CN115703856B - Ti (titanium) 3 AlC 2 -resin composite material and method for preparing the same - Google Patents
Ti (titanium) 3 AlC 2 -resin composite material and method for preparing the same Download PDFInfo
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- Powder Metallurgy (AREA)
Abstract
The application relates to Ti 3 AlC 2 -a process for the preparation of a resin composite comprising the steps of: ti is mixed with 3 AlC 2 Mixing the powder with an adhesive to make Ti 3 AlC 2 Bonding the powder together to obtain Ti 3 AlC 2 Mud; ti (Ti) 3 AlC 2 The diameter of the powder is 200nm-2 mu m, and the thickness is 20-200nm; for Ti 3 AlC 2 Performing pad rolling treatment on the mud to ensure that Ti is 3 AlC 2 Ti in mud 3 AlC 2 The powder is directionally arranged to obtain Ti with directional arrangement structure 3 AlC 2 A thin blank; ti of multiple directional arrangement structure 3 AlC 2 Stacking the thin blanks together for pressing treatment to obtain Ti 3 AlC 2 A blank body; for Ti 3 AlC 2 The green body is subjected to organic matter removal treatment and sintering treatment to obtain Ti 3 AlC 2 A skeleton; for Ti 3 AlC 2 Carrying out surface modification on the framework; impregnating surface-modified Ti with resin monomer solution 3 AlC 2 Framework, and obtaining Ti after polymerization and solidification of resin monomer solution 3 AlC 2 -a resin composite. The application is mainly used for preparing Ti by a simple process 3 AlC 2 Oriented arrangement of Ti in resin matrix 3 AlC 2 -a resin composite; the composite material has excellent bending strength, fracture toughness, conductivity and wear resistance.
Description
Technical Field
The application relates to the technical field of MAX phase ceramic-resin composite materials, in particular to a Ti phase ceramic-resin composite material 3 AlC 2 -resin composite material and method for preparing the same.
Background
Ceramics have the advantages of high strength, high hardness, high modulus, corrosion resistance, abrasion resistance, low density and the like, so that the ceramics become one of the most promising candidates for hot-end high-temperature components such as aerospace, armor protection, rail transit and the like. Wherein, due to MAX phase ceramic (such as Ti 3 AlC 2 、Ti 3 SiC 2 ) Has special nano lamellar crystal structure characteristics, so that the ceramic has the excellent mechanical properties of the ceramic and the electric conductivity and the heat conductivity of the metal. This property of MAX phase ceramics has attracted considerable attention from researchers. However, like traditional oxide or nitride ceramics, MAX-phase ceramics have strong covalent bonds, which make them brittle and have poor fracture toughness, and often have catastrophic failure under severe stress conditions, which seriously affects the application range. Therefore, the improvement of fracture toughness of the MAX phase ceramic as much as possible without decreasing strength is an urgent problem to be solved.
Currently, the conventional technology is to improve the performance of the MAX-phase ceramic matrix by adding second-phase particles, whiskers or fibers; although these methods can improve fracture toughness to some extent, the introduction of the second phase can present problems such as weak interfacial bonding force between the two phases, thermal expansion mismatch, etc.
As is well known, resins generally have good toughness and the resins are incorporated into MAX-phase ceramics to form a MAX-phase ceramic-resin composite with a certain structure. In the composite material, MAX phase ceramic is used as a strengthening phase, resin is used as a toughening phase, deflection and bridging of cracks are induced through a specific structure of the composite material, crack expansion resistance is increased, and the optimized mechanical property of the material along a specific direction is facilitated.
One prior art proposes Ti 3 AlC 2 The preparation method of the epoxy resin conductive composite material comprises the following specific scheme: adopts a blending method to lead the Ti to be granular 3 AlC 2 Are communicated with each other and uniformly dispersed in the epoxy resin matrix. However, ti is 3 AlC 2 The particle size is about 18. Mu.m, while a larger particle size leads to a coarse microstructure, and Ti 3 AlC 2 The particles are not completely communicated, obvious defects exist, the volume fraction is not more than 50%, the mechanical properties of the composite material are limited to a great extent, and the effect of excellent comprehensive mechanical properties cannot be achieved. In addition, the composite material adopts granular Ti 3 AlC 2 Failure to do soThe microstructure orientation is realized, and the mechanical property cannot be optimized.
The prior art proposes a layered alumina-epoxy resin composite material containing whiskers which are arranged in a direction perpendicular to a layer interface and a preparation method thereof, and aims to imitate a 'mineral bridge' structure of a shell pearl layer, form a 'whisker bridge' structure similar to a 'mineral bridge' structure in layered ceramics, and prepare the layered alumina-epoxy resin composite ceramic containing whiskers which are arranged in a direction perpendicular to the layer interface (silicon carbide whiskers are arranged as mineral bridges along the direction perpendicular to the interface between an alumina ceramic layer and an epoxy resin layer) so as to further improve the strong and toughness performance of the layered alumina-epoxy resin composite material. However, in the ceramic-based layered composite material, the thickness of the ceramic layer is 3-10 μm and the thickness of the resin layer is 10-80 μm, in contrast, the strength and hardness of the composite material are severely limited by the thinner ceramic layer. In addition, one end of a metal rod is inserted into the prepared suspension, the other end of the metal rod is immersed into the refrigerant, and the suspension is frozen from top to bottom by utilizing heat transfer of the metal rod to realize orientation.
In summary, the MAX phase ceramic is arranged in the MAX phase ceramic-resin composite material in an oriented way, so that the mechanical property of the MAX phase ceramic-resin composite material can be improved. However, the inventors of the present application found that: at present, ceramic powder which is selected when preparing ceramic-resin composite materials is generally in a micron size, so that a microstructure is easily coarse, and the granular powder cannot realize microstructure orientation; in addition, the existing method for realizing the directional arrangement has a plurality of limitations when preparing the ceramic-resin composite material with the directional lamellar structure (for example, only lamellar structure can be obtained, the orientation of ceramic phase can not be realized between the lamellar layers; moreover, the existing method for realizing directional arrangement is only limited to the preparation of small-size samples, the material preparation steps are more, the process is complex, and industrial production is difficult to realize.
Disclosure of Invention
In view of this, the present application provides a Ti 3 AlC 2 Resin composite material and preparation method thereof, and is mainly aimed at preparing Ti by using simple process 3 AlC 2 Oriented arrangement of Ti in resin matrix 3 AlC 2 -a resin composite.
