CN106927840A - The preparation that anti-thermal shock diphase ceramic material and the ceramics based on the material are let slip a remark - Google Patents

The preparation that anti-thermal shock diphase ceramic material and the ceramics based on the material are let slip a remark Download PDF

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CN106927840A
CN106927840A CN201710217529.2A CN201710217529A CN106927840A CN 106927840 A CN106927840 A CN 106927840A CN 201710217529 A CN201710217529 A CN 201710217529A CN 106927840 A CN106927840 A CN 106927840A
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thermal shock
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ceramic material
ceramics
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CN106927840B (en
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谢建林
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Shanghai Material Research Institute Co ltd
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Shanghai Institute of Materials
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Abstract

The present invention relates to anti-thermal shock diphase ceramic material and the preparation let slip a remark of the ceramics based on the material.By the raw material containing following mass fractions：Al2O369.01%~76.00%, ZrO217.01%~24.13%, SiO25.29%~5.97%, MgO 0.05%~0.89% or Y2O30.05%~1.33%, TiO20.05%~0.19%, bonding agent 0.5%~1.5% mixes；Through 90~220MPa isostatic pressings, in 1630~1680 DEG C of temperature range high temperature sinterings, anti-thermal shock diphase ceramic material is obtained and lets slip a remark.Described anti-thermal shock diphase ceramic material contains alpha-aluminium oxide phase, zirconium oxide phase and mullite phase, it is adaptable to is made anti-thermal shock complex phase ceramic and lets slip a remark.Compared with prior art, the anti-thermal shock diphase ceramic material that the present invention is provided, due to containing a considerable amount of relatively low thermel expansion coefficient mullite phases and erosion-resisting characteristics is good, intensity is high zirconium oxide, being corroded with high temperature resistant, molten-metal-resistant, and thermal shock resistance it is superior the features such as；Overcome traditional ceramics to let slip a remark shortcoming, be suitable for high temperature alloy powder by atomization.

