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WO2002022521A1 - Ceramiques a dilatation thermique negative isotrope et processus de fabrication - Google Patents

Ceramiques a dilatation thermique negative isotrope et processus de fabrication Download PDF

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Publication number
WO2002022521A1
WO2002022521A1 PCT/US2000/025487 US0025487W WO0222521A1 WO 2002022521 A1 WO2002022521 A1 WO 2002022521A1 US 0025487 W US0025487 W US 0025487W WO 0222521 A1 WO0222521 A1 WO 0222521A1
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phase
powder
thermal expansion
composition according
group
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English (en)
Inventor
Debra Anne Fleming
David Wilfried Johnson
Glen Robert Kowach
Paul Joseph Lemaire
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Nokia of America Corp
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Lucent Technologies Inc
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Priority to JP2002526722A priority Critical patent/JP2004509048A/ja
Priority to KR1020027006231A priority patent/KR20020063575A/ko
Priority to PCT/US2000/025487 priority patent/WO2002022521A1/fr
Publication of WO2002022521A1 publication Critical patent/WO2002022521A1/fr
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/01—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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/01—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
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02—Optical fibres with cladding with or without a coating
    • G02B6/02057—Optical fibres with cladding with or without a coating comprising gratings
    • G02B6/02076—Refractive index modulation gratings, e.g. Bragg gratings
    • G02B6/02171—Refractive index modulation gratings, e.g. Bragg gratings characterised by means for compensating environmentally induced changes
    • G02B6/02176—Refractive index modulation gratings, e.g. Bragg gratings characterised by means for compensating environmentally induced changes due to temperature fluctuations
    • G02B6/0218—Refractive index modulation gratings, e.g. Bragg gratings characterised by means for compensating environmentally induced changes due to temperature fluctuations using mounting means, e.g. by using a combination of materials having different thermal expansion coefficients

