CN111876697B - Multi-scale self-lubricating tungsten carbide-based composite material and preparation method thereof - Google Patents

Multi-scale self-lubricating tungsten carbide-based composite material and preparation method thereof Download PDF

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CN111876697B
CN111876697B CN202010577689.XA CN202010577689A CN111876697B CN 111876697 B CN111876697 B CN 111876697B CN 202010577689 A CN202010577689 A CN 202010577689A CN 111876697 B CN111876697 B CN 111876697B
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lubricating
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CN111876697A (en
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钟黎声
朱建雷
赵梓源
许云华
梁淑华
邹军涛
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Xian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
    • C22C47/062—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element from wires or filaments only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments

Abstract

The invention discloses a multi-scale self-lubricating tungsten carbide-based composite material, which consists of multi-scale particles and metal Nb fibers distributed in a net structure, wherein the multi-scale particles are distributed around the metal Nb fibers, the multi-scale particles comprise micron-sized WC particles, dispersedly distributed submicron-sized NbC particles, a uniformly distributed self-lubricating phase and a binding phase, the volume fraction of the micron-sized WC particles in the composite material is 60-80%, the volume fraction of the self-lubricating phase is 2.2-10%, the volume fraction of the submicron-sized NbC particles is 10-20%, the volume fraction of the binding phase is 2-10%, the volume fraction of the metal Nb fibers is 5-10%, and the sum of the volume percentages of the components is 100%. The invention also discloses a preparation method of the multi-scale self-lubricating tungsten carbide-based composite material, and the prepared multi-scale self-lubricating tungsten carbide-based composite material has the characteristics of high strength and wear resistance of the traditional self-lubricating wear-resistant ceramic material, and has good toughness and damage tolerance performance.

Description

Multi-scale self-lubricating tungsten carbide-based composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of metal ceramic composite materials, and relates to a multi-scale self-lubricating tungsten carbide-based composite material and a preparation method thereof.
Background
Under severe working conditions such as high temperature, high abrasion, high corrosion environment and the like, the material is required to have high strength and toughness, high wear resistance and corrosion resistance. Under such conditions, cermets are desirable materials. And further, a solid lubricating medium is added into a metal ceramic system to prepare the self-lubricating metal ceramic, so that the self-lubricating metal ceramic has high abrasion resistance and can realize self-lubrication on a friction surface.
At present, the metal ceramic wear-resistant material has wide application in the aspects of automobiles, high-speed rails, high-speed mechanical brake pads and the like. But certain micropores must exist in the metal ceramics to realize self-lubrication and are used as a lubricating medium diffusion channel. However, for the cermet, the fracture toughness of the cermet itself is low, and a microporous structure must exist in the material to realize the self-lubricating function, the micropores increase the porosity and the crack source of the material, and the microporous structure further deteriorates the mechanical properties of the material. Therefore, the self-lubricating function of the cermet material system is realized, the toughness of the material is not reduced, and the method is a technical difficulty for preparing the self-lubricating cermet matrix composite.
Therefore, the preparation of the high-strength high-toughness self-lubricating metal ceramic matrix composite material has important significance for the development of wear-resistant ceramic materials.
Disclosure of Invention
The invention aims to provide a multi-scale self-lubricating tungsten carbide-based composite material, which solves the problems that the existing metal ceramic material has poor toughness and high sudden fracture failure frequency.
The invention also aims to provide a preparation method of the multi-scale self-lubricating tungsten carbide-based composite material.
The first technical scheme adopted by the invention is that the multi-scale self-lubricating tungsten carbide-based composite material consists of a matrix and metal Nb fibers distributed in a net structure, wherein the matrix comprises micron-sized WC particles, submicron-sized NbC particles in dispersion distribution, a self-lubricating phase and a binding phase in uniform distribution.
The present invention is also technically characterized in that,
the volume fraction of micron-sized WC particles in the composite material is 60-80%, the volume fraction of self-lubricating phase is 2.2-10%, the volume fraction of submicron NbC particles is 10-20%, the volume fraction of binding phase is 2-10%, the volume fraction of metal Nb fiber is 5-10%, and the sum of the volume percentages of the above components is 100%.
Self-lubricating phase consisting of graphite and MoS2The composition of the binding phase is Fe.
