CN111014688A - Phosphorus-containing copper infiltration agent and preparation method thereof - Google Patents
Phosphorus-containing copper infiltration agent and preparation method thereof Download PDFInfo
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- CN111014688A CN111014688A CN201811177802.4A CN201811177802A CN111014688A CN 111014688 A CN111014688 A CN 111014688A CN 201811177802 A CN201811177802 A CN 201811177802A CN 111014688 A CN111014688 A CN 111014688A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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Abstract
The invention discloses a phosphorus-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: 1.8-2.7% of iron, 0.01-4.0% of phosphorus, 0.3-0.9% of carbon 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
Technical Field
The invention relates to the field of metallurgical materials, in particular to a phosphorus-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, the 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 are used as a defect to influence the properties of tensile strength, impact toughness, fatigue strength, hardness and the like of the parts, 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 efficiency of the prior art is about 85%, corrosion cracks are formed on the surface and the inner part of the part, the appearance and the impact strength of the product are affected, and the large-scale (25% -35%) defective products are caused. The defective products are usually removed by machining, which increases the processing cost.
Therefore, it is necessary to develop a copper infiltration agent capable of improving the product yield and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a phosphorus-containing copper infiltration agent, which comprises the following components in percentage by mass: 1.8-2.7% of iron, 0.01-4.0% of phosphorus, 0.3-0.9% of carbon 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 phosphorus and carbon raw materials are simple substances or compounds, and the particle size is smaller than 200 meshes.
The invention also aims to provide a preparation method of the phosphorus-containing copper 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 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. Phosphorus has the function of fluxing, and can improve the wettability of copper in iron and the permeability.
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
A phosphorus-containing copper infiltration agent comprises the following components in percentage by mass: 1.8 percent of iron, 0.01 percent of phosphorus, 0.3 percent of carbon and the balance of copper, wherein the iron material is reduced iron powder, the phosphorus material is phosphorus powder, the carbon material is carbon 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.
The particle size of the phosphorus powder is less than 300 meshes.
The granularity of the carbon powder is less than 300 meshes.
A method for preparing a phosphorus-containing copper infiltration agent comprises the following steps:
(1) weighing electrolytic copper powder: 97.89kg, reduced iron powder: 1.8kg, phosphorus powder: 0.01kg, carbon powder: 0.3kg, 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
A phosphorus-containing copper infiltration agent comprises the following components in percentage by mass: 2.7 percent of iron, 4.0 percent of phosphorus, 0.9 percent of carbon and the balance of copper, wherein the iron material is reduced iron powder, the phosphorus material is phosphorus powder, the carbon material is carbon 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.
The particle size of the phosphorus powder is less than 200 meshes.
The granularity of the carbon powder is less than 200 meshes.
A method for preparing a phosphorus-containing copper infiltration agent comprises the following steps:
(1) weighing electrolytic copper powder: 92.4kg, electrolytic iron powder: 2.7kg, ferrophosphorus powder: 4.0kg, carbon powder: 0.9kg, adding 5kg of zirconia ceramic balls according to the ball-material ratio of 1: 20, adding 0.15kg of ZnCl2 as a diffusion promoter, and mixing for 1.5h 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 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
A phosphorus-containing copper infiltration agent comprises the following components in percentage by mass: 2.3 percent of iron, 2 percent of phosphorus, 0.6 percent of carbon and the balance of copper, wherein the iron material is carbonyl iron powder, the phosphorus material is phosphorus powder, the carbon material is carbon powder and the copper 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.
The particle size of the phosphorus powder is less than 200 meshes.
The granularity of the carbon powder is less than 200 meshes.
A method for preparing a phosphorus-containing copper infiltration agent comprises the following steps:
(1) weighing atomized copper powder: 95.1kg, carbonyl iron powder: 2.3kg, phosphorus powder: 2kg, carbon powder: 0.6kg, 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 phosphorus-containing copper infiltration agent is characterized by comprising the following components in percentage by mass: 1.8-2.7% of iron, 0.01-4.0% of phosphorus, 0.3-0.9% of carbon and the balance of copper.
2. The phosphorus-containing copper infiltration agent according to claim 1, wherein the copper raw material comprises electrolytic copper powder, water atomized copper powder or gas atomized copper powder, the particle size is less than 100 meshes, and the loose packed density is 1.2-4.0 g/cm 3.
3. The phosphorus-containing copperizing agent as claimed in claim 1, wherein the iron 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 less than 150 meshes, and the particle size of the carbonyl iron powder is less than 700 meshes.
4. The phosphorus-containing copper infiltration agent according to claim 1, characterized in that the raw materials of phosphorus and carbon are simple substances or compounds, and the particle size is less than 300 meshes.
5. A process for the preparation of the phosphorus-containing bronze agent according to claim 1, characterized in that it 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.
6. The method according to claim 5, wherein the ceramic balls comprise alumina ceramic balls and zirconia ceramic balls.
7. The method as claimed in claim 5, wherein the diffusion promoter comprises one or more of NH4Cl, ZnCl2, NH4I and ZnI 2.
8. The method as claimed in claim 5, wherein the lubricant comprises zinc stearate, lithium stearate or micro wax powder.
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| CN201811177802.4A CN111014688A (en) | 2018-10-10 | 2018-10-10 | Phosphorus-containing copper infiltration agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111570819A (en) * | 2020-04-27 | 2020-08-25 | 江苏萌达新材料科技有限公司 | Preparation method of iron-copper-phosphorus alloy diffusion powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111570819A (en) * | 2020-04-27 | 2020-08-25 | 江苏萌达新材料科技有限公司 | Preparation method of iron-copper-phosphorus alloy diffusion powder |
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Application publication date: 20200417 |