CN114774759B - Layered gradient SiC ceramic reinforced iron-based wear-resistant material and preparation method thereof - Google Patents
Layered gradient SiC ceramic reinforced iron-based wear-resistant material and preparation method thereof Download PDFInfo
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- 238000007747 plating Methods 0.000 claims description 32
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
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- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2207/00—Aspects of the compositions, gradients
- B22F2207/01—Composition gradients
- B22F2207/03—Composition gradients of the metallic binder phase in cermets
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Abstract
The invention discloses a layered gradient SiC ceramic reinforced iron-based wear-resistant material and a preparation method thereof, belonging to the technical field of wear-resistant material preparation. The invention utilizes SiC ceramic particles with different scales and adds graphene as a sintering-aid phase to prepare the iron-based wear-resistant material. Firstly, uniformly mixing micron and millimeter double-scale SiC, graphene and iron powder by using a ball mill as the outermost layer of a layered material, then uniformly placing millimeter-grade SiC ceramic in the iron powder as the secondary outer layer, and finally, taking pure high-chromium iron powder as the middle layer. Finally forming the castellated layered iron-based SiC ceramic reinforced wear-resistant material with the outer layer, the secondary outer layer, the middle layer, the secondary outer layer and the outer layer. Aims to improve the wear resistance and hardness of the outer layer of the material and prolong the service life of the material, and the middle of the material has certain toughness and plasticity, thus being a high-efficiency and economical preparation technology for preparing the ceramic/metal wear-resistant material by industrialized prefabrication.
Description
Technical Field
The invention belongs to the technical field of wear-resistant material preparation, and particularly relates to a layered gradient SiC ceramic reinforced iron-based wear-resistant material and a preparation method thereof.
Background
Wear, as an important failure mode of service parts, has become a major bottleneck difficult to break through in the rapid development of related industries. The metal material consumed by the abrasion in China is about 300 million tons every year, and the direct economic loss caused by the abrasion is about more than 1000 billion yuan RMB. Therefore, the wear resistance of mechanical equipment and parts is improved, the operation cost of enterprises can be effectively reduced, and meanwhile, the improvement of the wear resistance can reduce production pause and cost increase caused by consumption of a large amount of manpower and material resources.
China is a big iron and steel country, wherein the abrasion loss of iron and steel materials is the most serious. At present, common wear-resistant steel materials comprise austenitic manganese steel, nickel hard cast iron, high-chromium cast iron and nodular cast iron, but the wear resistance of a single alloy reaches a bottleneck, and the wear resistance of the single alloy is difficult to further improve. Aiming at the situation, the ceramic material with high hardness and the iron-based alloy are effectively combined to prepare the ceramic/metal composite wear-resistant material, so that the ceramic/metal composite wear-resistant material has wide application prospect, and the high hardness, oxidation resistance and corrosion resistance of ceramic particles and the toughness of a metal matrix are combined in a high quality manner.
For ceramic reinforced metal composite materials, the addition of ceramic particles can effectively improve the strength and wear resistance of the materials, but inevitably at the expense of the plasticity of the materials. The comprehensive requirements of the actual working conditions on the wear resistance and the toughness of the surface layer of the material are high, and compared with the requirement, the core material is not in direct contact with the workpiece, the requirement on the strength is lower than that of the surface layer, and the specific surface of the toughness is higher.
Disclosure of Invention
Aiming at the problem of serious abrasion of the existing steel material, the invention provides a layered gradient SiC ceramic reinforced iron-based wear-resistant material and a preparation method thereof.
The invention provides a layered iron-based wear-resistant material, wherein the surface layer is formed by micron and millimeter double-scale SiC ceramic particles and doped with trace graphene to cooperatively enhance the iron-based wear-resistant material, so that the hardness of the surface layer is improved while higher plasticity is kept, the sub-outer layer structure is formed by the millimeter SiC particle enhanced iron-based composite material, and the middle layer is formed by iron-based alloy powder, so that the comprehensive improvement of the wear resistance, toughness and shock resistance of the composite material is finally realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a layered gradient SiC ceramic reinforced iron-based wear-resistant material comprises the following steps:
step 1, pretreating SiC ceramic particles;
step 2, carrying out chemical nickel plating on the pretreated ceramic particles;
step 4, mixing the SiC ceramic particles after the chemical nickel plating with iron powder to obtain mixed powder B;
step 5, layering and paving the mixed powder A, the mixed powder B and the iron powder into a die;
step 6, prepressing the mould paved in the step 5;
step 7, carrying out current-assisted sintering on the prepressed die to obtain a composite wear-resistant material;
and 8, polishing and cleaning the composite wear-resistant material to obtain the layered gradient SiC ceramic reinforced iron-based wear-resistant material.
