CN110357633A - A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic - Google Patents

A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic Download PDF

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CN110357633A
CN110357633A CN201910625528.0A CN201910625528A CN110357633A CN 110357633 A CN110357633 A CN 110357633A CN 201910625528 A CN201910625528 A CN 201910625528A CN 110357633 A CN110357633 A CN 110357633A
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aluminium
room temperature
carbon ceramic
graphene
titanium aluminium
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CN110357633B (en
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郝巍
倪娜
肖巍伟
赵晓峰
姜娟
范晓慧
郭芳威
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Shanghai Jiaotong University
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Abstract

The present invention relates to a kind of methods that room temperature quickly prepares titanium aluminium-carbon ceramic, and graphene oxide is dissolved in deionized water, and L-AA is added, controlled at 80-120 DEG C after stirring, reduction reaction sufficiently occurs, forms the graphene hydrogel of homogeneous texture, drying and dehydrating obtains graphene aerogel；Graphene aerogel, titanium valve, aluminium powder are uniformly mixed；Obtained mixed powder is pressed into green body, using platinized platinum as electrode, graphite column carries out flash burning sintering processes as pressurization contact, obtains fine and close and uniform titanium aluminium-carbon ceramic.Compared with prior art, the present invention is high using graphene auxiliary flash burning technology sintering preparation consistency, the titanium aluminium-carbon ceramic of purity is high, even grain size, and preparation process is simple, high-efficient and can complete at room temperature.

Description

A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic
Technical field
The present invention relates to ceramic preparation, a kind of method for quickly preparing titanium aluminium-carbon ceramic more particularly, to room temperature.
Background technique
Mn+1AXnMiddle M is transition element, such as V, Ti, and Ta etc., A are mainly III or IV race's element, such as Si, Al, Ga, Ge Deng X is C or N, n=1,2,3,4,5, they can be briefly referred to as 211 phase (Ti2AlC,Cr2AlC, Ta2AlC etc.), 312 phases (Ti3AlC2, Ti3SiC2), 413 phases and 523 phases.Mn+1AXn compound has similar hexagonal crystallographic texture, and space structure is P63/mmc.These compounds are thermodynamically stable lamellar compounds, have a wide range of applications field.For example, Ti3AlC2Crystalline substance Born of the same parents' parameter is a=b=0.30753nm, and c=1.8578nm, theoretical density is 4.25g/cm3.Ti (1) and Ti (2) is respectively 2a and 2f are occupied, Al atom is located at the position 2b, and C atom is in the position 2b (z=0.5701).Ti3AlC2Design feature is interpretable Are as follows: Al atom hierarchal arrangement has separated closelypacked Ti6C is octahedra, and the two is in periodical heap in the direction perpendicular to a axis Pile arrangement, octahedral center are C atoms, each structure cell is containing there are two Ti3AlC2.Titanium aluminium carbon (Ti3AlC2, Ti2AlC etc.) in Containing three kinds of ionic bond, covalent bond and metallic bond bonding patterns, not only there is metallicity here it is it but also there is the original of ceramic performance Cause.Ti-C key therein is covalent bond, and binding force is stronger, this makes titanium aluminium carbon elasticity modulus with higher (~300 GPa) With intensity (~760MPa).But inside Ti-Al key and Al atomic layer combined with metallic bond, it is this to tie between layers The feature of conjunction is similar with the Van der Waals force combination of graphite layers, this results in titanium aluminium carbon to have the spy of layer structure self-lubricating Property.Meanwhile titanium aluminium carbon has excellent high-temperature oxidation resistance, can form Al at 1200 DEG C or less2O3And TiO2Oxidation Film will form Al at a higher temperature2TiO5.The thermal expansion coefficient of titanium aluminium carbon is~9.0 × 10-6/ DEG C, with generation aluminium oxide Film (Al2O3, 9.3 × 10-6/ DEG C) similar thermal expansion coefficient, the binding force of oxide layer can be improved, further to matrix material Material carries out oxidation protection.And titanium aluminium carbon allows to restore discomposition damage because it is with special bonding performance, thus Also there is preferable tolerance to radiation injury.It may be applied to the following nuclear industry cladding nuclear fuels material.Therefore, titanium aluminium carbon Preparation and synthesis become one of the hot spot of recent domestic research.It is proposed it is a kind of simple, efficiently synthetic method to it not Carry out high-temperature field application to have great importance.
