CN115070038A - In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof - Google Patents
In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof Download PDFInfo
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- 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
The invention discloses an in-situ mixed dual-phase ceramic reinforced iron-based composite material and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, mixing spherical Ti powder with irregular shape B 4 C, high-energy ball milling and mixing the powder; second, high chromium cast ironBall milling and mixing the powder at low speed; thirdly, cold-pressing and preforming; fourthly, vacuum hot pressing sintering of stage heating. The invention utilizes high-energy ball milling to mill B 4 C powder is wrapped on the outer layer of the spherical Ti powder and is sintered to generate TiC and TiB in situ w The two-phase ceramic reinforcing phase is uniformly distributed in the high-chromium cast iron matrix, so that the distribution uniformity of the reinforcing phase and the bonding property with the matrix interface are improved, the two-phase ceramic reinforcing phase is prevented from being stripped or falling off from the high-chromium cast iron matrix, and TiC and TiB are fully exerted w The reinforcing effect of the dual-phase ceramic reinforcing phase improves the wear resistance, strength and impact resistance of the dual-phase ceramic reinforcing phase, enlarges the application range of the composite material, simplifies the process and saves the cost.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to an in-situ mixed dual-phase ceramic reinforced iron matrix composite material and a preparation method thereof.
Background
High-chromium cast iron has excellent wear resistance and is widely used in the fields of building materials, metallurgy, mines, electric power, cement, mechanical engineering and the like, for example, as a jaw plate, a plate hammer and a hammer head of a crusher for mines, a sleeve and a lining tile of a coal vertical mill, a grinding ball and a lining board of a ball mill, a roller and a guide plate of a rolling mill and the like. However, under the working condition of high wear resistance, the traditional high-chromium cast iron is difficult to meet the wear resistance requirement, has the problems of serious wear, serious short service life and the like, and is difficult to meet the requirement of practical application.
The composite material formed by adding the ceramic particles as the second phase into the metal matrix not only has the advantages of high hardness, high wear resistance, heat resistance, corrosion resistance and the like of the ceramic, but also can exert good toughness, plasticity, thermal conductivity and electrical conductivity of the metal matrix, so that the composite material is widely researched and applied at present. The TiC ceramic particles have the advantages of low density, high hardness, small friction coefficient, good high-temperature stability and the like, and can be added into iron-based, aluminum-based, titanium-based and other metal materials as a reinforcing phase to obviously improve the strength and hardness of the composite material.
Patent publication No. CN111519087A discloses adding TiC ceramic particles in high-chromium cast iron powder, obtaining mixed powder of the two by ball milling and mixing, and then obtaining TiC particle-reinforced high-chromium cast iron-based composite material through processes of compact sintering densification, quenching treatment, tempering treatment and the like. However, during abrasive wear of this type of composite, irregular TiC particles tend to cause stress concentrations at sharp corners, so that the loading stress is amplified, leading to the formation and propagation of microcracks. In addition, the TiC is poor in interface bonding with the matrix, so that reinforcing particles are easily debonded or broken in the service process, and the debonded or broken reinforcing particles become grinding particles, and finally the abrasion process is accelerated.
Among the preparation methods of the ceramic particle reinforced metal matrix composite, the in-situ reaction method has the advantages of simple preparation process, low cost, firm combination of a matrix and a reinforced phase interface, small in-situ generated particles and the like, so that the ceramic particle reinforced metal matrix composite is widely applied by people. In situ generated TiB w Ceramics are more considered to be excellent reinforcing phases in Ti-based composites. In addition, the in-situ hybrid reinforcement effect in the metal matrix composite is reported to be superior to the single reinforcement effect of any one of the ceramic phases.
The patent with publication number CN107267871B adopts aluminum hydroxide, aluminum micro powder mixture and MgF 2 The in-situ mixed particle reinforced iron-based composite material is prepared by proportioning, mixing, press forming and high-temperature sintering Ti powder, C powder, Cu powder, Ni powder and Fe powder according to a certain proportion. The iron-based composite material prepared by the method contains two reinforcing phases, but the method has the defects that the sintering process is complicated, and the prepared composite material has low hardness (lower than HRC 60), so that the iron-based composite material is difficult to be applied to occasions with high requirements on wear resistance.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of an in-situ mixed dual-phase ceramic reinforced iron-based composite material aiming at the defects of the prior art. The method utilizes high-energy ball milling to mix B 4 C powder is wrapped on the outer layer of the spherical Ti powder and is pressed with the matrix powder and is subjected to vacuum hot pressingSintering in-situ to produce TiC and TiB w The two-phase ceramic reinforcing phase is uniformly distributed in the high-chromium cast iron matrix, so that the distribution uniformity of the reinforcing phase and the bonding property with the matrix interface are improved, the two-phase ceramic reinforcing phase is prevented from being stripped or falling off from the high-chromium cast iron matrix, and TiC and TiB are fully exerted w The strengthening effect of the dual-phase ceramic reinforcing phase improves the hardness and the wear resistance of the dual-phase ceramic reinforcing phase, and overcomes the defects of poor bonding property of the ceramic reinforcing phase and a matrix, complex process, single reinforcing effect and low hardness of the composite material.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized by comprising the following steps of:
step one, mixing spherical Ti powder with irregular shape B 4 Putting the powder C into a stainless steel ball milling tank, and performing high-energy ball milling and mixing under a vacuum condition to obtain mixed powder A; the mixed powder A is an ellipsoidal Ti powder outer wrapping B 4 The structure of the C powder;
step two, putting the mixed powder A obtained in the step one and high-chromium cast iron powder into an agate grinding tank, and performing low-speed ball milling and mixing to obtain mixed powder B;
step three, placing the mixed powder B obtained in the step two into a graphite die for cold pressing and preforming to obtain a pressed blank;
step four, carrying out vacuum hot-pressing sintering of stage heating on the pressed compact obtained in the step three to obtain in-situ mixed TiC and TiB w A two-phase ceramic reinforced iron-based composite material.