Further, the step 1 of pretreating the SiC ceramic particles comprises: screening ceramic particles by using a 1 mm screen, gradually polishing the screened ceramic particles from coarse to fine by using 50-1500-mesh abrasive paper, putting the polished ceramic particles into 75% alcohol solution by volume percent, performing ultrasonic cleaning for 3-5 min at the ultrasonic frequency of 100kHz, cleaning by using deionized water, and drying until the surfaces are dried; and surface impurities and oil stains are removed, and the cleanness of a bonding interface of the ceramic particles and the metal matrix is ensured. Improve the wettability between the ceramic particles and the metal matrix, increase the bonding strength between the SiC particles and the matrix, and avoid the harmful reaction of impurities.
Further, the step 2 of performing chemical nickel plating on the pretreated ceramic particles comprises the following steps:
step a, soaking the pretreated ceramic particles in acetone for 5 min, sequentially soaking in 200 g/L sodium hydroxide solution and 2.4 mol/L hydrochloric acid solution for 22 min respectively, and carrying out ultrasonic cleaning for 3-5 min after each soaking;
b, putting the ceramic particles obtained in the step a into a stannous chloride acidic solution of 20 g/L, soaking for 2h at a constant temperature of 60 ℃, taking out, ultrasonically cleaning for 3-5 min, then putting into a palladium chloride solution of 0.5 g/L, soaking for 1h at a constant temperature of 60 ℃, and taking out;
and c, putting the ceramic particles obtained in the step b into a mixture of 20 g/L nickel chloride solution, 15 g/L sodium citrate solution, 10 g/L potassium sodium tartrate solution and 24 g/L sodium hypophosphite solution according to a volume ratio of 1: 1: 1: 1, magnetically stirring at a constant temperature of 56 ℃ for 3.5 hours, taking out and drying; drying the cleaned ceramic particles at the drying temperature of 110-120 ℃ for 5-8 min; ceramic particles contain a certain amount of moisture after electroless plating and are easily damaged during rework, and thus, in order to improve the strength of the ceramic particles, they are dried. After drying treatment, the ceramic particles have certain elasticity and strength. However, after excessive drying, the ceramic particles may re-adsorb moisture in the atmosphere to swell and crack. The above temperature ranges and drying times are most suitable after experimental tests.
The ratio of the ceramic particles to each solution in step c is 10 g/100 mL. The purpose of chemically plating nickel on the ceramic particles is to increase the wettability of the interface between the ceramic particles and the metal matrix, so that the interface between the ceramic particles and the metal matrix is more tightly combined, and the wear resistance of the prepared wear-resistant material is improved.
Further, in the step 3, the SiC ceramic particles after chemical nickel plating are mixed with iron powder and graphene, specifically, the SiC ceramic particles, the high-chromium cast iron powder and the graphene are mixed according to the volume ratio of 46-50: 48-52: 2. In the process that SiC ceramic particles after chemical nickel plating treatment are contacted with an iron powder matrix, the surface wettability is good, the interface bonding strength is improved, the residual stress at the interface is reduced, and compared with a ceramic reinforced composite material prepared by other methods, the ceramic reinforced composite material prepared by the method finally has good compactness and high bonding strength.
Further, the specific method for mixing in step 3 is as follows: putting SiC ceramic particles, high-chromium cast iron powder and graphene into a ball-milling tank, and then putting the ball-milling tank into a high-energy ball mill for high-energy ball-milling and mixing;
further, in the step 4, the SiC ceramic particles after the chemical nickel plating are mixed with iron powder, specifically, the SiC ceramic particles with the volume ratio of 1: 4-6 are mixed with high-chromium cast iron powder. According to different service environments and working condition requirements, SiC particle reinforced phases with different proportions can be flexibly added, for example, the proportion of the SiC particle reinforced phase can be properly increased for service environments with higher wear-resisting requirements.
Further, the specific method for mixing in step 4 is as follows: putting SiC ceramic particles and high-chromium cast iron powder into a ball-milling tank, and then putting the ball-milling tank into a high-energy ball mill for high-energy ball-milling and mixing; the rotation speed of the high-energy ball milling mixing is 1400 r/min, the time of the high-energy ball milling mixing is 10 h, and the ball mill stops for 15 min every time the ball mill rotates for 15 min; the step 5 is carried out in a vacuum glove box, wherein the mixed material is loaded into a graphite mold, the roughness of the inner wall of the graphite mold is Ra 0.06-0.15 mu m, and the size of the mold cavity is phi 30 mm multiplied by 70 mm;
further, in the step 5, the sequence of layered paving from bottom to top is as follows: the first layer of mixed powder A, the second layer of mixed powder B, the third layer of high-chromium cast iron powder, the fourth layer of mixed powder B and the fifth layer of mixed powder A. By designing different layer materials, the advantages of each layer are shown compared to a single layer material. The outermost layer is used as a wear-resistant layer, has higher wear resistance and meets the wear-resistant requirement. The secondary outer layer is used as a middle layer for reasonable gradient transition. The intermediate layer serves as a soft phase layer and plays a role of toughness when receiving a load such as impact or compression. The multiple layers are mutually matched, the advantages are fully realized, and the service life of the material in the whole service process is prolonged.
