CN109320213A - 一种高致密度耐火陶瓷制品及其制备工艺 - Google Patents

一种高致密度耐火陶瓷制品及其制备工艺 Download PDF

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CN109320213A
CN109320213A CN201811203513.7A CN201811203513A CN109320213A CN 109320213 A CN109320213 A CN 109320213A CN 201811203513 A CN201811203513 A CN 201811203513A CN 109320213 A CN109320213 A CN 109320213A
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parts
green body
glaze
compactness
raw material
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李淑梅
郑贵霞
李俊英
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Quanzhou City Fujian Province Industry And Trade Co Ltd Fit
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Quanzhou City Fujian Province Industry And Trade Co Ltd Fit
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Abstract

本发明涉及陶瓷制品技术领域，具体涉及一种高致密度耐火陶瓷制品及其制备工艺，包括坯体和釉料，所述坯体包括：白云石45份、木质素磺酸钠9份、氮化锆19份、粘土16份、硅酸铝14份、助熔料15份、镁铝尖晶石22份、莫来石13份、钠长石12份、氧化铝18份；所述釉料包括：莫来石24份、高岭土35份、铝酸钙17份、钾长石17份、粘土13份、六偏磷酸钠6份，其制备工艺包括以下步骤：配料；压制成型；上釉；二次压制；烧成。本发明工艺所生产陶瓷制品具有机械强度高、耐火性能强的优点。

Description

一种高致密度耐火陶瓷制品及其制备工艺
技术领域
本发明涉及陶瓷制品技术领域，具体涉及一种高致密度耐火陶瓷制品及其制备工艺。
背景技术
陶瓷制品生产在中国历史悠久，经过长时间的发展，陶瓷的制作工艺不断的完善，赋予了陶瓷制品各种不同的性能，从而更多的用于人们生活、生产当中，各式各样的餐具、茶具、洁具都随处可见陶瓷制品的身影，这些陶瓷制品不仅外形美观、造型多样，同时还具有易清洗、耐腐蚀等优点，深受消费者的喜爱。然而现在市场对陶瓷制品的其他性能提出了要求，以制造相应的功能性陶瓷制品，例如对耐火性和机械强度的要求，因此为了满足市场需要，耐火性能和机械强度性能的提高研究应该早日被提上日程，同时，陶瓷的高致密度结构不仅可以减少颗粒间气孔的直径，促进烧结，降低烧结温度，而且还有利于提高陶瓷制品力学性能，因此，提高陶瓷致密度也成为了一种提高陶瓷机械性能的捷径。
发明内容
本发明的目的在于克服现有技术的不足，提供一种高致密度耐火陶瓷制品及其制备工艺。本发明工艺所生产的陶瓷制品具有机械强度高、耐火性能强的优点。
一种高致密度耐火陶瓷制品，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石42-48份、木质素磺酸钠7-11份、氮化锆16-23份、粘土15-18份、硅酸铝13-15份、助熔料13-16份、镁铝尖晶石21-23份、莫来石11-14份、钠长石8-15份、氧化铝16-22份；所述釉料包括以下重量份的原料：莫来石23-25份、高岭土32-36份、铝酸钙14-18份、钾长石15-19份、粘土10-15份、六偏磷酸钠4-7份。
进一步地，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石45份、木质素磺酸钠9份、氮化锆19份、粘土16份、硅酸铝14份、助熔料15份、镁铝尖晶石22份、莫来石13份、钠长石12份、氧化铝18份；所述釉料包括以下重量份的原料：莫来石24份、高岭土35份、铝酸钙17份、钾长石17份、粘土13份、六偏磷酸钠6份。