The invention firstly utilizes a high-energy ball milling process to mix B 4 The powder C is wrapped on the outer layer of the spherical Ti powder, so that the contact area of the powder C and the spherical Ti powder is greatly increased, then the powder C and the matrix powder are uniformly mixed and are cold-pressed into a pressed blank, and then the pressed blank is subjected to vacuum hot-pressing sintering of stage heating, the temperature is raised to a lower temperature first and then is kept so that the powder B is heated 4 In-situ reaction of C powder and Ti powder to generate TiC and TiB w The temperature is raised to a higher temperature to melt and convert the high-chromium cast iron into a liquid phase, so that TiC and TiB are obtained w The biphase ceramic reinforcing phase is uniformly distributed in the high-chromium cast iron matrix, and improvesEnhance the phase distribution uniformity, thereby giving full play to TiC and TiB w Strengthening effect of biphase ceramic reinforcing phase, and TiC and TiB generated in situ w The interface bonding performance of the dual-phase ceramic reinforcing phase and the high-chromium cast iron matrix is better, so that the dual-phase ceramic reinforcing phase is not easy to strip or fall off from the high-chromium cast iron matrix in the service process of the composite material, the hardness and the wear resistance of the composite material are improved, and the composite material is suitable for occasions with high wear resistance requirements.
The preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized in that in the step one, the particle size of the spherical Ti powder is 1-200 mu m, and the irregular shape B is 4 The particle size of the C powder is 0.1-100 μm, and the spherical Ti powder and the irregular shape B 4 The molar ratio of the C powder is 2-20: 1. By the above-mentioned definition of particle size and molar ratio, the irregular shape B is ensured 4 The C powder is wrapped on the outer layer of the spherical Ti powder, which is beneficial to the subsequent Ti and B 4 C reaction promoting TiC and TiB w And (3) generation of a dual-phase ceramic reinforcing phase.
The preparation method of the in-situ hybrid dual-phase ceramic reinforced iron-based composite material is characterized in that in the step one, the rotation speed for high-energy ball milling and mixing is 300 r/min-500 r/min, the ball-material ratio is 2-20: 1, the ball milling time is 2 h-10 h, the mode is set to be that positive rotation and negative rotation are alternately carried out, and the ball milling is suspended for 10 min-60 min every 1 h. The high-energy ball milling parameters are beneficial to B with smaller granularity and higher hardness 4 The C powder is effectively coated on the surface of the spherical titanium powder with larger granularity and lower hardness, so that the contact area of the C powder and the spherical titanium powder is increased.
The preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized in that the high-chromium cast iron powder in the step two comprises the following components in percentage by mass: 2.0-3.3% of C, 11.0-30.0% of Cr, 0-1.5% of Si, 0-0.5% of Ni, 0-1.5% of B, 0-0.1% of V, 0-0.6% of Mn, 0-0.3% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 50-500 mu m, and the mass ratio of the mixed powder to the high-chromium cast iron powder is 1: 2-19. The high-chromium cast iron powder with the components and the granularity is common, and the universality of the method is improved.
The preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized in that in the second step, the rotation speed for low-speed ball milling and mixing is 150 r/min-250 r/min, the ball-material ratio is 2-10: 1, the ball milling time is 2 h-15 h, the mode is set to be that positive rotation and negative rotation are alternately carried out, and the ball milling is suspended for 10 min-30 min every 1 h. The low-speed ball milling parameters ensure the uniformity of ball milling mixed powder and improve the powder mixing efficiency.
The preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized in that the pressure of the cold pressing preforming in the third step is 10-50 MPa, and the pressure maintaining time is 5-60 min. The cold-pressing preforming process parameters are beneficial to improving the in-situ TiC and TiB mixture while ensuring the smooth forming of the pressed blank w The dual-phase ceramic enhances the internal bonding strength and compactness of the iron-based composite material.
The preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized in that the vacuum hot-pressing sintering process of the stage heating in the step four is as follows: the temperature is increased to 1050-1250 ℃ and is preserved for 15-120 min, then the temperature is increased to 1300-1550 ℃ at the speed of 10-20 ℃/min and is preserved for 30-120 min, then the temperature is decreased to 850-1100 ℃, the pressure is increased to 5-50 MPa at constant temperature, the pressure is preserved for 5-120 min, and the temperature is cooled to room temperature along with the furnace. According to the invention, the temperature is raised to 1050-1250 ℃ at a lower temperature in the vacuum hot-pressing sintering process for heat preservation, so that the spherical Ti powder and the irregular shape B are promoted 4 The C powder reacts preferentially to generate TiC and TiB w The biphase ceramic reinforcing phase ensures that the high-chromium cast iron is melted to generate a liquid phase by controlling the rate, the temperature and the heat preservation time of continuous temperature rise, and promotes TiC and TiB w The two-phase ceramic reinforcing phase is uniformly distributed in the high-chromium cast iron matrix; meanwhile, pressure is applied under the condition that a small amount of liquid phase exists by pressurizing and maintaining pressure after cooling, so that the in-situ mixing of TiC and TiB in the product is further improved w The density of the iron-based composite material is enhanced by the two-phase ceramic.
In addition, the invention also discloses an in-situ mixed dual-phase ceramic reinforced iron-based composite material prepared by the method, which is characterized by comprising a high-chromium cast iron matrix and a high-chromium cast iron matrix uniformly distributed on the high-chromium cast iron matrixTiC ceramic particles and TiB generated in situ in iron matrix w A ceramic particle mixed reinforcement phase; in-situ TiC and TiB doping w The hardness of the dual-phase ceramic reinforced iron-based composite material is HRC 65-73, the bending strength is 300 MPa-600 MPa, the compression strength is 900 MPa-1400 MPa, and the impact toughness is 6J/cm 2 ~12J/cm 2 。
The in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized in that TiC ceramic particles and TiB generated in situ w The size of the ceramic particles is 1-3 μm. The reinforcing phase with fine particle size not only improves the hardness of the composite material, but also can be uniformly dispersed in the high-chromium cast iron matrix, is firmly combined with the high-chromium cast iron matrix, and is not easy to strip or fall off from the high-chromium cast iron matrix in the service process.
Compared with the prior art, the invention has the following advantages:
1. the invention utilizes a high-energy ball milling process to mix B 4 The powder C is wrapped on the outer layer of the spherical Ti powder and is subjected to stage-heating vacuum hot-pressing sintering with the base powder compact to ensure that the powder B is subjected to stage-heating vacuum hot-pressing sintering 4 In-situ reaction of C powder and Ti powder to generate TiC and TiB w The two-phase ceramic reinforcing phase is uniformly distributed in the high-chromium cast iron matrix converted into the liquid phase, so that the distribution uniformity of the reinforcing phase and the bonding performance with the matrix interface are improved, and the TiC and TiB are fully exerted w The strengthening effect of the dual-phase ceramic reinforcing phase avoids the dual-phase ceramic reinforcing phase from peeling or falling off from the high-chromium cast iron matrix, and improves the hardness and the wear resistance of the composite material.
2. Compared with conventional Si 4 C reinforcement, B selected for use in the present invention 4 The C reinforcement provides 4B atoms and 1C atom, and both can combine with Ti atoms to form high hardness TiC ceramic and TiB w The ceramic reinforcing phase can be obtained in one step, the reinforcing effect of the reinforcing phase is improved, the composite material is endowed with excellent wear resistance and high hardness, and the process is simpler.
3. Compared with the added ceramic particle reinforcing phase, the invention adopts B 4 TiC and TiB generated in situ by reaction of C powder and Ti powder w High chromium cast iron base with two-phase ceramic reinforcing phaseThe distribution in the body is more uniform, the strengthening effect is better than that of a single ceramic strengthening phase, the preparation process is simple, and the cost is low.
4. In-situ TiC and TiB mixed prepared by the invention w The hardness of the dual-phase ceramic reinforced iron-based composite material is HRC 65-73, the bending strength is 300 MPa-600 MPa, the compression strength is 900 MPa-1400 MPa, and the impact toughness is 6J/cm 2 ~12J/cm 2 The composite material has excellent wear resistance, strength and impact resistance, and the application range of the composite material is expanded.
5. In-situ TiC and TiB mixed prepared by the invention w The biphase ceramic reinforced iron-based composite material can be prepared into a high-hardness composite material with excellent performance without conventional subsequent heat treatment processes such as quenching, annealing or tempering, and the like, and the cold press molding and the hot press sintering process are combined, so that the powder molding, in-situ reaction and densification processes are realized through one-step sintering, the preparation process flow is greatly shortened, and the production cost is reduced.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1a is an SEM photograph of spherical Ti powder in example 1 of the present invention.
