CN104178652B - Nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramic material and preparation method thereof - Google Patents
Nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramic material and preparation method thereof Download PDFInfo
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- CN104178652B CN104178652B CN201410395983.3A CN201410395983A CN104178652B CN 104178652 B CN104178652 B CN 104178652B CN 201410395983 A CN201410395983 A CN 201410395983A CN 104178652 B CN104178652 B CN 104178652B
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Abstract
The present invention relates to a kind of nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramic material and preparation method thereof, with 3% mole of Y2O3Stable cubic polycrystal zirconia and 3Y-TZP are matrix, with nickel cobalt (alloy) Ni1-xCox(wherein x=0.25～0.75) is magnetic second-phase, and the raw materials quality degree of this alloy is 1～40%。The present invention is with the stable cubic polycrystal zirconia of yttrium for matrix, by adding nickel cobalt (alloy) magnetic phase, adopts reducing atmosphere powder process and the two-stage process of inert atmosphere sintering, it is thus achieved that have the mechanics of excellence and the composite ceramics of magnetic performance。Improve the magnetic performance of alloy by adjusting cobalt content in the alloy, meanwhile, improve the mechanical property of material by adjusting alloy addition in zirconia base, finally obtain the composite having excellent mechanical and magnetic performance concurrently。
Description
Technical field
The invention belongs to a kind of ceramic composition being feature with composition, particularly to a kind of nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramic material and preparation method thereof。
Background technology
At present, the miniaturization of material devices, integrated and multifunction become the demand of Material Field development。For Inorganic Non-metallic Materials, the structure-function integration of ceramic material can expand its application in high-technology field, and this has been subjected to showing great attention to of scientific research personnel。Wherein, mixing in structural ceramics using magnetic-particle as second-phase, form the multiphase composite of " magnetic-particle dispersion phase/structural ceramics matrix ", it is while taking into account structural behaviour, possesses electromagnetic shielding, prevents interference or inhale wave energy。This kind of composite can be widely used in the fields such as space flight military project, mechanical industry, electronics, metallurgy, the energy。
Zirconia ceramics has the mechanical property of excellence, experiment with theoretical research become focus theme already, and, it is used widely as structural ceramics, wear resistant corrosion resistant pottery, high-temperature electrolysis material etc. in the industrial circle such as pottery, machinery, chemical industry, electronics, the energy。Wherein, the cubic polycrystal zirconia material of stabilized with yttrium oxide, is the one in toughened zirconia ceramics。Its sintering temperature is low, contains the tetragonal zircite phase of high-load, play transformation toughening effect, show splendid mechanical property inside when room temperature。If adding magnetic-particle dispersion phase in zirconia base, it will while taking into account its excellent mechanical performance, increase the character of its function aspects, widen its application, it is achieved structure-function integration。
Nickel metal/zirconia composite ceramics is using magnetic metal nickel as second-phase, is dispersed in the middle of zirconia base。When nickel metal dispersion is in the middle of cubic zirconia, it is possible to be applied to the anode material of fuel cell。This is because cubic zirconia is good ion conductor, nickel is good electronic conductor, and this anode material can be prepared by the method for reduction-oxidation nickel/zirconia composite ceramics and obtain enough porositys, is conducive to carrier to conduct。When nickel metal dispersion is in the middle of tetragonal zircite, owing to nickel and zirconic coefficient of thermal expansion mismatch degree are only small, causing that the residual stress of compound system is only small, this advantage ensure that mixing nickel will not have a strong impact on the mechanical property of composite ceramics。Simultaneously as scattered nickel metallic particles has magnetostrictive effect, when there being stress to put on composite ceramics, overall magnetic property changes, and this kind of effect can apply to the design of mechanics sensor。
