CN109180186A - The preparation method of bionical nacre MAX phase carbide ceramics based composites - Google Patents

The preparation method of bionical nacre MAX phase carbide ceramics based composites Download PDF

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CN109180186A
CN109180186A CN201811006638.0A CN201811006638A CN109180186A CN 109180186 A CN109180186 A CN 109180186A CN 201811006638 A CN201811006638 A CN 201811006638A CN 109180186 A CN109180186 A CN 109180186A
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max phase
sintering
nacre
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lamella
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CN109180186B (en
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杨锐
谢曦
崔玉友
贾清
柏春光
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Institute of Metal Research of CAS
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Abstract

The present invention relates to MAX phase ceramics based composites, specially a kind of method for preparing bionical nacre MAX phase carbide ceramics based composites.This method is using sheet MAX powder as constructing the brick for piling up composite material, using liquid medium crystal growth temperature gradient orientation, the stratiform solidification crystalline ceramic composite construction in similar natural peral shell is obtained by cryogenic freezing liquid medium, then dielectric crystal is got rid of, the idiosome of the ceramic macromolecular of continuous lamella hole and lamellar structure is obtained.In pressure sintering process, the carbide of sheet is generated using high molecular polymer as carbon source reaction in-situ.The final MAX phase lamella composition brick for obtaining nanometer or micron, constitutes long-range order brick-stucco structure of the imitative pearl layer material of plaster in the carbide lamella of MAX phase lamella central home growth.This structure has very high drag as the bioceramic of nature, to external load and crack propagation.

Description

The preparation method of bionical nacre MAX phase carbide ceramics based composites
Technical field
The present invention relates to MAX phase ceramics based composites, specially a kind of bionical nacre MAX phase carbide ceramics base is multiple The preparation method of condensation material.
Background technique
MAX phase ceramics are (such as: Ti3SiC2、Ti2AlC、Nb2AlC etc.) it is a kind of with nano ternary layer structure and numerous The processable ceramic of unique excellent properties, such material have both the property of ceramics and metal.Such as: the high-melting-point of ceramic material resists The performances such as oxidation and resistance to corrosion, the electric conductivity of metal, machinability, damage capacitive reactance, heat shock resistance, the resistance to spoke of nano ceramics It penetrates damaging.Due to its unique ternary nano layer structure, the fracture toughness of such ceramics is much higher than common aluminium oxide, carbonization The engineering ceramics such as silicon.But be compared to for metal, the intensity and fracture toughness of such ceramics are also far from enough, therefore pass through Intensity, fracture toughness, the preparation method of mechanical behavior under high temperature and the technology of the ceramics can be improved in the method research and development of bionic Seem extremely important.
The Nature forms many efficient and rational material components and structure in 1 years evolutionary process in organism, Testacean natural peral layer material is exactly one of them, such material has unique brick-ash structure, it is by 95% parts by volume The grey matter composition that the brick matter and 5% volume parts that several flaky calcium carbonate layers is constituted are constituted.Although composition is simple, by multiple Miscellaneous structure it is fine combination and have extraordinary comprehensive performance.The structure causes material to have excellent mechanical property, shell The natural peral layer of class can reach as many as several times of ordinary calcium carbonate.In recent years, people take a hint from natural biological research, Biomimetic features design concept is introduced in design of material, is efficiently evolved the material structure of formation by imitating and transplanting the Nature, Realize high-strength, the high-ductility characteristic of material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of bionical nacre MAX phase carbide ceramics based composites Method, solves existing MAX phase carbide ceramics intensity and poor toughness does not have the problems such as bionic structure.
