CN1098824C - 陶瓷蜂窝体的烧制方法 - Google Patents

陶瓷蜂窝体的烧制方法 Download PDF

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CN1098824C
CN1098824C CN98809798A CN98809798A CN1098824C CN 1098824 C CN1098824 C CN 1098824C CN 98809798 A CN98809798 A CN 98809798A CN 98809798 A CN98809798 A CN 98809798A CN 1098824 C CN1098824 C CN 1098824C
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honeycomb structure
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T·C·乔治乌
A·施密特
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Abstract

一种制造堇青石陶瓷蜂窝结构体的方法，包括如下步骤：配制包含高岭土、滑石、氧化铝和其它堇青石形成材料的混合物批料，该批料中各种原料的含量是有效量，从而能产生主要结晶相为堇青石的烧制蜂窝体；将该批料与有效量的载体和成形助剂均匀混合，上述的成形助剂能使批料具有可塑性并使形成的生坯具有一定强度；用挤压法将该批料成形为蜂窝结构体生坯，然后干燥和烧制蜂窝结构体生坯。蜂窝结构体生坯的烧制通过如下四步加热法进行：(1)将生坯加热到约为750-850℃的第一温度；(2)加热到约为1250-1350℃的第二温度；(3)最后加热到至少为1390℃的第三温度；(4)在至少1390℃至1420℃的温度保温约12-20小时。在一个实施方式中，在第一温度以上的各个烧制温度保持O2含量不超过6%的氧化性烧制气氛。或者在第一温度以上的各个烧制温度保持CO含量不超过3%的还原性烧制气氛(与氧化性相反)。

Description

陶瓷蜂窝体的烧制方法
本申请要求T.C.乔治乌和A.施密特在1997年10月3日提出的题目为“陶瓷蜂窝体的烧制方法”的美国专利临时申请No.60/061,262的优先权。
1.发明领域
本发明涉及堇青石陶瓷蜂窝结构体的制造方法。特别是，本发明涉及采用气氛控制的烧制来形成具有更好热膨胀和强度性能的堇青石陶瓷蜂窝结构体的制造方法。
2.发明背景
已知由堇青石(结晶硅酸铝镁材料，2MgO·2Al2O3·5SiO2)制成的通常形似蜂窝的结构在颇宽温度范围内具有低的热膨胀系数。因此，陶瓷体中这种相的主要部分赋予陶瓷体极好的耐热冲击性。
由于这种优异的耐热冲击性和耐熔性，现已发现含有堇青石或取代堇青石作为主要结晶相的挤压整体陶瓷蜂窝结构体可广泛用作治理内燃机燃烧废气的催化剂载体和过滤器。用这种材料制成的其它有用产品可用作流体过滤器(如柴油颗粒过滤器、超过滤装置)或Woodstove燃烧器的基板或发电厂的DeNOX催化转化器。
美国专利3,885,997(Frost等)、4,001,028(Frost等)、5,114,664(Beall等)和5,258,150(Merkel等)描述了由粘土、滑石和氧化铝的可挤压批料混合物制备这种蜂窝体的方法。当烧制挤压成形体时，上述组分反应形成堇青石。
虽然这些专利中所述的堇青石产品对于许多用途已具有足够的强度和耐热冲击性，但某些用途(如治理汽车废气的用途)涉及重复而强烈的机械冲击和热冲击。因此，需要小心包装，以最大限度地减少产品破裂的发生。对于这些用途，强度和/或耐热冲击性的改善是特别有利的。
因此，本发明的主要目的是提供堇青石陶瓷蜂窝结构体的制造方法。这种方法包括在控制气氛中的烧制，制成强度和耐热冲击性更高的堇青石陶瓷蜂窝结构体。
通过阅读如下的说明，可以明白本发明的其它目的。
                    发明概述
本发明提供制造强度和耐热冲击性更高的堇青石蜂窝结构体的一种方法。这种控制气氛的烧制法的另一个优点是烧制时收缩很低。
