CN112981265A - Carbon-free high-speed steel and preparation method thereof - Google Patents
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- C21D6/007—Heat treatment of ferrous alloys containing Co
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- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- 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%
- C22C33/0285—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 Cr, Co, or Ni having a minimum content higher than 5%
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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
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- 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
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
A carbon-free high-speed steel and a preparation method thereof. The carbon-free high-speed steel provided by the invention introduces iron powder to replace molybdenum powder and cobalt powder, and introduces a small amount of LaB6The tempering resistance and the red hardness of the material are improved, the transformation of austenite is delayed, the coarsening of the structure and the desolventizing of alloy elements during tempering are inhibited through the strengthening caused by the joint addition of La and B, and the red hardness and the hot hardness of the Fe-Co-Mo material are improved. Meanwhile, the preparation process is simple, the cost of raw materials is reduced, the excellent material performance of the cutter is shown, the manufactured cutter can keep high hardness under the long-time cutting action, the cutter does not stick to the cutter, and the preparation method has important application value in industry.
Description
Technical Field
The invention relates to the field of cutting titanium alloy, in particular to carbon-free high-speed steel and a preparation method thereof.
Background
The application of the titanium alloy is increasingly wide at present, the output of titanium processing materials in China is more than 55 million tons, the titanium alloy is used for aerospace, medicine, chemical engineering, war industry, automobiles, electric power and the like, the application proportion of high-end titanium materials represented by aerospace, medicine, war industry and ocean engineering is increased year by year, but in terms of the current cutter materials, due to the problems of low heat conductivity, high chemical activity and low elastic modulus of the titanium alloy, a large amount of heat generated by the titanium alloy in cutting cannot be conducted, the hardness of a cutter is reduced due to overhigh temperature, the cutting edge is rapidly abraded or cracked, the phenomenon of cutter sticking is serious, accumulated chips are easily generated, and a surface coating is taken away.
The existing titanium alloy processing cutter generally adopts hard alloy materials mainly comprising WC-CO, but carbide grows up at high temperature, and the large consumption of tungsten resources is not beneficial to the development of national conditions, so that a new material needs to be searched for replacing the hard alloy to make the cutter.
Boron plays an important role in sintering high-speed steel, such as increasing sintering activity and lowering sintering temperature, increasing hardenability of steel, and forming boride to strengthen high-speed steel. The rare earth elements have the effects of purifying grain boundaries, optimizing the distribution state of impurities in steel, improving the hot working state, optimizing impact heat, reducing abnormal growth tendency of crystal grains, improving tempering brittleness, reducing quenching cracking risk and the like. In CN107904474A inventionThe method for manufacturing the cutting tool by using the molybdenum-cobalt-boron ternary boride-based metal ceramic is provided; in the invention and creation of CN105603255A, 0.1-3.3% of LaB6 is added; the invention of CN110144512A proposes to add 0.2-20 parts of LaB6. For Fe-Co-Mo materials, a large amount of Fe element exists, so that the cost of raw materials is saved, but due to the large amount of Fe element, excessive addition of B element can cause generation of grid-shaped brittle ferroboron compounds, so that the materials are integrally brittle. However, too little B element is added, which cannot improve the hardness of the material, so that LaB needs to be researched6Influence of the addition amount of (B) on the hardness of the Fe-Co-Mo material.
Disclosure of Invention
In order to overcome the defects that the generation of grid-shaped brittle ferroboron compounds in the prior art causes the integral brittleness of materials and the hardness is lower, the invention provides the carbon-free high-speed steel and the preparation method thereof.
The carbon-free high-speed steel provided by the invention comprises 60-76% of Fe powder, 14.85-25% of Co powder, 9-15% of Mo powder and 0.05-0.15% of LaB6Powder composition; the percentage is mass percentage.
The Fe powder, the Co powder, the Mo powder and the LaB powder6The granularity of the powder is 74-100 um.
The preparation process of the carbon-free high-speed steel provided by the invention comprises the following steps:
step 1, ball milling:
the raw materials were weighed. Putting the weighed raw material powder into a ball mill, adding absolute ethyl alcohol, and carrying out ball milling on the raw material. A mixed powder was obtained.
During ball milling, the ball-material ratio is 3: 1-10: 1, the rotating speed of the ball mill is 180 r/min-220 r/min, and the ball milling time is 20-24 h.
Step 2, adding polyethylene glycol:
adding polyethylene glycol into the mixed powder obtained in the step 1; the addition amount of the polyethylene glycol is 1-2% of the mixed powder. A slurry mixture is obtained.
When polyethylene glycol is added, the polyethylene glycol is heated in a water bath to be dissolved in 100ml of absolute ethyl alcohol, and then the mixture is poured into the mixed powder and stirred uniformly.
