CN101805199B - Aluminium titanate nanofiber toughened alumina composite material and preparation method thereof - Google Patents
Aluminium titanate nanofiber toughened alumina composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminium titanate nanofiber toughened alumina composite material and a preparation method thereof, wherein the preparation method comprises the following steps: firstly preparing an aluminium titanate nanofiber precursor, then mixing the aluminium titanate nanofiber precursor into a hot alkali dispersed alumina suspension to form a colloidal composite suspension system, and preparing an aluminium titanate nanofiber toughened alumina-based novel composite material through drying, program temperature rise roasting and grinding processes. The alumina-based novel composite material of the invention has low sintering temperature, high fracture toughness, large anti-bending strength and excellent abrasion resisting and corrosion resisting performance and can be widely applied to multiple national economic development important trades of engineering machinery, mining metallurgy, power generation, airplane and vehicle exhaust emission, petroleum gas exploitation, storage and transportation, special processing cutters, electron electricity and the like with higher special requirements for the aspects of mechanical shock resistance, thermal shock resistance, high temperature resistance, corrosion resistance, abrasion resistance, high rigidity and the like.
Description
Technical field
The invention belongs to the NEW TYPE OF COMPOSITE field of functional materials, be specifically related to a kind of aluminium titanate nanofiber toughened wear-resistant, heat shock resistance alumina base advanced composite material and preparation method thereof that adopts.
Background technology
Owing to thering is high rigidity and excellent high temperature resistant, wear-resisting and corrosion resistance nature, aluminum oxide engineering machinery, aircraft and motor vehicle exhaust, electric and electronic, fossil energy (oil, Sweet natural gas, coal),, the numerous areas such as building, traffic, biomedicine obtain a wide range of applications.But, as stupalith, the sintering temperature of aluminum oxide is usually more than 1500 ℃, and lower fracture toughness property makes its fragility higher, anti-mechanical shock and processing characteristics are poor, in addition, the thermal expansivity of aluminum oxide is also relatively high, is also easily cracking damage under thermal shocking frequently.For mechanics of machinery, calorifics and the chemical application performance that meets long time stability, mainly by the doping approach, improve at present the respective performances of aluminum oxide.Material modified zirconium white, silicon carbide, boron nitride, titanium carbide, rare earth nitride, mullite, pure aluminium silicate, carbon material, vitreum, the metal etc. of comprising that adopt, the form of dopant material comprises irregular macrobead, superfine powder, fiber etc., doping way comprises single doping or compound prescription doping, also there is the different growth of employing alumina grain to carry out from toughness reinforcing correlative study [modern technologies pottery, 2006,3:31].
In the alumina modified system of exploitation at present, Zirconium powder prepares zirconium white modified aluminas (being commonly called as ZTA) [patent of invention 02111742.X as a kind of the most frequently used altered contents, 200610011190.2, 200710178148.4, 200910019968.8], but obtain good modified effect, need at first obtain and there is the nano ultrafine powders body, the zirconium white of the specific form such as sheet or wire, and by the zirconium white full and uniform dispersion in alumina powder, dispersing apparatus and processing requirement are higher, add zirconium white raw materials costliness, therefore the preparation cost of ZTA is higher, adopt the materials such as nitride, carbide and rare earth to be adulterated [patent of invention 200510044750.X, 200610043811.5,200910015239.5,200910072369.2], equally also face that cost of material is high, the problems such as preparation and dispersion technology complexity, although mullite and pure aluminium silicate are relatively cheap, its physical strength is poor, and toughening effect is limited, and the resistance to acid attack performance relative deficiency [patent of invention 200610091975.5 of mullite and pure aluminium silicate, mining metallurgical engineering, 2005,4:73], the preparation cost of carbon material (comprising carbon fiber and carbon nanotube) is higher, be not easy to disperse in aluminum oxide, and material modified need be under protection of inert gas could sintering, therefore, although the doping of carbon material can significantly improve the fracture toughness property of aluminum oxide, too high modification cost makes it be difficult to large-scale production, the limited [National University of Defense technology's journal of the market competitiveness, 1998,5:14, patent of invention 200710056691.7], although the simple glass body cheaply is easy to get, there will be the softening phenomenon that becomes fragile below 800 ℃, anti-machinery and thermal shock resistance properties need to improve, although the temperature that part special glass can anti-1200 ℃ of left and right, its price is very expensive, is not suitable for widely applying [vacuum electronic technology, 2005,4:15], but doping metals can improve the fracture toughness property and machine-shaping property of aluminum oxide, but metal proportion is large, resistance to acid attack ability, thermal expansivity and aluminum oxide difference greatly, be difficult for dispersed in aluminum oxide and need be in inert protective atmosphere sintering, greatly limited the application [nano heterogeneous ceramic of metal in alumina modified, Beijing: Chemical Industry Press, 2004:199].
