CN111014686A - Zinc-tin-containing copper infiltration agent and preparation method thereof - Google Patents

Zinc-tin-containing copper infiltration agent and preparation method thereof Download PDF

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Publication number
CN111014686A
CN111014686A CN201811176277.4A CN201811176277A CN111014686A CN 111014686 A CN111014686 A CN 111014686A CN 201811176277 A CN201811176277 A CN 201811176277A CN 111014686 A CN111014686 A CN 111014686A
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CN
China
Prior art keywords
zinc
tin
powder
copper
diffusion
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Pending
Application number
CN201811176277.4A
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Chinese (zh)
Inventor
邹勇平
吕廷镇
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Wuxi Hengteli Metal Products Co ltd
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Wuxi Hengteli Metal Products Co ltd
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Publication date
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Priority to CN201811176277.4A priority Critical patent/CN111014686A/en
Publication of CN111014686A publication Critical patent/CN111014686A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F3/26Impregnating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0425Copper-based alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • C22C9/04Alloys based on copper with zinc as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a zinc-tin-containing copper infiltration agent and a preparation method thereof, belonging to the technical field of powder metallurgy. The copper infiltration agent comprises the following components in percentage by mass: 1.0-3.5% of iron, 0.3-3.0% of manganese, 0.5-5.5% of zinc, 0.01-1.5% of tin and the balance of copper. The preparation method comprises the steps of weighing the raw materials according to the proportion, adding the ceramic balls or the stainless steel balls and the diffusion accelerant, mixing, feeding the powder into a hydrogen reduction furnace for diffusion at the diffusion temperature of 300-1000 ℃ for 0.5-25 h, cooling, discharging, crushing, screening and collecting, and then adding the lubricant for batching. The copper infiltration agent prepared by the invention has the characteristics of good formability, high infiltration efficiency, no corrosion, low residue and capability of obviously improving the density and mechanical property of the material. The method has simple process, and the required equipment is easy to operate and can be used for mass production.