At present for the research of nickel metal/tetragonal zircite this system of composite ceramics, mode [the H.Kondo adopting hot pressed sintering in the document reported more, T.Sekino, Y.-H.Choa, etal.Mechanicalandmagneticpropertiesofnickel-dispersedte tragonalzirconiananocomposites [J] .JournalofNanoscienceandNanotechnology, 2002,2 [5], 485-490；Li Peng, Zhou Wancheng, the .Ni/ZrO such as Li Yuqin2Compound Material Engineering and Dielectric Properties [J]. Rare Metals Materials and engineering, 2008, 37 [11], 1934-1937], also there is the bibliographical information mixing gas [S.Lopez-Esteban containing hydrogen, T.Rodriguez-Suarez, F.Esteban-Beteg ó n, etal.Mechanicalpropertiesandinterfacesofzirconia/nickeli nmicro-andnanocomposites [J] .Journalofmaterialsscience, 2006, 41, 5194 5199] and the method [H.Kondo of pure hydrogen high temperature sintering, T.Sekino, N.Tanaka, etal.Mechanicalandmagneticpropertiesofnovelyttria-stabil izedtetragonalzirconia/ninanocompositepreparedbythemodif iedinternalreductionmethod [J] .JournaloftheAmericanCeramicSociety, 2005, 88 [6], 1468-1473]。But the equipment cost of hot pressed sintering is higher, being not suitable for producing in enormous quantities, the safety issue of applied at elevated temperature hydrogen can not be ignored simultaneously。
The present invention is after summarizing the method for above pertinent literature report, improve, nickel magnetic is carried out mutually cobalt doped, form nickel cobalt (alloy), nickel cobalt (alloy) and zirconic mixed powder is made by low temperature hydrogen method of reducing, biscuit sinters out composite ceramics afterwards under an inert atmosphere, and the method is safer, and can extend to large-scale production。
Summary of the invention
The purpose of the present invention, it is on the basis of existing technology, with the stable cubic polycrystal zirconia of yttrium for matrix, by adding the nickel cobalt (alloy) magnetic phase of certain content, adopt powder reducing process and the two-stage process of inertia sintering, it is thus achieved that there is the mechanics of excellence and the composite ceramics of magnetic performance。Improve the magnetic performance of alloy by adjusting cobalt content in the alloy, meanwhile, improve the mechanical property of material by adjusting alloy addition in zirconia base, finally obtain the composite having excellent mechanical and magnetic performance concurrently。
The present invention is achieved by following technical solution。
A kind of nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics, its raw material components and content are as follows:
With 3% mole of Y2O3Stable cubic polycrystal zirconia and 3Y-TZP are matrix, with nickel cobalt (alloy) Ni1-xCoxFor magnetic second-phase, wherein x=0.25～0.75, the mass percentage content of this alloy raw material is 1～40%；
This nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics preparation method, specifically comprises the following steps that
(1) according to Ni1-xCoxThe stoichiometric proportion of alloy and the mass fraction of nickel cobalt (alloy), NiO, CoO, 3Y-TZP powder is mixed, with deionized water for medium ball milling 6 hours, drying, grinding, be put in the tube furnace under flowing hydrogen atmosphere and be reduced into nickel cobalt (alloy) zirconium oxide mixed-powder when being incubated 1.5 hours for 700 DEG C after sieving；
(2) mixed-powder that step (1) is obtained, after 100MPa is dry-pressing formed, 200MPa isostatic pressed is adopted to process again, biscuit is put in vacuum carbon tube furnace under an argon atmosphere through 1300～1500 DEG C of sintering, it is incubated 2 hours, obtains the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。
Described nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics, it is characterised in that described nickel cobalt (alloy) Ni1-xCox, x therein is 0.5。
Described nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics, it is characterised in that the addition of described step (2) nickel cobalt (alloy) is 10%, sintering temperature is 1400 DEG C。
The present invention is with the cubic polycrystal zirconia of stabilized with yttrium oxide for matrix, using nickel cobalt (alloy) as second-phase, adopt conventional inertia sintering method to prepare composite ceramics, make the sintering temperature sintering temperature lower than pure zirconia of composite ceramics, be conducive to fine grain to be formed, optimize microstructure。Meanwhile, obtained composite can coordinate the magnetic performance of the excellent mechanical property of zirconium oxide and nickel cobalt (alloy)。The method safe preparation process, equipment cost is relatively low, is suitable for industrialized mass, and production and application for structure-function integration material lay the foundation。
Accompanying drawing explanation
Fig. 1 is hysteresis curve figure under comparative example 1 room temperature；
Fig. 2 is the partial enlarged drawing of Fig. 1；
Fig. 3 is hysteresis curve figure under embodiment 2 room temperature；
Fig. 4 is the partial enlarged drawing of Fig. 3。
Detailed description of the invention
The nickel cobalt (alloy) of the present invention/cubic polycrystal zirconia composite ceramics, its raw material components and content are as follows:
With 3% mole of Y2O3Stable cubic polycrystal zirconia and 3Y-TZP are matrix, with nickel cobalt (alloy) Ni1-xCoxFor magnetic second-phase, wherein x=0.25～0.75, the mass percentage content of this alloy raw material is 1～40%；