Deficiency based on above-mentioned alumina modified research and development, reality be starved of under low cost the exploitation toughening effect obviously, thermal expansion matching and thermal shock resistance is excellent, the new modified alumina composite material of wear resistant corrosion resistant and preparation method thereof.Accordingly, this project be take first the oxide compound of aluminium or oxyhydroxide and titanium dioxide and is prepared the aluminium titanate nanofiber presoma as raw material, disperse again to form the paste shape material in the alkali thermal environment with aluminum oxide, after drying and simple temperature-programmed calcination, obtained first and take aluminium titanate nanofiber as the toughness reinforcing alumina matrix composite that obtains mutually, with respect to aluminum oxide and other material doped modified oxidized aluminum, the modified oxidized aluminum composite of aluminium titanate nanofiber disclosed by the invention had both had fracture toughness property and the bending strength significantly improved, simultaneously owing to having introduced the lower aluminium titanates of thermal expansivity, it is high temperature resistant and thermal shock resistance also obviously improves, it is a kind of engineering machinery that is hopeful very much to be applied to, mining is metallurgical, generating, aircraft and motor vehicle exhaust, the exploitation of oil and gas and accumulating, the physical process cutter, the new function material of the important industry of the multiple national economic development such as electric.
Summary of the invention
Technical problem solved by the invention is to provide a kind of aluminium titanate nanofiber toughened alumina composite material and preparation method thereof, to solve the shortcoming in the above-mentioned background technology.
A kind of aluminium titanate nanofiber toughened alumina composite material, its main body is Alpha-alumina, toughness reinforcing is diameter 30～100 nanometers, the aluminium titanate nanofiber of long 1～3 micron mutually, in matrix material, the mass content of aluminium titanates fibre is 3～30%, preferably 10～20%, prepared alumina base novel composite ceramic material, can be by being dispersed in heterogeneous micrometer fibers in matrix and composite toughening and the reinforcing effect of particle, matrix material can be at sintering below 1500 ℃, and after sintering, its fracture toughness property can reach 7.2～9.0MPam
1/2Bending strength 650～800MPa, there is good acid-alkali-corrosive-resisting performance simultaneously, its mechanics of machinery and chemical stability are better than aluminum oxide (corundum), zirconium white and strengthen the materials such as aluminum oxide (ZTA), are expected in antagonism impact fractures such as the exploitation of engineering machinery, electric, mining metallurgy, generating, aircraft and motor vehicle exhaust, oil and gas and accumulating, physical process cutters, resistance to wear, have aspect high rigidity, the mechanics of machinery such as high temperature resistant, corrosion-resistant and physicochemical property the important industry of the multiple national economic development of higher particular requirement.
A kind of preparation method of aluminium titanate nanofiber toughened alumina composite material comprises the following steps:
(1) prepare the aluminium titanate nanofiber presoma: be respectively to take γ-AlOOH and TiO at 2: 1 by aluminium/titanium mol ratio
2Powder, first latter's ultrasonic wave is scattered in the strong base solution of 5～20mol/L concentration, airtight thermal response temperature is 110～200 ℃, then adds γ-AlOOH to continue airtight thermal response 8～16 hours, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(2) prepare the pasty state composite precursor: take a certain amount of aluminum oxide, under agitation add in certain density hot alkaline solution, temperature is 110～200 ℃, continue stirring reaction 6～10 hours, the aluminium titanate nanofiber presoma that adds preparation in (1), continue stirring reaction 6～10 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(3) aftertreatment of composite precursor: by after the composite precursor drying, keeping temperature is 400～800 ℃ of insulations 60～150 minutes, pass through temperature-programmed calcination, 1000～1300 ℃ of section insulations are incubated 90～120 minutes, finally by grinding, obtain aluminium titanate nanofiber toughened alumina composite material.
