CN111531173B - Yttrium-containing powder metallurgy high-speed steel and preparation method thereof - Google Patents

Yttrium-containing powder metallurgy high-speed steel and preparation method thereof Download PDF

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CN111531173B
CN111531173B CN202010552868.8A CN202010552868A CN111531173B CN 111531173 B CN111531173 B CN 111531173B CN 202010552868 A CN202010552868 A CN 202010552868A CN 111531173 B CN111531173 B CN 111531173B
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yttrium
carbide powder
speed steel
carbide
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熊翔
杨宝震
刘如铁
陈洁
汪琳
廖宁
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Central South University
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    • 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
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • 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
    • C22C32/0047—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 carbides, nitrides, borides or silicides as the main non-metallic constituents
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    • C22C33/0264—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements the maximum content of each alloying element not exceeding 5%
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    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0292—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with more than 5% preformed carbides, nitrides or borides
    • C—CHEMISTRY; METALLURGY
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract

The invention discloses yttrium-containing powder metallurgy high-speed steel and a preparation method thereof. The raw materials comprise the following components in percentage by mass: 80-90 wt.% carbonyl iron powder; 3-9 wt.% of tungsten carbide powder; 2.5-8 wt.% of molybdenum carbide powder; 2-6 wt.% of chromium carbide powder; 1-3 wt.% of vanadium carbide powder; 0.02-0.10 wt.% of yttrium hydride powder. The preparation method comprises the steps of taking carbide powder, carbonyl iron powder and hydrogenated yttrium powder as raw materials, and preparing the high-performance powder metallurgy high-speed steel through the steps of ball milling mixing, vacuum drying, spark plasma sintering and the like. The invention has the advantages of high utilization rate of rare earth elements, simple process flow, low sintering temperature and the like. The spark plasma sintering powder metallurgy high-speed steel has low oxygen content, fine crystal grains, uniform carbide distribution and excellent bending strength and impact toughness.

Description

Yttrium-containing powder metallurgy high-speed steel and preparation method thereof
Technical Field
The invention belongs to the technical field of powder metallurgy high-speed steel manufacturing, and relates to yttrium-containing powder metallurgy high-speed steel and a preparation method thereof.
Background
High Speed Steel (HSS) is a high carbon, high alloy tool steel that accounts for over 30% of the global cutting tool consumption. The HSS has high abrasion resistance, red hardness and higher impact toughness and economy compared with ceramic cutters, and is suitable for preparing cutting tools with complex shapes, such as screw taps, gear inserts and the like. The mechanical properties of high speed steel are greatly influenced by the type, size and distribution of carbides in the structure.
High-speed steel prepared by the traditional casting process inevitably generates a coarse lewy body carbide segregation structure because alloy carbide is preferentially precipitated from liquid in the cooling process. The existence of segregation not only makes the hot forging and rolling of the steel difficult, but also significantly reduces the strength, wear resistance and other properties of the steel. In order to achieve a uniform distribution of the carbides, the most desirable method is to use powder metallurgy Process (PM). In the atomization powder preparation process, because the extremely fast solidification speed of the alloy liquid drops inhibits the formation of eutectic, very fine carbide particles can be generated inside the powder particles. By properly controlling the processing, these particles can remain in the sintered and heat treated final product, thereby improving the workability, wear resistance, and dimensional consistency during heat treatment of high speed steels. The powder cold pressing-sintering process is a widely adopted low-cost powder metallurgy product production method. Because active elements on the surfaces of powder particles are easy to oxidize in the powder preparation process, the oxygen content of the powder is too high and needs to be removed in the sintering process. However, too high a deoxidation temperature causes carbide growth and coarsening of grains, which seriously impairs the flexural strength and impact toughness of high-speed steel.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide yttrium-containing powder metallurgy high-speed steel and a preparation method thereof. According to the preparation method, the carbide is used as the raw material, so that the oxidation of active metal elements in the preparation process of the material can be avoided, and the oxygen content in the powder can be reduced; meanwhile, a proper amount of rare earth element yttrium is added, the surface activity of the rare earth element yttrium is strong, and the rare earth element yttrium can be combined with oxygen in a pressed compact during low-temperature sintering, so that the aim of removing oxygen in powder is fulfilled; by adopting SPS sintering, the heat preservation time can be effectively reduced, so that the growth and coarsening of crystal grains are avoided, and carbides in a material structure are finer and are distributed more dispersedly; finally, the material has more excellent bending strength, abrasion resistance and impact toughness.
