CN113528918A - Low-cobalt high-strength hard alloy and preparation method thereof - Google Patents
Low-cobalt high-strength hard alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
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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
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Abstract
The invention relates to the technical field of hard alloy, and particularly discloses a low-cobalt high-strength hard alloy which comprises the following raw materials in parts by weight: composite hard phase: 93.5-94.2 parts; bonding phase: 5.8-6.5 parts; the bonding phase is cobalt; the composite hard phase comprises tungsten carbide A with the Fisher grain size of 3.10-3.60 mu m. The preparation method comprises the following steps: preparing materials: filling the composite hard phase and the bonding phase in parts by weight into a ball milling cylinder; ball milling: adding hexane or alcohol, paraffin and stearic acid into the ball milling cylinder, covering the ball milling cylinder, starting a ball mill, and carrying out ball milling for 24-60 hours; preparing mixed granules, namely filtering and discharging slurry, and performing spray drying granulation on the slurry by using a spray tower to obtain the mixed granules required by pressing; pressing, namely pressing and molding the mixed granules by a die and a press machine to obtain a required hard alloy semi-finished blank; sintering, namely putting the hard alloy semi-finished blank into a pressure sintering furnace for high-temperature sintering; the preparation is completed. The invention has higher bending strength and toughness.
Description
Technical Field
The invention relates to the technical field of toughening and strengthening of a cemented carbide binding phase, in particular to a low-cobalt high-strength cemented carbide and a preparation method thereof.
Background
The requirements for hard alloy materials for high and low wind pressure down-the-hole drilling teeth for down-the-hole drilling machines, drill bit column teeth for light rock drills, drill teeth for full hydraulic drill trucks and the like are higher and higher, the cobalt content of the hard alloy in the application field is lower at present, and the cobalt content is about 5.8-8.5%. The working condition of the tooth is complex, and the tooth bears impact and rotary wear, and the tooth bears huge shear stress and impact load under the action of stress during the working of the tooth, so that the hard alloy material needs to have higher bending strength and toughness and higher hardness to meet the service life requirement of the working condition.
Under the condition that the cobalt content in the tungsten carbide-cobalt hard alloy is determined, the method for improving the strength of the hard alloy material comprises the following steps: the grain size of hard phase tungsten carbide in the alloy is reduced, the cobalt magnetism of the hard alloy is reduced, the solid solubility of W in a binding phase in the hard alloy is increased, the sub-grain structure defect of the tungsten carbide is reduced, and the like; the method for enhancing the toughness of the steel comprises the following steps: the grain size of hard phase tungsten carbide in the hard alloy is increased, the grain size composition of the tungsten carbide is improved, the morphology of the tungsten carbide is improved, the sub-grain structure defects of the tungsten carbide are reduced, and the like. Some patents CN101008064A "a whisker toughened tungsten carbide-Co based hard alloy material and a preparation method thereof", CN102912205A "a Sr2Nb2O7 toughened tungsten carbide-8% Co hard alloy composite material and a preparation method thereof", and CN1038822758 "a toughened hard alloy and a preparation method thereof" provide some methods for toughening the hard alloy, so as to improve the service life of the hard alloy.
In the current market, most brands show the phenomena of no wear resistance, broken teeth and the like when used in some special mines, and due to the high cobalt content, certain economic loss is caused to customers using tools, and the working efficiency and the progress of construction engineering are reduced.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-cobalt high-strength hard alloy and a preparation method thereof, and the low-cobalt high-strength hard alloy has higher bending strength and toughness.
The technical problem to be solved by the invention is as follows:
a low-cobalt high-strength hard alloy, which comprises the following composite hard phases: 93.5-94.2 parts;
bonding phase: 5.8-6.5 parts;
the bonding phase is cobalt;
the composite hard phase comprises tungsten carbide A with the Fisher grain size of 3.10-3.60 mu m.
In some possible embodiments, the composite hard phase further comprises tungsten carbide B having a fisher particle size of 2.50 μm to 3.00 μm; the weight ratio of the tungsten carbide A to the tungsten carbide B is 2.0-2.34: 1.
