CN114921680B - Strip-shaped silver-copper-titanium active solder and preparation method thereof - Google Patents
Strip-shaped silver-copper-titanium active solder and preparation method thereof Download PDFInfo
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- CN114921680B CN114921680B CN202210549951.9A CN202210549951A CN114921680B CN 114921680 B CN114921680 B CN 114921680B CN 202210549951 A CN202210549951 A CN 202210549951A CN 114921680 B CN114921680 B CN 114921680B
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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
- C22C5/08—Alloys based on silver with copper as the next major constituent
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
-
- 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
- B22F3/03—Press-moulding apparatus therefor
-
- 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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0236—Cold rolling
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
Abstract
The invention discloses a strip silver-copper-titanium active solder, wherein the titanium content is 1-7wt%, and elemental titanium is dispersed and distributed in a silver-copper alloy matrix. The invention also discloses a preparation method of the banded silver-copper-titanium active solder, which comprises the following steps: the silver-copper alloy powder and the titanium powder are uniformly mixed, cold-pressed into a block blank, then the block blank is sintered, and then cold-rolled and thinned to obtain the banded silver-copper-titanium active solder, wherein the grain diameter ratio of the silver-copper alloy powder to the titanium powder is more than or equal to 3. According to the invention, pure titanium powder with small particle size and silver-copper alloy powder with large particle size are mixed by a powder metallurgy method, and proper sintering conditions are combined, so that the situation that a Ti element and a Cu element are smelted to generate a chemical reaction to generate a brittle intermetallic compound is effectively avoided, the active solder has good plastic deformation capacity, and the high-activity banded silver-copper-titanium solder with the titanium content of 1-7wt% can be prepared.
Description
Technical Field
The invention relates to the technical field of brazing filler metal, in particular to a strip-shaped silver-copper-titanium active brazing filler metal and a preparation method thereof.
Background
The ceramic material generally has the problems of poor plasticity and toughness, difficult processing and difficult manufacture of large and complex structures, so that the practical application of the ceramic material is greatly limited; the metal material has good obdurability, and the requirements of modern engineering can be met only by combining the ceramic material with the metal material.
There are many methods for connecting ceramics and metals, among which the brazing method has the advantages of reliable joint, good repeatability, high production efficiency, etc., and is the most common method for connecting ceramics and metals. The brazing method includes an indirect brazing method and a direct brazing method. The direct brazing method is to directly connect the ceramic and the metal by using the active brazing filler metal, has the advantages of wide applicability, simple technology, high connection strength, good repeatability, relatively low production cost and the like, and becomes the key point of the connection research and application of the ceramic and the metal. The banded silver copper titanium active solder comprises: the shape and the size are easy to match with the joint, the use is simple, the possibility of oxidizing the active element in advance is low, and the joint connection is more reliable, so that the method is commonly used for connecting ceramics and metals.
The silver-copper-titanium active solder is generally prepared by adding titanium element into silver-copper alloy liquid through a metallurgical smelting method. The higher the content of titanium element, the higher the activity of the brazing filler metal, but the more brittle intermetallic compounds formed by titanium and copper increase, and the workability of the brazing filler metal alloy is rapidly lowered. When the titanium content is 1-3wt%, the silver-copper-titanium active solder can be processed into a belt shape by a rolling and thinning method; when the titanium content is more than 3wt%, the silver-copper-titanium active solder becomes very brittle and can only be processed into powder by a powder preparation method.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the strip-shaped silver-copper-titanium active solder and the preparation method thereof, the pure titanium powder with small particle size and the silver-copper alloy powder with large particle size are mixed by a powder metallurgy method, and the appropriate sintering condition is combined, so that the situation that a Ti element and a Cu element are smelted to generate a chemical reaction to generate a brittle intermetallic compound is effectively avoided, the active solder has good plastic deformation capability, and the high-activity strip-shaped silver-copper-titanium solder with the titanium content of 1-7wt% can be prepared.
The invention provides a strip silver-copper-titanium active solder, the titanium content is 1-7wt%, and simple substance titanium is dispersed and distributed in a silver-copper alloy matrix.
Preferably, the titanium content is 3-7wt%.
The invention also provides a preparation method of the banded silver-copper-titanium active solder, which comprises the following steps: the silver-copper alloy powder and the titanium powder are uniformly mixed, cold-pressed into a block blank, then the block blank is sintered, and then cold-rolled and thinned to obtain the banded silver-copper-titanium active solder, wherein the grain diameter ratio of the silver-copper alloy powder to the titanium powder is more than or equal to 3.