The invention relates to yttrium-containing powder metallurgy high-speed steel which comprises the following raw materials in percentage by mass: 80-90 wt.% carbonyl iron powder; 3-9 wt.% of tungsten carbide powder; 2.5-8 wt.% of molybdenum carbide powder; 2-6 wt.% of chromium carbide powder; 1-3 wt.% of vanadium carbide powder; 0.02-0.10 wt.% of yttrium hydride powder.
In the invention, carbonyl iron powder; tungsten carbide powder; molybdenum carbide powder; chromium carbide powder; vanadium carbide powder; the yttrium hydride powder is a raw material of high-speed steel, and carbides of alloy elements W, Mo, Cr and V have stable chemical properties and are not easy to react with oxygen at high temperature. Therefore, the carbide is taken as the raw material, oxidation of more active alloy elements can be effectively avoided, carbide particles can be used as a hard phase in the sintering process, a crystal boundary is stabilized, and growth of the crystal grains is hindered, so that a fine structure of the crystal grains is obtained, yttrium can strengthen the crystal boundary on one hand, and meanwhile, yttrium hydride is active in performance, and rare earth oxide generated by combination of yttrium element and oxygen can play a role in dispersion strengthening, so that the purpose of removing oxygen element in powder is achieved, and the sintering temperature is further reduced.
Of course, in order to make the high-speed steel have high strength and toughness and excellent wear resistance, the proportion of the above components is also important, for example, tungsten carbide powder can combine with Fe and a small amount of Mo and Cr to form a certain amount of refractory primary carbide M in the sintering process6And C, improving the wear resistance and hardness of the steel. In addition, after high-temperature solid solution, part of carbide is subjected to solid solution, and precipitates in the form of fine and dispersed MC carbide during tempering, thereby determining the red hardness of the steel. The addition of tungsten carbide is too little, which easily causes the reduction of the hardness of the material and reduces the abrasion resistance of the material. For example, the addition of excessive amount of yttrium hydride can cause the rare earth yttrium to be enriched and precipitated in grain boundaries, reduce the bonding force of the grain boundaries and cause the strength of the material to be reduced.
As a preferable scheme, the yttrium-containing powder metallurgy high-speed steel comprises the following raw materials in percentage by mass:
80-90 wt.% carbonyl iron powder; 4-6.5 wt.% of tungsten carbide powder; 2.5-5.5 wt.% molybdenum carbide powder; 2-5 wt.% of chromium carbide powder; 1-2.6 wt.% of vanadium carbide powder; 0.02-0.08 wt.% of yttrium hydride powder.
The invention relates to a preparation method of yttrium-containing powder metallurgy high-speed steel, which comprises the following steps: weighing carbonyl iron powder, tungsten carbide powder, molybdenum carbide powder, chromium carbide powder, vanadium carbide powder and yttrium hydride powder according to the designed component proportion, and performing ball milling and mixing to obtain mixed powder; and drying the mixed powder, placing the dried mixed powder into a mold, and performing SPS sintering in a vacuum atmosphere to obtain the yttrium-containing powder metallurgy high-speed steel, wherein the pressure of the SPS sintering is 20-40 MPa, the sintering temperature is 1080-1120 ℃, the sintering time is 5-10 min, and the vacuum degree is less than or equal to 5 Pa.
Preferably, the particle size range of the carbonyl iron powder is 5-10 μm, and the particle size ranges of the tungsten carbide powder, the molybdenum carbide powder, the chromium carbide powder, the vanadium carbide powder and the yttrium hydride powder are 0.5-2 μm.
Preferably, during ball milling, the ball-material ratio is 7-12: 1, the ball milling time is 20-60 hours, the rotating speed is 200-280 r/min, and the dispersing agent is absolute ethyl alcohol.
In practical operation, the ball mill is preferably a planetary ball mill, and the material of the pot body and the material of the grinding balls are preferably cemented carbide.