FIG. 1B shows an irregular shape B in example 1 of the present invention 4 SEM image of C powder.
FIG. 2 is an SEM photograph of mixed powder A in example 1 of the present invention.
FIG. 3 shows in-situ TiC and TiB doping prepared in example 1 of the present invention w Powder room temperature XRD pattern of the dual phase ceramic reinforced iron-based composite.
FIG. 4 shows in-situ TiC and TiB doping prepared in example 1 of the present invention w Stress-strain curve diagram of biphase ceramic reinforced iron-based composite material under compression condition.
FIG. 5 shows in-situ TiC and TiB doping prepared in example 1 of the present invention w And (3) a fracture morphology graph of the dual-phase ceramic reinforced iron-based composite material after bending fracture.
FIG. 6 shows in-situ TiC and TiB doping prepared in example 2 of the present invention w Two-phase ceramic reinforced iron-based composite material in compressed stripStress-strain diagram under the part.
FIG. 7 shows in-situ TiC and TiB doping prepared in example 2 of the present invention w And (3) a fracture morphology graph of the dual-phase ceramic reinforced iron-based composite material after bending fracture.
FIG. 8 is the in-situ TiC and TiB doping prepared in example 3 of the present invention w Stress-strain curve diagram of biphase ceramic reinforced iron-based composite material under compression condition.
FIG. 9 is the in-situ TiC and TiB doping prepared in example 3 of the present invention w And (3) a fracture morphology diagram of the dual-phase ceramic reinforced iron-based composite material after bending fracture.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, 126.8g of spherical Ti powder and 73.2g of irregular shape B are mixed 4 Putting the powder C into a vacuum stainless steel ball milling tank, filling stainless steel grinding balls, performing high-energy ball milling and mixing for 10 hours under the conditions of vacuum condition, the rotating speed of 300r/min and the ball-to-material ratio of 2:1, setting the mode to be that positive and negative rotation are alternately performed, and pausing for 10 minutes every 1 hour of ball milling to obtain mixed powder A; the mixed powder A is an ellipsoidal Ti powder outer wrapping B 4 The structure of the C powder; the particle size of the spherical Ti powder is 1-70 mu m, and the spherical Ti powder is irregular B 4 The granularity of the C powder is 0.1-30 mu m;
step two, putting 60g of the mixed powder A obtained in the step one and 120g of high-chromium cast iron powder into an agate grinding tank, putting agate grinding balls into the agate grinding tank, performing low-speed ball milling and mixing for 15 hours under the conditions that the rotating speed is 150r/min and the ball-to-material ratio is 2:1, setting the mode to be that forward and reverse rotation are alternately performed, and pausing for 10 minutes every 1 hour of ball milling to obtain mixed powder B; the high-chromium cast iron powder comprises the following components in percentage by mass: 2.0% of C, 30% of Cr, 0.5% of Si, 0.5% of Ni, 1.5% of B, 0.1% of V, 0.6% of Mn, 0.3% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 50-200 mu m;
step three, placing the mixed powder B obtained in the step two into a graphite die for cold pressing and preforming to obtain a pressed blank; the pressure of the cold pressing preforming is 10MPa, and the pressure maintaining time is 60 min;
step four, the stepPutting the pressed blank obtained in the third step into a vacuum hot-pressing sintering furnace for vacuum hot-pressing sintering with stage heating, firstly heating to 1050 ℃ and preserving heat for 120min, then heating to 1300 ℃ at the speed of 10 ℃/min and preserving heat for 120min, then cooling to 1100 ℃ and pressurizing to 5MPa at constant temperature and maintaining pressure for 5min, and cooling to room temperature along with the furnace to obtain in-situ mixed TiC and TiB w A two-phase ceramic reinforced iron-based composite; in-situ TiC and TiB doping w The biphase ceramic reinforced iron-based composite material comprises a high-chromium cast iron matrix, TiC ceramic particles and TiB which are uniformly distributed in the high-chromium cast iron matrix and generated in situ w The ceramic particles are mixed with a reinforcing phase.
TiC and TiB in situ doping prepared in this example w The properties of the dual-phase ceramic reinforced iron-based composite material, such as Rockwell hardness (HRC, measured at least at 5 different positions and averaged), three-point bending strength, compression strength, impact toughness and the like, are detected, the phase composition of the composite material is analyzed by an X-ray diffraction method, and the result shows that: in-situ TiC and TiB doping prepared in this example w The hardness of the two-phase ceramic reinforced iron-based composite material is HRC 69-73, the bending strength is 300 MPa-450 MPa, the compression strength is 1000 MPa-1300 MPa, and the impact toughness is 6J/cm 2 ~9J/cm 2 。
FIG. 1a is an SEM image of the spherical Ti powder of this example, and it can be seen from FIG. 1a that the Ti powder is spherical with smooth and clean surface and regular shape.
FIG. 1B shows an irregular shape B in this embodiment 4 SEM image of C powder, as can be seen from FIG. 1B, B 4 The C powder is irregular in shape.
