CN101070241A - Aluminium oxide silicon titanium carbonate/aluminium oxide lamina composite material and preparing method - Google Patents

Aluminium oxide silicon titanium carbonate/aluminium oxide lamina composite material and preparing method Download PDF

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CN101070241A
CN101070241A CN 200610046559 CN200610046559A CN101070241A CN 101070241 A CN101070241 A CN 101070241A CN 200610046559 CN200610046559 CN 200610046559 CN 200610046559 A CN200610046559 A CN 200610046559A CN 101070241 A CN101070241 A CN 101070241A
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aluminium oxide
silicon titanium
sintering
silicon
preparation
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CN100422109C (en
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周延春
万德田
包亦望
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Institute of Metal Research of CAS
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Abstract

This invention relates to the preparation method of an alumina / silicon titanium carbide / alumina (Al2O3 / Ti3SiC2 / Al2O3) sandwich laminar composite by in situ thermocompression /solid-liquid phase reaction. The invention adopts Al2O3 piece to adhere on surface of Ti3SiC2 to form enhanceing silicon titanium carbide (Ti3SiC2) of sandwich laminar composite; firstly , takes titanium power, silicon powder and graphite powder as raw material, mix 10 to 25 hours by physical mechanical process, gain mixture of original powder, then in graphite tooting, put original powder to middle of two Al2O3 pieces, coldd pressing for moulding, the pressure is 5 to 20MPa, sinter in hot pressing furnace that has shielding gas atmosphere, heating rate is 5 to 50 deg per minute, sintering temperature is 1400 to 1650deg, sintering time is 0.5 to 2 hours, sintering pressure 20 to 40 MPa.