Preferably, the grinding balls used for ball milling are composed of a grinding ball A with the diameter of 5mm and a grinding ball B with the diameter of 3mm, and the ratio of the grinding ball A to the grinding ball B is 1.5-3: 1.
Preferably, the drying is carried out in a vacuum environment, and the vacuum degree is less than or equal to 1 × 10-1Pa, the drying temperature is 70-80 ℃, and the drying time is 90-120 min.
As a preferred scheme, the temperature rise rate of the SPS sintering is more than or equal to 80 ℃/min, and preferably 90-100 ℃/min.
Principles and advantages
(1) In the invention, carbonyl iron powder; tungsten carbide powder; molybdenum carbide powder; chromium carbide powder; vanadium carbide powder; the yttrium hydride powder is a raw material of high-speed steel, and carbides of alloy elements W, Mo, Cr and V have stable chemical properties and are not easy to react with oxygen at high temperature. Therefore, the carbide is used as the raw material, so that the oxidation of the more active alloy elements can be effectively avoided. Under the synergistic action of the raw material components, the raw material size, the material mixing time and the SPS sintering procedure, the high-speed steel obtained by the invention contains fine and dispersed nano-scale carbides to improve the grindability and hardness of the material, and also contains micro-scale large-particle carbides within the range of 0.5-3 mu m to improve the wear resistance of the material.
(2) The rare earth element yttrium is added in the form of hydrogenated yttrium, the surface activity of the rare earth element yttrium is strong, the rare earth element yttrium can be combined with oxygen in a pressed compact when being sintered at a lower temperature, and the generated rare earth oxide can be uniformly and finely distributed in a matrix to generate a dispersion strengthening effect and improve the strength of the material. In addition, rare earth elements are introduced into the high-speed steel by using a powder metallurgy method, so that the mass fraction of the rare earth elements in the material can be more accurately controlled, and the waste of the rare earth elements is reduced.
(3) The invention combines the SPS rapid sintering process with the carbide powder as the raw material, effectively weakens the growth trend of carbide and matrix grains in the sintering process, and leads the carbide and the matrix grains in the final material structure to be finer.
(4) The invention has the advantages of high utilization rate of rare earth elements, simple process flow, low sintering temperature and the like. The spark plasma sintering powder metallurgy high-speed steel has low oxygen content, fine crystal grains, uniform carbide distribution and further improved bending strength and impact toughness.
Drawings
FIG. 1 is a SEM photograph of a typical microstructure of a PM HSS in an SPS sintered state prepared in example 1. The dark gray crystal grains in the microstructure are taken as a matrix, and the main component is Fe; the bright spherical crystal grains are composite carbide M6C, and the main components are W, Fe, Mo and C; the grey crystal grains are composite carbide MC, and the main components are V, Fe, Cr and C.
FIG. 2 is a SEM photograph of a typical microstructure of a PM HSS in an SPS sintered state prepared in example 2.
FIG. 3 is a SEM photograph of a typical microstructure of a PM HSS in an SPS sintered state prepared in example 3. The dark gray polygonal crystal grains in the microstructure are taken as a matrix, and the white area is a composite carbide M6C; the grey zone is the composite carbide MC.
FIG. 4 is an SEM photograph of a typical microstructure of an SPS sintered PM HSS prepared in comparative example 1. The gray area in the microstructure is a matrix, and the bright white area is coarsened composite carbide. As the SPS sintering temperature is increased, the carbides grow into stripes and aggregation occurs.
FIG. 5 is an SEM photograph of a typical microstructure of PM HSS after vacuum sintering as prepared in comparative example 2. The gray area in the microstructure is the matrix, the bright white crystal grain is the compound carbide M6C; the grey crystal grains are composite carbide MC. The average grain size of the matrix and carbide increases by a factor of 3-5 compared to SPS sintering.
FIG. 6 is an SEM photograph of a typical microstructure of PM HSS after vacuum sintering as prepared in comparative example 3. The microstructure showed agglomerated yttrium particles at the grain boundaries.
Detailed Description
For better understanding of the present invention, the present invention will be further described with reference to the following examples, but the embodiments of the present invention are not limited thereto.
