CN108500276B - Method for producing a part from a metal oxide - Google Patents
Method for producing a part from a metal oxide Download PDFInfo
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- CN108500276B CN108500276B CN201810442118.8A CN201810442118A CN108500276B CN 108500276 B CN108500276 B CN 108500276B CN 201810442118 A CN201810442118 A CN 201810442118A CN 108500276 B CN108500276 B CN 108500276B
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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
- B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
Abstract
The invention discloses a method for manufacturing a part by using metal oxide, which comprises the following steps: mixing and grinding iron oxide powder and graphite powder or iron oxide powder, alloy element oxide powder and graphite powder to obtain a raw material mixture; the raw material mixture is formed through mould or 3D printing to obtain a product green body; and (3) reducing and sintering the product green body in a sintering furnace with reducing or protective atmosphere to obtain a finished product. The invention directly manufactures the parts by grinding, forming, reducing and sintering the mixture of the metal oxide powder and the graphite powder, simplifies the production process of powder metallurgy and reduces the production cost.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a method for manufacturing a part by using metal oxide.
Background
Powder metallurgy is a process technique for producing metal powder or metal powder (or a mixture of metal powder and nonmetal powder) as a raw material, and then forming and sintering the raw material to produce metal materials, composite materials and various products.
In the existing powder metallurgy technology, the manufacturing process of stainless steel and other iron-based alloy powder is long, generally, iron oxide is reduced by coke in a blast furnace to obtain pig iron with high carbon content, then alloy elements are added after decarburization in the steel making process to obtain an ingot with required chemical components, and finally the ingot is melted again and then the powder is obtained by a water atomization or gas atomization method. The price of metal powder is much higher relative to the bulk metal material used for casting and forging, which makes the price of powder metallurgy generally higher than that of cast and forged parts, at a disadvantage in price competition.
Disclosure of Invention
The invention mainly aims to provide a method for manufacturing parts by using metal oxides, which aims to simplify the existing production process of powder metallurgy so as to reduce the production cost and improve the production efficiency.
In order to achieve the above object, the present invention provides a method for manufacturing a part from a metal oxide, comprising the steps of:
mixing and grinding iron oxide powder and graphite powder or iron oxide powder, alloy element oxide powder and graphite powder to obtain a raw material mixture;
the raw material mixture is formed through mould or 3D printing to obtain a product green body;
and (3) reducing and sintering the product green body in a sintering furnace with reducing or protective atmosphere to obtain a finished product.
Preferably, the step of mixing and grinding iron oxide powder and graphite powder, or iron oxide powder, alloying element oxide powder and graphite powder to obtain a raw material mixture comprises:
according to the mass percentage, 95-98% of iron oxide powder and 16-22% of graphite powder, or 70-93% of iron oxide powder, 7-30% of alloy element oxide powder and 16-22% of graphite powder are mixed and ball-milled in a ball mill for 4-12 hours to obtain a raw material mixture.
Preferably, the alloying element oxide powder comprises chromium oxide powder and nickel oxide powder; mixing and grinding iron oxide powder and graphite powder or iron oxide powder, alloy element oxide powder and graphite powder to obtain a raw material mixture, wherein the raw material mixture comprises:
ball-milling 95-98% of iron oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain a carbon steel raw material mixture;
ball-milling 90-93% of iron oxide powder, 7-8% of nickel oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain an alloy steel raw material mixture;
ball-milling 85-90% of iron oxide powder, 10-16% of chromium oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain a martensitic stainless steel raw material mixture;
and ball-milling 70-78% of iron oxide powder, 16-20% of chromium oxide powder, 7-8% of nickel oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain an austenitic stainless steel raw material mixture.