本发明涉及堇青石陶瓷蜂窝结构体的制造方法，这个方法包括如下步骤：配制包含高岭土、滑石、氧化铝和其它堇青石形成材料的混合物批料，该批料各种原料的含量是有效量，从而能烧制产生主要结晶相为堇青石的蜂窝体；将该批料与有效量的载体和成形助剂均匀混合，上述的成形助剂能使批料具有可塑性并使形成的生坯具有一定强度；用挤压法将批料成形为蜂窝结构体生坯，然后对蜂窝结构体生坯进行干燥和烧制。蜂窝结构体生坯的烧制通过如下四步加热法进行：(1)将生坯加热到约为750-850℃的第一温度；(2)加热到约为1250-1350℃的第二温度；(3)最后加热到至少为1390℃的第三温度；(4)在至少1390℃至1420℃的温度保温约12-20小时。在一个实施方式中，在第一温度以上的各个烧制温度保持O2含量不超过6％的氧化性烧制气氛。用这种控制氧化性的烧制方法可获得具有更好强度的堇青石陶瓷蜂窝结构体。
在另一个实施方式中，是用同样的控制四步烧制方法进行蜂窝结构体生坯的烧制，然而在第一温度以上的烧制温度保持CO量含不超过3％的还原性烧制气氛(与氧化性气氛相反)。用这种控制还原性的烧制法可以获得具有更好耐热冲击性、强度和烧制收缩的堇青石陶瓷蜂窝结构体。
                            附图简介
为了更好地理解本发明，给出了如下附图。
图1表示组成相似的三种挤压生坯分别在三种不同烧制气氛中烧制形成的含堇青石蜂窝体断裂模量(MOR)曲线的对比图。
图2表示组成相似的三种挤压生坯分别在四种不同烧制气氛中烧制形成的含堇青石蜂窝体热膨胀系数(CTE)的对比图。
图3表示组成相似的三种生坯分别在四种不同烧制气氛中烧制挤压形成的含堇青石蜂窝体断裂模量(MOR)的对比图。
图4表示组成相似的三种挤压生坯分别在四种不同烧制气氛中烧制形成的含堇青石蜂窝体烧制收缩的对比图。
发明的详细描述
用于制造本发明堇青石陶瓷结构体的陶瓷批料的原料可以选自任何合适的原料。高纯的粘土、滑石、二氧化硅、氧化铝、氢氧化铝、以及产生氧化镁的原料通常用于这种陶瓷，对本发明来说是令人满意的。然而，众所周知，如果存在氧化钙(CaO)和碱(如苏打和钾碱)之类的杂质，会对堇青石产物的热膨胀性和耐熔性能产生不利影响。因此，当需要产品有最佳的耐熔性和耐热冲击性时，应使用基本上不含Ca、Na和K的原料。
工业上用于制造的热膨胀很低的挤压堇青石陶瓷体的优选批料是粘土、滑石和氧化铝，且粘土一般是片状高岭土，不是堆积高岭土。片状高岭土可通过对堆积高岭土进行预处理获得，或者可用将结晶堆积物分散成片晶的方式处理包含粘土的原料批料。
将干批料制成适于用烧制法转变为堇青石的预成形体(即生坯)可以用任何一种已知的技术进行。批料可以与合适的粘合剂混合，然后压制成预成形体的形状，也可以用热压法成形，视堇青石产品中所需的孔隙率而异。
为了在工业上制造平的或薄壁堇青石陶瓷产品(后者如陶瓷蜂窝)，优选的成形技术是挤压。适于挤压的批料混合物可通过将于批料与合适的液体载体混合而成。该载体可包括水和挤压助剂，加入挤压助剂是为了使批料可以成形并使成形的生坯具有足够的强度以免在烧制前破裂。也可以将挤压助剂与陶瓷批料混合。
挤压助剂一般含有粘合剂和增塑剂；甲基纤维素和碱金属硬脂酸盐是一些已经使用或可以使用的挤压助剂的例子。这种批料一般含有25-35％水，具有足够的可塑性，很容易用挤压法制成薄壁(即壁厚小于1毫米)的预成形体。经塑化的批料也可通常用滚压法或压制法成形，滚压或压制成的生坯部件可以直接去烧制或在装配成更复杂的形状部件才去烧制。用于陶瓷生坯转变为含堇青石的陶瓷产品的烧制工艺对制成陶瓷的性能起很大作用。目前使用的常规烧制工艺包括在1340-1450℃的温度，并保持一般含高达6％O2的氧化性气氛中进行烧制。虽然这种常规烧制工艺已制成一些适用的含堇青石的陶瓷产品，但现已发现，改进烧制工艺可以改善各种性能，包括强度和耐热冲击性。