Further, the layered paving is performed from bottom to top, and the first layer of mixed powder A: second layer mixed powder B: third layer high chromium cast iron powder: fourth layer mixed powder B: the volume ratio of each layer of the fifth layer of mixed powder A is 2-6: 2-4: 3: 2-4: 2-6. Different thicknesses of each layer are designed to meet requirements under different service conditions, if the whole service environment has higher requirements on the wear resistance of the material, the outermost layer can be thicker, and if the requirements on the impact resistance and the compression performance are higher, the middle layer can be thicker.
Further, the mixed material is partially densified under the pre-pressing loading pressure of 5MPa in the step 6, so that the compactness of the mixed material is ensured to reach 70%.
Further, the current-assisted sintering in the step 7 is carried out in three stages in the pulse current sintering, wherein the first stage is sintering at 700 ℃ for 9 min, the second stage is sintering at 950 ℃ for 4 min, the third stage is heat preservation at 950 ℃ for 5 min, high-frequency pulse discharge, self-heat generation inside the powder and external water circulation cooling are carried out in the sintering process, and the vacuum degree is completed under the condition of being less than 4 Pa. Current produces a large amount of joule heat through mould and powder and is used for heating up in whole sintering process, and through the electric current of waiting to sinter the powder, because of there being the clearance between the initial stage powder granule, will produce spark discharge between the adjacent granule, some gas molecules are by ionization, and the positive ion and the electron that produce move to negative pole and positive pole respectively, along with ion density constantly increases, and the electric spark that produces between the granule is bigger and bigger for the oxide film on granule surface is broken, has reached the effect of purifying granule surface. Along with the completion of the purification of the particle surface, the discharge necking and the network bridging between the powder particles are promoted to form a sintering neck at the contact part of the powder particles under the action of high temperature and pressure. The sintering process is continuously carried out, and the skin effect of the current and the Joule formula know that the temperature of the particle surface is increased, the particle surface is locally melted to form a partial liquid phase, and the liquid phase is diffused to form rapid densification among particles under the action of pressure.
Further, the step 8 is to polish and clean the composite wear-resistant material, the composite wear-resistant material is placed on a smooth glass plane, the periphery of the composite material is sequentially and incrementally polished by abrasive paper from 50-1000 meshes and then wiped by alcohol solution with the volume percentage of 50%, and the iron-based wear-resistant material is naturally air-dried, so that the layered gradient SiC ceramic reinforced iron-based wear-resistant material is obtained.
The material prepared by the preparation method of the layered gradient SiC ceramic reinforced iron-based wear-resistant material.
Compared with the prior art, the invention has the following advantages:
1. compared with the materials such as austenitic manganese steel, nickel hard cast iron, high-chromium cast iron, nodular cast iron and the like obtained by an integral casting method, the material prepared by the method has better hardness and wear resistance. Compared with the melting by a blending method, the SiC ceramic reinforced iron-based wear-resistant material prepared by the invention does not have the phenomenon of uneven distribution of reinforcing phases such as segregation and agglomeration, and the prepared crystal grains are fine.
2. According to the method, graphene is used as a sintering-assisting phase and nickel is plated on the surface of the ceramic, so that the ceramic particles in the material are connected with an iron matrix more tightly, the porosity is smaller, the material is more compact, and the interface bonding quality is higher.
3. The method designs the 'hamburger-shaped' layered structure of the outer layer, the secondary outer layer, the middle layer, the secondary outer layer and the outer layer, thereby not only improving the surface wear resistance and hardness of the material, but also keeping the toughness and plasticity of the interior of the material and prolonging the service life of the material. Finally, the thickness of each layer of the layered composite material with the thickness of 11-23 mm is 2-6 mm, 2-4 mm, 3 mm, 2-4 mm and 2-6 mm respectively. And different thicknesses of each layer can be designed according to different service environments of materials, and the material has certain flexibility.
4. Compared with the traditional sintering method, the method of the invention adopts current-assisted sintering, because heat is provided by Joule heat, the powder is heated uniformly in the whole sintering process, the problems of segregation, coarse grains and the like do not occur, and the prepared material has uniform internal structure and fine grains. The current has certain activation and purification effects on the surfaces of the powder and the particles, and the connection performance between the powder, between the particles and the powder and between layers is good.
Drawings
FIG. 1 is a schematic view of a layered gradient SiC ceramic reinforced iron-based wear-resistant material according to the present invention.
FIG. 2 is a sectional view of the wire-cut layered gradient SiC ceramic reinforced iron-based wear-resistant material of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be specifically and specifically described below with reference to the embodiments of the present invention and the accompanying drawings. It should be noted that variations and modifications can be made by those skilled in the art without departing from the principle of the present invention, and these should also be construed as falling within the scope of the present invention.