Description

The preparation that anti-thermal shock diphase ceramic material and the ceramics based on the material are let slip a remark
Technical field
The present invention relates to a kind of ceramic material, more particularly, to anti-thermal shock diphase ceramic material and the ceramics based on the material The preparation let slip a remark.
Background technology
Superalloy powder is the important source material of contemporary metal increasing material manufacturing complex component, and it is prepared by atomization that ceramics are let slip a remark One of critical component of superalloy powder device.Traditional ceramics are let slip a remark, in built-in 1500 DEG C of motlten metals, outside high speed gas Flow the extreme environment of injection, it is easy to crack or " bursting ", or because high temperature resistant, the erosion of resistance to metal bath are poor, cause The superalloy powder balling-up that is made of atomization is poor, and can cause the danger that motlten metal quickly flows out from crack.
Chinese patent CN106242565A discloses a kind of wear-resisting ZrO2-Al2O3Complex phase ceramic particle and preparation method thereof and Using belonging to ceramic composite preparing technical field, wear-resisting ZrO2-Al2O3The mass fraction of complex phase ceramic particle constituent For：10%~90% stable ZrO2And 10%~90% Al2O3；Melted using electric smelting, water-cooled is prepared into rough surface, grain Footpath is the high-wearing feature ZrO of 0.5~7mm2-Al2O3Complex phase ceramic particle, production efficiency is high, stable performance, and by wear-resisting ZrO2- Al2O3Complex phase ceramic particle is applied to prepare the reinforcement of steel-based composite material, can significantly increase composite-material abrasive.But It is ZrO in the patent2-Al2O3Complex phase ceramic particle mainly improves material wear-resistant performance, without reference to improvement ceramic material Thermal shock resistance；The electric smelting more than 1800 DEG C is needed to melt, prepared by water-cooled, its preparation process high energy consumption；And only relate to 0.5~ The ZrO of 7mm2-Al2O3Wear-resistant ceramic particle, anti-thermal shock block is prepared without reference to by matrix of the material.
Chinese patent CN101209925B discloses a kind of aluminum oxide titanium white multiple phase fine ceramics material that improves and bends by force The method of degree and fracture toughness, solves existing Al2O3/TiO2The bending strength of complex phase ceramic, fracture toughness and hardness performance are low Problem.The step of the method is：In ball mill with deionized water do medium by fine alumina and nano titanium oxide powder, The PVA mixed synthesis uniform sizing material of modifying agent, binding agent；Then it is spray-dried and granulates again；Hot place then is carried out to gained powder Reason；Pre-molding is carried out through the powder of Overheating Treatment；Blank is sintered after carrying out cold isostatic compaction.The above method is realized finely The low temperature Fast Sintering of ceramics in ceramic material preparation process, hence it is evident that the cost of production is reduced, while improve the curved of product Qu Qiangdu, fracture toughness and hardness.The patent mainly improves existing Al2O3/TiO2The bending strength of complex phase ceramic, fracture are tough Property and the low problem of hardness performance, and have the advantages that low temperature Fast Sintering, while without reference to the anti-thermal shock for improving ceramic material Performance and high-temperature anti-corrosion performance, particularly in 1000~1500 DEG C of materials of sintering, resistance to elevated temperatures not enough, is not suitable for height Temperature alloy powder by atomization is let slip a remark；And primary raw material uses nano aluminium oxide and nano titania, relatively costly.
The content of the invention
The purpose of the present invention is exactly to provide a kind of anti-thermal shock complex phase for the defect for overcoming above-mentioned prior art to exist to make pottery The preparation that ceramic material and the ceramics based on the material are let slip a remark.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of anti-thermal shock diphase ceramic material, is made up of the raw material containing following mass fractions：Al2O369.01%~ 76.00%th, ZrO217.01%~24.13%, SiO25.29%~5.97%, MgO 0.05%~0.89% or Y2O3 0.05%~1.33%, TiO20.05%~0.19%, bonding agent 0.5%~1.5%.Described bonding agent is PVA, methyl One or more in cellulose or dextrin.Described bonding agent is one or more in PVA, methylcellulose or dextrin.
Al in raw material2O3A part forms resistant to elevated temperatures corundum phase discrete phase, the SiO contained in remainder and raw material2 The mullite phase of material is formed, less than described addition, it will cause the heat-resisting quantity and mechanical strength of material to decline；Al2O3 Addition is excessive, and the corundum phase/mullite ratio in composite is too high, it will cause the thermal shock resistance of material to decline.
17.01%~the 24.13%ZrO added in raw material2Composite toughening host material is formed with the aluminum oxide in material, Play the mechanical performance and thermal shock resistance of raising material, and the high-temperature anti-corrosion performance of composite can be improved.
The a small amount of MgO or Y added in raw material2O3、TiO2Mainly play sintering aid and Zirconia-stabilized dose.