In order to achieve the above purpose, the present application mainly provides the following technical solutions:
in one aspect, embodiments of the present application provide a Ti 3 AlC 2 -a process for the preparation of a resin composite comprising the steps of:
and (3) bonding: ti is mixed with 3 AlC 2 Mixing the powder with an adhesive to make Ti 3 AlC 2 Bonding the powder together to obtain Ti 3 AlC 2 Puree (dough mix); wherein the Ti is 3 AlC 2 The powder is nano flake Ti with the diameter of 200nm-2 mu m and the thickness of 20-200nm 3 AlC 2 Powder;
and (3) performing laminating and pressing: for the Ti 3 AlC 2 Performing pad rolling treatment on the mud to ensure that Ti is 3 AlC 2 Ti in mud 3 AlC 2 The powder is directionally arranged to obtain Ti with directional arrangement structure 3 AlC 2 A thin blank; ti of multiple directional arrangement structure 3 AlC 2 Stacking the thin blanks together for pressing treatment to obtain Ti 3 AlC 2 A blank body;
removing organic matters and sintering: for the Ti 3 AlC 2 The green body is subjected to organic matter removal treatment and sintering treatment to obtain Ti 3 AlC 2 A skeleton;
impregnating, polymerizing and curing the resin monomer: for the Ti 3 AlC 2 Carrying out surface modification on the framework; impregnating surface-modified Ti with resin monomer solution 3 AlC 2 A framework, and Ti is obtained after the polymerization and solidification of the resin monomer solution 3 AlC 2 -a resin composite.
Preferably, in the bonding step: the adhesive is one or more of polyvinyl alcohol adhesive, hydroxypropyl methyl cellulose adhesive, polyethylene glycol adhesive, sucrose adhesive, liquid paraffin adhesive and glycerol adhesive; preferably, the polyvinyl alcohol binder includes polyvinyl alcohol of low viscosity and water; further preferably, the mass fraction of the low-viscosity polyvinyl alcohol in the polyvinyl alcohol adhesive is 2-15%.
Preferably, ti is 3 AlC 2 Mixing the powder and the adhesive to obtain a mixture, and kneading the mixture until Ti 3 AlC 2 The powder is completely bonded together to obtain Ti 3 AlC 2 Mud.
Preferably, the step of the lapping process includes: causing the Ti to be 3 AlC 2 Rolling mud between two rollers of a roller machine to form a thin blank, folding the thin blank, rolling the thin blank, and repeatedly folding and rolling for a plurality of times to obtain Ti with a directional arrangement structure 3 AlC 2 A thin blank; preferably, the distance between the two rolls of the rolling mill is constant during a plurality of rolling operations.
Preferably, in the step of the pressing treatment: the temperature of the pressing treatment is 30-120 ℃, the pressure is 2-20MPa, and the time is 0.5-3h.
Preferably, the step of pressing treatment includes: ti of the orientation arrangement structure 3 AlC 2 Cutting thin blanks into multiple directional arrangement structures of same size 3 AlC 2 After the thin blanks are stacked together for pressing.
Preferably, the step of removing the organic matter includes: under a protective atmosphere (vacuum-pumping and then introducing protective gas such as hydrogen, argon and nitrogen), the Ti is prepared 3 AlC 2 Preserving the heat of the blank for a first set time at a heat preservation temperature; preferably, the heat preservation temperature is 300-700 ℃, and the first set time is 3-8 hours; preferably, the Ti is under a protective atmosphere 3 AlC 2 Heating the blank to a heat preservation temperature, and preserving heat for a first set time at the heat preservation temperature; further preferably, the Ti is used in the process of 3 AlC 2 In the process of heating the blank to the heat preservation temperature, the heating rate is 1-8 ℃/min。
Preferably, the step of sintering treatment includes: under the protection atmosphere (vacuumizing and then introducing protection gas such as hydrogen, argon and nitrogen), ti after organic matter removal treatment 3 AlC 2 Sintering the blank at sintering temperature to obtain Ti 3 AlC 2 A skeleton; wherein the sintering temperature is 700-1300 ℃, and the sintering treatment time is 1-5h; preferably, ti after organic matter removal is treated in a protective atmosphere 3 AlC 2 Heating the green body to the sintering temperature, wherein the heating rate is 2-10 ℃/min.
Preferably, the Ti is 3 AlC 2 The porosity of the framework is 10-70%.
Preferably, in the resin monomer impregnating, polymerization and curing step:
for the Ti 3 AlC 2 The step of surface modification of the skeleton comprises the following steps: subjecting the Ti to 3 AlC 2 Immersing the skeleton in a modifying liquid containing a silane coupling agent, and subjecting the Ti to a reaction 3 AlC 2 Surface modifying the skeleton, and taking out the Ti after surface modification after finishing the surface modification 3 AlC 2 Skeleton and drying; preferably, the mass percentage of the silane coupling agent in the modifying liquid is 5-25%; preferably, the solvent in the modifying liquid is a mixed liquid of methanol and water with the pH value adjusted to 4-7 by acetic acid; further preferably, the mass fraction of methanol in the mixed solution of methanol and water is 70-90%.
Preferably, in the resin monomer impregnating, polymerization and curing step: impregnating the surface-modified Ti with a resin monomer solution 3 AlC 2 Skeletons (amount of resin monomer and Ti) 3 AlC 2 With respect to the size of the skeleton, only Ti is required 3 AlC 2 The framework is completely immersed in resin monomer solution), and after the resin monomer is polymerized, heat treatment is carried out to cure the resin to obtain Ti 3 AlC 2 -a resin composite; preferably, the resin monomer solution includes methyl methacrylate and an initiator; further preferably, in the resin monomer solution, the initiationThe mass fraction of the agent is 0.2-1%; preferably, the temperature of the heat treatment is 40-90 ℃; preferably, the polymerization time of the resin monomer is 4 to 10 days; preferably, the resin monomer solution is dripped into an infiltration vessel, immersed into the sample, and vacuum assisted (due to Ti 3 AlC 2 The skeleton contains many pores, and the vacuum assistance is used for filling the resin monomer solution into Ti 3 AlC 2 In the pores of the framework), continuing to dropwise add the resin monomer solution until the sample is submerged, standing in the atmospheric environment, and waiting for polymerization of the resin monomer; further preferably, the vacuum assist time is 20-40min.