Example 1
90g (10 μm) of carbonyl iron powder, 0.02g (2 μm) of yttrium hydride powder, 4.26g (0.5 μm) of WC powder, 2.55g (1.5 μm) of Mo2C powder, 2.02g (1.5 μm) Cr3C2Powder and 1.17g (1.5 mu m) of VC powder are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the ball material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 40ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 40 hours, and the rotating speed is 220 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 90min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing 55g of mixed powder, putting the mixed powder into an SPS phi 40 mold, heating to 1080 ℃ at the heating rate of 100 ℃/min, sintering at the pressure of 40MPa for 10min, and keeping the vacuum degree in the furnace at 5Pa during sintering.
The results of the sintered body performance test are shown in table 1, and the microstructure is shown in fig. 1.
Example 2
97.4g (10 μm) of carbonyl iron powder, 0.05g (2 μm) of yttrium hydride powder, 7.67g (0.5 μm) of WC powder, 6.38g (1.5 μm) of Mo2C powder, 5.54g (1.5 μm) Cr3C2Powder and 3.01g (1.5 mu m) VC are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 45ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 50h, and the rotating speed is 200 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 100min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing 110g of mixed powder, putting the mixed powder into an SPS phi 60 die, heating to 1100 ℃ at the heating rate of 100 ℃/min, sintering at the pressure of 40MPa for 10min, and keeping the vacuum degree in the furnace at 5Pa during sintering.
The results of the sintered body performance test are shown in table 1, and the microstructure is shown in fig. 2.
Example 3
81.17g (5 μm) carbonyl iron powder, 0.08g (2 μm) yttrium hydride powder, 6.39g (0.5 μm) WC powder, 5.32g (1.5 μm) Mo2C powder, 4.62g (1.5 μm) Cr3C2Powder and 2.51g (1.5 mu m) of VC are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 40ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 60 hours, and the rotating speed is 250 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 120min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing 100g of mixed powder, placing the mixed powder into an SPS phi 60 mold, heating to 1120 ℃ at the heating rate of 100 ℃/min, sintering at the pressure of 40MPa for 8min, and keeping the vacuum degree in the furnace at 5Pa during sintering.
The results of the sintered body performance test are shown in table 1, and the microstructure is shown in fig. 3.
Comparative example 1
90g (10 μm) of carbonyl iron powder, 0.02g (2 μm) of yttrium hydride powder, 4.26g (0.5 μm) of WC powder, 2.55g (1.5 μm) of Mo2C powder, 2.02g (1.5 μm) Cr3C2Powder and 1.17g (1.5 mu m) of VC powder are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the ball material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 40ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 40 hours, and the rotating speed is 220 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 90min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing 55g of mixed powder, putting the mixed powder into an SPS phi 40 die, heating to 1180 ℃ at the heating rate of 100 ℃/min, wherein the sintering pressure is 40MPa, the sintering time is 10min, and the vacuum degree in the furnace is 5Pa during sintering.
The results of the sintered body performance test are shown in table 1, and the microstructure is shown in fig. 4.
Comparative example 2
90g (10 μm) of carbonyl iron powder, 0.02g (2 μm) of yttrium hydride powder, 4.26g (0.5 μm) of WC powder, 2.55g (1.5 μm) of Mo2C powder, 2.02g (1.5 μm) Cr3C2Powder and 1.17g (1.5 mu m) of VC powder are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the ball material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 40ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 40 hours, and the rotating speed is 220 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 90min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing the mixed materials, forming in a die by adopting bidirectional pressing, wherein the pressing pressure is 650MPa, the pressure maintaining time is 4s, and then demoulding to obtain a pressed blank.
Sintering the green compact in a vacuum furnace at a vacuum degree of 3 × 10-3pa, uniformly heating to 1150 ℃ at a heating rate of 8 ℃/min, preserving heat for 60min, then uniformly cooling to below 80 ℃ at a cooling rate of 70 ℃/min, and discharging to obtain a sintered body.
The results of the sintered body performance test are shown in table 1, and the microstructure is shown in fig. 5.