According to the invention, spherical powder is selected, the particle size ratio of the silver-copper alloy powder to the titanium powder is not less than 3, a block blank is obtained through compression molding, the silver-copper alloy powder with larger particle size is closely arranged to form a close-packed structure, the titanium powder with smaller particle size is distributed at the gap of the close-packed structure of the silver-copper alloy powder, and during sintering, the close-packed structure of the silver-copper alloy powder forms a whole, so that the silver-copper alloy solder has good plastic deformation capability, and the titanium powder at the gap has less influence on the plastic deformation capability of the silver-copper alloy forming the whole, thereby being capable of being processed into the strip-shaped silver-copper titanium solder with high titanium content.
When the ratio of the particle diameters of the silver-copper alloy powder and the titanium powder is less than 3, for example, the particle diameter is 1.5, 2, 2.5, etc., the titanium powder with larger particle diameter cannot be completely distributed in the gap of the silver-copper alloy powder close-packed structure, and the titanium powder and the silver-copper alloy powder form the close-packed structure together, so that the plastic deformation capability of the close-packed structure can be reduced, and the preparation of the strip-shaped high-activity silver-copper-titanium solder with high titanium content becomes difficult.
According to the invention, pure titanium powder with small particle size and silver-copper alloy powder with large particle size are mixed by a powder metallurgy method, and proper sintering conditions are combined, so that the situation that a Ti element and a Cu element are smelted to generate a chemical reaction to generate a brittle intermetallic compound is effectively avoided, the active solder has good plastic deformation capability, the high-activity strip-shaped silver-copper-titanium solder with the titanium content of 1-7wt% can be prepared, and the titanium element in the strip-shaped silver-copper-titanium solder is dispersed in a silver-copper alloy matrix in the form of simple substance titanium.
The particle size of the silver-copper alloy powder is not limited, and may be 50 to 200 mesh (i.e., 75 to 300 μm).
Preferably, the sphericity of the silver-copper alloy powder and the sphericity of the titanium powder are both more than or equal to 0.8.
The method screens the proper sphericity of the silver-copper alloy powder and the titanium powder, and can further avoid the influence of the titanium powder on the plastic deformation capacity of the formed integral silver-copper alloy.
Preferably, the oxygen content of the silver-copper alloy powder is 200ppm or less.
Preferably, the oxygen content of the titanium powder is less than or equal to 600ppm.
The invention limits the oxygen content in the silver-copper alloy powder and the titanium powder within a proper range, and can avoid the problem that the titanium powder is easy to oxidize to reduce the activity of the solder.
The content of silver and copper in the silver-copper alloy powder is not specified, and the content is selected according to actual production, for example, the content of silver can be 50%, 60%, 72%, 85% and the like.
Preferably, the silver content of the silver-copper alloy powder is 72%.
Preferably, the sintering mode is vacuum hot-pressing sintering.
Preferably, the degree of vacuum of sintering is less than or equal to 1X 10 -2 Pa。
Preferably, the sintering temperature is 500-700 ℃.
Preferably, the sintering time is 0.5-3h.
Preferably, the pressure at sintering is 1-6MPa.
According to the invention, vacuum hot-pressing sintering is selected to sinter the block blank, proper vacuum hot-pressing sintering conditions are selected, the sintering temperature is reduced, solid-phase sintering is realized, chemical reaction of Ti element and Cu element is prevented, and the generation of brittle intermetallic compounds is reduced, so that the plastic deformation capacity of the silver-copper alloy powder close-packed structure is further improved; and the vacuum sintering can further avoid the oxidation problem of the titanium powder.
When the cold rolling is carried out for thinning, the banded silver-copper-titanium active solder is finally prepared by multiple times of cold rolling for thinning and multiple times of vacuum annealing treatment; cold reduction and vacuum annealing are processes conventional in the art.
Has the advantages that:
1. according to the invention, spherical powder is selected, the particle size ratio of the silver-copper alloy powder to the titanium powder is not less than 3, a block blank is obtained through compression molding, the silver-copper alloy powder with larger particle size is closely arranged to form a close-packed structure, the titanium powder with smaller particle size is distributed at the gap of the close-packed structure of the silver-copper alloy powder, and during sintering, the close-packed structure of the silver-copper alloy powder forms a whole, so that the silver-copper alloy solder has good plastic deformation capability, and the titanium powder at the gap has less influence on the plastic deformation capability of the silver-copper alloy forming the whole, thereby being capable of being processed into the strip-shaped silver-copper titanium solder with high titanium content.