Preferably, the step of forming the raw material mixture by a mold or 3D printing to obtain a green product comprises:
pressing and forming the martensitic stainless steel raw material mixture or the austenitic stainless steel raw material mixture in a die cavity to obtain a product green body;
the step of reducing and sintering the product green body in a sintering furnace with reducing or protective atmosphere to obtain a finished product comprises the following steps:
heating to 1000 ℃ at the speed of 10 ℃/min in a tube furnace under the protection of argon, and preserving heat for 1-3 hours to carry out reduction;
heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours to sinter;
after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
Preferably, the step of forming the raw material mixture by a mold or 3D printing to obtain a green product comprises:
pressing and forming the carbon steel raw material mixture or the alloy steel raw material mixture in a die cavity to obtain a product green body;
the step of reducing and sintering the product green body in a sintering furnace with reducing or protective atmosphere to obtain a finished product comprises the following steps:
heating to 1000 ℃ at the speed of 10 ℃/min in a tube furnace under the protection of argon, and preserving heat for 1-3 hours to carry out reduction;
heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours to sinter;
after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
Preferably, the above method further comprises the steps of:
mixing the raw material mixture with a binder according to the volume fraction of 1:1, and heating and stirring;
extruding on a double-screw extruder and uniformly cutting into granular feed.
Preferably, the step of forming the raw material mixture by a mold or 3D printing to obtain a green product comprises:
and (3) putting the granular feed into an injection molding machine or a 3D printer, and preparing a product green body by an injection molding or 3D printing process.
Preferably, the step of reducing and sintering the green product in a sintering furnace under a reducing or protective atmosphere to obtain a finished product comprises:
heating to 600 ℃ at the speed of 1 ℃/min, and keeping the temperature for 1 hour;
then heating to 1000 ℃ at the speed of 10 ℃/min, and preserving heat for 1-3 hours;
finally, heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours;
after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
Preferably, before the step of reducing and sintering the product green body in a sintering furnace under a reducing or protective atmosphere to obtain a finished product, the method further comprises:
and immersing the product green body into n-hexane, and heating and extracting for a time to obtain a degreased product green body for reduction and sintering.
The method for manufacturing the part by the metal oxide reduces the metal oxide in the sintering process, and directly sinters the green compact of the metal oxide into a compact part with a complex shape and good mechanical properties. The invention directly manufactures stainless steel and other iron-based alloy parts by metal oxides, omits the processes of iron making, steel making, spraying and the like in the manufacture of stainless steel and other iron-based alloy powder, simplifies the production process of powder metallurgy and reduces the production cost.
Drawings
FIG. 1 is a flow chart of a method for fabricating a part from a metal oxide in accordance with an embodiment of the present invention;
fig. 2 is a drawing of a part manufactured by the method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to solve the above technical problem, the present invention provides a method for manufacturing a part from a metal oxide, as shown in fig. 1, the method comprising the steps of:
step S10, mixing and grinding iron oxide powder and graphite powder or iron oxide powder, alloy element oxide powder and graphite powder to obtain a raw material mixture; it should be understood that the raw material mixture in the embodiment of the present invention includes auxiliary materials such as a forming agent (paraffin, stearic acid, etc.) in addition to the iron oxide powder and the graphite powder and/or the alloying element oxide powder. In the present invention, first, iron oxide powder, oxide powder of alloying elements (e.g., chromium oxide, nickel oxide, copper oxide, molybdenum oxide, etc.), graphite powder, and a forming agent are mixed in a certain ratio, and then, the mixture is ground in a ball mill to be uniformly mixed, thereby obtaining a raw material mixture.
Step S20, the raw material mixture is printed and formed through a mould or 3D to obtain a product green body; the resulting raw mixture is then pressed in a mold or shaped by other powder metallurgy methods (e.g., injection molding, 3D printing, etc.) to yield a green product having a particular shape.
And step S30, the product green body is placed in a sintering furnace with reducing or protective atmosphere for reduction and sintering to obtain a finished product. After obtaining the product green compact, the product green compact is placed in a sintering furnace in a reducing or protective atmosphere (hydrogen, argon or nitrogen) to be heated, iron oxide and other metal oxides react with graphite at the temperature of more than 600 ℃, and the iron oxide and other metal oxides are reduced into single metal oxideMass metals with CO, CO2Gas escapes from the sample. After the reduction reaction is finished, the blank containing the mixture of the iron and other alloy metal elements is heated to a higher temperature for sintering, the iron and other alloy metal elements can be diffused and converted into a uniform alloy with stainless steel or other iron-based alloy components, and meanwhile, the blank can be greatly shrunk, so that the density of the material is close to the theoretical density of the material. Cooling the blank along with the furnace to manufacture high-density stainless steel or other iron-based alloy parts with corresponding grades.