FIG. 2 is a SEM image of the mixed powder A of this example, and it can be seen from FIG. 2 that after high energy ball milling and mixing, the spherical Ti powder becomes ellipsoidal and its outer layer is tightly wrapped with a layer B 4 The C particles form an approximate core-shell structure, so that the contact area between the C particles and the C particles is increased, and conditions are provided for the full reaction of the C particles and the C particles at high temperature.
FIG. 3 shows the in-situ TiC and TiB doping prepared in this example w The powder room temperature XRD pattern of the two-phase ceramic reinforced iron-based composite material can be seen from figure 3, and TiC and TiB exist in the composite material at the same time w Ceramic phase, which shows that the method of the invention successfully prepares in-situ TiC and TiB mixed w A biphase ceramic reinforced high-chromium cast iron-based composite material.
FIG. 4 shows the in-situ TiC and TiB doping prepared in this example w The stress-strain curve graph (three samples in total) of the dual-phase ceramic reinforced iron-based composite material under the compression condition can be seen from figure 4, and the compression strength of the composite material is 1000 MPa-1300 MPa.
FIG. 5 shows the in-situ TiC and TiB doping prepared in this example w The appearance of the fracture of the biphase ceramic reinforced iron-based composite material after bending fracture is shown in the figure 5, in the circle, the in-situ generated reinforced TiC ceramic particles and TiB w Ceramic particles, as can be seen from FIG. 5, the composite material is brittle fracture, and in-situ generated TiC ceramic particles and TiB w The ceramic particles are fine and only 1-3 μm.
Comparative example 1
This comparative example comprises the following steps:
step one, 38.1g of spherical Ti powder and 21.9g of irregular shape B 4 Placing the powder C and 120g of high-chromium cast iron powder into an agate grinding tank, adding agate grinding balls, performing low-speed ball milling and mixing for 15 hours under the conditions that the rotating speed is 150r/min and the ball-to-material ratio is 2:1, setting the mode to be that positive and negative rotation are alternately performed, and pausing for 10 minutes every 1 hour of ball milling to obtain mixed powder; the particle size of the spherical Ti powder is 1-70 mu m, and the spherical Ti powder is irregular B 4 The particle size of the C powder is 0.1-30 mu m; the high-chromium cast iron powder comprises the following components in percentage by mass: 2.0% of C, 30% of Cr, 0.5% of Si, 0.5% of Ni, 1.5% of B, 0.1% of V, 0.6% of Mn, 0.3% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 50-200 mu m;
step two, putting the mixed powder obtained in the step one into a graphite die for cold pressing and preforming to obtain a pressed blank; the pressure of the cold pressing preforming is 10MPa, and the pressure maintaining time is 60 min;
and step three, putting the pressed blank obtained in the step three into a vacuum hot-pressing sintering furnace for vacuum hot-pressing sintering with stage heating, firstly heating to 1050 ℃ and preserving heat for 120min, then heating to 1300 ℃ at the speed of 10 ℃/min and preserving heat for 120min, then cooling to 1100 ℃ and pressurizing to 5MPa at constant temperature and preserving pressure for 5min, and cooling to room temperature along with the furnace to obtain the high-chromium cast iron-based composite material.
The properties of the high-chromium cast iron-based composite material prepared by the comparative example, such as Rockwell hardness (HRC, measured in at least 5 different positions and averaged), three-point bending strength, compression strength, impact toughness and the like, were tested, and the results showed that: the high-chromium cast iron-based composite material prepared by the comparative example has the hardness of HRC 55-60, the bending strength of 200 MPa-350 MPa, the compression strength of 700 MPa-900 MPa and the impact toughness of 5J/cm 2 ~8J/cm 2 。
Comparative example 2
This comparative example comprises the following steps:
step one, putting 180g of high-chromium cast iron powder into an agate grinding tank, filling agate grinding balls, performing low-speed ball milling and mixing for 15 hours under the conditions that the rotating speed is 150r/min and the ball-to-material ratio is 2:1, setting the mode to be that positive and negative rotation are alternately performed, and pausing for 10 minutes every 1 hour of ball milling to obtain the high-chromium cast iron powder subjected to low-speed ball milling; the high-chromium cast iron powder comprises the following components in percentage by mass: 2.0% of C, 30% of Cr, 0.5% of Si, 0.5% of Ni, 1.5% of B, 0.1% of V, 0.6% of Mn, 0.3% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 50-200 mu m;
secondly, putting the high-chromium cast iron powder subjected to low-speed ball milling obtained in the first step into a graphite die for cold pressing and preforming to obtain a pressed blank; the pressure of the cold pressing preforming is 10MPa, and the pressure maintaining time is 60 min;
and step three, performing vacuum hot-pressing sintering of stage heating on the pressed blank obtained in the step three, heating to 1050 ℃ and preserving heat for 120min, then heating to 1300 ℃ at the speed of 10 ℃/min and preserving heat for 120min, then cooling to 1100 ℃, pressurizing to 5MPa at constant temperature and maintaining pressure for 5min, and cooling to room temperature along with a furnace to obtain the high-chromium cast iron base material.
