CN113024254B - High-wear-resistance powder metallurgy material and preparation method thereof - Google Patents
High-wear-resistance powder metallurgy material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of powder metallurgy, and particularly relates to a high-wear-resistance powder metallurgy material and a preparation method thereof. The product developed by the invention comprises aluminum nitride, silicon carbide and graphene; the aluminum nitride, the silicon nitride and the silicon carbide are dispersed among the graphene layers; and the adjacent lamellar structures in the graphene molecular structure are bridged by silicon carbide. During preparation, graphene oxide is dispersed in absolute ethyl alcohol, organic silicon, organic aluminum and fatty acid are added, and after heating reflux reaction, filtering, washing and drying are carried out to obtain a precursor; and (3) slowly heating the precursor to 1600-1800 ℃ in a nitrogen atmosphere, carrying out heat preservation reaction for 6-8h, cooling, and discharging to obtain the product. The product obtained by the invention has excellent wear resistance.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy. More particularly, relates to a high wear-resistant powder metallurgy material and a preparation method thereof.
Background
The aluminum-silicon powder metallurgy alloy has high wear resistance, high strength, good heat resistance and low thermal expansion coefficient. Hypereutectic aluminum-silicon alloys produced by conventional casting tend to have coarse, blocky or plate-like primary crystals which degrade the mechanical properties of the alloy, thus severely limiting the silicon content. The powder metallurgy method can avoid the problems, the size of primary crystal silicon can be refined by using a powder atomization technology and a rapid solidification technology, and the solid solubility of silicon in aluminum can be enlarged (increased from 1.95at percent to 10.16at percent). Due to the advantages, the powder metallurgy aluminum-silicon alloy is generally concerned by researchers in various countries.
The SiCp/Al composite material has high strength and rigidity, excellent wear resistance, good high temperature resistance and low thermal expansion coefficient, combines the high strength, high wear resistance and excellent high temperature performance of silicon carbide, and inherits the toughness and ductility of aluminum. Because the manufacturing process has simple equipment and low cost, the composite material can be produced in batch and can be manufactured into various parts and sections with complex shapes by using the conventional metal processing methods of casting, powder metallurgy, forging, welding and the like, and the composite material becomes one of the main directions of the research and development of the current metal matrix composite material. The method has great application potential in the fields of aerospace and military and the industries of automobiles, electronic instruments and the like.
Due to Al inherent to the surface of aluminum powder2O3The oxide film cannot be formed with a reducing gas (e.g. H)2) Reducing, high melting point and compact. The oxide film hinders diffusion of aluminum and other alloy elements, making sintering of a green compact made of the mixed element powder rather difficult. The sintering problem is finally solved by using a A1-50Fe master alloy, which is easily broken into fine powder. The addition of aluminum-based powder metallurgy in this manner virtually solves the problem of surface oxidation barrier at all. However, the bonding interface of the silicon carbide particles with the aluminum melt is not good, and it is difficult to increase the content of the particlesAmount and control of uniformity of particle distribution.
Disclosure of Invention
The invention aims to overcome the defects and defects that the actual enhancement of the wear resistance of a product cannot achieve the expected effect due to the fact that the interface between an added reinforcement such as silicon carbide particles and an aluminum melt is not good in the preparation process of the conventional aluminum-based wear-resistant material, and provides a high-wear-resistant powder metallurgy material and a preparation method thereof.
The invention aims to provide a high wear-resistant powder metallurgy material.
The invention also aims to provide a preparation method of the high wear-resistant powder metallurgy material.
The above purpose of the invention is realized by the following technical scheme:
a high wear-resistant powder metallurgy material comprises aluminum nitride, silicon carbide and graphene;
the aluminum nitride, the silicon nitride and the silicon carbide are dispersed among the graphene layers;
and adjacent lamellar structures in the graphene molecular structure are bridged by silicon carbide.
Further, the nano iron powder and the calcium fluoride are at least partially coated by silicon carbide.
A preparation method of a high wear-resistant powder metallurgy material comprises the following specific preparation steps:
preparing a precursor:
dispersing graphene oxide in absolute ethyl alcohol, adding organic silicon, organic aluminum and fatty acid, heating, refluxing, reacting, filtering, washing and drying to obtain a precursor;
pressing:
cold-pressing and molding the precursor to obtain a blank;
and (3) sintering:
and (3) slowly heating the blank body to 1600-1800 ℃ in a nitrogen atmosphere, carrying out heat preservation reaction for 6-8h, cooling, and discharging to obtain the product.
