CN101460423A - 韧性堇青石玻璃-陶瓷 - Google Patents

韧性堇青石玻璃-陶瓷 Download PDF

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CN101460423A
CN101460423A CNA200780020194XA CN200780020194A CN101460423A CN 101460423 A CN101460423 A CN 101460423A CN A200780020194X A CNA200780020194X A CN A200780020194XA CN 200780020194 A CN200780020194 A CN 200780020194A CN 101460423 A CN101460423 A CN 101460423A
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glass
pottery
phase
many
ceramic
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G·H·比尔
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Corning Inc
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Corning Inc
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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
    • C03C10/0036—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 a divalent metal oxide as main constituents
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

公开了一种内部成核的增韧的堇青石玻璃—陶瓷。堇青石玻璃—陶瓷具有能与氮化硅竞争的良好的抗氧化性和断裂韧性以及热膨胀系数。该玻璃—陶瓷可以以液体浇铸。退火产生高结晶度的材料，该材料综合了高硬度、高杨氏模量、良好的热稳定性、高强度、低密度和良好的介电性质。所述玻璃—陶瓷包含主要是堇青石的联锁晶相和具有拉长或针状结构的第二相。第三相可包含晶体陶瓷，能促进第二相的针形度。第三相优选能形成孪晶。

Description

韧性堇青石玻璃-陶瓷
发明领域
本发明涉及包含堇青石的增韧的玻璃-陶瓷混合物。
发明背景
在高温应用中，晶体材料与相应的玻璃态材料相比常具有优良的耐热变形性。晶体制品通常通过烧结制造。烧结具有一些缺陷，包括产生空隙和需要进行压制。相反，玻璃态制品能以几乎无空隙的状态浇铸。不幸的是，玻璃态材料在远低于其理论熔点时可能发生热变形。
现有技术揭示晶粒可以从最初的玻璃态材料退火，因而形成玻璃-陶瓷。玻璃-陶瓷与玻璃相比提高了耐热变形性。首先，通常在高于液相线温度将玻璃成形，然后在高于成核温度进行退火。玻璃在高于其液相线温度时的流体特性使其能够通过浇铸进行成形。成核温度是在玻璃内晶体开始形成和生长的温度。选择的成核温度应低于玻璃可能发生热变形时的温度。在退火期间，晶粒核化，开始生长，并最终包括了材料的大多数。高熔点化合物如二氧化钛能促进成核。当温度低于晶体的熔化温度时，晶体通常比相应的玻璃具有显著低的热变形。在要求耐热变形性的各种应用中一直使用玻璃-陶瓷。