The high-chromium cast iron base material prepared by the comparative example is tested for properties such as Rockwell hardness (HRC, at least 5 different positions are measured and averaged), three-point bending strength, compressive strength and impact toughness, and the results show that: the hardness of the high-chromium cast iron-based material prepared by the comparative example is HRC 50-54, the bending strength is 250 MPa-350 MPa, and the material is compressedThe strength is 650MPa to 800MPa, and the impact toughness is 4J/cm 2 ~8J/cm 2 。
Comparing example 1 with comparative examples 1 and 2, it can be seen that TiC and TiB mixed in situ prepared in this example are more than the high chromium cast iron base material without the reinforcing phase added in comparative example 2 w TiC and TiB in-situ mixed in dual-phase ceramic reinforced iron-based composite material w The ceramic double reinforcing phases exert reinforcing effect, and the hardness, bending strength, compression strength and impact toughness of the ceramic double reinforcing phases are all improved; in comparative example 1, spherical Ti powder and irregular shape B were used 4 In the high-chromium cast iron-based composite material prepared by directly ball-milling and mixing the C powder and the high-chromium cast iron powder at a low speed, although the spherical Ti powder and the irregular B powder are mixed 4 In-situ reaction of C powder to produce TiC and TiB w Ceramic double reinforcing phases, but the two phases cannot be fully mixed because of large particle size difference, and uniformly dispersed TiC and TiB cannot be obtained w The ceramic double reinforced phase, therefore, the reinforced effect of the reinforced phase in the high-chromium cast iron-based composite material is limited, and the improvement degrees of the hardness, the bending strength, the compression strength and the impact toughness are all weaker than that of the application, which shows that the application adopts high-energy ball milling to form the ellipsoidal Ti powder outer wrapping B 4 The method of mixing, pressing and sintering the C powder and the high-chromium cast iron powder improves the TiC and TiB w The distribution uniformity of the ceramic double-reinforced phases in the high-chromium cast iron matrix and the bonding performance with the high-chromium cast iron matrix interface are fully exerted, thereby the TiC and TiB w The strengthening effect of the dual-phase ceramic reinforcing phase avoids the dual-phase ceramic reinforcing phase from peeling or falling off from the high-chromium cast iron matrix, and improves the hardness and the wear resistance of the composite material.
Example 2
The embodiment comprises the following steps:
step one, 167.8g of spherical Ti powder and 32.2g of irregular shape B 4 Putting the powder C into a vacuum stainless steel ball milling tank according to the mol ratio of 6:1, filling stainless steel grinding balls, performing high-energy ball milling and mixing for 6 hours under the conditions of vacuum condition, the rotating speed of 400r/min and the ball-material ratio of 10:1, setting the mode to be that positive and negative rotation are alternately performed, and pausing for 30 minutes every 1 hour of ball milling to obtain mixed powder A; the mixed powder A is ellipseSpherical Ti powder outer wrapping B 4 The structure of the C powder; the particle size of the spherical Ti powder is 70-130 mu m, and the spherical Ti powder is irregular B 4 The granularity of the C powder is 30-70 mu m;
step two, putting 18g of the mixed powder A obtained in the step one and 162g of high-chromium cast iron powder into an agate grinding tank, putting agate grinding balls into the agate grinding tank, performing low-speed ball milling and mixing for 10 hours under the conditions that the rotating speed is 200r/min and the ball-to-material ratio is 5:1, setting the mode to be that forward and reverse rotation are alternately performed, and pausing for 20 minutes every 1 hour of ball milling to obtain mixed powder B; the high-chromium cast iron powder comprises the following components in percentage by mass: 3.3% of C, 25% of Cr, 0.5% of Si, 0.2% of Ni, 1.0% of B, 0.05% of V, 0.3% of Mn, 0.1% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 200-350 mu m;
step three, putting the mixed powder B obtained in the step two into a graphite die for cold pressing and preforming to obtain a pressed blank; the pressure of the cold pressing preforming is 25MPa, and the pressure maintaining time is 30 min;
step four, putting the pressed compact obtained in the step three into a vacuum hot-pressing sintering furnace for vacuum hot-pressing sintering with stage heating, firstly heating to 1150 ℃ and preserving heat for 90min, then heating to 1400 ℃ at the speed of 10 ℃/min and preserving heat for 75min, then cooling to 1000 ℃ and pressurizing to 30MPa at constant temperature and preserving pressure for 60min, and cooling to room temperature along with the furnace to obtain in-situ TiC hybrid and TiB w A two-phase ceramic reinforced iron-based composite; in-situ TiC and TiB doping w The biphase ceramic reinforced iron-based composite material comprises a high-chromium cast iron matrix, TiC ceramic particles and TiB which are uniformly distributed in the high-chromium cast iron matrix and generated in situ w The ceramic particles are mixed with a reinforcing phase.
