CN111172417A - Powder metallurgy material of endogenetic oxide strengthened alloy and preparation method thereof - Google Patents
Powder metallurgy material of endogenetic oxide strengthened alloy and preparation method thereof Download PDFInfo
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- CN111172417A CN111172417A CN202010066221.4A CN202010066221A CN111172417A CN 111172417 A CN111172417 A CN 111172417A CN 202010066221 A CN202010066221 A CN 202010066221A CN 111172417 A CN111172417 A CN 111172417A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/056—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using gas
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
- B22F2003/175—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging by hot forging, below sintering temperature
Abstract
The invention discloses a powder metallurgy material of endogenetic oxide strengthened alloy and a preparation method thereof, which directly prepare the oxide strengthened alloy by utilizing the crushing effect of a powder forging process on an oxide film. The oxide is thinned to be combined with a matrix at the broken part of the oxide film, the oxide product is transferred to the inside of the crystal grain and is uniformly distributed, the oxide film is well combined with the matrix, meanwhile, the alloy material is further densified by thermal processing, and the prepared alloy has excellent properties such as high strength, good plasticity and the like. The method does not need to add additional alloy elements, has low cost, can simultaneously carry out pre-oxidation treatment on a large number of products, is not limited by the load output capacity in the traditional vacuum hot pressing sintering, has simple production process and low production environment requirement, and can form oxides which are well combined with a matrix and are convenient for large-scale production.
Description
Technical Field
The invention belongs to the field of powder metallurgy materials, and relates to a powder metallurgy material of an endogenic oxide reinforced alloy and a preparation method thereof.
Background
Second phase strengthening is a primary method used to strengthen materials and can be divided into two types, an extra second phase and an endogenous second phase, depending on the manner in which the second phase is produced. Generally, the strengthening effect of the powder metallurgy material composite material prepared by the adding mode is often lower than that of the endogenous second phase because the added second phase is difficult to realize good metallurgical bonding with a matrix and the adding amount is limited, so that how to prepare the endogenous second phase strengthening alloy with fine and dispersed distribution has great research value.
Disclosure of Invention
The invention aims to solve the problems of poor composite material performance caused by poor bonding between an additional second phase and a matrix, limited doping amount and easy segregation when the size of the second phase is small in the existing powder metallurgy material in the prior art, and provides a powder metallurgy material of an endogenous oxide reinforced alloy and a preparation method thereof. The powder metallurgy material forging technology is a technology combining a conventional powder metallurgy material and high-temperature forging, can realize near-end or final forming, has high utilization rate of raw materials, can effectively crush oxides on the surface of powder due to strong flow of the powder under load in the forging process, can enhance the sintering performance of the powder, can convert unfavorable oxidation products into a strengthening phase, and has good combination with a matrix. Therefore, by intentionally introducing a certain amount of oxygen into the alloy material, the alloy material can be crushed and densified by powder forging to produce an oxide-strengthened alloy material.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a method for preparing a powder metallurgy material of an endogenic oxide strengthened alloy comprises the following steps:
step 1, placing initial alloy powder in a cold-pressing die for cold pressing to form a prefabricated part;
step 2, the prefabricated member obtained in the step 1 is placed in N2And O2Pre-sintering under no pressure in atmosphere, O2The volume fraction of the powder forging is 2-5%, hot forging is carried out on the pre-sintered part, then a surface oxide layer is removed, and the structural allowance is removed, so that the powder forging is obtained;
and 3, rolling, forging or extruding the powder forging obtained in the step 2 to obtain the powder metallurgy material.
The particle size of the initial alloy powder in the step 1 is 20-100 mu m.
The cold pressure in the step 1 is 400-700 MPa.
In the step 2, the pre-sintering temperature and the hot forging temperature are determined according to the MPIF Standard 35-2012 (Standard for powder metallurgy Structure part materials), and the pre-sintering time is 20-480 minutes.
And 2, removing the surface oxide layer through shot blasting, and removing the structural allowance through machining and fine trimming.
And 3, determining the hot working temperature of the powder forging according to Asm Handbook (materials engineering Handbook).
A powder metallurgy material prepared according to a method for preparing an endogenic oxide strengthened alloy powder metallurgy material, the powder metallurgy material comprising Fe40Mn40Co10Cr10。
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a method for preparing a powder metallurgy material of an endogenous oxide reinforced alloy, which is characterized in that a certain amount of oxygen is introduced in the pre-sintering process to form an oxide film on the surface of powder, and the oxide reinforced alloy is directly prepared by utilizing the crushing effect of a powder forging process on the oxide film. According to the method, additional alloy elements are not required to be added, the alloy powder is directly used, oxidation is carried out by means of air remained in the furnace during presintering, the cost is low, the presintering vacuum condition is reduced, the process is simple, a large number of test pieces can be simultaneously subjected to presintering, and the efficiency is high; the method fully utilizes the crushing effect of powder forging on the oxide film on the surface of the powder, refines the oxide to be combined with the substrate at the crushed part of the oxide film, transfers the oxidation product into the crystal grains, has uniform distribution and good combination of the oxide film and the substrate, and simultaneously utilizes hot working to further densify the alloy material, and the prepared alloy has excellent properties of high strength, good plasticity and the like.
