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CN115673317A - Preparation method of graphite-steel-based self-lubricating wear-resistant composite material - Google Patents

Preparation method of graphite-steel-based self-lubricating wear-resistant composite material Download PDF

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CN115673317A
CN115673317A CN202211038539.7A CN202211038539A CN115673317A CN 115673317 A CN115673317 A CN 115673317A CN 202211038539 A CN202211038539 A CN 202211038539A CN 115673317 A CN115673317 A CN 115673317A
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graphite
temperature
steel
percent
powder
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CN202211038539.7A
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�山泉
黄沁源
蒋业华
李祖来
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The invention relates to the field of preparation of wear-resistant materials, in particular to a preparation method of a graphite-steel-based self-lubricating wear-resistant composite material, which comprises the following steps: s1, pretreatment of graphite; s2, plating nickel on the surface of graphite; s3, pre-sintering treatment; and S4, putting the obtained sample into a vacuum smelting furnace for vacuum sintering, and cooling to room temperature along with the furnace. And obtaining a finished product. The invention prepares the nickel-coated graphite particles with a nearly spherical shape by a chemical coating method, the nickel-plated layer prevents graphite from being dissolved in molten steel to react during sintering, and the three-dimensional nearly spherical graphite structure with a micron scale is dispersed and distributed in a steel matrix, so that the steel matrix forms a porous structure taking the nearly spherical graphite as an mosaic to improve the mechanical property of the material, the graphite can reduce the friction coefficient, slow down the corrosion and oxidation process of a friction surface, and the heat conductivity can reduce the decomposition of the matrix material in the friction process.

