CN106278260A - A kind of preparation method of pair of rare earth ion tantalates high-temperature ceramics - Google Patents

A kind of preparation method of pair of rare earth ion tantalates high-temperature ceramics Download PDF

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CN106278260A
CN106278260A CN201610597143.4A CN201610597143A CN106278260A CN 106278260 A CN106278260 A CN 106278260A CN 201610597143 A CN201610597143 A CN 201610597143A CN 106278260 A CN106278260 A CN 106278260A
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rare earth
earth ion
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pair
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冯晶
汪俊
周荣
蒋业华
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Kunming University of Science and Technology
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    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The present invention relates to the preparation method of a kind of pair of rare earth ion tantalates high-temperature ceramics, belong to high-temperature ceramics preparing technical field.The molecular formula of of the present invention pair of rare earth ion tantalates high-temperature ceramics is (REa/REb=Y,La,Nd,Sm,Eu,Gd,Dy,Er,Yb;REaAnd REbCan not be same rare earth element).Raw materials used for rare earth oxide with tantalum oxide, weigh raw material in proportion, load weighted raw material is placed in ball grinder together with dehydrated alcohol and mixes, seal and be placed on ball milling on planetary ball mill, can mix homogeneously, carry out first sintering sintering after mixed powder is dried, is sieved.Will cooling take out after sample be ground, ball milling, be dried, sieve that it is real to be placed on mould inner pressure, then carry out double sintering.Present invention process purity is high, and impurity content is low, and product preparation cost is low, is suitable for batch production, and purpose product is expected to as novel fire resistant, antioxidation, wear-resistant ceramic material.