Definitions

  • This invention pertains to isotropic, negative thermal expansion ceramics, and to a process for preparing isotropic, negative thermal expansion ceramics which may, for instance, be used in temperature compensating grating packages.
  • ⁇ fiber is the thermal expansion of the fiber grating (for instance, 0.55 x 10 "6 °C " J )
  • A is the temperature sensitivity of the unpackaged grating (e.g., 0.0115 nm °C -1 for a particular 1550 nm grating)
  • P e is the photoelastic constant (typically 0.22)
  • ⁇ nom is the nominal grating wavelength ( ⁇ 1550 nm in many cases) .
  • CTE thermal expansion coefficient
  • a package material will still be beneficial even if its thermal expansion is not exactly equal to the ideal value. For the above assumptions a factor of about 20 improvement in temperature sensitivity would be achieved if the package material's thermal expansion coefficient were within 0.47 x 10 "6 °C ⁇ 1 of the ideal value. Such improvement in thermal stability of a fiber grating would be of commercial importance.
  • ZrW 2 0 e is metastable at room temperature, with the lower limit of stability being at 1105 ⁇ 3 °C, below which ZrW 2 0 8 decomposes into Zr0 2 and 0 3 .
  • Zr 2 0 8 has a relatively high and isotropic negative coefficient of thermal expansion (CTE) over an extensive range of temperatures that includes room temperature.
  • CTE isotropic negative coefficient of thermal expansion
  • the CTE is substantially constant from near absolute zero temperature to 150 °C, with a value near -10 x 10 "6 °C _1 .
  • the material exhibits an order-disorder transition at 150 °C, after which the CTE drops to -5 x 10 ⁇ 6 °C -1 . This value of the CTE is maintained until the decomposition of Zr 2 0 8 which occurs at a relatively high rate near 800 °C.
  • the invention is embodied in a method of making a ceramic body having isotropic negative thermal expansion, the body having a major constituent selected from the group consisting of ZrW 2 0 8 , HfW 2 0 8 , ZrV 2 0 7 and HfV 2 0 7 .
  • the method comprises the steps of providing a powder mixture, forming a "green" body that comprises the powder mixture, and heat treating the green body.
  • the powder mixture comprises a first and a second oxide precursor powder, selected respectively from the group consisting of Zr0 2 powder and Hf0 2 powder, and the group consisting of W0 3 powder and V 2 0 5 powder.
  • the heat treatment of the green body includes heating the body to. a temperature below the melting temperature of the selected constituent, such that the selected major constituent is formed from the green body by reactive sintering.
  • a green body we mean herein the compacted precursor powders as a monolithic body prior to sintering.
  • the powder mixture has a non- stoichiometric composition (e.g., excess Zr0 2 ) , and the heat treatment results in formation of a 2-phase material, e.g., ZrW 2 0 8 majority phase, with Zr0 2 inclusions dispersed in the majority phase.
  • a non- stoichiometric composition e.g., excess Zr0 2
  • the heat treatment results in formation of a 2-phase material, e.g., ZrW 2 0 8 majority phase, with Zr0 2 inclusions dispersed in the majority phase.
  • the powder mixture comprises a minor amount of a sintering aid (e.g., Y 2 0 3 , Bi 2 0 3 , A1 2 0 3 , ZnO, Ti0 2 , Sn0 2 ) , whereby the density of the sintered body is substantially increased.
  • a sintering aid e.g., Y 2 0 3 , Bi 2 0 3 , A1 2 0 3 , ZnO, Ti0 2 , Sn0 2
  • FIG. 1 SEM micrograph of a ZrW 2 O e -18 wt . % Zr0 2 monolith viewed with secondary electron imaging. Zr0 2 inclusions with various particle sizes having a maximum diameter of approximately 10 ⁇ m appear with darker contrast.
  • FIG. 3 Relative thermal expansion of a ZrW 2 0 8 -9.5 wt . % Zr0 2 monolith taken over an extensive temperature range.
  • the coefficient of thermal expansion (CTE) for the range -100 to 100 °C and 200 to 300 °C is -10 x 10 -6 and 3 x 10 "6 °C "1 , respectively.
  • -A reversible order-disorder transition takes place near 140 °C which does not compromise the mechanical strength of the monolith.
  • Figure 4 Relative thermal expansion over ambient working temperatures for several ZrW 2 0 8 -xZr0 2 monoliths.
  • compositions are presented (label, wt.% excess Zr0 2 , volume fraction Zr0 2 ) : a, 37.0%, 0.337; b, 19.5%, 0.174; c, 9.5%, 0.084, d, 0%, 0.
  • Nonlinearity of the thermal expansion is enhanced as the zirconia content increases.
  • Figure 5 illustrates the dependence of the Coefficient of Thermal Expansion (CTE) between 0 and 100 °C of two-phase ZrW 2 0 3 -xZr0 2 ceramics as weight percent of additional Zr0 2 .