The technical scheme is that
A kind of preparation method of bionical nacre MAX phase carbide ceramics based composites is made using sheet MAX powder Pass through cryogenic freezing to construct the brick for piling up composite material using liquid medium crystal growth in the orientation of temperature gradient Liquid medium solidifies crystalline ceramic composite construction to obtain the stratiform in similar natural peral shell, then gets rid of medium crystalline substance Body obtains the ceramic macromolecular idiosome of continuous lamella hole and lamellar structure;It is carbonized to ceramic macromolecular idiosome, utilizes height Molecularly Imprinted Polymer generates the carbide of sheet as carbon source reaction in-situ;Pressure sintering is carried out to the idiosome that carbonization is completed, is obtained Obtain bionical nacre MAX phase carbide ceramics based composites.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, the rule of sheet MAX powder For lattice having a size of 0.02~10 micron of thickness, 0.1~50 micron of width, liquid medium crystal is water, the tert-butyl alcohol or amphene, serialgram The structure of layer hole and the ceramic macromolecular idiosome of lamellar structure is: being determined by what the MAX powder of high molecular polymer glue connection was constituted To sheet skeleton, the continuous lamella hole that leaves after MAX powder piece interlayer is distilled by liquid medium crystal.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, ceramic matric composite tool There is long-range order brick-stucco structure of imitative pearl layer material, nanoscale or micron-sized MAX phase lamella constitute brick in the structure Block constitutes plaster in the carbide lamella of MAX phase lamella central home growth;Wherein, the specification of MAX phase lamella is thickness 0.02~10 micron, 0.1~50 micron of width;The specification of carbide lamella be 0.02~1 micron of thickness, MAX phase lamella with The weight ratio of carbide lamella is 5~50:1.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, includes the following steps:
(1) MAX phase powder, organic gel, the dispersing agent of nanometer or micron sheet are added in solvent, are uniformly mixed Slurry is formed, mixed method is ultrasonic wave dispersion, mechanical stirring or ball milling mixing;
(2) mixed slurry is fitted into mold, mold is put into the freezing equipment that can cause gradient low temperature and is carried out Directional solidification, cryogenic temperature and temperature gradient are determined by the physical chemistry coagulating property of compound slurry;
(3) after the completion of solidifying, the complete ceramic macromolecular idiosome of oriented growth is put into drying machine and is dried, drying parameter It is determined by the physicochemical characteristics of solvent;
(4) idiosome after the completion of drying is taken out and carries out carbonization technique, carbonization carries out in vacuum drying oven, carburizing temperature 400 ~600 DEG C, atmosphere 10-4Pa~10-2Pa vacuum environment, carbonization time 0.5~4 hour;
(5) pressure sintering is carried out to the idiosome that carbonization is completed, sintering temperature is by the granularity and MAX phase of the material powder used Type determine.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, solvent be water or other With liquid form, reducing temperature can be in solid-state, and be able to achieve the solvent of solid gaseous physical distillation transformation;Organic gel is polyethylene Alcohol, polyethylene glycol or carboxymethyl cellulose, dispersing agent are sodium alklyarylsulfonate, alkyl phenol polyvinylether or ammonium polyacrylate.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, it is by weight percentage, former MAX phase powder content in material is 30~60%, organic gel content is 2~10%, dispersant is 0.5~5%, solvent is Surplus.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, pressure sintering are hot pressing burning Connection, HIP sintering method or discharge plasma sintering method.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, hot pressing sintering method is direct Idiosome is packed into graphite jig, the hot pressed sintering in graphite jig, 500~2000 DEG C of sintering temperature, sintering pressure 1~ 200MPa, soaking time 10~3600 minutes, 1~100 DEG C/min of heating rate, sintering carried out under vacuum or argon atmosphere.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, HIP sintering method are Directly idiosome is fitted into hot isostatic pressing jacket, is then evacuated and hermetically sealed jacket;The HIP sintering in jacket, sintering 500~2000 DEG C of temperature, 1~800MPa of sintering pressure, soaking time 10~3600 minutes, 1~100 DEG C/min of heating rate, Sintering carries out under vacuum or argon atmosphere.
The preparation method of the bionical nacre MAX phase carbide ceramics based composites, discharge plasma sintering method It is that directly idiosome is fitted into sintering mold, is applying big pulse electric current sintering, 300~1800 DEG C of sintering temperature, sintering is pressed 1~400MPa of power, soaking time 5~600 minutes, 1~500 DEG C/min of heating rate, sintering under vacuum or argon atmosphere into Row.
