WO2017005752A1 - Keramiken und glaskeramiken mit niedriger oder negativer thermischer dehnung - Google Patents

Keramiken und glaskeramiken mit niedriger oder negativer thermischer dehnung Download PDF

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Publication number
WO2017005752A1
WO2017005752A1 PCT/EP2016/065876 EP2016065876W WO2017005752A1 WO 2017005752 A1 WO2017005752 A1 WO 2017005752A1 EP 2016065876 W EP2016065876 W EP 2016065876W WO 2017005752 A1 WO2017005752 A1 WO 2017005752A1
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WIPO (PCT)
Prior art keywords
thermal expansion
glass
mol
material according
ceramic
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Ceased
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PCT/EP2016/065876
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German (de)
English (en)
French (fr)
Inventor
Christian Thieme
Christian Rüssel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Priority to PL16734687T priority Critical patent/PL3319913T3/pl
Priority to EP16734687.3A priority patent/EP3319913B1/de
Priority to CN201680038157.0A priority patent/CN108064219A/zh
Priority to JP2017564609A priority patent/JP6978324B2/ja
Priority to US15/742,236 priority patent/US10501367B2/en
Publication of WO2017005752A1 publication Critical patent/WO2017005752A1/de
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C03B19/063—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction by hot-pressing powders
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    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Definitions