In another aspect, an embodiment of the present application provides a Ti 3 AlC 2 -a resin composite material, wherein the Ti 3 AlC 2 The resin composite is made of two-dimensional nano-platelet-shaped Ti 3 AlC 2 And a resin composition, wherein the Ti is in volume percent 3 AlC 2 30-90% of the total content of the resin and the balance of the resin; on microstructure, the Ti is 3 AlC 2 Nanoplatelets of Ti in resin composite 3 AlC 2 The resin matrix is preferentially oriented and arranged to form a two-phase continuous structure; preferably, in the dual-phase continuous structure, the Ti 3 AlC 2 The thickness of the lamellar layer is 20-200nm, and the spacing between lamellar layers is 0.1-1 μm; preferably, the resin is polymethyl methacrylate; preferably, the Ti is 3 AlC 2 The resin composite is made of Ti as defined in any one of the above 3 AlC 2 -a preparation method of a resin composite material; preferably, the Ti is 3 AlC 2 Nanoplatelets of Ti in resin composite 3 AlC 2 Is arranged in a preferred orientation in the resin matrix along the direction of rotation of the nip roll.
Compared with the prior art, the Ti of the application 3 AlC 2 The resin composite and the method for its preparation have at least the following advantageous effects:
the embodiment of the application provides Ti 3 AlC 2 Resin composite material and method for the production thereof by forming the same in nano-platelet form of Ti 3 AlC 2 Powder as raw material (thick)Having a degree of 20-200 nm) and then forming Ti by mixing it with a binder 3 AlC 2 After mud is processed, a roller mill is adopted to carry out a plurality of rolling treatment (rolling-folding-rolling) operations, thus realizing Ti 3 AlC 2 The directional arrangement of the powder, then the steps of pressing, removing organic matters, sintering, impregnating resin monomer, polymerizing and curing are carried out to obtain Ti 3 AlC 2 -a resin composite; in the preparation process, nano sheet Ti 3 AlC 2 Powder selecting and rolling process for realizing Ti 3 AlC 2 The powder is oriented so that the composite material has excellent strength. The Ti is 3 AlC 2 Resin composite material compared to Ti 3 AlC 2 The ceramic has obviously improved fracture toughness and dynamic energy consumption property, so that the ceramic has excellent comprehensive mechanical property and has considerable application prospect as a structural material.
It should be noted that: the preparation process of the application realizes nano flake Ti 3 AlC 2 The powder orientation method only needs flaky Ti 3 AlC 2 The powder has larger length-diameter ratio, no plasticizer is needed, the operation is simple, the process period is short, the efficiency is high, the cost is low, the prepared material has no size limitation, and the industrialization is easy to realize; in addition, the laminated structure formed in the repeated rolling and folding processes can reduce the thermal stress in the sintering process, and is easy to mold.
The foregoing description is only an overview of the present application, and is intended to provide a better understanding of the present application, as it is embodied in the following description, with reference to the preferred embodiments of the present application and the accompanying drawings.
Drawings
FIG. 1 is a drawing of the preparation of Ti according to example 1 3 AlC 2 -a process flow diagram of a resin composite;
FIG. 2 is a diagram of Ti obtained after sintering treatment according to the scheme of example 1 3 AlC 2 Macroscopic view (fig. 2 (a)) and microscopic structure view (fig. 2 (b)) of the skeleton;
FIG. 3 is a diagram of Ti prepared in example 1 3 AlC 2 Macro of resin composite materialView (fig. 3 (a)) and microstructure (b); wherein the bright white area in the figure is Ti 3 AlC 2 The dark black areas are resin.
FIG. 4 shows the Ti as prepared in example 1 3 AlC 2 Resin composite along vertical and parallel Ti 3 AlC 2 Room temperature three-point bending stress-strain curve of sheet direction (wherein the graph (a) in fig. 4 is vertical Ti 3 AlC 2 Room temperature three-point bending stress-strain curve in sheet direction, the graph (b) in FIG. 4 is parallel Ti 3 AlC 2 Room temperature three-point bending stress-strain curve for sheet direction).
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the application, the following detailed description refers to the specific implementation, structure, characteristics and effects according to the application of the application with reference to the accompanying drawings and preferred embodiments. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
The embodiment of the application provides Ti 3 AlC 2 The resin composite material and the preparation method thereof are as follows:
Ti 3 AlC 2 the resin composite is made of two-dimensional nano-platelet-shaped Ti 3 AlC 2 And a resin composition, wherein the Ti is in volume percent 3 AlC 2 30-90% of the total content of the resin and the balance of the resin; microstructure of Ti 3 AlC 2 Nanoplatelets of Ti in resin composite 3 AlC 2 The preferred orientation arrangement (preferred orientation arrangement along the rotation direction of the roller) in the resin matrix forms a two-phase continuous structure; preferably, in the dual-phase continuous structure, the Ti 3 AlC 2 The thickness of the sheet layer is 20-200nm, and the spacing between the sheet layers is 0.1-1 μm. Preferably, the resin is polymethyl methacrylate.
Wherein Ti is 3 AlC 2 Of a resin composite materialThe preparation method comprises the following steps:
and (3) bonding: ti is mixed with 3 AlC 2 Mixing the powder and the adhesive to obtain a mixture, and kneading the mixture until Ti 3 AlC 2 The powder is completely bonded together to obtain Ti 3 AlC 2 Mud. Wherein Ti is 3 AlC 2 The powder is nano flake Ti with the diameter of 200nm-2 mu m and the thickness of 20-200nm 3 AlC 2 And (3) powder.
Wherein the adhesive is one or more selected from polyvinyl alcohol, hydroxypropyl methylcellulose, polyethylene glycol, sucrose, liquid paraffin and glycerol.
Preferably, the adhesive is a low-viscosity polyvinyl alcohol solution, and the mass fraction of the low-viscosity polyvinyl alcohol in the low-viscosity polyvinyl alcohol solution is 2-15, preferably 7-15%. Preferably, the low viscosity polyvinyl alcohol is of type 1788.
And (3) performing laminating and pressing: for Ti 3 AlC 2 Performing pad rolling treatment on the mud to ensure that Ti is 3 AlC 2 Ti in mud 3 AlC 2 The powder is directionally arranged to obtain Ti with directional arrangement structure 3 AlC 2 A thin blank; ti of multiple directional arrangement structure 3 AlC 2 Stacking the thin blanks together for pressing treatment to obtain Ti 3 AlC 2 And (5) a blank body.
The process of the laminating rolling treatment comprises the following steps: using a rolling mill to make Ti 3 AlC 2 The mud passes between two rollers to form a thin blank, the thin blank is folded and rolled again, and the step is repeatedly operated (the roller machine is folded once to double the thickness on the premise of ensuring the distance between the two rollers to be unchanged (the roller machine is folded once to ensure the distance between the two rollers to be unchanged, the roller machine is rolled again, and the nano sheet-shaped Ti is promoted) 3 AlC 2 Powder orientation), rolling-folding-rolling Ti 3 AlC 2 Mud ", repeating the operation). In the continuous rolling process, the roller is applied to the nano sheet Ti 3 AlC 2 Shear forces on the powder promote Ti 3 AlC 2 The powder is preferentially oriented along the rotation direction of the roller so as to generate an orientation effect.