Description

A kind of preparation method of pair of rare earth ion tantalates high-temperature ceramics
Technical field
The present invention relates to the preparation method of a kind of pair of rare earth ion tantalates high-temperature ceramics, belong to high-temperature ceramics technology of preparing Field.
Background technology
From the point of view of the high-temperature ceramic materials of research in the past, it is likely to be suited for the main aerobic of ceramic material of high-temp heat barrier coating Change the zirconium oxide of yttrium/ceria stabilized, zirconium oxide/aluminium oxide, zirconic acid lanthanum, strontium zirconate, zirconium phosphate, Zirconium orthosilicate., zirconia titanate, Mo Lai Stone, rare earth oxide potteries etc., wherein zirconium oxide (YSZ) overall performance of stabilized with yttrium oxide is best, is to be widely used at present Ceramic heat-barrier coating.But thermal barrier coating ceramic material (YSZ) is only capable of steady operation in the environment of less than 1200 DEG C, works as work As temperature more than 1200 DEG C time, YSZ ceramic material is susceptible to phase transformation, and thermal coefficient of expansion and matrix material become not match that, Result in the formation of high-temperature ceramic materials crackle, cause thermal barrier coating ceramic material to come off inefficacy the most at last, be difficult to meet The requirement that before thermal engine, fuel gas inlet temperature improves constantly.Therefore, in the urgent need to seek one can long-term stable operation Novel thermal barrier coating ceramic material under 1200 DEG C of conditions above.
In previous literature, rare earth tantalate is studied and more concentrates on its structure and its photoluminescent property, king Fu Zhi et al. has synthesized (Lu1-xREx)TaO4Fluorophor (Lu=Y, Gd or La;RE=Tb or Eu;X=0.05~0.10);Li Bo Et al. use high-temperature solid phase reaction method synthesized M ' type YTaO4:Gd, Eu, reported Gd in detail3+、Eu3+The coactivated M ' of ion Type YTaO4Luminosity, have studied the energy transport phenomenon between luminescence process mesostroma, sensitizer and activator.China Patent CN 103923654A reports a kind of neodymium ytterbium codope rare earth positive tantalates up-conversion luminescent material, has chemical general formula MeTaO4:xNd3+, yYb3+. wherein, Me is the one in yttrium, lanthanum, gadolinium or lutecium element.And double rare earth ions prepared by the present invention Tantalates high-temperature ceramics is mainly used in heat barrier coat material, and its preparation method is simple, and it has good calorifics and mechanical property Energy.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of pair of rare earth ion tantalates high-temperature ceramics, specifically include with Lower step:
(1) by load weighted rare earth oxide and tantalum oxide mix homogeneously, carry out after mixed powder is dried, sieves First sintering;
(2) after stove is cold, sample being ground, ball milling, is dried, sieves, the powder after sieving is placed in mould inner pressure Real, obtain double rare earth ion tantalates high-temperature ceramics after then carrying out double sinteringDescribed REa/REbFor One in Y, La, Nd, Sm, Eu, Gd, Dy, Er, Yb, REaAnd REbIt can not be same rare earth element;
Described
Preferably, in step (2), in mechanical milling process, the rotating speed of ball mill is 300r/min~500r/min, and Ball-milling Time is 60~180min.
Preferably, in step of the present invention (2), the temperature of dry run is 60~80 DEG C, and drying time is 10~24 hours.
Preferably, of the present invention sieving crosses 300 mesh sieves for powder.
Preferably, in step of the present invention (1), the temperature of first sintering is 1500~1700 DEG C, and calcination time is 2~10 Hour.
Preferably, in step of the present invention (2) during mixed-powder compacting, dwell pressure is 8~12MPa, and the dwell time is 30 ~60min.
Preferably, in step of the present invention (2), double sintering temperature is 1500~1700 DEG C, and calcination time is 2~10 hours.
Prepared by the preparation method that another object of the present invention is to provide described double rare earth ion tantalates high-temperature ceramicss The double rare earth ion tantalates high-temperature ceramicss obtained.
The invention has the beneficial effects as follows:
(1) can mix homogeneously after ball mill mixes powder so that it is can composition reaction when calcining.
(2) relatively low ((5~8.5) × 10 of double rare earth ion tantalates at high temperature thermal coefficient of expansions obtained by–7K-1)。
(3) the double rare earth ion tantalates obtained by have good high high-temp stability, are expected to as novel high temperature pottery Ceramic material.
(4) the double rare earth ion tantalates obtained by have preferable mechanical property and calorifics compared with zirconium dioxide Matter.
Accompanying drawing explanation
Fig. 1 is the (Eu prepared by embodiment 1 technical scheme0.6Gd0.4TaO4) scanning electron microscope (SEM) photograph of high-temperature ceramics block (SEM collection of illustrative plates);
Fig. 2 is the (Eu prepared by embodiment 1 technical scheme0.6Gd0.4TaO4) and stabilized with yttrium oxide zirconium oxide (YSZ) The collection of illustrative plates of thermal conductivity.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail, but protection scope of the present invention is not limited to institute State content.
Embodiment 1
A kind of high temperature resistant, antioxidation, wear-resistant pair of rare earth ion tantalates high-temperature ceramic materials described in the present embodiment (Eu0.6Gd0.4TaO4) and preparation method thereof, specifically include following steps:
