CN111118384A - Method for in-situ synthesis of aluminum oxide reinforced iron-based powder metallurgy alloy - Google Patents
Method for in-situ synthesis of aluminum oxide reinforced iron-based powder metallurgy alloy Download PDFInfo
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- CN111118384A CN111118384A CN202010013500.4A CN202010013500A CN111118384A CN 111118384 A CN111118384 A CN 111118384A CN 202010013500 A CN202010013500 A CN 202010013500A CN 111118384 A CN111118384 A CN 111118384A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0235—Starting from compounds, e.g. oxides
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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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
- C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a method for in-situ synthesis of an alumina reinforced iron-based powder metallurgy alloy, which comprises the following steps: (1) firstly, carrying out oxidation treatment on iron powder, wherein the oxidation temperature of the oxidation treatment is 100-300 ℃, and the oxidation time is 0.5-1 h; (2) adding aluminum powder and zinc stearate into the iron powder after oxidation treatment for ball milling, wherein the content of the added aluminum powder is 1-10% of the total mass, and the content of the added zinc stearate is 1-2% of the total mass; (3) pressing and sintering the alloy powder, wherein the sintering temperature is 1000-1150 ℃, the temperature rising rate is 10-20 ℃/min, and the temperature is kept after sintering; in the method, the second phase particles are generated in situ, so that the complicated reinforcement pretreatment procedure in the traditional reinforcement addition mode is avoided, and the production efficiency can be greatly improved; the composite material prepared by the method has the advantages that the reinforcement is nucleated and grown in the metal matrix, so that the surface of the reinforcement is free from pollution, the compatibility between the matrix and the reinforcement is good, the interface bonding strength is higher, and the mechanical property of the product can be effectively improved.
Description
Technical Field
The invention relates to a method for in-situ synthesis of aluminum oxide reinforced iron-based powder metallurgy alloy, which is used for preparing the iron-based powder metallurgy alloy.
Background
Second phase particle reinforcement is a very common means of strengthening metals. The metal matrix composite reinforced by the method has the advantages of matrix metal and reinforcing phase, shows the performances of high strength, low cost, high modulus, easy manufacture, high wear resistance and the like, and has wide application prospect. The powder metallurgy method is beneficial to the introduction of second phase particles due to the special process flow of preparing the alloy through powder pressing and sintering, so that the metal prepared by the powder metallurgy method is particularly suitable for strengthening the second phase, the segregation of alloy components can be reduced to the maximum extent, thick and uneven structures are eliminated, and the performance of the material is greatly improved. Therefore, the method for preparing the metal matrix composite material by the powder metallurgy method is widely applied to the manufacturing of aircraft and automobile parts.
Al2O3Has high hardness, high wear resistance and good corrosion resistance, is difficult to dissolve in a metal matrix at high temperature, is an excellent reinforcing phase and is dispersed Al2O3The particles are beneficial to improving the mechanical property and creep resistance of iron-based powder metallurgy, have good development prospect, but because the external reinforcement body used in the prior art is enhanced, Al can be caused2O3The material has poor wettability and poor bonding with an iron matrix, thereby limiting the development of the material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for synthesizing aluminum oxide reinforced iron-based powder metallurgy alloy in situ to achieve the purpose of improving the mechanical property of iron-based powder metallurgy.
In order to solve the technical problems, the method for synthesizing the aluminum oxide reinforced iron-based powder metallurgy alloy in situ comprises the following steps:
(1) firstly, the iron powder is oxidized.
The purity of the iron powder used in the iron powder oxidation treatment is 99.5 percent, and the particle size is 300 meshes; the equipment used for oxidation is a KSL-1200X type muffle furnace, the oxidation temperature is 100-300 ℃, and the oxidation time is 0.5-1 h.
(2) And then adding aluminum powder and zinc stearate into the iron powder after the oxidation treatment for ball milling.
The purity of the used aluminum powder is 99.5 percent, the particle size is 400 meshes, and the adding content is 1 to 10 percent of the total mass (namely the total mass of the iron powder, the aluminum powder and the zinc stearate, the same below); the content of the added zinc stearate is 1 to 2 percent of the total mass, and the zinc stearate is used as a reinforcing agent and a release agent; the ball milling equipment is a QM-3SP2 planetary ball mill, the ball-material ratio is 10:1, the rotating speed is 300-400 r/min, and the time is about 2 h.
The iron oxide is obtained by oxidation treatment of iron powder, so that a layer of iron oxide is attached to the surface of iron powder particles, and under the condition that the content of the aluminum powder is matched with the oxidation time, the sufficient reaction of the iron oxide and the aluminum powder can be ensured.
(3) And finally, pressing and sintering the alloy powder to prepare a sample.