In the present invention, the preferred 8～15mol/L of described step (1) strong base solution concentration.
In the present invention, described TiO
2Powder and add γ-AlOOH after the top condition of airtight thermal response: 130～180 ℃ of temperature, react 10～12 hours.
In the present invention, preferably 130～180 ℃ of described step (2) hot alkaline solution temperature, concentration is 8～158～15mol/L preferably.
In the present invention, to add aluminum oxide and add the reaction times equal 1 after aluminium titanates nanometer presoma be 6～10 hours to described step.
In the present invention, in two sections processes of described temperature-programmed calcination, top condition is: first 500～700 ℃ of roasting, be incubated 60～150 minutes, and after roasting, 1100 ℃～1200 ℃ are incubated 90～120 minutes.
Beneficial effect:
One of outstanding advantages of the present invention is that preparation technology's flow process of disclosed aluminium titanate nanofiber toughened alumina composite material is simple, raw material sources are extensive, and can all adopt inorganics cheap and easy to get as raw material, do not use any tensio-active agent and organic solvent, preparation cost is low, be applicable to large-scale production, aluminium titanate nanofiber toughened alumina composite material prepared by the present invention, both had and compared corundum, fracture toughness property and bending strength that zirconium white modified aluminas (ZTA) is higher, also there is outstanding heat shock resistance and good abrasion resistance properties simultaneously, can be to fracture toughness property, heat shock resistance, the wear-resistant engineering machinery that waits the performance requriements harshness, mining is metallurgical, generating, aircraft and motor vehicle exhaust, the exploitation of oil and gas and accumulating, the physical process cutter, the field such as electric obtains widespread use.
The accompanying drawing explanation:
The microscopic appearance that Fig. 1 is aluminium titanate nanofiber toughened alumina composite material, i.e. SEM photo, the nanometer thread as the arrow indication in figure is the aluminium titanates fibre be dispersed in aluminum oxide base material;
The energy spectrogram that Fig. 2 is aluminium titanate nanofiber toughened alumina composite material, i.e. EDS spectrum;
The x-ray diffraction pattern that Fig. 3 is aluminium titanate nanofiber toughened alumina composite material, i.e. XRD spectrum;
Embodiment
In order to make technique means of the present invention, creation characteristic, workflow, using method reach purpose and effect is easy to understand, below in conjunction with concrete diagram, further set forth the present invention.
Embodiment 1
(i) prepare the aluminium titanate nanofiber presoma: take respectively 6 gram γ-AlOOH and 4 gram technical grade TiO
2Powder, first by TiO
2The powder ultrasonic wave is scattered in the sodium hydroxide solution of 5 mol/L, and 200 ℃ of airtight thermal responses are after 16 hours, then adds γ-AlOOH to continue airtight thermal response 8 hours, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(ii) prepare the pasty state composite precursor: take the non-setting aluminum oxide of 295 gram, under stirring, add in the sodium hydroxide solution of 5 mol/L, under continuing to stir, in 110 ℃, react 6 hours, the aluminium titanate nanofiber presoma that adds again preparation in (i), continue stirring reaction 6 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(iii) aftertreatment of composite precursor: by after the composite precursor drying, be incubated 120 minutes, rise to subsequently 150 minutes temperature-programmed calcinations of 1300 ℃ of sections insulations by 800 ℃ of sections, finally by ball milling, obtain the aluminium titanate nanofiber toughened alumina composite material that the toughened fiber mass content is 3%.
But prepared matrix material is sintering after 1380 ℃ are incubated 5 hours, the about 7.2MPam of the fracture toughness property of sintered compact
1/2, the about 650MPa of bending strength.