  • the change in CTE demonstrates a linear relationship to the relative amount of Zr0 2 inclusions.
  • additives which form a eutectic may be utilized as a liquid phase sintering aid, thereby significantly increasing the density of a ceramic.
  • Liquid phases accelerate material transport during sintering by serving as a solvent for the solid phase with subsequent precipitation to yield dense ceramics.
  • Monoliths of ZrW 2 0 8 -xZr0 2 prepared with a Y 2 0 3 additive have achieved, densities greater than 99% the calculated theoretical density ( Figure 1) .
  • the density of a high purity ZrW 2 0 8 monolith is only 92%.
  • oxides typically used as sintering aids including refractory oxides were investigated (Table 1) .
  • Densification via liquid phase sintering has been demonstrated in several ceramic systems and is extensively employed in the ceramic industry in order to decrease sintering times and temperatures. For effective liquid phase sintering, only 1 vol.% of liquid within grain boundaries is necessary to aid densification. Increasing the concentration of A1 2 0 3 , Ti0 2 , or Y 2 0 3 , to a few weight percent leads to complete decomposition of ZrW 2 0 8 and melting of the monolith at the sintering temperature. This suggests that a liquid phase is present at 1180° C even at low concentrations of additives. Similar equilibria have been observed in the alkali metal-W0 3 -Zr0 2 systems with eutectic temperatures below 600 °C. Consequently, liquid phase sintering is a preferred mechanism for enhanced densification.
  • the particle size, particle size distribution, and uniformity of particle packing are important factors in the densification process. In this study of the preparation of ZrW 2 0 8 'xZr0 2 monoliths, these factors have the greatest impact on sintered density. In general, smaller particles are more reactive and tend to densify at lower temperatures. Coarse particles have less surface energy which diminishes the driving force for consolidation. For conventional powder processing, the optimum particle diameter is approximately 1 ⁇ m. Particles significantly smaller than this are difficult to pack uniformly and densely due to agglomeration and undergo excessive shrinkage with entrapped porosity during firing. In addition, a range of particle sizes is advantageous towards achieving maximum packing density in the green body. However, non-uniformities in particle packing may result in voids which are difficult to eliminate during the densification process. Variations in green body densities produced during the forming process can also result in warpage during sintering.
  • the as-received mixture of powders had a bimodal particle size distribution around 600 ⁇ m and 50 ⁇ m. Monoliths fabricated from this coarse, unreactive material actually decreased in density after sintering. It was necessary to comminute the starting materials by vibratory milling. As the milling time increased the particle size initially decreased significantly to approximately 1 ⁇ m diameter. Milling times were limited to 16 h due to concerns of contamination from the grinding media.
  • the micros-tructure of a nearly stoichiometric ZrW 2 0 8 monolith reveals large grains of ZrW 2 O a having approximately a 20 ⁇ m diameter which form the matrix of the ceramic.
  • the uniform distribution of pores and grain sizes is indicative of a homogeneously sintered material.
  • a SEM micrograph of a ZrW 2 0 8 -18 wt.% Zr0 2 monolith is presented in Figure 2 in which excess zirconia is observed as nearly spherical inclusions having various diameters. Individual ZrW 2 0 8 grains cannot be distinguished in the SEM image.
  • the Zr0 2 volume fraction was below the percolation limit such that a 0-3 connectivity (isolated inclusions of Zr0 2 in a matrix of ZrW 2 0 8 ) was preserved.
  • the percolation limit for a second phase with monodisperse diameters has been calculated to exist at a critical volume fraction of 0.183. Although we have prepared samples with a greater volume fraction of zirconia, all evidence indicates isolated inclusions. Thus significantly higher volume fractions are necessary to reach the percolation limit which is due to the distribution of diameters of the inclusions. Beyond the percolation limit the properties of a monolith with two interpenetrating 3-dimensional matrices (3-3 connectivity) may demonstrate anomalies.
  • Powder X-ray diffraction indicates the presence of only the ⁇ -ZrW 2 0 8 phase (Powder Diffraction File, Joint Committee on Powder Diffraction Standards, JCPDS, Swarthmore, PA, card number 13-557) and monoclinic Baddeleyite Zr0 2 phase (JCPDS card number 37-1484) .