In a preferred embodiment, the step of mixing and grinding the iron oxide powder or the graphite powder of the oxide powder of the alloying element to obtain the raw material mixture comprises:
according to the mass percentage, 95-98% of iron oxide powder and 16-22% of graphite powder, or 70-93% of iron oxide powder, 7-30% of alloy element oxide powder and 16-22% of graphite powder are mixed and ball-milled in a ball mill for 4-12 hours to obtain a raw material mixture. The method provided by the invention is suitable for manufacturing high-density stainless steel or other iron-based alloy parts. In a preferred embodiment of the present invention, the alloying element oxide powder comprises chromium oxide powder and/or nickel oxide powder. The proportion can be reasonably selected according to the variety of materials and the product performance requirements, for example, about 74 percent of iron oxide powder, about 8 percent of nickel oxide powder and/or about 18 percent of chromium oxide powder and about 18 percent of graphite powder are mixed and ball-milled to obtain a raw material mixture. Alternatively, about 97% iron oxide powder and about 18% graphite powder may be mixed and ball-milled to obtain a raw material mixture. The time of ball milling can be selected according to the forming process of the green product in order to obtain a mixture on the order of tens or hundreds of nanometers. For example, assuming a pressing process, 8 to 12 hours, preferably 10 hours of ball milling, are selected; if the molding is injection molding or 3D printing process molding, 4 to 6 hours can be selected, and the ball milling is preferably performed for 5 hours because a granulation process is carried out subsequently.
In one embodiment, 95-98% of iron oxide powder and 16-22% of graphite powder are selected to be ball-milled in a ball mill for 8-12 hours to obtain a carbon steel raw material mixture. Specifically, about 97% of iron oxide powder and about 18% of graphite powder can be ball-milled in a ball mill for about 10 hours to obtain a carbon steel raw material mixture. The invention ball-mills 8 to 12 hours in a planetary ball mill, and can lead the powder granularity to reach hundreds of nanometers or even dozens of nanometers.
In another embodiment, 90-93% of iron oxide powder, 7-8% of nickel oxide powder and 16-22% of graphite powder can be selected to be ball-milled in a ball mill for 8-12 hours to obtain an alloy steel raw material mixture. Specifically, about 92% of iron oxide powder, about 7% of nickel oxide powder and about 18% of graphite powder can be ball-milled in a ball mill for about 10 hours to obtain an alloy steel raw material mixture of hundreds of nanometers or even tens of nanometers.
In another embodiment, 85-90% of iron oxide powder, 10-16% of chromium oxide powder and 16-22% of graphite powder are subjected to ball milling in a ball mill for 8-12 hours to obtain a martensitic stainless steel raw material mixture. Specifically, about 87% of iron oxide powder, about 13% of chromium oxide and about 18% of graphite powder can be subjected to ball milling in a ball mill for about 10 hours to obtain a martensitic stainless steel raw material mixture of hundreds of nanometers or even tens of nanometers.
In another embodiment, 70-78% of iron oxide powder, 16-20% of chromium oxide powder, 7-8% of nickel oxide powder and 16-22% of graphite powder are subjected to ball milling in a ball mill for 8-12 hours to obtain an austenitic stainless steel raw material mixture. Specifically, about 74% of iron oxide powder, about 18% of chromium oxide powder, about 7% of nickel oxide powder and about 18% of graphite powder can be ball-milled in a ball mill for about 10 hours to obtain a raw material mixture of several hundred or even several tens of nanometers of austenitic stainless steel.