On the other hand, the preparation method of the low-cobalt high-strength hard alloy specifically comprises the following steps:
preparing materials: filling the composite hard phase and the bonding phase in parts by weight into a ball milling cylinder;
ball milling: adding hexane or alcohol, paraffin and stearic acid into the ball milling cylinder, covering the ball milling cylinder, starting a ball mill, and carrying out ball milling for 24-60 hours;
preparing mixed granules, namely filtering and discharging slurry, and performing spray drying granulation on the slurry by using a spray tower to obtain the mixed granules required by pressing;
pressing, namely pressing and molding the mixed granules by a die and a press machine to obtain a required hard alloy semi-finished blank;
sintering, namely putting the hard alloy semi-finished blank into a pressure sintering furnace for high-temperature sintering;
completing the preparation:
in some possible embodiments, the pressing pressure is 180 to 200MPa during the pressing process.
In some possible embodiments, in the sintering process, the sintering temperature is 1410-1470 ℃, the heat preservation time is 90 minutes, and argon is added for pressure sintering at high temperature, wherein the pressure is 4-5 MPa.
In some possible embodiments, the paraffin wax is 2 parts, stearic acid is 0.05 parts, and hexane or alcohol is 400 ml/kg during ball milling.
Compared with the prior art, the invention has the beneficial effects that:
the invention has better breaking strength and wear resistance;
the invention adopts high-quality tungsten carbide which is reduced at high temperature and carbonized at high temperature as raw materials, improves the strength of the alloy by controlling the cobalt magnetism of the alloy, and meets the requirements of some special working conditions;
the magnetic range of the alloy cobalt is controlled, the bending strength of the prepared tungsten-cobalt non-uniform structure hard alloy with 5.8-6.5% of cobalt is more than or equal to 2800MPa, the hardness is HRA 89.8-90.8, and the metallographic phase is A02B00C00E 00;
according to the invention, tungsten carbide fine powder is dissolved and separated out in the sintering process through the high-temperature sintering temperature, so that crystal grains grow up along a certain direction to form strip-shaped and flaky crystal grains, and the bonding strength and toughness of tungsten carbide and a bonding phase are improved;
the invention controls the solubility of tungsten in cobalt phase by controlling the cobalt magnetic range of the alloy, so as to carry out solid solution strengthening on the alloy to meet the performance requirement of the alloy.
Drawings
FIG. 1 is a metallographic picture taken in accordance with example 1 of the present invention;
FIG. 2 is a metallographic picture according to example 2 of the present invention;
FIG. 3 is a metallographic picture according to example 3 of the present invention;
FIG. 4 is a metallographic picture taken in accordance with example 4 of the present invention;
FIG. 5 is a metallographic picture taken in accordance with example 5 of the present invention;
FIG. 6 is a metallographic picture taken in accordance with example 6 of the present invention;
FIG. 7 is a metallographic picture taken in accordance with example 7 of the present invention;
Detailed Description
To make the purpose, technical solutions and advantages of the present application clearer, the technical solutions in the present application will be clearly and completely described below with reference to the drawings in the present application, and it is obvious that the described embodiments are some, but not all embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The invention will be further explained with reference to the drawings and examples, which are illustrated in figures 1-7,
a low-cobalt high-strength hard alloy, which comprises the following composite hard phases: 93.5-94.2 parts;
bonding phase: 5.8-6.5 parts;
the bonding phase is cobalt;
the composite hard phase comprises tungsten carbide A with the Fisher grain size of 3.10-3.60 mu m.
In some possible embodiments, the composite hard phase further comprises tungsten carbide B having a fisher particle size of 2.50 μm to 3.00 μm; the weight ratio of the tungsten carbide A to the tungsten carbide B is 2.0-2.34: 1.