Description

A kind of aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material and preparation method
Technical field
The present invention relates to ceramic matric composite and preparation method, be specially a kind of in-situ hot pressing/solid-liquid phase reaction and prepare aluminum oxide/silicon titanium carbide/aluminum oxide sandwich stratified composite and preparation method thereof.
Background technology
Ti 3SiC 2It is a kind of novel ternary layered ceramic material.U.S. pottery (the Journal of theAmerican Ceramic Society 79 of association journal, 1953 (1996)) studies show that in that it combines the plurality of advantages of pottery and metal, have low density, high-modulus, high specific conductivity and thermal conductivity and easy characteristics such as processing, thereby have broad application prospects.But as a kind of potential high-temperature structural material, Ti 3SiC 2Hardness and on the low side at antioxidant property more than 1100 ℃, limited its widespread use.At biomaterial (Biomaterials.25,3593 (2004)) and biotechnology progress (Trends in Biotechnology.22,577 (2004)) studies show that in, with soft layer and hard layer space and combine and can obtain a kind of novel lamellar material, it combines soft material and mechanically resistant material advantage separately.Show that in U.S. pottery association journal (Journal of the AmericanCeramic Society 75,3396 (1992)) article the stratified material that the surface has a residual compressive stress can obtain higher intensity and fracture toughness property (with respect to single-material).
Summary of the invention
The object of the present invention is to provide a kind of mechanical property controlled (mainly being bending strength), high-temperature oxidation resistance excellence, purity height, simple to operate, easy control of process conditions, aluminium oxide stratiform that cost is low to strengthen the sandwich laminar composite (Al of silicon titanium carbide 2O 3/ Ti 3SiC 2/ Al 2O 3) and preparation method thereof.
Technical scheme of the present invention is:
A kind of aluminium oxide/silicon titanium carbide/aluminium oxide sandwich laminar composite is by outer field aluminium oxide (Al 2O 3) and middle silicon titanium carbide (Ti 3SiC 2) the base layer composition, wherein alumina layer can be adjusted arbitrarily with the bed thickness ratio of silicon titanium carbide base layer and (be preferably: 0＜bed thickness ratio≤0.35).
The preparation method of described aluminum oxide/silicon titanium carbide/aluminum oxide sandwich stratified composite is a raw material with simple substance titanium valve, silica flour, Graphite Powder 99 and alumina wafer.Matrix Ti 3SiC 2The mol ratio of middle Ti: Si: C is 3.0: (1～1.2): 2.0.Aluminium oxide (Al 2O 3) sheet is to adopt conventional doctor blading method preparation, directly buys gained.Control the thickness ratio of alumina layer and silicon titanium carbide base layer by adjusting alumina layer thickness or silicon-carbon titanium material grain weight amount.Silicon-carbon titanium material powder in graphite jig, is put into the up and down two-layer Al of being with the starting powder that mixes after physical mechanical method mixes 10～25 hours 2O 3Cold moudling after in the sheet; the pressure that applies is 5～20MPa; sintering in the hot pressing furnace that is connected with inert gas shielding atmosphere, heating rate are 5～50 ℃/minute, and sintering temperature is that 1400～1650 ℃, sintering time are that 0.5～2 hour, sintering pressure are 20～40MPa.Under lower temperature, in short time, prepare have high-purity, high-compactness, case hardness height, the superior Al of combination property such as antioxygenic property is good, bending strength is controlled 2O 3/ Ti 3SiC 2/ Al 2O 3Laminar composite.
The titanium valve of described adding, silica flour and graphite powder particle size range are 200～400 orders; Described alumina wafer is through doctor blading method preparation (directly buying); Described sintering processing is hot pressed sintering or HIP sintering; Described inert gas is argon gas, helium or neon; Described physical mechanical method mixes the ball-milling method that adopts under the alcohol medium.
Principle of design of the present invention is as follows:
The thermal expansivity (8.6 * 10 of aluminum oxide -6K -1) be slightly less than the thermal expansivity (9.2 * 10 of silicon titanium carbide -6K -1), at outer (Al 2O 3Layer) will produce residual compressive stress in.So, if with aluminium oxide as hard layer, the silicon titanium carbide is the Al that soft layer is used for preparing 2O 3/ Ti 3SiC 2/ Al 2O 3The sandwich laminar composite can improve silicon titanium carbide (Ti effectively 3SiC 2) intensity and case hardness.Because aluminium oxide has excellent antioxygenic property and reduces Al 2O 3/ Ti 3SiC 2/ Al 2O 3The efficient oxidation area in the sandwich laminar composite, thus silicon titanium carbide (Ti can be improved 3SiC 2) high-temperature oxidation resistance.In addition, owing to the silicon titanium carbide hardness (about 4GPa) of outer field aluminum oxide hardness (about 18GPa) far above base layer, the surface hardness of matrix material also will improve