In the embodiment of the invention, the austenitic stainless steel raw material mixture or the martensitic stainless steel raw material mixture can be pressed and formed in a die cavity to obtain a product green compact; and then placing the product green body in a sintering furnace with reducing or protective atmosphere for reducing and sintering to obtain a finished product. Specifically, after a product green body is obtained, the temperature can be raised to 1000 ℃ at the speed of 10 ℃/min in a tube furnace under the protection of argon, and the temperature is kept for 1-3 hours for reduction; heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours to sinter; after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
For the iron-based part, a carbon steel raw material mixture or an alloy steel raw material mixture can be pressed and formed in a die cavity to obtain a product green body; the green product is then reduced and sintered at a relatively low temperature in a sintering furnace in a reducing or protective atmosphere, as follows: heating to 1000 ℃ at the speed of 10 ℃/min in a tube furnace under the protection of argon, and preserving heat for 1-3 hours; finally, heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours to sinter; after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
The method can also form the product green body through injection molding and 3D printing, and in a preferred embodiment of the invention, the process for forming the product green body through injection molding and 3D printing further comprises the following steps: mixing the raw material mixture with a binder according to the volume fraction of 1:1, and heating and stirring; extruding the mixture on a double-screw extruder and uniformly cutting the mixture into granular feed; and (3) putting the granular feed into an injection molding machine or a 3D printer, and preparing a product green body by an injection molding or 3D printing process.
In the embodiment of the present invention, when the raw material mixture includes chromium oxide powder and nickel oxide powder, the reduction temperature may be slightly lower than that of the pressing process, for example, the temperature is raised to 600 ℃ at a rate of 1 ℃/min, and the temperature is maintained for 1 hour; then heating to 1000 ℃ at the speed of 10 ℃/min, and preserving heat for 1-3 hours; finally, heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours; after sintering, cooling to 800 ℃ at the speed of 5 ℃/min, and then cooling along with the furnace to obtain a finished product. In the embodiment of the present invention, before performing the step of placing the product green compact in a sintering furnace of a reducing or protective atmosphere for reducing and sintering to obtain a finished product, the method further includes: and immersing the product green body into n-hexane, and heating and extracting for a time to obtain a degreased product green body for reduction and sintering. Specifically, the product green body can be uniformly placed on a stainless steel screen mesh, immersed in n-hexane, heated to 50 ℃, and extracted for 48 hours to obtain a degreased blank.
The above is only a part or preferred embodiment of the present invention, and neither the text nor the drawings should limit the scope of the present invention, and all equivalent structural changes made by the present specification and the contents of the drawings or the related technical fields directly/indirectly using the present specification and the drawings are included in the scope of the present invention.
Claims (7)
1. A method of manufacturing a part from a metal oxide, comprising the steps of:
mixing 95-98% of iron oxide powder and 16-22% of graphite powder by mass percentage, or mixing 70-93% of iron oxide powder, 7-30% of alloy element oxide powder and 16-22% of graphite powder by mass percentage, and ball-milling for 4-12 hours in a ball mill to obtain a raw material mixture;
the raw material mixture is formed through mould or 3D printing to obtain a product green body;
heating the product green blank to 1000 ℃ at a speed of 10 ℃/min in a tube furnace under the protection of argon, and preserving heat for 1-3 hours to reduce the product green blank;
heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours to sinter;
after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
2. The method of manufacturing a part from a metal oxide according to claim 1, wherein the alloying element oxide powder comprises a chromium oxide powder and a nickel oxide powder; the step of mixing and grinding iron oxide powder and graphite powder or iron oxide powder, alloy element oxide powder and graphite powder to obtain a raw material mixture comprises the following steps:
ball-milling 95-98% of iron oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain a carbon steel raw material mixture; or the like, or, alternatively,
ball-milling 90-93% of iron oxide powder, 7-8% of nickel oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain an alloy steel raw material mixture; or the like, or, alternatively,
ball-milling 85-90% of iron oxide powder, 10-16% of chromium oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain a martensitic stainless steel raw material mixture; or the like, or, alternatively,
and ball-milling 70-78% of iron oxide powder, 16-20% of chromium oxide powder, 7-8% of nickel oxide powder and 16-22% of graphite powder in a ball mill for 8-12 hours to obtain an austenitic stainless steel raw material mixture.
3. The method of manufacturing a part from a metal oxide according to claim 2, wherein the step of shaping the raw material mixture through a die or 3D printing to obtain a green product comprises:
and pressing and forming the martensitic stainless steel raw material mixture or the austenitic stainless steel raw material mixture in a die cavity to obtain a product green body.
