CN106187112A - A kind of aluminium oxide titanium carbide base composite ceramic material and preparation method thereof - Google Patents

A kind of aluminium oxide titanium carbide base composite ceramic material and preparation method thereof Download PDF

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CN106187112A
CN106187112A CN201610518352.5A CN201610518352A CN106187112A CN 106187112 A CN106187112 A CN 106187112A CN 201610518352 A CN201610518352 A CN 201610518352A CN 106187112 A CN106187112 A CN 106187112A
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graphene
titanium carbide
ceramic material
composite ceramic
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李作丽
赵军
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Shandong University
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Abstract

The invention belongs to materials science field, relate to a kind of aluminium oxide titanium carbide base composite ceramic material and preparation method thereof.The present invention uses submicron alumina, submicron titanium carbide and Graphene to be raw material, aluminium oxide titanium carbide base composite ceramic material is prepared by batch mixing, ball milling, drying and screening, die-filling, vacuum heating-press sintering process, wherein the mass percent of Graphene is 0.2～0.3%, is evenly distributed in aluminium oxide carbonization Titanium base.Material particle size is evenly distributed, and its bending strength and fracture toughness all improve 10～20% than the material being not added with Graphene.This composite ceramic material is suitable for making the cutting tool that fracture toughness and bending strength require higher difficult-to-machine material.