Further, the specific preparation steps further comprise:
in the preparation process of the precursor, before heating reflux reaction, nano iron powder and calcium fluoride are added.
Further, the specific preparation steps further comprise:
in the preparation process of the precursor, ammonium nitrate with the mass of 3-5% of that of the graphene oxide is added before the heating reflux reaction.
Further, the slow temperature rise is as follows: heating to 800-1000 ℃ at the rate of 5-10 ℃/min, and heating to 1600-1800 ℃ at the rate of 0.3-0.5 ℃/min.
Further, the silicone is selected from: any one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
Further, the organic aluminum is selected from any one of aluminum isopropoxide, aluminum ethoxide and trimethylaluminum.
Further, the fatty acid is selected from: any one of linoleic acid, linolenic acid, arachidonic acid and stearic acid.
The beneficial technical effects are as follows:
(1) in the technical scheme, organosilicon and organic aluminum are used as dehydrating agents in the preparation process of the precursor to absorb water molecules generated by an esterification reaction of anhydrous ethanol and fatty acid in the heating reflux process, at the moment, the generation rate of the water molecules is relatively low, and the water molecules are uniformly generated at each corner in the system, so that the uniformity of the hydrolysis reaction of the organosilicon and the organic aluminum can be ensured, a hydrolysate can be quickly adsorbed and fixed by graphene oxide and is embedded into an inter-graphene oxide layer structure, and because carboxyl exists in the edge region of the graphene oxide and hydroxyl and epoxy exist in a conjugate region, polar groups can generate a strong hydrogen bond action with the hydrolysate of the organosilicon and the organic aluminum, so that a physical cross-linked network structure is formed in the precursor, and in the subsequent slow heating process, the dehydration reaction of the precursor and the dehydration process firstly occur, the dissipation of water molecules can widen the distance between graphene oxide layers to a certain degree, and nitrogen enters the interior of the graphene oxide layers to carry out high-temperature reaction more conveniently, so that aluminum nitride, silicon nitride and silicon carbide are generated by reaction at higher temperature, and the defects of graphene oxide can be repaired and reduced in the reaction process of the products; the wear-resistant powder metallurgy material taking graphene as a base and aluminum nitride, silicon nitride and silicon carbide as reinforcing phases is formed, silicon carbide is generated substantially in the process that silicon oxide utilizes carbon elements of the graphene to form Si-C chemical bonding, and when crystals grow up, graphene lamellar structures at two ends are bridged, so that the structural stability of the wear-resistant material is effectively improved, and the overall wear resistance is further improved;
(2) according to the technical scheme, the organic silicon and the organic aluminum are compounded to serve as the dehydrating agent and the hydrolysis system, so that due to the difference between the hydrolysis rate of the organic silicon and the hydrolysis rate of the organic aluminum, the hydrolysis product molecular size of the organic silicon and the hydrolysis product molecular size of the organic aluminum, an individual with a smaller molecule can carry out crystal form repair on the individual with a smaller molecule to a certain extent, and the defect that the wear resistance is reduced due to the product defect caused by the crystal defect of a precursor of the hydrolysis product is avoided;
(3) in addition, because the addition of the nanometer iron powder and the calcium fluoride is actually added in the preparation process of the precursor, the silicon carbide crystal grows gradually around the catalytic system and is coated in the precursor, the silicon carbide crystal and the precursor are used as reinforcements in the sintering process, the physical structure stability of the silicon carbide crystal is improved, and the technical contribution to the structure stability of the product is finally made;
(4) according to the technical scheme, a small amount of ammonium nitrate is further introduced, in the preparation process of the product, the ammonium nitrate can be violently decomposed at a relatively low temperature, and the precursor can be rapidly refined by the gas generated by decomposition, so that high-temperature sintering can be more sufficient and easier to perform, and the reduction of wear resistance caused by non-uniformity among components is avoided.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
Preparing a precursor:
according to the weight parts, 20 parts of graphene oxide, 20 parts of organic aluminum, 15 parts of organic silicon, 400 parts of absolute ethyl alcohol, 40 parts of fatty acid, 1 part of nano iron powder, 2 parts of calcium fluoride and 3% ammonium nitrate of graphene oxide are taken in sequence;
firstly, mixing graphene oxide and absolute ethyl alcohol, pouring the mixture into a reactor, and carrying out ultrasonic dispersion for 30min at the temperature of 55 ℃ and the ultrasonic frequency of 60kHz to obtain dispersion liquid;
sequentially adding organic silicon, organic aluminum, fatty acid, nano iron powder, calcium fluoride and ammonium nitrate into the dispersion liquid, heating and refluxing for 8 hours at the temperature of 75 ℃, stopping the reaction, filtering, collecting a filter cake, washing the filter cake with absolute ethyl alcohol for 3 times, washing the filter cake with deionized water for 2 times, transferring the filter cake washed with the deionized water into an oven, and drying at the temperature of 100 ℃ to constant weight to obtain a precursor;
pressing:
pressing the precursor under the pressure of 400MPa for 5min to obtain a blank;
and (3) sintering:
transferring the obtained blank into a tubular furnace, introducing nitrogen into the tubular furnace at the speed of 100mL/min, heating to 800 ℃ at the speed of 5 ℃/min under the protection of the nitrogen, heating to 1600 ℃ at the speed of 0.3 ℃/min, carrying out heat preservation reaction for 6h, stopping heating, cooling to room temperature along with the furnace, and discharging to obtain the high-wear-resistant powder metallurgy material;
the silicone is selected from: methyl orthosilicate; the organic aluminum is selected from aluminum isopropoxide; the fatty acid is selected from: linoleic acid.
