CN101530952A - Boracic Cu-P-based amorphous brazing filler metal and method for preparing same - Google Patents
Boracic Cu-P-based amorphous brazing filler metal and method for preparing same Download PDFInfo
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- CN101530952A CN101530952A CN200910031190A CN200910031190A CN101530952A CN 101530952 A CN101530952 A CN 101530952A CN 200910031190 A CN200910031190 A CN 200910031190A CN 200910031190 A CN200910031190 A CN 200910031190A CN 101530952 A CN101530952 A CN 101530952A
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Abstract
The invention discloses a boracic Cu-P-based amorphous brazing filler metal and a method for preparing the same, which belong to the technical field of the brazing of amorphous brazing filler metal and copper as well as copper alloy. The amorphous brazing filler metal comprises the following components in percentage by weight: 7.2 percent of P, 14.0 percent of Ni, 5.4 percent of Sn, 0.02 to 0.04 percent of B, 0.2 percent of Si, and the balance of Cu. The amorphous brazing filler metal is prepared by adopting a rapid solidification technique, and the prepared brazing filler metal has a bright and clean surface, two smooth sides and better toughness. The melting temperature of the amorphous brazing filler metal is between 602 and 663 DEG C and the brazing temperature is between 670 and 720 DEG C. The amorphous brazing filler metal is applicable to the brazing of the copper and the copper alloy, and applicable brazing process methods comprise flame brazing, furnace brazing, gas shield brazing, salt bath brazing, and the like. By adopting the amorphous brazing filler metal to perform flame brazing of red copper, the wetting property of the brazing filler metal is obviously better than the brazing filler metal with same components prepared by a conventional melting technique, and the shear strength of a brazed joint is more than 112 MPa.
Description
Technical field
The present invention relates to a kind of boracic Cu-P based amorphous brazing filler metal and preparation method thereof, be specifically related to the boracic Cu-P-Sn-Ni-Si amorphous brazing filler metal and the preparation method of a kind of brazed copper and copper alloy, belong to amorphous brazing filler metal and copper and copper alloy soldering tech field.
Background technology
The fusing point of silver-base solder is moderate, good manufacturability, and have good intensity, toughness, electric conductivity, thermal conductivity and corrosion resistance, in each field of modern industry, obtain extensive use as electronics, household electrical appliances, space flight and aviation, the energy, automobile making etc.Along with the progress of development of science and technology and society, also growing to the demand of silver-base solder, the consumption that China only is used to make silver-base solder aspect silver every year reaches more than the kiloton.But silver is noble metal. belong to state's control goods and materials, China all needs a large amount of silver of import every year.In addition, most of silver-base solders all contain poisonous element cadmium.In order to reduce cost, avoid contaminated environment, exploitation joint silver, silver-substituted solder are the research forward position and the focus in domestic and international soldering field always, have bigger economic benefit and social benefit.
Cu-P base solder is with its low fusing point, good soldering processes performance, and distinctive self-fluxing effect (to the red copper soldering) and cheap advantages such as price are a kind of most promising generation Ag solders.But Cu-P base solder is owing to contain frangible compounds Cu
3P causes alloy at room temperature to be fragility, and strength of joint and toughness are more far short of what is expected than silver-base solder, the solder processing difficulties, and with the conventional method band that is difficult to laminate, this has just caused Cu-P base solder application limit.Adopt flash set technology to prepare the Cu-P based amorphous brazing filler metal, can solve solder and prepare moulding, and improve the performance of solder.Consider that from amorphous formation ability binary Cu-P system forms the poor ability of amorphous, the ternary system behind the adding Ni, amorphous formation ability strengthens greatly, and adds the quaternary system of Sn again, and amorphous formation ability is got back and is further strengthened.Consider that from the braze ability of Cu-P base solder phosphorus can obviously reduce the solder fusing point, improves liquidity, and red copper is had the self-fluxing ability.But with the increase of phosphorus content, the plasticity toughness of solder then reduces, at normal temperatures the processability variation; Add nickel in the solder, then improve fusing point, but can improve wetability, improve strength of joint and corrosion resistance Fe, Co, Ni base alloy.Add tin in the solder, can reduce fusing point, improve wetability.But the intensity of joint is reduced.
In order to obtain the Cu-P based amorphous brazing filler metal and to improve its braze ability, must be optimized design to Cu-P base alloying component, take into account the amorphous formation ability and the braze ability of alloy, on the basis of the above, add certain trace element again, further improve the performance of Cu-P based amorphous brazing filler metal, thereby make the Cu-P based amorphous brazing filler metal really enter the practicability stage, and the acquisition extensive use, this is preparation of Cu-P based amorphous brazing filler metal and copper and copper alloy soldering tech field technical problem anxious to be solved.