Description

A kind of alumina-titanium carbide based composite ceramic material and preparation method thereof
Technical field
The invention belongs to materials science field, particularly to a kind of alumina-titanium carbide based composite ceramic material and Preparation method.
Background technology
Due to alumina-titanium carbide base ceramic cutting tool material have that fusing point is high, wearability is strong, thermochemistry the best, firmly Degree advantages of higher, is suitable for cutting difficult-to-machine material.But the intensity of alumina-titanium carbide base ceramic material and fracture toughness are relatively Low, the life-span of cutter is difficult to improve.The toughness of pottery is the key problem of ceramic material research field.Graphene has uniqueness Two-dimensional structure, is the hardest the thinnest a kind of material with carbon element in known materials, and its thickness is 0.34nm, and intensity reaches 130GPa, elastic Modulus is 1.0TPa, and thermal conductivity, up to 5000W/ (m.K), adds Graphene in ceramic matrix, and the mechanical property of its excellence can Play in the composite toughened and reinforced effect (Li Jianlin, Chen Binbin, Zhang Wen etc. pottery/Graphene block composite material Progress [J]. Journal of Inorganic Materials, 2014,29 (3): 225-236).Document (Hu Yangyang, Xu Chonghai, Xiao Guangchun, etc. oxygen Change preparation and the performance [J] of aluminum/graphene oxide composite ceramics. silicate journal, 2016 (3)) report a kind of hot pressed sintering Al2O3/ GS composite ceramic material, its by alumina modified and with Graphene parcel prepare Al2O3/ GS composite ceramics material Material, this material preparation process is complicated, and is limited by the feature of alumina substrate, and material bending strength is low.
Adding Graphene in alumina-titanium carbide base ceramic material can make ceramic material be internally formed weak faying face, Increase energy to failure thus toughened and reinforced to material.But the addition of Graphene and dispersion effect greatly affect material bending strength Raising with fracture toughness.Graphene is easily reunited, and its dispersion effect is affected by many factors, such as dispersant, adds Enter intensity and the time etc. of amount and ultrasonic disperse.Therefore, for alumina-titanium carbide material system, the graphite of optimum is chosen Alkene addition, uses rational dispersing technology, can be effectively improved the comprehensive mechanical property of this composite ceramic material.
Summary of the invention
It is an object of the invention to for above-mentioned the deficiencies in the prior art, it is provided that a kind of comprehensive mechanical property is good, production technology The alumina-titanium carbide based composite ceramic material of easy, applicable industrialized production and preparation method.
The present invention is achieved in the following ways:
A kind of aluminum oxide/titanium carbide based composite ceramic material, with alumina-titanium carbide as matrix, is characterized in that: oxidation Containing equally distributed Graphene in aluminum-titanium carbide matrix；The mass percent of Graphene is aluminum oxide-titanium carbide Titanium base 0.2～0.3%.Graphene has refined crystal grain, adds transgranular fracture；Material part grain boundaries is weak binding interface, contributes to Improve bending strength and the fracture toughness of material.This composite ceramic material is suitable for making fracture toughness and bending strength requirement The cutting tool of higher difficult-to-machine material.
The preparation method of above-mentioned alumina-titanium carbide based composite ceramic material, is characterized in that comprising the following steps:
(1) graphene dispersion
Polyvinylpyrrolidone (PVP) is joined in ethanol solution, stirring while adding is completely dissolved to PVP；Will Graphene is added slowly in PVP solution, stirs, and ultrasonic disperse forms graphene suspension；Graphene content is Al2O3The 0.2～0.3% of/TiC mixed-powder gross mass, PVP and Graphene mass ratio are 1:3～5；
(2) batch mixing
By volume percentage ratio 7:3 weighs Al2O3With TiC powder mixing, add Al2O3/ TiC mixed-powder gross mass 1% MgO be sintering aid, be subsequently adding the graphene suspension of preparation in dehydrated alcohol and step (1)；Stirring while adding, then surpass Sound dispersion forms the slurry of mix homogeneously；Mixed slurry is poured in ball milling bucket, add Al2O3Mill ball, dry powder and ball weight ratio For 1:5；Ball milling 60～72 hours on ball mill, vacuum dried, sieve, the material powder being uniformly mixed；
(3) hot pressed sintering
Material powder step (2) prepared loads in graphite jig, is sintered under vacuum conditions, sintering process For: when room temperature～1200 DEG C, heating rate is 40 DEG C/min, at 1200 DEG C, is incubated 5 minutes；When 1200 DEG C-1700 DEG C, Heating rate is 35 DEG C/min, and uniform pressurization makes pressure steadily rise to 30MPa；1700 DEG C, under the conditions of pressure 30MPa, insulation 10 minutes, then power-off naturally cooled to room temperature.
The preparation method of above-mentioned a kind of alumina-titanium carbide based composite ceramic material, is characterized in that Graphene in step (1) The ultrasonic disperse time is 2～3 hours, and polyvinylpyrrolidone (PVP) and Graphene mass ratio are 1:3～5；Step (2) is mixed Close before slurry grinds and need ultrasonic disperse 0.5～1 hour.
Material part grain boundaries of the present invention forms weak binding interface, and Graphene is evenly distributed, and material granule size is uniform.Power Test shows, add 0.2～0.3% Graphene after, the bending strength of aluminum oxide/titanium carbide based composite ceramic material and disconnected Split toughness to be greatly improved, be suitable for making the cutting tool that fracture toughness and bending strength require higher difficult-to-machine material.