  • the invention relates to ceramics and glass ceramics with low and / or negative coefficients of thermal expansion.
  • Such zero strain materials are also used for precision applications, such as: B. large-scale telescope mirror or in micro-optics. Of course, these materials are conceivable in many applications in which thermal shock resistance over a more or less wide temperature range is required, such. B. in cookware.
  • the already mentioned negative or very low thermal expansion can by crystalline phases with low or negative elongation, such as.
  • ß-spodumene high temperature modification of LiAISi 2 0 6
  • ß-eucryptite LiAISi0 4
  • cordierite g 2 Al 2 Si 5 0i8
  • high quartz or ß-quartz mixed crystals can be achieved.
  • quartz glass In addition to various glass ceramics, quartz glass also has a very low expansion coefficient (0.5-10 "6 K -1 ), which continues to be deposited by doping with TiO 2 can be lowered. The production of this material is because of the extremely high melting temperatures (> 2200 ° C), however, difficult, expensive and therefore expensive.
  • low-elongation glass-ceramics such as. B. Ceran ® by melting and subsequent crystallization of glasses from the system Li 2 O-Al 2 O 3 - prepared SiO 2 .
  • Such lithium aluminosilicate glasses are described for example in EP 0 995 723 B1, US RE 29 437 E and DE 39 27 174 A1, which, however, all require particularly high melting temperatures.
  • alkaline earth oxides are possible as additives. However, these oxides are not added to affect the crystal phase, but merely to alter the properties of the glass.
  • a lithium aluminosilicate glass in which BaO is used to improve the crystallization behavior and to reduce the viscosity.
  • BaO is known to significantly increase the coefficient of expansion of a glass.
  • DE 21 32 788 C glasses which are doped by the incorporation of up to 2% by weight of BaO and / or CaO and up to 12% by weight of rare earth oxides, however, increase the expansion coefficient.
  • the negative strain is also achieved here, inter alia, by crystals with the same structure type as ß-quartz.
  • the high quartz structure is stabilized here by aluminum oxide as well as mono- (Li 2 O, Na 2 O) or divalent (ZnO, MgO) oxides. Very high melting temperatures of 1550 to 1600 ° C are mentioned.
  • WO 2005/009 916 A1 describes that the negative elongation can be achieved by the crystallization of ⁇ -eukryptite and ⁇ -quartz. Both ZnO and BaO and / or SrO may be added. However, incorporation of these components in crystal phases is not mentioned. In the embodiments, a minimum melting temperature of 1480 ° C is given.
  • alkaline earth oxides such as BaO or SrO have only been added to the glasses to lower the melting temperature, perhaps also to suppress the tendency to crystallize. This could be done only in small quantities, since such oxides increase the thermal expansion coefficients of the glass-ceramics.
  • the invention is therefore based on the object of demonstrating a possibility by which ceramics with the least possible effort at low melting temperature and / or glass ceramics with low or negative thermal expansion can be produced.
  • the specified compositions form solid solutions, wherein the elements listed as component M can substitute each other in almost any concentration. The stoichiometry of these silicates and their structure may differ more or less strongly. Also, Si0 2 can be substituted for Ge0 2 .
  • the compound BaZn 2 Si 2 O is present at room temperature as a monoclinic low temperature phase which converts to a high temperature orthorhombic phase at 280 ° C (JH Lin, GX Lu, J. Du, MZ Su, C.K Loong, JW Richardson Jr. , J. Phys. Chem. Solids 60, 1999, 975-983).
  • the thermal expansion coefficient of the low-temperature phase is very high, at 13-16-10 "6 K ' ⁇ the phase transformation is associated with a volume increase of 2.8% and the high-temperature phase then has a high temperature, depending on the composition, a very small or also a negative thermal expansion (M. Kerstan, M. Muller, C. Russel, J. Solid State Chem. 188, 2012, 84-91).
  • the material produced according to the invention can on the one hand be sintered from powders, the Bai described above.
  • x Sr x M 2 Si 2 O 7 phase is the main crystal phase.
  • the powder used for sintering may contain one or more other crystalline or amorphous phases.
  • the powders described can be obtained by solid state reactions z. B. from oxides and carbonates, or by other methods, for example by sol-gel, coprecipitation method, or by means of gas phase reactions.
  • the material according to the invention can also be obtained by controlled crystallization of glass. This is possible because the components of the crystalline phases of the invention are also part of many relatively crystallization-stable glasses. If only a relatively small amount of SiO 2 is added to a Bai.xSr x M 2 Si 2 O 7 composition, a relatively stable glass can already be obtained.
  • the stability of the glass can be further improved by adding further components, such as B 2 O 3 , La 2 O 3 or ZrO 2 , since these components suppress the nucleation in the chemical compositions according to the invention in low concentrations. In higher concentrations, however, La 2 Ü 3 or ZrO 2 may have the opposite effect, ie nucleation and thus crystallization, and thus act as nucleants.
  • the coefficient of expansion of glass ceramics can be varied within wide limits by varying the BaO / SrO ratio, without causing important glass properties such , As the glass transition temperature or the expansion coefficient of the pure glass to be significantly changed.
  • composition Bai. x Sr x M 2 Si 2 O 7 also the component M of considerable importance.
  • M Zn
  • the crystalline phase according to the invention can be stabilized as soon as about 10 mol% of the BaO are replaced by SrO.
  • component M ions of the following bivalent metals can be used: Mg, Ni, Co, Fe, Cu, Mn.