The preparation method of nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics, specific as follows:
According to Ni1-xCoxThe stoichiometric proportion of alloy and the mass fraction of nickel cobalt (alloy), NiO, CoO, 3Y-TZP powder is mixed, with deionized water for medium in planetary ball mill with the rotating speed ball milling 6 hours of 800 revs/min, the slurry drying after ball milling, grinding, crossing 80 mesh sieves, now powder is light grey。Being put in afterwards in tube furnace, in being incubated 1.5 hours for 700 DEG C when, low temperature is reduced into nickel cobalt (alloy) zirconium oxide mixed-powder under a hydrogen atmosphere, and powder presents Dark grey。
The mixed-powder that reduction is obtained; after 100MPa dry-pressing; adopt 200MPa cold isostatic compaction again; the biscuit of molding is put in vacuum carbon tube furnace under argon atmosphere and sinters 2 hours through 1300～1500 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。
Again the nickel cobalt (alloy) obtained/cubic polycrystal zirconia composite ceramics is adopted conventional method, carry out mechanical property and magnetic performance test。
Comparative example 1
Learnt from else's experience reduction after nickel by powder; join in 3Y-TZP; the mass percentage content of nickel is 10%, is put in vacuum carbon tube furnace by base substrate under argon shield and sinters 2 hours through 1400 DEG C, obtains the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 95.2%, and bending strength reaches 596MPa, and fracture toughness is 5.2MPam1/2, can read according to the hysteresis curve of Fig. 1 and Fig. 2, in composite, the saturation magnetic field intensity of metallic nickel reaches 44.3emu/g, and coercive field is 2.2Oe。From this comparative example 1 it can be seen that when not mixing cobalt, composite has just reached basic sintering, and properties also has considerable room for improvement。
Embodiment 1
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.25 (i.e. x=0.25) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 10% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1400 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 96.5%, and bending strength reaches 650MPa, and fracture toughness reaches 5.5MPam1/2, the saturation magnetic field intensity 80.9emu/g of alloy in composite, coercive field is 4.3Oe。The present embodiment compares with comparative example 1 it can be seen that when strontium doping amount is 0.25, the mechanical property of material improves, and saturation magnetic field intensity improves, and mixes cobalt element formation alloy and not only increases mechanical property, and improves the magnetic of composite。
Embodiment 2
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.5 (i.e. x=0.5) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 10% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1400 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 97.9%, bending strength 801MPa, fracture toughness 5.7MPam1/2, can read according to the hysteresis curve of Fig. 3 and Fig. 4, the saturation magnetic field intensity 95.7emu/g of alloy, coercive field 16.8Oe in composite。
Embodiment 3
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.75 (i.e. x=0.75) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 10% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1400 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 96.9%, bending strength 581MPa, fracture toughness 5.3MPam1/2, in composite, the saturation magnetic field intensity of alloy reaches 95.7emu/g, coercive field 12.9Oe。According to embodiment 2 and the present embodiment it can be seen that the incorporation of cobalt is too much, although can improve magnetic, but also reducing the mechanical property of material, therefore cobalt can not mix too much。
Embodiment 4
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.5 (i.e. x=0.5) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 10% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1300 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 90.8%, bending strength 418MPa, fracture toughness 3.9MPam1/2, in composite, the saturation magnetic field intensity of alloy is 96.1emu/g, coercive field 10.1Oe。This example demonstrates that, sintering temperature is too low, and composite does not sinter, and the mechanical property of material is not good。
Embodiment 5
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.5 (i.e. x=0.5) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 10% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1500 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 96.8%, bending strength 711MPa, fracture toughness 4.8MPam1/2, in composite, the saturation magnetic field intensity of alloy is 94.2emu/g, coercive field 14.3Oe。This example demonstrates that, sintering temperature is too high, pottery internal grain undue growth, have impact on the mechanical property of material。In conjunction with the situation of above-described embodiment, illustrating that sintering temperature can not be too low too high, optimal sintering temperature is 1400 DEG C。
