CN111088446B - Copper-phosphorus brazing filler metal and preparation method thereof - Google Patents
Copper-phosphorus brazing filler metal and preparation method thereof Download PDFInfo
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- CN111088446B CN111088446B CN201911417250.4A CN201911417250A CN111088446B CN 111088446 B CN111088446 B CN 111088446B CN 201911417250 A CN201911417250 A CN 201911417250A CN 111088446 B CN111088446 B CN 111088446B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
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- 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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- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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Abstract
The invention relates to a copper-phosphorus brazing filler metal and a preparation method thereof, and provides a technical scheme for solving the problems that the copper-phosphorus brazing filler metal in the prior art is high in production cost, not safe enough and easy to generate pollution: the copper-phosphorus brazing filler metal comprises the following components in percentage by weight: 6.6 to 7.4 percent of P, and the balance of Cu; the preparation method of the copper-phosphorus brazing filler metal comprises the following steps: weighing raw materials; vertically placing an electrolytic copper plate at the bottom of the crucible; preparing a premix; vertically inserting an electrolytic copper bar into the premix; isolating the premix from air; preheating, degassing and drying; smelting; slag is fished; refining; and (5) casting. The copper-phosphorus brazing filler metal is reasonable in proportion, low in melting temperature and high in cost performance; the preparation process of the copper-phosphorus brazing filler metal does not need to manufacture a high-phosphorus copper-phosphorus intermediate alloy in advance, so that the production steps are simplified, the production cost is reduced, the loss of phosphorus elements is low, the reaction is safe and stable, and the energy is saved and the environment is protected.
Description
Technical Field
The invention relates to a brazing filler metal and a preparation method thereof, in particular to a copper-phosphorus brazing filler metal and a preparation method thereof.
Background
At present, copper-phosphorus solder is smelted to ensure the stability of components, phosphorus is added in the form of high-phosphorus copper-phosphorus intermediate alloy, the specific steps are firstly melting electrolytic copper, then adding the high-phosphorus copper-phosphorus intermediate alloy, and casting is carried out after the components are uniform and the temperature is proper. The production method needs to use electrolytic copper and yellow phosphorus to manufacture the high-phosphorus copper-phosphorus intermediate alloy in advance, so that the consumption of energy and materials is increased, time and labor are wasted, the production cost is high, and the high-phosphorus copper-phosphorus intermediate alloy reacts violently in the smelting process to generate a large amount of phosphorus pentoxide smoke, so that the environmental pollution is caused, and the method is not safe and environment-friendly.
For example, chinese patent publication No. CN110218894A, whose publication No. 20190910, discloses a method for producing a phosphor-copper brazing filler metal by one-step smelting, which adopts red clay to cover red phosphorus, and allows the red phosphorus to react with copper tubes inserted therein; although the cost is low, the laterite has poor air isolation capability, phosphorus pentoxide can be generated in the reaction, and the environment is polluted; the red phosphorus reacts with copper directly, so the reaction is severe and the safety is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the copper-phosphorus brazing filler metal and the preparation method thereof, wherein the copper-phosphorus brazing filler metal is reasonable in structural design, proper in proportioning, energy-saving, environment-friendly, low in cost and low in loss.
The technical scheme adopted by the invention for solving the problems is as follows: the copper-phosphorus brazing filler metal comprises the following components in percentage by weight: 6.6 to 7.4 percent of P, and the balance of Cu.
