CN107235726A - A kind of negative thermal expansion ceramic materials A l2‑xScxMo3O12And preparation method thereof - Google Patents

A kind of negative thermal expansion ceramic materials A l2‑xScxMo3O12And preparation method thereof Download PDF

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CN107235726A
CN107235726A CN201710345736.6A CN201710345736A CN107235726A CN 107235726 A CN107235726 A CN 107235726A CN 201710345736 A CN201710345736 A CN 201710345736A CN 107235726 A CN107235726 A CN 107235726A
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thermal expansion
negative
negative thermal
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ceramic materials
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刘红飞
张义池
郑倩
张志萍
杨露
曾祥华
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Yangzhou University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped 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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide

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Abstract

The invention discloses a kind of negative thermal expansion ceramic materials A l2‑ xScxMo3O12And preparation method thereof.Wherein 0.35≤x≤0.45.Belong to inorganic non-metallic negative expansion field of functional materials, negative expansion Al2‑xScxMo3O12Ceramic material is to analyze pure Sc2O3、Al2O3And MoO3For raw material, prepared using stepwise solid phase sintering process, according to certain mol ratio by being weighed to starting oxides, batch mixing ball milling, shaping, distribution pre-burning is final is sintered at 750 800 DEG C, the oblique side's phase negative thermal expansion material Al prepared2‑xScxMo3O12Ceramics, phase free from foreign meter, compact structure has stable negative expansion performance in room temperature to its melting range.Such as Al1.6Sc0.4Mo3O12Ceramics are in room temperature within the temperature range of 700 DEG C, and its coefficient of linear thermal expansion is 2.19 × 10‑6/ K, thermal dilatometry near-linear, no phase transformation occurs, and hot expansibility is stable, with preferable negative expansion performance, while provided by the present invention prepare negative thermal expansion material Al2‑xScxMo3O12Preparation method it is relatively simple, short preparation period, cost are low, environment friendly and pollution-free, thus with preferable application prospect.