significantly.Therefore, our design and Al of preparing 2O 3/ Ti 3SiC 2/ Al 2O 3The sandwich laminar composite is on the one hand because high rigidity and the excellent oxidation resistance of aluminium oxide can improve silicon titanium carbide (Ti 3SiC 2) case hardness and antioxygenic property, the thermal coefficient of expansion of aluminium oxide is slightly less than the thermal coefficient of expansion of silicon titanium carbide and the residual compressive stress that forms can improve silicon titanium carbide (Ti on the other hand 3SiC 2) intensity.In addition, owing to the residual stress that not mating of thermal coefficient of expansion forms can be calculated by theory, the value added of its intensity also can be calculated, thereby reaches the controlled purpose of intensity of prepared sandwich composite.
Advantage of the present invention is:
1, purity height, surface hardness height, mechanical property is controlled, high-temperature oxidation resistance good.Adopt the Al of the inventive method preparation 2O 3/ Ti 3SiC 2/ Al 2O 3Laminar composite mainly by silicon titanium carbide and aluminium oxide two phase compositions, only contains a small amount of impurity phase titanium carbide in the silicon-carbon titanium layer.Utilize the present invention, original position synthetic silicon titanium carbide matrix and aluminum oxide lamella have preferably consistency and have formed a stronger interface, and reinforced effects is improved greatly.Al 2O 3/ Ti 3SiC 2/ Al 2O 3The case hardness of composite, elastic modelling quantity, bending strength, high-temperature oxidation resistance etc. are all than pure Ti 3SiC 2Be significantly improved.With Al 2O 3Layer and Ti 3SiC 2Base layer bed thickness ratio be 0.12 o'clock be example, the elastic modelling quantity of composite reaches 372GPa, case hardness is 17.9GPa, bending strength is 531MPa, respectively than Ti 3SiC 2Improved about 19.2%, 348%, 11.8%.Experimental results show that Al 2O 3/ Ti 3SiC 2/ Al 2O 3The bending strength of composite has obvious relation with bed thickness than (aluminium oxide/silicon titanium carbide), increase afterwards earlier within the specific limits and reduce, and the intensity level that calculates with theory and variation tendency thereof all meet fine, the intensity that shows this composite is recently controlled by adjusting bed thickness, and can be with the prediction of residual stress calculation method, so its intensity has controllability.In addition, can predict, because aluminium oxide (Al 2O 3) reducing the efficient oxidation area in composite, composite antioxygenic property one at high temperature increases surely.
2, technology is simple, and cost is low.The present invention is that sintering carries out simultaneously with densified by the reaction of in-situ hot pressing/solid-liquid phase, and the silicon titanium carbide is synthetic by in-situ hot pressing, and aluminium oxide synthesizes by sintering, finally obtains Al 2O 3/ Ti 3SiC 2/ Al 2O 3The sandwich laminar composite.Because the appearance of liquid phase is arranged in sintering process, utilize the quick mass transport process of liquid phase, chemical time is shortened greatly, make again densification process become very easy.With respect to first synthesizing ceramic powder, mixed sintering had both made technological process become simply again, had saved again expense.In addition, in order to obtain the composite of different layers thickness rate, only need to adopt different-thickness Al 2O 3Thin slice or with outer Al 2O 3Layer grinds off corresponding thickness and gets final product, and provides convenience for satisfying different working conditions and saving material.
Description of drawings
Fig. 1 is Al 2O 3/ Ti 3SiC 2/ Al 2O 3Backscattered electron photo after the composite polishing.
Fig. 2 is Al 2O 3/ Ti 3SiC 2/ Al 2O 3The bending strength of composite and bed thickness are than (individual layer Al 2O 3Layer thickness/Ti 3SiC 2Matrix ligament thickness) relation between reaches the contrast with calculated value.
Fig. 3 is Al 2O 3/ Ti 3SiC 2/ Al 2O 3The fracture backscattered electron photo of composite after having surveyed bending strength.
Embodiment
Below by example in detail the present invention is described in detail.
Embodiment 1
Be 200～400 purpose titanium valves 17.84 gram, silica flour 4.18 grams and graphite powder 2.98 grams ball milling 10 hours in the alcohol medium with particle size range, in graphite jig the raw meal that mixes being put into all is up and down aluminium oxide (Al 2O 3) afterwards cold moudling of sheet (thickness is 0.5 millimeter, and diameter is 50 millimeters), the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 1550 ℃ of insulations 1 hour, and pressure is added to 25MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 25MPa.Whole sintering process all is to carry out under argon shield, the product of acquisition through X-ray diffraction analysis as can be known, skin mainly is α-Al 2O 3, thickness is 280 microns, internal layer is for containing the silicon titanium carbide (Ti of a small amount of impurity phase titanium carbide (TiC) particle 3SiC 2), thickness is 2.6 millimeters, impurity phase titanium carbide content is lower than 7wt.% (weight content).