The pressing process comprises the following steps: cutting the green body slices into the same size and stacking the green body slices together for pressing, wherein the temperature is 30-120 ℃, the pressure is 2-20MPa, and the pressure maintaining time is 0.5-3h.
Removing organic matters and sintering: for Ti 3 AlC 2 The green body is subjected to organic matter removal treatment and sintering treatment to obtain Ti 3 AlC 2 And (3) a framework.
The method specifically comprises the following steps: for Ti 3 AlC 2 Heating and heat-preserving the blank body in argon atmosphere, wherein the heat-preserving temperature is 300-700 ℃, the heat-preserving time is 3-8h, and the heating rate is 1-8 ℃/min (the organic matter removing treatment is the above). For the Ti 3 AlC 2 The atmosphere of sintering treatment is argon or nitrogen or vacuum atmosphere, the sintering temperature is 700-1300 ℃, the sintering treatment time is 1-5h, and the heating rate is 2-10 ℃/min.
Ti 3 AlC 2 The porosity of the framework is 10-70%.
The sintering temperature affects the porosity, the higher the sintering temperature, the lower the porosity.
Impregnating, polymerizing and curing the resin monomer: for the Ti 3 AlC 2 Carrying out surface modification on the framework; impregnating surface-modified Ti with resin monomer solution 3 AlC 2 Skeleton until resin monomer solution is polymerized and solidified to obtain Ti 3 AlC 2 -a resin composite.
Wherein, for Ti 3 AlC 2 The specific steps of the surface modification of the framework are as follows: preparing a mixed solution of methanol and water, wherein the mass percentage of the methanol is 70% -90%; adding acetic acid into the mixed solution of methanol and water, and adjusting the pH value of the mixed solution to 4-7; adding a silane coupling agent (preferably gamma-methacryloxypropyl trimethoxy silane) with the mass percent of 5-25% into the mixed solution, and stirring to obtain a modified solution; ti is mixed with 3 AlC 2 Immersing the framework into the modifying liquid and standing, and taking out and drying after modification is finished.
Resin monomer impregnating Ti 3 AlC 2 The specific steps of skeleton, polymerization and solidification are as follows: preparing a resin monomer solution comprising methyl methacrylate and an initiatorThe mass of the initiator accounts for 0.2-1% of the mass of the resin monomer solution; dripping resin monomer solution into an infiltration container, and slowly immersing Ti 3 AlC 2 Vacuum assist for 20-40min; continuously dripping methyl methacrylate solution until Ti is submerged 3 AlC 2 Standing the framework in the atmospheric environment, and polymerizing methyl methacrylate; after polymerization is completed, ti is added 3 AlC 2 The backbone is heat treated at 40-90 c to ensure adequate cure of the polymerized methyl methacrylate.
(A) The composite material of the application has the components of nano sheet Ti 3 AlC 2 Powder and resin, flake Ti 3 AlC 2 The reinforcing phase realizes powder orientation in the process of multiple lapping and rolling, and the reinforcing effect of the reinforcing phase is fully exerted in the composite material, so that the composite material has excellent strength.
(B) The composite material of the application is compared with Ti 3 AlC 2 The ceramic has obviously improved fracture toughness and dynamic energy consumption property, so that the ceramic has excellent comprehensive mechanical property and considerable application prospect as a structural material
(C) The nano flaky Ti is realized in the composite material 3 AlC 2 The powder orientation method only needs flaky Ti 3 AlC 2 The powder has larger length-diameter ratio, no plasticizer is needed, the operation is simple, the process period is short, the efficiency is high, the cost is low, the prepared material has no size limitation, and the industrialization is easy to realize; in addition, the laminated structure formed in the repeated rolling and folding processes can reduce the thermal stress in the sintering process, and is easy to mold.
The application is further illustrated by the following examples:
example 1
This example mainly prepared a Ti 3 AlC 2 -a resin composite. Wherein the raw materials mainly comprise nano-sheet Ti 3 AlC 2 Powder (diameter 500+ -50 nm, thickness 50+ -10 nm), low viscosity polyvinyl alcohol (model 1788), deionized water, methanol solution, acetic acid solution, gamma-methacryloyloxy groupPropyl trimethoxysilane, methyl methacrylate; the specific preparation process is shown in figure 1.
And (3) bonding: 10g of low-viscosity polyvinyl alcohol was added to 100mL of deionized water, and continuous mechanical stirring was performed at 100℃until the polyvinyl alcohol was completely dissolved, to obtain a liquid polyvinyl alcohol adhesive having a mass fraction of 10%. 30g of nano-platelet-shaped Ti was weighed with an electronic balance having an accuracy of 0.0001 3 AlC 2 Pouring the powder into a surface dish, then dripping 15mL of the liquid polyvinyl alcohol adhesive into the surface dish, and continuously and mechanically stirring to obtain Ti 3 AlC 2 Mixing powder with liquid polyvinyl alcohol adhesive, and kneading repeatedly to obtain nanometer sheet Ti 3 AlC 2 The powder is completely adhered together to form Ti 3 AlC 2 Mud (i.e., dough-like mixture).
And (3) performing laminating and pressing: rolling Ti by a roll mill 3 AlC 2 The Ti obtained by the first rolling is rolled on the premise of ensuring the constant distance between the two rollers 3 AlC 2 Folding and rolling the thin blank, repeating for 30 times to obtain nano sheet Ti 3 AlC 2 The powder is preferentially oriented and arranged along the rotation direction of the roller under the action of the shearing force applied by the roller, and finally Ti with an oriented and arranged structure is obtained 3 AlC 2 A thin blank; ti is mixed with 3 AlC 2 Cutting the thin blank into 3×3cm pieces, placing the pieces in a steel mold, compressing the blank in a direction perpendicular to the sheet by using a hot press at 100deg.C under 6MPa for 1 hr, cooling, relieving pressure, and cooling to give Ti 3 AlC 2 The green body is removed from the mold and dried.
Removing organic matters and sintering: ti is mixed with 3 AlC 2 Placing the blank body in a tube furnace, heating from room temperature to 600 ℃ at a heating rate of 2 ℃/min under the condition of argon atmosphere, preserving heat for 5 hours, and then cooling to room temperature at the heating rate of 2 ℃/min to remove organic matters. Ti to remove organic matters 3 AlC 2 Placing the blank in a hot-pressing furnace, vacuumizing the hot-pressing furnace, introducing argon into the hot-pressing furnace, heating from room temperature to 900 ℃ at a heating rate of 10 ℃/min under the argon atmosphere,preserving heat for 1h, and then cooling to room temperature at a cooling rate of 10 ℃/min to obtain the porous Ti with the micro-directional structure 3 AlC 2 A skeleton, as shown in FIG. 2, of Ti 3 AlC 2 The porosity of the scaffold was about 62%.