Summary of the invention
The objective of the invention is in order to solve the room temperature fragility and the formability problem of Cu-P base solder.Provide a kind of fusing point low, processing easily, the amorphous brazing filler metal that brazing property is good is to enlarge the application of this type of silver-substituted solder.It adopts flash set technology to produce amorphous filler metal by adding trace alloying element and optimizing Cu-P-Sn-Ni-Si base alloying component, is used for brazed copper and copper alloy, guarantees good brazing manufacturability and joint mechanical property.
To achieve these goals, technical scheme of the present invention is: a kind of boracic Cu-P-based amorphous brazing filler metal is characterized in that: the component of this solder and content (by mass percentage) are: P:7.2%; Ni:14.0%; Sn:5.4%; B:0.02～0.04%; Si:0.2%; All the other are Cu, and gross mass percentage is 100%.
The Ni of the above, the purity of Sn and Cu is more than 99.9%.
To achieve these goals, another technical scheme of the present invention is: a kind of preparation method of boracic Cu-P-based amorphous brazing filler metal is characterized in that comprising the steps:
(1) with P; Ni; Sn; B; Si; After the Cu raw material are pulverized respectively, weighing prescription on electronic balance, wherein the mass fraction of boron is 13.5% in the Cu-B alloy, and the mass fraction of silicon is 15% in the cupro silicon, and the mass fraction of phosphorus is 14.56% in the copper-phosphorus alloy;
(2) will place the WS-2 type high vacuum Ar atmosphere protection non-consumable arc furnace of Chinese Academy of Sciences's Beijing physical study manufacturing by the batching of above-mentioned prescription, electric arc furnaces has 5 copper crucibles, put a pure Ti sample in one of them crucible, all the other four crucibles can be put four kinds of batchings with prescription or different formulations simultaneously;
(3) before the melting, be evacuated to 10 earlier in the stove
-2Pa after applying argon gas prepurging 3-4 time, is evacuated to 10
-2Pa, applying argon gas is to-0.06MPa once more;
(4) before the formal melting, pure Ti sample of melt back is with residual oxygen in the further removal atmosphere;
(5) during the melting sample, even in order to make cast alloy, melt back 3-4 time under function composite by electromagnetic stirring of the sample in the water jacketed copper crucible, and use the stirring rod sample that overturns;
(6) behind the electric arc melting, sample is weighed, the weightlessness of finding sample can think that alloy actual constituent and nominal composition basically identical, the sample after the melting promptly are the foundry alloys of preparation amorphous brazing filler metal in 0.1%;
(7) with after the foundry alloy pulverizing, the single roller of the HVDS-II high vacuum that instrument technical development limited liability company system of section makes in the Shenyang of packing into gets rid of in the quartz glass tube of band machine, and the quartz ampoule nozzle is rectangle, and its length is a=6-8mm; Width b=0.5-1mm;
(8) quartz glass tube is installed in the induction heating circle that gets rid of the band machine, and its nozzle to copper roller surface spacing is adjusted to b
n=0.8-1mm is dull and stereotyped stream with the liquid that guarantees to be injected on the copper roller, and forms condition of steady flow;
(9) close fire door, adopt mechanical pump to be evacuated to 5.6 * 10
-1Pa, molecular pump pumping high vacuum to 7.5 * 10
-4Pa, cavity is full of high-purity Ar gas to-0.05MPa then;
(10) open motor, make copper roller rotating speed u
s=38-41m/s, copper roller diameter are 230mm, and copper roller width is 40mm;
(11) open high frequency electric source, to fully evenly fusion, it melts and sprays temperature T=1173-1273K with the foundry alloy high-frequency induction heating in the quartz glass tube, insulation superheated melt 0.5～1 minute;
(12) the Ar atmospheric pressure is transferred to p=50kPa, with the cooling copper roller surface of the superheated melt continuous injection in the quartz glass tube to the high speed rotation, liquid metal forms the paper tinsel band shape owing to be subjected to chilling, thereby obtains amorphous filler metal with the high pressure argon gas.
Adopting the amorphous foil tape thickness of above-mentioned steps and technology preparation is 0.08 ± 0.002mm, and any surface finish, and both sides are smooth, have toughness preferably.