Further, described anti-thermal shock diphase ceramic material contains alpha-oxidation aluminium phase (corundum phase), zirconium oxide phase and not Carry out stone phase.Zirconium oxide phase and corundum are discrete phase in composite diphase material, with high temperature resistant, corrosion resistant feature.Zirconium oxide phase It is evenly distributed in corundum discrete phase, in sintering process, is cooled down with temperature, tetragonal phase zirconium oxide is partly or entirely transformed into list Oblique zirconium oxide, and with certain volumetric expansion, in Al2O3And ZrO2Grain boundaries produce compression, play the work of composite toughening With.Mullite is Al2O3And SiO2The mineral for generating at high temperature, crystal is fine acicular.The coefficient of expansion (25~1000 DEG C) 5.3 ×10- 6/ DEG C, with good thermal shock resistance, in material of the invention, acicular mullite is interspersed to be distributed between discrete phase, Further increase the thermal shock resistance that complex phase ceramic of the invention is let slip a remark.
The preparation method of described anti-thermal shock diphase ceramic material, comprises the following steps：
1) by the raw material containing following mass fractions：Al2O369.01%~76.00%, ZrO217.01%~24.13%, SiO25.29%~5.97%, MgO 0.05%~0.89% or Y2O30.05%~1.33%, TiO20.05%~ 0.19%th, bonding agent 0.5%~1.5% adds water mixing, and amount of water accounts for the 4-6% of raw material and water gross weight；
2) above-mentioned blending constituent is burnt through 90~220MPa isostatic pressings in 1630~1680 DEG C of temperature range high temperature Knot, with stove Temperature fall, is obtained anti-thermal shock diphase ceramic material.
The present invention also provides the ceramics based on the anti-thermal shock diphase ceramic material and lets slip a remark.
The preparation method that described ceramics are let slip a remark, comprises the following steps：
1) by the raw material containing following mass fractions：Al2O369.01%~76.00%, ZrO217.01%~24.13%, SiO25.29%~5.97%, MgO 0.05%~0.89% or Y2O30.05%~1.33%, TiO20.05%~ 0.19%th, bonding agent 0.5%~1.5% adds water mixing, and amount of water accounts for the 4-6% of raw material and water gross weight；
2) by above-mentioned blending constituent through 90~220MPa isostatic pressings to let slip a remark, it is high in 1630~1680 DEG C of temperature ranges Temperature sintering, is obtained anti-thermal shock complex phase ceramic and lets slip a remark.
Described ceramics are let slip a remark and are mainly used in high temperature alloy powder by atomization.
The present invention is in optimized selection by raw material with raw material proportioning, and on the basis of raw material selection, optimizes high temperature The technique of sintering so that material contains alpha-oxidation aluminium phase, zirconium oxide phase and mullite phase.The temperature of high temperature sintering of the present invention Had a major impact for the performance of material with the time, if bad result of burning till, temperature mistake can be produced in other temperature sintering Low or soaking time is too short, can produce underburnt, the mechanical performance reduction of material；Temperature is too high or soaking time is long, can produce Sintering warpage.
Described anti-thermal shock diphase ceramic material contains alpha-oxidation aluminium phase, zirconium oxide phase and mullite phase, with resistance to height Temperature, molten-metal-resistant corrode, and thermal shock resistance it is superior the features such as, be particularly suited for being made anti-thermal shock complex phase ceramic and let slip a remark, Therefore, let slip a remark the invention provides a kind of ceramics based on anti-thermal shock diphase ceramic material, overcome that traditional ceramics lets slip a remark lacks Point, described anti-thermal shock complex phase ceramic is let slip a remark for high temperature alloy powder by atomization.
Compared with prior art, the beneficial effects of the invention are as follows：The anti-thermal shock diphase ceramic material of offer, due to containing suitable The zirconium oxide that relatively low thermel expansion coefficient mullite phase and erosion-resisting characteristics are good, intensity is high of quantity, with high temperature resistant, molten-metal-resistant Corrode, and thermal shock resistance it is superior the features such as；Overcome traditional ceramics to let slip a remark shortcoming, be applicable for high temperature alloy powder by atomization.
Brief description of the drawings
Fig. 1：Anti-thermal shock complex phase ceramic is let slip a remark X-Ray collection of illustrative plates and analysis result；
Fig. 2：Let slip a remark using ceramics of the present invention the superalloy powder SEM photograph being made.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Weigh in proportion containing oxidation yttrium partially stabilized zirconium oxide, aluminum oxide, silica, raw titanium oxide material：The change of raw material Learning constituent mass fraction is, Al2O369.02%th, ZrO223.63%th, SiO25.80%th, Y2O31.33%th, TiO2 0.19%th, PVA bonding agents 0.5%；5% water is added, raw material is mixed, sieved, granulate, be then then added in mould, then Through 220MPa isostatic pressings, at a temperature of 1630 DEG C being incubated 3h burns till, that is, anti-thermal shock composite ceramics is obtained and lets slip a remark blank, then It is machined, its appearance and size is reached atomization and prepare superalloy powder device matching requirements.Gained composite ceramic material Strata behavior result is shown in Fig. 1, and 1 is shown in Table using result and related data.
Embodiment 2