Design philosophy of the invention is:
The present invention prepares bionical nacre MAX phase carbide ceramics based composites by simple and environmentally-friendly method, utilizes Sheet MAX powder piles up the brick of material as constructing, and by cryogenic freezing liquid medium, utilizes liquid medium crystal growth In the orientation of temperature gradient, crystalline ceramic composite construction is solidified to obtain the stratiform in similar natural peral shell, is then gone Dielectric crystal is removed, the idiosome of the ceramic macromolecular of continuous lamella hole and lamellar structure is obtained.In pressure sintering process, utilize High molecular polymer (i.e. organic gel, packet polyvinyl alcohol, polyethylene glycol or carboxymethyl cellulose etc.) is raw as carbon source reaction in-situ At the carbide of sheet, finally obtains nanoscale or micron-sized MAX phase lamella in the structure and constitute brick, in MAX photograph The nano silicon carbide nitride layer of layer central home growth constitutes brick-stucco structure of the imitative pearl layer material of plaster.This structure is such as It is the same with the bioceramic of nature, there is very high drag to external load and crack propagation.
The invention has the advantages and beneficial effects that:
(1) present invention process route and preparation method are simple, green and pollution-free using raw material and preparation method, are easy to It is widely applied.
(2) the method for the present invention adapts to all MAX phase systems, can prepare all such bionic ceramic bases of MAX phase type Composite material.
(3) ceramics prepared by the present invention are designed using bionics principle, and mechanical property greatly improves, this bionical knot Structure causes the property of ceramics excellent.
Detailed description of the invention
Fig. 1 is the sample microstructure morphology obtained after being freeze-dried.
Fig. 2 is nacre Ti after the completion of sintering3AlC2/ TiC nanocomposite vertical slice direction fracture picture.
Specific embodiment
Since the present invention covers technical method and route is extensive, for help to further understand the purpose of this discovery, scheme, Specific example is first combined to carry out the description of further complete display with advantage.Simultaneously it is to be noted that example disclosed below It is merely possible to the part enumerated work and embodiment, and not all scheme can be implemented.It is all to use right of the present invention Technical method in claimed range, is within the scope of protection of the invention.
Embodiment 1
In the present embodiment, bionical nacre MAX phase carbide ceramics based composites the preparation method is as follows:
By 200 nanometers of granularity of sheet Ti3AlC2100 grams of powder, 5 grams of the polyvinyl alcohol of molecular weight 4000, dispersing agent poly- third It 2 grams of olefin(e) acid ammonium, adds in 200 grams of deionized waters, mechanical stirring is uniformly mixed.Slurry after being simply mixed is put into In the polyurethane ball-milling pot of 500mL, the iron ball of 200 grams of polyurethane cladding is added.Ball grinder is mounted on planetary ball mill Ball milling is carried out, the slurry after ball milling is taken out after 380 revs/min of rotational speed of ball-mill, ball milling 10 hours, it is stand-by to sort out ball milling pearl. The slurry of acquisition is fitted into Teflon mould, mold bottom places copper sheet, and is passed through liquid nitrogen, liquid nitrogen stream from copper sheet bottom It is 5L/ hours fast, it will finally be taken out after the complete freeze forming of slurry.The solid mixt of freeze forming is put into freeze drier In, setting freeze-drying temperature at -50 DEG C, vacuum degree 10Pa, took out after 50 hours by freeze-drying.
As shown in Figure 1, the sample microstructure morphology obtained after freeze-drying, the solid mixt is by nanometer Ti3AlC2 Powder, and organic matter for curing molding form, wherein nanometer Ti3AlC2Powder ball combinate form is at lamella and is orientated tissue, in lamella Between be made of continuous lamella hole, be continuous through the bore hole size of idiosome at 10~30 microns.The solid mixt is put into very Sintering in empty hot-pressed sintering furnace, 1250 DEG C of sintering temperature, pressure 40MPa, sintering atmosphere 10-3Pa vacuum condition.After the completion of sintering, Obtain fine and close nacre Ti3AlC2/ TiC nanocomposite.
As shown in Fig. 2, nacre Ti after the completion of sintering3AlC2/ TiC nanocomposite vertical slice direction fracture picture, By picture it is found that Ti3AlC2It piles up with good orientation and in brick, the TiC of Nanoparticulate is distributed in Ti3AlC2Brick Between be in putty-like, Ti3AlC2The specification of phase lamella is 100~300 nanometers of thickness, 1~3 micron of width, the specification of TiC layer Having a size of 100~300 nanometers, Ti3AlC2Weight ratio with TiC is 6:1.