The invention discloses a powder metallurgy material prepared by an endogenic oxide reinforced alloy powder metallurgy material preparation method, which can be seen from an electronic metallographic photograph that no oxide exists in a sample after conventional vacuum hot-pressing sintering, but a large amount of oxidation products exist in the interior of crystal grains and on crystal boundaries of an alloy after preoxidation treatment, and the oxidation products are further refined and uniformly distributed after hot rolling. The powder metallurgy material prepared by the preparation method of the invention generates a large amount of oxides in the crystal grains, is uniformly distributed, has small size, and is the reason that the alloy has excellent performance under the treatment of the process.
Drawings
FIG. 1 is a drawing graph of an alloy obtained by conventional vacuum hot-pressing sintering, hot rolling, pre-oxidation treatment, powder forging, and pre-oxidation, powder forging and hot rolling preparation processes corresponding to comparative example 1, comparative example 2 and example 1 of the present invention;
FIG. 2 is an electronic metallographic scanning photograph of an alloy obtained by different preparation processes corresponding to comparative example 1, comparative example 2 and example 1 of the present invention, (a) a conventional vacuum hot-pressing sintering and hot-rolling preparation process, (b) a pre-oxidation and powder forging preparation process, (c) a pre-oxidation, powder forging and hot-rolling preparation process;
FIG. 3 is a transmission photograph of an alloy obtained by the corresponding pre-oxidation + powder forging + hot rolling manufacturing process in example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
a method for preparing a powder metallurgy material of an endogenic oxide strengthened alloy comprises the following steps:
1) self-making or purchasing initial alloy powder with the particle size of 20-100 mu m;
2) carrying out cold pressing on the alloy powder obtained in the step 1) in a cold pressing die, wherein the pressure is 400-700MPa, and forming a prefabricated part;
3) placing the prefabricated member obtained in the step (2) in a sintering furnace, and performing sintering in the presence of N2+(2-5vol.％)O2Performing pressureless pre-sintering in atmosphere, determining proper pre-sintering temperature and forging temperature according to the MPIF Standard 35-2012 Standard, sintering for 20-480 minutes under vacuum condition, then placing the pre-sintered part into a hot forging die cavity for hot forging at the hot forging temperature, performing shot blasting after forging to remove a surface oxide layer, and performing machining and fine trimming to remove structural allowance to obtain a powder forging piece;
4) and rolling, forging or extruding the powder forging according to the alloy hot working temperature determined by Asm Handbook to obtain the powder metallurgy material.
The following list illustrates several embodiments of the invention:
example 1
Example 1 provides a Fe40Mn40Co10Cr10Powder metallurgy material, self-made Fe40Mn40Co10Cr10An alloy powder having a particle size of 40 μm; placing the alloy powder in a cold pressing die for cold pressing, wherein the pressure is 700MPa, and forming a prefabricated part; the obtained preform is placed in a sintering furnace in N2+2vol.％O2Performing pressureless pre-sintering in atmosphere, namely sintering for 240 minutes at 1150 ℃ under a vacuum condition and pre-oxidizing, then putting the pre-sintered parts into a hot forging die cavity, performing hot forging at 1100 ℃, performing shot blasting after forging to remove a surface oxide layer, and performing machining and fine trimming to remove the structural allowance, thereby obtaining a powder forging piece; hot rolling the powder forging at 1000 ℃ to obtain Fe40Mn40Co10Cr10Powder metallurgy material.
Example 2
Example 2 provides a Fe40Mn40Co10Cr10Powder metallurgy material, purchase Fe40Mn40Co10Cr10An alloy powder having a particle size of 100 μm; placing the alloy powder in a cold pressing die for cold pressing, wherein the pressure is 400MPa, and forming a prefabricated part; placing the obtained preform inIn a sintering furnace, in N2+5vol.％O2Performing pressureless pre-sintering in atmosphere, namely sintering for 20 minutes at 1150 ℃ under a vacuum condition and pre-oxidizing, then putting the pre-sintered parts into a hot forging die cavity, performing hot forging at 1100 ℃, performing shot blasting after forging to remove a surface oxide layer, and performing machining and fine trimming to remove the structural allowance to obtain a powder forging piece; forging the powder forging at 1000 ℃ to obtain Fe40Mn40Co10Cr10Powder metallurgy material.
