CN107140954A - The preparation method of the dispersed enhancing alumina composite material of graphene oxide - Google Patents
The preparation method of the dispersed enhancing alumina composite material of graphene oxide Download PDFInfo
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- CN107140954A CN107140954A CN201710548635.9A CN201710548635A CN107140954A CN 107140954 A CN107140954 A CN 107140954A CN 201710548635 A CN201710548635 A CN 201710548635A CN 107140954 A CN107140954 A CN 107140954A
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Abstract
The present invention discloses a kind of preparation method of the dispersed enhancing alumina composite material of graphene oxide, comprises the following steps:Prepare the graphene oxide hydrosol;Prepare TiO2CuO sintering aids;Prepare AlOOH colloidal sols;AlOOH colloidal sols are added into TiO by certain percentage by weight2CuO sintering aids, then by GO/ α Al2O3Ratio of the weight than 0.2% 0.6% the graphene oxide hydrosol is dispersed in AlOOH colloidal sols, be heated to moisture evaporation, obtain gel, through shaping, dry, calcining and hot pressed sintering, produce.The present invention realizes graphene oxide in α Al2O3It is dispersed in matrix, obtain splendid Strengthening and Toughening effect.
Description
Technical field
The present invention relates to field of composite material preparation, and in particular to the dispersed enhancing alumina composite material of graphene oxide
The preparation method of material.
Background technology
αα-Al2O3Base advanced structural ceramic material has that high mechanical strength, insulaion resistance are big, hardness is high, corrosion-resistant, resistance to
Outstanding advantages such as mill, high temperature resistant, and aboundresources is cheap, are that purposes most wide, volume of production and marketing is most in current oxide ceramics
Big ceramic new material, available for fields such as Aero-Space, defence and militaries.But aluminum oxide also has the shortcomings that itself, such as fragility
Greatly, thermal shock resistance is poor etc. but its low toughness limits its development, can make mechanical property by graphene oxide toughness reinforcing
It is improved.Graphene oxide (Graphene Oxide, GO) chemical method prepares the intermediate product of graphene, the crystalline substance with two dimension
Its big Main Mechanical of body structure, light weight and specific surface area and graphene are almost not different, and contain hydroxyl in structure
The hydrophilic radicals such as base (- OH), carboxyl (- COOH), epoxy radicals (- O-), with water solubility.The graphene oxide hydrosol can be with
AIOOH colloidal sols dissolve each other, so in α-Al2O3Finely dispersed GO is added in ceramics, is extracted by graphene film, for crackle
Bridge joint and crackle meet the extension that graphene direction deflection etc. hinders crackle, improve the fracture toughness of composite.However, such as
What realizes that GO being uniformly distributed in the base is still that GO strengthens the great difficult problem of ceramic matric composite.Mechanical ball mill and ultrasonic powder
Broken method the more graphene of the reunion of multilayer can be peeled off into few layer and composite granule is well mixed, but ball milling and
The graphene-structured that can be damaged in crushing process, the composite materials property prepared is had a greatly reduced quality;Mechanical ball mill and ultrasound
Cycle needed for crushing graphene is long, efficiency bottom, and the individual layer high to transparency for being difficult is graphene, it is also difficult in matrix
In be uniformly dispersed, the application which limits graphene as reinforcement in ceramics, scattering problem be still perplex this class material
Expect the huge obstacle of research and development.
The content of the invention
To solve the above problems, the invention provides a kind of dispersed enhancing alumina composite of graphene oxide hydrosol
The preparation method of material, realizes graphene oxide in α-Al2O3It is dispersed in matrix, increase not only for graphene oxide
The exploitation of Strong oxdiative aluminum matrix composite, which has, to be obviously of great immediate significance, also compound for the enhanced ceramic base of graphene
Material provides beneficial reference, promotes graphene enhancing ceramic matric composite fast-developing.