The usable material chamber adiabator compressive strength reaches 2500MPa, 18~21MPa.m of fracture toughness1/2, much higher than common Ti3AlC27~8MPa.m1/2Fracture Toughness, 1100 DEG C of compressive strengths of high-temperature behavior reach 200MPa, much higher than common Ti3AlC2100MPa intensity.
Embodiment 2
In the present embodiment, bionical nacre MAX phase carbide ceramics based composites the preparation method is as follows:
By 220 nanometers of granularity of sheet Nb2200 grams of AlC powder, 6 grams of the polyvinyl alcohol of molecular weight 4000, dispersing agent poly- third It 3 grams of olefin(e) acid ammonium, adds in 250 grams of amphenes, mechanical stirring is uniformly mixed.Slurry after being simply mixed is put into 500mL's In polyurethane ball-milling pot, the iron ball of 250 grams of polyurethane cladding is added.Ball grinder is mounted on planetary ball mill and carries out ball It grinds, the slurry after ball milling is taken out after 400 revs/min of rotational speed of ball-mill, ball milling 10 hours, it is stand-by to sort out ball milling pearl.It will obtain Slurry be fitted into Teflon mould, mold bottom places copper sheet, and is passed through liquid nitrogen, liquid nitrogen flow velocity 1L/ from copper sheet bottom Hour, it will finally be taken out after the complete freeze forming of slurry.The solid mixt of freeze forming is put into and is dried in drying machine, is set dry For temperature at 25 DEG C, one atmospheric pressure of environment takes out solid mixt, nanometer Nb after 10 hours dry2AlC powder ball combinate form is at lamella With orientation tissue, it is made of continuous lamella hole among lamella, the bore hole size of lamella hole is at 20~50 microns.By the solid-state Mixture is put into vacuum sintering funace and is sintered, and 1350 DEG C of sintering temperature, pressure 40MPa, sintering atmosphere 10-3Pa vacuum item Part.After the completion of sintering, fine and close nacre Nb is obtained2AlC/NbC nanocomposite.Nb2AlC has good orientation and is in Brick is piled up, and the NbC of Nanoparticulate is distributed in Nb2It is in putty-like, Nb between AlC brick2The specification of AlC phase lamella is thickness 150~320 nanometers, 1~3 micron of width are spent, NbC layers of specification is 100~300 nanometers, Nb2The weight ratio of AlC and NbC Example is 8:1.
The usable material chamber adiabator compressive strength reaches 260MPa, 18~21MPa.m of fracture toughness1/2, it is much higher than common Nb2AlC 7~8MPa.m1/2Fracture Toughness, 1400 DEG C of bending strengths of high-temperature behavior reach 450MPa, are much higher than common Nb2AlC's The intensity of 300MPa.

Claims (10)

1. a kind of preparation method of bionical nacre MAX phase carbide ceramics based composites, which is characterized in that utilize sheet MAX powder piles up the brick of composite material as constructing, and using liquid medium crystal growth in the orientation of temperature gradient, passes through Cryogenic freezing liquid medium solidifies crystalline ceramic composite construction to obtain the stratiform in similar natural peral shell, then gets rid of Dielectric crystal obtains the ceramic macromolecular idiosome of continuous lamella hole and lamellar structure;It is carbonized to ceramic macromolecular idiosome, The carbide of sheet is generated using high molecular polymer as carbon source reaction in-situ;The idiosome completed to carbonization carries out pressurization burning Knot, obtains bionical nacre MAX phase carbide ceramics based composites.
2. the preparation method of bionical nacre MAX phase carbide ceramics based composites described in accordance with the claim 1, feature It is, the specification of sheet MAX powder is 0.02~10 micron of thickness, and 0.1~50 micron of width, liquid medium crystal is The structure of the ceramic macromolecular idiosome of water, the tert-butyl alcohol or amphene, continuous lamella hole and lamellar structure is: by high molecular polymer The orienting piece layered framework that the MAX powder of glue connection is constituted, MAX powder piece interlayer leave continuous after being distilled by liquid medium crystal Lamella hole.