Impregnating, polymerizing and curing the resin monomer: the configuration mass ratio is 9:1 and deionized water, and dropwise adding glacial acetic acid to the mixed solution under stirring to adjust the pH of the mixed solution to 4, and then adding 50g of gamma-methacryloxypropyl trimethoxysilane thereto, and stirring with a magnetic stirrer to obtain a silane coupling agent solution. Ti is mixed with 3 AlC 2 Slowly immersing the skeleton into a silane coupling agent solution, standing for 24 hours at room temperature and atmospheric environment, and drying to obtain Ti with modified surface 3 AlC 2 And (3) a framework. 1g of azobisisobutyronitrile initiator was added to 200g of methyl methacrylate monomer, and stirred with a magnetic stirrer until completely dissolved, to obtain a resin monomer solution. Surface-modified Ti under vacuum of 1Pa 3 AlC 2 Slowly immersing the skeleton in the resin monomer solution, sealing, standing in atmospheric environment, slowly polymerizing resin monomer, and heat treating at 80deg.C for 2 hr for complete solidification to obtain Ti 3 AlC 2 -a resin composite.
Ti prepared in this example 3 AlC 2 A resin composite, the microstructure of which is shown in figure 3. As can be seen from fig. 3: bright white nano flake Ti with volume fraction of 38% 3 AlC 2 The powder is arranged in a preferred orientation in a dark resin matrix, and the two phases show a bicontinuous structure. Wherein Ti is 3 AlC 2 The thickness of the sheet layer is 100+/-10 nm, ti 3 AlC 2 The spacing between the sheets was 100.+ -.10 nm.
Through testing, ti prepared in this example 3 AlC 2 The resin composite is parallel to Ti 3 AlC 2 The hardness in the lamellar direction was 0.79GPa, perpendicular to Ti 3 AlC 2 The hardness in the lamellar direction was 1.03GPa; the flexural strength in the direction perpendicular to the sheet was about 160MPa, parallel to Ti 3 AlC 2 Flexural strength in the sheet direction was about 68MPa, corresponding three-point bending stress-strain curve is shown in FIG. 4; perpendicular to Ti 3 AlC 2 Fracture toughness in the lamellar direction was 2.34MPa m 0.5 In parallel with Ti 3 AlC 2 Fracture toughness in the lamellar direction of 2.04MPa m 0.5 . In addition, ti prepared in this example 3 AlC 2 Resin composite with Si 3 N 4 Friction coefficient at counter-grinding is 0.48, conductivity is 26S.m -1 。
Example 2
This example mainly prepared a Ti 3 AlC 2 -a resin composite. Wherein the raw materials used were the same as in example 1.
The preparation process of this example differs from that of example 1 in that: removing organic matters and sintering. The organic matter removal and sintering steps of the embodiment are as follows: ti is mixed with 3 AlC 2 Placing the blank body in a tube furnace, heating from room temperature to 600 ℃ at a heating rate of 2 ℃/min under the condition of argon atmosphere, preserving heat for 5 hours, and then cooling to room temperature at the heating rate of 2 ℃/min to remove organic matters. Ti to remove organic matters 3 AlC 2 Placing the blank in a hot-pressing furnace, vacuumizing the hot-pressing furnace, introducing argon into the hot-pressing furnace, heating from room temperature to 800 ℃ at a heating rate of 2 ℃/min under the argon atmosphere, preserving heat for 1h, and cooling to room temperature at a cooling rate of 10 ℃/min to obtain the porous Ti with the micro-directional structure 3 AlC 2 A skeleton, as shown in FIG. 2, of Ti 3 AlC 2 The porosity of the scaffold was about 69%.
Other steps are consistent.
Through testing, ti prepared in this example 3 AlC 2 -resin composite material, in parallel to Ti 3 AlC 2 The hardness in the lamellar direction was 0.63GPa, perpendicular to Ti 3 AlC 2 The hardness in the lamellar direction was 0.94GPa; perpendicular to Ti 3 AlC 2 The flexural strength in the lamellar direction was about 150MPa, parallel to Ti 3 AlC 2 The flexural strength in the sheet direction was about 65MPa; fracture toughness in the direction perpendicular to the sheet layer was 3.03MPa m 0.5 In parallel withIn Ti 3 AlC 2 Fracture toughness in the lamellar direction was 2.83MPa m 0.5 The method comprises the steps of carrying out a first treatment on the surface of the In addition, ti prepared in this example 3 AlC 2 Resin composite with Si 3 N 4 Friction coefficient at the time of counter grinding was 0.36, conductivity was 20.2S.m -1 。
Example 3
This example mainly prepared a Ti 3 AlC 2 -a resin composite. Wherein the raw materials used were the same as in example 1.
The preparation process of this example differs from that of example 1 in that: removing organic matters and sintering. The organic matter removal and sintering steps of the embodiment are as follows: ti is mixed with 3 AlC 2 Placing the blank body in a tube furnace, heating from room temperature to 600 ℃ at a heating rate of 2 ℃/min under the condition of argon atmosphere, preserving heat for 5 hours, and then cooling to room temperature at the heating rate of 2 ℃/min to remove organic matters. Ti to remove organic matters 3 AlC 2 Placing the blank in a hot-pressing furnace, vacuumizing the hot-pressing furnace, introducing argon into the hot-pressing furnace, heating from room temperature to 1200 ℃ at a heating rate of 2 ℃/min under the argon atmosphere, preserving heat for 1h, and cooling to room temperature at a cooling rate of 10 ℃/min to obtain the porous Ti with the micro-directional structure 3 AlC 2 A skeleton, as shown in FIG. 2, of Ti 3 AlC 2 The porosity of the scaffold was about 44%.
Other steps are consistent.