Example 3
Example 3 provides a Fe40Mn40Co10Cr10Powder metallurgy material, purchase Fe40Mn40Co10Cr10An alloy powder having a particle size of 20 μm; placing the alloy powder in a cold pressing die for cold pressing under the pressure of 600MPa to form a prefabricated part; the obtained preform is placed in a sintering furnace in N2+3vol.％O2Performing pressureless pre-sintering in atmosphere, namely sintering for 480 minutes at 1150 ℃ under a vacuum condition and pre-oxidizing, then putting the pre-sintered parts into a hot forging die cavity and performing hot forging at 1100 ℃, performing shot blasting after forging to remove a surface oxide layer and performing machining and fine trimming to remove the structural allowance, thus obtaining a powder forging piece; carrying out hot extrusion on the powder forging piece at 1000 ℃ to obtain Fe40Mn40Co10Cr10Powder metallurgy material.
Comparative example 1
This comparative example 1 provides a Fe40Mn40Co10Cr10Powder metallurgy material, self-made Fe40Mn40Co10Cr10Alloy powder with the grain size of 40 mu m is sintered in a sintering furnace under vacuum hot pressing, namely under vacuum conditions, at 1150 ℃ for 120 minutes and 45MPa, and then hot rolled at 1000 ℃ to obtain Fe40Mn40Co10Cr10Powder metallurgy material.
Comparative example 2
This comparative example 2 provides a Fe40Mn40Co10Cr10Powder metallurgy material, self-made Fe40Mn40Co10Cr10An alloy powder having a particle size of 40 μm; placing the alloy powder in a cold pressing die for cold pressing, wherein the pressure is 700MPa, and forming a prefabricated part; the obtained preform is placed in a sintering furnace in N2+2vol.％O2Pressureless pre-sintering in atmosphere, namely sintering for 240 minutes at 1150 ℃ under vacuum condition and pre-oxidizing, then placing the pre-sintered part into a hot forging die cavity for hot forging at 1100 ℃, performing shot blasting after forging to remove a surface oxide layer, and performing machining and fine trimming to remove the structural allowance to obtain Fe40Mn40Co10Cr10Powder metallurgy material.
The tensile curve of the alloy prepared by the three processes of conventional vacuum hot-pressing sintering, hot rolling, preoxidation, powder forging and hot rolling corresponding to the comparative example 1, the comparative example 2 and the example 1 of the invention is shown in figure 1, and it can be seen that the strength of the alloy after the treatment of preoxidation, powder forging and hot rolling is far higher than that of the alloy prepared by the first two processes, and the plasticity is not significantly reduced compared with that of the conventional vacuum hot-pressing sintered part; as shown in fig. 2, it can be seen from the electronic metallography that no oxide exists in the sample after the conventional vacuum hot-pressing sintering (fig. 2a), but a large amount of oxidation products exist in the interior of the crystal grains and on the grain boundary of the alloy after the pre-oxidation treatment (fig. 2b), and after the hot rolling (fig. 2c), the oxidation products are further refined and uniformly distributed; as shown in FIG. 3, it can be seen from the transmission photograph of the alloy that a large amount of oxides (Fe without pre-oxidation treatment) were generated inside the crystal grains40Mn40Co10Cr10The alloy is a single phase, no precipitated phase exists), the distribution is uniform, the size is small, and the alloy has excellent performance under the treatment of the process.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. A method for preparing a powder metallurgy material of an endogenic oxide strengthened alloy is characterized by comprising the following steps:
step 1, placing initial alloy powder in a cold-pressing die for cold pressing to form a prefabricated part;
step 2, the prefabricated member obtained in the step 1 is placed in N2And O2Pre-sintering under no pressure in atmosphere, O2The volume fraction of the powder forging is 2-5%, hot forging is carried out on the pre-sintered part, then a surface oxide layer is removed, and the structural allowance is removed, so that the powder forging is obtained;
and 3, rolling, forging or extruding the powder forging obtained in the step 2 to obtain the powder metallurgy material.
2. The method of producing a powder metallurgy of an endogenously produced oxide-strengthened alloy according to claim 1, wherein the particle size of the starting alloy powder in step 1 is 20-100 μm.
3. The method for preparing a powder metallurgy material of an endogenic oxide strengthened alloy according to claim 1, wherein the cold pressing pressure in step 1 is 400-700 MPa.
4. The method for preparing the powder metallurgy material of the endogenic oxide strengthened alloy according to claim 1, wherein the pre-sintering temperature and the hot forging temperature in the step 2 are determined according to MPIF Standard 35-2012, and the pre-sintering time is 20-480 minutes.
5. The method for producing a powder metallurgy material of an endogenetic oxide strengthened alloy according to claim 1, wherein the surface oxide layer is removed by shot blasting in step 2, and the structural balance is removed by machining and finishing.
6. The method for preparing a powder metallurgy material of an endogenetic oxide strengthened alloy according to claim 1, wherein in step 3, the hot working temperature of the powder forging is determined according to Asm Handbook.
7. A powder metallurgy material produced by the method for producing an endogenic oxide strengthened alloy powder metallurgy material according to any one of claims 1 to 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113351866A (en) * | 2021-04-25 | 2021-09-07 | 西安交通大学 | Powder metallurgy preparation method of oxide-reinforced high-entropy alloy |
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