Relative to prior art achievement, the present invention has the following advantages:
(1) Graphene is evenly distributed.Observe from fracture SEM images and find that Graphene is sheet-like morphology, be evenly distributed on oxygen Change on the interface of aluminum and titanium carbide.
(2) material part grain boundaries forms weak binding interface.Under external force, at weak interface, preferentially produce micro-crack, The energy of dissipation lead crack extension, hinders the extension of lead crack so that the bending strength of material and fracture toughness improve.
(3) bending strength and the fracture toughness of material strengthens.Relatively it is not added with the alumina-titanium carbide composite ceramic of Graphene Ceramic material, material bending strength and the fracture toughness of adding Graphene all improve 10～20%.
(4) material preparation process is easy, and controllability is strong, easily realizes bending strength and fracture toughness alumina-based ceramic material Preparation.
Detailed description of the invention
Three most preferred embodiments of the present invention are given below:
Embodiment 1
(1) aluminium oxide and the Graphene of titanium carbide mixed-powder gross mass 0.2% are weighed, by Graphene and PVP mass ratio 3:1 weighs PVP, both is successively added in 200ml dehydrated alcohol and stirs, ultrasonic disperse 2 hours；By submicron alpha-Al2O3 (0.5 μm), submicron TiC (0.5 μm) 7:3 by volume mix, and add aluminium oxide and titanium carbide mixed-powder mass fraction is Graphene suspension after the MgO of 1% and dispersion, adds Al by the ratio of grinding media to material of 5:12O3Mill ball, anhydrous by 200ml:60g Ethanol material, than adding dehydrated alcohol, ultrasonic disperse 0.5 hour, is then placed in ball milling bucket high speed ball milling 60 hours.
(2) composite mortar after ball milling is put into vacuum drying oven, dry under the conditions of vacuum is-0.8MPa and 120 DEG C Dry, cross 150 mesh sieves, obtain finely disseminated mixed-powder.
(3) mixed-powder step (2) prepared loads in graphite jig, puts into vacuum hotpressing stove sintering, during sintering, Vacuum remains at below 10Pa, and sintering process is: when room temperature～1200 DEG C, and heating rate is 40 DEG C/min, 1200 DEG C, it is incubated 5 minutes；When 1200 DEG C-1700 DEG C, heating rate is 35 DEG C/min, uses manual pressure mode, makes pressure Add to 30MPa power even；1700 DEG C, under the conditions of pressure 30MPa, be incubated 10 minutes, then power-off naturally cools to Room temperature.
The mechanical property of material is: bending strength 878～956MPa, and fracture toughness is 5.12～5.72MPa.m1/2。
Embodiment 2
(1) aluminium oxide and the Graphene of titanium carbide mixed-powder gross mass 0.3% are weighed, by Graphene and PVP mass ratio 3:1 weighs PVP, both is successively added in 200ml dehydrated alcohol and stirs, ultrasonic disperse 2 hours；By submicron alpha-Al2O3 (0.5 μm), submicron TiC (0.5 μm) 7:3 by volume mix, and add aluminium oxide and titanium carbide mixed-powder mass percent Be 1% MgO and dispersion after graphene suspension, by 5:1 ratio of grinding media to material add Al2O3Mill ball, by the nothing of 200ml:60g Water-ethanol material, than adding dehydrated alcohol, ultrasonic disperse 0.5 hour, is then placed in ball milling bucket high speed ball milling 60 hours.
(2) composite mortar after ball milling is put into vacuum drying oven, dry under the conditions of vacuum is-0.8MPa and 120 DEG C Dry, cross 150 mesh sieves, obtain finely disseminated mixed-powder.
(3) mixed-powder step (2) prepared loads in graphite jig, puts into vacuum hotpressing stove sintering, during sintering, Vacuum remains at below 10Pa, and sintering process is: when room temperature～1200 DEG C, and heating rate is 40 DEG C/min, 1200 DEG C, it is incubated 5 minutes；When 1200 DEG C-1700 DEG C, heating rate is 35 DEG C/min, uses manual pressure mode, makes pressure Add to 30MPa power even；1700 DEG C, under the conditions of pressure 30MPa, be incubated 10 minutes, then power-off naturally cools to Room temperature.
The mechanical property of material is: bending strength 908～978MPa, and fracture toughness is 5.53～6.12MPa.m1/2。
Embodiment 3
(1) aluminium oxide and the Graphene of titanium carbide mixed-powder gross mass 0.25% are weighed, by Graphene and PVP mass ratio 5:1 weighs PVP, both is successively added in 200ml dehydrated alcohol and stirs, ultrasonic disperse 2 hours；By submicron alpha-Al2O3 (0.5 μm), submicron TiC (0.5 μm) 7:3 by volume mix, and add aluminium oxide and titanium carbide mixed-powder mass percent Be 1% MgO and dispersion after graphene suspension, by 5:1 ratio of grinding media to material add Al2O3Mill ball, by the nothing of 200ml:60g Water-ethanol material, than adding dehydrated alcohol, ultrasonic disperse 0.5 hour, is then placed in ball milling bucket high speed ball milling 60 hours.
(2) composite mortar after ball milling is put into vacuum drying oven, dry under the conditions of vacuum is-0.8MPa and 120 DEG C Dry, cross 150 mesh sieves, obtain finely disseminated mixed-powder.
(3) mixed-powder step (2) prepared loads in graphite jig, puts into vacuum hotpressing stove sintering, during sintering, Vacuum remains at below 10Pa, and sintering process is: when room temperature～1200 DEG C, and heating rate is 40 DEG C/min, 1200 DEG C, it is incubated 5 minutes；When 1200 DEG C-1700 DEG C, heating rate is 35 DEG C/min, uses manual pressure mode, makes pressure Add to 30MPa power even；1700 DEG C, under the conditions of pressure 30MPa, be incubated 10 minutes, then power-off naturally cools to Room temperature.
The mechanical property of material is: bending strength 933～1037MPa, and fracture toughness is 5.75～6.33MPa.m1/2。