一种这样的玻璃-陶瓷组合物包括包含堇青石的主晶相。堇青石是硅酸铝镁，S.D.Stookey在美国专利第2,920,971号中对其进行了描述，堇青石可以用于需要难熔材料的应用。堇青石玻璃-陶瓷具有良好的硬度和耐热变形性，但是具有热膨胀系数(CTE)高和只有平均断裂韧性的缺陷。例如，一种堇青石玻璃-陶瓷的断裂韧性为2.2MPa·m0.5，在25-1000℃的温度范围内的平均CTE为57 x 10-7/℃。差的断裂韧性导致形成裂纹并扩大，这样会使制品在应力下破碎或断裂。高CTE降低了耐热冲击性。较低的断裂韧性和较高的CTE限制了堇青石玻璃-陶瓷的应用。
在要求较低CTE和较高断裂韧性的应用中使用氮化硅。氮化硅的CTE约为30 x 10-7/℃，断裂韧性约为6MPa·m0.5。氮化硅比大多数金属具有更好的高温性能，综合了高强度、蠕变阻力和抗氧化性。这些性质使氮化硅可以替代涡轮和往复式发动机中的金属，并用作发动机部件、轴承和切削工具。此外，与大多数陶瓷材料相比，氮化硅的低热膨胀系数提供了良好的耐热冲击性。否则作为不足之处，氮化硅可能很难产生完全致密的材料(经常需要进行热压)，不容易烧结，在某些条件下可能发生氧化，并且不能加热超过1850℃，超过该温度会分解为硅和氮。这些缺陷使氮化硅部件成本高，因而限制了使用氮化硅部件的应用。
因此需要替代氮化硅的材料。所述材料应相对价廉并容易制造。较好地，应能够经受模塑，并结合了低CTE和高断裂韧性。
发明概述
本发明描述内部核化的堇青石玻璃—陶瓷。堇青石玻璃—陶瓷结合了良好的断裂韧性与低CTE。此外，本发明可以以液体浇铸，但是在退火后基本为晶体，并具有高硬度、高杨氏模量、良好的热稳定性、高强度、低密度和良好的介电性质。
本发明的堇青石玻璃—陶瓷具有包含联锁的晶相的微结构，所述联锁的晶相主要是基本上由拉长的堇青石晶粒组成的第一相和具有拉长的或针状结构的第二相。还可以存在第三相，第三相包含能够形成孪晶(twinning)的晶体陶瓷。与形成孪晶相关的能量可以进一步提高断裂韧性。
本发明的玻璃—陶瓷涉及内部核化的堇青石玻璃—陶瓷。所述堇青石玻璃—陶瓷结合了以下特性：在2.5-6.0MPa.m0.5范围的高断裂韧性；在25-1000℃的温度范围内为20-50 x 10-7/℃的低热膨胀系数；努普值(Knoop)大于800的高硬度；大于10GPa的高杨氏模量；在高于或等于1200℃的热稳定性；一般大于200MPa的高强度；约2.5-2.9g/cc的低密度；以及具有高电阻率、低介电常数和损耗正切的良好介电性质。本发明还涉及一种堇青石玻璃—陶瓷，通过产生联锁晶相的微结构来实现高断裂韧性，在该联锁晶相中，堇青石占主导，且至少有一个相被高度拉长或呈针状。任选地，希望另外有一个能够形成薄片孪晶的相，例如但不限于顽辉石(MgSiO3)和/或钙长石(CaAlSi2O8)。已知孪晶能提高断裂韧性。
在另一个实施方式中，本发明的堇青石玻璃—陶瓷的CTE小于35 x 10-7/℃，断裂韧性最大约为6.0MPa·m0.5。低CTE能提高耐热冲击性。较高的断裂韧性降低了裂纹产生并扩大的速率，因而降低了断裂的危险性。本发明的堇青石玻璃—陶瓷与氮化硅相比，降低了CTE并提高了断裂韧性。有利的是，堇青石玻璃—陶瓷可以利用流体玻璃态精确浇铸，不需要热压；与氮化硅相比，具有较低的密度和优良的抗氧化性。
附图简述
图1示出本发明的微结构。
发明详述
一种增韧的低CTE堇青石玻璃—陶瓷包含多个相，其中至少一个相是针状的。玻璃—陶瓷包括当基本为玻璃态的材料在升高温度下退火时能产生基本为晶体的材料的任何材料。退火导致一个或多个晶相成核。通过用高熔点化合物如二氧化钛引晶，可以加速成核。当达到预定水平的结晶度，通常是超过80％，更优选大于90％时，退火完成。
本发明的玻璃—陶瓷包含多个晶相。重要的是，任何残余玻璃不得在材料中形成连续的相。为此，结晶度应至少约为85体积％，更优选大于90体积％。典型的增韧的低CTE堇青石玻璃—陶瓷的残余玻璃少于5体积％。所述晶相包含至少两个联锁的相。