Through testing, ti prepared in this example 3 AlC 2 -resin composite material, in parallel to Ti 3 AlC 2 The hardness in the lamellar direction was 1.01GPa, perpendicular to Ti 3 AlC 2 The hardness in the lamellar direction was 1.30GPa; perpendicular to Ti 3 AlC 2 The flexural strength in the lamellar direction was about 201MPa, parallel to Ti 3 AlC 2 The flexural strength in the sheet direction was about 94MPa; perpendicular to Ti 3 AlC 2 Fracture toughness in the sheet direction was 1.94MPa m 0.5 In parallel with Ti 3 AlC 2 Fracture toughness in the lamellar direction was 1.51MPa m 0.5 The method comprises the steps of carrying out a first treatment on the surface of the In addition, the composite material is combined with Si 3 N 4 During counter grindingHas a friction coefficient of 0.56 and a conductivity of 32S.m -1 。
As can be seen from the above embodiments of the present application, the nano sheet-like Ti is realized 3 AlC 2 The orientation of the powder can improve the mechanical properties, especially the strength, of the composite material. The embodiment of the application adopts a composition composite design, and is characterized by strong Ti 3 AlC 2 Introducing ductile resin to make nano flake Ti in composite material 3 AlC 2 The powder is arranged in the resin matrix in an oriented manner, and a bicontinuous structure is shown. The embodiment of the application prepares the Ti with excellent bending strength, fracture toughness, conductivity and wear resistance by a simple process 3 AlC 2 -a resin composite.
Comparative example 1
This comparative example mainly prepares a Ti 3 AlC 2 -a resin composite. Wherein the raw material is nano sheet Ti 3 AlC 2 Powder (diameter 500+ -50 nm, thickness 50+ -10 nm). The specific preparation process is as follows:
preparing a framework: 100g of nano sheet Ti is weighed by an electronic balance with the precision of 0.0001 3 AlC 2 Pouring powder into a graphite crucible with the diameter of 50mm, placing the graphite crucible into a hot pressing furnace, heating the powder from room temperature to 900 ℃ at the heating rate of 10 ℃/min under the condition of argon protection atmosphere, preserving the heat for 1h, and cooling the powder to room temperature at the heating rate of 10 ℃/min to obtain the porous Ti without the micro-directional structure 3 AlC 2 A scaffold having a porosity of about 73%.
Impregnating, polymerizing and curing the resin monomer: the configuration mass ratio is 9:1 and deionized water, and then adding dropwise glacial acetic acid to the mixture under stirring to adjust the pH of the mixture to 4, and then adding 100g of gamma-methacryloxypropyl trimethoxysilane thereto, and stirring with a magnetic stirrer to obtain a modified liquid. Ti is mixed with 3 AlC 2 Slowly immersing the skeleton into the modifying liquid, standing for 24 hours at room temperature and atmospheric environment, and drying to obtain Ti with modified surface 3 AlC 2 And (3) a framework. 2g of azobisisobutyronitrile initiator were added to 400g of methyl methacrylateAnd (3) stirring the monomers by using a magnetic stirrer until the monomers are completely dissolved, so as to obtain a resin monomer solution. Surface-modified Ti under vacuum of 1Pa 3 AlC 2 Slowly immersing the skeleton in the resin monomer solution, sealing, standing in atmospheric environment, slowly polymerizing resin monomer, and heat treating at 80deg.C for 2 hr for complete solidification to obtain Ti 3 AlC 2 -a resin composite.
Through testing, ti prepared in this comparative example 3 AlC 2 -resin composite material, in parallel to Ti 3 AlC 2 The hardness in the lamellar direction was 0.51GPa, perpendicular to Ti 3 AlC 2 The hardness in the lamellar direction was 0.84GPa; perpendicular to Ti 3 AlC 2 The flexural strength in the lamellar direction was about 105MPa, parallel to Ti 3 AlC 2 The flexural strength in the sheet direction was about 43MPa; fracture toughness in the direction perpendicular to the sheet was 1.79Pa m 0.5 In parallel with Ti 3 AlC 2 Fracture toughness in the lamellar direction was 1.32MPa m 0.5 The method comprises the steps of carrying out a first treatment on the surface of the In addition, ti prepared in this example 3 AlC 2 Resin composite with Si 3 N 4 Friction coefficient at counter-grinding is 0.24, conductivity is 19.6S.m -1 。
Comparative example 1 is the preparation of Ti directly by blending 3 AlC 2 Resin composite without alignment of nano-platelet Ti 3 AlC 2 The powder is oriented. From comparison of the data of comparative example 1 and the above examples, it can be seen that Ti prepared in comparative example 1 3 AlC 2 The resin composite is poor in hardness, flexural strength, fracture toughness, coefficient of friction, electrical conductivity.
Comparative example 2
This comparative example mainly prepares a Ti 3 AlC 2 -a resin composite. Wherein the raw material is micron flake Ti 3 AlC 2 Powder (diameter 16+ -1 μm, thickness 500+ -50 nm).
The other steps are identical to those of comparative example 1.
Through testing, ti prepared in this comparative example 3 AlC 2 -resin composite materialIn parallel with Ti 3 AlC 2 The hardness in the lamellar direction was 0.57GPa, perpendicular to Ti 3 AlC 2 The hardness in the lamellar direction was 0.92GPa; perpendicular to Ti 3 AlC 2 The flexural strength in the lamellar direction was about 83MPa, parallel to Ti 3 AlC 2 The flexural strength in the sheet direction was about 32MPa; fracture toughness in the direction perpendicular to the sheet layer was 1.91MPa m 0.5 In parallel with Ti 3 AlC 2 Fracture toughness in the lamellar direction of 1.47MPa m 0.5 The method comprises the steps of carrying out a first treatment on the surface of the In addition, ti prepared in this example 3 AlC 2 Resin composite with Si 3 N 4 Friction coefficient at the time of counter grinding was 0.31, conductivity was 19.2S.m -1 。
Comparative example 2. Compared to comparative example 1, nano-platelet-shaped Ti 3 AlC 2 The powder is replaced with micron-sized powder. From comparison of the data of comparative example 2 and the above examples, it can be seen that Ti prepared in comparative example 2 3 AlC 2 The resin composite is poor in hardness, flexural strength, fracture toughness, coefficient of friction, electrical conductivity.
Comparative example 3
This comparative example mainly prepares a Ti 3 AlC 2 -a resin composite. Wherein the raw materials used were the same as those of comparative example 1. The method comprises the following specific steps:
configuration Ti 3 AlC 2 And (3) sizing: 65g of deionized water was added dropwise to a 250ml plastic jar, and 35g of nanoplatelets of Ti were weighed using an electronic balance with an accuracy of 0.0001 3 AlC 2 Pouring the powder into a wide-mouth bottle, and continuously mechanically stirring until Ti is obtained 3 AlC 2 The powder is uniformly dispersed in water. The jar was placed in a water bath at 70 ℃ for 30min and then 0.325g of propylhydroxy methylcellulose powder was added and mechanically stirred continuously until completely dispersed in the slurry. The slurry was removed and after cooling, 0.35g of Darvan CN dispersant was added to the slurry and stirred until uniformly dispersed. Finally, 5 zirconia balls with diameters of 3mm and 6mm were added, and the balls were sealed and placed on a drum ball mill with a rotation speed of 300rpm for ball milling for 24 hours.