Up to the present, there are many kinds of the methods of the titanium aluminium-carbon ceramic of preparation, such as carburizing reagent method [N.C. Ghosh, S.P.Harimkar,Consolidation and synthesis of MAX phases by Spark Plasma Sintering(SPS):a review,Advances in science and technology of Mn+1AXn phases, Woodhead Publishing Limited, Oklahoma State University, USA, 2012.], hot pressure reaction sintering Method [Jae-Ho Han, Sung-Sic Hwang, Dongyun Lee, Sang-Whan Park, Synthesis and mechanical properties of Ti3AlC2by hot pressing TiCx/Al powder mixture,Journal Of the European Ceramic Society 28 (2008) 979-988.], discharge plasma sintering method [Ludi Xu, Degui Zhu,Yunlong Liu,Tohru S.Suzuki,Byung-nam Kim, Yoshio Sakka,Salvatore Grassoa,,Chunfeng Hu,Effect of texture on oxidation resistance of Ti3AlC2, Journal of the European Ceramic Society 38 (2018) 3417-3423.], mechanical alloying method [Bilge Yaman Islak,Erhan Ayas.Evaluation of properties of spark plasma sintered Ti3SiC2and Ti3SiC2/SiC composites.Ceramics International 45(2019) 12297-12306.] and self-propagating high-temperature reaction method [Maryam Akhlaghi, Seyed Ali Tayebifard, Esmaeil Salahi,Mehdi Shahedi Asl,Gert Schmidt.Self-propagating high- temperature synthesis of Ti3AlC2MAX phase from mechanically-activated Ti/Al/ Graphite powder mixture, Ceramics International 44 (2018) 9671-9678.] above method is equal It needs to carry out under the high temperature conditions, generally passes through two-step method using carbothermic method and prepare Ti3AlC2Ceramics will first pass through carbon heat Ceramic powder is prepared under reduction method hot conditions, and final ceramics, such long period, technique are then prepared by sintering Complexity can not regulate and control ceramic crystalline grain size and microstructure by control powder granule size.Hot pressing sintering method needs Ceramics are sintered under the conditions of higher temperature, it is easy to lead to ceramic crystalline grain abnormal growth, influence the performance of later period ceramics；And it puts Although electro-plasma sintering process can be with Fast Sintering ceramics, still temperature is higher, the high requirements on the equipment；It is mechanical simultaneously Alloying prepare titanium aluminium-carbon ceramic be also required to later period pyroreaction sintering can just obtain final target product；Self-propagating high-temperature The titanium aluminium-carbon ceramic of reaction method preparation is also required to carry out synthetic reaction, the composition of material under own material system offer higher temperature It is difficult to control with grain size, and is difficult so that ceramic sintered compact, simultaneously because localized heat inside material system The presence of stress leads to the defects of there are crackles inside ceramics, in this way will be unfavorable to ceramic later period performance.
Summary of the invention
The object of the invention is in order to overcome above-mentioned titanium aluminium-carbon ceramic high―temperature nuclei and sintering the high requirements on the equipment, The uncontrollable prior art disadvantage of complex process and a kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic is provided.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
Graphene oxide is dissolved in deionized water, L-AA is added, controlled at 80-120 DEG C after stirring, Reduction reaction sufficiently occurs, forms the graphene hydrogel of homogeneous texture；
By graphene hydrogel drying and dehydrating, how empty pine and the biggish graphene aerogel of specific surface area are obtained；
Graphene aerogel, titanium valve, aluminium powder are uniformly mixed；
Obtained mixed powder is pressed into green body, using platinized platinum as electrode, graphite column carries out flash burning as pressurization contact Sintering processes obtain fine and close and uniform titanium aluminium-carbon ceramic.
Further, it is 50~300V/cm, current density 80-500mA/ that electric field strength is controlled when flash burning sintering processes mm2, it is 10-50MPa that sintering, which applies pressure, and vacuum degree control is in 1-15Pa.
More further, when flash burning sintering processes, control electric field strength is 80~200V/cm, current density 80- 180mA/mm2, it is 20-40MPa that sintering, which applies pressure, and vacuum degree control is in 1-6Pa.