To achieve the above object, the technical scheme taken of the present invention is:
The preparation method of the dispersed enhancing alumina composite material of graphene oxide, comprises the following steps:
S1, with 1000ml beakers the 400ml concentrated sulfuric acids are measured, be placed in 0 DEG C of ice bath, 5g graphite is first added again under magnetic agitation
5g potassium nitrate is added, and is slowly added to 40g potassium permanganate in 40min under magnetic stirring, turns after 38 DEG C of insulation 4.5h of oil bath, turns
0 DEG C of ice bath, is slowly added to 400ml deionized waters, turns after 80 DEG C of insulation 30min of oil bath, adds 40ml hydrogen peroxide (H2O2, 30%),
Again plus 100-200ml deionized waters, mixed liquor is obtained;
S2, by after mixed liquor quiescent setting, supernatant is outwelled, plus distilled water is settled to after 1000ml, under glass bar stirring
Plus 50ml hydrochloric acid (HCl, 36%);Quiescent setting, goes supernatant, plus distilled water to be settled to after 1000ml, and glass bar stirring is lower to be added
50ml hydrochloric acid, quiescent setting removes supernatant, until it is static without supernatant when, precipitation is poured into bag filter, be put into equipped with distillation
Dialysed 1 month in the container of water, wherein, the water in container is changed once for one day, and dialysis to pH value is 6.5 or so, ultrasonication
2h has obtained the nano graphene oxide hydrosol;
S3, by TiO2Ball milling mixing is carried out by weight 4: 1 with CuO, ratio of grinding media to material 15: 1, rotating speed is 250r/min, ball
Grind after 20h, obtain TiO2- CuO sintering aids, take out standby;
S4, with beaker 400ml distilled water heating water bath is measured to 90 DEG C, add after 30g aluminium isopropoxides, 90 DEG C of hydrolysis 4h,
Add 2mlHNO3(65%), 90 DEG C of insulation 10h, obtain AIOOH colloidal sols;
S5, the AIOOH colloidal sols of gained by certain percentage by weight are added into TiO2- CuO sintering aids, then by GO:
α-Al2O3Ratio of the weight than 0.2%-0.6% the graphene oxide hydrosol is dispersed in AIOOH colloidal sols, be heated to moisture
Evaporation, obtains gel, and GO/ α-Al are prepared through shaping, dry, calcining and hot pressed sintering2O3Composite;Wherein, the work of hot pressed sintering
Skill condition is 1500 DEG C, and 20MPa is incubated 1h hot pressed sinterings.
The invention has the advantages that:
Alumina precursor is prepared using sol-gel process, and the GO hydrosols are dispersed in AIOOH colloidal sols, is realized
GO/ α-Al dispersed GO2O3Composite, obtains splendid Strengthening and Toughening effect, is combined not only for GO enhancing alumina bases
The exploitation of material, which has, to be obviously of great immediate significance, and also provides beneficial for the enhanced ceramic matric composites of other GO
Use for reference, promote GO enhancing ceramic matric composites fast-developing.
Brief description of the drawings
Fig. 1 is the atomic force microscopy diagram of the graphene oxide hydrosol used in the present invention.
Fig. 2 is the x-ray photoelectron energy spectrum diagram (XPS) of graphene oxide.
Fig. 3 is addition sintering aid GO/ α-Al in the embodiment of the present invention2O3The bending strength of composite.
Fig. 4 is addition sintering aid GO/ α-Al in the embodiment of the present invention2O3Bending when GO contents are 0 in composite is carried
Lotus-displacement curve;
Fig. 5 is addition sintering aid GO/ α-Al in the embodiment of the present invention2O3Load when GO contents are 0.2% in composite
Lotus-displacement curve.
Fig. 6 is addition sintering aid GO/ α-Al in the embodiment of the present invention2O3Load when GO contents are 0.6% in composite
Lotus-displacement curve.
Fig. 7 is GO/ α-Al2O3Composite Three Points Bending Specimen fracture apperance.
Embodiment
In order that objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
Describe in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Embodiment
S1, with 1000ml beakers the 400ml concentrated sulfuric acids are measured, be placed in 0 DEG C of ice bath, 5g graphite is first added again under magnetic agitation
5g potassium nitrate is added, and is slowly added to 40g potassium permanganate in 40min under magnetic stirring, turns after 38 DEG C of insulation 4.5h of oil bath, turns
0 DEG C of ice bath, is slowly added to 400ml deionized waters, turns after 80 DEG C of insulation 30min of oil bath, adds 40ml hydrogen peroxide (H2O2, 30%),
Again plus 100-200ml deionized waters, mixed liquor is obtained;
S2, by after mixed liquor quiescent setting, supernatant is outwelled, plus distilled water is settled to after 1000ml, under glass bar stirring
Plus 50ml hydrochloric acid (HCl, 36%);Quiescent setting, goes supernatant, plus distilled water to be settled to after 1000ml, and glass bar stirring is lower to be added