Example 1
A preparation method of a layered gradient SiC ceramic reinforced iron-based wear-resistant material comprises the following steps:
step 1, pretreating SiC ceramic particles;
screening out ceramic particles with the diameter of about 1 mm by using a stainless steel screen with the diameter of 1 mm, and ensuring the granularity uniformity of the used ceramic particles; carrying out ultrasonic cleaning on the screened ceramic particles in 75% alcohol solution by volume percentage, carrying out ultrasonic treatment at 100kHz for 3 min, and removing surface impurities and oil stains to ensure that the bonding interface of the ceramic particles and the metal matrix is clean;
step 2, chemically plating nickel on SiC ceramic particles; the nickel plating step is as follows:
a. soaking the ceramic particles in acetone for 5 min, sequentially soaking in 200 g/L sodium hydroxide solution and 2.4 mol/L hydrochloric acid solution for 22 min, and performing ultrasonic cleaning after each soaking;
b. b, placing the ceramic particles obtained in the step a into a stannous chloride acidic solution of 20 g/L, soaking for 2 hours at a constant temperature of 60 ℃, taking out, ultrasonically cleaning, placing into a palladium chloride solution of 0.5 g/L, and soaking for 1 hour at a constant temperature of 60 ℃;
c. putting the ceramic particles obtained in the step b into a mixture of a nickel chloride solution of 20 g/L, a sodium citrate solution of 15 g/L, a potassium sodium tartrate solution of 10 g/L and a sodium hypophosphite solution of 24 g/L according to a volume ratio of 1: 1: 1: 1, magnetically stirring at a constant temperature of 56 ℃ for 3.5 hours, taking out and drying;
the ratio of ceramic particles to each solution was 10 g/100 mL.
placing the SiC ceramic particles subjected to chemical nickel plating in an oven for drying, wherein the temperature of the oven is set to be 110 ℃, and the holding time is 5 min;
step 4, filling the SiC ceramic particles, the high-chromium cast iron powder and the graphene into a ball-milling tank, and then placing the ball-milling tank into a high-energy ball mill for high-energy ball-milling mixing; wherein the volume ratio of the SiC ceramic particles, the high-chromium cast iron powder and the graphene filled in the ball milling tank is 46:52: 2. The rotation speed of the high-energy ball milling mixing is 1400 r/min, the time of the high-energy ball milling mixing is 10 h, wherein the ball mill rotates for 15 min and stops for 15 min.
Step 5, mixing the SiC ceramic particles obtained in the step 3 with high-chromium cast iron powder to form a mixed material;
firstly, putting dried SiC ceramic particles and high-chromium iron powder into a ball-milling tank according to the volume ratio of 1: 4, wherein the ball-milling parameters are as follows: the ball milling speed is 1400 r/min, the ball milling time is 10 h, wherein the ball milling is stopped for 15 min after 15 min, iron-based powder with a certain thickness is uniformly attached to the surface of the nickel-plated ceramic particles, a high-quality ceramic/nickel/alloy bonding interface is formed, the interface can be formed while the direct contact of the ceramic particles is avoided, and the wear resistance of the whole material is further ensured;
step 6, filling the mixed material into a graphite mold in a vacuum glove box; the roughness of the inner wall of the graphite mould is Ra 0.06-0.15 μm, and the size of the mould cavity is phi 30 mm multiplied by 70 mm;
mixing the SiC ceramic particles after chemical nickel plating with iron powder and graphene to obtain mixed powder A; mixing the SiC ceramic particles after chemical nickel plating with iron powder to obtain mixed powder B;
the mixed material sequence is a layer of mixed powder A, a layer of mixed powder B, a layer of high-chromium cast iron powder, a layer of mixed powder B and a layer of mixed powder A, the mixed powder A is laid layer by layer from bottom to top, and the volume ratio of each layer is 2: 4: 3: 4: 2;
step 7, putting the graphite mold filled with the mixed material into a press machine for prepressing;
placing the graphite mold filled with the mixed material under a press, and loading the pressure to 5MPa to partially densify the mixed material to ensure that the density of the mixed material reaches 70%;
step 8, sintering the pulse current to form the composite wear-resistant material;
the pulse current sintering comprises the following specific steps:
opening a furnace door of a pulse current sintering furnace, placing a graphite mold filled with mixed powder on a lower electrode, ensuring that the graphite mold and the lower electrode are centered and in close contact, placing an upper electrode above the graphite mold, adjusting the vertical displacement of the upper electrode, loading a little pressure to ensure that the graphite mold and the upper and lower electrodes are centered and in close contact, and then closing the furnace door;
starting a vacuum pump switch, vacuumizing the furnace chamber, and keeping the vacuum degree in the furnace chamber to be less than 5 Pa;
starting an external water cooling circulation system to cool the whole sintering furnace system;
starting a power switch of the pulse current sintering device, loading the sintering pressure to 40 MPa, setting the sintering temperature to 950 ℃ and keeping the temperature for 5 min; sintering the mixed material by pulse current to obtain a layered gradient SiC ceramic reinforced iron-based composite wear-resistant material;
closing a power switch of the pulse current sintering device to slowly cool the sintering furnace system, and closing a vacuum pump switch when the temperature of the graphite mold is cooled to be below 150 ℃;
sixthly, opening the furnace door of the pulse current sintering furnace, adjusting the vertical direction of the upper electrode to move upwards, taking out the graphite mold, and closing the furnace door of the sintering furnace.