Technical parameter involved in the application, for example, the preparation process of graphene aerogel, powder granule size, proportion, Electric field strength, current density, sintering application pressure, vacuum degree that milling parameters and flash burning technology use when being sintered etc. are all It is by many experiments and based on the result summarized after materials chemistry thermodynamics and kinetic reaction mechanism.First in flash burning mistake Cheng Zhong, there are more physical processes such as electric field, thermal field and its coupling.Therefore, sintering mechanism is also likely to be based on these objects The comprehensive function of reason process.Only under above-mentioned technical parameter range, the preparation process of graphene aerogel, powder granule ruler Flash carbonization reaction-sintered prepares densification during flash burning could occur under conditions of very little, proportion, ball milling and flash burning technique Titanium aluminium-carbon ceramic.Conversely, graphene aerogel preparation technology parameter, particle size and proportion are not above-mentioned parameter, flash burning electricity Field intensity is excessive, and current density is excessive, and sintering application pressure is excessive, and ceramic systems energy is higher, and flash burning acutely makes carbonization not Occur completely, while will lead to abnormal grain growth, leads to ceramic structure and degradation；In addition, vacuum degree is excessively high, although not It can cause material oxidation, but be not easy to ceramic material and generate Joule heat under the function of current.Similarly, flash burning electric field strength is too Small, current density is too small, applies that pressure is too small to be will lead to inside ceramics and grain boundaries energy is too low, and electric current is too low cannot to cause sudden strain of a muscle Burning process, and then diffusion-sintering reaction densification cannot be induced to enough energy are provided inside crystal grain and crystal boundary, that is, react Energy needed for object and interface Joule heat are not enough to provide sintering causes ceramic material inside carburizing reagent incomplete, and defect is more And consistency is lower, grain boundaries second are mutually complex, in turn result in ceramic material structure and degradation；In addition, vacuum degree It is lower, under high energy and joule thermal drivers, material internal material and interface oxygen content is higher easily causes oxidation, in this way Carburizing reagent sintering densification inside ceramic material is prevented, target titanium aluminum-carbon ceramic material also just can not be normally obtained.
Further, the solid content in graphene oxide solution is 3-10g/L.
Further, the concentration of L-AA is 0.5-5g/L in graphene oxide solution.
Further, condition drying and dehydrating 4-12h of the graphene hydrogel at 50-80 DEG C.
Further, the partial size of the titanium valve is 1-10 μm, and the partial size of the aluminium powder is 1-10 μm.
Further, the graphene aerogel, titanium valve, aluminium powder molar ratio be (1~10): (1~20): (1~ 10)。
Further, ball milling is carried out using planetary ball mill, so that graphene aerogel, titanium valve and aluminium powder uniformly mix It closes.
Further, the mass ratio of graphene aerogel in ball mill, titanium valve, the mixed powder of aluminium powder and ballstone is 1: (8 ~20), drum's speed of rotation turns for 200-500, Ball-milling Time 6-24h.
Titanium aluminium-carbon ceramic is prepared by using redox graphene auxiliary flash burning technology sintering, and can be with flexible modulation It forms with microstructure the microstructure and properties for optimizing and improving titanium aluminium-carbon ceramic.Firstly, using the stone prepared Black alkene aeroge is as carbon source, using aluminium powder and titanium valve as silicon source and titanium source, by high-energy ball milling admixture activation powder, so Cold isostatic compaction preform blank is used afterwards；Then in flash burning sintering process, it is anti-that carbonization occurs for graphene and aluminium powder and titanium valve It answers, while applying pressure Fast Sintering under room temperature electric field action and densifying the titanium aluminium-carbon ceramic to be formed.What sintering was prepared Titanium aluminium-carbon ceramic is fine and close and purity is high, crystallite dimension are smaller and controllable, and tradition is avoided to prepare sintered titanium aluminium-carbon ceramic method high temperature The problems such as grain growth and microstructure of the uncontrollable ceramics of sintering, and complex process, the high requirements on the equipment.