Description

Preparation method of graphite-steel-based self-lubricating wear-resistant composite material
Technical Field
The invention relates to the field of preparation of wear-resistant materials, in particular to a preparation method of a graphite-steel-based self-lubricating wear-resistant composite material.
Background
Wear is now the most prominent failure mode of mechanical parts, and according to statistics, about 30% of the primary energy worldwide each year is consumed by friction, and the material wear caused by friction also causes about 60% of the mechanical parts to fail. Reducing material wear by improving lubrication performance has become an important measure to increase the reliability of mechanical equipment, extend the service life of the equipment, and save raw materials and energy. With the rapid development of industry, the demands for precision and efficiency in the manufacturing field and mechanical equipment are increasingly urgent. The basic transmission parts need to ensure the tiny assembly clearance and excellent lubricating condition as far as possible on the premise of achieving precision and high efficiency, and the traditional fluid medium lubricating mode cannot be met at the moment, so that the material has the self-lubricating property on the premise of ensuring the mechanical property of the material, which is very important.
The iron-based self-lubricating material has very wide research and application potential due to high cost performance, and iron graphite series metal generally refers to a metal material with a matrix structure consisting of iron-carbon alloy and free graphite. Because the structure and the performance of the iron-carbon alloy are wide in adjustable range, the graphite in the matrix can provide excellent lubricating performance under the friction action, and the graphite and the matrix have excellent comprehensive performance and higher cost performance after being combined by a certain metal manufacturing process, so that the iron-carbon alloy has a huge application prospect as a self-lubricating antifriction material.
Disclosure of Invention
The invention aims to provide a preparation method of a graphite-steel-based self-lubricating wear-resistant composite material aiming at the problems in the background art.
The technical scheme of the invention is as follows: a preparation method of a graphite-steel-based self-lubricating wear-resistant composite material comprises the following specific steps:
s1, pretreatment of graphite;
selecting natural graphite powder with the granularity of 50-70 microns, putting the natural graphite powder into an alumina crucible, putting the alumina crucible into a box-type resistance furnace, slowly heating to 500 ℃, and preserving heat for 2 hours to obtain graphite particles A;
s2, plating nickel on the surface of graphite;
adding the graphite particles A into a nickel sulfate solution, and fully mixing to obtain a mixture B;
adding the mixture B into an autoclave for hydrogen reduction reaction, and adding an alcohol surfactant and a universal catalyst in the reaction process to obtain graphite particles C with uniform nickel coating;
s3, pre-sintering treatment;
adding steel powder with the particle size of less than 45um and graphite particles C into a ball mill according to the mass ratio of 19;
introducing the mixed powder D into a beaker, putting the beaker into a vacuum drying oven for pre-drying, keeping the temperature for 5h at the drying temperature of 90 ℃, then heating to 200 ℃ and keeping the temperature for 12h, finally taking out the powder, pouring the powder into a grinding pot to separate the dried agglomerated powder, finally introducing the powder after mixing into a die, and performing compression molding by using a tablet press to obtain a sample E; wherein the tablet press obtains pressure of 15Mpa, and the pressure maintaining time is 15min;
and S4, placing the obtained sample E into a vacuum smelting furnace for vacuum sintering, and cooling to room temperature along with the furnace. And obtaining a finished product F.
Preferably, the grinding ball added in S3 comprises abrasive grains a with the mass of 5g and abrasive grains b with the mass of 1 g;
the number ratio of the abrasive grains a to the abrasive grains b is 1:5.
preferably, the temperature control process of the sample E in S4 during vacuum sintering is as follows:
heating the temperature in the vacuum smelting furnace from room temperature to 500 ℃ at the heating rate of 5 ℃/min;
then the temperature in the vacuum melting furnace is increased from 500 ℃ to 800 ℃ at the temperature increasing speed of 10 ℃/min;
then, according to the temperature rise speed of 5 ℃/min, the temperature in the vacuum smelting furnace is raised from 800 ℃ to 1000 ℃;
then the temperature in the vacuum melting furnace is increased from 1000 ℃ to 1350 ℃ at the temperature rising speed of 2.5 ℃/min, and the temperature is preserved for 120min.
Preferably, the finished product F comprises the following components in percentage by mass: 0.4 to 0.6 percent of C, 0.1 to 0.25 percent of Si, 20 to 24 percent of Mn, 3 to 4 percent of Cr, 0.06 to 0.095 percent of Ti, 0.44 to 0.65 percent of V, 0.2 to 0.4 percent of Mo, 0.2 to 0.3 percent of N, less than 0.01 percent of P, less than 0.01 percent of S, and the balance of Fe and inevitable impurities.
Preferably, the graphite particles in the finished product F have a structure of a nearly spherical structure with a diameter of 50-70 microns.
Preferably, the rotation speed of the ball mill in S3 is 30r/min, and the ball milling time is 12h.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
graphite is a solid self-lubricating material with good performance, has good thermal stability, lubricity and wear resistance, and is not corroded by strong alkali, strong acid and organic solvent at normal temperature. Meanwhile, the graphite microcrystal has an adhesion effect on metal during friction, and in the service process of the friction, the metal on the friction surface is adhered to enable the graphite particles in the shearing and tearing process to be tightly adsorbed in the metal oxide, so that an oxidation film formed on the friction surface also has an anti-friction effect. When the solid lubricant in the graphite lubricating material can be continuously supplemented and the continuity and the integrity of the solid lubricating film are maintained, good lubricating and self-repairing effects are achieved.
The graphite-steel-based self-lubricating wear-resistant composite material provided by the invention is prepared by preparing nearly spherical nickel-coated graphite particles by a chemical coating method, and designing a powder sintering process, wherein a nickel-plated layer coated on the outer layer of the graphite particles prevents graphite from being dissolved in molten steel to react during sintering, so that a micron-scale three-dimensional nearly spherical graphite structure is dispersed in a steel base, a steel base forms a porous framework with the nearly spherical graphite as an mosaic body to improve the mechanical property of the material, the graphite can reduce the friction coefficient, slow down the corrosion and oxidation process of a friction surface, and the thermal conductivity can reduce the decomposition of the base material in the friction process.
