CN109706342B - Copper-zinc-silicon-based powdery brazing material containing alterant and preparation method thereof - Google Patents
Copper-zinc-silicon-based powdery brazing material containing alterant and preparation method thereof Download PDFInfo
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Abstract
The invention provides a copper-zinc-silicon-based powdery brazing material containing an alterant, which comprises 28-35 parts of zincwt% silicon 4-6wt1-3% of tinwt0.2-2% of alterantwt0.2-2% of nickelwtPercent, manganese 0.8-2wt% iron 0.5-2wtPercent, and the balance copper. The modifier can adopt metal indium or lanthanum cerium composite metal or a mixture of metal indium and lanthanum cerium composite metal. The preparation method comprises the following steps: (1) smelting copper and silicon into an intermediate alloy, and smelting copper and nickel into the intermediate alloy; (2) rolling iron into foil strips, and rolling and pressing alterant; (3) melting the rest of copper, copper-silicon intermediate alloy and copper-nickel intermediate alloy; (4) respectively adding zinc, tin, manganese and an iron belt with a modifier into a furnace in sequence, mixing and stirring; (5) the powder brazing material is prepared by gas atomization or water atomization. The invention can be used for the free-cutting and corrosion-resistant copper-based powder metallurgy products or alloy powder for improving the sharpness of diamond tools.
Description
Technical Field
The invention belongs to the field of powder metallurgy, and particularly relates to a copper-zinc-silicon-based powdery brazing material containing an alterant and a preparation method thereof.
Background
The powder metallurgy technology is an industrial technology for preparing metal materials, composite materials and various products by molding and sintering metal powder or alloy powder serving as a raw material, and is widely applied to the fields of traffic, machinery, electronics, aerospace, new energy, superhard tools and the like. The metal powder or alloy powder is used as a powder metallurgy raw material, is a base and a stone of a powder metallurgy industrial product, and qualified powder meeting the requirements can be prepared only by relating proper components and adopting a proper forming process.
The copper-based alloy powder has excellent obdurability and wear resistance, and is widely applied to research and preparation of high-strength high-conductivity copper-based composite materials and high-strength high-wear-resistance copper-based composite materials, particularly the copper-based powder metallurgy friction materials are developed most rapidly. Brass alloys of copper and zinc, with zinc contents generally lower than 46 for industrial usewt% and the alloy has good wear resistance and mechanical property, and simple brass has poor cutting property and poor corrosion resistance and is easy to generate dezincification corrosion in the processing process. The comprehensive performance of the alloy is improved by adding other elements into simple brass to form complex brass, silicon element is an important added element in the complex brass, the wear resistance and corrosion resistance of the brass can be improved, the fluidity of the copper-zinc-silicon alloy is only equivalent to that of gray cast iron and aluminum-silicon, the cutting performance is excellent, and the copper-zinc-silicon alloy is an excellent wear-resistant material. Meanwhile, a certain modifier is added into the copper-zinc-silicon alloy to refine crystal grains and improve the wear resistance and the stress corrosion resistance of the alloy.
The preparation process of the alloy powder generally adopts a crushing method, an atomization method and a chemical method, and the atomization method is widely applied to industrial production due to cleanness and high efficiency. The atomization method firstly melts the alloy into alloy high-temperature melt, and the high-temperature melt is atomized and crushed into powder particles by high-pressure gas or water. In the preparation and application processes of the copper-zinc-silicon alloy powder, the problems of unstable powder quality, component segregation and the like often occur, mainly due to poor component design and improper smelting atomization process.
Disclosure of Invention
In order to solve the problems, the invention provides the copper-zinc-silicon-based powdery brazing material containing the modifier and the preparation method thereof, which ensure that all elements are completely alloyed, and the prepared powder has stable and reliable performance and has the advantages of excellent machinability, wear resistance and stress corrosion resistance.