The grain diameter of the micron-sized WC particles is 20-30 μm, and the grain diameter of the submicron NbC particles is 500-900 nm.
The diameter of the metal Nb fiber is 300-700 mu m.
The second technical scheme adopted by the invention is that the preparation method of the multi-scale self-lubricating tungsten carbide-based composite material comprises the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder;
step 2: the WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS which are weighed in the step 12Uniformly mixing the powder to form mixed powder;
and step 3: adding paraffin powder into the mixed powder, and then putting the mixed powder into a mixing roll for mixing treatment to form uniform materials;
and 4, step 4: adopting refractory metal Nb fibers to prefabricate a net structure to form a refractory metal fiber net;
and 5: preliminarily laying the mixed material and the fiber mesh layer by layer in a mould to form a prefabricated body, wherein the distance between fiber mesh layers in the prefabricated body is 1-5 mm;
step 6: and (3) placing the prefabricated body in a high-temperature die, then assembling the prefabricated body in a high-temperature sintering furnace for isothermal hot-pressing sintering, and finally cooling and demolding to obtain the multi-scale self-lubricating tungsten carbide-based composite material.
In step 4, the fiber diameter of the fiber in the refractory metal fiber net is 600-1000 μm, and the fiber distance in the fiber net is 3-6 times of the fiber diameter.
In the step 6, in the isothermal hot-pressing sintering process, the furnace temperature is firstly increased to 800 ℃ for degreasing treatment, then the furnace temperature is increased to 1165 ℃ and 1250 ℃ for heat preservation for 0.2h-2h, then the temperature is reduced to 1100 ℃ for heat preservation for 4-8h, and finally the temperature is cooled to the room temperature.
And 6, in the isothermal hot-pressing sintering process, the temperature rise speed in the high-temperature sintering furnace is 5-10 ℃/min, and in the cooling process, the temperature drop speed in the high-temperature sintering furnace is 2-5 ℃/min.
In step 6, the furnace pressure is 5-10MPa at 1165-1250 ℃, and the furnace pressure is 20-50MPa in the isothermal treatment process at 1100 ℃.
The invention has the beneficial effects that the tungsten carbide-based composite material consists of particles and metal fibers distributed in a net shape, the particles with different sizes are uniformly distributed around the metal fibers, and the particles comprise micron-sized WC particles, dispersedly distributed submicron-sized NbC particles and uniformly distributed self-lubricating phase MoS2And a binding phase Fe, a self-lubricating phase consisting of graphite and MoS2Composition, graphite and MoS2The self-lubricating material has good self-lubricating effect, and micropores in the matrix provide diffusion channels for self-lubricating phases; the micron-sized WC particles and the submicron-sized carbide particles in the matrix have larger size difference, so that cracks on the material have different expansion and deflection mechanisms among particles with different phases and sizes, and the effect of multi-scale toughening is achieved; the metal Nb fiber has higher shaping, can absorb local excessive residual stress, provides high-efficiency fiber toughening effect, enables the multi-scale self-lubricating tungsten carbide-based composite material to have the characteristics of high strength, wear resistance and the like of the traditional self-lubricating wear-resistant ceramic material, and greatly improves the toughness of the traditional self-lubricating metal ceramic material through the synergistic effect of multi-scale strengthening and toughening of the fiber, so that the composite material has good damage tolerance performance; the wear-resistant material can be widely applied to wear-resistant parts such as brake discs, wear-resistant shaft sleeves and wear-resistant pipe fittings, and has wide application prospect.
Drawings
FIG. 1 is a schematic view of the local microstructure of the multi-scale self-lubricating tungsten carbide-based composite material of the present invention;
FIG. 2 is a sectional macroscopic view of the multi-scale self-lubricating tungsten carbide-based composite material prepared in example 1 of the present invention;
FIG. 3 is a sectional high magnification microstructure of the multi-scale self-lubricating tungsten carbide-based composite material prepared in example 1 of the present invention.
In the figure, 1, metal Nb fiber, 2, submicron NbC particle, 3, binding phase, 4, micron WC particle, and 5, self-lubricating phase.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a multi-scale self-lubricating tungsten carbide-based composite material, which is shown in figure 1 and consists of a matrix andcomposed of metal Nb fibers 1 distributed in a net structure, a substrate comprises micron-sized WC particles 4, submicron-sized NbC particles 2 distributed in a dispersed manner, a self-lubricating phase 5 and a binding phase 3 distributed uniformly, wherein the self-lubricating phase 5 comprises graphite and MoS2The binder phase 3 is Fe.