第一晶相包含拉长的堇青石晶粒。第二相为针状，包含钛酸盐，例如，钛酸镁、钛酸铝或它们的组合。任选地，可以存在第三相，该相优选包括能形成薄片孪晶的陶瓷化合物。孪晶陶瓷化合物包括顽辉石(MgSiO3)和斜长石，如钙长石(CaAl2Si2O8)。图1示出本发明的玻璃陶瓷的显微照片，包含六边形堇青石的黑色晶体、针状钛酸铝镁的白色晶体和钙长石的灰色晶体。
该玻璃—陶瓷包含50-80体积％的堇青石。与氮化硅不同，因为堇青石已经是氧化物，所以具有固有的抗氧化性。堇青石相包含6/m2/m2/m的六边形晶体结构。堇青石晶粒的长宽比至少为2:1，优选至少为5:1。该拉长的结构可促进与其他晶粒的联锁。而且，拉长的堇青石晶粒可以使第二相沿拉长的堇青石晶粒边界生长，因而提高了第二相的针形度(acicularity)。
玻璃—陶瓷包含8-20体积％的针状第二相。在玻璃退火期间，第二相在约850℃开始结晶，最后在约1100℃形成堇青石。进一步退火能够使第二相沿堇青石的晶粒边界生长。第二晶相的长宽比应至少为5:1。观察到针形度可高至20∶1。预期对针形度没有理论上限。测得的针形度明显小于实际的针形度，除非第二相沿显微照片的平面下落。第二相晶粒的针状结构使这些晶粒与大量其他相或晶粒相互作用。第二相包含在本性上能以针状条形形态生长的晶体。化合物包括例如，镁和铝的钛酸盐。其他合适的化合物为本领域的技术人员所皆知。在退火过程中，使玻璃流态化能促进针状化(acicularization)。例如，低氧化硅玻璃具有粘度随温度大幅度变化的曲线，这种特性使晶体能在优选的方向上生长。针状相进行取向处理可得到在机械或电学性质上基本呈各向异性的玻璃—陶瓷，根据应用可能需要这种玻璃—陶瓷。
该玻璃—陶瓷可包含第三晶相。第三相最多可占玻璃—陶瓷的20体积％，优选至少约10体积％。较好地，第三晶相提高了第二相的针形度。不希望受这种解释的限制，但第三相可能是因为以下两个原因而提高了针形度。第一，包含大于约90％堇青石的玻璃—陶瓷会产生长宽比小于2:1的堇青石晶体。短而结实的堇青石晶粒在物理上限制了第二相的拉长生长。第二，高堇青石玻璃包含显著量的氧化铝。高氧化铝玻璃不能像低氧化铝玻璃那样使那么多的氧化钛溶解。因此，可能形成较少的针状钛酸盐。还可能发生过早的相分离和成乳白色，由此损害了第二相带来的益处。包含第三相提高了堇青石晶体的长宽比，并阻止钛酸盐发生相分离。
第三相包含晶体陶瓷化合物，该化合物能够使第二相以针状生长。较好地，第三相具有形成薄片孪晶的能力。这种陶瓷通过沿平行的成对平面滑移而成为孪晶。孪晶消散了能量并提高了断裂韧性。玻璃—陶瓷可包含最多20体积％的第三晶相。孪晶陶瓷包括斜长石，如钙长石、Sr-长石、Ba-长石，以及辉石，如顽辉石和铝顽辉石(aluminous enstatite)。根据应用，长石应不含或含有极少量的钠化合物。含钠长石可具有有害的介电性质、微波透射性，并能减缓退火期间的结晶，因此产生较高的残余玻璃。
预期除了薄片孪晶相外，第三相中还可以另外包含或代之以选自下组的晶相：镁橄榄石、氟云母(fluormica)、氟闪石玻璃陶瓷(fluoramphibole)、块硅镁石、尖晶石、假蓝宝石、多铝红柱石和硬硅钙石。可以包含这些晶相作为提高玻璃—陶瓷的总体韧性的手段。具体地，预期/理论上有以下提高韧性的机理：(1)镁橄榄石、氟闪石玻璃陶瓷、块硅镁石、多铝红柱石和硬硅钙石相因为存在叶片形晶体而提高了韧性；(2)尖晶石和假蓝宝石晶相因为晶相的高模量能使破裂偏移而提高了韧性；和(3)氟云母晶相通常具有良好的开裂，而能提高玻璃—陶瓷的韧性。
玻璃—陶瓷可以由包含以下组分(按重量％计)的组合物形成：35-50％的SiO2，10-35％的Al2O3，10-25％的MgO，7-20％的TiO2，最多至5％的CaO和最多至10％的Sr0，最多至5％的F，其中Ca0和SrO之和至少为0.5％。可以将该组合物制成玻璃并成形为要求的形状。可方便地加入添加剂以利于加工，使组合物包含最多至5重量％的BaO、MnO、FeO、CoO、ZnO、As2O3、Sb2O3、B2O3、Na2O和K2O。形成的成形体从1100-1300℃退火足够的时间，以达到要求的结晶度。常规的退火时间约为10小时。结晶度通常大于85％。退火产生的玻璃—陶瓷包含间断的玻璃相和许多陶瓷相，包括堇青石、钛酸盐和任选的孪晶陶瓷。该玻璃—陶瓷的断裂模量为40,000psi，比标准堇青石玻璃—陶瓷的断裂模量大50％以上。该玻璃—陶瓷的CTE小于35 x 10-7/℃，断裂任选最高至约6.0MPa·m0.5。