Weigh in proportion containing magnesia partial stabilized zirconium oxide, aluminum oxide, silica, raw titanium oxide material.The change of raw material Learning constituent mass fraction is, Al2O376%th, ZrO217.36%th, SiO25.97%th, MgO 0.62%, TiO20.05%th, dextrin Bonding agent 1.5%；5% water is added, raw material is mixed, sieved, granulate, be then then added in mould, then it is quiet through 90MPa etc. Molded, at a temperature of 1670 DEG C being incubated 2.5h burns till, that is, anti-thermal shock composite ceramics is obtained and lets slip a remark blank, then machined, Its appearance and size is reached atomization and prepare superalloy powder device matching requirements.1 is shown in Table using result and related data.
Embodiment 3
Weigh in proportion containing magnesia partial stabilized zirconium oxide, aluminum oxide, silica, raw titanium oxide material：The chemical group of raw material Point mass fraction is：Al2O374.02%th, ZrO219.30%th, SiO25.84%th, MgO 0.71%, TiO20.08%th, methyl is fine The plain bonding agent 0.8% of dimension；5% water is added, raw material is mixed, sieved, granulate, be then then added in mould, then through 160MPa Isostatic pressing, at a temperature of 1670 DEG C being incubated 2.5h burns till, that is, anti-thermal shock composite ceramics is obtained and lets slip a remark blank, then add through machine Work, makes its appearance and size reach atomization and prepares superalloy powder device matching requirements.1 is shown in Table using result and related data.
Embodiment 4
Oxidation yttrium partially stabilized zirconium oxide, aluminum oxide, silica, raw titanium oxide material are weighed in proportion：The chemistry of raw material Constituent mass fraction is, Al2O374.55%th, ZrO218.95%th, SiO25.29%th, Y2O30 1.07%, MgO 0.05%, TiO20.08%th, PVA bonding agents 0.6%；5% water is added, raw material is mixed, sieved, granulate, be then then added to mould In, then through 100MPa isostatic pressings, at a temperature of 1660 DEG C being incubated 3h burns till, that is, anti-thermal shock composite ceramics is obtained and lets slip a remark hair Base, then it is machined, its appearance and size is reached atomization and prepare superalloy powder device matching requirements.Using result and phase Close data and be shown in Table 1.
Embodiment 5
The yttrium partially stabilized zirconium oxide of oxidation and magnesia_partially stabilized zirconia, aluminum oxide, oxidation are weighed in proportion Silicon, raw titanium oxide material：The chemical constituent mass fraction of raw material is, Al2O374.63%th, ZrO218.91%th, SiO25.50%th, Y2O30.53%th, MgO 0.35%, TiO20.08%th, PVA bonding agents 0.6%；5% water is added, raw material is mixed, sieving, Granulation, is then then added in mould, then through 100MPa isostatic pressings, insulation 3h burns till at a temperature of 1660 DEG C, that is, make Anti-thermal shock composite ceramics is let slip a remark blank, it is then machined, its appearance and size is reached atomization and is prepared superalloy powder and fill Put matching requirements.1 is shown in Table using result and related data.
Embodiment 6
Magnesia_partially stabilized zirconia, aluminum oxide, silica, raw titanium oxide material are weighed in proportion：The chemistry of raw material Constituent mass fraction is, Al2O369.02%th, ZrO224.13%th, SiO25.80%th, MgO 0.89%, TiO20.12%th, PVA bonding agents 0.5%, add 5% water, and raw material is mixed, and sieve, granulate, and are then then added in mould, then through 100MPa etc. Hydrostatic profile, at a temperature of 1660 DEG C being incubated 3h burns till, that is, anti-thermal shock composite ceramics is obtained and lets slip a remark blank, then machined, Its appearance and size is reached atomization and prepare superalloy powder device matching requirements.1 is shown in Table using result and related data.
The anti-thermal shock composite ceramics of table 1 is let slip a remark material analysis and application result
Anti-thermal shock composite ceramics prepared by Example 1-6 is let slip a remark, and preparing superalloy powder device in atomization loads onto, Contacted with 1500 DEG C of high temperature melting alloys in upper end and inner side, under 10~70 DEG C of high speed winds cool conditions in lower surface and lower end outside, Applied and examined.Result shows that embodiment 1-6 composite ceramicses are let slip a remark with high temperature melting alloys contact surface and melting do not occur Metal attack, overall structure stabilization, also occurs without any cracking, slag-off phenomenon.Anti-thermal shock composite ceramics leakage prepared by embodiment 1 Superalloy powder sphericity ＞ 0.9 (see Fig. 2) prepared by mouth atomization, anti-thermal shock composite ceramics prepared by embodiment 2-6 is let slip a remark It is atomized the superalloy powder sphericity for preparing also all ＞ 0.9.
Above example shows that composite ceramics of the invention is let slip a remark stable performance, and good thermal shock, refractoriness is high, atomization system Standby superalloy powder good sphericity, purity is high, it is adaptable to 3D printing.Corroded with high temperature resistant, molten-metal-resistant, Yi Jikang The features such as thermal shock performance is superior；The shortcoming that traditional ceramics are let slip a remark is overcome, is suitable for high temperature alloy powder by atomization, there is wide Application prospect.
The above-mentioned description to embodiment is to be understood that and use invention for ease of those skilled in the art. Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability Field technique personnel announcement of the invention, does not depart from improvement that scope made and modification all should be of the invention Within protection domain.