In the composite material, the volume fraction of micron-sized WC particles 4 is 60-80%, the volume fraction of self-lubricating phase 5 is 2.2-10%, the volume fraction of submicron NbC particles 2 is 10-20%, the volume fraction of binding phase 3 is 2-10%, the volume fraction of metal Nb fiber 1 is 5-10%, and the sum of the volume percentages of the above components is 100%.
The grain diameter of the micron-sized WC particles 4 is 20-30 μm, the grain diameter of the submicron-sized NbC particles 2 is 500-900 nm, the metal Nb fiber 1 is a refractory metal fiber, the melting point is high, and the diameter of the metal Nb fiber is 300-700 μm.
The invention relates to a preparation method of a multi-scale self-lubricating tungsten carbide-based composite material, which comprises the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder; wherein, the mass percent of WC particles is 53-76%, the mass percent of Fe powder is 3.1-14%, the mass percent of Nb powder is 9.5-19%, the mass percent of graphite powder is 0.2-4.5%, MoS2The mass percent of the components is 4.5-13%, and the sum of the mass percent of the components is 100%;
step 2: the WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS which are weighed in the step 12Uniformly mixing the powder to form mixed powder;
and step 3: adding a proper amount of paraffin powder into the mixed powder in the step 2, and putting the mixed powder into a mixer for mixing to form a uniform material; wherein the paraffin powder has a particle size of about 25 μm and accounts for 0.6-0.9 wt% of the mixed powder.
And 4, step 4: prefabricating a fiber mesh by using refractory metal Nb fibers to prepare a refractory metal Nb fiber mesh; wherein the diameter of the metal Nb fiber is 600-1000 μm, and the distance between the fibers in the fiber net is 3-6 times of the diameter of the fiber;
and 5: laying the uniform material obtained in the step 3 and the Nb fiber nets prepared in the step 4 in a mold layer by layer to form a prefabricated body, wherein the distance between the fiber net layers in the prefabricated body is more than 1mm and less than 5 mm;
step 6: step 5, placing the prefabricated body into a hot-pressing sintering furnace for isothermal hot-pressing sintering, firstly heating the furnace to 500-; then cooling to 1100 deg.C, maintaining for 4-8h, wherein the furnace pressure is 20-50MPa, and cooling to room temperature. In the isothermal and normal pressure sintering process, the temperature rise speed in the high temperature sintering furnace is 5 ℃/min-10 ℃/min, and in the cooling process, the temperature fall speed in the high temperature sintering furnace is 2 ℃/min-5 ℃/min. And finally, cooling and demolding to obtain the multi-scale self-lubricating tungsten carbide-based composite material.
Example 1
The preparation method of the multi-scale self-lubricating tungsten carbide-based composite material comprises the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder; the average particle size of WC particles is 20 μm, the average particle size of Fe powder is 1 μm, the average particle size of Nb powder is 1 μm, and the purity of the above powders is more than 99.5%; wherein the mass fraction of WC is 53%, the mass fraction of Fe powder is 13%, the mass fraction of Nb powder is 19%, the mass fraction of graphite powder is 4.5%, and MoS2The mass fraction of the components is 10.5 percent, and the sum of the mass percentages of the components is 100 percent;
step 2: using a low-energy mixer to mix the WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS weighed in the step 12Uniformly mixing the powder to form mixed powder, so that the graphite is uniformly adhered to the surface of the metal particles;
and step 3: adding a proper amount of paraffin powder into the mixed powder in the step 2, and putting the mixed powder into a mixer for mixing to form a uniform material; wherein the paraffin powder has a particle size of about 25 μm and accounts for 0.6 wt% of the mixed powder.