The equipment used in the pressing and sintering process is a YLJ-40 type powder tablet press, the pressure is 450Mpa, the pressure maintaining time is 4-6 min, the powder is pressed into a cylinder with the diameter of 20mm, and the alloy powder used in each pattern is about 6 g; the sintering process is carried out in a vacuum environment, the sintering temperature is 1000-1150 ℃, the temperature rising rate is 10-20 ℃/min, and the sintering heat preservation time is about 1 hour.
According to the invention, iron oxide obtained by oxidizing iron powder reacts with aluminum powder in the sintering process to generate an alumina reinforced matrix in situ, and the generated alumina is uniformly distributed in the matrix, so that the dispersion strengthening effect is good, the comprehensive mechanical property of the product is improved, and the creep resistance of the matrix is greatly improved.
The content of the reinforcing phase alumina depends on the oxidation degree of the iron powder and the addition amount of the aluminum powder, the oxidation temperature of the invention is 100-300 ℃, and tests show that: because the influence of the temperature on the oxidation degree of the iron powder is exponentially increased, when the temperature is lower than 100 ℃, the oxidation degree of the iron powder is very small, and the content of iron oxide is low; when the temperature is higher than 300 ℃, the final sample is broken during sintering due to the excessive content of iron oxide, and cannot be formed.
The addition of the aluminum powder aims at eliminating iron oxide in the matrix, and the alumina is generated in situ to strengthen the matrix, according to the thermite reaction equation: 2AL + Fe2O3＝2Fe+Al2O3It can be concluded that the reaction is complete when the mass ratio of aluminum to iron oxide is 27:80, that residual iron oxide is present when the aluminum content is low, thereby reducing the mechanical properties and corrosion resistance of the product, etc., and that when the aluminum content is too high, although aluminum can reduce notch sensitivity of the matrix and refine grains, it has an adverse effect on hot workability and weldability of the product, and thus the amount of aluminum remaining can also be controlled. Based on the consideration of the factors, the invention determines that the aluminum powder with the mass of 1-10% of the total mass is added, and the test result shows that when the oxidation temperature is 100 ℃ and the content of the aluminum powder is 5%, the two have better proportion, and the hardness also reaches the maximum value in all samples.
According to the method for synthesizing the aluminum oxide reinforced iron-based powder metallurgy alloy in situ, the second-phase particles are generated in situ, so that a complicated reinforcement pretreatment procedure in the traditional reinforcement addition mode is avoided, namely the complicated reinforcement pretreatment procedure is omitted, and the production efficiency can be greatly improved; the composite material prepared by the method has the advantages that the reinforcement is nucleated and grown in the metal matrix, so that the surface of the reinforcement is free from pollution, the compatibility between the matrix and the reinforcement is good, the interface bonding strength is higher, and the mechanical property of the product can be effectively improved. The iron-based composite material prepared by the invention has the advantages that the alumina generated in situ is dispersed and distributed in the matrix, good second phase strengthening is generated, and the hardness of the product can be obviously improved.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a metallographic structure diagram of example 1.
FIG. 2 is a metallographic structure diagram of example 2.
FIG. 3 is a metallographic structure chart of example 3.
Detailed Description
Comparative example 1
Firstly, adding 1 percent of zinc stearate into 60g of iron powder (with the purity of 99.5 percent and the particle size of 300 meshes), putting the iron powder into a ball milling tank, mixing the iron powder and the zinc stearate at the ball material ratio of 10:1 at the rotating speed of 300r/min for 2 hours, then pressing metal powder (about 6g) into a cylinder with the diameter of 20mm by using the pressure of 450Mpa, keeping the pressure for 6 minutes, and finally sintering the pressed pattern in a vacuum sintering furnace at the sintering temperature of 1100 ℃ for 1 hour.
Example 1
60g of iron powder (with the purity of 99.5 percent and the particle size of 300 meshes) is put in a muffle furnace and is oxidized for 1 hour at the temperature of 100 ℃, then zinc stearate with the total mass of 1 percent and aluminum powder with the total mass of 1 percent (with the purity of 99.5 percent and the particle size of 400 meshes) are added into the iron powder and are ball-milled in a QM-3SP2 planetary ball mill, the mixture is mixed for 2 hours at the ball-material ratio of 10:1 at the rotating speed of 300r/min, then metal powder (about 6g) is pressed into a cylinder with the diameter of 20mm under the pressure of 450MPa, the pressure maintaining time is 6 minutes, finally the pressed pattern is put in a vacuum sintering furnace for sintering, the sintering temperature is 1100 ℃, and the heat preservation time is 1 hour.
Example 2
The difference between this example and example 1 is that: the oxidation time is 0.5h, and the content of the added aluminum powder is 5 percent of the total mass.
Example 3
The difference between this example and example 1 is that: the content of the added aluminum powder is 10 percent of the total mass, and the rotating speed of the ball mill is 400 r/min.