Comparative example 3
90g (10 μm) of carbonyl iron powder, 0.50g (2 μm) of yttrium hydride powder, 4.26g (0.5 μm) of WC powder, 2.55g (1.5 μm) of Mo2C powder, 2.02g (1.5 μm) Cr3C2Powder and 1.17g (1.5 mu m) of VC powder are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the ball material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 40ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 40 hours, and the rotating speed is 220 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 90min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing the mixed materials, forming in a die by adopting bidirectional pressing, wherein the pressing pressure is 650MPa, the pressure maintaining time is 4s, and then demoulding to obtain a pressed blank.
Sintering the pressed compact in a vacuum furnace at a vacuum degree of 3 × 10-3pa, uniformly heating to 1150 ℃ at a heating rate of 8 ℃/min, preserving heat for 60min, then uniformly cooling to below 80 ℃ at a cooling rate of 70 ℃/min, and discharging to obtain a sintered body.
The results of the sintered body performance test are shown in table 1, and the microstructure is shown in fig. 6.
Comparative example 4
90g (10 μm) of carbonyl iron powder, 0.02g (2 μm) of yttrium hydride powder, 8.5g (0.5 μm) of WC powder, 2.55g (1.5 μm) of Mo2C powder, 2.02g (1.5 μm) Cr3C2Powder and 1.17g (1.5 mu m) of VC powder are filled in a hard alloy ball milling tank, and the weight ratio of the powder to the ball material is 10: 1, size-to-sphere ratio 5: 3 adding a hard alloy ball; after 40ml of absolute ethyl alcohol is added, the ball milling tank is fixed on a planetary ball mill for ball milling, the ball milling time is 40 hours, and the rotating speed is 220 r/min.
And pouring the ball-milled slurry into a tray, paving the tray and putting the tray into a vacuum drying oven, wherein the drying temperature is 70 ℃, the drying time is 90min, and then uniformly sieving the powder through a 100-mesh sieve to obtain dry mixed powder.
Weighing 55g of mixed powder, putting the mixed powder into an SPS phi 40 die, heating to 1180 ℃ at the heating rate of 100 ℃/min, wherein the sintering pressure is 40MPa, the sintering time is 10min, and the vacuum degree in the furnace is 5Pa during sintering.
The results of the sintered body performance test are shown in table 1.
TABLE 1 basic Properties of the examples and of the samples obtained in comparative examples
Figure BDA0002543207790000071
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.

Claims (3)

1. A preparation method of yttrium-containing powder metallurgy high-speed steel is characterized by comprising the following steps: the method comprises the following steps: weighing the following raw materials in proportion by design: carbonyl iron powder, tungsten carbide powder, molybdenum carbide powder, chromium carbide powder, vanadium carbide powder and yttrium hydride powder, and performing ball milling and mixing to obtain mixed powder; drying the mixed powder, placing the dried mixed powder in a mould, and performing SPS sintering in a vacuum atmosphere to obtain yttrium-containing powder metallurgy high-speed steel;
the raw materials comprise the following components in percentage by mass: 80-90 wt.% carbonyl iron powder; 3-9 wt.% of tungsten carbide powder; 2.5-8 wt.% of molybdenum carbide powder; 2-6 wt.% of chromium carbide powder; 1-3 wt.% of vanadium carbide powder; 0.02-0.10 wt.% yttrium hydride powder;
the grinding balls used for ball milling are composed of a grinding ball A with the diameter of 5mm and a grinding ball B with the diameter of 3mm, and the ratio of the grinding ball A to the grinding ball B is 1.5-3: 1;
the drying is carried out in a vacuum environment with the vacuum degree less than or equal to 1 multiplied by 10-1Pa, drying at the temperature of 70-80 ℃ for 90-120 min;
the pressure of the SPS sintering is 20-40 MPa, the sintering temperature is 1080-1120 ℃, the sintering time is 5-10 min, and the vacuum degree is less than or equal to 5 Pa.
2. The method of claim 1, wherein the yttrium-containing powder metallurgy high-speed steel comprises: the particle size range of the carbonyl iron powder is 5-10 mu m, and the particle size ranges of the tungsten carbide powder, the molybdenum carbide powder, the chromium carbide powder, the vanadium carbide powder and the yttrium hydride powder are 0.5-2 mu m.