Description

A kind of negative thermal expansion ceramic materials A l2-xScxMo3O12And preparation method thereof
Technical field
The invention belongs to inorganic functional ceramic Material Field, and in particular to a kind of negative thermal expansion ceramic materials A l2- xScxMo3O12And preparation method thereof.
Background technology
With the change of temperature " expanding with heat and contract with cold " occurs for the most of materials of nature, but also has a few materials to occur " heat Contracting cold expanding " phenomenon, this kind of material is referred to as negative thermal expansion material.Negative thermal expansion material is in Aero-Space, microelectronics, optics and micro- There is huge potential application foreground in the fields such as machinery.With the development of science and technology, high-accuracy device will to the accurate dimension of itself More and more higher is sought, this function to device is also most important.And it is often that device is tired that thermal coefficient of expansion, which mismatches the thermal stress produced, The main cause that labor, hydraulic performance decline, failure are even broken and come off.Device size is often because of the change of operating ambient temperature Change, cause the performance of device unstable or even fail.Negative thermal expansion material is provided such issues that be found to be solution May.
Negative thermal expansion material mainly has three below series：AM2O7Series（A=Zr, Hf; M=V, P）；AM2O8Series（A =Zr, Hf; M=W, Mo）；A2M3O12Series（A=Sc, Yb, In, Y, etc.; M=W, Mo）.Although by years of researches With exploration, it was found that some new negative thermal expansion materials, but all there is certain deficiency in its negative expansion performance.Such as AM2O8System There is phase transformation in row negative thermal expansion material, can cause the mutation of its hot expansibility in the range of its negative expansion relevant temperature； AM2O7The negative expansion of the negative thermal expansion material of series just shows as negative expansion more than 102 DEG C.A2M3O12（A=Sc, Yb, In, Y, etc.; M=W, Mo）Serial negative thermal expansion material is numerous, and is rapidly developed in the last few years with its excellent performance. Research shows：The hot expansibility of the series material depends primarily on A cations, and different A cations can cause A2M3O12 Different thermal expansion characters are presented in series material.When A is Y3+, Ho3+, Tm3+, Er3+, Yb3+, Lu3+During element, the negative heat in the part is swollen The easy moisture absorption in atmosphere of swollen material, at room temperature thermal coefficient of expansion show as just, as temperature is raised, losing after the crystallization water, ability table It is now excellent negative heat expansion characteristics, meeting moisture absorption again, loses negative heat expansion characteristics after temperature is reduced to room temperature.This easy moisture absorption Thermal expansion character caused by defect, which changes, to be difficult to overcome, and hinders it to move towards practical application.But when A is In3+, Fe3+, Cr3+, Al3+During element, the part negative thermal expansion material then non-hygroscopic deliquescence.The tungstates and molybdate of this five kinds of elements include monocline Mutually with tiltedly two kinds of crystal structures of square phase, positive thermal expansion is presented in wherein monoclinic phase, tiltedly square that negative expansion is mutually presented.With the change of temperature Change, the transformation of the opposite tiltedly square phase of monocline can occur for the series material.Wherein Al2Mo3O12From monoclinic phase（Positive expansion）To oblique side Phase（Negative expansion）Phase transition temperature be 200 DEG C.It is this more than room temperature due to the change of phase transition temperature, the thermal expansion brought Performance is by just to negative change, being applied to detrimental effect, by ion doping, by Al2Mo3O12Transformation temperature move to Below room temperature, a kind of New Negative Thermal Expansion Material is prepared, there is important Research Significance and practical value.
The content of the invention
It is an object of the invention to provide one kind, with stablizing, negative expansion performance, synthesis cost are low, make more than room temperature The simple New Negative Thermal Expansion Material Al of standby technique2-xScxMo3O12And preparation method thereof,
Realizing the technical solution of above-mentioned purpose is：
A kind of negative thermal expansion ceramic materials A l2-xScxMo3O12, the material is with Sc2O3、Al2O3And MoO3For raw material, consolidated using substep Phase method is synthetically prepared, wherein 0.35≤x≤0.45.
A kind of above-mentioned negative thermal expansion material Al2-xScxMo3O12Preparation method, comprise the following steps：
（1）Synthesize Al2-xScxMo3O12Raw material to analyze pure Sc2O3、Al2O3And MoO3Powder, 180 are placed in before weighing by raw material DEG C baking oven in dry 24~36 h, according to metering than weighing Sc2O3、Al2O3And MoO3Raw material, ball milling 3-6 after being mixed in water H, the raw material after ball milling mixing is dried in 120~150 DEG C of baking ovens, then sinters 6-12h at 600~750 DEG C；
（2）By step（1）The powder of middle pre-burning grinds 1-2h with agate mortar, adds the poly- second for accounting for presoma gross mass 2~4% Enol, grinding 20-40min makes to be well mixed, the then cold moudling tabletting under 100-150MPa；
（3）By step（2）Material after middle tabletting, is placed in stove in 500 DEG C of 0.5~1h of dumping, is burnt in 750-1100 DEG C of high temperature Negative thermal expansion ceramic materials A l is obtained after 12~24h of knot, furnace cooling2-xScxMo3O12。
A kind of above-mentioned negative expansion Al2-xScxMo3O12In the preparation method of ceramics, step（1）In, raw material Sc2O3、Al2O3 And MoO3Mol ratio be x: 2-x: 6, 0.35≤x≤0.45.