Example 4
The difference between this example and example 1 is that: the oxidation treatment temperature of the iron powder is 200 ℃, and the pressure maintaining time is 4 min.
Example 5
The difference between this example and example 1 is that: the temperature of the oxidation treatment of the iron powder is 200 ℃ and the content of the added aluminum powder is 5 percent of the total mass.
Example 6
The difference between this example and example 1 is that: the temperature of the iron powder oxidation treatment is 200 ℃ and the content of the added aluminum powder is 10 percent of the total mass.
Example 7
The difference between this example and example 1 is that: the iron powder oxidation treatment temperature is 300 ℃, and the sintering temperature is 1150 ℃.
And respectively adopting a metallographic microscope and a micro Vickers hardness tester to carry out metallographic structure observation and micro hardness test on the surface of the powder metallurgy product. And measuring 10 points of microhardness respectively, and removing the highest value and the lowest value to obtain average hardness. Microhardness was performed according to standard GB/T4340.1-2009. The test results are shown in table 1.
TABLE 1 test results
The sample prepared by the method generates a black alumina structure in situ at the junction of the matrix, generates second-phase reinforcement, and greatly improves the hardness compared with the comparative example 1; the oxidation temperature of iron powder and the content of aluminum have different degrees of influence on the strength of a sample, and test results show that: in the range of the oxidation temperature of 100-300 ℃, the higher the oxidation temperature is, namely the greater the oxidation degree of the iron powder is, the lower the hardness of the final product is, and the hardness of the product is the highest when the aluminum content is about 5%.
The above embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation fall within the protection scope of the present invention.
Claims (10)
1. The method for synthesizing the aluminum oxide reinforced iron-based powder metallurgy alloy in situ is characterized by comprising the following steps of:
(1) firstly, carrying out oxidation treatment on iron powder, wherein the oxidation temperature of the oxidation treatment is 100-300 ℃, and the oxidation time is 0.5-1 h;
(2) adding aluminum powder and zinc stearate into the iron powder after the oxidation treatment for ball milling, wherein the adding content of the aluminum powder is 1-10% of the total mass, and the adding content of the zinc stearate is 1-2% of the total mass;
(3) and finally, pressing and sintering the alloy powder, wherein the sintering temperature is 1000-1150 ℃, the temperature rising rate is 10-20 ℃/min, and the temperature is kept after sintering.
2. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in the step (1), the purity of the iron powder is 99.5%, and the particle size is 300 meshes.
3. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in the step (1), the oxidation treatment equipment is a KSL-1200X type muffle furnace.
4. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in the step (2), the purity of the aluminum powder is 99.5%, and the particle size is 400 meshes.
5. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in the step (2), the ball milling apparatus is a QM-3SP2 planetary ball mill.
6. The method of in situ synthesizing an alumina reinforced iron based powder metallurgy alloy according to claim 5, wherein: the ball-milling ball-material ratio is 10:1, the rotating speed is 300-400 r/min, and the ball-milling time is 2 h.
7. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in step (3), the equipment used for compression is a YLJ-40 type powder tablet press.
8. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in the step (3), the pressing pressure is 450MPa, and the pressure maintaining time is 4-6 min.
9. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in step (3), the sintering process is performed in a vacuum environment.
10. The method of in situ synthesizing an alumina reinforced iron-based powder metallurgy alloy according to claim 1, wherein: in the step (3), the sintering holding time is 1 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0599225A1 (en) * | 1992-11-20 | 1994-06-01 | Nisshin Steel Co., Ltd. | Iron-based material having excellent oxidation resistance at elevated temperatures and process for the production thereof |
| CN101996723A (en) * | 2010-09-29 | 2011-03-30 | 清华大学 | Composite soft magnetic powder core and preparation method thereof |
| CN109487110A (en) * | 2018-12-20 | 2019-03-19 | 河南科技大学 | A kind of in-situ authigenic Al2O3P Steel Base Surface Composite Produced precast body, preparation method and application |
-
2020
- 2020-01-07 CN CN202010013500.4A patent/CN111118384A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0599225A1 (en) * | 1992-11-20 | 1994-06-01 | Nisshin Steel Co., Ltd. | Iron-based material having excellent oxidation resistance at elevated temperatures and process for the production thereof |
| CN101996723A (en) * | 2010-09-29 | 2011-03-30 | 清华大学 | Composite soft magnetic powder core and preparation method thereof |
| CN109487110A (en) * | 2018-12-20 | 2019-03-19 | 河南科技大学 | A kind of in-situ authigenic Al2O3P Steel Base Surface Composite Produced precast body, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 王芬等: "原位合成Al2O3／FeAl复合材料的组织与性能", 《陕西科技大学学报》 * |
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