For the in-situ TiC and TiB mixture prepared in this example w The Rockwell hardness (HRC, at least 5 different positions are measured and an average value is taken) of the dual-phase ceramic reinforced iron-based composite material, the three-point bending strength, the compression strength, the impact toughness and other properties are detected, and the result shows that: in-situ TiC and TiB doping prepared in this example w The hardness of the two-phase ceramic reinforced iron-based composite material is HRC 65-70, the bending strength is 350 MPa-500 MPa, the compression strength is 900 MPa-1400 MPa, and the impact toughness is 7J/cm 2 ~12J/cm 2 。
FIG. 6 shows the in-situ TiC and TiB doping prepared in this example w The stress-strain curve of the two-phase ceramic reinforced iron-based composite material under the compression condition can be seen from FIG. 6, and the in-situ TiC and TiB are mixed w The compression strength of the two-phase ceramic reinforced iron-based composite material is 900 MPa-1400 MPa.
FIG. 7 shows the in-situ TiC and TiB doping process in this example w The appearance of the fracture of the biphase ceramic reinforced iron-based composite material after bending fracture is shown in the figure 7, in the circle, the in-situ generated reinforced TiC ceramic particles and TiB w Ceramic particles, as can be seen from FIG. 7, the composite material is brittle fracture, and TiC ceramic particles and TiB generated in situ w The ceramic particles are fine and only 1-3 μm.
Example 3
The embodiment comprises the following steps:
step one, 189.1g of spherical Ti powder and 10.9g of irregular shape B 4 Putting the powder C into a vacuum stainless steel ball milling tank according to a molar ratio of 20:1, filling stainless steel grinding balls, performing high-energy ball milling and mixing for 2 hours under the conditions of vacuum condition, the rotating speed of 500r/min and the ball-material ratio of 20:1, setting the mode to be that positive and negative rotation are alternately performed, and pausing for 60 minutes every 1 hour of ball milling to obtain mixed powder A; the mixed powder A is an ellipsoidal Ti powder outer wrapping B 4 C the structure of the powder; the particle size of the spherical Ti powder is 130-200 mu m, and the irregular shape B 4 The granularity of the C powder is 70-100 mu m;
step two, putting 9g of the mixed powder A obtained in the step one and 171g of high-chromium cast iron powder into an agate grinding tank, filling agate grinding balls, performing low-speed ball milling and mixing for 2 hours under the conditions that the rotating speed is 250r/min and the ball-to-material ratio is 10:1, setting the mode to be that forward and reverse rotation are alternately performed, and pausing for 10 minutes every 1 hour of ball milling to obtain mixed powder B; the high-chromium cast iron powder comprises the following components in percentage by mass: 2.2% of C, 11.0% of Cr, 1.0% of Si, 0.3% of Ni, 0.6% of B, 0.1% of Mn, 0.2% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 350-500 mu m;
step three, placing the mixed powder B obtained in the step two into a graphite die for cold pressing and preforming to obtain a pressed blank; the pressure of the cold pressing preforming is 50MPa, and the pressure maintaining time is 5 min;
step four, putting the pressed blank obtained in the step three into a vacuum hot-pressing sintering furnace for vacuum hot-pressing sintering with stage heating, firstly heating to 1250 ℃, preserving heat for 15min, then heating to 1550 ℃ at the rate of 20 ℃/min, preserving heat for 30min, then cooling to 850 ℃, pressurizing to 50MPa at constant temperature, preserving pressure for 120min, cooling to room temperature along with the furnace, and obtaining in-situ TiC and TiB w A two-phase ceramic reinforced iron-based composite; in-situ TiC and TiB doping w The biphase ceramic reinforced iron-based composite material comprises a high-chromium cast iron matrix, TiC ceramic particles and TiB which are uniformly distributed in the high-chromium cast iron matrix and generated in situ w The ceramic particles are mixed with a reinforcing phase.
TiC and TiB in situ doping prepared in this example w The Rockwell hardness (HRC, at least 5 different positions are measured and an average value is taken) of the dual-phase ceramic reinforced iron-based composite material, the three-point bending strength, the compression strength, the impact toughness and other properties are detected, and the result shows that: in-situ TiC and TiB doping prepared in this example w The hardness of the two-phase ceramic reinforced iron-based composite material is HRC 68-71, the bending strength is 450 MPa-600 MPa, the compression strength is 950 MPa-1150 MPa, and the impact toughness is 6J/cm 2 ~10J/cm 2 。
FIG. 8 shows the in-situ TiC and TiB doping prepared in this example w The stress-strain curve of the two-phase ceramic reinforced iron-based composite material under the compression condition can be seen from FIG. 8, and the in-situ TiC and TiB are mixed w The compression strength of the two-phase ceramic reinforced iron-based composite material is 950 MPa-1150 MPa.