Description

Zinc-tin-containing copper infiltration agent and preparation method thereof
Technical Field
The invention relates to the field of metallurgical materials, in particular to a zinc-tin-containing copper infiltration agent and a preparation method thereof.
Background
At present, sintered steel parts for powder metallurgy are increasingly widely applied in industrial production, particularly in the automobile machinery industry due to the characteristics of low cost and easy processing, and the parts are commonly used sintered steel gears, cams, valve seats, exhaust valve seats and the like, and when the parts are in service in certain severe environments, the parts are required to have good wear resistance and impact resistance, and also are required to maintain higher strength and hardness. However, powder metallurgy sintered steel parts manufactured by the conventional pressing-sintering process cannot reach a completely compact state in the pressing process, and the residual pores affect the properties of tensile strength, impact toughness, fatigue strength, hardness and the like of the parts as a defect, so that the parts cannot meet the use requirements. Therefore, eliminating or reducing the residual porosity is the most effective way to obtain high density, high performance sintered steel, and copper infiltration is a common method. Research shows that when copper or copper alloy powder is used for infiltration of sintered steel, the pores in the sintered steel can be obviously reduced or eliminated, the density is increased, and the mechanical property and the dynamic property (such as impact toughness and fatigue) are improved. Compared with the traditional densification process such as re-pressing and re-sintering, powder forging, warm pressing and the like, the copper infiltration method has the advantages of low cost, simple process, easy adjustment and the like, so that the method has increasingly expanded application range since the method is published in the United states in the fortieth century, and is an indispensable densification process for producing high-performance iron-based powder metallurgy parts at present.
The copper infiltration agent produced by the traditional process generally has the problems of corrosion of a matrix, surface residues, low copper infiltration rate and the like, so that the product percent of pass is low, and therefore, the components of the copper infiltration agent need to be optimized.
Disclosure of Invention
The invention aims to provide a zinc-tin-containing copper infiltration agent, which comprises the following components in percentage by mass: 1.0-3.5% of iron, 0.3-3.0% of manganese, 0.5-5.5% of zinc, 0.01-1.5% of tin and the balance of copper.
Preferably, the copper raw material comprises electrolytic copper powder, water atomized copper powder or gas atomized copper powder, the granularity is less than 100 meshes, and the apparent density is 1.2-4.0 g/cm 3.
Preferably, the iron raw material comprises electrolytic iron powder, reduced iron powder or carbonyl iron powder, wherein the particle size of the electrolytic iron powder and the particle size of the reduced iron powder are smaller than 150 meshes, and the particle size of the carbonyl iron powder is smaller than 700 meshes.
Preferably, the manganese, zinc and tin raw materials are simple substances, alloys or compounds, and the particle size is smaller than 200 meshes.
Another object of the present invention is to provide a method for preparing a zinciferous tin bronze infiltration agent, which comprises the following steps:
(1) weighing the raw materials according to the proportion, adding ceramic balls or stainless steel balls according to the ball material mass ratio of 1: 5-20, adding a diffusion promoter accounting for 0.1-1% of the total mass of the raw materials according to the weight percentage, and mixing for 0.5-2 hours in a mixer;
(2) after the material mixing process is finished, feeding the powder into a hydrogen reduction furnace for diffusion, wherein the diffusion temperature is 300-1000 ℃, and the diffusion time is 0.5-25 h;
(3) cooling, discharging, crushing, screening and collecting, and then adding a lubricant accounting for 0-1.5% of the total mass of the raw materials according to weight percentage for batching.
Preferably, the ceramic balls comprise alumina ceramic balls and zirconia ceramic balls.
Preferably, the diffusion promoter comprises one or more of NH4Cl, ZnCl2, NH4I and ZnI 2.
Preferably, the lubricant comprises zinc stearate, lithium stearate or microwax.
The invention has the beneficial effects that: the copper infiltration agent has reasonable components, high infiltration rate, no erosion and residue on the surface of the product after infiltration, uniform appearance and greatly improved density and mechanical property of the product.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
The zinc-tin-containing copper infiltration agent comprises the following components in percentage by mass: 1.0 percent of iron, 0.3 percent of manganese, 0.5 percent of zinc, 0.01 percent of tin and the balance of copper, wherein the iron raw material is reduced iron powder, and the copper raw material is electrolytic copper powder.
The granularity of the electrolytic copper powder is less than 100 meshes, and the apparent density is 2.0g/cm 3.
The particle size of the reduced iron powder is less than 150 meshes.
A method for preparing a zinc-tin-containing copper infiltration agent comprises the following steps:
(1) weighing electrolytic copper powder: 98.19kg, reduced iron powder: 1kg, manganese powder: 0.3kg, zinc powder: 0.5kg, tin powder: 0.01kg, adding 5kg of alumina ceramic balls according to the ball-material ratio of 1: 20, adding 0.2kg of NH4Cl as a diffusion promoter, and mixing for 1 hour in a mixer;
(2) after the material mixing process is finished, feeding the powder into a hydrogen reduction furnace for diffusion, wherein the diffusion temperature is 800 ℃, and the diffusion time is 90 min;
(3) cooling with circulating water, crushing, sieving with 100 mesh sieve, collecting, adding 0.5kg zinc stearate, and mixing to obtain the final product.
Example 2
The zinc-tin-containing copper infiltration agent comprises the following components in percentage by mass: 3.5 percent of iron, 3.0 percent of manganese, 5.5 percent of zinc, 1.5 percent of tin and the balance of copper, wherein the iron material is reduced iron powder, and the copper material is electrolytic copper powder.
The granularity of the electrolytic copper powder is less than 100 meshes, and the apparent density is 2.0g/cm 3.
The particle size of the reduced iron powder is less than 150 meshes.
A method for preparing a zinc-tin-containing copper infiltration agent comprises the following steps:
(1) weighing electrolytic copper powder: 86.5kg, electrolytic iron powder: 3.5kg, manganese powder: 3kg, zinc powder: 5.5kg of zirconium oxide ceramic balls and 1.5kg of tin powder are added according to the ball-material ratio of 1: 20, 0.15kg of ZnCl2 is added as a diffusion promoter, and the mixture is mixed in a mixer for 1.5 hours;
(2) after the material mixing process is finished, feeding the powder into a hydrogen reduction furnace for diffusion, wherein the diffusion temperature is 600 ℃, and the diffusion time is 120 min;
(3) cooling by circulating water, discharging and crushing, screening and collecting by a 100-mesh sieve, and then adding 0.4kg of lithium stearate for mixing to prepare the copper-infiltrated agent.
Example 3
The zinc-tin-containing copper infiltration agent comprises the following components in percentage by mass: 2.3 percent of iron, 2.5 percent of manganese, 3 percent of zinc, 0.8 percent of tin and the balance of copper, wherein the iron raw material is carbonyl iron powder, and the copper raw material is atomized copper powder.
The granularity of the atomized copper powder is less than 100 meshes, and the apparent density is 2.0g/cm 3.
The granularity of the carbonyl iron powder is less than 700 meshes.
A method for preparing a zinc-tin-containing copper infiltration agent comprises the following steps:
(1) weighing atomized copper powder: 91.4kg, carbonyl iron powder: 2.3kg, ferromanganese powder: 2.5kg, zinc powder: 3kg of tin powder and 0.8kg of tin powder, adding 5kg of stainless steel balls and 0.25kg of NH4I as a diffusion promoter according to the ball-material ratio of 1: 20, and mixing for 2 hours in a mixer;
(2) after the material mixing process is finished, feeding the powder into a hydrogen reduction furnace for diffusion, wherein the diffusion temperature is 850 ℃, and the diffusion time is 100 min;
(3) cooling with circulating water, crushing after discharging, collecting by 100-mesh sieve, adding 0.3kg of micro wax powder, and batching to prepare the copper-infiltrated agent.
While the preferred embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the invention is not limited thereto, and that various changes and modifications may be made without departing from the spirit of the invention, and the scope of the appended claims is to be accorded the full range of equivalents.