And 3, vacuum drying:
the resulting slurry mixture was dried in a vacuum oven. A dry powder was obtained.
The heating rate of the drying box is 1 ℃/min; the drying temperature is 70-100 ℃, and the vacuum degree is-0.1 Mpa. The drying time is 20-24 h.
Step 4, mould pressing and forming:
and placing the obtained powder in a die for mechanical compression molding. A shaped block is obtained. The pressure of the compression molding is 400-450 MPa, and the pressure maintaining time is 2-3 min.
And 5, vacuum sintering:
putting the molded block obtained in the step 3 into a vacuum sintering furnace, vacuumizing the vacuum sintering furnace to 1 x 10-12 MPa, heating to 200 ℃ from room temperature at the heating rate of 5 ℃/min, and keeping the temperature for 5 min; after the heat preservation is finished, continuously heating from 200 ℃ to 400 ℃ at the speed of 5 ℃/min and preserving the heat for 10 min; continuously heating from 400 ℃ to 600 ℃ at the speed of 5 ℃/min and preserving heat for 30 min; the temperature is increased from 600 ℃ to 700 ℃ at the speed of 5 ℃/min and kept for 30 min. Continuously heating from 700 ℃ to 1000 ℃ at the speed of 5 ℃/min and preserving heat for 10 min; the temperature was raised from 1000 ℃ to 1370 ℃ at a rate of 5 ℃/min and held for 30 min. And after the heat preservation is finished, cooling the formed block body to room temperature along with the furnace, and taking out the sintered formed block body to obtain the carbon-free high-speed steel prefabricated body.
Step 6, heat treatment:
sealing the obtained carbon-free high-speed steel prefabricated body in a quartz tube in vacuum, and annealing at 1150 ℃ for 30 min; and cooling along with the furnace, and then performing oil quenching according to a conventional method. Vacuum packaging again after oil quenching, tempering in a 600 ℃ tube furnace for 60min, and air cooling. Obtaining the required carbon-free high-speed steel.
The carbon-free high-speed steel does not contain carbon element, so that the growth of carbide does not occur at high temperature, and the carbon-free high-speed steel is easy to process after solution treatment and is suitable for manufacturing cutters.
The cutter in the prior art generates a large amount of heat during processing of titanium alloy, the heat cannot be conducted, the hardness of the cutter is reduced due to too high temperature, the cutting edge is rapidly abraded or cracked, the phenomenon of cutter adhesion is serious, accumulated chips are easily generated, and a surface coating is taken away. The conventional powder metallurgy high-speed steel has the problems of poor tempering resistance, slightly low hot hardness, difficult processing after quenching and the like, and due to the existence of carbide, the carbide is also aggregated, so that the condition of sticking the cutter occurs.
Aiming at the defects in the prior art, the invention provides a carbon-free and tungsten-free material.
Compared with the invention and creation disclosed in CN107904474A, the invention introduces iron powder to replace molybdenum powder and cobalt powder, and the beneficial effects are as follows:
in the invention, a small amount of LaB is doped in FeCoMo6By the LaB of6On the premise of ensuring the hardness of the material, a small amount of LaB is introduced6To improve the tempering resistance and red hardness of the material. Meanwhile, the preparation process is simple, and due to the addition of a large amount of Fe, the raw material cost is controlled, the excellent performance of the cutter material is shown, and the preparation method has important application value in industry.
FeCoMo is a catalyst for the formation of a large number of mu-phases (Fe, Co)7Mo6As a strengthening mechanism, compared with the conventional high-speed steel, the high-speed steel has stronger tempering resistance and higher hot hardness. Therefore, the method has the advantage of being unique in the aspect of processing titanium alloy, stainless steel and high-temperature alloy. Compared with the conventional high-speed steel containing carbon, the material is easy to process after solution treatment, can keep high hardness under the action of long-time cutting, and is not sticky to a knife.
Boron plays an important role in sintering high-speed steel, such as increasing sintering activity and lowering sintering temperature, increasing hardenability of steel, and forming boride to strengthen high-speed steel. The rare earth elements have the effects of purifying grain boundaries, optimizing the distribution state of impurities in steel, improving the hot working state, optimizing impact heat, reducing abnormal growth tendency of crystal grains, improving tempering brittleness, reducing quenching cracking risk and the like. LaB6The addition of the Fe-Co-Mo alloy improves the red hardness and the hot hardness of the Fe-Co-Mo material. LaB6The addition of (A) is a reinforcement caused by the co-addition of La and BThe method is to delay the transformation of austenite, inhibit the coarsening of the structure and the desolventizing of alloy elements during tempering.