Drawings
FIG. 1 is a schematic view of near-spherical graphite and steel-based co-strengthening according to an embodiment of the present invention.
Detailed Description
Example one
The invention provides a preparation method of a graphite-steel-based self-lubricating wear-resistant composite material, which comprises the following specific steps:
s1, pretreatment of graphite;
selecting natural graphite powder with the granularity of 50-70 microns, putting the natural graphite powder into an alumina crucible, putting the alumina crucible into a box-type resistance furnace, slowly heating to 450-550 ℃, and preserving heat for 1.5-2.5 hours to obtain graphite particles A;
further, the heating temperature is 450 ℃, and the heat preservation time is 1.5h;
further, the heating temperature is 500 ℃, and the heat preservation time is 2h;
furthermore, the heating temperature is 550 ℃, and the heat preservation time is 2.5h;
s2, plating nickel on the surface of graphite;
adding the graphite particles A into a nickel sulfate solution, and fully mixing to obtain a mixture B;
wherein, the nickel sulfate solution is prepared by mixing nickel sulfate, ammonium sulfate and ammonia water according to certain weight percentage;
adding the mixture B into an autoclave for hydrogen reduction reaction, and adding an alcohol surfactant and a universal catalyst in the reaction process to obtain graphite particles C with uniform nickel coating;
s3, pre-sintering treatment;
adding steel powder with the particle size of less than 45um and graphite particles C into a ball mill according to the mass ratio of 19;
introducing the mixed powder D into a beaker, putting the beaker into a vacuum drying oven for pre-drying, keeping the temperature for 5h at the drying temperature of 90 ℃, then heating to 200 ℃ and keeping the temperature for 12h, finally taking out the powder, pouring the powder into a grinding pot to separate the dried agglomerated powder, finally introducing the powder after mixing into a die, and performing compression molding by using a tablet press to obtain a sample E; wherein, the pressure obtained by the tablet press is 10-20 Mpa, and the pressure maintaining time is 10-20 min; the rotating speed of the ball mill is 25-35 r/min, and the ball milling time is 10-14 h;
further, the pressure obtained by a tablet press is 10Mpa, and the pressure maintaining time is 10min; the rotating speed of the ball mill is 25r/min, and the ball milling time is 10h;
further, the pressure obtained by a tablet press is 15Mpa, and the pressure maintaining time is 15min; the rotating speed of the ball mill is 30r/min, and the ball milling time is 12h;
further, the pressure obtained by the tablet press is 20Mpa, and the pressure maintaining time is 20min; the rotating speed of the ball mill is 35r/min, and the ball milling time is 14h;
and S4, placing the obtained sample E into a vacuum smelting furnace for vacuum sintering, and cooling to room temperature along with the furnace. And obtaining a finished product F.
Example two
Compared with the first embodiment, the grinding ball added in the embodiment S3 of the preparation method of the graphite-steel-based self-lubricating wear-resistant composite material provided by the invention comprises 5g of abrasive grains a and 1g of abrasive grains b;
the number ratio of the abrasive grains a to the abrasive grains b is 1:5.
EXAMPLE III
Compared with the first embodiment, the preparation method of the graphite-steel-based self-lubricating wear-resistant composite material provided by the invention has the following temperature control process when the sample E is subjected to vacuum sintering in the embodiment S4:
heating the temperature in the vacuum smelting furnace from room temperature to 500 ℃ at the heating rate of 5 ℃/min;
then the temperature in the vacuum melting furnace is increased from 500 ℃ to 800 ℃ at the temperature increasing speed of 10 ℃/min;
then, according to the temperature rise speed of 5 ℃/min, the temperature in the vacuum smelting furnace is raised from 800 ℃ to 1000 ℃;
then the temperature in the vacuum melting furnace is increased from 1000 ℃ to 1350 ℃ at the temperature rising speed of 2.5 ℃/min, and the temperature is preserved for 120min.
Example four
Compared with the first embodiment, the preparation method of the graphite-steel-based self-lubricating wear-resistant composite material provided by the invention has the following advantages that a finished product F comprises the following components in percentage by mass: 0.4 to 0.6 percent of C, 0.1 to 0.25 percent of Si, 20 to 24 percent of Mn, 3 to 4 percent of Cr, 0.06 to 0.095 percent of Ti, 0.44 to 0.65 percent of V, 0.2 to 0.4 percent of Mo, 0.2 to 0.3 percent of N, less than 0.01 percent of P, less than 0.01 percent of S, and the balance of Fe and inevitable impurities;
as shown in FIG. 1, the graphite particles in the final product F have a nearly spherical structure with a diameter of 50-70 μm.
In conclusion, the spherical graphite powder with the grain size of 20-30 microns is selected to be compounded with the steel matrix, so that the nearly spherical graphite structure with the micron scale is in dispersion distribution in the steel matrix, the synergistic strengthening effect of the matrix and graphite subjects is exerted, the spherical graphite plays a dispersion strengthening effect in the steel matrix, and the spherical porous skeleton structure in the steel matrix plays a spherical porous size effect, so that the specific strength of the composite material can be increased compared with the traditional steel composite material; the nickel coating layer outside the nearly spherical graphite blocks the graphite from being dissolved in molten steel to react when the powder is sintered after being mixed, prevents the graphite from being dissolved in a steel matrix to further precipitate hard and brittle cementite and reduce the toughness of the material, and simultaneously, a transition reaction zone with better mechanical property is formed at the interface of the nickel coating layer and the steel matrix, so that the strength of the graphite-steel matrix interface is improved, the defect caused by mechanical inlaying of uncoated nickel graphite and the matrix is improved, and the steel matrix forms a spherical framework taking the nearly spherical graphite as an inlaid body. The addition of the graphite reduces the friction coefficient of the material in the friction service process, the graphite is continuously separated out in the friction process to play a self-lubricating role, the stability and impermeability of the graphite can slow down the corrosion and oxidation processes of the friction surface, and the heat conductivity can reduce the decomposition of the base material in the friction process.
The embodiments of the present invention have been described in detail with reference to the drawings, but the present invention is not limited thereto, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.