进一步地，所述助熔料由氧化钙和氧化镁按照重量比为3:2的比例混合而成。
本发明还提供一种制备所述高致密度耐火陶瓷制品的工艺，包括以下步骤：
步骤1、按照重量份称取坯体原料粉碎后放入球磨机中混合球磨，加入坯体原料总质量30-45％的水，球磨12-15h，通过100-200目筛后再于-23℃温度下冷冻干燥至含水量为5-8％，得到坯料；
步骤2、按照重量份称取釉料原料粉碎后放入球磨机中混合球磨，加入釉料原料总重量24-36％的水，球磨8-12h，通过6-8％万孔筛后再于-36℃温度下冷冻干燥至含水量为1-3％，得到釉料；
步骤3、将步骤1所得的坯料放入压制成型机的模具中，增大压制成型机中的压力至280-300Mpa，并升高压制成型机中的温度至550-700℃，热压35-40min后脱模，冷却至30-40℃，得到坯体，其中压制成型机是由创佳鸿机械设备有限公司生产的型号为CH-FM的压制成型机；
步骤4、将有机结合剂均匀涂覆于步骤3得到的坯体表面，涂覆量为坯体总质量的2.5-4％，再使用步骤2得到的釉料对坯体上釉，釉层厚度为0.3-0.5mm，放于温度为35-38℃，湿度为60-75％的环境中静置10-12h；
步骤5、将上釉后的坯体再次放入压制成型机的模具中，热压10-14min后脱模，热压温度为900-1150℃，热压压力为120-140Mpa，冷却至40-48℃，得到二次热压的坯体；
步骤6、将二次热压的坯体放入窑炉中烧成12-18h，烧成温度为1530-1640℃，得到高致密度耐火陶瓷制品；
进一步地，所述步骤3中加压速率为18-20Mpa/min，步骤5中加压速率为12-14Mpa/min。
进一步地，所述步骤4有机结合剂由羧甲基纤维素钠、氢化松香酯和水按照质量比为8:3:2的比例混合而成。
进一步地，所述步骤3和步骤5中热压前在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的1.8-2.4％。
有益效果
本发明的有益效果如下：
（1）、本发明采用白云石作为坯体的主要原料，当白云石经1500℃煅烧时，分解出氧化钙和氧化镁，其中氧化镁转变为方镁石，氧化钙转变为结晶a-CaO，结构致密，抗水性强，耐火度高达2300℃；氮化锆的加入可以提高陶瓷制品的硬度和耐热性能，然而其熔点较高，需要很高的烧成温度，因此本发明采用了氧化钙和氧化镁作为助熔剂，能显著减低氮化锆的熔融温度，并能促使钠长石的熔融，生成长石玻璃体充填于坯体的莫来石晶粒之间，使坯体致密而减少空隙，从而提高陶瓷制品的致密度以及机械强度；氧化铝和铝铁尖晶石本身具有高硬度和高熔点的特点，其加入可提升陶瓷制品的耐火性能和硬度；硅酸铝和粘土都具有很强的粘结性，能加强陶瓷中晶体之间的粘连，从而减少孔隙率，提高陶瓷致密度，而且硅酸铝常在工业上用作筑玻璃窑，具有优异的耐火性能，其加入能有效提高陶瓷制品的耐火性能；木质素磺酸钠作为减水剂，能减少坯体中的水分来降低其在烧成后的孔隙率，从而提高陶瓷的致密度；本发明采用莫来石、高岭土、铝酸钙、钾长石、粘土以及六偏磷酸钠作为釉料原料，莫来石具有膨胀均匀、热震稳定性极好、荷重软化点高、高温蠕变值小、硬度大的特点，在1300℃时抗弯强度达570MPa，断裂韧性KIC达5.7MPa，均比常温时高1.6倍，这种随温度升高，强度和韧性不仅不衰减反而大幅度提高，结合硅酸钙的低导热系数以及耐热性能，能大幅度提高釉层的耐火能力；六偏磷酸钠作为分散剂，能让釉料分散均匀，减少因流动不足而产生的空隙，从而提升釉层的致密度。