As can be seen from FIGS. 1 and 2, LaB6The addition of (a) reduces the agglomeration of the Fe-Co-Mo raw powder, making the powder diameter smaller, thereby affecting the subsequent sintering process. As can be seen from FIGS. 3 and 4, LaB6The addition of (b) results in a higher densification of the sintered material.
Drawings
FIG. 1 is 0.1% LaB6Electron micrograph of Fe-Co-Mo powder.
FIG. 2 is 0% LaB6Electron micrograph of Fe-Co-Mo powder.
FIG. 3 is 0% LaB6Electron microscope image of the Fe-Co-Mo sintered material.
FIG. 4 is 0.1% LaB6Electron microscope image of the Fe-Co-Mo sintered material.
Fig. 5 is a flow chart of the present invention.
Detailed Description
The invention relates to a carbon-free high-speed steel and a preparation method thereof, and technical characteristics of the carbon-free high-speed steel are described through six specific embodiments. The preparation processes in the embodiments are the same, and the process parameters are different.
The carbon-free high-speed steel is prepared from 60-76% of Fe powder, 14.85-24.95% of Co powder, 9-15% of Mo powder and 0.05-0.15% of LaB6Powder composition; the percentage is mass percentage.
The Fe powder, the Co powder, the Mo powder and the LaB powder6The purity of the powder is 99.9 percent, the purity is in mass percent, and the granularity is 74-100 um.
Table 1: components of the examples
The invention provides a specific process for preparing the carbon-free high-speed steel, which comprises the following steps:
step 1, ball milling:
the raw materials were weighed. Putting the weighed raw material powder into a ball mill, adding absolute ethyl alcohol, and carrying out ball milling on the raw material. The ball-material ratio is 3: 1-10: 1, the rotating speed of the ball mill is 180 r/min-220 r/min, and the ball milling time is 20-24 h. A mixed powder was obtained.
TABLE 2 Process parameters for step 1 in the examples
Step 2, adding polyethylene glycol:
adding polyethylene glycol into the mixed powder obtained in the step 1; the addition amount of the polyethylene glycol is 1-2% of the mixed powder. The adding method is that the polyethylene glycol is heated in water bath and dissolved in 100ml of absolute ethyl alcohol, then the mixture is poured into the mixed powder, and then the mixture is stirred uniformly. A slurry mixture is obtained.
Table 3 process parameters for step 2 in the examples:
and 3, vacuum drying:
and (3) drying the slurry mixture obtained in the step (2) in a vacuum drying oven for 20-24 hours at the drying temperature of 70-100 ℃ under the vacuum degree of-0.1 Mpa. The heating rate of the drying box is 1 ℃/min. Preferably 24 hours and 80 ℃. A dry powder was obtained.
TABLE 4 Process parameters for step 3 in the examples
Step 4, mould pressing and forming:
and (4) placing the powder obtained in the step (3) into a die for mechanical compression molding. The pressure of the compression molding is 400-450 MPa, and the pressure maintaining time is 2-3 min. A shaped block is obtained.
TABLE 5 Process parameters for step 4 in the examples
And 5, vacuum sintering:
putting the molded block obtained in the step 3 into a vacuum sintering furnace, vacuumizing the vacuum sintering furnace to 1 x 10-12 MPa, heating to 200 ℃ from room temperature at the heating rate of 5 ℃/min, and keeping the temperature for 5 min; after the heat preservation is finished, continuously heating from 200 ℃ to 400 ℃ at the speed of 5 ℃/min and preserving the heat for 10 min; continuously heating from 400 ℃ to 600 ℃ at the speed of 5 ℃/min and preserving heat for 30 min; the temperature is increased from 600 ℃ to 700 ℃ at the speed of 5 ℃/min and kept for 30 min. Continuously heating from 700 ℃ to 1000 ℃ at the speed of 5 ℃/min and preserving heat for 10 min; the temperature was raised from 1000 ℃ to 1370 ℃ at a rate of 5 ℃/min and held for 30 min. And after the heat preservation is finished, cooling the formed block body to room temperature along with the furnace, and taking out the sintered formed block body to obtain the carbon-free high-speed steel prefabricated body.
Step 6, heat treatment:
and performing standard metallographic treatment on the obtained carbon-free high-speed steel prefabricated body after linear cutting through heat treatment. Specifically, the carbon-free high-speed steel prefabricated body is sealed in a quartz tube in vacuum, and is annealed for 30min at 1150 ℃; and cooling along with the furnace, and then performing oil quenching according to a conventional method. Vacuum packaging again after oil quenching, tempering in a 600 ℃ tube furnace for 60min, and air cooling. Obtaining the required carbon-free high-speed steel.