按照本发明的方法，是使用一种四步的烧制方法获得堇青石蜂窝结构体。在该工艺中，先将陶瓷蜂窝结构体生坯加热到一个温度，在此温度下可以完全燃尽结构体内存在的有机物质并除去吸附水分。该第一烧制步骤一般需要加热到750-850℃之间的第一温度。在该第一烧制步骤后，第二烧制步骤是在O2含量不超过6％的氧化性气氛中将蜂窝结构体生坯进一步加热到约为1250-1350℃的第二温度。第三加热步骤是将陶瓷结构体生坯在仍保持O2含量不超过6％的氧化性气氛中加热到至少1390℃但低于1420℃的第三温度。最后，第四烧制步骤是在1390℃或更高的温度将结构蜂窝保温足够长的时间，使陶瓷体完全结晶化。保温时间大约12-20小时一般是足够的。在保温的第四步中，继续保持O2含量不超过6％的氧化性气氛。使用这种低氧的控制烧制工艺，可以获得具有比用常规烧制工艺烧制的堇青石陶瓷强度更高的堇青石陶瓷蜂窝结构体。
在上述四步烧制工艺的优选实施方式中，使用如下温度范围：(1)第一温度的范围约为790-810℃，800℃左右是最优选的温度；(2)第二温度的范围约为1275-1285℃，1280℃左右是最优选的温度；(3)第三温度的范围约为1400-1405℃，1430℃是最优选的。
上述四步烧制工艺的优选加速速率如下：(1)在从第一温度到第二温度范围的烧制过程中，优选的加热速率约为40-100℃；(2)在从第二温度到第三温度的烧制过程中，优选的加热速率约为10-50℃。
上述四步烧制工艺的优选气氛是保持如下O2含量的氧化性气氛：(1)在从第一温度到第二温度的整个烧制过程中约为5％O2；(2)在从第二温度到第三温度的整个烧制过程中约为1％O2；和(3)在整个保温过程中约为2％O2。
上述四步烧制的一个变化形式是在整个保温的第四烧制步骤中保持含2％CO的还原性气氛。用这种控制烧制工艺得到的陶瓷堇青石蜂窝结构体，其耐热冲击性一般比用常规烧制法制得的结构体更好，而强度相似。
在又一个实施方式中，蜂窝结构体生坯的烧制采用相同的第一烧制步骤，但在此第一烧制步骤后，接下来的三个烧制步骤虽是以前相同的温度条件，保持的却不是氧化性烧制气氛，而是CO含量不超过约3％的还原性烧制气氛。使用这种低还原性的控制烧制工艺，可以得到耐热冲击性、强度和烧制收缩率都比用常规烧制工艺烧制的堇青石陶瓷更高的堇青石陶瓷蜂窝结构体。
参照如下一些详细的实施例可以更好地理解本发明，但这些实施例仅用来说明本发明的优选实施方式。
实施例
制备了三种陶瓷批料。这些批料适用于制造具有如下组成(按重量份计)的含堇青石的陶瓷。
                             表I原料                            实施例1   实施例2   实施例3Georgia Kaolin Hydrite MP粘土    12.5％   12.5％    12.5％Georgia Kaolin Glomax LL粘土     21％     21％      21％Barretts Minerals 96-76滑石      35％     35％      35％Alcoa HVAFG氧化铝                14％     -         -Alcan C701RGE氧化铝              -        14％      14％Unimin Imsil二氧化硅             2.5％    2.5％     2.5％循环再用的生坯                   12％     12％      12％甲基纤维素增塑剂/粘合剂          2.5％    2.5％     2.5％碱金属硬脂酸挤压助剂             0.5％    0.5％     0.5％
将三种批料所含的原料充分混和，形成均匀的批料。
在“LODIGE”犁片剪切式混合器(Stamford，CT)中将水加入干的批料，由上述干的批料分别制成三个实施例的挤压批料。加水量约占总批料重量的31％，继续混合3分钟，获得混合均匀的批料。在约2800psi的压力下分别挤压这三个混合批料，形成直径为4.0-5.66″、长度为3.8-6.0″和有400个蜂窝/英寸2的蜂窝状生坯。
然后分别按如下表II和表III中所列的六种烧制工艺对获得的陶瓷蜂窝状生坯进行干燥和烧制，将其转变成堇青石陶瓷。所有的陶瓷生坯用表II和表III中所示相同的时间/温度规程和不同的烧制气氛进行烧制；这样，每种蜂窝状陶瓷生坯就转变为含堇青石的陶瓷蜂窝体。