（2）、本发明使用压制成型机对坯体进行塑型，生产工艺简单，效率高，节省了成本；本发明在压制坯体的时候采用280-300Mpa的压力，并在二次热压时采用120-140Mpa的压力，压力对陶瓷制品的密度、强度、孔隙率等性能的影响比其他因素更重要，在上述压力范围内时，随着压力的增大，陶瓷的密度也显著的增大，而超过这一范围后压力的增长所带来的密度增大已经不太明显，这主要是由于模具内的颗粒开始是松散堆积的状态，因受到外界压力而发生位移，从而重新排列，细小的颗粒会填充大颗粒之间的缝隙，使陶瓷的致密度得到明显的提高，在上述压制过程中分别采用加压速率为18-20Mpa/min和12-14Mpa/min，加压速率对坯体的性能也有较大影响，如果加压过快，空隙中的气体就不容易完全排出，而加压速率太慢会导致生产率的降低；本发明在制备坯料和釉料时分别使用-23℃和-36℃的温度来进行冷冻干燥，能有效降低水分含量，水分含量对坯体和釉层的致密度有很大影响，含水量过大则干燥收缩大，对尺寸的控制就困难，并且成型时粉料易与模具发生粘连，从而影响坯体的致密度，含水量过小，又会影响造粒粉的破碎性能，不利于得到高致密度的坯体和釉料，冷冻干燥还能增强坯体和釉料的吸附性，利于釉料和坯体的结合；本发明中的氮化锆具有优异的耐火性及硬度，但它熔点高、高键能、低自扩散系数等特性导致其难以烧成致密，所以采用1530-1640℃的烧成温度能使其达到最高致密度。
（3）、本发明采用100-200目筛与6-8％万孔筛分别对坯体浆料与釉料浆料过筛，为的是控制陶瓷制品原料颗粒的细度，原料颗粒细度对陶瓷制品的致密度有着显著的影响，相同压力作用下，细度大的颗粒压坯密度大，细度小的颗粒烧成密度大，同一密度的颗粒，压坯密度和烧成密度均随压力增大而增大，因此，考虑到最终的陶瓷的烧成，颗粒细度在上述范围内能得到最好的陶瓷制品致密度；本发明采用由羧甲基纤维素钠、氢化松香酯和水按照质量比为8:3:2的比例混合而成的结合剂能有效增加坯体与釉层的粘结能力，采用由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂防止了颗粒受到压力而粘连在模具表面，造成破损。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明。
实施例1
一种高致密度耐火陶瓷制品，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石42份、木质素磺酸钠7份、氮化锆16份、粘土15份、硅酸铝13份、助熔料13份、镁铝尖晶石21份、莫来石11份、钠长石8份、氧化铝16份，所述助熔料由氧化钙和氧化镁按照重量比为3:2的比例混合而成；所述釉料包括以下重量份的原料：莫来石23份、高岭土32份、铝酸钙14份、钾长石15份、粘土10份、六偏磷酸钠4份。
本实施例还提供一种制备所述高致密度耐火陶瓷制品的工艺，包括以下步骤：
步骤1、按照重量份称取坯体原料粉碎后放入球磨机中混合球磨，加入坯体原料总质量30％的水，球磨12h，通过100目筛后再于-23℃温度下冷冻干燥至含水量为5％，得到坯料；
步骤2、按照重量份称取釉料原料粉碎后放入球磨机中混合球磨，加入釉料原料总重量24％的水，球磨8h，通过6％万孔筛后再于-36℃温度下冷冻干燥至含水量为1％，得到釉料；
步骤3、在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的1.8％，将步骤1所得的坯料放入压制成型机的模具中，增大压制成型机中的压力至280Mpa，加压速率为18Mpa/min，并升高压制成型机中的温度至550℃，热压35min后脱模，冷却至30℃，得到坯体；
步骤4、将由羧甲基纤维素钠、氢化松香酯和水按照质量比为8:3:2的比例混合而成的有机结合剂均匀涂覆于步骤3得到的坯体表面，涂覆量为坯体总质量的2.5％，再使用步骤2得到的釉料对坯体上釉，釉层厚度为0.3mm，放于温度为35℃，湿度为60％的环境中静置10h；
步骤5、在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的1.8％将上釉后的坯体再次放入压制成型机的模具中，热压10min后脱模，热压温度为900℃，热压压力为120Mpa，加压速率为12Mpa/min，冷却至40℃，得到二次热压的坯体；
步骤6、将二次热压的坯体放入窑炉中烧成12h，烧成温度为1530℃，得到高致密度耐火陶瓷制品；
实施例2
一种高致密度耐火陶瓷制品，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石45份、木质素磺酸钠9份、氮化锆19份、粘土16份、硅酸铝14份、助熔料15份、镁铝尖晶石22份、莫来石13份、钠长石12份、氧化铝18份；所述釉料包括以下重量份的原料：莫来石24份、高岭土35份、铝酸钙17份、钾长石17份、粘土13份、六偏磷酸钠6份。