Embodiment 2
Be 200～400 purpose titanium valves 8.92 gram, silica flour 2.09 grams and graphite 1.49 grams ball milling 15 hours in the alcohol medium with particle size range, in graphite jig the raw meal that mixes being put into all is up and down aluminium oxide (Al 2O 3) afterwards cold moudling of sheet (thickness is 1 millimeter, and diameter is 50 millimeters), the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 15 ℃/minute, is heated to 1560 ℃ of insulations 1 hour, and pressure is added to 30MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 30MPa.Whole sintering process all is to carry out under argon shield, the product of acquisition through X-ray diffraction analysis as can be known, skin mainly is α-Al 2O 3, thickness is 550 microns, internal layer is for containing the silicon titanium carbide (Ti of a small amount of impurity phase titanium carbide (TiC) particle 3SiC 2), thickness is 1.3 millimeters, impurity phase titanium carbide content is lower than 7wt.% (weight content).
Embodiment 3
Be 200～400 purpose titanium valves 53.52 gram, silica flour 12.10 grams and graphite 8.94 grams ball milling 20 hours in the alcohol medium with particle size range, in graphite jig the raw meal that mixes being put into all is up and down aluminium oxide (Al 2O 3) afterwards cold moudling of sheet (thickness is 4 millimeters, and diameter is 50 millimeters), the pressure that applies is 10MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 20 ℃/minute, is heated to 1600 ℃ of insulations 1 hour, and pressure is added to 30MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 40MPa.Whole sintering process all is to carry out under argon shield, the product of acquisition through X-ray diffraction analysis as can be known, skin mainly is α-Al 2O 3, thickness is 2.1 millimeters, internal layer is for containing the silicon titanium carbide (Ti of a small amount of impurity phase titanium carbide (TiC) particle 3SiC 2), thickness is 8.5 millimeters, impurity phase titanium carbide content is lower than 7wt.% (weight content).
Comparative example
Adopt the technology identical with embodiment 2 to prepare Ti 3SiC 2(containing a small amount of TiC), the density that Archimedes's method records is 4.49g/cm 3Vickers hardness is 4.02GPa; Elastic modelling quantity is 312GPa; Bending strength is 475MPa; The Al of gained among the described embodiment 1,2,3 2O 3/ Ti 3SiC 2/ Al 2O 3The case hardness of composite all is the hardness of aluminium oxide, elastic modelling quantity and bending strength then with alumina layer/silicon-carbon titanium layer bed thickness than relevant.When alumina layer/silicon-carbon titanium layer bed thickness ratio is between 0～0.35, Al 2O 3/ Ti 3SiC 2/ Al 2O 3Every mechanical performance index of composite all is better than Ti 3SiC 2Specify below and form Al 2O 3/ Ti 3SiC 2/ Al 2O 3Tissue and performance variation behind the composite.
Fig. 1 is Al 2O 3/ Ti 3SiC 2/ Al 2O 3Backscattered electron photo after the composite polishing.That skin is darker is Al 2O 3Layer, the intermediate layer of white light tone is Ti 3SiC 2Matrix, what contain a small amount of grey black in the intermediate layer is impurity phase TiC particle mutually.Al as seen from the figure 2O 3Layer and Ti 3SiC 2The base layer interface is clear, is not having at the interface obvious crackle and defective to exist.Fig. 2 is Al 2O 3/ Ti 3SiC 2/ Al 2O 3The bending strength of composite and bed thickness than the relation between (mono-layer oxidized aluminium lamination/silicon-carbon titanium layer) and with the contrast of calculated value.As seen improved Ti more significantly by this stratiform composite methods 3SiC 2Intensity.Along with the increase of Thickness Ratio (alumina layer/silicon-carbon titanium layer), the intensity of composite increases afterwards earlier and reduces, and has an optimal layer thickness rate value so that intensity reaches maximum.Experiment shows that thickness all is the intensity that is higher than the silicon titanium carbide than the intensity of gained matrix material in 0～0.14 scope at least.In addition, from Fig. 2, can also see the theoretical strength that calculates by the residual stress equilibrium relation, no matter its size and variation trends are all coincide finely with the experiment measuring value.This and the Al that above mentions 2O 3/ Ti 3SiC 2/ Al 2O 3It is consistent that the intensity of composite has controllability.Fig. 3 is Al 2O 3/ Ti 3SiC 2/ A1 2O 3The backscattered electron photo of the fracture of composite after having surveyed bending strength.Do not having slippage and crackle to produce at the interface, illustrate that the interface of aluminum oxide and silicon titanium carbide is a strong interface in matrix material, for passing through stratiform composite methods raising Ti 3SiC 2Intensity lay a good foundation.
By embodiment 1, embodiment 2, embodiment 3 and comparative example as seen, the Al of this method preparation 2O 3/ Ti 3SiC 2/ Al 2O 3The sandwich laminar composite has purity height, density height, case hardness height, and mechanical property is good and have advantages such as controllability (mainly being bending strength), high-temperature oxidation resistance excellence.

