CN113088748B - Preparation method of gold solder - Google Patents
Preparation method of gold solder Download PDFInfo
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- CN113088748B CN113088748B CN202110365307.1A CN202110365307A CN113088748B CN 113088748 B CN113088748 B CN 113088748B CN 202110365307 A CN202110365307 A CN 202110365307A CN 113088748 B CN113088748 B CN 113088748B
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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
- C22C5/02—Alloys based on gold
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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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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3013—Au as the principal constituent
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a preparation method of a gold solder, which comprises the following steps: (1) powder ball milling: ball-milling gold powder and tin powder together to obtain a gold-tin mixed material; ball-milling zinc powder and copper powder together to obtain a zinc-copper mixed material; (2) respectively tabletting the obtained mixed materials; (3) respectively smelting the obtained pressed sheets to obtain two alloys; (4) respectively weighing the gold-tin alloy and the zinc-copper alloy obtained in the step (3), putting the gold-tin alloy and the zinc-copper alloy into a non-consumable vacuum arc furnace, smelting under the protection of inert gas, and cooling to obtain gold solder; the solder raw material comprises the following components: gold, tin, zinc and copper. The gold ornament welding line prepared by the method has better mechanical property than the main body after being welded by the gold welding flux, excellent wettability and no color difference between the welding line and the gold ornament main body.
Description
Technical Field
The invention relates to the technical field of metal welding material preparation, in particular to a preparation method of a gold solder.
Background
Gold is one of the main ornaments materials in people's life at present, and is widely popular, in the manufacture or repair of gold ornaments, welding is one of the common techniques, welding, also called fusion, is a manufacturing process and a technique for joining metal or other thermoplastic materials such as plastics in a heating, high-temperature or high-pressure mode, and the essence of the gold ornaments is a technological process for connecting two or more kinds of materials of the same kind or different kinds into a whole through the combination and diffusion between atoms or molecules, and the method for promoting the combination and diffusion between the atoms and the molecules is heating or pressurizing, or heating and pressurizing simultaneously. Brazing means that a metal material with a melting point lower than that of a base metal is used as brazing filler metal, the liquid brazing filler metal is used for wetting the base metal, filling a joint gap, and mutually diffusing with the base metal to realize linking of a weldment, so that the brazing filler metal is suitable for welding processing of various materials, and is also suitable for welding processing of different metals or different materials. Is especially suitable for welding gold. During the welding process, the workpiece and the solder are melted to form a molten zone, and the molten pool is cooled and solidified to form the connection between the materials. In this process, pressure is also typically applied.
The joint formed during welding, which connects two joined bodies, is called a weld seam. When welding, the two sides of the weld joint are subjected to welding heat, and structural and performance changes occur, and the area is called a heat affected zone. In welding, weldability is deteriorated depending on the material of the workpiece, welding material, welding current, and the like. This results in the need to adjust the welding conditions, preheating at the interface of the weldment prior to welding, holding while welding and post-weld heat treatment to improve the weld quality of the weldment. The mutual position of the welded bodies in space is called as a welding joint, and the strength of the joint is influenced by the quality of the welding seam and is also related to the geometric shape, the size, the stress condition, the working condition and the like of the joint. The basic forms of the joint include butt joint, lap joint, T-joint (positive connection), angle joint and the like.
The traditional gold welding materials such as gold-tin alloy welding materials, gold-silver-nickel alloy welding materials and the like have low gold content of the welding materials, and excessive other metals are introduced, so that the gold content of the gold ornament is reduced, the color difference of the welding parts is often obvious, the welding strength is low, and the welding is easy to open.