4. The method of manufacturing a part from a metal oxide according to claim 2, wherein the step of shaping the raw material mixture through a die or 3D printing to obtain a green product comprises:
and pressing and forming the carbon steel raw material mixture or the alloy steel raw material mixture in a die cavity to obtain a product green body.
5. A method of manufacturing a part from a metal oxide, comprising the steps of:
according to the mass percentage, 95-98% of iron oxide powder and 16-22% of graphite powder, or 70-93% of iron oxide powder, 7-30% of alloy element oxide powder and 16-22% of graphite powder are mixed and ball-milled in a ball mill for 4-12 hours to obtain a raw material mixture, and the raw material mixture is mixed with a binder according to the volume fraction of 1:1 and heated and stirred; extruding the mixture on a double-screw extruder and uniformly cutting the mixture into granular feed;
the raw material mixture is formed through mould or 3D printing to obtain a product green body;
when the raw material mixture comprises chromium oxide powder and nickel oxide powder, placing the product green body in a sintering furnace in a reducing or protective atmosphere,
heating to 600 ℃ at the speed of 1 ℃/min, and keeping the temperature for 1 hour;
then heating to 1000 ℃ at the speed of 10 ℃/min, and preserving heat for 1-3 hours;
finally, heating to 1350-1400 ℃ at the speed of 5 ℃/min, and preserving heat for 2-4 hours;
after sintering, the temperature is reduced to 800 ℃ at the speed of 5 ℃/min, and then the product is cooled along with the furnace to obtain the finished product.
6. The method of manufacturing a part from a metal oxide according to claim 5, wherein the step of forming the raw material mixture into a green product by means of a die or 3D printing comprises:
and (3) putting the granular feed into an injection molding machine or a 3D printer, and preparing a product green body by an injection molding or 3D printing process.
7. The method of manufacturing a part from a metal oxide according to claim 5, further comprising, before the step of performing the step of reducing and sintering the green product in a sintering furnace in a reducing or protective atmosphere to produce a finished product:
and immersing the product green body into n-hexane, and heating and extracting for a time to obtain a degreased product green body for reduction and sintering.
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| CN110164677B (en) * | 2019-06-11 | 2020-11-06 | 莱芜职业技术学院 | Preparation of iron-based soft magnetic composite material wire for 3D printing |
| CN110918997A (en) * | 2019-11-20 | 2020-03-27 | 内蒙古科技大学 | Method for preparing porous stainless steel from iron scale |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US2065618A (en) * | 1933-12-28 | 1936-12-29 | John A Dienner | Metal and method of producing the same |
| JPS62164847A (en) * | 1986-01-17 | 1987-07-21 | Nippon Steel Corp | Manufacture of porous sintered compact |
| DE10014403A1 (en) * | 2000-03-24 | 2001-09-27 | Wolfgang Kochanek | Process for the powder metallurgy production of metal bodies comprises mixing a metal compound powder such as oxide powder with a rheology-improving additive, removing the additive; and reducing the metal compound using a reducing gas |
| CN101670438A (en) * | 2008-09-12 | 2010-03-17 | 深圳市注成科技有限公司 | Metal injection molding product and carbon control method thereof in manufacturing process |
| CN102337408B (en) * | 2011-08-30 | 2013-03-20 | 顾卫东 | Two-step reduction method for recycling stainless steel scales |
| BRPI1105355B1 (en) * | 2011-12-20 | 2018-12-04 | Univ Federal De Santa Catarina Ufsc | porous body manufacturing process by powder metallurgy and metallurgical composition of particulate materials |
| DE102013212528A1 (en) * | 2013-06-27 | 2014-12-31 | Robert Bosch Gmbh | Process for producing a steel shaped body |
| CN106077605A (en) * | 2016-06-06 | 2016-11-09 | 芜湖启泽信息技术有限公司 | A kind of 3D prints powder and 3D Method of printing |
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Denomination of invention: Methods of manufacturing parts with metal oxide Effective date of registration: 20210511 Granted publication date: 20200630 Pledgee: CITIC Bank Limited by Share Ltd. Shenzhen branch Pledgor: SHENZHEN AILIJIA MATERIALS TECHNOLOGY Co.,Ltd. Registration number: Y2021980003453 |
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