Example 2
Preparing a precursor:
according to the weight parts, 25 parts of graphene oxide, 26 parts of organic aluminum, 20 parts of organic silicon, 450 parts of absolute ethyl alcohol, 60 parts of fatty acid, 2 parts of nano iron powder, 3 parts of calcium fluoride and 4% ammonium nitrate of graphene oxide are taken in sequence;
firstly, mixing graphene oxide and absolute ethyl alcohol, pouring the mixture into a reactor, and carrying out ultrasonic dispersion for 50min at the temperature of 60 ℃ and the ultrasonic frequency of 100kHz to obtain dispersion liquid;
sequentially adding organic silicon, organic aluminum, fatty acid, nano iron powder, calcium fluoride and ammonium nitrate into the dispersion liquid, heating and refluxing for 9 hours at the temperature of 78 ℃, stopping the reaction, filtering, collecting a filter cake, washing the filter cake with absolute ethyl alcohol for 4 times, washing the filter cake with deionized water for 3 times, transferring the filter cake washed with the deionized water into an oven, and drying at the temperature of 105 ℃ to constant weight to obtain a precursor;
pressing:
pressing the precursor under the pressure of 500MPa for 8min to obtain a blank;
and (3) sintering:
transferring the obtained blank into a tubular furnace, introducing nitrogen into the tubular furnace at the speed of 300mL/min, heating to 900 ℃ at the speed of 8 ℃/min under the protection of nitrogen, heating to 1700 ℃ at the speed of 0.4 ℃/min, carrying out heat preservation reaction for 7h, stopping heating, cooling to room temperature along with the furnace, and discharging to obtain the high-wear-resistant powder metallurgy material;
the silicone is selected from: ethyl orthosilicate; the organic aluminum is selected from aluminum ethoxide; the fatty acid is selected from: linolenic acid.
Example 3
Preparing a precursor:
according to the weight parts, 30 parts of graphene oxide, 30 parts of organic aluminum, 30 parts of organic silicon, 500 parts of absolute ethyl alcohol, 80 parts of fatty acid, 3 parts of nano iron powder, 4 parts of calcium fluoride and ammonium nitrate accounting for 5% of the mass of the graphene oxide are taken in sequence;
firstly, mixing graphene oxide and absolute ethyl alcohol, pouring the mixture into a reactor, and carrying out ultrasonic dispersion for 60min at the temperature of 65 ℃ and the ultrasonic frequency of 120kHz to obtain dispersion liquid;
sequentially adding organic silicon, organic aluminum, fatty acid, nano iron powder, calcium fluoride and ammonium nitrate into the dispersion liquid, heating and refluxing for 10 hours at the temperature of 80 ℃, stopping the reaction, filtering, collecting a filter cake, washing the filter cake with absolute ethyl alcohol for 5 times, washing the filter cake with deionized water for 4 times, transferring the filter cake washed with the deionized water into an oven, and drying at the temperature of 110 ℃ to constant weight to obtain a precursor;
pressing:
pressing the precursor under the pressure of 600MPa for 10min to obtain a blank;
and (3) sintering:
transferring the obtained blank into a tubular furnace, introducing nitrogen into the tubular furnace at the rate of 500mL/min, heating to 1000 ℃ at the rate of 10 ℃/min under the protection of nitrogen, heating to 1800 ℃ at the rate of 0.5 ℃/min, keeping the temperature for reaction for 8 hours, stopping heating, cooling to room temperature along with the furnace, and discharging to obtain the high-wear-resistant powder metallurgy material;
the silicone is selected from: propyl orthosilicate; the organic aluminum is selected from trimethyl aluminum; the fatty acid is selected from: stearic acid.