In order to achieve the purpose, the invention adopts the technical scheme that:
a copper-zinc-silicon-based powdery brazing material containing a modifier is characterized in that: copper-zinc-silicon based powdery brazing materialThe weight percentage comprises: 28 to 35wt% of zinc 4-6wt% of silicon, 1-3wt% of tin, 0.2-2wt% of modifying agent, 0.2-2wt% of nickel, 0.8-2wt% of manganese and 0.5-2wt% iron, balance copper, said modifier comprising a combination of indium metal and lanthanum cerium metal.
Further, the alterant comprises the following components in percentage by mass: 0.5 to 2wt% of lanthanum cerium composite metal.
Further, the alterant comprises the following components in percentage by mass: 0.2 to 1wt% of metallic indium and 0-1.5wt% of lanthanum cerium composite metal.
Further, the lanthanum-cerium composite metal comprises lanthanum and cerium.
Further, the alterant comprises the following components in percentage by mass: 0.2 to 2wt% metallic indium.
The invention also provides a preparation method of the copper-zinc-silicon-based powdery brazing material containing the alterant, which is characterized by comprising the following steps of: the method comprises the following specific steps:
step one, dividing copper into three parts, melting the first part of copper and all silicon, and smelting the molten copper and the silicon into a copper-silicon intermediate alloy; melting the second part of copper and all nickel, and smelting the copper and the nickel into a copper-nickel intermediate alloy;
rolling the iron into a foil, and rolling the alterant into the foil and compacting the foil;
step three, melting the copper of the third part and the copper-silicon intermediate alloy and the copper-nickel intermediate alloy obtained in the step one in a medium-frequency smelting furnace, and adding charcoal to cover in the melting process;
step four, respectively adding zinc, tin, manganese and an iron belt with a modifier into a smelting furnace in sequence according to the mass fraction, and mixing and stirring;
fifthly, heating until the added metal is completely melted and the alloy melt is sprayed;
and step six, casting the alloy melt obtained in the step five, and crushing and scattering the melt flow by an air atomization or water mist method to prepare the copper-zinc-silicon-based powdery brazing material containing the alterant.
Further, in the first step, the mass ratio of copper to silicon is 9: 1; the mass ratio of copper to nickel is 7: 3.
Further, in the second step, foil strips with the thickness of 0.1-0.5 mm and the width of 2-10 mm are rolled according to the adding amount of iron, and alterant is involved and compacted to prevent leakage.
Further, in the third step, the copper-silicon intermediate alloy and the copper-nickel intermediate alloy are completely melted, and the melt temperature is higher than 1100 ℃.
Further, in the fifth step, the heating temperature of the melt is 150-250 ℃ higher than the melting point of the alloy, and the melt is subjected to flaming.
The copper-zinc-silicon-based powdery brazing material containing the alterant is formed and sintered, the microstructure of a sintered body is alpha-phase complex brass, and vermicular and flower-like silver gray (beta' + gamma) phases are dispersed in a matrix. The alpha-phase brass has good plasticity and high strength; the beta 'phase is hard and brittle, and a small amount of beta' phase can increase the strength of a sintered body; the gamma phase is ordered body-centered cubic structure, electronic compound structure Cu5Zn8The structure is hard and brittle, the plasticity and the processability of the brass alloy are reduced, but intermittent grinding is easy to generate in the grinding process, and the cutting efficiency is increased by intermittent chip removal of the gamma phase in the complex brass.
When the content of zinc is lower than 28, the copper-zinc-silicon-based powder brazing material containing trace alterant of the inventionwt% of the total content of the gamma phase in the alloy is small, and the effect on the cutting performance of the alloy is small; when the zinc content exceeds 35wt% of the total amount of the (β' + γ) phase in the alloy increases, the alloy strength rapidly decreases, and the material reliability decreases.