Claims (6)

1. The preparation method of the graphite-steel-based self-lubricating wear-resistant composite material is characterized by comprising the following specific steps of:
s1, pretreatment of graphite;
selecting natural graphite powder with the granularity of 50-70 microns, putting the natural graphite powder into an alumina crucible, putting the alumina crucible into a box-type resistance furnace, slowly heating to 500 ℃, and preserving heat for 2 hours to obtain graphite particles A;
s2, plating nickel on the surface of graphite;
adding the graphite particles A into a nickel sulfate solution, and fully mixing to obtain a mixture B;
adding the mixture B into an autoclave for hydrogen reduction reaction, and adding an alcohol surfactant and a universal catalyst in the reaction process to obtain graphite particles C with uniform nickel coating;
s3, pre-sintering treatment;
adding steel powder with the particle size of less than 45um and graphite particles C into a ball mill according to the mass ratio of 19;
introducing the mixed powder D into a beaker, putting the beaker into a vacuum drying oven for pre-drying, keeping the temperature for 5h at the drying temperature of 90 ℃, then heating to 200 ℃ and keeping the temperature for 12h, finally taking out the powder, pouring the powder into a grinding pot to separate the dried agglomerated powder, finally introducing the powder after mixing into a die, and performing compression molding by using a tablet press to obtain a sample E; wherein the pressure obtained by the tablet press is 15Mpa, and the pressure maintaining time is 15min;
and S4, putting the obtained sample E into a vacuum smelting furnace for vacuum sintering, and cooling to room temperature along with the furnace. And obtaining a finished product F.
2. The method for preparing the graphite-steel-based self-lubricating wear-resistant composite material according to claim 1, wherein the grinding ball added in the step S3 comprises 5g of abrasive particles a and 1g of abrasive particles b;
the number ratio of the abrasive grains a to the abrasive grains b is 1:5.
3. the preparation method of the graphite-steel-based self-lubricating wear-resistant composite material as claimed in claim 1, wherein the temperature control process during vacuum sintering of the sample E in S4 is as follows:
heating the temperature in the vacuum smelting furnace from room temperature to 500 ℃ at the heating rate of 5 ℃/min;
then the temperature in the vacuum melting furnace is increased from 500 ℃ to 800 ℃ at the temperature increasing speed of 10 ℃/min;
then, according to the temperature rise speed of 5 ℃/min, raising the temperature in the vacuum smelting furnace from 800 ℃ to 1000 ℃;
then the temperature in the vacuum melting furnace is increased from 1000 ℃ to 1350 ℃ at the temperature rising speed of 2.5 ℃/min, and the temperature is preserved for 120min.
4. The preparation method of the graphite-steel-based self-lubricating wear-resistant composite material as claimed in claim 1, wherein the finished product F comprises the following components in percentage by mass: 0.4 to 0.6 percent of C, 0.1 to 0.25 percent of Si, 20 to 24 percent of Mn, 3 to 4 percent of Cr, 0.06 to 0.095 percent of Ti, 0.44 to 0.65 percent of V, 0.2 to 0.4 percent of Mo, 0.2 to 0.3 percent of N, less than 0.01 percent of P, less than 0.01 percent of S, and the balance of Fe and inevitable impurities.
5. The method for preparing the graphite-steel-based self-lubricating abrasion-resistant composite material as claimed in claim 1, wherein the graphite particles in the finished product F are of a nearly spherical structure with the diameter of 50-70 microns.
6. The preparation method of the graphite-steel-based self-lubricating wear-resistant composite material as claimed in claim 1, wherein the rotation speed of a ball mill in S3 is 30r/min, and the ball milling time is 12h.
CN202211038539.7A 2022-08-29 2022-08-29 Preparation method of graphite-steel-based self-lubricating wear-resistant composite material Pending CN115673317A (en)

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CN115673317A true CN115673317A (en) 2023-02-03

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