time, unstable finished product quality and higher cost in the whole production process are effectively solved, the preparation of the silver-tungsten contact material can be realized through a one-step method, the operation procedure is saved, the stable product preparation process is ensured and maintained, stable products with high quality and high yield are realized, and the overall cost is reduced.
While the invention has been shown and described with reference to certain preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. An infiltration processing technology is characterized by comprising the following steps:
preparing tungsten and silver powder;
compacting tungsten and silver powder to obtain green compact, and controlling the density of the green compact to 12.0-16.0g/cm at a specified pressure, i.e. 40-350KN3The mass percentage of the infiltration silver is 15-25 percent;
carrying out primary silver infiltration processing on the pressed green body without sintering;
machining the billet subjected to the primary silver infiltration processing;
carrying out final inspection and loading on the silver-tungsten contact material obtained by mechanical processing,
in the primary infiltration process, the infiltration temperature is adjusted as follows, the silver solution is firstly insulated for 15-50 minutes at 1010-1060 ℃ and then insulated for 25-60 minutes at 1070-1170 ℃.
2. The infiltration processing of claim 1,
in the primary infiltration processing, the infiltration temperature is adjusted as follows, the silver liquid is firstly preserved for 20-40 minutes at 1020-1050 ℃ and then preserved for 30-50 minutes at 1090-1150 ℃.
3. The infiltration processing of claim 2,
in the primary infiltration process, the infiltration temperature is adjusted as follows, the silver liquid is firstly insulated for 28-32 minutes at 1030-1040 ℃ and then insulated for 38-42 minutes at 1105-1115 ℃.
4. The infiltration processing of claim 1,
the specified pressure is 50-200 KN.
5. The infiltration processing process of any one of claims 1-4,
and carrying out primary silver infiltration processing by using a continuous furnace.
6. The infiltration processing process of any one of claims 1-4,
the mass percentage of the infiltration silver is 18-22%.
7. A silver-tungsten contact material is characterized in that,
is a silver-tungsten contact material prepared by the infiltration processing technology of any one of claims 1 to 6.
8. The silver tungsten contact material according to claim 7,
the diameter of the silver-tungsten contact material is less than 40mm, and the height of the silver-tungsten contact material is less than 5 mm.
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| 电力机车调压开关用Ag-W70触头材料;谢健全;《粉末冶金工业》;20000831;第10卷(第4期);第30-33页 * |
| 银钨触头材料的制备工艺及使用性能;孟繁琦等;《材料导报》;20060531;第20卷;第321-324页 * |
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