The preparation method of the copper-phosphorus brazing filler metal comprises the following steps:
s1, weighing raw materials including red phosphorus, copper-phosphorus solder wire particles, a plurality of electrolytic copper plates, a plurality of electrolytic copper rods and electrolytic copper solids according to the weight percentage of 6.6-7.4 percent of P and the balance of Cu; wherein the weight of the copper-phosphorus brazing filler metal wire particles is not more than half of the weight of the red phosphorus; selecting the size of the electrolytic copper plate suitable for the crucible;
s2: vertically placing electrolytic copper plates at the bottom of a crucible, placing a plurality of electrolytic copper plates in parallel, and enabling the distance between every two adjacent electrolytic copper plates to be larger than 30 mm;
s3, taking a proper amount of refractory material, mixing red phosphorus, copper phosphorus brazing filler metal wire particles and the refractory material into premix, placing the premix in a crucible, and paving;
s4, vertically inserting the electrolytic copper rod into the premix, taking a proper amount of refractory material, uniformly covering the premix with the refractory material, and tightly pressing to ensure that no gap exists between the refractory material and the inner wall of the crucible and the premix is isolated from air;
s5, adding a proper amount of electrolytic copper melt into the crucible, wherein the electrolytic copper melt is obtained by melting part of electrolytic copper solid in advance, adjusting the power of the crucible to 5kw, preheating for 3-5 minutes, degassing and drying, and the highest temperature in the crucible is not higher than 100 ℃;
s6, melting the residual electrolytic copper solid, slowly pouring the molten electrolytic copper into the crucible to enable the molten electrolytic copper to uniformly cover the refractory material, and then increasing the power of the crucible to 120kw to start melting;
s7, breaking the refractory material by using a graphite rod after the electrolytic copper rod and the electrolytic copper sheet in the crucible are completely melted and have no reaction noise;
s8, keeping the crucible power at 120kw for two minutes, then dragging slag, adjusting the crucible power to 10kw after dragging slag, and refining for 3 min;
and S9, standing the crucible for cooling after refining, and casting after the temperature is reduced to 990 ℃ to obtain the copper-phosphorus brazing filler metal cast ingot.
Preferably, the crucible in the invention is a crucible of an intermediate frequency furnace.
Preferably, the phosphorus content in the copper-phosphorus brazing filler metal wire particles is 6.8-7.2%.
Preferably, the diameter of the copper-phosphorus brazing filler wire particles in the invention is not more than 10 mm; the length of the copper-phosphorus brazing filler metal wire particles is not more than 5 mm.
Preferably, the electrolytic copper rod is a solid oxygen-free copper rod.
Preferably, the number of the electrolytic copper rods is 3-4.
Preferably, the number of the electrolytic copper plates in the present invention is 3.
Preferably, the refractory material in the present invention is plant ash.
Compared with the prior art, the invention has the following advantages and effects:
1. the copper-phosphorus brazing filler metal is reasonable in proportion, the proportion is the best proportion determined through multiple tests, the melting temperature is low, the wettability, the flowability and the plasticity are considered, noble metal materials such as silver are not added, the cost is low, and the cost performance is high.
2. The preparation process of the copper-phosphorus brazing filler metal does not need to manufacture a high-phosphorus copper-phosphorus intermediate alloy in advance, so that the production steps are simplified, the production cost is reduced, and the preparation method is energy-saving and environment-friendly.
3. The invention isolates red phosphorus from air by using refractory materials and molten electrolytic copper liquid, prevents the red phosphorus from violently reacting with oxygen at higher temperature to generate phosphorus pentoxide smoke, greatly reduces the loss of phosphorus elements and prevents the environment from being polluted.
4. The invention adopts a gradual smelting mode, the reaction is firstly carried out below the refractory material, after the solid oxygen-free copper rod is melted, the upper and lower layer spaces of the refractory material are communicated, and phosphorus is then reacted with the molten electrolytic copper liquid above the refractory material, so that the smelting process is designed to be safer and more stable.
5. The invention adopts a premixing mode to reduce the contact area of red phosphorus and copper and reduce the intensity of reaction.
Detailed Description
The present invention is further illustrated by the following examples, which are illustrative of the present invention and are not to be construed as being limited thereto.
Examples 1 to 9.