A kind of above-mentioned negative expansion Al2-xScxMo3O12The preparation method of ceramics, step（1）Raw material Sc during middle ball milling2O3、 Al2O3And MoO3Quality：Agate ball：The mass ratio of water is 1:4:2.
A kind of above-mentioned negative expansion Al2-xScxMo3O12In the preparation method of ceramics, step（2）During middle cold moudling, The two-stage is divided progressively to be pressurized, respectively the min of pressurize 2 at 1/2 and final molding pressure of final molding pressure.
A kind of above-mentioned negative expansion Al2-xScxMo3O12In the preparation method of ceramics, step（1）With（3）Described in be sintered in Sintered in batch-type furnace, heating rate is 7 DEG C/min.
Using X-ray diffractometer（XRD）Phase structure is carried out to sample to analyze；Using SEM （SEM）Observation prepares the cross-section morphology of ceramics sample；Using thermomechanical analyzer（TMA）Negative expansion is carried out to ceramics sample It can characterize.
Compared with prior art, its remarkable advantage is the present invention：With raw material Sc2O3、Al2O3And MoO3Mol ratio be 0.2: 0.8 :Exemplified by 3, the negative thermal expansion material Al prepared to the present invention1.6Sc0.4Mo3O12Specific performance, which carries out detection and analysis, to be sent out It is existing：It is tiltedly square phase Al to prepare sample1.6Sc0.4Mo3O12Ceramics, form solid solution, and peak free from foreign meter, ceramic structure is fine and close, and should Material has stable and good negative expansion performance in room temperature and the above, and its thermal dilatometry is in room temperature to 700 DEG C of temperature In the range of be almost straight line, illustrate that its hot expansibility is stable.In test temperature is interval, its thermal linear expansion coefficient is up to- 2.19×10-6/K.And preparation technology is simple, sintering temperature is low, and cost is low, environment friendly and pollution-free, is with a wide range of applications And application prospect.
Brief description of the drawings
Fig. 1 is negative thermal expansion material Al of the present invention1.6Sc0.4Mo3O12XRD spectrum.
Fig. 2 is negative thermal expansion material Al of the present invention1.6Sc0.4Mo3O12The section SEM spectrum of ceramics.
Fig. 3 is negative thermal expansion material Al of the present invention1.6Sc0.4Mo3O12The thermal dilatometry of ceramics.
Embodiment
This experiment is raw materials used to be： Sc2O3（Analysis is pure）、Al2O3（Analysis is pure）And MoO3（Analysis is pure）.
Solid phase method prepares negative thermal expansion material Al2-xScxMo3O12, wherein 0.35≤x≤0.45, with reference to example pair The present invention is further described.
Embodiment 1
（1）Synthesize Al1.6Sc0.4Mo3O12Raw material to analyze pure Sc2O3、Al2O3And MoO3Powder, weighs according to metering ratio Sc2O3:Al2O3:MoO3=0.2：0.8：3, raw material is placed in 180 DEG C of baking oven before weighing and dries 24 h, ball after being mixed in water 3 h are ground, the raw material after ball milling mixing is dried in 120 DEG C of baking ovens, then 6 h are sintered at 740 DEG C；
（2）By step（1）The powder of middle pre-burning grinds 20 min with agate mortar, adds the poly- second for accounting for presoma gross mass 2% Enol, 40 min of grinding make to be well mixed, the then cold moudling tabletting under 100 MPa；
（3）By step（2）Material after middle tabletting, is placed in stove in 500 DEG C of h of dumping 1, in 800 DEG C of h of high temperature sintering 18, Negative thermal expansion ceramic materials A l is obtained after furnace cooling1.6Sc0.4Mo3O12。
Embodiment 2
（1）Synthesize Al1.62Sc0.38Mo3O12Raw material to analyze pure Sc2O3、Al2O3And MoO3Raw material, is placed in by powder before weighing 28 h are dried in 180 DEG C of baking oven, according to metering than the Sc that weighs2O3:Al2O3:MoO3=0.19：0.81：3, ball after being mixed in water 5 h are ground, raw material after ball milling mixing is dried in 130 DEG C of baking ovens, then 8 h are sintered at 710 DEG C；
（2）By step（1）The powder of middle pre-burning grinds 10 min with agate mortar, adds and accounts for the poly- of presoma gross mass 2.5% Vinyl alcohol, 30 min of grinding make to be well mixed, the then cold moudling tabletting under 125 MPa；
（3）By step（2）Material after middle tabletting, is placed in stove in 500 DEG C of h of dumping 1.5, in 770 DEG C of h of high temperature sintering 20, Negative thermal expansion ceramic materials A l is obtained after furnace cooling1.62Sc0.38Mo3O12。
Embodiment 3
（1）Synthesize Al1.54Sc0.46Mo3O12Raw material to analyze pure Sc2O3、Al2O3And MoO3Raw material, is placed in by powder before weighing 36 h are dried in 180 DEG C of baking oven, according to metering than the Sc that weighs2O3:Al2O3:MoO3=0.23：0.77：3, ball after being mixed in water 6 h are ground, raw material after ball milling mixing is dried in 150 DEG C of baking ovens, then 7 h are sintered at 730 DEG C；
（2）By step（1）The powder of middle pre-burning grinds 15 min with agate mortar, adds the poly- second for accounting for presoma gross mass 3% Enol, 20 min of grinding make to be well mixed, the then cold moudling tabletting under 150 MPa；
（3）By step（2）Material after middle tabletting, is placed in stove in 500 DEG C of h of dumping 2, in 750 DEG C of high temperature sintering 12h, with Negative thermal expansion ceramic materials A l is obtained after stove cooling1.54Sc0.46Mo3O12。
Lower Fig. 1 is to prepare Al1.6Sc0.4Mo3O12The XRD spectrum of ceramics, the Al prepared as we know from the figure1.6Sc0.4Mo3O12For tiltedly side Phase, with higher degree, peak free from foreign meter.Fig. 2 is negative thermal expansion material Al1.6Sc0.4Mo3O12SEM spectrum, can be with from figure Find out and prepare ceramics sample compact structure；Fig. 3 is to prepare negative thermal expansion material Al1.6Sc0.4Mo3O12Thermal dilatometry, show The material has a good negative expansion performance, its thermal dilatometry in room temperature to being almost straight line within the temperature range of 700 DEG C, Illustrate that its hot expansibility is stable.In test temperature is interval, its thermal linear expansion coefficient is up to -2.19 × 10-6/K。