Step 9, polishing and cleaning the composite wear-resistant material;
and (3) placing the composite wear-resistant material on a smooth glass plane, sequentially and progressively grinding the periphery of the composite material by using abrasive paper from 50-1000 meshes, polishing, wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the layered gradient SiC ceramic reinforced iron-based wear-resistant material.
Example 2
A preparation method of a layered gradient SiC ceramic reinforced iron-based wear-resistant material comprises the following steps:
step 1, pretreating SiC ceramic particles;
screening out ceramic particles with the diameter of about 1 mm by using a stainless steel screen with the diameter of 1 mm, and ensuring the granularity uniformity of the used ceramic particles; carrying out ultrasonic cleaning on the screened ceramic particles in 75% alcohol solution by volume percentage, carrying out ultrasonic treatment at 100kHz for 5 min, and removing surface impurities and oil stains to ensure that the bonding interface of the ceramic particles and the metal matrix is clean;
step 2, chemically plating nickel on SiC ceramic particles; the nickel plating step is as follows:
a. soaking the ceramic particles in acetone for 5 min, sequentially soaking in 200 g/L sodium hydroxide solution and 2.4 mol/L hydrochloric acid solution for 22 min, and performing ultrasonic cleaning after each soaking;
b. b, placing the ceramic particles obtained in the step a into a stannous chloride acidic solution of 20 g/L, soaking for 2 hours at a constant temperature of 60 ℃, taking out, ultrasonically cleaning, placing into a palladium chloride solution of 0.5 g/L, and soaking for 1 hour at a constant temperature of 60 ℃;
c. putting the ceramic particles obtained in the step b into a mixture of a nickel chloride solution of 20 g/L, a sodium citrate solution of 15 g/L, a potassium sodium tartrate solution of 10 g/L and a sodium hypophosphite solution of 24 g/L according to a volume ratio of 1: 1: 1: 1, magnetically stirring at a constant temperature of 56 ℃ for 3.5 hours, taking out and drying;
the ratio of ceramic particles to each solution was 10 g/100 mL.
placing the SiC ceramic particles subjected to chemical nickel plating in an oven for drying, wherein the temperature of the oven is set to be 120 ℃, and the holding time is 8 min;
step 4, filling the SiC ceramic particles, the high-chromium cast iron powder and the graphene into a ball-milling tank, and then placing the ball-milling tank into a high-energy ball mill for high-energy ball-milling mixing; wherein the volume ratio of the SiC ceramic particles, the high-chromium cast iron powder and the graphene filled in the ball milling tank is 50:50: 2. The rotation speed of the high-energy ball milling mixing is 1400 r/min, the time of the high-energy ball milling mixing is 10 h, wherein the ball mill rotates for 15 min and stops for 15 min.
Step 5, mixing the SiC ceramic particles obtained in the step 3 with high-chromium cast iron powder to form a mixed material;
firstly, mixing dried SiC ceramic particles and high-chromium iron powder according to the volume ratio of 1: 6, putting the mixture into a ball milling tank, wherein the ball milling parameters are as follows: the ball milling speed is 1400 r/min, the ball milling time is 10 h, wherein the ball milling is stopped for 15 min after 15 min, iron-based powder with a certain thickness is uniformly attached to the surface of the nickel-plated ceramic particles, a high-quality ceramic/nickel/alloy bonding interface is formed, the interface can be formed while the direct contact of the ceramic particles is avoided, and the wear resistance of the whole material is further ensured;
step 6, filling the mixed material into a graphite mold in a vacuum glove box; the roughness of the inner wall of the graphite mould is Ra 0.06-0.15 μm, and the size of the mould cavity is phi 30 mm multiplied by 70 mm;
mixing the SiC ceramic particles subjected to chemical nickel plating with iron powder and graphene to obtain mixed powder A; mixing the SiC ceramic particles after chemical nickel plating with iron powder to obtain mixed powder B;
the mixed material comprises a layer of mixed powder A, a layer of mixed powder B, a layer of high-chromium cast iron powder, a layer of mixed powder B and a layer of mixed powder A which are sequentially laid from bottom to top, wherein the volume ratio of each layer is 6:2:3:2: 6.