Freezing casting and vacuumAnd (3) freeze drying: pouring the ball-milled slurry into a rectangular polymethyl methacrylate mould with the size of 20mm multiplied by 20mm, sealing the lower end of the mould by a polydimethyl oxygen alkane base with the inclination angle of 25 degrees, placing the mould on a copper plate, linking the other side of the copper plate with a copper rod with one end immersed in liquid nitrogen, directionally solidifying water in the slurry from bottom to top through cooling the copper plate, and enabling nano-sheet Ti to be directionally solidified by ice crystals growing along the solidification direction 3 AlC 2 The powder is extruded between the ice crystals to realize the directional arrangement of the powder. Taking out the slurry from the mold after the slurry is completely solidified, placing the slurry in a freeze dryer with cold trap temperature of-60 ℃ and vacuum degree of 1Pa for 72 hours to remove water, and finally obtaining Ti with directional porous structure composed of lamellar layers 3 AlC 2 And (3) a framework.
The steps of removing organic matters and sintering, impregnating resin monomers, polymerizing and curing are the same as those of comparative example 1.
Through testing, ti prepared in this comparative example 3 AlC 2 -resin composite material, in parallel to Ti 3 AlC 2 The hardness in the lamellar direction was 0.87GPa, perpendicular to Ti 3 AlC 2 The hardness in the lamellar direction was 1.05GPa; perpendicular to Ti 3 AlC 2 The flexural strength in the lamellar direction was about 151MPa, parallel to Ti 3 AlC 2 The flexural strength in the sheet direction was about 59MPa; perpendicular to Ti 3 AlC 2 Fracture toughness in the lamellar direction was 1.52MPa m 0.5 In parallel with Ti 3 AlC 2 Fracture toughness in the lamellar direction was 1.09MPa m 0.5 The method comprises the steps of carrying out a first treatment on the surface of the In addition, the composite material is combined with Si 3 N 4 Friction coefficient at the time of counter grinding is 0.49, conductivity is 25S.m -1 。
Comparative example 3 is Ti prepared by an orientation method using an ice template 3 AlC 2 -a resin composite; the composite material has good hardness and strength, but poor toughness and friction coefficient; because the ice template orientation method can orient the nano sheets in each sheet layer though being capable of orienting the sheet layer structure, but the packing rolling orientation method of the embodiment of the application can orient not only the sheet layer structure, but also each nano sheet layerThe nano sheets in the lamellar structure can be oriented, so that the application can induce crack deflection and improve the toughness of the composite material.
The above description is only of the preferred embodiments of the present application, and is not intended to limit the present application in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present application still fall within the scope of the technical solution of the present application.
Claims (28)
1. Ti (titanium) 3 AlC 2 -a process for the preparation of a resin composite, characterized in that it comprises the following steps:
and (3) bonding: ti is mixed with 3 AlC 2 Mixing the powder with an adhesive to make Ti 3 AlC 2 Bonding the powder together to obtain Ti 3 AlC 2 Mud; wherein the Ti is 3 AlC 2 The powder is nano flake Ti with the diameter of 200nm-2 mu m and the thickness of 20-200nm 3 AlC 2 Powder;
and (3) performing laminating and pressing: for the Ti 3 AlC 2 Performing pad rolling treatment on the mud to ensure that Ti is 3 AlC 2 Ti in mud 3 AlC 2 The powder is directionally arranged to obtain Ti with directional arrangement structure 3 AlC 2 A thin blank; ti of multiple directional arrangement structure 3 AlC 2 Stacking the thin blanks together for pressing treatment to obtain Ti 3 AlC 2 A blank body; the step of the lap rolling treatment comprises the following steps: causing the Ti to be 3 AlC 2 Rolling mud between two rollers of a roller machine to form a thin blank, folding the thin blank, rolling the thin blank, and repeatedly folding and rolling for a plurality of times to obtain Ti with a directional arrangement structure 3 AlC 2 A thin blank; in the step of the press treatment: the temperature of the pressing treatment is 30-120 ℃, the pressure is 2-20MPa, and the time is 0.5-3h;
removing organic matters and sintering: for the Ti 3 AlC 2 The green body is subjected to organic matter removal treatment and sintering treatment to obtain Ti 3 AlC 2 A skeleton;
impregnating, polymerizing and curing the resin monomer: for the Ti 3 AlC 2 Carrying out surface modification on the framework; impregnating surface-modified Ti with resin monomer solution 3 AlC 2 A framework, and Ti is obtained after the polymerization and solidification of the resin monomer solution 3 AlC 2 -a resin composite.
2. Ti according to claim 1 3 AlC 2 -a method for preparing a resin composite material, characterized in that in said bonding step:
the adhesive is one or more of polyvinyl alcohol adhesive, hydroxypropyl methyl cellulose adhesive, polyethylene glycol adhesive, sucrose adhesive, liquid paraffin adhesive and glycerol adhesive.
3. Ti according to claim 2 3 AlC 2 -a process for the preparation of a resin composite, characterized in that the polyvinyl alcohol binder comprises a low viscosity polyvinyl alcohol and water; wherein the mass fraction of the low-viscosity polyvinyl alcohol in the polyvinyl alcohol adhesive is 2-15%.
4. Ti according to claim 1 3 AlC 2 -a method for preparing a resin composite material, characterized in that in said bonding step:
ti is mixed with 3 AlC 2 Mixing the powder and the adhesive to obtain a mixture, and kneading the mixture until Ti 3 AlC 2 The powder is completely bonded together to obtain Ti 3 AlC 2 Mud.
5. Ti according to claim 1 3 AlC 2 -a method for the preparation of a resin composite material, characterized in that the distance between the two rolls of the rolling mill is unchanged during a plurality of rolling operations.
6. Ti according to claim 1 3 AlC 2 -a process for the preparation of a resin composite, characterized in that the pressThe preparation process comprises the following steps: ti of the orientation arrangement structure 3 AlC 2 Cutting thin blanks into multiple directional arrangement structures of same size 3 AlC 2 After the thin blanks are stacked together for pressing.
7. Ti according to claim 1 3 AlC 2 -a process for the preparation of a resin composite, characterized in that said step of organic matter removal treatment comprises:
under a protective atmosphere, make the Ti 3 AlC 2 The blank is kept at the heat preservation temperature for a first set time.
8. Ti according to claim 7 3 AlC 2 -a process for the preparation of a resin composite, characterized in that, in said step of organic matter removal treatment:
the heat preservation temperature is 300-700 ℃ and the first set time is 3-8h.