In the copper-zinc-silicon-based powdery brazing material containing trace modifier, the modifier can refine alloy grains and promote the generation of primary dendrite, and the sintered body has fine structure grains and compact structure in the powder pressing and sintering process. The metal indium is an excellent alterant of the brass alloy, diffuses to the outside of primary dendrite in the form of solute in the alloy solidification process, prevents the primary dendrite from growing, forms composition supercooling at the bottom of the dendrite, generates necking to form free dendrite, further ensures the refinement of tissue crystal grains, and adds 0.2 trace metal indiumwt% can improve the comprehensive performance of the alloy. Since indium is a rare and noble metal, consideration is given toThe comprehensive factors of the performance and the price of the material are that the content of the metal indium is 0.2-2wt% of the total weight of the composition. The lanthanum-cerium composite metal is a modifier used in the copper alloy, a certain amount of lanthanum and cerium are added to generate adsorption and chemical reaction in an alloy crystal boundary, a certain amount of hard and brittle rare earth copper alloy compound is generated in the crystal boundary, the effect of refining the crystal grains is achieved for the alloy, when the lanthanum-cerium composite metal modifier is added excessively, a large amount of hard and brittle intermetallic compound is produced, the material performance is degraded, and the thermal stability of the material is influenced, wherein the content of the lanthanum-cerium composite metal modifier is 0.5-2wt% of the total weight of the composition. The invention comprehensively considers the problems of the price of metal indium and the poor heat stability of the modifier of lanthanum and cerium metals in the lanthanum-cerium composite metal, the modifier is a mixture of metal indium and the lanthanum-cerium composite metal, and the component is preferably 0.2-1wt% of metallic indium and 0-1.5wt% of a mixture of lanthanum cerium complex metals.
In the preparation method, the copper-silicon and copper-nickel intermediate alloy is firstly prepared, so that the proper smelting temperature, sufficient alloying of elements and accurate components are ensured in the smelting process. According to the addition of iron, the iron is rolled into a foil strip, and the alterant is rolled into the foil strip to be compacted, so that leakage is avoided. In the smelting process, the iron belt with the alterant is pressed into the melt, so that the low-melting-point metal indium and lanthanum cerium composite metal is prevented from floating and oxidizing, and the modification effect is ensured.
The invention has the beneficial effects that:
1. according to the copper-zinc-silicon-based powdery brazing material containing the alterant, the elements are completely alloyed through an alloy smelting process, the gas content of an alloy melt is low, the copper-zinc-silicon-based powdery brazing material is cleanly and efficiently prepared through an atomization method, the prepared powdery brazing material is accurate in component and stable and reliable in performance;
2. the preparation process of the powdery brazing material has strong controllability and is suitable for large-scale continuous production, the prepared copper-zinc-silicon-based powdery brazing material powder containing trace alterant has good process stability, and industrial products prepared by the powder metallurgy technology have excellent wear resistance, machinability and stress corrosion resistance;
3. the copper-zinc-silicon-based powdery brazing material containing the alterant has the advantages of low content of rare and precious metals in the raw materials, low manufacturing cost and reusable foundry returns;
4. the modifier has excellent performance, and provides a new direction for the research and development of the copper-zinc-silicon-based alloy modifier.
Drawings
FIG. 1 is a schematic view of a grinding and abrasion tester;
FIG. 2 is a graph comparing results of grinding tests;
FIG. 3 is a back-scattered electron image of the surface ground state of the sintered body of the powdered brazing material with Cu-Zn-Si base according to example 1;
FIG. 4 is a back-scattered electron image of the surface ground state of the sintered body of the powdered brazing material with Cu-Zn-Si base in example 2;
FIG. 5 is a back-scattered electron image of the surface ground state of the sintered body of the powdered brazing material with Cu-Zn-Si base according to example 3;
FIG. 6 is a photomicrograph of the alloy powder of example 1;
FIG. 7 is a photomicrograph of the alloy powder of example 2;
FIG. 8 is a photomicrograph of the alloy powder of example 3;
FIG. 9 is a photomicrograph of HSi80-3 alloy powder.
Wherein, each reference number in the figure is: 1. sand paper; 2. wearing the sample; 3. and (4) loading.
Detailed Description
FIG. 1 is a schematic diagram of a sintered body grinding and abrasion tester prepared from the copper-zinc-silicon-based powdery brazing material. The test method comprises the following steps: sandpaper 1 is mounted on the disc and an abrasive wear specimen 2 is pressed against the sandpaper 1 with a certain load 3. When the disc rotates according to the preset rotating speed, the tested sample radially moves linearly on the sand paper 1, and after the sample finishes the set friction stroke, the abrasion loss of the sample is measured. The wear resistance of the sample is shown by referring to a national standard 80-3 silicon brass pre-alloyed powder sintered sample.
