CN103992112B

CN103992112B - One kind synthesis Ti2The method of SC ceramics

Info

Publication number: CN103992112B
Application number: CN201410209209.9A
Authority: CN
Inventors: 关春龙; 李文凤; 任宁; 田野; 卢新坡; 王顺; 秦越; 孙纳纳; 赵志伟
Original assignee: Henan University of Technology
Current assignee: Henan University of Technology
Priority date: 2014-05-19
Filing date: 2014-05-19
Publication date: 2018-04-27
Anticipated expiration: 2034-05-19
Also published as: CN103992112A

Abstract

A kind of microwave synthesizes Ti₂The preparation method of SC ceramics, it is characterised in that：The method step is as follows：According to 2:(1.0~1.3):1:The molar ratio of (0.1 ~ 0.3) takes titanium valve, sulphur powder, graphite powder and aluminium powder, and tabletting is carried out after mixing, and by the pellet material being pressed into, microwave heating synthesizes high-purity Ti under the protection for the inert gas not chemically reacted with raw material and reactant afterwards₂SC ceramics.By this method, Ti can quickly be prepared₂SC ceramic powders, reaction temperature and reaction time are greatly reduced, with conventional Ti₂SC ceramic preparations improve decades of times compared to efficiency, while obtain preferable single-phase sample.

Description

One kind synthesis Ti2The method of SC ceramics

Technical field

The present invention provides a kind of preparation method of microwave synthesis inorganic ceramic material, in particular to a kind of microwave Synthesize Ti₂SC ceramic materials, belong to non-oxide ceramics preparation field.

Background technology

Ti₂SC is M_n+1AX_n（n=1,2,3）A member in ternary layered compound in " 211 " phase family, it belongs to hexagonal crystal System, it, which has, is similar to metal excellent high heat conductance and high conductivity, and has preferable corrosion resistance.At the same time Ti₂SC also has high intensity possessed by ceramics, and good high-temperature oxidation resistance concurrently.Therefore, Ti₂SC as high-temperature oxidation resistant and Corrosion-resistant ceramic component and protective coating have wide in fields such as aerospace, nuclear industry, communications and transportation, petrochemical industry and metallurgy Wealthy application prospect.The Ti in whole MAX phases family₂SC has the feature of lattice constant c minimums, this allows for Ti₂SC has very More special performance, such as highest Vickers hardness (8GPa) and highest room temperature thermal conductivity（60W/mK）Deng.These cause more Carry out the concern of more investigation of materials persons.

But for the research compared to more other MAX phases, Ti₂The research of SC is very few, is particularly utilizing simple substance element system It is even more to be rarely reported in terms of standby correlative study, this is because elemental sulfur is easy to distillation volatilization in heating process.At present, Ti₂SC block materials are mostly by hot pressed sintering Ti₂The method acquisition of SC powders [J.Am.Ceram, 2007,90: 3953~3958; J.Appl.Phys, 2008, 104: 033502; Scripta Mater, 2011, 65:573~ 576].Recently, Wen Bin Zhu et al. [J.Alloys Comp, 2013,566:191~195] with metallic titanium powder, two sulphur It is raw material to change titanium valve and carbon dust, uses traditional hot-pressing sintering method to be synthesized when 1600 °C of pressure are small for 30MPa insulations 2 Ti₂SC block materials.2013, Chinese invention patent（CN103253667A）Report one kind and utilize high temperature by raw material of simple substance High pressure method is to synthesize Ti under the conditions of 1600 °C of pressure are 2~6GPa in temperature₂SC materials.It can be seen from the above that synthesis at present Ti₂The temperature of SC materials is all in nearly 1600 °C of high temperature, and generated time is very long wants several hours.In consideration of it, have to look for The new process that energy consumption is low and production efficiency is high substitutes existing preparation Ti₂The technique of SC ceramic materials.The present invention uses microwave The method of heating can be in low temperature and the very short time just prepares the very high Ti of purity₂SC ceramic materials.

The content of the invention

The object of the invention is exactly to provide a kind of microwave synthesis for the shortcoming in the presence of the above-mentioned prior art Ti₂The preparation method of SC ceramic powders.The present invention is heated by microwave and is passed through inert atmosphere, and firing rate is fast, synthesis temperature Low, the reaction time is short, and synthetic reaction generally need to only heat several minutes.