Step 7, putting the graphite mold filled with the mixed material into a press machine for prepressing;
placing the graphite mold filled with the mixed material under a press, and loading the pressure to 5MPa to partially densify the mixed material to ensure that the density of the mixed material reaches 70%;
step 8, sintering the pulse current to form the composite wear-resistant material;
the pulse current sintering comprises the following specific steps:
opening a furnace door of a pulse current sintering furnace, placing a graphite mold filled with mixed powder on a lower electrode, ensuring that the graphite mold and the lower electrode are centered and in close contact, placing an upper electrode above the graphite mold, adjusting the vertical displacement of the upper electrode, loading a little pressure to ensure that the graphite mold and the upper and lower electrodes are centered and in close contact, and then closing the furnace door;
secondly, starting a vacuum pump switch, vacuumizing the furnace chamber, and keeping the vacuum degree in the furnace chamber to be less than 4 Pa;
starting an external water cooling circulation system to cool the whole sintering furnace system;
starting a power switch of the pulse current sintering device, loading the sintering pressure to 40 MPa, setting the sintering temperature to 950 ℃ and keeping the temperature for 5 min; the mixed material is sintered by pulse current to form a layered gradient SiC ceramic reinforced iron-based composite wear-resistant material;
closing a power switch of the pulse current sintering device to slowly cool the sintering furnace system, and closing a vacuum pump switch when the temperature of the graphite mold is cooled to be below 150 ℃;
sixthly, opening the furnace door of the pulse current sintering furnace, adjusting the vertical direction of the upper electrode to move upwards, taking out the graphite mold, and closing the furnace door of the sintering furnace.
Step 9, polishing and cleaning the composite wear-resistant material;
and (3) placing the composite wear-resistant material on a smooth glass plane, sequentially and progressively grinding the periphery of the composite material by using abrasive paper from 50-1000 meshes, polishing, wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the layered gradient SiC ceramic reinforced iron-based wear-resistant material.
Example 3
A preparation method of a layered gradient SiC ceramic reinforced iron-based wear-resistant material comprises the following steps:
step 1, pretreating SiC ceramic particles;
screening out ceramic particles with the diameter of about 1 mm by using a stainless steel screen with the diameter of 1 mm, and ensuring the granularity uniformity of the used ceramic particles; carrying out ultrasonic cleaning on the screened ceramic particles in 75% alcohol solution by volume percentage, carrying out ultrasonic treatment at 100kHz for 5 min, and removing surface impurities and oil stains to ensure that the bonding interface of the ceramic particles and the metal matrix is clean;
step 2, chemically plating nickel on SiC ceramic particles; the nickel plating step is as follows:
a. soaking the ceramic particles in acetone for 5 min, sequentially soaking in 200 g/L sodium hydroxide solution and 2.4 mol/L hydrochloric acid solution for 22 min, and performing ultrasonic cleaning after each soaking;
b. b, placing the ceramic particles obtained in the step a into a stannous chloride acidic solution of 20 g/L, soaking for 2 hours at a constant temperature of 60 ℃, taking out, ultrasonically cleaning, placing into a palladium chloride solution of 0.5 g/L, and soaking for 1 hour at a constant temperature of 60 ℃;
c. putting the ceramic particles obtained in the step b into a mixture of a nickel chloride solution of 20 g/L, a sodium citrate solution of 15 g/L, a potassium sodium tartrate solution of 10 g/L and a sodium hypophosphite solution of 24 g/L according to a volume ratio of 1: 1: 1: 1, magnetically stirring at a constant temperature of 56 ℃ for 3.5 hours, taking out and drying;
the ratio of ceramic particles to each solution was 10 g/100 mL.
placing the SiC ceramic particles subjected to chemical nickel plating in an oven for drying, wherein the temperature of the oven is set to be 115 ℃, and the holding time is 7 min;
step 4, filling the SiC ceramic particles, the high-chromium cast iron powder and the graphene into a ball-milling tank, and then placing the ball-milling tank into a high-energy ball mill for high-energy ball-milling mixing; wherein the volume ratio of the SiC ceramic particles, the high-chromium cast iron powder and the graphene filled in the ball milling tank is 48:52: 2. The rotation speed of the high-energy ball milling mixing is 1400 r/min, the time of the high-energy ball milling mixing is 10 h, wherein the ball mill rotates for 15 min and stops for 15 min.
Step 5, mixing the SiC ceramic particles obtained in the step 3 with high-chromium cast iron powder to form a mixed material;
firstly, mixing dried SiC ceramic particles and high-chromium iron powder according to the volume ratio of 1: 5, putting the mixture into a ball milling tank, wherein the ball milling parameters are as follows: the ball milling speed is 1400 r/min, the ball milling time is 10 h, wherein the ball milling is stopped for 15 min after 15 min, iron-based powder with a certain thickness is uniformly attached to the surface of the nickel-plated ceramic particles, a high-quality ceramic/nickel/alloy bonding interface is formed, the interface can be formed while the direct contact of the ceramic particles is avoided, and the wear resistance of the whole material is further ensured;
step 6, filling the mixed material into a graphite mold in a vacuum glove box; the roughness of the inner wall of the graphite mould is Ra 0.06-0.15 μm, and the size of the mould cavity is phi 30 mm multiplied by 70 mm;
mixing the SiC ceramic particles after chemical nickel plating with iron powder and graphene to obtain mixed powder A; mixing the SiC ceramic particles after chemical nickel plating with iron powder to obtain mixed powder B;
the mixed material comprises a layer of mixed powder A, a layer of mixed powder B, a layer of high-chromium cast iron powder, a layer of mixed powder B and a layer of mixed powder A which are sequentially laid from bottom to top, wherein the volume ratio of each layer is 5:3:3:3: 5.