本发明的玻璃—陶瓷可以形成任意的制品。所述玻璃—陶瓷尤其适合于要求低CTE、良好的断裂韧性或抗氧化性的制品。一种这类制品是雷达屏蔽器。堇青石玻璃—陶瓷固有的抗氧化性使其能够用于氮化硅可能被氧化的应用。此外，堇青石玻璃—陶瓷的常规密度为2.63-2.77g/cm3，而氮化硅的密度约为3.30g/cm3。主要由增韧的堇青石玻璃—陶瓷组成的制品的质量小于同样的氮化硅制品。
实施例1
制备基本上由45重量％氧化硅、28重量％氧化铝、14重量％氧化镁、2重量％氧化钙和10重量％氧化钛组成的混合物。将该混合物加热形成透明琥珀色的玻璃，并浇铸成形。将该成形体首先于800℃退火2小时。于1200℃进一步退火10小时，直到达到95体积％的结晶度。产生的玻璃—陶瓷的CTE为30 x 10-7/℃，断裂韧性为3.8MPa·m0.5。现有技术中的堇青石玻璃—陶瓷的CTE为55 x 10-7/℃，断裂韧性为2.2MPa·m0.5。本发明的堇青石玻璃—陶瓷的CTE减小近50％，同时断裂韧性提高了70％以上。
下面表1给出本发明的代表性组合物的例子。除非另外指出，有关组合物的资料是作为批料时的重量％。
表1
Figure A200780020194D00101
*经分析得出的组成
显然，对本发明的各种修改和变动都是可能的。因此，应理解，在以下权利要求书的范围之内，不需要具体的描述，即可以实施本发明。虽然参照一些优选实施方式描述了本发明，但是对本发明的不同变动、修改和添加对本领域技术人员而言是显而易见的。所有这些修改、变动和添加形式都包含在本发明的范围之内，本发明的范围仅受所附权利要求书的限制。

Claims (23)

1.一种具有高断裂韧性和低热膨胀系数的玻璃—陶瓷，该玻璃—陶瓷由包含按重量％计的以下组分的组合物形成：
SiO2                     35-50％
Al2O3                    10-35％
MgO                      10-25％
TiO2                     7-20％
CaO                      最多至5％
SrO                      最多至10％
F                        最多至5％
前提是CaO和SrO之和为至少0.5％，其中玻璃—陶瓷包含具有联锁的第一和第二晶相的微结构，所述晶相中至少一相是针状的。
2.如权利要求1所述的玻璃—陶瓷，其特征在于所述第一相包含六边形堇青石。
3.如权利要求1所述的玻璃—陶瓷，其特征在于所述第二相为针状的，包含钛酸盐。
4.如权利要求3所述的玻璃—陶瓷，其特征在于所述钛酸盐选自下组：钛酸镁、钛酸铝和它们的组合。
5.如权利要求2所述的玻璃—陶瓷，其特征在于所述第一相占所述玻璃—陶瓷的50-80体积％。
6.如权利要求1所述的玻璃—陶瓷，其特征在于所述针状相占所述玻璃—陶瓷的8-20体积％。
7.如权利要求1所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷包含最多至20体积％的第三晶相，该晶相包含孪晶陶瓷化合物。
8.如权利要求7所述的玻璃—陶瓷，其特征在于，所述孪晶陶瓷化合物选自下组：钙长石、Sr-长石、Ba-长石、顽辉石和铝顽辉石。
9.权利要求1所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷包含最多至20体积％的第三晶相，所述第三晶相选自下组：氟云母、氟闪石玻璃陶瓷、块硅镁石、尖晶石、假蓝宝石、多铝红柱石、镁橄榄石和硬硅钙石。