| Example number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| P content (%) | 6.6 | 6.7 | 6.8 | 6.9 | 7.0 | 7.1 | 7.2 | 7.3 | 7.4 |
| Cu content (%) | Balance of | Balance of | Balance of | Balance of | Balance of | Balance of | Balance of | Balance of | Balance of |
TABLE 1 quality percentage table of copper-phosphorus brazing filler metal in examples 1-9
The preparation method of the copper-phosphorus brazing filler metal in the embodiments 1 to 9 comprises the following steps:
s1, weighing raw materials according to the table 1, wherein the raw materials comprise red phosphorus, copper-phosphorus brazing filler metal wire particles, a plurality of electrolytic copper plates, a plurality of electrolytic copper rods and electrolytic copper solids; wherein the weight of the copper-phosphorus brazing filler metal wire particles is not more than half of the weight of the red phosphorus; selecting the size of the electrolytic copper plate suitable for the crucible;
s2: vertically placing electrolytic copper plates at the bottom of a crucible, placing a plurality of electrolytic copper plates in parallel, and enabling the distance between every two adjacent electrolytic copper plates to be larger than 30 mm;
s3, taking a proper amount of refractory material, mixing red phosphorus, copper phosphorus brazing filler metal wire particles and the refractory material into premix, placing the premix in a crucible, and paving;
s4, vertically inserting the electrolytic copper rod into the premix, taking a proper amount of refractory material, uniformly covering the premix with the refractory material, and tightly pressing to ensure that no gap exists between the refractory material and the inner wall of the crucible and the premix is isolated from air;
s5, adding a proper amount of electrolytic copper melt into the crucible, wherein the electrolytic copper melt is obtained by melting part of electrolytic copper solid in advance, adjusting the power of the crucible to 5kw, preheating for 3-5 minutes, degassing and drying, and the highest temperature in the crucible is not higher than 100 ℃;
s6, melting the residual electrolytic copper solid, slowly pouring the molten electrolytic copper into the crucible to enable the molten electrolytic copper to uniformly cover the refractory material, and then increasing the power of the crucible to 120kw to start melting;
s7, breaking the refractory material by using a graphite rod after the electrolytic copper rod and the electrolytic copper sheet in the crucible are completely melted and have no reaction noise;
s8, keeping the crucible power at 120kw for two minutes, then dragging slag, adjusting the crucible power to 10kw after dragging slag, and refining for 3 min;
and S9, standing the crucible for cooling after refining, and casting after the temperature is reduced to 990 ℃ to obtain the copper-phosphorus brazing filler metal cast ingot.
In the embodiment, the crucible is an intermediate frequency furnace crucible; the phosphorus content in the copper-phosphorus brazing filler metal wire particles is 6.8-7.2%; the diameter of the copper-phosphorus brazing filler metal wire particles is not more than 10 mm; the length of the copper-phosphorus brazing filler metal wire particles is not more than 5 mm; the copper-phosphorus brazing filler metal wire particles are not high-phosphorus alloy, can be prepared by the preparation method of the copper-phosphorus brazing filler metal in the embodiment 3-7 or can be purchased directly, and the amount is small, so that the cost is not influenced; the electrolytic copper rod is a solid oxygen-free copper rod; the number of the electrolytic copper rods is 3-4; the number of the electrolytic copper plates is 3; the refractory material is plant ash.
In the examples 1 to 9, a gradual smelting mode is adopted, the reaction is firstly carried out below the refractory material, red phosphorus and copper-phosphorus brazing filler wire particles are firstly melted and react in the temperature rising process to generate a part of intermediate, then the bottoms of the electrolytic copper sheet and the solid oxygen-free copper rod are melted and added into the reaction, and after the solid oxygen-free copper rod is melted to communicate the upper and lower layer spaces of the refractory material, the molten electrolytic copper liquid above the refractory material is added into the smelting reaction, so that the reaction is carried out step by step, the intensity of the reaction can be greatly reduced, and the reaction process is safer and more stable; moreover, the refractory material is doped in the premix, so that the contact area of red phosphorus and copper is reduced, and the intensity of the reaction can be reduced; meanwhile, the red phosphorus is isolated from the air by using a refractory material and molten electrolytic copper liquid, the isolation effect of the solid and liquid combination mode is better, the red phosphorus can be basically and completely isolated from the air, the red phosphorus is prevented from violently reacting with oxygen at a higher temperature to generate phosphorus pentoxide smoke, the loss of phosphorus elements is greatly reduced, the energy is saved, the environment is protected, and the environment pollution is prevented.
The copper-phosphorus solder in the embodiments 1 to 9 has low melting temperature, combines wettability, fluidity and plasticity, does not contain noble metal materials such as silver and the like, and has low cost and high cost performance.