On the other hand, the preparation method of the low-cobalt high-strength hard alloy specifically comprises the following steps:
preparing materials: filling the composite hard phase and the bonding phase in parts by weight into a ball milling cylinder;
ball milling: adding hexane or alcohol, paraffin and stearic acid into the ball milling cylinder, covering the ball milling cylinder, starting a ball mill, and carrying out ball milling for 24-60 hours;
preparing mixed granules, namely filtering and discharging slurry, and performing spray drying granulation on the slurry by using a spray tower to obtain the mixed granules required by pressing;
pressing, namely pressing and molding the mixed granules by a die and a press machine to obtain a required hard alloy semi-finished blank;
sintering, namely putting the hard alloy semi-finished blank into a pressure sintering furnace for high-temperature sintering;
completing the preparation:
in some possible embodiments, the pressing pressure is 180 to 200MPa during the pressing process.
In some possible embodiments, in the sintering process, the sintering temperature is 1410-1470 ℃, the heat preservation time is 90 minutes, and argon is added for pressure sintering at high temperature, wherein the pressure is 4-5 MPa.
In some possible embodiments, the paraffin wax is 2 parts, stearic acid is 0.05 parts, and hexane or alcohol is 400 ml/kg during ball milling.
Example 1:
in this embodiment, the specific ratio of the high-strength cemented carbide is as follows: 94 parts of high-temperature reduced and high-temperature carbonized tungsten carbide with the Fisher particle size of 3.10-3.60 mu m and 6 parts of cobalt powder, wherein the total amount is 100 parts; then, 2 parts of paraffin, 0.05 part of stearic acid and 400 ml/kg of hexane or alcohol are additionally added.
The preparation method comprises the following specific steps:
the method comprises the following steps: preparing materials;
tungsten carbide A with the Fisher particle size of 3.10-3.60 mu m and cobalt powder are weighed according to the weight ratio and are loaded into a ball mill cylinder, wherein the total carbon of the tungsten carbide is adjusted by tungsten powder or carbon black, and the ratio of the burdening balls to the material is 4: 1.
step two: ball milling;
adding 400 ml/kg of hexane or alcohol, 2 parts of paraffin and 0.05 part of stearic acid into the ball milling barrel, covering the ball milling barrel, starting the ball mill to perform rolling ball milling, stopping ball milling for 36 hours, adding cobalt powder, performing ball milling for 24 hours, stopping ball milling, and discharging, wherein the diameter of hard alloy balls subjected to rolling ball milling is 6.35 millimeters YG6 hard alloy balls.
Step three: preparing mixed granules;
and (4) filtering the ball-milling time to discharge slurry, and performing spray drying granulation on the slurry by a spray tower to obtain mixed granules required by pressing.
Step four: pressing;
and pressing and molding the mixed granules by a die and a press machine, wherein the pressing pressure is 180-200 MPa, and thus the required hard alloy semi-finished blank is prepared.
Step five: sintering;
and (2) putting the prepared hard alloy semi-finished blank into a pressure sintering furnace, removing the forming agent in a hydrogen carrier gas dewaxing-pressure sintering integrated furnace, sintering at the sintering temperature of 1390-1460 ℃ for 90 minutes, adding argon gas during high-temperature sintering, and performing pressure sintering at the pressure of 4-5 MPa.
The preparation is completed.
The embodiment 2-the embodiment 4 adopt the same raw materials as the embodiment 1, and the preparation is realized by controlling different sintering temperatures and the relative cobalt and cobalt magnetic percentages;
examples 2-4 differ from example 1 in the sintering temperature and the magnetic percentage of cobalt in the relative proportion, the green bodies were inspected after the preparation, and fig. 1-4 are metallographic pictures of physical properties such as
Table 1 shows:
TABLE 1
As can be seen from the data in table 1, in examples 1 to 4, the same tungsten carbide has the same content as cobalt, and the mixture obtained by ball milling has the effect of cobalt magnetism on the alloy performance at different sintering temperatures, and in the case of low cobalt magnetism (in the case of no decarburization), tungsten in the alloy plays a role of solid solution strengthening, so that the strength of the alloy is improved, and the fracture toughness of the alloy performance is also affected differently. However, as the cobalt magnetism increases, that is, the carbon content in the alloy increases, the W in the alloy is reduced in melting and even carburization occurs, which affects the strength and other properties of the alloy. Example 4 carburization of the alloy after sintering was caused by the difference in the residual carbon in the alloy due to the difference in the dewaxing process in sintering, and the strength of the alloy became low and did not meet the design requirements.