2. According to the invention, vacuum hot-pressing sintering is selected to sinter the block blank, and proper vacuum hot-pressing sintering conditions are selected, so that the sintering temperature is reduced, solid-phase sintering is realized, the chemical reaction of Ti element and Cu element is prevented, and the generation of brittle intermetallic compounds is reduced, thereby further improving the plastic deformation capacity of the silver-copper alloy powder close-packed structure; and the vacuum sintering can further avoid the oxidation problem of the titanium powder.
3. The method screens proper silver-copper alloy powder particle size and the sphericity of the silver-copper alloy powder and the titanium powder, and can further avoid the influence of the titanium powder on the plastic deformation capacity of the formed integral silver-copper alloy; the invention limits the oxygen content in the silver-copper alloy powder and the titanium powder within a proper range, and can avoid the problem that the titanium powder is easy to oxidize to reduce the activity of the solder.
4. According to the invention, pure titanium powder with small particle size and silver-copper alloy powder with large particle size are mixed by a powder metallurgy method, and proper sintering conditions are combined, so that the situation that a Ti element and a Cu element are smelted to generate a chemical reaction to generate a brittle intermetallic compound is effectively avoided, the active solder has good plastic deformation capability, the high-activity strip-shaped silver-copper-titanium solder with the titanium content of 1-7wt% can be prepared, and the titanium element in the strip-shaped silver-copper-titanium solder is dispersed in a silver-copper alloy matrix in the form of simple substance titanium.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a strip silver copper titanium active solder comprises the following steps:
taking silver-copper alloy powder with 72wt% of silver and the balance of copper, wherein the particle size of the silver-copper alloy powder is 50-200 meshes (namely the particle size is 75-300 mu m), the sphericity is more than or equal to 0.8, and the oxygen content is less than or equal to 200ppm;
taking pure titanium powder with the grain diameter of-500 meshes (namely the grain diameter is less than or equal to 25 mu m), the sphericity is more than or equal to 0.8 and the oxygen content is less than or equal to 600 ppm;
uniformly mixing 96 parts of silver-copper alloy powder and 4 parts of pure titanium powder, putting into a die, and prepressing into a block blank with the size of 20 multiplied by 100 multiplied by 200mm under the pressure of 300 MPa;
then putting the block blank into a hot-pressing mould, and adjusting the vacuum degree to be less than or equal to 1 multiplied by 10 -2 Carrying out vacuum hot-pressing sintering for 1h at the temperature of 500 ℃ and the pressure of 4MPa under Pa, and cooling; then, a two-roller mill and a four-roller mill are used for carrying out multi-pass cold rolling reduction and vacuum annealing treatment to obtain a strip material with the thickness of 0.1mm, and finally, the strip material is cut to obtain the strip silver copper titanium active solder with the thickness of 0.1mm and the width of 80mm, wherein the weight percentage of the strip silver copper titanium active solder is as follows: 69% of Ag, 27% of Cu and 4% of Ti.
Example 2
A preparation method of a strip silver copper titanium active solder comprises the following steps:
taking silver-copper alloy powder with silver content of 60wt% and the balance copper, wherein the particle size of the silver-copper alloy powder is 30-50 meshes (namely the particle size is 300-550 mu m), the sphericity is more than or equal to 0.8, and the oxygen content is less than or equal to 200ppm;
taking pure titanium powder with the particle size of-1000 meshes (namely the particle size is less than or equal to 13 mu m), the sphericity is more than or equal to 0.8 and the oxygen content is less than or equal to 600 ppm;
uniformly mixing 99 parts of the silver-copper alloy powder and 1 part of pure titanium powder, putting the mixture into a die, and prepressing the mixture into a block blank with the size of 20 multiplied by 100 multiplied by 200mm under the pressure of 400 MPa;
then putting the block blank into a hot-pressing mould, and adjusting the vacuum degree to be less than or equal to 1 multiplied by 10 -2 Carrying out vacuum hot-pressing sintering for 0.5h at the temperature of 600 ℃ and the pressure of 6MPa, and cooling; then, a two-roll mill and a four-roll mill are used for carrying out multi-pass cold rolling reduction and vacuum annealing treatment to obtain a strip with the thickness of 0.1mm, and finally, the strip-shaped silver-copper-titanium active solder with the thickness of 0.1mm and the width of 80mm is obtained by cutting, wherein the weight percentage of the strip-shaped silver-copper-titanium active solder is as follows: 59.4% of Ag, 39.6% of Cu and 1% of Ti.