Embodiment 6
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.5 (i.e. x=0.5) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 5% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1400 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Its relative density reaches 98.8%, bending strength 818MPa, fracture toughness 7.7MPam1/2, the saturation magnetic field intensity 46.8emu/g of alloy, coercive field 6.3Oe in composite。This example demonstrates that, when the addition of magnetic phase is 5%, the relative density of material is significantly high, bending strength and fracture toughness are also higher, but owing to magnetic phase addition is a half, saturation magnetic field intensity and coercive field decline only about half of, illustrate that the addition of magnetic phase can not be too low。
Embodiment 7
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.5 (i.e. x=0.5) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 1% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1400 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Testing through mechanical property and magnetic performance, composite ceramics has good mechanics and magnetic performance。
Embodiment 8
Learnt from else's experience the nickel cobalt (alloy) powder that doping ratio is 0.5 (i.e. x=0.5) of cobalt after reduction; join in 3Y-TZP; the mass percentage content of nickel cobalt (alloy) is the 40% of 3Y-TZP; base substrate is put in vacuum carbon tube furnace under argon shield and sinters 2 hours through 1400 DEG C, obtain the higher nickel cobalt (alloy) of consistency/cubic polycrystal zirconia composite ceramics。Testing through mechanical property and magnetic performance, composite ceramics has good mechanics and magnetic performance。
Nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramic material that the present invention proposes and preparation method thereof, having passed through embodiment to be described, content as herein described substantially can be modified or suitably change realizing the present invention with combination by person skilled in without departing from present disclosure, spirit and scope。Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are considered as including in the spirit of the present invention, scope and content。
Claims (3)
1. nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics, its raw material components and content are as follows:
With 3% mole of Y2O3Stable cubic polycrystal zirconia and 3Y-TZP are matrix, with nickel cobalt (alloy) Ni1-xCoxFor magnetic second-phase, wherein x=0.25～0.75, the mass percentage content of this alloy raw material is 1～40%；
This nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics preparation method, specifically comprises the following steps that
(1) according to Ni1-xCoxThe stoichiometric proportion of alloy and the mass fraction of nickel cobalt (alloy), NiO, CoO, 3Y-TZP powder is mixed, with deionized water for medium ball milling 6 hours, drying, grinding, be put in the tube furnace under flowing hydrogen atmosphere and be reduced into nickel cobalt (alloy) zirconium oxide mixed-powder when being incubated 1.5 hours for 700 DEG C after sieving；
(2) mixed-powder that step (1) is obtained, after 100MPa is dry-pressing formed, 200MPa isostatic pressed is adopted to process again, biscuit is put in vacuum carbon tube furnace under an argon atmosphere through 1300～1500 DEG C of sintering, it is incubated 2 hours, obtains nickel cobalt (alloy)/cubic polycrystal zirconia composite ceramics。
2. nickel cobalt (alloy) according to claim 1/cubic polycrystal zirconia composite ceramics, it is characterised in that described nickel cobalt (alloy) Ni1-xCox, x therein is 0.5。
3. nickel cobalt (alloy) according to claim 1/cubic polycrystal zirconia composite ceramics, it is characterised in that the mass fraction of described step (2) nickel cobalt (alloy) is 10%, sintering temperature is 1400 DEG C。
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| US4885266A (en) * | 1982-06-01 | 1989-12-05 | Commonwealth Scientific And Industrial Research Organization | Zirconia ceramic materials and method for making same |
| CN101063187A (en) * | 2007-05-23 | 2007-10-31 | 济南钢铁股份有限公司 | Preparation method of ceramic-metal composite material |
| CN101591741A (en) * | 2009-06-19 | 2009-12-02 | 中南大学 | A kind of is the ceramic matric composite and the metal phase adding method thereof of metallographic phase with the copper alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4885266A (en) * | 1982-06-01 | 1989-12-05 | Commonwealth Scientific And Industrial Research Organization | Zirconia ceramic materials and method for making same |
| CN101063187A (en) * | 2007-05-23 | 2007-10-31 | 济南钢铁股份有限公司 | Preparation method of ceramic-metal composite material |
| CN101591741A (en) * | 2009-06-19 | 2009-12-02 | 中南大学 | A kind of is the ceramic matric composite and the metal phase adding method thereof of metallographic phase with the copper alloy |
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