Example 5:
in this embodiment, the specific ratio of the high-strength cemented carbide is as follows: 65.8 parts of high-temperature reduced and high-temperature carbonized tungsten carbide with the Fisher granularity of 3.10-3.60 mu m, 28.2 parts of high-temperature reduced and high-temperature carbonized tungsten carbide with the Fisher granularity of 2.50-3.00 mu m and 6 parts of cobalt powder, wherein the total amount is 100 parts. Then, 2 parts of paraffin, 0.05 part of stearic acid and 400 ml/kg of hexane or alcohol are additionally added.
The preparation method comprises the following specific steps:
the method comprises the following steps: preparing materials;
tungsten carbide A with the Fisher particle size of 3.10-3.60 mu m, tungsten carbide B with the Fisher particle size of 2.50-3.00 mu m and cobalt powder are weighed according to the weight ratio and are filled into a ball mill cylinder, wherein the total carbon in the tungsten carbide A and the tungsten carbide B is adjusted by tungsten powder or carbon black, and the ratio of the materials in the material mixing ball to the materials is 4: 1.
step two: ball milling;
adding 400 ml/kg of hexane or alcohol, 2 parts of paraffin and 0.05 part of stearic acid into the ball milling barrel, covering the ball milling barrel, starting the ball mill to perform rolling ball milling, stopping ball milling for 36 hours, adding cobalt powder, performing ball milling for 24 hours, stopping ball milling, and discharging, wherein the diameter of hard alloy balls subjected to rolling ball milling is 6.35 millimeters.
Step three: preparing mixed granules;
and (4) filtering the ball-milling time to discharge slurry, and performing spray drying granulation on the slurry by a spray tower to obtain mixed granules required by pressing.
Step four: pressing;
and pressing and molding the mixed granules by a die and a press machine, wherein the pressing pressure is 180-200 MPa, and thus the required hard alloy semi-finished blank is prepared.
Step five, sintering;
and (2) putting the prepared hard alloy semi-finished blank into a pressure sintering furnace, removing the forming agent in a hydrogen carrier gas dewaxing-pressure sintering integrated furnace, sintering at the sintering temperature of 1390-1460 ℃ for 90 minutes, adding argon gas during high-temperature sintering, and performing pressure sintering at the pressure of 4-5 MPa.
The preparation is completed.
Examples 6 and 7 adopt the method of the above example 5 to control different sintering temperatures and relative cobalt magnetic percentages to realize preparation;
the difference between the examples 6 and 7 and the example 5 lies in the difference between the sintering temperature and the magnetic percentage of the cobalt and cobalt which are relatively matched, the green body is inspected after the preparation is completed, and the metallographic pictures of the examples 5 to 7 in sequence are shown in the figures 5 to 7, and the physical properties of the metallographic pictures are shown in the table 2:
TABLE 2
Two kinds of tungsten carbide were used in example 6, one kind of tungsten carbide was used in example 1, and they were sintered at different sintering temperatures, respectively, and the properties of the alloy showed differences when the alloy was carburized due to the influence of dewaxing, wherein the greatest influence was the strength of the alloy, which was greatly reduced.
Wherein, the relative cobalt magnetic percentage is the percentage of cobalt magnetic of the alloy divided by the percentage of cobalt in the mixture; as can be seen from tables 1 and 2, the activity of the tungsten carbide fine powder is increased by ball milling for a long time, and the tungsten carbide fine powder is dissolved and precipitated by high-temperature sintering, so that grains grow in a certain direction to form long flaky grains, thereby improving the bonding strength and toughness of the tungsten carbide and the binder phase. Meanwhile, the solubility of the cobalt in a cobalt phase is controlled by controlling the cobalt magnetic range of the alloy to perform solid solution strengthening on the alloy so as to meet the performance requirement of the alloy. The prepared alloy has the cobalt content of 5.8-6.5%, the hardness HRA of 89.8-90.8, the bending strength of more than or equal to 2800MPa, the fracture toughness of more than or equal to 10.3MPa and the metallographic phase A02B00C00E00, and the percentage of the relative cobalt to the magnetic alloy is 79-96% calculated according to the cobalt content of the ingredients.