Flash burning technology is that one kind can make electrolyte ceramics sintering densification in a very short period of time under lower temperature conditions A kind of method.First by electrolyte ceramics powder dry pressing, it is subsequently attached in circuit, electrolyte sample is applied Add a fixed initial voltage, and electrolyte ceramics green body is placed in heating or room temperature in furnace.When furnace temperature reaches one When fixed value, electric current moment is steeply risen in circuit.In this way, electrolyte ceramics can be within several seconds time, densified sintering product.Cause To occur the starting point of the electric current steeply risen and sintering in sintering process, have the advantage that (1) sintering temperature is low； (2) sintering rate is fast；(3) the Isothermal sinter time is short；It (4) being capable of fine and close some electrolysis that densification is difficult in conventional high-temperature sintering Matter, such as BZY；(5) addition sintering aid is not needed；(6) device is easy.During flash burning, there are electric field, thermal field and its couplings More physical processes such as effect.Therefore, sintering mechanism is also likely to be the comprehensive function based on these physical processes.Mainstream at present Academic viewpoint mainly includes that joule heating effect is theoretical, the promotion densification that is rapidly heated is theoretical, grain contact point local heat effect reason By with defect intreractive theory etc..Including ion conductor (a variety of cubes of such as 3YSZ and 8YSZ, tetragonal zircite phase), insulator (Al2O3), semiconductor (BaTiO3, ZnO and SiC etc.) and eka-gold attribute conductivity ceramics (Co2MnO4And ZrB2) etc..8YSZ can be Under the electric field action of 120V/cm, at 750 DEG C, at a temperature of conventional sintered material, densification is realized.
The present invention is high using graphene auxiliary flash burning technology sintering preparation consistency, the titanium of purity is high, even grain size So on the one hand aluminium-carbon ceramic using redox graphene as carbon source, realizes generation flash burning fabricated in situ at room temperature Prepare titanium aluminium carbon MAX phase；On the other hand, under electric field action, while certain pressure is provided and allows ceramics in room temperature item Sintering densification under part, this will provide a kind of method for being synthetically prepared ceramics under room temperature, can flexible Effective Regulation ceramics Composition, structure and performance.
Compared with prior art, the invention has the following advantages that
(1) using redox graphene aeroge as carbon source, while flash burning technology being assisted to prepare burning under room temperature Form a point controllable titanium aluminium carbon MAX phase ceramics.
(2) flash burning technology is used simultaneously, and one-step method is sintered by reaction in-situ and prepares titanium aluminium carbon MAX phase ceramics, it is prepared Ceramic dense and crystallinity is good, even grain size distribution, structure-controllable.
(3) this method prepares that titanium aluminium carbon MAX phase ceramics preparation temperature is low, simple process is controllable, reaction-sintered is high-efficient, And it is low for equipment requirements.
(4) the titanium aluminium carbon MAX phase ceramics structure of this method preparation is uniformly and consistency can achieve 92%-100%.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection scope.
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 3-10g/L, and ultrasonic vibration 30-100min, then magnetic agitation 1-12h are used, so that graphene oxide is completely dissolved in Uniform solution is formed in ionized water, states L-AA is added in solution then up, controlling its concentration is 0.5-5g/L, And magnetic agitation 1-12h is then allowed to stand in 80-120 DEG C of baking oven, makes it that reduction reaction sufficiently occur, and forms uniformly knot The graphene hydrogel of structure；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 4- in 50-80 DEG C of electric drying oven with forced convection 12h obtains how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (1-10 μm) and micron level aluminium are taken Powder (Al) (1-10 μm), according to molar ratio are as follows: graphene aerogel: (1~10) Ti: Al=: (1~20): the ratio of (1~10) Example mixing, and ball milling is carried out using planetary ball mill, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix It closes, the mass ratio for controlling mixed powder and ballstone is 1: (8~20), drum's speed of rotation turn for 200-500, obtain after ball milling 6-24h Obtain mixed uniformly powder.
(4) by the mixed powder in step 3 use isostatic cool pressing pre-molding cylinder green body (diameter for 5-30 mm, height For 1-10mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls sample as pressurization contact Electric field strength is 50~300V/cm, and current density is 80-500 mA/mm2, it is 10-50MPa, vacuum degree control that sintering, which applies pressure, In 1-15Pa fine and close and uniform titanium aluminium-carbon ceramic can be obtained, consistency is up to 92%-100% in system.
More detailed case study on implementation below, by following case study on implementation further illustrate technical solution of the present invention with And the technical effect that can be obtained.