本实施例还提供一种制备所述高致密度耐火陶瓷制品的工艺，包括以下步骤：
步骤1、按照重量份称取坯体原料粉碎后放入球磨机中混合球磨，加入坯体原料总质量37％的水，球磨13h，通过100目筛后再于-23℃温度下冷冻干燥至含水量为7％，得到坯料；
步骤2、按照重量份称取釉料原料粉碎后放入球磨机中混合球磨，加入釉料原料总重量32％的水，球磨10h，通过7％万孔筛后再于-36℃温度下冷冻干燥至含水量为2％，得到釉料；
步骤3、在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的2％，将步骤1所得的坯料放入压制成型机的模具中，增大压制成型机中的压力至290Mpa，加压速率为19Mpa/min，并升高压制成型机中的温度至620℃，热压37min后脱模，冷却至35℃，得到坯体；
步骤4、将由羧甲基纤维素钠、氢化松香酯和水按照质量比为8:3:2的比例混合而成的有机结合剂均匀涂覆于步骤3得到的坯体表面，涂覆量为坯体总质量的3％，再使用步骤2得到的釉料对坯体上釉，釉层厚度为0.4mm，放于温度为37℃，湿度为67％的环境中静置11h；
步骤5、在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的2.2％将上釉后的坯体再次放入压制成型机的模具中，热压12min后脱模，热压温度为1000℃，热压压力为130Mpa，加压速率为13Mpa/min，冷却至44℃，得到二次热压的坯体；
步骤6、将二次热压的坯体放入窑炉中烧成16h，烧成温度为1585℃，得到高致密度耐火陶瓷制品；
实施例3
一种高致密度耐火陶瓷制品，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石48份、木质素磺酸钠11份、氮化锆23份、粘土18份、硅酸铝15份、助熔料16份、镁铝尖晶石23份、莫来石14份、钠长石15份、氧化铝22份，所述助熔料由氧化钙和氧化镁按照重量比为3:2的比例混合而成；所述釉料包括以下重量份的原料：莫来石25份、高岭土36份、铝酸钙18份、钾长石19份、粘土15份、六偏磷酸钠7份。
本实施例还提供一种制备所述高致密度耐火陶瓷制品的工艺，包括以下步骤：
步骤1、按照重量份称取坯体原料粉碎后放入球磨机中混合球磨，加入坯体原料总质量45％的水，球磨15h，通过200目筛后再于-23℃温度下冷冻干燥至含水量为8％，得到坯料；
步骤2、按照重量份称取釉料原料粉碎后放入球磨机中混合球磨，加入釉料原料总重量36％的水，球磨12h，通过8％万孔筛后再于-36℃温度下冷冻干燥至含水量为3％，得到釉料；
步骤3、在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的2.4％，将步骤1所得的坯料放入压制成型机的模具中，增大压制成型机中的压力至300Mpa，加压速率为20Mpa/min，并升高压制成型机中的温度至700℃，热压40min后脱模，冷却至40℃，得到坯体；
步骤4、将由羧甲基纤维素钠、氢化松香酯和水按照质量比为8:3:2的比例混合而成的有机结合剂均匀涂覆于步骤3得到的坯体表面，涂覆量为坯体总质量的4％，再使用步骤2得到的釉料对坯体上釉，釉层厚度为0.5mm，放于温度为38℃，湿度为75％的环境中静置12h；
步骤5、在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂，涂抹量为坯体总质量的2.4％将上釉后的坯体再次放入压制成型机的模具中，热压14min后脱模，热压温度为1150℃，热压压力为140Mpa，加压速率为14Mpa/min，冷却至48℃，得到二次热压的坯体；
步骤6、将二次热压的坯体放入窑炉中烧成18h，烧成温度为1640℃，得到高致密度耐火陶瓷制品；
对比例1
对比例1与实施例2的原料配方与制备方法相同，不同之处在于对比例1坯体原料中将白云石与氮化锆换成了高岭土。
对比例2
对比例1与实施例2的原料配方与制备方法相同，不同之处在于对比例2中没有采用压制成型机对坯体以及釉料进行压制。
通过对实施例1-实施例3以及对比例1和对比例2所制成的陶瓷制品分别进型硬度、热稳定性以及导热系数测试，测试方法如下：