And 4, step 4: prefabricating a fiber mesh by using refractory metal Nb fibers to prepare a refractory metal Nb fiber mesh; wherein the diameter of the metal Nb fiber is 1000 μm, and the fiber spacing is 3000 μm;
and 5: laying the uniform material obtained in the step 3 and the Nb fiber nets prepared in the step 4 in a die layer by layer to form a prefabricated body, wherein the distance between the fiber net layers in the prefabricated body is 5 mm;
step 6: placing the preform prepared in the step 5 in a high-temperature hot-pressing furnace for isothermal hot-pressing sintering, wherein in the sintering process, the atmosphere in the high-temperature sintering furnace is argon protective gas, the temperature of the furnace is firstly increased to 500 ℃ for degreasing treatment for 8h, then the temperature of the furnace is increased to 1165 ℃, the temperature is kept for 0.2h, and the furnace pressure is 5MPa in the heat preservation process; then reducing the furnace temperature to 1100 ℃ and preserving the temperature for 4h, wherein the furnace pressure is 50MPa in the preserving process; the temperature rise speed in the high-temperature sintering furnace is 10 ℃/min; then cooling to room temperature along with the furnace temperature. The cooling speed in the high-temperature sintering furnace is 5 ℃/min; finally, demoulding the composite material, and taking out the blank in the mould to obtain the multi-scale self-lubricating tungsten carbide-based composite material.
The prepared multi-scale self-lubricating tungsten carbide-based composite material is processed with metallographic phase, the internal microstructure characteristics are observed, FIG. 2 is a sectional macroscopic view of the multi-scale self-lubricating tungsten carbide-based composite material prepared in example 1, fig. 3 is a sectional high magnification microstructure of the multi-scale self-lubricating tungsten carbide-based composite material prepared in example 1, and as can be seen from fig. 3, the composite material prepared in example 1, the structure composition of the composite material mainly comprises multi-scale carbide particles, metal Nb fibers 1, a self-lubricating phase 5 and a binding phase 3, and specifically comprises micron-sized WC particles 4 in a matrix, submicron NbC particles 2 in dispersed distribution, metal Nb fibers 1 in a net structure, submicron-sized NbC particles 2 in annular distribution along the circumferential direction of the metal Nb fibers, a self-lubricating phase 5 in uniform distribution and a certain amount of Fe binding phase 3, wherein the self-lubricating phase is graphite and MoS.2。
Through measurement, the dimension of micron-sized WC ceramic particles in the composite material is about 20 μm, the dimension of the dispersed submicron NbC particles is about 800nm, and the dimension of the annularly distributed submicron NbC particles is 500nm-800 nm; the remaining metal Nb fibers have a diameter of about 700 μm, graphite and MoS2The uniform distribution, the binding phase Fe is uniformly distributed among the carbide particles.
Measured, the tungsten carbide-based composite materialThe volume fraction of micron-sized WC particles in the material is about 60%, the volume fraction of dispersed submicron-sized NbC particles is about 10%, the volume fraction of submicron-sized NbC particles annularly distributed along the circumferential direction of the metal Nb fiber is about 5%, the volume fraction of the binding phase Fe is about 10%, and the self-lubricating phase (graphite + MoS)2) Is about 10%, and the density of the composite material is about 98%.
Example 2
The preparation method of the multi-scale self-lubricating tungsten carbide-based composite material comprises the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder; the mean particle size of the WC particles was 30 μm, that of the Fe powder was 1 μm, that of the Nb powder was 5 μm, and that of the MoS2The average particle size of the powder is 1 mu m, and the purity of the metal powder is more than 99.5 percent; wherein the mass fraction of WC is 76%, the mass fraction of Fe powder is 5%, the mass fraction of Nb powder is 13.9%, the mass fraction of graphite powder is 0.2%, and MoS2The mass fraction of (A) is 4.9%;
step 2: adopting a low-energy ball mill to weigh the WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS weighed in the step 12Uniformly mixing the powder to form mixed powder, so that the graphite is uniformly adhered to the surface of the metal particles;
and step 3: adding a proper amount of paraffin powder into the mixed powder in the step 2, and putting the mixed powder into a mixer for mixing to form a uniform material; wherein the paraffin powder has a particle size of about 25 μm and accounts for 0.9 wt% of the mixed powder.