  • the lower detectable limit of other phases by X-ray diffraction is estimated to be 1%.
  • ZrW 2 0 8 has demonstrated a negative thermal expansion from 0.3 to 1050 K.
  • the temperature dependence of the thermal expansion of a monolith of ZrW 2 0 8 with 9.5 wt.% excess Zr0 2 is shown in Figure 3.
  • the order-disorder phase transition at 150°C is reversible and does not compromise the mechanical strength of the monoliths.
  • cracking due to the large difference in thermal expansion of ZrW 2 0 8 and Zr0 2 was not observed over the temperature range of -100° to 300 °C.
  • the linear negative thermal expansion of the composite facilitates its utilization in applications.
  • the coefficient of thermal expansion of diphasic ceramic monoliths can be tuned by compensating the large negative thermal expansion of ZrW 2 0 8 with a material having a positive CTE such as Zr0 2 .
  • Zirconia was chosen as the second phase for its thermodynamic stability in the presence of ZrW 2 0 8 and for the ease of processing via the reactive sintering technique.
  • Several other refractories react with ZrW 2 0 8 at the sintering temperature and therefore lead to irreproducible results due to decomposition.
  • the thermal expansion of Zr0 2 is roughly linear from 20 to 100 °C with a CTE of 8 x 10 "6 "C” 1 .
  • Heating rates up to 20 °C/min to temperatures of 400 °C with a TMA analyzer did not reveal any decomposition or cracking which would be distinguished as irreproducibility or discontinuities in the CTE, respectively. Degradation of the ceramics was not observed through several heating and cooling cycles.
  • n eff the effective refractive index for the guided mode in the fiber
  • ⁇ the period of the index modulations of the fiber ( ⁇ 0.5 ⁇ m for a particular 1550 n grating) .
  • the Bragg wavelength of a fiber Bragg grating is temperature dependent primarily due to the temperature dependence of the refractive index of the silica based glass, In addition, the Bragg wavelength is strain dependent by altering the fringe spacing. As the temperature increases the refractive index of glass increases and vice versa. Also, due to the positive thermal expansion of silica (CTE ⁇ 0.5 xlO "6 °C "1 ) , the fringe spacing increases slightly with temperature.
  • the wavelength shift that corresponds to refractive index (n) changes due to temperature (T) variations and thermal expansion of silica glass ( ⁇ therma i) can be calculated as follows:
  • ⁇ ⁇ ⁇ ( — + ⁇ ⁇ kcrm ⁇ l ) ⁇ T n a l
  • the grating wavelength is also sensitive to strain. If a grating is stretched, then the grating wavelength will increase.
  • the strain and wavelength relationship can be presented as follows:
  • the grating that is compensated by a ZrW 2 0 8 '9.5 wt.% Zr0 2 monolith demonstrates a 0.05 nm deviation from -40 to 80 °C, which is nearly ideal.
  • This substrate can be utilized to fabricate a thermally compensated package suitable for WDM (wavelength division multiplex) applications.
  • the monoliths demonstrate brittle failure having an approximate conchoidal fracture surface.
  • the mechanism proceeds via intergranular fracture around Zr0 2 inclusions and intragranular throughout the ZrW 2 0 8 matrix. Therefore shearing at boundaries between ZrW 2 0 8 grains does not occur at room temperature.
  • Reactive sintering of W0 3 and Zr0 2 powders produces dense monoliths with adequate strengths .
  • the reactive sintering technique circumvents the inherent metastability of ZrW 2 0 8 in the early stages of densification, thereby yielding reproducible fabrication conditions .
  • Monoliths containing zirconia inclusions demonstrate a range of thermal expansion coefficients linearly related to the volume fraction of Zr0 2 .
  • a monolith of ZrW 2 0 8 • xZr0 2 which exhibits a negative thermal expansion in the desired range, has been successfully prepared and shown to thermally compensate a fiber Bragg grating .
  • Example 1 Preparation of ZrW 2 0 8 composite ceramics via reactive sintering technique utilizing methyl ethyl ketone (MEK) as the milling solvent.
  • MEK methyl ethyl ketone
  • Example 2 Preparation of ZrW 2 0 8 composite ceramics via reactive sintering technique utilizing water as the milling solvent .
  • Example 3 Extrusion of pre-reacted powders.
  • Example 4 Preparation of ZrV 2 0 7 composite ceramics via reactive sintering technique utilizing water as the milling solvent .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Composite Materials (AREA)
  • Light Guides In General And Applications Therefor (AREA)