3. The method of claim 1, wherein the yttrium-containing powder metallurgy high-speed steel comprises: the temperature rise rate of the SPS sintering is more than or equal to 80 ℃/min.
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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003239035A (en) * 2002-02-14 2003-08-27 Mitsubishi Materials Corp Composite soft magnetic sintered material with high strength, high density, and high resistivity, and its manufacturing method
CN102071360A (en) * 2011-01-14 2011-05-25 华南理工大学 Tungsten carbide particle-enhanced iron-based powder metallurgy material and preparation method thereof
CN102251132A (en) * 2011-07-06 2011-11-23 北京科技大学 Method for preparing cobalt-based ODS (Ozone Depleting Substance) alloy through mechanochemical reaction process
CN102277525A (en) * 2011-08-23 2011-12-14 北京科技大学 Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel
CN103182506A (en) * 2013-03-29 2013-07-03 华南理工大学 TiCp/M2 high-speed steel composite material and SPS (spark plasma sintering) preparation method thereof
CN103233182A (en) * 2013-06-07 2013-08-07 北京科技大学 Forming method for nanometer beta' phase element and nanometer oxide composite reinforced Fe-based ODS alloy
CN103966500B (en) * 2014-05-22 2017-11-14 北京航空航天大学 A kind of ODS high temperature alloys for adding composite oxides nano particle and preparation method thereof
CN108642402A (en) * 2018-06-04 2018-10-12 湘潭大学 Novel aluminum nitride dispersion-strengtherning powder metallurgy aluminium high-speed steel and preparation method thereof
CN109112357A (en) * 2018-08-10 2019-01-01 中南大学 A kind of preparation method of titanium alloy material connection rod of automobile engine
CN110499441A (en) * 2019-09-02 2019-11-26 鞍钢股份有限公司 Nano-structure oxide dispersion strengthening vanadium alloy and preparation method thereof
CN110629100A (en) * 2019-10-29 2019-12-31 中南大学 Preparation method of oxide dispersion strengthened nickel-based high-temperature alloy
CN111172470A (en) * 2020-01-08 2020-05-19 中南大学 High-performance powder metallurgy pressed sintered type semi-high-speed steel and preparation method thereof

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003239035A (en) * 2002-02-14 2003-08-27 Mitsubishi Materials Corp Composite soft magnetic sintered material with high strength, high density, and high resistivity, and its manufacturing method
CN102071360A (en) * 2011-01-14 2011-05-25 华南理工大学 Tungsten carbide particle-enhanced iron-based powder metallurgy material and preparation method thereof
CN102251132A (en) * 2011-07-06 2011-11-23 北京科技大学 Method for preparing cobalt-based ODS (Ozone Depleting Substance) alloy through mechanochemical reaction process
CN102277525A (en) * 2011-08-23 2011-12-14 北京科技大学 Method for preparing oxide dispersion reinforced stainless steel powder and stainless steel
CN103182506A (en) * 2013-03-29 2013-07-03 华南理工大学 TiCp/M2 high-speed steel composite material and SPS (spark plasma sintering) preparation method thereof
CN103233182A (en) * 2013-06-07 2013-08-07 北京科技大学 Forming method for nanometer beta' phase element and nanometer oxide composite reinforced Fe-based ODS alloy
CN103966500B (en) * 2014-05-22 2017-11-14 北京航空航天大学 A kind of ODS high temperature alloys for adding composite oxides nano particle and preparation method thereof
CN108642402A (en) * 2018-06-04 2018-10-12 湘潭大学 Novel aluminum nitride dispersion-strengtherning powder metallurgy aluminium high-speed steel and preparation method thereof
CN109112357A (en) * 2018-08-10 2019-01-01 中南大学 A kind of preparation method of titanium alloy material connection rod of automobile engine
CN110499441A (en) * 2019-09-02 2019-11-26 鞍钢股份有限公司 Nano-structure oxide dispersion strengthening vanadium alloy and preparation method thereof
CN110629100A (en) * 2019-10-29 2019-12-31 中南大学 Preparation method of oxide dispersion strengthened nickel-based high-temperature alloy
CN111172470A (en) * 2020-01-08 2020-05-19 中南大学 High-performance powder metallurgy pressed sintered type semi-high-speed steel and preparation method thereof

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