  • compositions listed in the table below are prepared by conventional ceramic processes (solid phase reaction). This means that the starting materials are tempered below the liquidus temperature for 30-50 hours. In between, the powders are ground several times and homogenized (4 to 10 times). The phase purity is checked by X-ray powder diffractometry. BaC0 3 , SrC0 3 , ZnO, Si0 2 , Ge0 2> MgO, MnC0 3 , NiO, Fe (COO) 2 -2H 2 0, Co 3 0 4 and CuO are used as raw materials. Two crystal structures can be stabilized. X-ray powder diffractometry is used to check whether the monoclinic or orthorhombic modification is stable at room temperature. The latter has the desired negative thermal expansion. The table shows which of the two phases is stable at room temperature. In some compositions, both phases are adjacent. The iron-containing samples were prepared under argon atmosphere.
  • Powders containing predominantly the orthorhombic modification exhibit negative or very low thermal expansion coefficients after prior isostatic pressing and subsequent sintering.
  • barium strontium and zinc acetate are dissolved in the correct stoichiometry in deionized water.
  • the appropriate amount of colloidal Si0 2 is added with a particle size ⁇ 50 nm.
  • the water is evaporated within a day until a viscous mass is formed. This is dried, ground with the aid of a ball mill, mixed with a 1% solution of polyvinyl alcohol in water and dried again.
  • the resulting powder is uniaxially pressed and sintered at 1 130 ° C.
  • the resulting ceramic is examined by X-ray powder diffractometry.
  • the crystal structure corresponds to that of high-temperature BaZn 2 Si 2 07, as they are was also found in Example 1.
  • the ceramic phase is pure and exhibits a linear coefficient of thermal expansion of -12 x 10 "6 K '1.
  • a glass with the composition 8 BaO ' - 8 SrO ⁇ 34 ZnO ⁇ 46 Si0 2 -1 Zr0 2 ⁇ 3 La 2 0 3 is melted at a temperature of 1450 ° C in a platinum crucible.
  • the glass shows a very low viscosity ( ⁇ 10 Pas) at this temperature.
  • the crystallization of a cylindrical sample about 20 mm in length and 8 mm in diameter at 900 ° C for 5 h gives a linear thermal expansion coefficient of 0.5-10 "6 K " 1 (measured in the temperature range between 25 and 300 ° C).
  • a glass with the composition 8 BaO-8 SrO-30 ZnO-5 MgO-45 Si0 2 -2 Zr0 2 2 La 2 0 3 is melted at 1400 to 1450 ° C in a platinum crucible.
  • the glass has after five hours of crystallization at 900 ° C a linear thermal expansion coefficient of -2-10 "6 K '1 (measured in the temperature range between 25 and 300 ° C) on.
  • a glass with the composition 8 BaO-8 SrO-30 ZnO-5 CoO-45 Si0 2 -1 Zr0 2 -1 La 2 0 3 -2 B 2 0 3 is at 1350 to 1450 ° G in the Al 2 0 3 crucible melted. After five hours of crystallization at 900 ° C, the glass-ceramic has a linear thermal expansion coefficient of -2.4-10 "6 K " 1 (measured in the temperature range between 25 and 300 ° C).
  • a glass with the composition 8 BaO-8 SrO-34 ZnO-44 Si0 2 -1 Zr0 2 -1 La 2 0 3 -4 B 2 0 3 is comminuted to an average particle size ⁇ 10 ⁇ .
  • the glass powder thus obtained is treated with a 1% solution of polyvinyl butyrate! mixed in water and dried. Subsequently, the powder is cold isostatically pressed using a silicone mold. The compact is finally sintered at 900 ° C for 5 h. During heating, the powder is compacted by viscous flow, then crystallized the glass. In the temperature range between 100 and 500 ° C results in a linear thermal expansion coefficient of 4.1 -10 6 K "1 .
  • a glass with the composition 7.5 BaO-7.5 SrO-32 ZnO-47 Si0 2 -5 Zr0 2 '1 La 2 0 3 is melted at 1350 to 1450 ° G.
  • the glass transition temperature is 695 ° C.
  • Crystallization at 815 ° C for 20 h leads to the formation of crystals of composition Bao.5Sro.5Zn 2 Si 2 07.
  • Small amounts of Zr0 2 also crystallize. This acts as a nucleating agent.
  • the glasses crystallized at 815 ° C have a linear thermal expansion coefficient of -2.M 0 '6 K "1 .
  • a ceramic having the composition Sro.sBao.sZm.gNio.iS Oy is prepared via a solid phase reaction.
  • the appropriate amounts of BaC0 3 , SrC0 3 , ZnO, NiO and Si0 2 are slurried in ethanol and then ground in a planetary mill to an average particle size ⁇ 3 ⁇ .
  • the mixture of starting materials and ethanol is then dried for 3 h at 1 10 ° C.
  • the resulting powder is converted by a temperature treatment at 1200 ° C for 10 h in the corresponding nearly phase-pure ceramic.
  • the ceramic is then again ground to a mean particle size ⁇ 3 ⁇ and pressed uniaxially.
  • the compact is sintered at 1200 ° C for 10 h.
  • the dilatometric measurement shows an expansion coefficient of -19.3-10 "6 K " 1 in the temperature range between 100 and 300 ° C.
  • a glass with the composition 8BaO 8SrO 30ZnO 5MgO 45Si0 2 3B 2 0 3 is melted at 1350 ° C in a platinum crucible.
  • the raw materials BaC0 3 , SrC0 3 , ZnO, MgO, SiO 2 , and H 3 BO 3 are used.
  • the glass is poured into a preheated to 700 ° C steel mold and then transferred to a cooling oven, which was also preheated to 700 ° C, and then cooled at 2 K / min.
  • a glass ceramic is produced which has a thermal expansion close to zero, measured in the Temperature range between room temperature and 650 ° C, has. This can thus be used as a carrier material for optical components.

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CN113087518B (zh) * 2021-03-03 2022-04-22 华中科技大学 一种负热膨胀系数微波陶瓷及其3d打印介质谐振器天线
CN114195516B (zh) * 2021-12-03 2022-11-11 郑州大学 一种具有超宽温度下近零膨胀系数的陶瓷材料及其制备方法
CN114315351B (zh) * 2022-01-24 2022-09-23 河南大学 一种高熵近零膨胀钒酸盐陶瓷材料及其烧结合成方法
CN115925401B (zh) * 2022-11-10 2023-07-25 华中科技大学 一种低介硅酸盐微波介质陶瓷材料及其制备方法
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EP3319913A1 (de) 2018-05-16
JP2018527274A (ja) 2018-09-20
DE102015110831A1 (de) 2017-01-12
EP3319913B1 (de) 2020-06-17
JP6978324B2 (ja) 2021-12-08
CN108064219A (zh) 2018-05-22
PL3319913T3 (pl) 2021-01-25

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