The fusion temperature scope of this amorphous brazing filler metal is 602～663 ℃, 670～720 ℃ of brazing temperatures.This solder is applicable to the soldering of copper and copper alloy, and suitable process for soldering has gas brazing, furnace brazing, gas shiled soldering and salt bath brazing etc.Adopt this solder gas brazing red copper, solder wetting is significantly better than the congruent solder of conventional melting technique preparation, and shearing strength of joint is greater than 112MPa.
The advantage that a kind of boracic Cu-P-based amorphous brazing filler metal of the present invention and preparation method thereof has:
(1) adopts flash set technology to prepare Cu-P base paper tinsel band solder, solved conventional hot-working means and Cu-P base solder can't be processed into the difficulty of paper tinsel band;
(2) adopt the amorphous filler metal of emergency cooling process preparation to compare with congruent conventional solder: the solder fusion temperature is lower, and melting region is narrower, and wetability on red copper and shearing strength of joint all are higher than conventional solder, and be as shown in table 1 below;
(3) the micro-B that adds in the solder helps improving the amorphous formation ability of Cu-P-Sn-Ni-Si alloy, and micro-B then can play the surface-active effect in liquid solder, improve the wetability of liquid solder, micro-B then can crystal grain thinning in the brazed seam, improves tissue, improves the soldered fitting performance;
(4) intensity of amorphous filler metal soldered fitting is that far above the main cause of congruent conventional solder the fusion temperature of amorphous brazing filler metal is low, and melting region is narrow, and wetability is good, thereby helps obtaining high-quality brazed seam; This thermodynamics unstable state of amorphous state tissue helps quickening the diffusion of atom in the brazing process and the interaction of joint area mother metal and solder, so the diffusion depth of amorphous filler metal soldered fitting zone element and the uniformity coefficient of distribution are all greater than conventional solder, its brazed seam metallurgical quality is better than the brazed seam of conventional solder brazing; In addition, the more conventional solder much less of amorphous filler metal impurities and gas.
Table 1 Cu-7.2P-5.4Sn-14Ni-0.2Si-0.03B amorphous brazing filler metal and the contrast of conventional solder performance
| Solder | Fusion temperature (℃) | Spreading area (mm 2) | Shearing strength of joint (MPa) | Remarks |
| Conventional solder | 604-663 | 133 | 114 | Mother metal is a red copper |
| Amorphous brazing filler metal | 603-647 | 167 | 149 | Mother metal is a red copper |
The specific embodiment
Embodiment 1:
The component prescription: the component of solder and content are by mass percentage: P:7.2%; Ni:14.0%;
Sn:5.4%; B:0.03%; Si:0.2%; All the other are Cu.
The preparation method:
(1) with P; Ni; Sn; B; Si; After the Cu raw material are pulverized respectively, weighing prescription on electronic balance, wherein the mass fraction of boron is 13.5% in the Cu-B alloy, and the mass fraction of silicon is 15% in the cupro silicon, and the mass fraction of phosphorus is 14.56% in the copper-phosphorus alloy;
(2) will place the WS-2 type high vacuum Ar atmosphere protection non-consumable arc furnace of Chinese Academy of Sciences's Beijing physical study manufacturing by the batching of above-mentioned prescription, electric arc furnaces has 5 copper crucibles, put a pure Ti sample in one of them crucible, all the other four crucibles can be put four kinds of batchings with prescription or different formulations simultaneously;
(3) before the melting, be evacuated to 10 earlier in the stove
-2Pa after applying argon gas prepurging 3-4 time, is evacuated to 10
-2Pa, applying argon gas is to-0.06MPa once more;
(4) before the formal melting, pure Ti sample of melt back is with residual oxygen in the further removal atmosphere;
(5) during the melting sample, even in order to make cast alloy, melt back 3-4 time under function composite by electromagnetic stirring of the sample in the water jacketed copper crucible, and use the stirring rod sample that overturns;
(6) behind the electric arc melting, sample is carried out weighing, the weightlessness of finding sample can think that alloy actual constituent and nominal composition basically identical, the sample after the melting promptly are the foundry alloys of preparation amorphous brazing filler metal in 0.1%;
(7) with after the foundry alloy pulverizing, the single roller of the HVDS-II high vacuum that instrument technical development limited liability company system of section makes in the Shenyang of packing into gets rid of in the quartz glass tube of band machine, and the quartz ampoule nozzle is rectangle, and its length is a=6-8mm; Width b=0.5-1mm;
(8) quartz glass tube is installed in the induction heating circle that gets rid of the band machine, and its nozzle to copper roller surface spacing is adjusted to b
n=0.8-1mm is dull and stereotyped stream with the liquid that guarantees to be injected on the copper roller, and forms condition of steady flow;
(9) close fire door, adopt mechanical pump to be evacuated to 5.6 * 10
-1Pa, molecular pump pumping high vacuum to 7.5 * 10
-4Pa, cavity is full of high-purity Ar gas to-0.05MPa then;
(10) open motor, make copper roller rotating speed u
s=38-41m/s, copper roller diameter are 230mm, and copper roller width is 40mm;
(11) open high frequency electric source, to fully evenly fusion, it melts and sprays temperature T=1173-1273K with the foundry alloy high-frequency induction heating in the quartz glass tube, insulation superheated melt 0.5～1 minute;
(12) the Ar atmospheric pressure is transferred to p=50kPa, with the cooling copper roller surface of the superheated melt continuous injection in the quartz glass tube to the high speed rotation, liquid metal forms the paper tinsel band shape owing to be subjected to chilling, thereby obtains amorphous filler metal with the high pressure argon gas.