Example 3
A preparation method of a strip silver-copper-titanium active solder comprises the following steps:
taking silver-copper alloy powder with 50wt% of silver and the balance of copper, and sieving the silver-copper alloy powder with 50-200 meshes (the grain diameter is 75-300 mu m), wherein the sphericity is more than or equal to 0.8, and the oxygen content is less than or equal to 200ppm;
taking pure titanium powder with the particle size of-500 meshes (namely the particle size is less than or equal to 25 mu m), the sphericity is more than or equal to 0.8 and the oxygen content is less than or equal to 600 ppm;
mixing 93 parts of silver-copper alloy powder and 7 parts of pure titanium powder uniformly, putting into a die, and prepressing into a block blank with the size of 20 multiplied by 100 multiplied by 200mm under the pressure of 350 MPa;
then putting the block blank into a hot-pressing mould, and adjusting the vacuum degree to be less than or equal to 1 multiplied by 10 -2 Pa, the temperature is 700 ℃, the pressure is 2MPa, and the vacuum hot pressing sintering is carried out for 3h and the cooling is carried out; then, a two-roller mill and a four-roller mill are used for carrying out multi-pass cold rolling reduction and vacuum annealing treatment to obtain a strip material with the thickness of 0.1mm, and finally, the strip material is cut to obtain the strip silver copper titanium active solder with the thickness of 0.1mm and the width of 80mm, wherein the weight percentage of the strip silver copper titanium active solder is as follows: 46.5% of Ag, 46.5% of Cu and 7% of Ti.
Example 4
A preparation method of a strip silver copper titanium active solder comprises the following steps:
taking silver-copper alloy powder with the silver content of 85wt% and the balance copper, wherein the particle size of the silver-copper alloy powder is 50-200 meshes (namely the particle size is 75-300 mu m), the sphericity is more than or equal to 0.8, and the oxygen content is less than or equal to 200ppm;
taking pure titanium powder with the particle size of-500 meshes (namely the particle size is less than or equal to 25 mu m), the sphericity is more than or equal to 0.8 and the oxygen content is less than or equal to 600 ppm;
mixing 94.5 parts of silver-copper alloy powder and 5.5 parts of pure titanium powder uniformly, putting into a die, and prepressing into a block blank with the size of 20 multiplied by 100 multiplied by 200mm under the pressure of 350 MPa;
then putting the block blank into a hot-pressing mould, and adjusting the vacuum degree to be less than or equal to 1 multiplied by 10 -2 Carrying out vacuum hot-pressing sintering for 2h at the temperature of 600 ℃ and the pressure of 3MPa, and cooling; then, a two-roller mill and a four-roller mill are used for carrying out multi-pass cold rolling reduction and vacuum annealing treatment to obtain a strip material with the thickness of 0.1mm, and finally, the strip material is cut to obtain the strip silver copper titanium active solder with the thickness of 0.1mm and the width of 80mm, wherein the weight percentage of the strip silver copper titanium active solder is as follows: 80.3 percent of Ag, 14.2 percent of Cu and 5.5 percent of Ti.
The vacuum annealing treatment can remove stress and eliminate work hardening phenomenon.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The strip silver-copper-titanium active solder is characterized in that the titanium content is 1-7wt%, and elemental titanium is dispersed and distributed in a silver-copper alloy matrix;
the preparation method of the banded silver-copper-titanium active solder comprises the following steps: uniformly mixing silver-copper alloy powder and titanium powder, cold-pressing into a block blank, sintering the block blank, and then cold-rolling and thinning to obtain the banded silver-copper-titanium active solder, wherein the grain diameter ratio of the silver-copper alloy powder to the titanium powder is more than or equal to 3;
the sintering mode is vacuum hot-pressing sintering; the sintering temperature is 500-600 ℃; the pressure during sintering is 1-6MPa.
2. The silver-copper-titanium ribbon active solder according to claim 1, wherein the titanium content is 3 to 7wt%.
3. The banded silver-copper-titanium active solder according to claim 1 or 2, characterized in that the sphericity of the silver-copper alloy powder and the titanium powder is not less than 0.8.
4. The ribbon-shaped silver-copper-titanium active solder according to claim 1 or 2, wherein the oxygen content of the silver-copper alloy powder is 200ppm or less.
5. The ribbon-shaped silver-copper-titanium active solder according to claim 1 or 2, characterized in that the oxygen content of titanium powder is 600ppm or less.
6. The silver-copper-titanium ribbon active solder according to claim 1 or 2, wherein the degree of vacuum of sintering≤1×10 - 2 Pa。
7. The ribbon-shaped silver copper titanium active solder according to claim 1 or 2, characterized in that the sintering time is 0.5-3h.
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