The invention is further described and compared in terms of performance with reference to the following specific examples.
Firstly, the properties of the prepared copper-zinc-silicon-based powdery brazing material containing the alterant are described as follows:
example 1
The copper-zinc-silicon-based powdery brazing material containing trace alterant comprises the following chemical components: zinc 30wt% silicon 4wt% tin 1wt% indium 0.5wt% lanthanum cerium composite metal 1wt% nickel 0.2 wt% manganese 0.8 wt % iron 1 wtPercent, balance copper and inevitable impurity elements.
Taking 100 parts of copper-zinc-silicon-based powdery brazing material as an example, firstly, 9 parts of copper and 1 part of silicon are mixed and smelted into a copper-silicon intermediate alloy, and 7 parts of copper and 3 parts of nickel are mixed and smelted into a copper-nickel intermediate alloy; rolling the iron sheet into a foil strip with the thickness of 0.2mm and the width of 5mm, rolling 0.5 part of metal indium and 1 part of lanthanum-cerium composite metal into the foil strip and compacting. Then melting and smelting the residual copper, the copper-silicon intermediate alloy and the copper-nickel intermediate alloy in an intermediate frequency furnace, adding charcoal as a covering agent, and ensuring the furnace temperature to be more than 1100 ℃; sequentially adding 30 parts of zinc, 1 part of tin, 0.8 part of manganese and an iron belt with a modifier into a furnace for smelting and melting, heating to 1020-1150 ℃ after metals are completely melted and stirred, and enabling an alloy melt to have a flaming phenomenon; and pouring the alloy melt, crushing and scattering the melt flow by utilizing high-pressure gas atomization, collecting and screening to obtain the-200-mesh copper-zinc-silicon-based powdery brazing material.
Measuring the loose density of powder in a powder material comprehensive performance tester, analyzing the melting point of alloy powder by a relaxation-resistant analyzer, and measuring the oxygen content of the powder by nitrogen-hydrogen-oxygen combined measurement; the method comprises the steps of performing compression molding under 20MPa, performing compression sintering at 680-720 ℃ to obtain a wear sample, measuring the hardness of a sintered body through a Rockwell hardness tester, measuring the bending strength of the sintered body through a universal mechanical testing machine, and comparing the wear resistance of the sintered body through a grinding wear testing machine. Through the analysis and test means, the basic performance of the copper-zinc-silicon-based powdery brazing material is measured.
The basic properties of the copper-zinc-silicon-based powdery brazing material are as follows:
example 2
The chemical composition of the copper-zinc-silicon-based powdery brazing material containing trace alterant is designed as: zinc 28wt% silicon 5wt% tin 2wt% indium 0.8wt% lanthanum cerium composite metal 1wt% nickel 1wt% manganese 1wt% iron 1wtPercent, balance copper and inevitable impurity elements.
Taking 100 parts of silicon brass prealloying powder as an example, firstly, 9 parts of copper and 1 part of silicon are proportioned and smelted into a copper-silicon intermediate alloy, and 7 parts of copper and 3 parts of nickel are proportioned and smelted into a copper-nickel intermediate alloy; rolling the iron sheet into a foil strip with the thickness of 0.2mm and the width of 5mm, rolling 0.8 parts of metal indium and 1 part of lanthanum-cerium composite metal into the foil strip and compacting. Then melting and smelting the residual copper, the copper-silicon intermediate alloy and the copper-nickel intermediate alloy in an intermediate frequency furnace, adding charcoal as a covering agent, and ensuring the furnace temperature to be over 1200 ℃; adding 28 parts of zinc, 2 parts of tin, 1 part of manganese and an iron belt with a modifier into a furnace in sequence for smelting and melting, heating to 1000-1150 ℃ after metals are completely melted and stirred, and enabling an alloy melt to have a flaming phenomenon; and pouring the alloy melt, crushing and scattering the melt flow by utilizing high-pressure gas atomization, collecting and screening to obtain the-200-mesh copper-zinc-silicon-based powdery brazing material.