The fusion temperature scope of this solder is 603-647 ℃, and the shearing strength of joint of gas brazing red copper is 149MPa.
Embodiment 2:
The component prescription: the component of solder and content are by mass percentage: P:7.2%; Ni:14%; Sn:5.4%; B:0.02%; Si:0.2%; All the other are Cu.
Preparation method: identical with embodiment 1 preparation method.
The fusion temperature scope of this solder is 602～646 ℃, and the shearing strength of joint of gas brazing red copper is 112MPa.
Embodiment 3:
The component prescription: the component of solder and content are by mass percentage: P:7.2%; Ni:14%; Sn:5.4%; B:0.04%; Si:0.2%; All the other are Cu.
Make each method: identical with embodiment 1 preparation method.
The fusion temperature scope of this solder is 637～663 ℃, and the shearing strength of joint of gas brazing red copper is 121MPa.
Claims (3)
1, a kind of boracic Cu-P-based amorphous brazing filler metal is characterized in that: the component of this solder and content are by mass percentage: P:7.2%; Ni:14.0%; Sn:5.4%; B:0.02～0.04%; Si:0.2%; All the other are Cu, and gross mass percentage is 100%.
2, a kind of boracic Cu-P-based amorphous brazing filler metal according to claim 1 is characterized in that: described Ni, the purity of Sn and Cu is more than 99.9%.
3, a kind of method for preparing the described boracic Cu of claim 1-P based amorphous brazing filler metal is characterized in that following these steps to carrying out:
(1) with P; Ni; Sn; B; Si; After the Cu raw material are pulverized respectively, weighing prescription on electronic balance, wherein the mass fraction of boron is 13.5% in the Cu-B alloy, and the mass fraction of silicon is 15% in the cupro silicon, and the mass fraction of phosphorus is 14.56% in the copper-phosphorus alloy;
(2) will place the WS-2 type high vacuum Ar atmosphere protection non-consumable arc furnace of Chinese Academy of Sciences's Beijing physical study manufacturing by the batching of above-mentioned prescription, electric arc furnaces has 5 copper crucibles, put a pure Ti sample in one of them crucible, all the other four crucibles can be put four kinds of batchings with prescription or different formulations simultaneously;
(3) before the melting, be evacuated to 10 earlier in the stove
-2Pa after applying argon gas prepurging 3-4 time, is evacuated to 10
-2Pa, applying argon gas is to-0.06MPa once more;
(4) before the formal melting, pure Ti sample of melt back is with residual oxygen in the further removal atmosphere;
(5) during the melting sample, even in order to make cast alloy, melt back 3-4 time under function composite by electromagnetic stirring of the sample in the water jacketed copper crucible, and use the stirring rod sample that overturns;
(6) behind the electric arc melting, sample is weighed, the weightlessness of finding sample can think that alloy actual constituent and nominal composition basically identical, the sample after the melting promptly are the foundry alloys of preparation amorphous brazing filler metal in 0.1%;
(7) with after the foundry alloy pulverizing, the single roller of the HVDS-II high vacuum that instrument technical development limited liability company system of section makes in the Shenyang of packing into gets rid of in the quartz glass tube of band machine, and the quartz glass tube nozzle is rectangle, and its length is a=6-8mm; Width b=0.5-1mm;
(8) quartz glass tube is installed in the induction heating circle that gets rid of the band machine, and its nozzle to copper roller surface spacing is adjusted to b
n=0.8-1mm is dull and stereotyped stream with the liquid that guarantees to be injected on the copper roller, and forms condition of steady flow;
(9) close fire door, adopt mechanical pump to be evacuated to 5.6 * 10
-1Pa, molecular pump pumping high vacuum to 7.5 * 10
-4Pa, cavity is full of high-purity Ar gas to-0.05MPa then;
(10) open motor, make copper roller rotating speed u
s=38-41m/s, copper roller diameter are 230mm, and copper roller width is 40mm;
(11) open high frequency electric source, to fully evenly fusion, it melts and sprays temperature T=1173-1273K with the foundry alloy high-frequency induction heating in the quartz glass tube, insulation superheated melt 0.5～1 minute;
(12) the Ar atmospheric pressure is transferred to p=50kPa, with the cooling copper roller surface of the superheated melt continuous injection in the quartz glass tube to the high speed rotation, liquid metal forms the paper tinsel band shape owing to be subjected to chilling, thereby obtains amorphous filler metal with the high pressure argon gas.