In specific embodiment of the present invention,
Graphene oxide powder is produced by Shanghai carbon source Hui Gu new material Science and Technology Ltd., diameter: 0.5-10 μ M, the number of plies: 1-5 layers, single layer rate > 99%, purity >=99.9%.
L-AA is produced by Shanghai Mike's woods biochemical technology Co., Ltd, purity >=99.0%.
Titanium valve is produced by Shanghai ultra micro nanosecond science and technology Co., Ltd, purity >=99.0%.
Aluminium powder is produced by Shanghai ultra micro nanosecond science and technology Co., Ltd, purity >=99.0%.
The power of supersonic generator is 500~1500W, and it is by city of Kunshan's Ultrasound Instrument that the concussion time, which is 10~100min, The production of device Co., Ltd.
Ball-milling technology is the model QM-3SP4 type produced by Nanjing University using planetary ball mill.
Isostatic cool pressing equipment is the model YLJ-CIP-20B produced by Hefei ,Anhui Ke Jing Materials Technology Ltd. Type split type cold isostatic press manually.
AC constant voltage constant-current supply is the model ALP-1000V 1A produced by Jiangsu Yangzhou Ding Hua Electronics Co., Ltd. Type power supply.
Flash burning equipment is vacuum high-temperature tube furnace, is the VBF- produced by Hefei ,Anhui Materials Technology Ltd. 1200X-HB type tube furnace.
Drying is the DHG- produced by Shanghai Yiheng Scientific Instruments Co., Ltd using electric drying oven with forced convection 9075A type.
Embodiment 1:
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 3g/L, and ultrasonic vibration 40min, then magnetic agitation 3h are used, so that graphene oxide is completely dissolved in shape in deionized water It at uniform solution, states L-AA is added in solution then up, control its concentration as 1g/L, and magnetic agitation 3h, It is then allowed to stand in 80 DEG C of baking oven, makes it that reduction reaction sufficiently occur, form the graphene hydrogel of homogeneous texture；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 4h in 50 DEG C of electric drying oven with forced convection, obtained To how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (1 μm) and micron level aluminium powder are taken (Al) (1 μm), according to molar ratio are as follows: graphene aerogel: Ti: Al=2: 3: 1 ratio mixing, and use planetary ball Grinding machine carries out ball milling, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix, controls the matter of mixed powder and ballstone For amount than being 1: 10, drum's speed of rotation is 300 turns, obtains mixed uniformly powder after ball milling 8h.
(4) mixed powder in step 3 is used into isostatic cool pressing pre-molding cylinder green body (diameter is highly for 10 mm 3mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls the electric field of sample as pressurization contact Intensity is 120V/cm, current density 200mA/mm2, it is 30MPa that sintering, which applies pressure, and vacuum degree control can be obtained in 2Pa To fine and close and uniform titanium aluminium-carbon ceramic, consistency is up to 95%.
Embodiment 2:
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 5g/L, and ultrasonic vibration 60min, then magnetic agitation 5h are used, so that graphene oxide is completely dissolved in shape in deionized water It at uniform solution, states L-AA is added in solution then up, control its concentration as 2g/L, and magnetic agitation 8h, It is then allowed to stand in 90 DEG C of baking oven, makes it that reduction reaction sufficiently occur, form the graphene hydrogel of homogeneous texture；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 8h in 60 DEG C of electric drying oven with forced convection, obtained To how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (2 μm) and micron level aluminium powder are taken (Al) (2 μm), according to molar ratio are as follows: graphene aerogel: Ti: Al=1: 2: 1 ratio mixing, and use planetary ball Grinding machine carries out ball milling, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix, controls the matter of mixed powder and ballstone For amount than being 1: 12, drum's speed of rotation is 400 turns, obtains mixed uniformly powder after ball milling 12h.
(4) mixed powder in step 3 is used into isostatic cool pressing pre-molding cylinder green body (diameter is highly for 20 mm 5mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls the electric field of sample as pressurization contact Intensity is 240V/cm, current density 400mA/mm2, it is 40MPa that sintering, which applies pressure, and vacuum degree control can be obtained in 5Pa To fine and close and uniform titanium aluminium-carbon ceramic, consistency is up to 97%.