Disclosure of Invention
In order to solve the problems of poor appearance of a weldment, poor joint performance of the weldment, poor adaptability to the shape of a butt joint and the like caused by the traditional gold solder, the invention provides a novel preparation method of the gold solder, and the scheme is as follows:
a preparation method of gold solder comprises the following steps:
(1) powder ball milling: respectively weighing gold powder, tin powder, zinc powder and copper powder according to raw material components of the solder; putting gold powder and tin powder into a ball milling tank for ball milling to obtain a gold-tin mixed material; putting the zinc powder and the copper powder into a ball milling tank for ball milling to obtain a zinc-copper mixed material;
(2) tabletting respectively: putting the obtained gold-tin mixture into a tabletting mold for tabletting to obtain a gold-tin tablet; putting the obtained zinc-copper mixed material into a tabletting mold for tabletting to obtain a zinc-copper tabletting;
(3) respectively smelting: placing the obtained gold-tin tablet into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain gold-tin alloy; putting the obtained zinc-copper tablets into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain zinc-copper alloy;
(4) preparing gold solder: respectively weighing the gold-tin alloy and the zinc-copper alloy obtained in the step (3) according to raw material components of the solder, putting the gold-tin alloy and the zinc-copper alloy into a non-consumable vacuum arc furnace, smelting under the protection of inert gas, and cooling to obtain gold solder;
the solder raw material comprises the following components: gold, tin, zinc and copper.
Preferably, the solder raw material components comprise the following components in parts by mass: 84-96 parts of gold, 4-9 parts of tin, 2-6 parts of zinc and 0.5-1 part of copper.
Preferably, the solder raw material components comprise the following components in parts by mass: 88 parts of gold, 9 parts of tin, 5 parts of zinc and 0.6 part of copper.
Preferably, the solder raw material components comprise the following components in parts by mass: 94 parts of gold, 6 parts of tin, 3 parts of zinc and 0.9 part of copper.
Preferably, the ball milling in the step (1) is carried out under the ball milling conditions of the gold-tin mixture including: the diameter of the stainless steel ball comprises 4mm and 8mm, the ratio of the two is 3: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing vacuum degree of the ball milling tank is 5-8Pa, the ball milling rotating speed is 150-.
Preferably, the ball milling in the step (1) and the ball milling conditions of the zinc-copper mixture comprise: the diameter of the stainless steel ball comprises 6mm and 8mm, the ratio of the two is 1: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing vacuum degree of the ball milling tank is 1-4Pa, the ball milling rotating speed is 200-250r/min, and the ball milling time is 60-90 min.
Preferably, in the tabletting of the step (2), the pressure is 6-9MPa and the pressure maintaining time is 5-7min in the gold-tin tabletting preparation process; in the preparation process of the zinc-copper tablet, the pressure is 10-13MPa, and the pressure maintaining time is 12-15 min.
Preferably, the smelting in the step (3) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10-3Pa, thenArgon is filled; the gold-tin alloy smelting conditions comprise: the smelting voltage is 220V, the smelting current is 5-15A, and the smelting time is 30-60 s; the smelting conditions of the zinc-copper alloy comprise the following steps: the smelting voltage is 220V, the smelting current is 30-45A, and the smelting time is 30-60 s.
Preferably, the smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10-3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: 1) starting first smelting, closing electric arc, and turning over after alloy in the smelting tank is solidified; 2) starting the second smelting, and closing the electric arc to obtain liquid alloy; 3) and rapidly cooling the liquid alloy to room temperature to obtain the gold solder.
Preferably, the smelting in the step (4), wherein in the step 1), the first smelting is carried out, the smelting voltage is 220V, the smelting current is 25-35A, and the smelting time is 30-60 s; step 2), performing secondary smelting, wherein the smelting voltage is 220V, the smelting current is 15-30A, and the smelting time is 30-60 s; and 3) rapidly cooling, wherein the cooling rate is 30-50 ℃/s, and the cooling time is 15-40 s.
Preferably, the smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10-3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: firstly, starting first smelting, closing electric arc, and turning over after alloy in a smelting tank is solidified; secondly, starting to smelt for the second time, and closing electric arcs to obtain liquid alloy; thirdly, rapidly cooling the liquid alloy, and rolling the cooled alloy to obtain the gold solder.