Claims (6)

1. a kind of negative thermal expansion ceramic materials A l2-xScxMo3O12, it is characterised in that the material is with Sc2O3、Al2O3And MoO3For original Material, it is synthetically prepared using solid state reaction, wherein 0.35≤x≤0.45.
2. the negative thermal expansion ceramic materials A l described in a kind of claim 12-xScxMo3O12Preparation method, it is characterised in that bag Include following steps：
（1）With high-purity Sc2O3、Al2O3And MoO3For raw material, raw material is placed in 180 DEG C of baking oven before weighing and dries 24-36 H, raw material is weighed according to certain mol proportion, the h of ball milling 3~6 after being mixed in water, by the raw material after ball milling mixing in 120-150 Dried in DEG C baking oven, then sinter 6~8 h at 500~550 DEG C, 20~50 min of grinding are removed after furnace cooling, are cold-pressed into After type 6~8 h are sintered at 710~740 DEG C；
（2）By step（1）The sample of middle pre-burning grinds 10~20 min with agate mortar, and addition accounts for presoma gross mass 2~3% Polyvinyl alcohol, grinding 20~40 min make to be well mixed, the then cold moudling tabletting under 100-150 MPa；
（3）By step（2）Material after middle tabletting, is placed in stove in 500 DEG C of h of dumping 1~2, is burnt in 750~800 DEG C of high temperature The h of knot 18~24, obtains negative thermal expansion ceramic materials A l after furnace cooling2-xScxMo3O12。
3. the negative thermal expansion ceramic materials A l described in claim 22-xScxMo3O12Preparation method, it is characterised in that step（1） In, raw material Sc2O3、Al2O3And MoO3Mol ratio be x：2-x：6,0.35≤x≤0.45.
4. the negative thermal expansion ceramic materials A l described in claim 22-xScxMo3O12Preparation method, it is characterised in that step（1） Raw material Sc during middle ball milling2O3、Al2O3And MoO3Quality：Agate ball：The mass ratio of water is 1:4:2.
5. the negative thermal expansion ceramic materials A l described in claim 22-xScxMo3O12Preparation method, it is characterised in that step（2） During middle cold moudling, a point two-stage is progressively pressurized, the pressurize at 1/2 and final molding pressure of final molding pressure respectively 2 min。
6. the negative thermal expansion ceramic materials A l described in claim 22-xScxMo3O12Preparation method, it is characterised in that step（1） With（3）Described in be sintered in Muffle furnace sinter, heating rate be 7 DEG C/min.
CN201710345736.6A 2017-05-17 2017-05-17 A kind of negative thermal expansion ceramic materials A l2‑xScxMo3O12And preparation method thereof Pending CN107235726A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113149646A (en) * 2021-04-22 2021-07-23 河南大学 High-entropy low-thermal-expansion ceramic material and sintering synthesis method thereof
CN115448717A (en) * 2022-09-27 2022-12-09 厦门稀土材料研究所 Rare earth-based molybdate high-entropy negative thermal expansion ceramic material and preparation method thereof
CN115594490A (en) * 2022-08-25 2023-01-13 山东大学（Cn） Low-thermal-expansion alumina-based ceramic cutter material and preparation process thereof

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Publication number Priority date Publication date Assignee Title
CN105254297A (en) * 2015-09-29 2016-01-20 扬州大学 Negative thermal expansion ceramic material ScxIn2-xW3O12 and preparation method thereof

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张伟等: "Al2Mo3O12的制备及其负热膨胀性能研究", 《硅酸盐通报》 *
马健: "A(2-x)B(x)M3O12(A=Er,In;B=La,Sc;M=W,Mo)系负热膨胀材料的制备和性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113149646A (en) * 2021-04-22 2021-07-23 河南大学 High-entropy low-thermal-expansion ceramic material and sintering synthesis method thereof
CN115594490A (en) * 2022-08-25 2023-01-13 山东大学（Cn） Low-thermal-expansion alumina-based ceramic cutter material and preparation process thereof
CN115594490B (en) * 2022-08-25 2023-04-14 山东大学 Low-thermal-expansion alumina-based ceramic cutter material and preparation process thereof
CN115448717A (en) * 2022-09-27 2022-12-09 厦门稀土材料研究所 Rare earth-based molybdate high-entropy negative thermal expansion ceramic material and preparation method thereof

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Application publication date: 20171010