具体如表II所示，所用的烧制工艺分为如下几类：(1)烧制工艺1表示采用常规气氛的烧制工艺；(2)烧制工艺2表示使用含O2量特别高的气氛的烧制工艺；(3)烧制工艺3表示使用含O2量低的气氛的本发明烧制工艺的一个实施方式；(4)烧制工艺4-6表示使用还原性气氛的本发明烧制工艺的一些实施方式。
                         表II
 烧制工艺编号     温度范围(℃)     烧制气氛
    123456     800-11601160-12801280-1403在1403℃保温800-11601160-12801280-1403在1403℃保温800-11601160-12801280-1403在1403℃保温800-11601160-12801280-1403在1403℃保温800-11601160-12801280-1403在1403℃保温800-11601160-12801280-1403在1403℃保温     6％O26％O26％O24％O29％O29％O27％O27％O25％O25％O21％O22％O26％O26％O26％O22％CO2％CO1％O22％CO2％CO2％CO2％CO2％CO2％CO
              表III
 加热速率(℃/小时)     温度范围(℃)
    5586100934072403576     室温-600℃600-700700-900900-10401040-11601160-12801280-13201320-13901390-13971397-1403
对烧制获得的堇青石陶瓷蜂窝体(三种相似的组成和使用6种不同气氛烧制的)进行了物理性能的测定。下表IV记录了三种挤压生坯在不同气氛下烧制的蜂窝体的测量结果。表IV中包括了每种陶瓷体的平均断裂模量(MOR)(单位为kPa)。也记录了各种陶瓷体在25-800℃范围内测得的平均热膨胀系数值(CTE)(单位为10-7/℃)以及平均烧制尺寸收缩率(单位为％)(即蜂窝体生坯和烧制蜂窝体的尺寸之差除以蜂窝体生坯尺寸所表示的百分数)。
                               表IV
  挤压料/实施例编号  烧制工艺     MOR(kPa)     CTE(10-7/℃)    收缩率(％)
    123     123456123456123456     10009601030102510301080935910955925970985104510401060101510751130     3.35------3.553.954.104.35------3.754.254.754.40------4.054.554.95     2.65------2.652.452.351.95------1.951.751.702.15------2.151.951.90
研究上述表中数据可得结果如下。首先，在低O2气氛条件下烧制的堇青石陶瓷体比在常规或高O2气氛条件下烧制的堇青石陶瓷体具有更高的MOR。图1更清楚地说明这个结果；即按烧制工艺3(低O2)烧制的三种组合物比按烧制工艺1或2烧制的相同组合物都具有更高的MOR。第二，在还原性条件下烧制的堇青石陶瓷体比在常规气氛烧制条件下烧制的堇青石陶瓷体具有更高的CTE。图2更清楚地说明这个结果；即按烧制工艺6(在整个烧制过程中保持2％CO)烧制的组合物比在烧制工艺1的常规烧制条件下烧制的相同组合物具有更高的CTE。第三，在还原性气氛条件下烧制的堇青石陶瓷体比在常规气氛烧制条件下烧制的陶瓷体具有更高的MOR。图3更清楚地说明这个结果；即在烧制工艺5或6的还原性条件下烧制的所有三种组合物比在烧制工艺1的常规气氛条件下烧制的相同组合物具有更高的MOR。最后，在还原性气氛条件下烧制的堇青石陶瓷体比在常规气氛烧制条件下烧制的陶瓷体具有更低的烧制收缩。图4更清楚地说明这个结论；即按烧制工艺5的还原性条件烧制的所有三个组合物比在烧制工艺1的常规气氛条件下烧制的相同组合物具有更低的烧制收缩百分率。