Preferably, the smelting in the step (4), wherein in the step (i), the smelting voltage is 220V, the smelting current is 25-35A, and the smelting time is 30-60s for the first smelting; secondly, smelting for the second time, wherein the smelting voltage is 220V, the smelting current is 15-30A, and the smelting time is 30-60 s; and step three, rapidly cooling at the cooling rate of 30-50 ℃/s until the alloy temperature reaches 200 ℃ and 220 ℃, and rolling to 0.15-1.00 mm.
Preferably, the gold has a purity of 99.99%, the tin has a purity of 99.9%, the zinc has a purity of 99.99%, and the copper has a purity of 99.9%.
The invention has the beneficial effects that:
1. the invention adopts the methods of mixing, ball milling and smelting a plurality of alloy raw materials respectively, overcomes the technical problems of independent condensation, difficult mutual melting and difficult formation of a dispersed reinforcing phase among materials caused by one-step mixing, ball milling and smelting of the plurality of raw materials in the traditional process, and enhances the physical and mechanical properties. The mechanical property of the welding line of the gold ornamental article after welding is superior to that of the main body.
2. When the alloy gold solder is used, tests show that the wetting angle of the liquid solder is 23.3-25.7 degrees, the surface tension is low, the alloy gold solder has excellent wetting performance, various complex and fine joint shapes can be directly and rapidly wetted, and the alloy gold solder is suitable for welding over-fine and complex gold parts.
3. The color of various k gold to pure gold can be adapted by adjusting the content of each component in the formula, and no color difference exists between a welding line and the gold ornament main body.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The following examples and comparative examples are parallel runs, with the same processing steps and parameters, unless otherwise indicated. In the following examples, the purity of gold was 99.99%, the purity of tin was 99.9%, the purity of zinc was 99.99%, and the purity of copper was 99.9%.
Example 1 a gold solder preparation:
(1) powder ball milling: respectively weighing gold powder, tin powder, zinc powder and copper powder according to raw material components of the solder; putting gold powder and tin powder into a ball milling tank for ball milling to obtain a gold-tin mixed material; putting the zinc powder and the copper powder into a ball milling tank for ball milling to obtain a zinc-copper mixed material;
(2) tabletting respectively: putting the obtained gold-tin mixture into a tabletting mold for tabletting to obtain a gold-tin tablet; putting the obtained zinc-copper mixed material into a tabletting mold for tabletting to obtain a zinc-copper tabletting;
(3) respectively smelting: placing the obtained gold-tin tablet into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain gold-tin alloy; putting the obtained zinc-copper tablets into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain zinc-copper alloy;
(4) preparing gold solder: respectively weighing the gold-tin alloy and the zinc-copper alloy obtained in the step (3) according to raw material components of the solder, putting the gold-tin alloy and the zinc-copper alloy into a non-consumable vacuum arc furnace, smelting under the protection of inert gas, and cooling to obtain gold solder;
the solder raw material comprises the following components: gold, tin, zinc and copper.
The solder comprises the following raw material components in parts by weight: 96 parts of gold, 9 parts of tin, 2 parts of zinc and 0.5 part of copper.
Ball milling is carried out on the gold-tin mixed material in the step (1), and the ball milling conditions comprise: the diameter of the stainless steel ball comprises 4mm and 8mm, the ratio of the two is 3: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing degree of a ball milling tank is 5-8Pa, the ball milling rotating speed is 150r/min, and the ball milling time is 30 min.
The ball milling in the step (1) is carried out, and the ball milling conditions of the zinc-copper mixed material comprise: the diameter of the stainless steel ball comprises 6mm and 8mm, and the proportion of the stainless steel ball to the stainless steel ball is 1: 1, introducing inert gas into a ball milling tank in an environment, wherein the vacuumizing vacuum degree of the ball milling tank is 1Pa, the ball milling rotating speed is 200r/min, and the ball milling time is 60 min.
Performing tabletting, namely performing gold-tin tabletting under the pressure of 6MPa for 5min in the preparation process of the gold-tin tabletting; in the preparation process of the zinc-copper tablet, the pressure is 10MPa, and the pressure maintaining time is 12 min.