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| CN101829860A (en) * | 2010-04-20 | 2010-09-15 | 哈尔滨工业大学 | Welding wire for unpreheated welding of red copper thick and large part and preparation method thereof |
| CN102744534A (en) * | 2012-07-27 | 2012-10-24 | 张国华 | Preparation method of silver-free solder and product |
| CN104384750A (en) * | 2014-11-17 | 2015-03-04 | 刘桂芹 | Lead-free copper-based amorphous brazing material |
| 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 |
| CN104439764A (en) * | 2014-11-17 | 2015-03-25 | 刘桂芹 | Manufacturing method for lead-free copper-based amorphous brazing filler metal strip |
| CN104439755A (en) * | 2014-11-17 | 2015-03-25 | 刘桂芹 | Manufacturing method for lead-free copper-based amorphous brazing filler metal |
| CN104551439A (en) * | 2014-11-17 | 2015-04-29 | 刘桂芹 | Lead-free copper-based amorphous solder strip |
| CN105479034A (en) * | 2014-10-09 | 2016-04-13 | 核工业西南物理研究院 | Copper-based brazing filler metal for tungsten/copper welding and preparing method of brazing filler metal |
| CN106041106A (en) * | 2016-07-21 | 2016-10-26 | 安徽旭晶粉体新材料科技有限公司 | Boron-containing copper alloy powder prepared with secondary water-mist method |
| CN108340096A (en) * | 2018-02-02 | 2018-07-31 | 杭州华光焊接新材料股份有限公司 | Amorphous brazing filler metal welding wire production method |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101829860A (en) * | 2010-04-20 | 2010-09-15 | 哈尔滨工业大学 | Welding wire for unpreheated welding of red copper thick and large part and preparation method thereof |
| CN102744534A (en) * | 2012-07-27 | 2012-10-24 | 张国华 | Preparation method of silver-free solder and product |
| CN104400260B (en) * | 2014-09-27 | 2017-08-04 | 宁波银马焊材科技有限公司 | The manufacture craft of extrusion ingot containing copper-phosphorus brazing 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 |
| CN105479034A (en) * | 2014-10-09 | 2016-04-13 | 核工业西南物理研究院 | Copper-based brazing filler metal for tungsten/copper welding and preparing method of brazing filler metal |
| CN105479034B (en) * | 2014-10-09 | 2019-02-01 | 核工业西南物理研究院 | A kind of tungsten/brazing connects with copper base solder and preparation method thereof |
| CN104439764A (en) * | 2014-11-17 | 2015-03-25 | 刘桂芹 | Manufacturing method for lead-free copper-based amorphous brazing filler metal strip |
| CN104439755A (en) * | 2014-11-17 | 2015-03-25 | 刘桂芹 | Manufacturing method for lead-free copper-based amorphous brazing filler metal |
| CN104551439A (en) * | 2014-11-17 | 2015-04-29 | 刘桂芹 | Lead-free copper-based amorphous solder strip |
| CN104384750A (en) * | 2014-11-17 | 2015-03-04 | 刘桂芹 | Lead-free copper-based amorphous brazing material |
| CN106041106A (en) * | 2016-07-21 | 2016-10-26 | 安徽旭晶粉体新材料科技有限公司 | Boron-containing copper alloy powder prepared with secondary water-mist method |
| CN108340096A (en) * | 2018-02-02 | 2018-07-31 | 杭州华光焊接新材料股份有限公司 | Amorphous brazing filler metal welding wire production method |
| CN108340096B (en) * | 2018-02-02 | 2020-08-04 | 杭州华光焊接新材料股份有限公司 | Amorphous solder wire manufacturing method |
| CN117680673A (en) * | 2023-12-22 | 2024-03-12 | 广东省科学院新材料研究所 | Copper-based amorphous powder for ultra-high-speed blue laser cladding and application thereof |
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