And 4, step 4: prefabricating a fiber mesh by using refractory metal Nb fibers to prepare a refractory metal Nb fiber mesh; wherein the diameter of the metal Nb fiber is 600 μm, and the fiber spacing is 3600 μm;
and 5: laying the uniform material obtained in the step 3 and the Nb fiber nets prepared in the step 4 in a die layer by layer to form a prefabricated body, wherein the distance between the fiber net layers in the prefabricated body is 1 mm;
step 6: step 5, placing the prefabricated body into a hot-pressing sintering furnace for isothermal hot-pressing sintering, wherein the atmosphere in the high-temperature sintering furnace is argon protective gas, raising the temperature of the furnace to 800 ℃, keeping the temperature for 2 hours, dewaxing, raising the temperature of the furnace to 1250 ℃, keeping the temperature for 0.2 hours, and keeping the furnace pressure at 10MPa in the heat preservation process; then, cooling to 1100 ℃, and preserving heat for 8 hours, wherein the furnace pressure is 20MPa in the heat preservation process; and finally cooling to room temperature. In the isothermal hot-pressing sintering process, the temperature rise speed in the high-temperature sintering furnace is 8 ℃/min, and in the cooling process, the temperature drop speed in the high-temperature sintering furnace is 4 ℃/min; and finally, taking out the mold in the furnace, and carrying out demolding treatment on the mold to obtain the multi-scale self-lubricating tungsten carbide-based composite material.
Through measurement, the volume fraction of micron-sized WC particles in the multi-scale self-lubricating tungsten carbide-based composite material is about 80%, the volume fraction of dispersed submicron-sized NbC particles is about 5%, the volume fraction of submicron-sized NbC particles annularly distributed along the circumferential direction of the metal Nb fiber is about 5%, the volume fraction of the Fe phase is about 2%, and the self-lubricating phase (graphite + MoS) is formed2) Is about 3% and the density of the material is about 97%.
In the material, the dimension of micron-sized WC ceramic particles is about 30 μm, the dimension of the dispersed submicron NbC particles is about 900nm, and the dimension of the annularly distributed submicron NbC particles is 500-700 nm; the remaining metallic Nb fibers have a diameter of about 300 μm, a graphite phase and MoS2The uniform distribution, the binding phase Fe is uniformly distributed among the carbide particles.
Example 3
The preparation method of the multi-scale self-lubricating tungsten carbide-based composite material comprises the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder; the mean particle size of the WC particles was 25 μm, that of the Fe powder was 1 μm, that of the Nb powder was 5 μm, MoS2The average particle size of the powder is 1 mu m, and the purity of the metal powder is more than 99.5 percent; wherein the mass fraction of WC is 60%, the mass fraction of Fe powder is 12%, the mass fraction of Nb powder is 17.8%, the mass fraction of graphite powder is 0.2%, and MoS2The mass fraction of (A) is 10%;
step 2: using low energy ball millsThe WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS weighed in the step 1 are mechanically mixed2Uniformly mixing the powder to form mixed powder, so that the graphite is uniformly adhered to the surface of the metal particles;
and step 3: adding a proper amount of paraffin powder into the mixed powder in the step 2, and putting the mixed powder into a mixer for mixing to form a uniform material; wherein the paraffin powder has a particle size of about 25 μm and accounts for 0.7 wt% of the mixed powder.
And 4, step 4: prefabricating a fiber mesh by using refractory metal Nb fibers to prepare a refractory metal Nb fiber mesh; wherein the diameter of the metal Nb fiber is 800 μm, and the distance between fibers in the fiber net is 3000 μm;
and 5: laying the uniform material obtained in the step 3 and the Nb fiber nets prepared in the step 4 in a die layer by layer to form a prefabricated body, wherein the distance between the fiber net layers in the prefabricated body is 3 mm;
step 6: and 5, placing the prefabricated body into a hot-pressing sintering furnace for isothermal hot-pressing sintering, wherein in the isothermal hot-pressing sintering process, the atmosphere in the high-temperature sintering furnace is argon protective gas. Firstly, heating the furnace to 600 ℃, preserving the temperature for 7h, degreasing, then heating the furnace to 1250 ℃, preserving the temperature for 0.5h, wherein the furnace pressure is 8MPa in the heat preservation process; then, cooling to 1100 ℃, and preserving heat for 4 hours, wherein the furnace pressure is 30MPa in the heat preservation process; and finally cooling to room temperature. In the isothermal and normal-pressure sintering process, the temperature rise speed in the high-temperature sintering furnace is 10 ℃/min, and in the cooling process, the temperature drop speed in the high-temperature sintering furnace is 5 ℃/min; and finally, taking out the mold in the furnace, and carrying out demolding treatment on the mold to obtain the multi-scale self-lubricating tungsten carbide-based composite material.