Claims (8)

1. The zinc-tin-containing copper infiltration agent is characterized by comprising the following components in percentage by mass: 1.0-3.5% of iron, 0.3-3.0% of manganese, 0.5-5.5% of zinc, 0.01-1.5% of tin and the balance of copper.
2. The zinc-tin-containing copper infiltration agent according to claim 1, characterized in that the copper raw material comprises electrolytic copper powder, water atomized copper powder or gas atomized copper powder, the granularity is less than 100 meshes, and the loose packed density is 1.2-4.0 g/cm 3.
3. The agent of claim 1, wherein the iron source material comprises electrolytic iron powder, reduced iron powder or carbonyl iron powder, wherein the particle size of the electrolytic iron powder and the reduced iron powder is less than 150 mesh, and the particle size of the carbonyl iron powder is less than 700 mesh.
4. The zinc-tin-containing copper infiltration agent according to claim 1, characterized in that the manganese, zinc and tin raw materials are simple substances, alloys or compounds, and the particle size is less than 200 meshes.
5. A method for producing the copper-infiltrated agent containing zinc tin according to claim 1, comprising the steps of:
(1) weighing the raw materials according to the proportion, adding ceramic balls or stainless steel balls according to the ball material mass ratio of 1: 5-20, adding a diffusion promoter accounting for 0.1-1% of the total mass of the raw materials according to the weight percentage, and mixing for 0.5-2 hours in a mixer;
(2) after the material mixing process is finished, feeding the powder into a hydrogen reduction furnace for diffusion, wherein the diffusion temperature is 300-1000 ℃, and the diffusion time is 0.5-25 h;
(3) cooling, discharging, crushing, screening and collecting, and then adding a lubricant accounting for 0-1.5% of the total mass of the raw materials according to weight percentage for batching.
6. The method for preparing the zinc-tin-containing copperizing agent according to claim 5, wherein the ceramic balls comprise alumina ceramic balls and zirconia ceramic balls.
7. The method for preparing the zinc-tin-containing copperizing agent according to claim 5, wherein the diffusion promoter comprises one or more of NH4Cl, ZnCl2, NH4I and ZnI 2.
8. The method of claim 5, wherein the lubricant comprises zinc stearate, lithium stearate or micro wax powder.
CN201811176277.4A 2018-10-10 2018-10-10 Zinc-tin-containing copper infiltration agent and preparation method thereof Pending CN111014686A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811176277.4A CN111014686A (en) 2018-10-10 2018-10-10 Zinc-tin-containing copper infiltration agent and preparation method thereof

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Application Number Priority Date Filing Date Title
CN201811176277.4A CN111014686A (en) 2018-10-10 2018-10-10 Zinc-tin-containing copper infiltration agent and preparation method thereof

Publications (1)

Publication Number Publication Date
CN111014686A true CN111014686A (en) 2020-04-17

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Application publication date: 20200417