硬度测试：使用金刚石压头加载压入法，测试维氏硬度，即用对角面为136°的金刚石四棱椎体做压头，在9.807~490.3（1~50kgf）的载荷作用下，压入陶瓷表面，保持一定时间后卸除载荷，材料表面便留下一个压痕，测量压痕对角线的长度和压痕面积，求出单位面积上承受的载荷——应力，即维氏硬度HV，数值越高，硬度越大。
热稳定性测试：分别取5片陶瓷制品碎片作为试样，置于280℃条件下保温300分钟，保温结束后取出试样并进行核算，在15s内急速投入温度为20℃的水中，浸泡10分钟，其中，水的重量与试样重量之比为8：1，水面高出试样25mm，取出试样用布揩干，涂上红色墨水，检查有无裂纹，24 h后再复查一次，产生裂纹越少，试样的热稳定性越好。
导热系数测试：GB/T 17911-2006 《耐火材料陶瓷纤维制品测试方法》。
测试结果如下表1所示：
从上表1可以看出白云石与氮化锆作为坯体原料明显增强了陶瓷制品的耐火性和致密度，采用压制成型机进行压制提高了陶瓷制品的致密度，同时，实施例2各项检测数值均最好，为最优实施例。
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种高致密度耐火陶瓷制品，其特征在于，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石42-48份、木质素磺酸钠7-11份、氮化锆16-23份、粘土15-18份、硅酸铝13-15份、助熔料13-16份、镁铝尖晶石21-23份、莫来石11-14份、钠长石8-15份、氧化铝16-22份；所述釉料包括以下重量份的原料：莫来石23-25份、高岭土32-36份、铝酸钙14-18份、钾长石15-19份、粘土10-15份、六偏磷酸钠4-7份。
2.根据权利要求1所述的一种高致密度耐火陶瓷制品，其特征在于，包括坯体和釉料，所述坯体包括以下重量份的原料：白云石45份、木质素磺酸钠9份、氮化锆19份、粘土16份、硅酸铝14份、助熔料15份、镁铝尖晶石22份、莫来石13份、钠长石12份、氧化铝18份；所述釉料包括以下重量份的原料：莫来石24份、高岭土35份、铝酸钙17份、钾长石17份、粘土13份、六偏磷酸钠6份。
3.根据权利要求1或2所述的一种高致密度耐火陶瓷制品，其特征在于，所述助熔料由氧化钙和氧化镁按照重量比为3:2的比例混合而成。
4.一种制备权利要求1至2所述高致密度耐火陶瓷制品的工艺，其特征在于，包括以下步骤：
步骤1、按照重量份称取坯体原料粉碎后放入球磨机中混合球磨，加入坯体原料总质量30-45％的水，球磨12-15h，通过100-200目筛后再于-23℃温度下冷冻干燥至含水量为5-8％，得到坯料；
步骤2、按照重量份称取釉料原料粉碎后放入球磨机中混合球磨，加入釉料原料总重量24-36％的水，球磨8-12h，通过6-8％万孔筛后再于-36℃温度下冷冻干燥至含水量为1-3％，得到釉料；
步骤3、将步骤1所得的坯料放入压制成型机的模具中，增大压制成型机中的压力至280-300Mpa，并升高压制成型机中的温度至550-700℃，热压35-40min后脱模，冷却至30-40℃，得到坯体；
步骤4、将有机结合剂均匀涂覆于步骤3得到的坯体表面，再使用步骤2得到的釉料对坯体上釉，釉层厚度为0.3-0.5mm，放于温度为35-38℃，湿度为60-75％的环境中静置10-12h；
步骤5、将上釉后的坯体再次放入压制成型机的模具中，热压10-14min后脱模，热压温度为900-1150℃，热压压力为120-140Mpa，冷却至40-48℃，得到二次热压的坯体；
步骤6、将步骤5得到的二次热压的坯体放入窑炉中烧成12-18h，烧成温度为1530-1640℃，得到高致密度耐火陶瓷制品。
5.根据权利要求4所述的一种高致密度耐火陶瓷制品的制备工艺，其特征在于，所述步骤3中加压速率为18-20Mpa/min，步骤5中加压速率为12-14Mpa/min。
6.根据权利要求4所述的一种高致密度耐火陶瓷制品的制备工艺，其特征在于，所述步骤4有机结合剂由羧甲基纤维素钠、氢化松香酯和水按照质量比为8:3:2的比例混合而成。
7.根据权利要求4所述的一种高致密度耐火陶瓷制品的制备工艺，其特征在于，所述步骤3和步骤5中热压前在模具内表面涂抹了由甲基硅油、聚醚以及松香酸按照质量比为5:2:3的比例混合而成脱模剂。
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