Step 7, putting the graphite mold filled with the mixed material into a press machine for prepressing;
placing the graphite mold filled with the mixed material under a press, and loading the pressure to 4 MPa to partially densify the mixed material, so as to ensure that the compactness of the mixed material reaches 70%;
step 8, sintering the pulse current to form the composite wear-resistant material;
the pulse current sintering comprises the following specific steps:
opening a furnace door of a pulse current sintering furnace, placing a graphite mold filled with mixed powder on a lower electrode, ensuring that the graphite mold and the lower electrode are centered and in close contact, placing an upper electrode above the graphite mold, adjusting the vertical displacement of the upper electrode, loading a little pressure to ensure that the graphite mold and the upper and lower electrodes are centered and in close contact, and then closing the furnace door;
secondly, starting a vacuum pump switch, vacuumizing the furnace chamber, and keeping the vacuum degree in the furnace chamber to be less than 4 Pa;
starting an external water cooling circulation system to cool the whole sintering furnace system;
starting a power switch of the pulse current sintering device, loading the sintering pressure to 40 MPa, setting the sintering temperature to 950 ℃ and keeping the temperature for 5 min; sintering the mixed material by pulse current to obtain a layered gradient SiC ceramic reinforced iron-based composite wear-resistant material;
closing a power switch of the pulse current sintering device to slowly cool the sintering furnace system, and closing a vacuum pump switch when the temperature of the graphite mold is cooled to be below 150 ℃;
sixthly, opening the furnace door of the pulse current sintering furnace, adjusting the vertical direction of the upper electrode to move upwards, taking out the graphite mold, and closing the furnace door of the sintering furnace.
Step 9, polishing and cleaning the composite wear-resistant material;
and (3) placing the composite wear-resistant material on a smooth glass plane, sequentially and progressively grinding the periphery of the composite material by using abrasive paper from 50-1000 meshes, polishing, wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the layered gradient SiC ceramic reinforced iron-based wear-resistant material.
In conclusion, the method can design different thicknesses of each layer according to different service environments of materials, has certain flexibility, and ensures that the surface layer is micron and millimeter double-scale SiC ceramic particles and is doped with trace graphene to cooperatively reinforce the iron-based wear-resistant material, so that the hardness of the surface layer is improved and the surface layer keeps higher plasticity; the secondary outer layer tissue is millimeter SiC particle reinforced iron-based composite material, the middle layer is iron-based alloy powder, and finally the comprehensive improvement of the wear resistance, toughness and impact resistance of the composite material is realized; see in particular tables 1 and 2.
Table 1 physical properties of the examples
Table 2 hardness parameters of each layer in example three
| Outermost layer | Second outer layer | Intermediate layer | |
| Hardness (HV) | 677.9 | 614.2 | 569.9 |
Those skilled in the art will appreciate that the invention may be practiced without these specific details. Although illustrative embodiments of the present invention have been described above to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, and various changes may be made apparent to those skilled in the art as long as they are within the spirit and scope of the present invention as defined and defined by the appended claims, and all matters of the invention which utilize the inventive concepts are protected.
Claims (6)
1. A preparation method of a layered gradient SiC ceramic reinforced iron-based wear-resistant material is characterized by comprising the following steps: the method comprises the following steps:
step 1, pretreating SiC ceramic particles;
step 2, carrying out chemical nickel plating on the pretreated ceramic particles;
step 3, mixing the SiC ceramic particles after the chemical nickel plating with iron powder and graphene to obtain mixed powder A;
step 4, mixing the SiC ceramic particles after the chemical nickel plating with iron powder to obtain mixed powder B;
step 5, layering and paving the mixed powder A, the mixed powder B and the iron powder into a die;
step 6, prepressing the mould paved in the step 5;
step 7, carrying out current-assisted sintering on the prepressed die to obtain a composite wear-resistant material;
step 8, polishing and cleaning the composite wear-resistant material to obtain a layered gradient SiC ceramic reinforced iron-based wear-resistant material;
mixing the SiC ceramic particles after the chemical nickel plating with iron powder and graphene, specifically mixing the SiC ceramic particles, high-chromium cast iron powder and graphene in a volume ratio of 46-50: 48-52: 2;
step 4, mixing the SiC ceramic particles after the chemical nickel plating with iron powder, specifically mixing the SiC ceramic particles with a volume ratio of 1: 4-6 with high-chromium cast iron powder;
the step 5 of laying layer by layer from bottom to top is as follows: a first layer of mixed powder A, a second layer of mixed powder B, a third layer of high-chromium cast iron powder, a fourth layer of mixed powder B and a fifth layer of mixed powder A;
the layered pavement is paved from bottom to top, and the first layer of mixed powder A: second layer mixed powder B: third layer high chromium cast iron powder: fourth layer mixed powder B: and the fifth layer of the mixed powder A has a volume ratio of 2-6: 2-4: 3: 2-4: 2-6.