Embodiment 2
(i) prepare the aluminium titanate nanofiber presoma: take respectively 60 gram γ-AlOOH and 40 gram analytical pure TiO
2Powder, first by TiO
2The powder ultrasonic wave is scattered in the potassium hydroxide solution of 20 mol/L, and 110 ℃ of airtight thermal responses are after 8 hours, then adds γ-AlOOH to continue airtight thermal response 16 hours, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(ii) prepare the pasty state composite precursor: take 212.5 gram Alpha-aluminas, under stirring, add in the potassium hydroxide solution of 20 mol/L, under continuing to stir, in 200 ℃, react 10 hours, the aluminium titanate nanofiber presoma that adds again preparation in (i), continue stirring reaction 10 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(iii) aftertreatment of composite precursor: by after the composite precursor drying, be incubated 300 minutes, rise to subsequently 60 minutes temperature-programmed calcinations of 1000 ℃ of sections insulations by 400 ℃ of sections, finally by ball milling, obtain the aluminium titanate nanofiber toughened alumina composite material that the toughened fiber mass content is 30%.
But prepared matrix material is sintering after 1500 ℃ are incubated 2 hours, the about 8.1MPam of the fracture toughness property of sintered compact
1/2, the about 715MPa of bending strength.
Embodiment 3
(i) prepare the aluminium titanate nanofiber presoma: take respectively 30 gram γ-AlOOH and 20 gram technical grade TiO
2Powder, first by TiO
2The powder ultrasonic wave is scattered in the potassium hydroxide solution of 8 mol/L, and 130 ℃ of airtight thermal responses are after 12 hours, then adds γ-AlOOH to continue airtight thermal response 12 hours, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(ii) prepare the pasty state composite precursor: take 182 gram gama-aluminas, under stirring, add in the potassium hydroxide solution of 15 mol/L, under continuing to stir, in 180 ℃, react 8 hours, the aluminium titanate nanofiber presoma that adds again preparation in (i), continue stirring reaction 8 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(iii) aftertreatment of composite precursor: by after the composite precursor drying, be incubated 270 minutes, rise to subsequently 120 minutes temperature-programmed calcinations of 1200 ℃ of sections insulations by 500 ℃ of sections, finally by ball milling, obtain the aluminium titanate nanofiber toughened alumina composite material that the toughened fiber mass content is 20%.
But prepared matrix material is sintering after 1460 ℃ are incubated 3.5 hours, the about 8.8MPam of the fracture toughness property of sintered compact
1/2, the about 775MPa of bending strength.
Embodiment 4
(i) prepare the aluminium titanate nanofiber presoma: take respectively 18 gram γ-AlOOH and 12 gram technical grade TiO
2Powder, first by TiO
2The powder ultrasonic wave is scattered in the sodium hydroxide solution of 12 mol/L, and 150 ℃ of airtight thermal responses are after 10 hours, then adds γ-AlOOH to continue airtight thermal response 10 hours, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(ii) prepare the pasty state composite precursor: take 155 gram Alpha-aluminas, under stirring, add in the sodium hydroxide solution of 12 mol/L, under continuing to stir, in 160 ℃, react 9 hours, the aluminium titanate nanofiber presoma that adds again preparation in (i), continue stirring reaction 9 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(iii) aftertreatment of composite precursor: by after the composite precursor drying, be incubated 240 minutes, rise to subsequently 90 minutes temperature-programmed calcinations of 1100 ℃ of sections insulations by 600 ℃ of sections, finally by ball milling, obtain the aluminium titanate nanofiber toughened alumina composite material that the toughened fiber mass content is 15%.
But prepared matrix material is sintering after 1430 ℃ are incubated 4 hours, the about 9.0MPam of the fracture toughness property of sintered compact
1/2, the about 800MPa of bending strength.