The volume fraction of micron-sized WC particles in the multi-scale self-lubricating tungsten carbide-based composite material is about 62%, the volume fraction of dispersed submicron-sized NbC particles is about 10%, the volume fraction of submicron-sized NbC particles annularly distributed along the circumferential direction of the metal Nb fiber is about 10%, the volume fraction of the metal Nb fiber is about 5%, the volume fraction of the Fe phase is about 5%, and the self-lubricating phase (graphite + MoS) is formed2) Is about 8%, and the density of the material is about 98.5%.
In the material, the micron-sized WC ceramic particles have the size of about 25 mu m and are distributed in a dispersion wayThe submicron NbC particles have the size of about 900nm, and the submicron NbC particles are annularly distributed and have the size of 500-700 nm; the remaining metallic Nb fibers have a diameter of about 500 μm, a graphite phase and MoS2The uniform distribution, the binding phase Fe is uniformly distributed among the carbide particles.
Example 4
The preparation method of the multi-scale self-lubricating tungsten carbide-based composite material comprises the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder; the average particle size of WC particles is 30 μm, the average particle size of Fe powder is 5 μm, the average particle size of Nb powder is 5 μm, and the purity of the above metal powder is more than 99.5%; wherein the mass fraction of WC is 65%, the mass fraction of Fe powder is 7.5%, the mass fraction of Nb powder is 15%, the mass fraction of graphite powder is 3.5%, and MoS2The mass fraction of (A) is 9%;
step 2: adopting a low-energy ball mill to weigh the WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS weighed in the step 12Uniformly mixing the powder to form mixed powder, so that the graphite is uniformly adhered to the surface of the metal particles;
and step 3: adding a proper amount of paraffin powder into the mixed powder in the step 2, and putting the mixed powder into a mixer for mixing to form a uniform material; wherein the paraffin powder has a particle size of about 25 μm and accounts for 0.7 wt% of the mixed powder.
And 4, step 4: prefabricating a fiber mesh by using refractory metal Nb fibers to prepare a refractory metal Nb fiber mesh; wherein the diameter of the metal Nb fiber is 700 μm, and the fiber spacing is 2100 μm;
and 5: laying the powder obtained in the step 3 and the Nb fiber nets prepared in the step 4 in a die layer by layer to form a prefabricated body, wherein the distance between the fiber net layers in the prefabricated body is 2 mm;
step 6: and 5, placing the prefabricated body into a hot-pressing sintering furnace for isothermal hot-pressing sintering, wherein in the isothermal hot-pressing sintering process, the atmosphere in the high-temperature sintering furnace is argon protective gas. Firstly, heating the furnace to 700 ℃, preserving heat for 6h, degreasing, then heating the furnace to 1250 ℃, preserving heat for 1h, wherein the furnace pressure is 8MPa in the heat preservation process; then, cooling to 1100 ℃, and preserving heat for 6h, wherein the furnace pressure is 40MPa in the heat preservation process; and finally cooling to room temperature. In the isothermal and normal-pressure sintering process, the temperature rise speed in the high-temperature sintering furnace is 5 ℃/min, and in the cooling process, the temperature drop speed in the high-temperature sintering furnace is 2 ℃/min; and finally, taking out the mold in the furnace, and carrying out demolding treatment on the mold to obtain the multi-scale self-lubricating tungsten carbide-based composite material.
The volume fraction of micron-sized WC particles in the multi-scale self-lubricating tungsten carbide-based composite material is about 60 percent, the volume fraction of dispersed submicron-sized NbC particles is about 10 percent, the volume fraction of submicron-sized NbC particles annularly distributed along the circumferential direction of the metal Nb fiber is about 7 percent, the volume fraction of the metal Nb fiber is about 10 percent, the volume fraction of the Fe phase is about 3 percent, and the self-lubricating phase (graphite + MoS) is formed by the graphite and the MoS2) Is about 10%, the density of the material is about 98.6%.