Weigh europium oxide 5.2788g, Gadolinia. 3.6249g, tantalum oxide 11.0473g, in dehydrated alcohol after mixing, put Ball milling (rotating speed of ball mill is 400r/min, and Ball-milling Time is 120min), the mixing good by ball milling in planetary ball mill Thing crosses 300 mesh sieves, by its pre-burning 5 hours at 1650 DEG C after being dried 16 hours at 74 DEG C.
After first time calcining raw materials, compound is ground to molecule (10~30 μm), is again dissolved in anhydrous second In alcohol, it is placed in ball milling in planetary ball mill (rotating speed of ball mill is 400r/min, and Ball-milling Time is 120min), ball milling is good Mixture be dried at 74 DEG C after 16 hours and cross 300 mesh sieves, then with mould, compressing (dwell pressure is 11MPa, pressurize Time is 40min), compressing after, it is calcined 5 hours at 1650 DEG C, is cooled to room temperature, i.e. obtain required fine and close Block double rare earth ion tantalates (Eu0.6Gd0.4TaO4) high-temperature ceramics, reaction equation is 0.3Eu2O3+0.2Gd2O3+ 0.5Ta2O5=Eu0.6Gd0.4TaO4
Double rare earth ion tantalates (Eu that the present embodiment prepares0.6Gd0.4TaO4) high-temperature ceramics purity height, pattern Good, SEM collection of illustrative plates as shown in Figure 1.As in figure 2 it is shown, (the Eu obtained by this experiment0.6Gd0.4TaO4) with currently used 8YSZ (2~3.5W.m-1k-1) compare, (Eu0.6Gd0.4TaO4) there is relatively low thermal conductivity, show (Eu0.6Gd0.4TaO4) in high-temperature hot Barrier coating use has preferable thermal property.In terms of mechanics, relatively low hardness number (648HV) can stop residual effectively Residue stress and the propagation of crackle, improve appearance toughness and the fracture toughness of high-temp heat barrier coating.Record through test (Eu0.6Gd0.4TaO4) mean thermal expansion coefficients be about 8.5 × 10–7K-1
Embodiment 2
A kind of novel fire resistant, antioxidation, wear-resistant pair of rare earth ion tantalates high-temperature ceramic materials described in the present embodiment (La0.75Sm0.25TaO4) and preparation method thereof, specifically include following steps:
Weigh lanthana 4.8871g, Disamarium trioxide 1.7435g, tantalum oxide 8.8378g, in dehydrated alcohol after mixing, be placed in Ball milling (rotating speed of ball mill is 350r/min, and Ball-milling Time is 140min), the mixture good by ball milling in planetary ball mill 300 mesh sieves are crossed, by its pre-burning 8 hours at 1550 DEG C after being dried 20 hours at 65 DEG C.
After first time calcining raw materials, compound is ground to molecule (10~30 μm), is again dissolved in anhydrous second In alcohol, it is placed in ball milling in planetary ball mill (rotating speed of ball mill is 350r/min, and Ball-milling Time is 140min), ball milling is good Mixture be dried at 65 DEG C after 20 hours and cross 300 mesh sieves, then with mould, compressing (dwell pressure is 9MPa, pressurize Time is 55min), compressing after, it is calcined 8 hours at 1550 DEG C, is cooled to room temperature, i.e. obtain required fine and close block The double rare earth ion tantalates (La of shape0.75Sm0.25TaO4) high-temperature ceramics, reaction equation is 0.375La2O3+0.125Sm2O3+ 0.5Ta2O5=La0.75Sm0.25TaO4
Embodiment 3
A kind of novel fire resistant, antioxidation, wear-resistant pair of rare earth ion tantalates high-temperature ceramic materials described in the present embodiment (Y0.5Dy0.5TaO4) and preparation method thereof, specifically include following steps:
Weigh yittrium oxide 5.6452g, dysprosia 9.3249g, tantalum oxide 22.0946g, in dehydrated alcohol after mixing, put Ball milling (rotating speed of ball mill is 300r/min, and Ball-milling Time is 180min), the mixing good by ball milling in planetary ball mill Thing crosses 300 mesh sieves, by its pre-burning 10 hours at 1650 DEG C after being dried 24 hours at 60 DEG C.
After first time calcining raw materials, compound is ground to molecule (10~30 μm), is again dissolved in anhydrous second In alcohol, it is placed in ball milling in planetary ball mill (rotating speed of ball mill is 300r/min, and Ball-milling Time is 180min), ball milling is good Mixture be dried at 60 DEG C after 24 hours and cross 300 mesh sieves, then with mould, compressing (dwell pressure is 8MPa, pressurize Time is 60min), compressing after, it is calcined 10 hours at 1650 DEG C, is cooled to room temperature, i.e. obtain required fine and close Block double rare earth ion tantalates (Y0.5Dy0.5TaO4) high-temperature ceramics, reaction equation is 0.25Y2O3+0.25Dy2O3+ 0.5Ta2O5=Y0.5Dy0.5TaO4
Embodiment 4
A kind of novel fire resistant, antioxidation, wear-resistant pair of rare earth ion tantalates high-temperature ceramics tantalic acid described in the present embodiment Salt (Er0.8Yb0.2TaO4) ceramic material and preparation method thereof, specifically include following steps:
Weigh Erbia 7.6503g, ytterbium oxide 1.9703g, tantalum oxide 11.0473g, in dehydrated alcohol after mixing, put Ball milling (rotating speed of ball mill is 500r/min, and Ball-milling Time is 60min), the mixture good by ball milling in planetary ball mill 300 mesh sieves are crossed, by its pre-burning 2 hours at 1700 DEG C after being dried 10 hours at 80 DEG C.
After first time calcining raw materials, compound is ground to molecule (10~30 μm), is again dissolved in anhydrous second In alcohol, it is placed in ball milling in planetary ball mill (rotating speed of ball mill is 500r/min, and Ball-milling Time is 60min), ball milling is good Mixture be dried at 80 DEG C after 10 hours and cross 300 mesh sieves, then with mould, compressing (dwell pressure is 12MPa, pressurize Time is 30min), compressing after, it is calcined 2 hours at 1700 DEG C, is cooled to room temperature, i.e. obtain required fine and close block The double rare earth ion tantalates (Er of shape0.8Yb0.2TaO4) high-temperature ceramics, reaction equation is 0.4Er2O3+0.1Yb2O3+0.5Ta2O5 =Er0.8Yb0.2TaO4