The purpose of the present invention can be realized by following technique measures：

The microwave synthesis Ti of the present invention₂The preparation method step of SC ceramic materials is as follows：According to 2:(1.0~1.3):1: The molar ratio of (0.1 ~ 0.3) takes titanium valve, sulphur powder, graphite powder and aluminium powder, and tabletting is carried out after mixing, the sheet body material that will be pressed into afterwards Expect that microwave heating synthesizes high-purity Ti under the protection for the inert gas not chemically reacted with raw material and reaction product₂SC makes pottery Porcelain.

Heretofore described microwave heating time is 5 ~ 20 minutes, and heating-up temperature is 800 ~ 1100 °C；The inertia Gas is argon gas.

Evaluation method：Sample is characterized with XRD.

With existing preparation Ti₂The method of SC materials is compared, and beneficial effects of the present invention are as follows：

（1）The present invention is easy to operate, and technique is simple.The present invention selects commercially available titanium valve, sulphur powder, graphite powder and aluminium powder, former Material is cheap and easy to get；In addition, compared with hot pressing and sintering technique compare, the present invention using oneself assembling microwave heat dress Put, it is not high to equipment requirement；Without pressurization during operation, easy to operate, technique is simple.

（2）Ti in prepared sample₂SC phase contents are higher, tiny close to single-phase and crystal grain.

（3）Preparation time is short, and cost is low.The present invention make full use of microwave fast heating can suppress S powder volatilization and Under the double action of the reaction heat of exothermic reaction between Ti, S and C, Fast back-projection algorithm Ti in a short time₂SC materials.With tradition Preparation method（Such as hot-pressing sintering technique）Compare, efficiency improves decades of times, has the characteristics that energy saving, efficient.Heated using microwave Method prepares Ti₂SC materials, substantially reduce the reaction time and reduce reaction temperature, in 800 ~ 1100 °C and 5 ~ 20min conditions Under can prepare Ti₂SC, greatlys save the energy, improves production efficiency.

Brief description of the drawings

Attached drawing 1 is Ti₂SC diffraction patterns.

Embodiment：

Embodiment 1：

With titanium valve, sulphur powder, graphite powder and aluminium powder are raw material, according to Ti:S:C:Al=2: (1.0~1.3):1: (0.1~ 0.3) molar ratio is weighed, and powder is uniformly mixed, and is pressed into disk, and then disk is put in microwave heating equipment cavity and is added Heat, reacts under the protection of argon gas（60 ~ 100ml/min of argon flow amount）Carry out, sintering time is 8 minutes, and sintering temperature is 900 °C, you can Ti is made₂SC materials.

Embodiment 2：

With titanium valve, sulphur powder and graphite powder are raw material, according to Ti:S:C:Al =2: (1.0~1.3):1:(0.1 ~ 0.3) Molar ratio is weighed, and powder is uniformly mixed, and is pressed into disk, and then disk is put in microwave heating equipment and is heated, is reacted Under the protection of argon gas（60 ~ 100ml/min of argon flow amount）Carry out, sintering temperature is 1000 °C, and sintering time is 10 minutes, you can Ti is made₂SC materials.

Embodiment 3：

With titanium valve, sulphur powder and graphite powder are raw material, according to Ti:S:C:Al =2: (1.0~1.3):1:(0.1 ~ 0.3) Molar ratio is weighed, and powder is uniformly mixed, and is pressed into disk, and then disk is put in microwave heating equipment and is heated, is reacted Under the protection of argon gas（60 ~ 100ml/min of argon flow amount）Carry out, sintering power is that temperature is 1100 °C, and sintering time is 8 points Clock, you can Ti is made₂SC materials.

Claims

1. a kind of microwave synthesizes Ti₂The preparation method of SC ceramic materials, it is characterised in that：The method step is as follows：With titanium valve, Sulphur powder, graphite powder and aluminium powder are raw material, according to Ti:S:C:Al=2: (1.0~1.3):1:The molar ratio of (0.1 ~ 0.3) is weighed, Powder is uniformly mixed, is pressed into disk, then disk is put in microwave heating equipment cavity and is heated, reacts the guarantor in argon gas Shield is lower to be carried out, and argon flow amount is 60 ~ 100ml/min, and sintering time is 8 minutes, and sintering temperature is 900 °C, you can is made Ti₂SC materials.