Embodiment 3:
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 3g/L, and ultrasonic vibration 100min, then magnetic agitation 10h are used, so that graphene oxide is completely dissolved in deionized water Uniform solution is formed, states L-AA is added in solution then up, controls its concentration as 0.5g/L, and magnetic agitation 10h is then allowed to stand in 80 DEG C of baking oven, makes it that reduction reaction sufficiently occur, and forms the graphene hydrogel of homogeneous texture；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 12h in 50 DEG C of electric drying oven with forced convection, Obtain how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (1 μm) and micron level aluminium powder are taken (Al) (1 μm), according to molar ratio are as follows: graphene aerogel: Ti: Al=1: 1: 1 ratio mixing, and use planetary ball Grinding machine carries out ball milling, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix, controls the matter of mixed powder and ballstone Amount is than being 1: 8, and drum's speed of rotation is 200 turns, and ball milling obtains mixed uniformly powder afterwards for 24 hours.
(4) mixed powder in step 3 is used into isostatic cool pressing pre-molding cylinder green body (diameter is highly for 30 mm 8mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls the electric field of sample as pressurization contact Intensity is 50V/cm, current density 500mA/mm2, it is 40MPa that sintering, which applies pressure, and vacuum degree control can be obtained in 15Pa To fine and close and uniform titanium aluminium-carbon ceramic, consistency is up to 95%.
Embodiment 4:
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 10g/L, and ultrasonic vibration 60min, then magnetic agitation 5h are used, so that graphene oxide is completely dissolved in shape in deionized water It at uniform solution, states L-AA is added in solution then up, control its concentration as 5g/L, and magnetic agitation 8h, It is then allowed to stand in 100 DEG C of baking oven, makes it that reduction reaction sufficiently occur, form the graphene hydrogel of homogeneous texture；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 4h in 80 DEG C of electric drying oven with forced convection, obtained To how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (5 μm) and micron level aluminium powder are taken (Al) (8 μm), according to molar ratio are as follows: graphene aerogel: Ti: Al=5: 20: 3 ratio mixing, and use planetary ball Grinding machine carries out ball milling, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix, controls the matter of mixed powder and ballstone For amount than being 1: 20, drum's speed of rotation is 300 turns, obtains mixed uniformly powder after ball milling 18h.
(4) mixed powder in step 3 is used into isostatic cool pressing pre-molding cylinder green body (diameter is highly for 20 mm 5mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls the electric field of sample as pressurization contact Intensity is 200V/cm, current density 180mA/mm2, it is 20MPa that sintering, which applies pressure, and vacuum degree control can be obtained in 1Pa To fine and close and uniform titanium aluminium-carbon ceramic, consistency is up to 96%.
Embodiment 5:
A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, comprising:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 5g/L, and ultrasonic vibration 60min, then magnetic agitation 5h are used, so that graphene oxide is completely dissolved in shape in deionized water It at uniform solution, states L-AA is added in solution then up, control its concentration as 2g/L, and magnetic agitation 8h, It is then allowed to stand in 90 DEG C of baking oven, makes it that reduction reaction sufficiently occur, form the graphene hydrogel of homogeneous texture；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 8h in 60 DEG C of electric drying oven with forced convection, obtained To how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (2 μm) and micron level aluminium powder are taken (Al) (2 μm), according to molar ratio are as follows: graphene aerogel: Ti: Al=1: 2: 1 ratio mixing, and use planetary ball Grinding machine carries out ball milling, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix, controls the matter of mixed powder and ballstone For amount than being 1: 12, drum's speed of rotation is 400 turns, obtains mixed uniformly powder after ball milling 12h.
(4) mixed powder in step 3 is used into isostatic cool pressing pre-molding cylinder green body (diameter is highly for 20 mm 5mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls the electric field of sample as pressurization contact Intensity is 240V/cm, current density 400mA/mm2, it is 40MPa that sintering, which applies pressure, and vacuum degree control can be obtained in 5Pa To fine and close and uniform titanium aluminium-carbon ceramic, consistency is up to 97%.