50ml hydrochloric acid, quiescent setting removes supernatant, until it is static without supernatant when, precipitation is poured into bag filter, be put into equipped with distillation
Dialysed 1 month in the container of water, wherein, the water in container is changed once for one day, and dialysis to pH value is 6.5 or so, ultrasonication
2h has obtained the nano graphene oxide hydrosol;
S3, the SP-3 types planetary ball mill produced using Nanjing University are by TiO2With CuO ball is carried out by weight 4: 1
Mill mixing, ratio of grinding media to material 15: 1 after rotating speed is 250r/min, ball milling 20h, obtains TiO2- CuO sintering aids, take out standby;
S3, with beaker 400ml distilled water heating water bath is measured to 90 DEG C, add after 30g aluminium isopropoxides, 90 DEG C of hydrolysis 4h,
Add 2mlHNO3(65%), 90 DEG C of insulation 10h, obtain AIOOH colloidal sols;
S4, the AIOOH colloidal sols of appropriate gained certain percentage by weight added into TiO2- CuO sintering aids, are then pressed
GO/α-Al2O3Ratio of the weight than 0.2%-0.6% the graphene oxide hydrosol is dispersed in AIOOH colloidal sols, be heated to
Moisture evaporation, obtains gel, and GO/ α-Al are prepared through shaping, dry, calcining and hot pressed sintering2O3Composite;Wherein, hot pressed sintering
Process conditions be 1500 DEG C, 20MPa, be incubated 1h hot pressed sinterings;
Fig. 1 is the atomic force microscopy diagram of graphene oxide, it can be seen that the scattered nanometer formed of oxidized and ultrasonic wave
Graphene oxide has obtained effective stripping, the shape characteristic of multilayer is no longer presented, graphene oxide sheet is in the hydrosol without group
Poly- to be uniformly dispersed, the size of piece is 5-6 μm, and thickness is 1nm or so, illustrates that the higher lamella of graphene oxide extent of exfoliation compares
Thin, oxidation processes are changed originally more complete graphite platelet structure.
Fig. 2 is engagement keys of the x-ray photoelectron energy spectrum diagram (XPS) to oxygen-containing functional group and surface of graphene oxide carbon atom
Analyzed, the graphene sheet layer after Fig. 2 display oxidations carries the characteristic peak of many oxygen-containing functional groups, such as carboxyl, hydroxyl
With the functional group such as epoxide group.
The composite bending strength of different GO contents is as shown in figure 3, with the increase of GO contents, the bending resistance of composite
Intensity increases to 355MPa for 0.2% to 0.6% composite mean intensity in increase, GO contents from 282MPa, hence it is evident that high
Alumina ceramic material mean intensity (167MPa) when carbon fiber content is 0%;When GO contents are 0.6%, composite wood
The mean intensity of material reaches 355MPa, is 2.1 times of the sample mean intensity without GO prepared under the same terms.
Fig. 4-Fig. 6 is respectively that GO contents are respectively 0%, 0.2%, during 0.6% composite material three-point bending test
Load-displacement curves, GO contents for 0.2% composite load displacement curve it is similar to 0%, brittle fracture feature is bright
It is aobvious, but (b) has bigger load, and work to break of the work to break absorbed during fracture also than 0% aluminum oxide is big.And 0.6% it is compound
Material, starts non-linear break of appearance in load-displacement curves and ratchet-like fluctuation occurs, slight sound is sent with the increase of load
Sound, is provided with the load-displacement curves of nonlinear characteristic, shows that material absorbs work to break in fracture.
Fig. 7 is the GO/ α-Al that GO contents are 0.2%2O3Crackle on the section parallel with pressure direction in composite sample
SEM patterns.From fracture apperance it can be seen that individual layer is close to transparent graphene oxide small pieces, because the color of alumina substrate is
Grey, graphene oxide small pieces are difficult to observe in the base, but still can see and dialled from matrix in fracture apperance
The single-layer graphene oxide small pieces gone out, graphene oxide toughened aluminum oxide matrix is extracted by graphene oxide sheet, for splitting
The bridge joint and crackle of line meet the extension that graphene film direction deflection etc. hinders crackle, improve the fracture toughness of composite
's.Graphene oxide may also be extracted or the unsticking in the interface cohesion with matrix from matrix, so that composite exists
Crackle deflects during fracture, thus extends the extension approach of crackle, is formd in alumina matrix composite new
Energy absorbing mechanism, so that the toughness of material is improved.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (2)