The smelting in the step (3) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10- 3Pa, then filling argon; gold (gold)-the tin alloy melting conditions comprise: the smelting voltage is 220V, the smelting current is 5A, and the smelting time is 30 s; the smelting conditions of the zinc-copper alloy comprise the following steps: the smelting voltage is 220V, the smelting current is 30A, and the smelting time is 30 s.
The smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum electric arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10- 3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: 1) starting first smelting, closing electric arc, and turning over after alloy in the smelting tank is solidified; 2) starting the second smelting, and closing the electric arc to obtain liquid alloy; 3) and rapidly cooling the liquid alloy to room temperature to obtain the gold solder. Smelting in the step (4), wherein in the step 1), the first smelting is carried out, the smelting voltage is 220V, the smelting current is 25A, and the smelting time is 30 s; step 2), performing secondary smelting, wherein the smelting voltage is 220V, the smelting current is 15A, and the smelting time is 30 s; and 3) rapidly cooling at the cooling rate of 30-50 ℃/s.
Example 2 a gold solder preparation:
(1) powder ball milling: respectively weighing gold powder, tin powder, zinc powder and copper powder according to raw material components of the solder; putting gold powder and tin powder into a ball milling tank for ball milling to obtain a gold-tin mixed material; putting the zinc powder and the copper powder into a ball milling tank for ball milling to obtain a zinc-copper mixed material;
(2) tabletting respectively: putting the obtained gold-tin mixture into a tabletting mold for tabletting to obtain a gold-tin tablet; putting the obtained zinc-copper mixed material into a tabletting mold for tabletting to obtain a zinc-copper tabletting;
(3) respectively smelting: placing the obtained gold-tin tablet into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain gold-tin alloy; putting the obtained zinc-copper tablets into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain zinc-copper alloy;
(4) preparing gold solder: respectively weighing the gold-tin alloy and the zinc-copper alloy obtained in the step (3) according to raw material components of the solder, putting the gold-tin alloy and the zinc-copper alloy into a non-consumable vacuum arc furnace, smelting under the protection of inert gas, and cooling to obtain gold solder;
the solder raw material comprises the following components: gold, tin, zinc and copper.
The solder comprises the following raw material components in parts by weight: 88 parts of gold, 9 parts of tin, 5 parts of zinc and 0.6 part of copper.
Ball milling is carried out on the gold-tin mixed material in the step (1), and the ball milling conditions comprise: the diameter of the stainless steel ball comprises 4mm and 8mm, the ratio of the two is 3: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing vacuum degree of a ball milling tank is 8Pa, the ball milling rotating speed is 180r/min, and the ball milling time is 60 min.
The ball milling in the step (1) is carried out, and the ball milling conditions of the zinc-copper mixed material comprise: the diameter of the stainless steel ball comprises 6mm and 8mm, and the proportion of the stainless steel ball to the stainless steel ball is 1: 1, introducing inert gas into a ball milling tank in an environment, wherein the vacuumizing vacuum degree of the ball milling tank is 4Pa, the ball milling rotating speed is 250r/min, and the ball milling time is 90 min.
Performing tabletting, namely performing gold-tin tabletting under the pressure of 9MPa for 7min in the preparation process of the gold-tin tabletting; in the preparation process of the zinc-copper tablet, the pressure is 13MPa, and the pressure maintaining time is 15 min.
The smelting in the step (3) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10- 3Pa, then filling argon; the gold-tin alloy smelting conditions comprise: the smelting voltage is 220V, the smelting current is 15A, and the smelting time is 60 s; the smelting conditions of the zinc-copper alloy comprise the following steps: the smelting voltage is 220V, the smelting current is 45A, and the smelting time is 60 s.
The smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum electric arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10- 3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: firstly, starting first smelting, closing electric arc, and turning over after alloy in a smelting tank is solidified; secondly, starting to smelt for the second time, and closing electric arcs to obtain liquid alloy; thirdly, rapidly cooling the liquid alloy, and rolling the cooled alloy to obtain the gold solder. Smelting in the step (4), wherein in the step (I), the first smelting is carried out, the smelting voltage is 220V, the smelting current is 35A, and the smelting time is60 s; secondly, smelting for the second time, wherein the smelting voltage is 220V, the smelting current is 30A, and the smelting time is 60 s; and step three, rapidly cooling at the cooling rate of 30-50 ℃/s until the alloy temperature reaches 220 ℃, and rolling to 0.15-1.00 mm.
Example 3 a gold solder preparation:
(1) powder ball milling: respectively weighing gold powder, tin powder, zinc powder and copper powder according to raw material components of the solder; putting gold powder and tin powder into a ball milling tank for ball milling to obtain a gold-tin mixed material; putting the zinc powder and the copper powder into a ball milling tank for ball milling to obtain a zinc-copper mixed material;
(2) tabletting respectively: putting the obtained gold-tin mixture into a tabletting mold for tabletting to obtain a gold-tin tablet; putting the obtained zinc-copper mixed material into a tabletting mold for tabletting to obtain a zinc-copper tabletting;
(3) respectively smelting: placing the obtained gold-tin tablet into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain gold-tin alloy; putting the obtained zinc-copper tablets into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain zinc-copper alloy;
(4) preparing gold solder: respectively weighing the gold-tin alloy and the zinc-copper alloy obtained in the step (3) according to raw material components of the solder, putting the gold-tin alloy and the zinc-copper alloy into a non-consumable vacuum arc furnace, smelting under the protection of inert gas, and cooling to obtain gold solder;
the solder raw material comprises the following components: gold, tin, zinc and copper.
The solder comprises the following raw material components in parts by weight: 94 parts of gold, 6 parts of tin, 3 parts of zinc and 0.9 part of copper.
Ball milling is carried out on the gold-tin mixed material in the step (1), and the ball milling conditions comprise: the diameter of the stainless steel ball comprises 4mm and 8mm, and the proportion of the stainless steel ball to the stainless steel ball is 3: 1, introducing inert gas into a ball milling tank in an environment, wherein the vacuumizing vacuum degree of the ball milling tank is 7Pa, the ball milling rotating speed is 160r/min, and the ball milling time is 45 min.
The ball milling in the step (1) is carried out, and the ball milling conditions of the zinc-copper mixed material comprise: the diameter of the stainless steel ball comprises 6mm and 8mm, the ratio of the stainless steel ball to the stainless steel ball is 1: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing vacuum degree of a ball milling tank is 3Pa, the ball milling rotating speed is 250r/min, and the ball milling time is 70 min.
Performing tabletting, namely performing gold-tin tabletting under the pressure of 7MPa for 6min in the preparation process of the gold-tin tabletting; in the preparation process of the zinc-copper tablet, the pressure is 12MPa, and the pressure maintaining time is 14 min.
The smelting in the step (3) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10- 3Pa, then filling argon; the gold-tin alloy smelting conditions comprise: the smelting voltage is 220V, the smelting current is 10A, and the smelting time is 45 s; the smelting conditions of the zinc-copper alloy comprise the following steps: the smelting voltage is 220V, the smelting current is 35A, and the smelting time is 45 s.
The smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum electric arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10- 3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: firstly, starting first smelting, closing electric arc, and turning over after alloy in a smelting tank is solidified; secondly, starting to smelt for the second time, and closing electric arcs to obtain liquid alloy; thirdly, rapidly cooling the liquid alloy, and rolling the cooled alloy to obtain the gold solder. Smelting in the step (4), wherein in the step (i), the smelting voltage is 220V, the smelting current is 30A, and the smelting time is 45s for the first smelting; secondly, smelting for the second time, wherein the smelting voltage is 220V, the smelting current is 25A, and the smelting time is 45 s; and step three, rapidly cooling the alloy to the alloy temperature of 210 ℃ at the cooling rate of 30-50 ℃/s, and rolling the alloy to 0.15-1.00 mm.