9. Ti according to claim 7 3 AlC 2 -a process for the preparation of a resin composite, characterized in that, in said step of organic matter removal treatment:
under a protective atmosphere, subjecting the Ti to 3 AlC 2 Heating the blank to a heat preservation temperature, and preserving heat for a first set time at the heat preservation temperature.
10. Ti according to claim 9 3 AlC 2 -a process for the preparation of a resin composite, characterized in that, in the presence of said Ti 3 AlC 2 In the process of heating the blank to the heat preservation temperature, the heating rate is 1-8 ℃/min.
11. Ti according to claim 1 3 AlC 2 -a method for preparing a resin composite, characterized in that said step of sintering treatment comprises:
under the protection atmosphere, ti after the organic matter removal treatment 3 AlC 2 Green body in-burningSintering at junction temperature to obtain Ti 3 AlC 2 A skeleton; wherein the sintering temperature is 700-1300 ℃, and the sintering treatment time is 1-5h.
12. Ti according to claim 11 3 AlC 2 A process for preparing the resin composite material, which is characterized in that Ti after organic matter removal is treated in a protective atmosphere 3 AlC 2 Heating the green body to the sintering temperature, wherein the heating rate is 2-10 ℃/min.
13. Ti according to claim 1 3 AlC 2 -a process for the preparation of a resin composite, characterized in that said Ti 3 AlC 2 The porosity of the framework is 10-70%.
14. Ti according to claim 1 3 AlC 2 -a process for the preparation of a resin composite, characterized in that in the resin monomer impregnation, polymerization curing step:
for the Ti 3 AlC 2 The step of surface modification of the skeleton comprises the following steps: subjecting the Ti to 3 AlC 2 Immersing the skeleton in a modifying liquid containing a silane coupling agent, and subjecting the Ti to a reaction 3 AlC 2 Surface modifying the skeleton, and taking out the Ti after surface modification after finishing the surface modification 3 AlC 2 And (5) skeleton and drying.
15. Ti according to claim 14 3 AlC 2 -a process for the preparation of a resin composite, characterized in that in the modifying liquid: the mass percentage of the silane coupling agent is 5-25%.
16. Ti according to claim 14 3 AlC 2 -a process for the preparation of a resin composite, characterized in that in the modifying liquid: the solvent is a mixture of methanol and water with pH value adjusted to 4-7 by acetic acid.
17. Root of Chinese characterTi according to claim 16 3 AlC 2 The preparation method of the resin composite material is characterized in that the mass fraction of the methanol in the mixed liquid of the methanol and the water is 70-90%.
18. Ti according to claim 14 3 AlC 2 -a process for the preparation of a resin composite, characterized in that in the resin monomer impregnation, polymerization curing step:
impregnating the surface-modified Ti with a resin monomer solution 3 AlC 2 A framework, after the resin monomer solution is polymerized, heat treatment is carried out to solidify the resin, thus obtaining Ti 3 AlC 2 -a resin composite.
19. Ti according to claim 18 3 AlC 2 -a process for the preparation of a resin composite, characterized in that the resin monomer solution comprises methyl methacrylate and an initiator; wherein, in the resin monomer solution, the mass fraction of the initiator is 0.2-1%.
20. Ti according to claim 18 3 AlC 2 -a process for the preparation of a resin composite, characterized in that the temperature of the heat treatment is between 40 and 90 ℃.
21. Ti according to claim 18 3 AlC 2 -a process for the preparation of a resin composite, characterized in that the polymerization time of the resin monomer is 4-10 days.
22. Ti according to claim 18 3 AlC 2 The preparation method of the resin composite material is characterized in that the resin monomer solution is dripped into an infiltration container, the infiltration container is immersed into a sample, the vacuum assistance is carried out, the dripping of the resin monomer solution is continued until the sample is submerged, the resin monomer solution is stood under the atmospheric environment, and the resin monomer solution is polymerized.
23. The method of claim 22Ti of (2) 3 AlC 2 -a process for the preparation of a resin composite, characterized in that the vacuum-assisted time is 20-40min.
24. Ti (titanium) 3 AlC 2 -a resin composite material, characterized in that the Ti 3 AlC 2 The resin composite is made of two-dimensional nano-platelet-shaped Ti 3 AlC 2 And a resin composition, wherein the Ti is in volume percent 3 AlC 2 30-90% of the total content of the resin and the balance of the resin;
on microstructure, the Ti is 3 AlC 2 Nanoplatelets of Ti in resin composite 3 AlC 2 Is arranged in a preferential orientation in the resin matrix to form a biphasic continuous structure.
25. Ti according to claim 24 3 AlC 2 -a resin composite material, characterized in that,
in the dual-phase continuous structure, the Ti 3 AlC 2 The thickness of the sheet layer is 20-200nm, and the spacing between the sheet layers is 0.1-1 μm.
26. Ti according to claim 24 3 AlC 2 -a resin composite, characterized in that the resin is polymethyl methacrylate.
27. Ti according to claim 24 3 AlC 2 -a resin composite material, characterized in that the Ti 3 AlC 2 Nanoplatelets of Ti in resin composite 3 AlC 2 Is arranged in a preferred orientation in the resin matrix along the direction of rotation of the nip roll.
28. Ti according to any one of claims 24-27 3 AlC 2 -a resin composite material, characterized in that the Ti 3 AlC 2 -the resin composite is made of Ti as claimed in any one of claims 1 to 23 3 AlC 2 -a resin composite material.
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| KR20090025941A (en) * | 2007-09-07 | 2009-03-11 | 한국기계연구원 | A manufacturing method of phosphorus dioxidized copper sheet using three-layer stack accumulative roll-bonding process |
| CN102424920A (en) * | 2011-09-14 | 2012-04-25 | 上海交通大学 | In-situ preparation method of micro nano laminated metal-based composite material |
| CN108752821A (en) * | 2018-06-14 | 2018-11-06 | 中国科学院金属研究所 | Silicon carbide with microcosmic oriented structure/resin bionic composite material and preparation method thereof |
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|---|---|---|---|---|
| KR20090025941A (en) * | 2007-09-07 | 2009-03-11 | 한국기계연구원 | A manufacturing method of phosphorus dioxidized copper sheet using three-layer stack accumulative roll-bonding process |
| CN102424920A (en) * | 2011-09-14 | 2012-04-25 | 上海交通大学 | In-situ preparation method of micro nano laminated metal-based composite material |
| CN108752821A (en) * | 2018-06-14 | 2018-11-06 | 中国科学院金属研究所 | Silicon carbide with microcosmic oriented structure/resin bionic composite material and preparation method thereof |
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