由上述的详细分析可知，本发明烧制工艺中所用的气氛的变化对堇青石陶瓷蜂窝结构体的性质、特别是强度和耐冲击性有显著的影响。因此，应当注意，每种情况下所用的气氛应按堇青石陶瓷结构体所需的性能根据实验加以确定。

Claims (23)

1.一种堇青石蜂窝结构体的制造方法，该方法包括如下步骤：
配制包含高岭土、滑石、氧化铝和其它堇青石形成材料的混合物批料，该批料中各种原料的含量是有效量，这些原料组合起来能产生主要结晶相为堇青石的烧制蜂窝体；
将该批料与有效量的载体和成形助剂均匀混合，所述的成形助剂能使批料具有可塑性并使形成的生坯具有一定强度；
用挤压法将批料成形为蜂窝结构体生坯，然后干燥该蜂窝结构体生坯；
按如下步骤烧制蜂窝结构体生坯：将该生结构体加热到为750-850℃的第一温度，然后加热到为1250-1350℃的第二温度，再加热到至少为1390℃的第三温度，最后在第三温度保温12-20小时，在第一温度以上的各个温度保持O2含量不超过6％的氧化性气氛。
2.如权利要求1所述的堇青石蜂窝结构体，其特征在于第一温度的范围为790-810℃。
3.如权利要求1所述的堇青石蜂窝结构体，其特征在于第一温度为800℃。
4.如权利要求1所述的堇青石蜂窝结构体，其特征在于第二温度的范围为1275-1285℃。
5.如权利要求1所述的堇青石蜂窝结构体，其特征在于从第一温度到第二温度范围的烧制期间使用40-100℃的加热速率。
6.如权利要求1所述的堇青石蜂窝结构体，其特征在于从第一温度到第二温度范围的烧制期间使用10-50℃的加热速率。
7.如权利要求1所述的堇青石蜂窝结构体，其特征在于第二温度为1280℃。
8.如权利要求1所述的堇青石蜂窝结构体，其特征在于第三温度为1403℃。
9.如权利要求1所述的堇青石蜂窝结构体，其特征在于从第一温度到第二温度的整个烧制期间保持O2含量为5％的氧化性气氛。
10.如权利要求1所述的堇青石蜂窝结构体，其特征在于在从第二温度到第三温度的整个烧制期间保持O2含量为1％的氧化性气氛。
11.如权利要求1所述的堇青石蜂窝结构体，其特征在于在整个保温期间保持O2含量为含2％的氧化性气氛。
12.如权利要求1所述的堇青石蜂窝结构体，其特征在于在整个保温期间保持CO含量为2％的还原性气氛。
13.一种堇青石蜂窝结构体的制造方法，该方法包括如下步骤：
配制包含高岭土、滑石、氧化铝和其它堇青石形成材料的混合物批料，该批料中各种原料的含量是有效量，这些原料组合起来能产生主要结晶相为堇青石的烧制蜂窝体；
将该批料与有效量的载体和成形助剂均匀混合，所述的成形助剂能使批料具有可塑性并使形成的生坯具有一定强度；
用挤压法将批料成形为蜂窝结构体生坯，然后干燥该蜂窝结构体生坯；
按如下步骤烧制蜂窝结构体生坯：将该生结构体加热到为750-850℃的第一温度，然后加热到为1250-1350℃的第二温度，再加热到至少为1390℃的第三温度，最后在第三温度保温12-20小时，在第一温度以上的各个温度保持CO含量不超过3％的还原性气氛。
14.如权利要求13所述的堇青石蜂窝结构体，其特征在于第一温度的范围为790-810℃。
15.如权利要求13所述的堇青石蜂窝结构体，其特征在于第一温度为800℃。
16.如权利要求13所述的堇青石蜂窝结构体，其特征在于第二温度为1275-1285℃。
17.如权利要求13所述的堇青石蜂窝结构体，其特征在于在从第一温度到第二温度范围的烧制期间使用40-100℃的加热速率。
18.如权利要求13所述的堇青石蜂窝结构体，其特征在于在从第二温度到第三温度范围的烧制期间使用10-50℃的加热速率。
19.如权利要求13所述的堇青石蜂窝结构体，其特征在于第二温度为1280℃。
20.如权利要求13所述的堇青石蜂窝结构体，其特征在于第三温度为1403℃。
21.如权利要求13所述的堇青石蜂窝结构体，其特征在于从第一温度到第二温度的整个烧制期间保持CO含量为2％的还原性气氛。
22.如权利要求13所述的堇青石蜂窝结构体，其特征在于在1100-1300℃的烧制期间保持O2含量不超过6％的氧化性气氛。
23.如权利要求1所述的堇青石蜂窝结构体，其特征在于所述的氧化性气氛含1％O2。
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