Through detection, the melting points of the solders obtained in the above examples 1-3 are 905.5 +/-13.3 ℃, 885.1 +/-12.6 ℃ and 893.7 +/-11.0 ℃, which are all obviously lower than the melting point of gold, and the problems of welding interface physical property reduction and the like caused by gold melting in the welding process can be avoided. The solders of examples 1 to 3 are respectively used for welding a pure gold main body, and after the welding joint is polished and the like, zero color difference between the solder and the main body is realized. The wetting angles of the liquid solder of the solders obtained in the embodiments 1 to 3 on the surface of the foot gold are respectively 24.5 degrees, 23.3 degrees and 25.7 degrees (average values of three times are respectively taken), the solders have excellent wetting performance, and the liquid solder of the solders obtained in the embodiments 1 to 3 is adopted to respectively wet gold part joints such as butt joint, lap joint, T-shaped joint (positive cross joint), angle joint, irregular multi-concave joint and the like, so that the fast wetting is realized, and the liquid solder is suitable for welding of extremely fine and complicated gold parts.
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (9)
1. A preparation method of gold solder is characterized by comprising the following steps: the method comprises the following steps:
(1) powder ball milling: respectively weighing gold powder, tin powder, zinc powder and copper powder according to raw material components of the solder; putting gold powder and tin powder into a ball milling tank for ball milling to obtain a gold-tin mixed material; putting the zinc powder and the copper powder into a ball milling tank for ball milling to obtain a zinc-copper mixed material;
(2) tabletting respectively: putting the obtained gold-tin mixture into a tabletting mold for tabletting to obtain a gold-tin tablet; putting the obtained zinc-copper mixed material into a tabletting mold for tabletting to obtain a zinc-copper tabletting;
(3) respectively smelting: placing the obtained gold-tin tablet into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain gold-tin alloy; putting the obtained zinc-copper tablets into a crucible in a non-consumable vacuum arc furnace, and smelting under the protection of inert gas to obtain zinc-copper alloy;
(4) preparing gold solder: respectively weighing the gold-tin alloy and the zinc-copper alloy obtained in the step (3) according to raw material components of the solder, putting the gold-tin alloy and the zinc-copper alloy into a non-consumable vacuum arc furnace, smelting under the protection of inert gas, and cooling to obtain gold solder;
the solder raw material comprises the following components: gold, tin, zinc, copper; the solder comprises the following raw material components in parts by weight: 84-96 parts of gold, 4-9 parts of tin, 2-6 parts of zinc and 0.5-1 part of copper.
2. The method for preparing gold solder according to claim 1, characterized in that: ball milling is carried out on the gold-tin mixed material in the step (1), and the ball milling conditions comprise: the diameter of the stainless steel ball comprises 4mm and 8mm, the ratio of the two is 3: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing vacuum degree of the ball milling tank is 5-8Pa, the ball milling rotating speed is 150-.
3. The method for preparing gold solder according to claim 1, characterized in that: the ball milling in the step (1) is carried out, and the ball milling conditions of the zinc-copper mixed material comprise: the diameter of the stainless steel ball comprises 6mm and 8mm, the ratio of the two is 1: 1, the environment is inert gas, before the inert gas is introduced, the vacuumizing vacuum degree of the ball milling tank is 1-4Pa, the ball milling rotating speed is 200-250r/min, and the ball milling time is 60-90 min.
4. The method for preparing gold solder according to claim 1, characterized in that: performing tabletting in the step (2), wherein in the preparation process of the gold-tin tabletting, the pressure is 6-9MPa, and the pressure maintaining time is 5-7 min; in the preparation process of the zinc-copper tablet, the pressure is 10-13MPa, and the pressure maintaining time is 12-15 min.
5. The method for preparing gold solder according to claim 1, characterized in that: the smelting in the step (3) is carried out by firstly vacuumizing a non-consumable vacuum arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10-3Pa, then filling argon; the gold-tin alloy smelting conditions comprise: the smelting voltage is 220V, the smelting current is 5-15A, and the smelting time is 30-60 s; the smelting conditions of the zinc-copper alloy comprise the following steps: the smelting voltage is 220V, the smelting current is 30-45A, and the smelting time is 30-60 s.