2. The method for preparing the layered gradient SiC ceramic reinforced iron-based wear-resistant material according to claim 1, wherein the method comprises the following steps: the step 2 of chemically plating nickel on the pretreated ceramic particles comprises the following steps:
step a, putting pretreated ceramic particles into acetone for soaking for 5 min, sequentially soaking in 200 g/L sodium hydroxide solution and 2.4 mol/L hydrochloric acid solution for 22 min respectively, and carrying out ultrasonic cleaning for 3-5 min after each soaking;
b, putting the ceramic particles obtained in the step a into a stannous chloride acidic solution of 20 g/L, soaking for 2h at a constant temperature of 60 ℃, taking out, ultrasonically cleaning for 3-5 min, then putting into a palladium chloride solution of 0.5 g/L, soaking for 1h at a constant temperature of 60 ℃, and taking out;
and c, putting the ceramic particles obtained in the step b into a mixture of a nickel chloride solution of 20 g/L, a sodium citrate solution of 15 g/L, a potassium sodium tartrate solution of 10 g/L and a sodium hypophosphite solution of 24 g/L according to a volume ratio of 1: 1: 1: 1, magnetically stirring at a constant temperature of 56 ℃ for 3.5 hours, taking out and drying; drying the cleaned ceramic particles at the drying temperature of 110-120 ℃ for 5-8 min;
the ratio of the ceramic particles to each solution in step c is 10 g/100 mL.
3. The method for preparing the layered gradient SiC ceramic reinforced iron-based wear-resistant material according to claim 2, wherein the method comprises the following steps: and 7, the current-assisted sintering is carried out in a pulse current sintering device in three stages, wherein the first stage is sintering at 700 ℃ for 9 min, the second stage is sintering at 950 ℃ for 4 min, the third stage is heat preservation at 950 ℃ for 5 min, high-frequency pulse discharge, self-heat generation inside the powder and external water circulation cooling are carried out in the sintering process, and the vacuum degree is less than 4 Pa.
4. The method for preparing the layered gradient SiC ceramic reinforced iron-based wear-resistant material according to claim 3, wherein the method comprises the following steps: the step 1 of pretreating the SiC ceramic particles comprises the following steps: screening ceramic particles by using a 1 mm screen, gradually polishing the screened ceramic particles from coarse to fine by using 50-1500-mesh abrasive paper, putting the polished ceramic particles into 75% alcohol solution by volume percent, performing ultrasonic cleaning for 3-5 min at the ultrasonic frequency of 100kHz, cleaning by using deionized water, and drying until the surfaces are dried;
and 8, polishing and cleaning the composite wear-resistant material, namely placing the composite wear-resistant material on a smooth glass plane, sequentially and progressively polishing the periphery of the composite material by using abrasive paper from 50-1000 meshes, then wiping the composite material by using an alcohol solution with the volume percentage of 50%, and naturally drying to obtain the layered gradient SiC ceramic reinforced iron-based wear-resistant material.
5. The method for preparing the layered gradient SiC ceramic reinforced iron-based wear-resistant material according to claim 4, wherein the step of preparing the layered gradient SiC ceramic reinforced iron-based wear-resistant material comprises the following steps: the specific method for mixing in the step 3 is as follows: putting SiC ceramic particles, high-chromium cast iron powder and graphene into a ball-milling tank, and then placing the ball-milling tank into a high-energy ball mill for high-energy ball-milling mixing; the specific method for mixing in the step 4 is as follows: putting SiC ceramic particles and high-chromium cast iron powder into a ball-milling tank, and then putting the ball-milling tank into a high-energy ball mill for high-energy ball-milling and mixing; the rotation speed of the high-energy ball milling mixing is 1400 r/min, the time of the high-energy ball milling mixing is 10 h, and the ball mill stops for 15 min every time the ball mill rotates for 15 min; the step 5 is carried out in a vacuum glove box, wherein the mixed material is loaded into a graphite mold, the roughness of the inner wall of the graphite mold is Ra 0.06-0.15 mu m, and the size of the mold cavity is phi 30 mm multiplied by 70 mm; and (3) partially densifying the mixed material under the pre-pressing loading pressure of 5MPa in the step 6, and ensuring that the compactness of the mixed material reaches 70%.
6. A material prepared by the preparation method of the layered gradient SiC ceramic reinforced iron-based wear-resistant material as claimed in any one of claims 1 to 5.
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