1. the preparation method of the dispersed enhancing alumina composite material of graphene oxide, it is characterised in that comprise the following steps:
S1, with 1000ml beakers the 400ml concentrated sulfuric acids are measured, be placed in 0 DEG C of ice bath, 5g graphite is first added under magnetic stirring and is added again
Enter 5g potassium nitrate, and be slowly added to 40g potassium permanganate in 40min under magnetic stirring, turn after 38 DEG C of insulation 4.5h of oil bath, turn 0
DEG C ice bath, is slowly added to 400ml deionized waters, turns after 80 DEG C of insulation 30min of oil bath, add 40ml mass fractions for 30% it is double
Oxygen water, then add 100-200ml deionized waters, obtain mixed liquor;
S2, by after mixed liquor quiescent setting, outwell supernatant, plus distilled water is settled to after 1000ml, glass bar stirring it is lower plus
50ml mass fractions are 36% hydrochloric acid;Quiescent setting, goes supernatant, plus distilled water to be settled to after 1000ml, glass bar stirring
Down plus hydrochloric acid that 50ml mass fractions are 36%, quiescent setting removes supernatant, until it is static without supernatant when, precipitation is poured into
In bag filter, it is put into the container equipped with distilled water and dialyses 1 month, wherein, the water in container is changed once for one day, dialysis to pH value
For 6.5 or so, ultrasonication 2h has obtained the nano graphene oxide hydrosol;
S3, by TiO2Ball milling mixing is carried out by weight 4: 1 with CuO, ratio of grinding media to material 15: 1, rotating speed is 250r/min, ball milling 20h
Afterwards, TiO is obtained2- CuO sintering aids, take out standby;
S4, with beaker 400ml distilled water heating water bath is measured to 90 DEG C, add after 30g aluminium isopropoxides, 90 DEG C of hydrolysis 4h, add
2ml mass fractions are 65% HNO3, 90 DEG C are incubated 10h, obtain AlOOH colloidal sols;
S5, the AlOOH colloidal sols of gained by certain percentage by weight are added into TiO2- CuO sintering aids, then by GO: α-
Al2O3Ratio of the weight than 0.2%-0.6% the graphene oxide hydrosol is dispersed in AlOOH colloidal sols, be heated to moisture steaming
Hair, obtains gel, and GO/ α-Al are prepared through shaping, dry, calcining and hot pressed sintering2O3Composite.
2. the preparation method of the dispersed enhancing alumina composite material of the graphene oxide according to claim 1,
Characterized in that, the process conditions of hot pressed sintering are 1500 DEG C, 20MPa is incubated 1h hot pressed sinterings.
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Cited By (8)
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CN107746283A (en) * | 2017-10-27 | 2018-03-02 | 兰州理工大学 | A kind of preparation method of the dispersed enhancing alumina composite material of CNT |
CN108249898A (en) * | 2018-01-22 | 2018-07-06 | 吴亚良 | A kind of preparation method of high-performance bullet proof composite plating |
CN109928757A (en) * | 2018-12-26 | 2019-06-25 | 武汉理工大学 | A kind of self assembly boron carbide-graphene composite ceramics and preparation method thereof |
CN110143810A (en) * | 2019-05-22 | 2019-08-20 | 哈尔滨工业大学 | A kind of preparation method of oriented alignment graphene/alumina composite ceramic |
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CN107746283A (en) * | 2017-10-27 | 2018-03-02 | 兰州理工大学 | A kind of preparation method of the dispersed enhancing alumina composite material of CNT |
CN107746283B (en) * | 2017-10-27 | 2020-11-13 | 兰州理工大学 | Preparation method of carbon nano tube uniformly dispersed and reinforced alumina composite material |
CN108249898A (en) * | 2018-01-22 | 2018-07-06 | 吴亚良 | A kind of preparation method of high-performance bullet proof composite plating |
CN108249898B (en) * | 2018-01-22 | 2021-04-02 | 绍兴市梓昂新材料有限公司 | Preparation method of high-performance composite bulletproof plate |
CN109928757A (en) * | 2018-12-26 | 2019-06-25 | 武汉理工大学 | A kind of self assembly boron carbide-graphene composite ceramics and preparation method thereof |
CN109928757B (en) * | 2018-12-26 | 2021-04-27 | 武汉理工大学 | Self-assembled boron carbide-graphene composite ceramic and preparation method thereof |
CN110143810A (en) * | 2019-05-22 | 2019-08-20 | 哈尔滨工业大学 | A kind of preparation method of oriented alignment graphene/alumina composite ceramic |
CN110282959A (en) * | 2019-07-31 | 2019-09-27 | 深圳烯创先进材料研究院有限公司 | A kind of method of graphene Strengthening and Toughening aluminium oxide ceramics |
CN114195553A (en) * | 2021-12-23 | 2022-03-18 | 广西蒙娜丽莎新材料有限公司 | Preparation method of fibrous nano-alumina modified ceramic glazed tile |
CN115466129A (en) * | 2022-08-10 | 2022-12-13 | 电子科技大学长三角研究院(湖州) | Preparation method of graphene-toughened alumina composite ceramic |
CN115650707A (en) * | 2022-11-03 | 2023-01-31 | 中国人民解放军陆军装甲兵学院 | Preparation method of magnesia-alumina transparent ceramic |
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