Claims (3)

1. an aluminum oxide/titanium carbide based composite ceramic material, with alumina-titanium carbide as matrix, is characterized in that: aluminium oxide- Containing equally distributed Graphene in titanium carbide matrix；The mass percent of Graphene be aluminum oxide-titanium carbide Titanium base 0.2～ 0.3%.
The preparation method of a kind of alumina-titanium carbide based composite ceramic material the most according to claim 1, is characterized in that bag Include following steps:
(1) graphene dispersion
Polyvinylpyrrolidone is joined in ethanol solution, stirring while adding be completely dissolved to polyvinylpyrrolidone； Graphene is added slowly in polyvinylpyrrolidonesolution solution, stirs, and ultrasonic disperse forms graphene suspension；Stone Ink alkene content is Al2O3The 0.2～0.3% of/TiC mixed-powder gross mass, polyvinylpyrrolidone and Graphene mass ratio are 1: 3～5；
(2) batch mixing
By volume percentage ratio 7:3 weighs Al2O3With TiC powder mixing, add Al2O3The MgO of/TiC mixed-powder gross mass 1% For sintering aid, it is subsequently adding the graphene suspension of preparation in dehydrated alcohol and step (1)；Stirring while adding, more ultrasonic point Dissipate the slurry forming mix homogeneously；Mixed slurry is poured in ball milling bucket, add Al2O3Mill ball, dry powder is 1 with ball weight ratio: 5；Ball milling 60～72 hours on ball mill, vacuum dried, sieve, the material powder being uniformly mixed；
(3) hot pressed sintering
Material powder step (2) prepared loads in graphite jig, is sintered under vacuum conditions, and sintering process is: Room temperature～when 1200 DEG C, heating rate is 40 DEG C/min, at 1200 DEG C, is incubated 5 minutes；When 1200 DEG C-1700 DEG C, heat up Speed is 35 DEG C/min, and uniform pressurization makes pressure steadily rise to 30MPa；1700 DEG C, under the conditions of pressure 30MPa, be incubated 10 points Clock, then power-off naturally cools to room temperature.
The preparation method of a kind of alumina-titanium carbide based composite ceramic material the most according to claim 2, is characterized in that step Suddenly in (1), the Graphene ultrasonic disperse time is 2～3 hours, and in step (2), mixed slurry needs ultrasonic disperse 0.5～1 little before grinding Time.
CN201610518352.5A 2016-07-01 2016-07-01 A kind of aluminium oxide titanium carbide base composite ceramic material and preparation method thereof Pending CN106187112A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106699140A (en) * 2017-02-08 2017-05-24 无锡工艺职业技术学院 High-hardness ceramic cutting head
CN106747431A (en) * 2017-02-24 2017-05-31 华南理工大学 A kind of Graphene ceramic composite powder and preparation method thereof
CN106830900A (en) * 2017-02-08 2017-06-13 无锡工艺职业技术学院 A kind of high-hardness ceramic cutter
CN107010977A (en) * 2017-05-19 2017-08-04 合肥龙图腾信息技术有限公司 A kind of Resisting fractre ceramic material and preparation method thereof
CN108424161A (en) * 2018-04-13 2018-08-21 山东大学 A kind of preparation method of the diphase ceramic material of graphene Strengthening and Toughening
CN109182815A (en) * 2018-10-23 2019-01-11 湖南大学 A kind of Cu-Co-Gr composite material and preparation method
CN113880557A (en) * 2021-08-18 2022-01-04 郑州航空工业管理学院 AL2O3-cBN-based ceramic cutting tool material and method for producing the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1454869A (en) * 2003-06-04 2003-11-12 山东大学 Gradient function ceramic cutter material and preparing method thereof
CN101857438A (en) * 2010-05-25 2010-10-13 山东大学 Method for preparing aluminum oxide-titanium carbide-zirconium oxide nanocomposite ceramic material
CN103044014A (en) * 2013-01-17 2013-04-17 山东大学 Preparation method of graphene-nanosheet-reinforced alumina ceramic

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1454869A (en) * 2003-06-04 2003-11-12 山东大学 Gradient function ceramic cutter material and preparing method thereof
CN101857438A (en) * 2010-05-25 2010-10-13 山东大学 Method for preparing aluminum oxide-titanium carbide-zirconium oxide nanocomposite ceramic material
CN103044014A (en) * 2013-01-17 2013-04-17 山东大学 Preparation method of graphene-nanosheet-reinforced alumina ceramic

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106699140A (en) * 2017-02-08 2017-05-24 无锡工艺职业技术学院 High-hardness ceramic cutting head
CN106830900A (en) * 2017-02-08 2017-06-13 无锡工艺职业技术学院 A kind of high-hardness ceramic cutter
CN106747431A (en) * 2017-02-24 2017-05-31 华南理工大学 A kind of Graphene ceramic composite powder and preparation method thereof
CN106747431B (en) * 2017-02-24 2020-09-22 华南理工大学 Graphene-ceramic composite powder and preparation method thereof
CN107010977A (en) * 2017-05-19 2017-08-04 合肥龙图腾信息技术有限公司 A kind of Resisting fractre ceramic material and preparation method thereof
CN108424161A (en) * 2018-04-13 2018-08-21 山东大学 A kind of preparation method of the diphase ceramic material of graphene Strengthening and Toughening
CN109182815A (en) * 2018-10-23 2019-01-11 湖南大学 A kind of Cu-Co-Gr composite material and preparation method
CN113880557A (en) * 2021-08-18 2022-01-04 郑州航空工业管理学院 AL2O3-cBN-based ceramic cutting tool material and method for producing the same

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