CN106083074B - 一种用于3D打印的Al2O3-ZrO2原料及生产高抗热震、特异形制品的工艺 - Google Patents

一种用于3D打印的Al2O3-ZrO2原料及生产高抗热震、特异形制品的工艺 Download PDF

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CN106083074B
CN106083074B CN201610388985.9A CN201610388985A CN106083074B CN 106083074 B CN106083074 B CN 106083074B CN 201610388985 A CN201610388985 A CN 201610388985A CN 106083074 B CN106083074 B CN 106083074B
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陈松林
袁林
魏瀚
王俊涛
刘锡俊
陈雪峰
胡建辉
胡建坤
刘士范
蒋正跃
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YIXING REFRACTORY MATERIAL CO Ltd
RUITAI TECHNOLOGY Co Ltd
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Abstract

本发明涉及一种利用Al2O3‑ZrO2陶瓷原料粉采用3D打印生产高抗侵蚀、高抗热震、特异形耐火材料的制品及其生产工艺。按比例混合α‑Al2O3粉、ZrO2粉、β‑Si3N4粉、Si粉、CeO2粉、MgAl2O4粉、聚羧酸粉，加水湿磨至d90为1～2μm，烘干得到混合粉，再将混合粉和丙烯酸酯按比例强力混碾，得到用于3D打印的陶瓷原料粉。用3D打印机打印成所需的特异形耐火材料制品，成型温度130～190℃，压力2～8MPa，经紫外线固化和烧结后制成。本发明生产工艺优势为无需等静压成形和后加工，使用优势为适用于洁净钢生产，对超洁净超低碳钢无污染，适用于连铸功能耐火材料、超洁净超低碳钢等领域的功能件等。