FIG. 9 shows the in-situ TiC and TiB doping process in this example w The appearance of the fracture of the biphase ceramic reinforced iron-based composite material after bending fracture is shown in the figure 9, in the circle, the in-situ generated reinforced TiC ceramic particles and TiB w Ceramic particles, as can be seen from FIG. 9, the composite material is brittle fracture, and in-situ generated TiC ceramic particles and TiB w The ceramic particles are fine and only 1-3 μm.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (9)
1. The preparation method of the in-situ mixed dual-phase ceramic reinforced iron-based composite material is characterized by comprising the following steps of:
step one, mixing spherical Ti powder with irregular shape B 4 Putting the powder C into a stainless steel ball milling tank, and performing high-energy ball milling and mixing under a vacuum condition to obtain mixed powder A; the mixed powder A is an ellipsoidal Ti powder outer wrapping B 4 The structure of the C powder;
step two, putting the mixed powder A obtained in the step one and high-chromium cast iron powder into an agate grinding tank, and performing low-speed ball milling and mixing to obtain mixed powder B;
step three, placing the mixed powder B obtained in the step two into a graphite die for cold pressing and preforming to obtain a pressed blank;
step four, carrying out vacuum hot-pressing sintering of stage heating on the pressed compact obtained in the step three to obtain in-situ mixed TiC and TiB w A two-phase ceramic reinforced iron-based composite material.
2. The method for preparing an in-situ hybrid dual-phase ceramic reinforced iron-based composite material according to claim 1, wherein the particle size of the spherical Ti powder in the first step is 1-200 μm, and the irregular shape B is 4 The particle size of the C powder is 0.1-100 μm, and the spherical Ti powder and the irregular shape B 4 The molar ratio of the C powder is 2-20: 1.
3. The preparation method of the in-situ hybrid dual-phase ceramic reinforced iron-based composite material as claimed in claim 1, wherein the rotation speed for the high-energy ball milling mixing in the step one is 300r/min to 500r/min, the ball-to-material ratio is 2 to 20:1, the ball milling time is 2h to 10h, the mode is set to be that positive and negative rotation are alternately performed, and the ball milling is suspended for 10min to 60min every 1 h.
4. The method for preparing an in-situ hybrid dual-phase ceramic reinforced iron-based composite material according to claim 1, wherein the high-chromium cast iron powder in the second step comprises the following components in percentage by mass: 2.0-3.3% of C, 11.0-30.0% of Cr, 0-1.5% of Si, 0-0.5% of Ni, 0-1.5% of B, 0-0.1% of V, 0-0.6% of Mn, 0-0.3% of Mo and the balance of Fe; the particle size of the high-chromium cast iron powder is 50-500 mu m, and the mass ratio of the mixed powder to the high-chromium cast iron powder is 1: 2-19.
5. The method for preparing an in-situ hybrid dual-phase ceramic reinforced iron-based composite material according to claim 1, wherein the low-speed ball milling and mixing in the second step are performed at a rotation speed of 150r/min to 250r/min, a ball-to-material ratio of 2 to 10:1, a ball milling time of 2h to 15h, and a mode of alternating forward rotation and reverse rotation is set, and the ball milling is suspended for 10min to 30min every 1 h.
6. The method for preparing an in-situ hybrid dual-phase ceramic reinforced iron-based composite material according to claim 1, wherein the pressure of the cold pressing pre-forming in the third step is 10MPa to 50MPa, and the pressure holding time is 5min to 60 min.
7. The method for preparing an in-situ hybrid dual-phase ceramic reinforced iron-based composite material according to claim 1, wherein the vacuum hot-pressing sintering process of the step four with the temperature rise comprises the following steps: the temperature is increased to 1050-1250 ℃ and is preserved for 15-120 min, then the temperature is increased to 1300-1550 ℃ at the speed of 10-20 ℃/min and is preserved for 30-120 min, then the temperature is decreased to 850-1100 ℃, the pressure is increased to 5-50 MPa at constant temperature, the pressure is preserved for 5-120 min, and the temperature is cooled to room temperature along with the furnace.
8. An in-situ hybrid dual-phase ceramic reinforced iron-based composite material prepared by the method of any one of claims 1 to 7, wherein the composite material comprises a high-chromium cast iron matrix, and TiC ceramic particles and TiB which are uniformly distributed in the high-chromium cast iron matrix and are generated in situ w A ceramic particle mixed reinforcement phase; the in-situ mixed TiC and TiBw ceramic reinforced iron-based composite materialThe hardness of the material is HRC 65-73, the bending strength is 300 MPa-600 MPa, the compression strength is 900 MPa-1400 MPa, and the impact toughness is 6J/cm 2 ~12 J/cm 2 。
9. The in-situ hybrid dual-phase ceramic reinforced iron-based composite material of claim 8, wherein the in-situ formed TiC ceramic particles and TiB w The size of the ceramic particles is 1-3 μm.
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