3. the preparation method of bionical nacre MAX phase carbide ceramics based composites described in accordance with the claim 1, feature It is, ceramic matric composite has long-range order brick-stucco structure of imitative pearl layer material, nanoscale or micro- in the structure The MAX phase lamella of meter level constitutes brick, constitutes plaster in the carbide lamella of MAX phase lamella central home growth;Wherein, MAX phase The specification of lamella is 0.02~10 micron of thickness, 0.1~50 micron of width;The specification of carbide lamella is thickness 0.02 ~1 micron, the weight ratio of MAX phase lamella and carbide lamella is 5~50:1.
4. according to the preparation side of bionical nacre MAX phase carbide ceramics based composites described in one of claims 1 to 3 Method, which comprises the steps of:
(1) MAX phase powder, organic gel, the dispersing agent of nanometer or micron sheet are added in solvent, are uniformly mixed and are formed Slurry, mixed method are ultrasonic wave dispersion, mechanical stirring or ball milling mixing;
(2) mixed slurry is fitted into mold, mold is put into the freezing equipment that can cause gradient low temperature and is oriented Solidification, cryogenic temperature and temperature gradient are determined by the physical chemistry coagulating property of compound slurry;
(3) after the completion of solidifying, the complete ceramic macromolecular idiosome of oriented growth is put into drying machine and is dried, drying parameter is by molten The physicochemical characteristics of agent determines;
(4) idiosome after the completion of drying is taken out and carries out carbonization technique, carbonization carries out in vacuum drying oven, carburizing temperature 400~600 DEG C, atmosphere 10-4Pa~10-2Pa vacuum environment, carbonization time 0.5~4 hour;
(5) pressure sintering is carried out to the idiosome that carbonization is completed, sintering temperature is by the granularity of material powder used and the kind of MAX phase Class determines.
5. the preparation method of bionical nacre MAX phase carbide ceramics based composites according to claim 4, feature Be, solvent be water or other with liquid form, reducing temperature can be in solid-state, and be able to achieve solid gaseous physical distillation transformation Solvent;Organic gel is polyvinyl alcohol, polyethylene glycol or carboxymethyl cellulose, and dispersing agent is sodium alklyarylsulfonate, alkyl phenol Polyvinylether or ammonium polyacrylate.
6. the preparation method of bionical nacre MAX phase carbide ceramics based composites according to claim 4, feature It is, by weight percentage, the MAX phase powder content in raw material is 30~60%, organic gel content is 2~10%, dispersion Agent content is 0.5~5%, solvent is surplus.
7. the preparation method of bionical nacre MAX phase carbide ceramics based composites according to claim 4, feature It is, pressure sintering is hot pressing sintering method, HIP sintering method or discharge plasma sintering method.
8. the preparation method of bionical nacre MAX phase carbide ceramics based composites according to claim 7, feature It is, hot pressing sintering method is that idiosome is directly packed into graphite jig, the hot pressed sintering in graphite jig, sintering temperature 500~ It 2000 DEG C, 1~200MPa of sintering pressure, soaking time 10~3600 minutes, 1~100 DEG C/min of heating rate, is sintered true It is carried out under empty or argon atmosphere.
9. the preparation method of bionical nacre MAX phase carbide ceramics based composites according to claim 7, feature It is, HIP sintering method is that directly idiosome is fitted into hot isostatic pressing jacket, is then evacuated and hermetically sealed jacket;It is wrapping HIP sintering in set, 500~2000 DEG C of sintering temperature, 1~800MPa of sintering pressure, soaking time 10~3600 minutes, 1~100 DEG C/min of heating rate, sintering carries out under vacuum or argon atmosphere.
10. the preparation method of bionical nacre MAX phase carbide ceramics based composites according to claim 7, special Sign is that discharge plasma sintering method is that directly idiosome is fitted into sintering mold, is applying big pulse electric current sintering, sintering It 300~1800 DEG C of temperature, 1~400MPa of sintering pressure, soaking time 5~600 minutes, 1~500 DEG C/min of heating rate, burns Knot carries out under vacuum or argon atmosphere.
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CN113182521A (en) * 2021-01-22 2021-07-30 河南科技大学 Ti2AlC/TiAl bionic micro-nano laminated composite material and preparation method thereof
CN113277851A (en) * 2021-06-29 2021-08-20 中国科学院金属研究所 Ceramic-metal bionic nano composite material and preparation method thereof
CN116239368A (en) * 2023-03-03 2023-06-09 中国科学技术大学 Preparation method of ceramic-metal composite material and ceramic-metal composite material

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