Claims (8)

1. the preparation method of double rare earth ion tantalates high-temperature ceramicss, it is characterised in that specifically include following steps:
(1) by load weighted rare earth oxide and tantalum oxide mix homogeneously, first after mixed powder is dried, is sieved, is carried out Secondary sintering;
(2) after stove is cold, sample being ground, ball milling, is dried, sieves, it is real that the powder after sieving is placed in mould inner pressure, so After carry out double sintering after obtain double rare earth ion tantalates high-temperature ceramics;Described REa/REbFor Y, La, One in Nd, Sm, Eu, Gd, Dy, Er, Yb, and REaAnd REbFor different rare earth elements;
Described:
The preparation method of the most according to claim 1 pair of rare earth ion tantalates high-temperature ceramics, it is characterised in that: step (2) in, in mechanical milling process, the rotating speed of ball mill is 300r/min~500r/min, and Ball-milling Time is 60~180min.
The preparation method of the most according to claim 1 pair of rare earth ion tantalates high-temperature ceramics, it is characterised in that: step (2) in, the temperature of dry run is 60~80 DEG C, and drying time is 10~24 hours.
The preparation method of the most according to claim 1 pair of rare earth ion tantalates high-temperature ceramics, it is characterised in that: the most sieved In journey, powder crosses 300 mesh sieves.
The preparation method of the most according to claim 1 pair of rare earth ion tantalates high-temperature ceramics, it is characterised in that: step (1) in, the temperature of first sintering is 1500~1700 DEG C, and calcination time is 2~10 hours.
The preparation method of the most according to claim 1 pair of rare earth ion tantalates high-temperature ceramics, it is characterised in that: step (2), in during mixed-powder compacting, dwell pressure is 8~12 MPa, and the dwell time is 30~60min.
The preparation method of the most according to claim 1 pair of rare earth ion tantalates high-temperature ceramics, it is characterised in that: step (2) in, double sintering temperature is 1500~1700 DEG C, and calcination time is 2~10 hours.
8. one kind by the preparation method of the double rare earth ion tantalates high-temperature ceramicss described in claim 1 to 8 any claim The double rare earth ion tantalates high-temperature ceramicss prepared.
CN201610597143.4A 2016-07-27 2016-07-27 A kind of preparation method of pair of rare earth ion tantalates high-temperature ceramics Pending CN106278260A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107585787A (en) * 2017-08-30 2018-01-16 昆明工匠涂层科技有限公司 Rare earth ion tantalates of Sm Eu Dy tri- and preparation method and application
CN107662947A (en) * 2017-08-30 2018-02-06 昆明工匠涂层科技有限公司 Rare earth ion tantalates of Sm Eu Gd tri- and preparation method and application
CN107698255A (en) * 2017-08-30 2018-02-16 昆明工匠涂层科技有限公司 Rare earth ion tantalates of Eu Gd Dy tri- and preparation method and application
CN109836155A (en) * 2019-01-18 2019-06-04 昆明理工大学 A kind of double rare earth tantalate solid solution refractory ceramics of densification ferroelasticity and preparation method thereof
CN110002871A (en) * 2019-04-26 2019-07-12 昆明理工大学 A kind of two-phase rare earth tantalate ceramics and preparation method thereof
CN110002872A (en) * 2019-04-26 2019-07-12 昆明理工大学 A kind of rare earth tantalic acid ytterbium ceramics and preparation method thereof of anti-low melting point oxide corrosion
CN110002870A (en) * 2019-04-26 2019-07-12 昆明理工大学 A kind of rare earth tantalate ceramics and preparation method thereof of anti-low melting point oxide corrosion
CN110078507A (en) * 2019-06-18 2019-08-02 昆明理工大学 A kind of high entropy rare earth toughening tantalates ceramics and preparation method thereof
CN110759733A (en) * 2019-11-19 2020-02-07 湘潭大学 Y0.5Dy0.5Ta0.5Nb0.5O4Tantalum ceramic material and preparation method thereof
CN111138191A (en) * 2019-12-27 2020-05-12 江苏师范大学 Eu (Eu)3+Ion activated tantalate fluorescent ceramic and synthesis method and application thereof
CN113603140A (en) * 2021-08-31 2021-11-05 陕西天璇涂层科技有限公司 Method for preparing double rare earth tantalate hollow sphere powder by centrifugal spray granulation method
CN114956813A (en) * 2022-05-11 2022-08-30 中钢集团洛阳耐火材料研究院有限公司 Y 0.5 Gd 0.5 TaO 4 Preparation method of nano powder