Claims (9)

1. a kind of anti-thermal shock diphase ceramic material, it is characterised in that be made up of the raw material containing following mass fractions：Al2O3 69.01%~76.00%, ZrO217.01%~24.13%, SiO25.29%~5.97%, MgO 0.05%~0.89% Or Y2O30.05%~1.33%, TiO20.05%~0.19%, bonding agent 0.5%~1.5%.
2. a kind of anti-thermal shock diphase ceramic material according to claim 1, it is characterised in that described bonding agent be PVA, One or more in methylcellulose or dextrin.
3. a kind of anti-thermal shock diphase ceramic material according to claim 1, it is characterised in that described anti-thermal shock complex phase pottery Ceramic material contains alpha-oxidation aluminium phase, zirconium oxide phase and mullite phase.
4. the preparation method of a kind of anti-thermal shock diphase ceramic material as any one of claim 1-3, it is characterised in that Comprise the following steps：
1) by the raw material containing following mass fractions：Al2O369.01%~76.00%, ZrO217.01%~24.13%, SiO2 5.29%~5.97%, MgO 0.05%~0.89% or Y2O30.05%~1.33%, TiO20.05%~0.19%, tie Mixture 0.5%~1.5% adds water mixing；
2) by above-mentioned blending constituent through 90~220MPa isostatic pressings, in 1630~1680 DEG C of temperature range high temperature sinterings, system Obtain anti-thermal shock diphase ceramic material.
5. the preparation method of anti-thermal shock diphase ceramic material according to claim 4, it is characterised in that step 1) in add water Amount accounts for the 4-6% of raw material and water gross weight.
6. a kind of ceramics based on anti-thermal shock diphase ceramic material any one of claim 1-3 are let slip a remark.
7. the preparation method that a kind of ceramics as claimed in claim 6 are let slip a remark, it is characterised in that comprise the following steps：
1) by the raw material containing following mass fractions：Al2O369.01%~76.00%, ZrO217.01%~24.13%, SiO2 5.29%~5.97%, MgO 0.05%~0.89% or Y2O30.05%~1.33%, TiO20.05%~0.19%, tie Mixture 0.5%~1.5% adds water mixing；
2) by above-mentioned blending constituent through 90~220MPa isostatic pressings to let slip a remark, burnt in 1630~1680 DEG C of temperature range high temperature Knot, is obtained anti-thermal shock complex phase ceramic and lets slip a remark.
8. the preparation method that ceramics according to claim 7 are let slip a remark, it is characterised in that step 1) in amount of water account for raw material with The 4-6% of water gross weight.
9. the application that a kind of ceramics as claimed in claim 6 are let slip a remark, it is characterised in that described ceramics are let slip a remark and closed for high temperature Golden powder by atomization.
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CN113956024A (en) * 2021-11-29 2022-01-21 上海材料研究所 Thermal shock resistant composite ceramic material

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CN1162580A (en) * 1996-12-23 1997-10-22 唐山市燕山产业有限公司 Wear resistant sintered zirconium boule composite and manufacture thereof
CN101300207A (en) * 2005-09-26 2008-11-05 圣戈班欧洲设计研究中心 Sintered refractory product exhibiting enhanced thermal shock resistance

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Publication number Priority date Publication date Assignee Title
CN1162580A (en) * 1996-12-23 1997-10-22 唐山市燕山产业有限公司 Wear resistant sintered zirconium boule composite and manufacture thereof
CN101300207A (en) * 2005-09-26 2008-11-05 圣戈班欧洲设计研究中心 Sintered refractory product exhibiting enhanced thermal shock resistance

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113956024A (en) * 2021-11-29 2022-01-21 上海材料研究所 Thermal shock resistant composite ceramic material
CN113956024B (en) * 2021-11-29 2023-02-28 上海材料研究所 Thermal shock resistant composite ceramic material

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