Description

一种用于3D打印的Al2O3-ZrO2原料及生产高抗热震、特异形制 品的工艺
技术领域
本发明涉及一种利用Al2O3-ZrO2陶瓷原料粉采用3D打印生产高抗侵蚀、高抗热震、特异形耐火材料的制品及其生产工艺，属无机非金属材料的耐火材料技术领域。该工艺优势为耐火材料制品具有高抗侵蚀和高抗热震性能，特别适用于特异形耐火材料制品，无需等静压成形和后加工，对超洁净超低碳钢无污染，适用于连铸功能耐火材料、超洁净超低碳钢等领域的功能件等。
背景技术
薄板坯浸入式水口是连续铸钢设备中安装在中间罐底部并插入结晶器钢液面以下的连铸用耐火套管。薄板坯浸入式水口的形状为扁平鸭嘴状，水口壁厚度仅为1cm左右，且不同位置上的管壁厚度不同，常伴有复合结构，这种特异型制品成型很困难，一般采用等静压成型工艺，生产成本高，且合格率很低。
3D打印技术具有成形复杂形状和保持精确尺寸的优势，采用3D打印技术开发无需等静压成形的特异形连铸用功能件成为首选的技术。通过人为的干涉，3D打印技术还可人为调节耐火材料的气孔率，提高耐火材料的抗热震性，从而使不含碳、不污染超洁净钢的复合材料可能成为连铸用耐火材料功能件。本发明就是引入ZrO2，采用丙烯酸酯作为粘结材料打印 Al2O3-ZrO2陶瓷坯体，经烧结获得大量微裂纹和微气孔，得到具有高抗侵蚀性、高抗热震性、特异形的连铸用功能耐火材料制品。
发明内容
本发明的目的是研究一种利用Al2O3-ZrO2陶瓷原料粉采用3D打印生产高抗侵蚀、高抗热震、特异形耐火材料的制品及其生产工艺，是发挥3D打印成复杂形状的优势，采用微裂纹和微气孔增韧机制提高不含碳的功能耐火材料抗热震性，通过引入ZrO2复合Al2O3材料，采用丙烯酸酯作为粘结材料打印Al2O3-ZrO2陶瓷坯体，经烧结获得大量微裂纹和微气孔，得到具有高抗侵蚀性、高抗热震性、特异形的功能耐火材料制品。
本发明的技术方案如下：
(1)所述陶瓷原料粉按重量百分比配料：80-90wt％的α-Al2O3粉、5-12wt％的ZrO2粉、2～4wt％的β-Si3N4粉、1～2wt％的Si粉、0.5～1.5wt％的CeO2粉、0.5～2wt％的MgAl2O4粉、0.2～0.5wt％的聚羧酸。
(2)一种利用Al2O3-ZrO2陶瓷原料粉采用3D打印生产高抗侵蚀、高抗热震、特异形耐火材料的制品的生产工艺为：将所述原料粉按比例混合，加水湿磨至d90为1～2μm，烘干，得到混合粉，将混合粉和丙烯酸酯按20～25∶1的比例强力混碾，将混碾后的粉料用3D打印机打印成所需的特异形耐火材料制品坯体，成型温度在130～190℃范围内，压力在2～8MPa的范围内，将坯体在紫外线箱内固化1～2h后再在1600℃保温5～8h烧成，得到所需的特异形耐火材料制品。
本发明的高抗侵蚀、高抗热震的特异形功能耐火材料件，在1100℃×0.5h水急冷的条件下，可循环15次以上，抗热震性优异。
本发明基于普通的3D打印技术，能满足各种特异形耐火材料制品的快速成形和精确尺寸打印要求，一次成形结构复杂的部件，无需再加工。
本发明的Al2O3-ZrO2陶瓷原料粉和制品及其生产工艺可以满足超洁净钢冶炼用功能件，还可用于生产各种要求具有高抗侵蚀性、高抗热震性、形状特殊的耐火材料制品。其打印速度快，成品率高、生产成本低，易推广应用，经济和社会效益前景十分广阔。
具体实施方式
实施例一
(1)将80wt％的α-Al2O3粉、12wt％的ZrO2粉、3wt％的β-Si3N4粉、2wt％的Si粉、1wt％的CeO2粉、1.5wt％的MgAl2O4粉、0.5wt％的聚羧酸。
(2)加水混合、湿磨至d90为1.5μm，烘干，得到混合粉。
(3)将得到的混合粉和丙烯酸酯按20∶1的比例强力混碾，得到用于3D打印的陶瓷原料粉。
(4)将陶瓷原料粉用3D打印机打印，成型参数为：成型温度在135±5℃范围，压力在 3±0.5MPa的范围内，成所需的特异形耐火材料制品。
(5)将特异形制品在紫外线箱内固化1h。
(6)将固化后的特异形制品在1600℃保温5h烧成，得到高抗侵蚀、高抗热震、特异形耐火材料制品。
本发明的高抗侵蚀、高抗热震的特异形功能耐火材料件，在1100℃×0.5h水急冷的条件下，经过19次循环断裂，抗热震性能优异。
实施例二
(1)将90wt％的α-Al2O3粉、5wt％的ZrO2粉、2wt％的β-Si3N4粉、1wt％的Si粉、0.5wt％的CeO2粉、1wt％的MgAl2O4粉、0.5wt％的聚羧酸。
(2)加水混合、湿磨至d90为2μm，烘干，得到混合粉。
(3)将得到的混合粉和丙烯酸酯按25∶1的比例强力混碾，得到用于3D打印的陶瓷原料粉。
(4)将陶瓷原料粉用3D打印机打印，成型参数为：成型温度在145±5℃范围，压力在 5±0.5MPa的范围内，成所需的特异形耐火材料制品。
(5)将特异形制品在紫外线箱内固化1.5h。
(6)将固化后的特异形制品在1600℃保温8h烧成，得到高抗侵蚀、高抗热震、特异形耐火材料制品。
本发明的高抗侵蚀、高抗热震的特异形功能耐火材料件，在1100℃×0.5h水急冷的条件下，经15次循环断裂，抗热震性能优异。
实施例三
(1)将85wt％的α-Al2O3粉、7wt％的ZrO2粉、4wt％的β-Si3N4粉、1wt％的Si粉、1wt％的CeO2粉、1.8wt％的MgAl2O4粉、0.2wt％的聚羧酸。
(2)加水混合、湿磨至d90为1μm，烘干，得到混合粉。
(3)将得到的混合粉和丙烯酸酯按25∶1的比例强力混碾，得到用于3D打印的陶瓷原料粉。
(4)将陶瓷原料粉用3D打印机打印，成型参数为：成型温度在180±5℃范围，压力在 7±0.5MPa的范围内，成所需的特异形耐火材料制品。
(5)将特异形制品在紫外线箱内固化2h。
(6)将固化后的特异形制品在1600℃保温5h烧成，得到高抗侵蚀、高抗热震、特异形耐火材料制品。
本发明的高抗侵蚀、高抗热震的特异形功能耐火材料件，在1100℃×0.5h水急冷的条件下，经16次循环断裂，抗热震性能优异。

Claims (1)

1.一种耐火材料制品的制备方法，其特征在于：所述原料粉的重量百分比为：
α-Al2O3粉， 80-90 wt%；
ZrO2粉， 5-12 wt%；
β-Si3N4粉， 2-4 wt%；
Si粉， 1-2 wt %；
CeO2粉， 0.5-1.5 wt%；
MgAl2O4粉， 0.5-2 wt %；
聚羧酸粉， 0.2-0.5 wt %；
将上述原料粉按比例混合，加水湿磨至d90为1～2μm，烘干，得到混合粉，将混合粉和丙烯酸酯按20～25:1的比例强力混碾，将混碾后的粉料用3D打印机打印成所需的特异形耐火材料制品坯体，成型参数为：成型温度在130～190℃范围内，压力在2～8MPa 的范围内，将坯体在紫外线箱内固化1～2h后再在1600℃保温5～8h烧成。
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