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CN105777118A (en) * 2016-02-19 2016-07-20 昆明理工大学 Lanthanide rare-earth tantalite high-temperature ceramic and preparation method thereof

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CN101269960A (en) * 2008-04-30 2008-09-24 哈尔滨工业大学 Composite rare earth zirconate thermal barrier coating ceramic material and preparation method thereof
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Cited By (17)

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CN107662947B (en) * 2017-08-30 2019-09-10 昆明工匠涂层科技有限公司 Tri- rare earth ion tantalates of Sm-Eu-Gd and the preparation method and application thereof
CN107662947A (en) * 2017-08-30 2018-02-06 昆明工匠涂层科技有限公司 Rare earth ion tantalates of Sm Eu Gd tri- and preparation method and application
CN107698255A (en) * 2017-08-30 2018-02-16 昆明工匠涂层科技有限公司 Rare earth ion tantalates of Eu Gd Dy tri- and preparation method and application
CN107585787A (en) * 2017-08-30 2018-01-16 昆明工匠涂层科技有限公司 Rare earth ion tantalates of Sm Eu Dy tri- and preparation method and application
CN107698255B (en) * 2017-08-30 2020-12-08 昆明工匠涂层科技有限公司 Eu-Gd-Dy three rare earth ion tantalate and preparation method and application thereof
CN109836155A (en) * 2019-01-18 2019-06-04 昆明理工大学 A kind of double rare earth tantalate solid solution refractory ceramics of densification ferroelasticity and preparation method thereof
CN110002871A (en) * 2019-04-26 2019-07-12 昆明理工大学 A kind of two-phase rare earth tantalate ceramics and preparation method thereof
CN110002870A (en) * 2019-04-26 2019-07-12 昆明理工大学 A kind of rare earth tantalate ceramics and preparation method thereof of anti-low melting point oxide corrosion
CN110002872A (en) * 2019-04-26 2019-07-12 昆明理工大学 A kind of rare earth tantalic acid ytterbium ceramics and preparation method thereof of anti-low melting point oxide corrosion
CN110078507A (en) * 2019-06-18 2019-08-02 昆明理工大学 A kind of high entropy rare earth toughening tantalates ceramics and preparation method thereof
CN110078507B (en) * 2019-06-18 2020-12-18 昆明理工大学 High-entropy rare earth toughened tantalate ceramic and preparation method thereof
CN110759733A (en) * 2019-11-19 2020-02-07 湘潭大学 Y0.5Dy0.5Ta0.5Nb0.5O4Tantalum ceramic material and preparation method thereof
CN110759733B (en) * 2019-11-19 2022-05-31 湘潭大学 Y0.5Dy0.5Ta0.5Nb0.5O4Tantalum ceramic material and preparation method thereof
CN111138191A (en) * 2019-12-27 2020-05-12 江苏师范大学 Eu (Eu)3+Ion activated tantalate fluorescent ceramic and synthesis method and application thereof
CN111138191B (en) * 2019-12-27 2022-03-22 江苏师范大学 Eu (Eu)3+Ion activated tantalate fluorescent ceramic and synthesis method and application thereof
CN113603140A (en) * 2021-08-31 2021-11-05 陕西天璇涂层科技有限公司 Method for preparing double rare earth tantalate hollow sphere powder by centrifugal spray granulation method
CN114956813A (en) * 2022-05-11 2022-08-30 中钢集团洛阳耐火材料研究院有限公司 Y 0.5 Gd 0.5 TaO 4 Preparation method of nano powder

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