Claims (7)

1, a kind of aluminium oxide silicon titanium carbonate/aluminium oxide lamina composite is characterized in that: the sandwich laminar composite Al that is made up of alumina layer and silicon titanium carbide base layer 2O 3/ Ti 3SiC 2/ Al 2O 3, skin is aluminium oxide, the intermediate layer is the silicon-carbon titanium layer.
2, according to the preparation method of the described aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material of claim 1, it is characterized in that: with simple substance titanium valve, silica flour, Graphite Powder 99 and alumina wafer is raw material; Matrix Ti 3SiC 2The mol ratio of middle Ti: Si: C is 3.0: (1～1.2): 2.0; Come the thickness ratio of controlled oxidation aluminium lamination and silicon titanium carbide base layer by adjusting alumina wafer thickness or silicon-carbon titanium material grain weight amount, in graphite jig, the starting powder that mixes is put into the two-layer Al of being up and down 2O 3Back coldmoulding in the sheet; the pressure that applies is 5～20MPa; sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere, temperature rise rate are 5～50 ℃/minute, and sintering temperature is that 1400～1650 ℃, sintering time are that 0.5～2 hour, sintering pressure are 20～40MPa.
3, according to the preparation method of the described aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material of claim 2, it is characterized in that: the titanium valve of described adding, silica flour, Graphite Powder 99 size range are 200～400 orders; Described alumina wafer is to adopt doctor blading method to prepare gained, and thickness is 0.5～4 millimeter.
4, according to the preparation method of the described aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material of claim 2, it is characterized in that: described sintering processing is hot pressed sintering or HIP sintering.
5, according to the preparation method of the described aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material of claim 2, it is characterized in that: described rare gas element is argon gas, helium or neon.
6, according to the preparation method of the described aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material of claim 2, it is characterized in that: silicon titanium carbide starting powder mixed 10～25 hours through physical mechanical method.
7, according to the preparation method of the described aluminium oxide silicon titanium carbonate/aluminium oxide lamina matrix material of claim 6, it is characterized in that: described physical mechanical method mixes employing ball milling in the alcohol medium.
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Cited By (7)

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CN101747075B (en) * 2008-12-10 2012-05-23 中国科学院金属研究所 Porous conductive MAX phase ceramics and preparation method and use thereof
CN106830883A (en) * 2016-12-05 2017-06-13 苏州洛特兰新材料科技有限公司 A kind of antistatic composite ceramic material for adding Titanium and preparation method thereof
CN107488043A (en) * 2016-06-12 2017-12-19 中国科学院宁波材料技术与工程研究所 Multilayer complex films, its preparation method and the application as carborundum and its composite connecting material
CN109180161A (en) * 2018-08-24 2019-01-11 济南大学 A kind of high-purity titanium silicon carbide/alumina composite material and preparation method thereof
CN110184549A (en) * 2019-07-05 2019-08-30 苏州大学 Sandwich structure composite material and preparation method
CN113582673A (en) * 2021-08-26 2021-11-02 济南大学 Aluminum oxide/titanium silicon carbon layered composite material and in-situ preparation method thereof
CN115073152A (en) * 2022-07-22 2022-09-20 内蒙古工业大学 Laminated ceramic composite material and preparation method thereof, lanthanum chromate ceramic and manufacturing process thereof

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CN1234641C (en) * 2003-05-28 2006-01-04 中国科学院金属研究所 Preparing method for Ti3 SiC2 material without TiC impurity

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101747075B (en) * 2008-12-10 2012-05-23 中国科学院金属研究所 Porous conductive MAX phase ceramics and preparation method and use thereof
CN107488043A (en) * 2016-06-12 2017-12-19 中国科学院宁波材料技术与工程研究所 Multilayer complex films, its preparation method and the application as carborundum and its composite connecting material
CN107488043B (en) * 2016-06-12 2022-10-25 中国科学院宁波材料技术与工程研究所 Multilayer composite film, preparation method thereof and application of multilayer composite film as silicon carbide and composite material connecting material thereof
CN106830883A (en) * 2016-12-05 2017-06-13 苏州洛特兰新材料科技有限公司 A kind of antistatic composite ceramic material for adding Titanium and preparation method thereof
CN109180161A (en) * 2018-08-24 2019-01-11 济南大学 A kind of high-purity titanium silicon carbide/alumina composite material and preparation method thereof
CN109180161B (en) * 2018-08-24 2021-07-06 济南大学 High-purity titanium silicon carbide/alumina composite material and preparation method thereof
CN110184549A (en) * 2019-07-05 2019-08-30 苏州大学 Sandwich structure composite material and preparation method
CN113582673A (en) * 2021-08-26 2021-11-02 济南大学 Aluminum oxide/titanium silicon carbon layered composite material and in-situ preparation method thereof
CN115073152A (en) * 2022-07-22 2022-09-20 内蒙古工业大学 Laminated ceramic composite material and preparation method thereof, lanthanum chromate ceramic and manufacturing process thereof

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