Comparative example 1
This comparative example differs from example 1 in that: no silicone was added and the remaining conditions were kept unchanged.
Comparative example 2
This comparative example differs from example 1 in that: nano iron powder and calcium fluoride are not added, and other conditions are kept unchanged.
Comparative example 3
The comparative example differs from example 1 in that: no ammonium nitrate was added and the remaining conditions were maintained.
Comparative example 4
This comparative example differs from example 1 in that: graphene oxide is not added, the rest conditions are kept unchanged, and the rest conditions are kept unchanged.
The products obtained in examples 1 to 3 and comparative examples 1 to 4 were subjected to performance tests, and the specific test methods and test results were as follows:
an MMU-10G high-temperature end face abrasion tester is used for carrying out an end face abrasion test, a grinding disc is rotated in a unidirectional mode in a pin disc type sliding friction mode, and the rotating speed is 400 r/min. The diameter of the test piece is 20.6mm, the abrasion time is 20min, the pressure F borne by the test piece is 1256N, the friction pair is quenching GCr12, and the hardness is 63 HRC. Cleaning the abraded test piece with acetone, naturally drying, measuring the weight before and after abrasion by using an electronic balance with the precision of one ten-thousandth, and calculating the weight difference to be the abrasion loss, wherein the specific test result is shown in table 1;
table 1: product performance test results
| Abrasion loss/mg | |
| Example 1 | 2.5 |
| Example 2 | 2.4 |
| Example 3 | 2.2 |
| Comparative example 1 | 15.6 |
| Comparative example 2 | 5.6 |
| Comparative example 3 | 6.2 |
| Comparative example 4 | 18.9 |
As can be seen from the test results in Table 1, the product obtained by the invention has excellent wear-resisting effect.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. A preparation method of a high wear-resistant powder metallurgy material is characterized by comprising the following steps:
preparing a precursor:
dispersing graphene oxide in absolute ethyl alcohol, adding organic silicon, organic aluminum and fatty acid, heating, refluxing, reacting, filtering, washing and drying to obtain a precursor;
pressing:
cold-pressing and molding the precursor to obtain a blank;
and (3) sintering:
heating the blank body in a nitrogen atmosphere at the speed of 5-10 ℃/min to the temperature of 800-;
the specific preparation steps further comprise: in the preparation process of the precursor, before heating reflux reaction, adding nano iron powder and calcium fluoride;
the specific preparation steps further comprise:
in the preparation process of the precursor, ammonium nitrate with the mass of 3-5% of that of the graphene oxide is added before the heating reflux reaction.
2. The method of claim 1, wherein the silicone is selected from the group consisting of: any one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
3. The method for preparing a highly wear-resistant powder metallurgy material according to claim 1, wherein the organic aluminum is selected from any one of aluminum isopropoxide, aluminum ethoxide and trimethyl aluminum.
4. The method of claim 1, wherein the fatty acid is selected from the group consisting of: any one of linoleic acid, linolenic acid, arachidonic acid and stearic acid.
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| CN107619263A (en) * | 2017-10-13 | 2018-01-23 | 齐鲁工业大学 | One kind addition graphene oxide coated Si3N4The Al of composite granule2O3Base ceramic cutting tool material and preparation method thereof |
| CN108046774B (en) * | 2017-12-11 | 2020-11-24 | 中国科学院理化技术研究所 | Preparation method of graphene ceramic composite material |
| CN111484832B (en) * | 2019-01-25 | 2021-06-22 | 中国科学院宁波材料技术与工程研究所 | Graphene/silicon carbide nanowire composite structure thermal interface material |
| CN111825459B (en) * | 2019-04-23 | 2021-05-18 | 中国科学院金属研究所 | Silicon carbide/graphene bionic composite material for bulletproof armor and preparation method thereof |
| CN110590346A (en) * | 2019-10-11 | 2019-12-20 | 林国强 | High-heat-conductivity wear-resistant material for circulating fluidized bed boiler |
| CN112057747B (en) * | 2020-08-17 | 2021-05-07 | 菏泽鑫盛达新材料有限公司 | Graphene material for hot compress material and preparation method thereof |
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