Measuring the loose density of powder in a powder material comprehensive performance tester, analyzing the melting point of alloy powder by a relaxation-resistant analyzer, and measuring the oxygen content of the powder by nitrogen-hydrogen-oxygen combined measurement; the method comprises the steps of performing compression molding under 20MPa, performing compression sintering at 680-720 ℃ to obtain a wear sample, measuring the hardness of a sintered body through a Rockwell hardness tester, measuring the bending strength of the sintered body through a universal mechanical testing machine, and comparing the wear resistance of the sintered body through a grinding wear testing machine. Through the analysis and test means, the basic performance of the copper-zinc-silicon-based powdery brazing material is measured.
The basic properties of the copper-zinc-silicon-based powdery brazing material are as follows:
example 3
The copper-zinc-silicon-based powdery brazing material containing trace alterant comprises the following chemical components: zinc 30wt% silicon 6wt% tin 1wt% indium 2wt0.5% of lanthanum-cerium composite metalwt% nickel 1wt% of manganese1wt% iron 1wtPercent, balance copper and inevitable impurity elements.
Taking 100 parts of silicon brass prealloying powder as an example, firstly, 9 parts of copper and 1 part of silicon are proportioned and smelted into a copper-silicon intermediate alloy, and 7 parts of copper and 3 parts of nickel are proportioned and smelted into a copper-nickel intermediate alloy; rolling the iron sheet into a foil strip with the thickness of 0.2mm and the width of 5mm, rolling 2 parts of metal indium and 0.5 part of lanthanum-cerium composite metal into the foil strip and compacting. Then melting and smelting the residual copper, the copper-silicon intermediate alloy and the copper-nickel intermediate alloy in an intermediate frequency furnace, adding charcoal as a covering agent, and ensuring the furnace temperature to be over 1200 ℃; sequentially adding 30 parts of zinc, 1 part of tin, 1 part of manganese and an iron belt with a modifier into a furnace for smelting and melting, heating to 1020-1160 ℃ after metals are completely melted and stirred, and enabling an alloy melt to have a flaming phenomenon; and pouring the alloy melt, crushing and scattering the melt flow by utilizing high-pressure gas atomization, collecting and screening to obtain the-200-mesh copper-zinc-silicon-based powdery brazing material.
Measuring the loose density of powder in a powder material comprehensive performance tester, analyzing the melting point of alloy powder by a relaxation-resistant analyzer, and measuring the oxygen content of the powder by nitrogen-hydrogen-oxygen combined measurement; the method comprises the steps of performing compression molding under 20MPa, performing compression sintering at 680-720 ℃ to obtain a wear sample, measuring the hardness of a sintered body through a Rockwell hardness tester, measuring the bending strength of the sintered body through a universal mechanical testing machine, and comparing the wear resistance of the sintered body through a grinding wear testing machine. Through the analysis and test means, the basic performance of the copper-zinc-silicon-based powdery brazing material is obtained.
The basic properties of the copper-zinc-silicon-based powdery brazing material are as follows:
comparing the grinding performance of the prepared copper-zinc-silicon-based powdery brazing material containing the alterant:
the components of the comparison sample accord with the chemical components of silicon brass HSi80-3, 200-mesh alloy powder is prepared through gas atomization, and the abrasion sample is formed through pressing and sintering at the temperature of 720-750 ℃ under the pressure of 20 MPa. The abrasion tests of the sintered silicon brass HSi80-3 blocks, examples 1, 2 and 3 blocks were conducted by the abrasion tester of FIG. 1, wherein the weight loss was faster when the blocks were weighed every 15 minutes, indicating that the blocks were less abrasion resistant, and the abrasion performance was comparable as shown in FIG. 2. According to the data in the figure, the abrasion resistance of the sintered body is as follows: example 2 is superior to example 3 to HSi80-3 than example 1.