Abstract

La présente invention concerne des monolithes qui présentent des coefficients réglables de dilatation thermique compris entre environ -5 à -11 x10-6 °C-1 autour de la température ambiante. Ces céramiques à deux phases, qui sont fabriquées, par exemple par frittage réactif de WO¿3? et de ZrO2, sont constituées d'une matrice de ZrW2O8 avec des adjonctions de ZrO2 dont les diamètres sont inférieurs à 10 νm. Des additifs peuvent accroître la densité de ces monolithes de plus de 98 % de la densité calculée. Les densités d'ébauche crue, la répartition des tailles des particules préfrittées, la pression de frittage, la microstructure et les propriétés mécaniques sont examinées. On peut utiliser ces céramiques comme substrats de façon à compenser thermiquement les réseaux de Bragg à fibres.
PCT/US2000/025487 2000-09-15 2000-09-15 Ceramiques a dilatation thermique negative isotrope et processus de fabrication Ceased WO2002022521A1 (fr)

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JP2002526722A JP2004509048A (ja) 2000-09-15 2000-09-15 等方性、負熱膨張セラミックスおよび製造方法
KR1020027006231A KR20020063575A (ko) 2000-09-15 2000-09-15 등방성 네가티브 열팽창 세라믹 및 이의 제조방법
PCT/US2000/025487 WO2002022521A1 (fr) 2000-09-15 2000-09-15 Ceramiques a dilatation thermique negative isotrope et processus de fabrication

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT502394B1 (de) * 2005-09-07 2007-03-15 Arc Seibersdorf Res Gmbh Verfahren zur herstellung eines keramischen werkstoffes und keramischer werkstoff
CN102432292A (zh) * 2011-09-22 2012-05-02 郑州大学 一种纳米负膨胀陶瓷Zr2(WO4)(PO4)2的烧结合成方法
JP2014019628A (ja) * 2012-07-20 2014-02-03 Taiheiyo Cement Corp 低熱膨張セラミックス、露光装置用ステージおよび低熱膨張セラミックスの製造方法
JP2015010006A (ja) * 2013-06-27 2015-01-19 太平洋セメント株式会社 負膨張セラミックス
CN105392922A (zh) * 2013-07-12 2016-03-09 株式公司品维斯 金属氧化物膜结构物
WO2017005752A1 (fr) 2015-07-06 2017-01-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Céramiques et vitrocéramiques présentant une dilatation thermique basse ou négative

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JP5156859B2 (ja) * 2006-10-04 2013-03-06 カヤバ工業株式会社 空圧緩衝器
JP2014051416A (ja) * 2012-09-07 2014-03-20 Taiheiyo Cement Corp 低熱膨張セラミックス、露光装置用ステージおよび低熱膨張セラミックスの製造方法
WO2015005735A1 (fr) * 2013-07-12 2015-01-15 (주)펨빅스 Structure de film d'oxyde métallique
CN104120309B (zh) * 2014-07-14 2017-01-11 郑州大学 一种金属-负热膨胀材料复合材料及其制备方法

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WO1999064898A2 (fr) * 1998-05-19 1999-12-16 Corning Incorporated Materiaux a expansion thermique negative, procede de preparation et utilisations de ces materiaux

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WO1999064898A2 (fr) * 1998-05-19 1999-12-16 Corning Incorporated Materiaux a expansion thermique negative, procede de preparation et utilisations de ces materiaux

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT502394B1 (de) * 2005-09-07 2007-03-15 Arc Seibersdorf Res Gmbh Verfahren zur herstellung eines keramischen werkstoffes und keramischer werkstoff
CN102432292A (zh) * 2011-09-22 2012-05-02 郑州大学 一种纳米负膨胀陶瓷Zr2(WO4)(PO4)2的烧结合成方法
JP2014019628A (ja) * 2012-07-20 2014-02-03 Taiheiyo Cement Corp 低熱膨張セラミックス、露光装置用ステージおよび低熱膨張セラミックスの製造方法
JP2015010006A (ja) * 2013-06-27 2015-01-19 太平洋セメント株式会社 負膨張セラミックス
CN105392922A (zh) * 2013-07-12 2016-03-09 株式公司品维斯 金属氧化物膜结构物
CN105392922B (zh) * 2013-07-12 2018-04-10 株式公司品维斯 金属氧化物膜结构物
WO2017005752A1 (fr) 2015-07-06 2017-01-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Céramiques et vitrocéramiques présentant une dilatation thermique basse ou négative
DE102015110831A1 (de) 2015-07-06 2017-01-12 Friedrich-Schiller-Universität Jena Keramiken und Glaskeramiken mit niedriger oder negativer thermischer Dehnung
US10501367B2 (en) 2015-07-06 2019-12-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Ceramics and glass ceramics exhibiting low or negative thermal expansion

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KR20020063575A (ko) 2002-08-03

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