Embodiment 5
(i) prepare the aluminium titanate nanofiber presoma: take respectively 15 gram γ-AlOOH and 10 gram technical grade TiO
2Powder, first by TiO
2The powder ultrasonic wave is scattered in the potassium hydroxide solution of 10 mol/L, and 180 ℃ of airtight thermal responses are after 10 hours, then adds γ-AlOOH to continue airtight thermal response 10 hours, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(ii) prepare the pasty state composite precursor: take 205 gram gama-aluminas, under stirring, add in the potassium hydroxide solution of 12 mol/L, under continuing to stir, in 130 ℃, react 7 hours, the aluminium titanate nanofiber presoma that adds again preparation in (i), continue stirring reaction 7 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(iii) aftertreatment of composite precursor: by after the composite precursor drying, be incubated 180 minutes, rise to subsequently 120 minutes temperature-programmed calcinations of 1200 ℃ of sections insulations by 700 ℃ of sections, finally by ball milling, obtain the aluminium titanate nanofiber toughened alumina composite material that the toughened fiber mass content is 10%.
But prepared matrix material is sintering after 1380 ℃ are incubated 5 hours, the about 7.8MPam of the fracture toughness property of sintered compact
1/2, the about 690MPa of bending strength.
Above demonstration and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. the preparation method of an aluminium titanate nanofiber toughened alumina composite material, is characterized in that, comprises the following steps:
(1) prepare the aluminium titanate nanofiber presoma: be respectively to take γ-AlOOH and TiO at 2: 1 by aluminium/titanium mol ratio
2Powder, first latter's ultrasonic wave is scattered in the strong base solution of 5～20mol/L concentration, airtight thermal response temperature is 110～200 ℃, add again γ-AlOOH to continue airtight thermal response 8～16 hours, temperature of reaction is 110～200 ℃, and deionized water centrifuge washing repeatedly obtains white aluminium titanate nanofiber presoma;
(2) prepare the pasty state composite precursor: take a certain amount of aluminum oxide, under agitation add in certain density hot alkaline solution, temperature is 110～200 ℃, continue stirring reaction 6～10 hours, the aluminium titanate nanofiber presoma that adds preparation in (1), continue stirring reaction 6～10 hours, finally with deionized water, repeatedly after ultrasonic, centrifuge washing, obtain the pasty state composite precursor;
(3) aftertreatment of composite precursor: by after the composite precursor drying, keeping temperature is 400～800 ℃ of insulations 60～150 minutes, by temperature-programmed calcination, 1000～1300 ℃ of sections are incubated 90～120 minutes, finally by grinding, obtain aluminium titanate nanofiber toughened alumina composite material.
2. the preparation method of a kind of aluminium titanate nanofiber toughened alumina composite material according to claim 1, is characterized in that, described step (1) strong base solution concentration 8～15mol/L.
3. the preparation method of a kind of aluminium titanate nanofiber toughened alumina composite material according to claim 1, is characterized in that, described TiO
2Powder and add γ-AlOOH after the condition of airtight thermal response: 130～180 ℃ of temperature, react 10～12 hours.
4. the preparation method of a kind of aluminium titanate nanofiber toughened alumina composite material according to claim 1, is characterized in that, 130～180 ℃ of described step (2) hot alkaline solution temperature, concentration 8～15mol/L.
5. the preparation method of a kind of aluminium titanate nanofiber toughened alumina composite material according to claim 1, it is characterized in that, two sections process conditionals of described temperature-programmed calcination are: front 500～700 ℃ of insulations of roasting 60～150 minutes, after roasting, 1100 ℃～1200 ℃ are incubated 90～120 minutes.
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| WO2009108299A1 (en) * | 2008-02-29 | 2009-09-03 | Corning Incorporated | Anisotropic porous ceramic article and manufacture thereof |
| CN101607830A (en) * | 2009-07-16 | 2009-12-23 | 安吉县杭达耐火材料有限公司 | The preparation method of a kind of fiber reinforced aluminum titanate composite material and goods |
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| US20070152364A1 (en) * | 2005-11-16 | 2007-07-05 | Bilal Zuberi | Process for extruding a porous substrate |
| WO2009108299A1 (en) * | 2008-02-29 | 2009-09-03 | Corning Incorporated | Anisotropic porous ceramic article and manufacture thereof |
| CN101607830A (en) * | 2009-07-16 | 2009-12-23 | 安吉县杭达耐火材料有限公司 | The preparation method of a kind of fiber reinforced aluminum titanate composite material and goods |
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