In the material, the dimension of micron-sized WC ceramic particles is about 30 μm, the dimension of the dispersed submicron NbC particles is about 800nm, and the dimension of the annularly distributed submicron NbC particles is 500-700 nm; the remaining metal Nb fibers have a diameter of about 450 μm, a graphite phase and MoS2The uniform distribution, the binding phase Fe is uniformly distributed among the carbide particles.

Claims (2)

1. A preparation method of a multi-scale self-lubricating tungsten carbide-based composite material is characterized by comprising the following steps:
step 1, weighing the following components of WC particles, Fe powder, Nb powder, graphite powder and MoS respectively2Powder;
step 2: the WC particles, the Fe powder, the Nb powder, the graphite powder and the MoS which are weighed in the step 12Uniformly mixing the powder to form mixed powder;
and step 3: adding paraffin powder into the mixed powder, and then putting the mixed powder into a mixing roll for mixing treatment to form uniform materials;
and 4, step 4: adopting refractory metal Nb fibers to prefabricate a net structure to form a refractory metal fiber net;
and 5: preliminarily laying the mixed material and the fiber mesh layer by layer in a mould to form a prefabricated body, wherein the distance between fiber mesh layers in the prefabricated body is 1-5 mm;
step 6: placing the prefabricated body in a high-temperature die, then assembling the prefabricated body into a high-temperature sintering furnace for isothermal hot-pressing sintering, and finally cooling and demolding to obtain the multi-scale self-lubricating tungsten carbide-based composite material;
in the isothermal hot-pressing sintering process, the furnace temperature is firstly increased to 800 ℃ for degreasing treatment, then the furnace temperature is increased to 1165 ℃ and 1250 ℃ for heat preservation for 0.2h-2h, then the temperature is reduced to 1100 ℃ for heat preservation for 4-8h, and finally the temperature is cooled to the room temperature; the temperature rising speed in the high-temperature sintering furnace is 5 ℃/min-10 ℃/min, and the temperature falling speed in the high-temperature sintering furnace is 2 ℃/min-5 ℃/min in the cooling process; 1165-1250 deg.C, and 20-50MPa in the 1100 deg.C isothermal treatment process;
the multi-scale self-lubricating tungsten carbide-based composite material consists of a matrix and metal Nb fibers (1) distributed in a net structure, wherein the matrix comprises micron-sized WC particles (4), submicron-sized NbC particles (2) distributed in a dispersed manner, a self-lubricating phase (5) and a binding phase (3) distributed uniformly; in the composite material, the volume fraction of micron-sized WC particles (4) is 60-80%, the volume fraction of self-lubricating phase (5) is 2.2-10%, the volume fraction of submicron-sized NbC particles (2) is 10-20%, the volume fraction of binding phase (3) is 2-10%, the volume fraction of metal Nb fiber (1) is 5-10%, and the sum of the volume percentages of the components is 100%; the self-lubricating phase (5) consists of graphite and MoS2The composition is that the binding phase (3) is Fe; the grain diameter of the micron-sized WC particles (4) is 20-30 μm, and the grain diameter of the submicron-sized NbC particles (2) is 500-900 nm; the diameter of the metal Nb fiber (1) is 300-700 mu m.
2. The method for preparing the multi-scale self-lubricating tungsten carbide-based composite material according to the claim 1, wherein in the step 4, the diameter of the fiber in the refractory metal fiber mesh is 600 μm to 1000 μm, and the distance between the fibers in the fiber mesh is 3 times to 6 times the diameter of the fiber.
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JPS5330407A (en) * 1976-09-01 1978-03-22 Tokushiyu Muki Zairiyou Kenkiy Process for production of composite material based on siliconncarbideefibreereinforced light alloy
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CN106498314A (en) * 2016-11-25 2017-03-15 太原理工大学 A kind of WC TaC Csf obdurability materials and preparation method thereof
CN109402479A (en) * 2018-12-17 2019-03-01 四川理工学院 A kind of high abrasion obdurability NbC base light-weight metal ceramal and preparation method thereof
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Publication number Priority date Publication date Assignee Title
JPS5330407A (en) * 1976-09-01 1978-03-22 Tokushiyu Muki Zairiyou Kenkiy Process for production of composite material based on siliconncarbideefibreereinforced light alloy
CN104630664A (en) * 2015-02-25 2015-05-20 中国地质大学（北京） Method for preparing novel carbon fiber toughened Ti (C,N) based metal ceramic material
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