The hardness of the carbon-free high-speed steel obtained in each example of the present invention was tested. The test results are shown in table 6:
table 6: with the addition of LaB6Hardness value of carbon-free high-speed steel
Claims (8)
1. The carbon-free high-speed steel is characterized by comprising 60-76% of Fe powder, 14.85-25% of Co powder, 9-15% of Mo powder and 0.05-0.15% of LaB6Powder composition; the percentage is mass percentage.
2. The carbon-free high-speed steel according to claim 1, wherein the Fe powder, Co powder, Mo powder and LaB powder6The granularity of the powder is 74-100 um.
3. A method for preparing the carbon-free high-speed steel according to claim 1, which comprises the following specific steps:
step 1, ball milling:
weighing raw materials; putting the weighed raw material powder into a ball mill, adding absolute ethyl alcohol, and carrying out ball milling on the raw material; obtaining mixed powder;
step 2, adding polyethylene glycol:
adding polyethylene glycol into the mixed powder obtained in the step 1; the addition amount of the polyethylene glycol is 1-2% of the mixed powder; obtaining a slurry mixture;
step 3, vacuum drying;
putting the slurry mixture obtained in the step 2 into a vacuum drying oven for drying; obtaining a dry powder;
step 4, mould pressing and forming:
placing the obtained powder in a die for mechanical compression molding; obtaining a molded block;
and 5, vacuum sintering:
putting the molded block obtained in the step 3 into a vacuum sintering furnace, vacuumizing the vacuum sintering furnace to 1 x 10-12 MPa, heating to 200 ℃ from room temperature at the heating rate of 5 ℃/min, and keeping the temperature for 5 min; after the heat preservation is finished, continuously heating from 200 ℃ to 400 ℃ at the speed of 5 ℃/min and preserving the heat for 10 min; continuously heating from 400 ℃ to 600 ℃ at the speed of 5 ℃/min and preserving heat for 30 min; continuously heating from 600 ℃ to 700 ℃ at the speed of 5 ℃/min and preserving heat for 30 min; continuously heating from 700 ℃ to 1000 ℃ at the speed of 5 ℃/min and preserving heat for 10 min; heating from 1000 deg.C to 1370 deg.C at a rate of 5 deg.C/min and holding for 30 min; after the heat preservation is finished, cooling the formed block body to room temperature along with the furnace, and taking out the sintered formed block body to obtain a carbon-free high-speed steel prefabricated body;
step 6, heat treatment:
sealing the obtained carbon-free high-speed steel prefabricated body in a quartz tube in vacuum, and annealing at 1150 ℃ for 30 min; cooling with the furnace and then performing oil quenching according to a conventional method; vacuum packaging again after oil quenching, tempering in a 600 ℃ tube furnace for 60min, and air cooling; obtaining the required carbon-free high-speed steel.
4. The method for preparing the carbon-free high-speed steel according to claim 3, wherein the ball-to-material ratio during ball milling is 3: 1-10: 1, the rotating speed of the ball mill is 180 r/min-220 r/min, and the ball milling time is 20-24 h.
5. The method for preparing carbon-free high-speed steel according to claim 3, wherein the polyethylene glycol is added by dissolving the polyethylene glycol in 100ml of absolute ethanol in a water bath, pouring the solution into the mixed powder, and stirring the solution uniformly.
6. The method for preparing the carbon-free high-speed steel according to claim 3, wherein the drying temperature is 70 to 100 ℃ and the vacuum degree is-0.1 MPa during the vacuum drying; the drying time is 20-24 h.
7. The method for manufacturing a carbon-free high-speed steel according to claim 6, wherein the temperature rise rate of the drying oven at the time of vacuum drying is 1 ℃/min.
8. The method for preparing carbon-free high-speed steel according to claim 3, wherein the pressure of the press forming is 400 to 450MPa, and the dwell time is 2 to 3 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114561596A (en) * | 2022-01-20 | 2022-05-31 | 长沙市萨普新材料有限公司 | Carbon-free high-speed steel piercing plug with strong hardening effect through intermetallic compounds and preparation method thereof |
| CN114561588A (en) * | 2022-01-20 | 2022-05-31 | 长沙市萨普新材料有限公司 | High-boron high-silicon powder high-speed steel and preparation and application of precursor powder thereof |
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| CN103741049A (en) * | 2014-01-21 | 2014-04-23 | 湘潭大学 | Iron-based abrasion-resistant alloy based on Laves phase strengthening and preparation method thereof |
| CN110257688A (en) * | 2019-06-28 | 2019-09-20 | 鞍钢股份有限公司 | One kind Powder High-speed Steels containing boride and preparation method thereof |
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| CN114561596A (en) * | 2022-01-20 | 2022-05-31 | 长沙市萨普新材料有限公司 | Carbon-free high-speed steel piercing plug with strong hardening effect through intermetallic compounds and preparation method thereof |
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