The foregoing detailed description of the embodiments of the present application has been presented, and specific examples have been applied in the present application to explain the principles and implementations of the present application, and the above description of the embodiments is only used to help understand the method and the core ideas of the present application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (6)
1. A low-cobalt high-strength hard alloy is characterized in that: the composite material comprises the following raw materials in parts by weight:
composite hard phase: 93.5-94.2 parts;
bonding phase: 5.8-6.5 parts;
the bonding phase is cobalt;
the composite hard phase comprises tungsten carbide A with the Fisher grain size of 3.10-3.60 mu m.
2. A low cobalt high strength cemented carbide according to claim 1 wherein: the composite hard phase also comprises tungsten carbide B with the Fisher particle size of 2.50-3.00 mu m; the weight ratio of the tungsten carbide A to the tungsten carbide B is 2.0-2.34: 1.
3. The method for preparing a low-cobalt high-strength cemented carbide according to claim 1 or 2, characterized in that: the method specifically comprises the following steps:
preparing materials: filling the composite hard phase and the bonding phase in parts by weight into a ball milling cylinder;
ball milling: adding hexane or alcohol, paraffin and stearic acid into the ball milling cylinder, covering the ball milling cylinder, starting a ball mill, and carrying out ball milling for 24-60 hours;
preparing mixed granules, namely filtering and discharging slurry, and performing spray drying granulation on the slurry by using a spray tower to obtain the mixed granules required by pressing;
pressing, namely pressing and molding the mixed granules by a die and a press machine to obtain a required hard alloy semi-finished blank;
sintering, namely putting the hard alloy semi-finished blank into a pressure sintering furnace for high-temperature sintering;
the preparation is completed.
4. The method for preparing the cemented carbide with the mixed crystal microstructure according to claim 3, wherein: in the pressing process, the pressing pressure is 180-200 MPa.
5. The method for preparing the cemented carbide with the mixed crystal microstructure according to claim 4, wherein: in the sintering process, the sintering temperature is 1390-1470 ℃, the heat preservation time is 90 minutes, argon is added during high-temperature sintering for pressure sintering, and the pressure is 4-5 MPa.
6. The method for preparing the cemented carbide with the mixed crystal microstructure according to claim 3, wherein: 2 parts of paraffin, 0.05 part of stearic acid and 400 ml/kg of hexane or alcohol.
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| CN114855018A (en) * | 2022-04-28 | 2022-08-05 | 晋城鸿智纳米光机电研究院有限公司 | Preparation method of nano hard alloy |
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| JP2016160500A (en) * | 2015-03-03 | 2016-09-05 | 日立金属株式会社 | Wc-based cemented carbide and production method therefor |
| CN105132779A (en) * | 2015-07-31 | 2015-12-09 | 株洲硬质合金集团有限公司 | Tungsten-carbide-based cemented carbide and preparation method thereof |
| CN107585768A (en) * | 2017-10-24 | 2018-01-16 | 株洲硬质合金集团有限公司 | A kind of method that oxidation-reduction method prepares superfine tungsten carbide powder |
| CN108048723A (en) * | 2017-11-17 | 2018-05-18 | 北京有色金属研究总院 | A kind of wide size distribution hard alloy and preparation method thereof |
| CN109487142A (en) * | 2018-12-03 | 2019-03-19 | 株洲硬质合金集团有限公司 | A kind of thermal crack resistant mixed crystal hard alloy and preparation method thereof |
| CN111187960A (en) * | 2019-12-31 | 2020-05-22 | 株洲硬质合金集团有限公司 | Double-crystal hard alloy and preparation method thereof |
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| CN114855018A (en) * | 2022-04-28 | 2022-08-05 | 晋城鸿智纳米光机电研究院有限公司 | Preparation method of nano hard alloy |
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