Through a grinding wear test, the grinding state of the surface of the three-component sintering body is shown in fig. 3, 4 and 5, an intermittent chip removal groove is formed on the surface of the tire body, and the cutting performance of the tire body is improved.
Finally, the prepared copper-zinc-silicon-based powdery brazing material containing the alterant is subjected to a corrosion test:
preparing (50 +/-5) g/L sodium chloride solution according to a neutral salt spray test of GB/T10125-, after the salt spray corrosion test box is confirmed to normally operate, the alloy powder prepared in the embodiment is respectively placed in the salt spray corrosion box, the samples are contrastively analyzed under an optical microscope at intervals of 24 hours, the results of the microphotographs of the alloy powders of the three examples shown in FIGS. 6, 7 and 8 show that the copper-zinc-silicon based powdered brazing materials of examples 1, 2 and 3 have no discoloration, the microphotographs of the alloy powders of HSi80-3 shown in FIG. 9, the HSi80-3 alloy powder in the picture has slight color change, which shows that the corrosion resistance of the copper-zinc-silicon-based powdery brazing material containing trace alterant is superior to that of the common silicon brass alloy powder.
Claims (6)
1. A preparation method of copper-zinc-silicon-based powdery brazing material containing alterant is characterized by comprising the following steps: the copper-zinc-silicon-based powdery brazing material comprises the following components in percentage by mass: 28-35 wt% of zinc, 4-6 wt% of silicon, 1-3 wt% of tin, 0.2-2 wt% of modifier, 0.2-2 wt% of nickel, 0.8-2 wt% of manganese, 0.5-2 wt% of iron and the balance of copper, wherein the modifier is metal indium and lanthanum cerium composite metal;
the method comprises the following specific steps:
step one, dividing copper into three parts, melting the first part of copper and all silicon, and smelting the molten copper and the silicon into a copper-silicon intermediate alloy; melting the second part of copper and all nickel, and smelting the copper and the nickel into a copper-nickel intermediate alloy;
rolling the iron into a foil, and rolling the alterant into the foil and compacting the foil;
step three, melting the copper of the third part and the copper-silicon intermediate alloy and the copper-nickel intermediate alloy obtained in the step one in a medium-frequency smelting furnace, and adding charcoal to cover in the melting process;
step four, respectively adding zinc, tin, manganese and an iron belt with a modifier into a smelting furnace in sequence according to the mass fraction, and mixing and stirring;
fifthly, heating until the added metal is completely melted and the alloy melt is sprayed;
and step six, casting the alloy melt obtained in the step five, and crushing and scattering the melt flow by an air atomization or water mist method to prepare the copper-zinc-silicon-based powdery brazing material containing the alterant.
2. The method of claim 1 for preparing a powdered brazing material based on copper, zinc and silicon containing alterant, wherein the method comprises the following steps: the alterant comprises 0.2-1 wt% of metallic indium and 0.5-1.5 wt% of lanthanum-cerium composite metal by mass percent.
3. The method of claim 1 for preparing a powdered brazing material based on copper, zinc and silicon containing alterant, wherein the method comprises the following steps: in the first step, the mass ratio of copper to silicon is 9: 1; the mass ratio of copper to nickel is 7: 3.
4. The method of claim 1 for preparing a powdered brazing material based on copper, zinc and silicon containing alterant, wherein the method comprises the following steps: and in the second step, the foil strips with the thickness of 0.1-0.5 mm and the width of 2-10 mm are rolled according to the addition amount of iron, and the alterant is involved and compacted to prevent leakage.
5. The method of claim 1 for preparing a powdered brazing material based on copper, zinc and silicon containing alterant, wherein the method comprises the following steps: in the third step, the copper-silicon intermediate alloy and the copper-nickel intermediate alloy are completely melted, and the melt temperature is higher than 1100 ℃.
6. The method of claim 1 for preparing a powdered brazing material based on copper, zinc and silicon containing alterant, wherein the method comprises the following steps: in the fifth step, the heating temperature of the melt is 150-250 ℃ higher than the melting point of the alloy, and the melt is subjected to flaming.
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