10.如权利要求7所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷包含最多至20体积％的第三相。
11.如权利要求1所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷在25-1000℃温度范围的CTE为20-50 x 10-7/℃，努普硬度大于800。
12.如权利要求1所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷的杨氏模量大于10GPa。
13.如权利要求1所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷的断裂韧性为2.5-6.0MPa.m0.5。
14.一种形成增韧的堇青石玻璃—陶瓷制品的方法，该方法包括以下步骤：
a)掺混组合物，该组合物包含按重量％计的以下组分：35-50％的SiO2，10-35％的Al2O3，10-25％的MgO，7-20％的TiO2，最多至5％的CaO、最多至10％的SrO和最多至5％的F，其中CaO和SrO之和至少为0.5％；
b)将组合物加热成流体玻璃；
c)使组合物形成具有要求的形状的成形体；
d)将该成形体冷却为固体玻璃；
e)将所述固体玻璃在1100-1300℃退火足够的时间，以达到至少85体积％的结晶度。
15.如权利要求14所述的方法，其特征在于所述成形步骤包括浇铸流体玻璃。
16.如权利要求14所述的方法，其特征在于，该方法还包括对所述成形体冷却之后但在进行退火之前的热处理，该热处理步骤包括在至少800℃加热所述成形体1小时以上。
17.一种堇青石玻璃—陶瓷，包含至少以下三个相：
a)50-80体积％的第一相，该相主要由长宽比至少为2∶1的堇青石组成；
b)8-20体积％的第二相，该相主要由长宽比至少为5∶1的钛酸盐组成；
c)最多至20体积％的第三相，该第三相选自下组：钙长石、顽辉石、铝顽辉石、镁橄榄石、氟云母、氟闪石玻璃陶瓷、块硅镁石、Sr-长石、Ba-长石、尖晶石、假蓝宝石、多铝红柱石和硬硅钙石。
18.如权利要求17所述的堇青石玻璃—陶瓷，其特征在于，所述第一相的长宽比至少为5:1。
19.如权利要求17所述的堇青石玻璃—陶瓷，其特征在于，所述玻璃—陶瓷包含10-20体积％的第三相。
20.一种玻璃—陶瓷，其在25-300℃温度范围的CTE为20-50 x 10-7/℃，断裂韧性为2.5-6.0MPa.m0.5，所述玻璃—陶瓷由包含以下按重量％计的组分的组合物形成：
SiO2                   35-50％
Al2O3                  10-35％
MgO                    10-25％
TiO2                   7-20％
CaO                    最多至5％
SrO                    最多至10％
F                      最多至5％
前提是CaO和SrO之和为至少0.5％，其中玻璃—陶瓷包含具有联锁和针状的第一和第二晶相的微结构。
21.如权利要求20所述的玻璃—陶瓷，其特征在于，所述第二相包含选自下组的钛酸盐：钛酸镁、钛酸铝和它们的组合。
22.如权利要求20所述的玻璃—陶瓷，其特征在于所述玻璃—陶瓷还包含具有孪晶陶瓷化合物的第三晶相，所述孪晶化合物选自下组：钙长石、Sr-长石、Ba-长石、顽辉石和铝顽辉石。
23.如权利要求20所述的玻璃—陶瓷，其特征在于，所述玻璃—陶瓷包含选自下组的第三晶相：镁橄榄石、氟云母、氟闪石玻璃陶瓷、块硅镁石、尖晶石、假蓝宝石、多铝红柱石和硬硅钙石。
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