Embodiment 6:
(1) graphene oxide (diameter: 0.5-10 μm, the number of plies: 1-5 layers) is taken to be dissolved in deionized water, configuration solid content is 6g/L, and ultrasonic vibration 60min, then magnetic agitation 5h are used, so that graphene oxide is completely dissolved in shape in deionized water It at uniform solution, states L-AA is added in solution then up, control its concentration as 1g/L, and magnetic agitation 8h, It is then allowed to stand in 80 DEG C of baking oven, makes it that reduction reaction sufficiently occur, form the graphene hydrogel of homogeneous texture；
(2) graphene hydrogel obtained in step 1 is put into drying and dehydrating 8h in 60 DEG C of electric drying oven with forced convection, obtained To how empty pine and the biggish graphene aerogel of specific surface area；
(3) graphene aerogel obtained in step 2, micron level titanium valve (Ti) (10 μm) and micron level aluminium powder are taken (Al) (10 μm), according to molar ratio are as follows: graphene aerogel: Ti: Al=10: 1: 10 ratio mixing, and using planetary Ball mill carries out ball milling, so that above-mentioned graphene aerogel, titanium valve and aluminium powder uniformly mix, controls mixed powder and ballstone Mass ratio is 1: 10, and drum's speed of rotation is 400 turns, obtains mixed uniformly powder after ball milling 12h.
(4) mixed powder in step 3 is used into isostatic cool pressing pre-molding cylinder green body (diameter is highly for 20 mm 5mm), then using platinized platinum as electrode, graphite column carries out flash burning sintering process, controls the electric field of sample as pressurization contact Intensity is 300V/cm, current density 80mA/mm2, it is 10MPa that sintering, which applies pressure, and vacuum degree control can be obtained in 5Pa Fine and close and uniform titanium aluminium-carbon ceramic, consistency is up to 98%.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example. Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close Suitable mode combines.
The above-mentioned description to embodiment is for ease of ordinary skill in the art to understand and use the invention.It is ripe The personnel for knowing art technology obviously easily can make various modifications to these embodiments, and general original described herein It ought to use in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, this field Technical staff's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be in guarantors of the invention Within the scope of shield.

Claims (10)

1. a kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic, which is characterized in that this method comprises:
Graphene oxide is dissolved in deionized water, L-AA is added, controlled at 80-120 DEG C after stirring, is sufficiently sent out Raw reduction reaction, forms the graphene hydrogel of homogeneous texture；
By graphene hydrogel drying and dehydrating, how empty pine and the biggish graphene aerogel of specific surface area are obtained；
Graphene aerogel, titanium valve, aluminium powder are uniformly mixed；
Obtained mixed powder is pressed into green body, using platinized platinum as electrode, graphite column carries out flash burning sintering as pressurization contact Processing obtains fine and close and uniform titanium aluminium-carbon ceramic.
2. the method that a kind of room temperature according to claim 1 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that flash burning sintering It is 50~300V/cm, current density 80-500mA/mm that electric field strength is controlled when processing2, it is 10- that sintering, which applies pressure, 50MPa, vacuum degree control is in 1-15Pa.
3. the method that a kind of room temperature according to claim 1 or 2 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that flash burning It is 80~200V/cm, current density 80-180mA/mm that electric field strength is controlled when sintering processes2, it is 20- that sintering, which applies pressure, 40MPa, vacuum degree control is in 1-6Pa.
4. the method that a kind of room temperature according to claim 1 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that graphite oxide Solid content in alkene solution is 3-10g/L.
5. the method that a kind of room temperature according to claim 1 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that graphite oxide The concentration of L-AA is 0.5-5g/L in alkene solution.
6. the method that a kind of room temperature according to claim 1 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that the graphite Condition drying and dehydrating 4-12h of the alkene hydrogel at 50-80 DEG C.
7. the method that a kind of room temperature according to claim 1 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that the titanium valve Partial size be 1-10 μm, the partial size of the aluminium powder is 1-10 μm.
8. the method that a kind of room temperature according to claim 1 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that the graphite Alkene aeroge, titanium valve, aluminium powder molar ratio be (1~10): (1~20): (1~10).
9. a kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic described according to claim 1 or 7 or 8, which is characterized in that adopt Ball milling is carried out with planetary ball mill, so that graphene aerogel, titanium valve and aluminium powder uniformly mix.
10. the method that a kind of room temperature according to claim 9 quickly prepares titanium aluminium-carbon ceramic, which is characterized in that ball mill Middle graphene aerogel, titanium valve, the mixed powder of aluminium powder and ballstone mass ratio be 1: (8~20), drum's speed of rotation 200- 500 turns, Ball-milling Time 6-24h.
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