In addition, it should be noted that the specific embodiments described in the present specification may be different in the components, the shapes of the components, the names of the components, and the like, and the above description is only an illustration of the structure of the present invention. Equivalent or simple changes in the structure, characteristics and principles of the invention are included in the protection scope of the patent. Various modifications, additions and substitutions for the specific embodiments described may be made by those skilled in the art without departing from the scope of the invention as defined in the accompanying claims.
Claims (1)
1. A preparation method of a copper-phosphorus brazing filler metal comprises the following components in percentage by weight: 6.6 to 7.4 percent of P and the balance of Cu, and is characterized by comprising the following steps:
s1, weighing raw materials according to the weight percentage, wherein the raw materials comprise red phosphorus, copper-phosphorus brazing filler metal wire particles, a plurality of electrolytic copper plates, a plurality of electrolytic copper rods and electrolytic copper solids; wherein the weight of the copper-phosphorus brazing filler metal wire particles is not more than half of the weight of the red phosphorus; selecting the size of the electrolytic copper plate suitable for the crucible;
s2: vertically placing electrolytic copper plates at the bottom of a crucible, placing a plurality of electrolytic copper plates in parallel, and enabling the distance between every two adjacent electrolytic copper plates to be larger than 30 mm;
s3, taking a proper amount of refractory material, mixing red phosphorus, copper phosphorus brazing filler metal wire particles and the refractory material into premix, placing the premix in a crucible, and paving;
s4, vertically inserting the electrolytic copper rod into the premix, taking a proper amount of refractory material, uniformly covering the premix with the refractory material, and tightly pressing to ensure that no gap exists between the refractory material and the inner wall of the crucible and the premix is isolated from air;
s5, adding a proper amount of electrolytic copper melt into the crucible, wherein the electrolytic copper melt is obtained by melting part of electrolytic copper solid in advance, adjusting the power of the crucible to 5kw, preheating for 3-5 minutes, degassing and drying, and the highest temperature in the crucible is not higher than 100 ℃;
s6, melting the residual electrolytic copper solid, slowly pouring the molten electrolytic copper into the crucible to enable the molten electrolytic copper to uniformly cover the refractory material, and then increasing the power of the crucible to 120kw to start melting;
s7, breaking the refractory material by using a graphite rod after the electrolytic copper rod and the electrolytic copper sheet in the crucible are completely melted and have no reaction noise;
s8, keeping the crucible power at 120kw for two minutes, then dragging slag, adjusting the crucible power to 10kw after dragging slag, and refining for 3 min;
s9, standing the crucible for cooling after refining, and casting after the temperature is reduced to 990 ℃ to obtain a copper-phosphorus brazing filler metal cast ingot;
the crucible is an intermediate frequency furnace crucible; the phosphorus content in the copper-phosphorus brazing filler metal wire particles is 6.8-7.2%; the diameter of the copper-phosphorus brazing filler metal wire particles is not more than 10 mm; the length of the copper-phosphorus brazing filler metal wire particles is not more than 5 mm; the electrolytic copper rod is a solid oxygen-free copper rod; the number of the electrolytic copper rods is 3-4; the number of the electrolytic copper plates is 3; the refractory material is plant ash.
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| CN201911417250.4A CN111088446B (en) | 2019-12-31 | 2019-12-31 | Copper-phosphorus brazing filler metal and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268567A (en) * | 2011-07-25 | 2011-12-07 | 浙江信和焊材制造有限公司 | Preparation method of copper-phosphorus alloy |
| CN104400260A (en) * | 2014-09-27 | 2015-03-11 | 宁波银马焊材科技有限公司 | Production process of extrusion ingot containing copper phosphorus brazing filler metal |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268567A (en) * | 2011-07-25 | 2011-12-07 | 浙江信和焊材制造有限公司 | Preparation method of copper-phosphorus alloy |
| CN104400260A (en) * | 2014-09-27 | 2015-03-11 | 宁波银马焊材科技有限公司 | Production process of extrusion ingot containing copper phosphorus brazing filler metal |
Non-Patent Citations (1)
| Title |
|---|
| 磷铜钎料的研究与应用;李宝绵等;《黄金学报》;19990630;第1卷(第2期);表1 * |
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