6. The method for preparing gold solder according to claim 1, characterized in that: the smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum electric arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10-3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: 1) starting the first meltingClosing the electric arc, and turning over after the alloy in the smelting tank is solidified; 2) starting the second smelting, and closing the electric arc to obtain liquid alloy; 3) and rapidly cooling the liquid alloy to room temperature to obtain the gold solder.
7. The method for preparing gold solder according to claim 6, characterized in that: smelting in the step (4), wherein in the step 1), the first smelting is carried out, the smelting voltage is 220V, the smelting current is 25-35A, and the smelting time is 30-60 s; step 2), performing secondary smelting, wherein the smelting voltage is 220V, the smelting current is 15-30A, and the smelting time is 30-60 s; and 3) rapidly cooling, wherein the cooling rate is 30-50 ℃/s, and the cooling time is 15-40 s.
8. The method for preparing gold solder according to claim 1, characterized in that: the smelting in the step (4) is carried out by firstly vacuumizing a non-consumable vacuum electric arc furnace with the vacuum degree of 0.8 multiplied by 10-3-3×10-3Pa, then filling argon; the smelting of the step (4) further comprises the following steps: firstly, starting first smelting, closing electric arc, and turning over after alloy in a smelting tank is solidified; secondly, starting to smelt for the second time, and closing electric arcs to obtain liquid alloy; thirdly, rapidly cooling the liquid alloy, and rolling the cooled alloy to obtain the gold solder.
9. The method for preparing gold solder according to claim 8, wherein: smelting in the step (4), wherein in the step (i), the smelting voltage is 220V, the smelting current is 25-35A, and the smelting time is 30-60 s; secondly, smelting for the second time, wherein the smelting voltage is 220V, the smelting current is 15-30A, and the smelting time is 30-60 s; and step three, rapidly cooling at the cooling rate of 30-50 ℃/s until the alloy temperature reaches 200 ℃ and 220 ℃, and rolling to 0.15-1.00 mm.
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| JPS5698436A (en) * | 1979-12-11 | 1981-08-07 | Seiko Epson Corp | Gold solder |
| CN103100825A (en) * | 2013-01-07 | 2013-05-15 | 广州先艺电子科技有限公司 | Manufacturing method for pre-alloying gold-tin pre-forming soldering lug |
| CN103938013B (en) * | 2014-03-10 | 2016-01-20 | 中南大学 | A kind of preparation method of homogeneous microstructure Sn/Au eutectic alloy foil sheet |
| US10512988B2 (en) * | 2014-03-25 | 2019-12-24 | Sumitomo Metal Mining Co., Ltd. | Coated solder material and method for producing same |
| CN106498197B (en) * | 2016-10-18 | 2018-03-06 | 广西大学 | A kind of preparation method of Sn Cu Al series lead-free solders |
| CN106975737B (en) * | 2017-03-30 | 2018-10-09 | 中南大学 | A kind of efficient die casting preparation method of ultra-thin Sn/Au eutectic material |
| CN107177751B (en) * | 2017-04-25 | 2019-08-30 | 广西大学 | The good lead-free solder and preparation method thereof of a kind of corrosion-resistant and wetability |
| CN108374104A (en) * | 2018-03-09 | 2018-08-07 | 广西大学 | A kind of low melting point Sn-Bi-Al series lead-free solder alloy materials and preparation method thereof |
| CN109022842B (en) * | 2018-07-30 | 2020-01-03 | 中南大学 | Method for preparing superfine structure gold-tin eutectic alloy soldering lug through one-step vacuum suction casting |
| CN108941973A (en) * | 2018-08-15 | 2018-12-07 | 深圳市荟艺珠宝实业有限公司 | A kind of gold solder and its preparation method and application |
| CN112281017B (en) * | 2020-10-29 | 2022-03-11 | 中南大学 | Preparation method of Au-20Sn foil |
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