CN106631032B - 一种高纯二硼化钛粉体及其制备方法 - Google Patents

一种高纯二硼化钛粉体及其制备方法 Download PDF

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CN106631032B
CN106631032B CN201610890116.6A CN201610890116A CN106631032B CN 106631032 B CN106631032 B CN 106631032B CN 201610890116 A CN201610890116 A CN 201610890116A CN 106631032 B CN106631032 B CN 106631032B
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黄小红
侯广生
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Shandong Jingyi New Material Co.,Ltd.
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Abstract

本发明公开了一种高纯的二硼化钛粉体及其制备方法。该粉体由以下质量百分比的原料成分经混料、煅烧、精磨而成；碳化硼25～45wt.％,二氧化钛30～50wt.％，炭黑15～35wt.％，催化剂1～5wt.％，各成分用量之和为100％。将原料放入刀型混料机中干混30‑60min；直接放入中频加热炉中烧成，烧成温度2000‑2200℃，烧成30‑40h,自然冷却；将结晶体置于快速磨中精磨得到需求的均匀粒度的二硼化钛粉体。本发明工艺简单、产物稳定，得到的粉体纯度高，粒度分布均匀。

Description

一种高纯二硼化钛粉体及其制备方法
技术领域
本发明属于新材料粉末冶金领域，特别涉及一种高纯二硼化钛粉末及其制备方法。
背景技术
二硼化钛是一种性能优异的新型材料，特点是高熔点(2980℃)、高硬度 (2800-3400kg/m2，显微硬度为2.9GPa)、优良的抗氧化性及导电性能。由于其可抗熔融金属的腐蚀，可用于熔融金属坩埚 和电解池电极的制造；可作为多元复合材料的重要组元，与 TiC、TiN、SiC等材料组成复合材料，制作各种耐高温部件及功能部件，如高温坩埚、引擎部件等，也是制作装甲防护材料的最好材料之一。
关于二硼化钛粉体的合成已有较多的报道。东北大学王兆文等(王兆文,邱竹贤.二硼化钛粉末的研制[J].轻金属,1997(8):28-32.)总结了二硼化钛粉末的研究进展，认为：二硼化钛粉末的制备方法有直接合成法、气相沉积法、金属还原法、碳热还原法、熔盐电解法和溶剂法等，其中直接合成法和气相沉积法是两种获得较高纯度二硼化钛粉体的有效方法。直接合成法是用金属钛和硼直接反应合成二硼化钛，该法具有反应温度较低，反应条件易控以及反应产物较纯的优点，但原料金属钛和硼价格昂贵，不适用于工业批量生产。气相沉积法可得到纯度较高的二硼化钛，但产物产量低、反应时间长，只适用于少量制取和表面镀膜使用。
如何研究一种纯度高、粒度小且均匀、工艺简单的二硼化钛粉体制备方法是国内外学者的研究热点。中国专利文件CN 105439161 A公开了一种二硼化钛纳米颗粒的制备方法：将硼酸、石墨、镁粉、硬脂酸按着比例配料，置于氩气保护的球磨中球磨3-8小时，然后在氩气的保护下于800-1000℃下煅烧，保温0.5-3h，然后酸洗除去杂质,再经多次水洗、烘干得到二硼化钛纳米粉体。本方法制得二硼化钛的纯度高，但混料时间长，且球磨介质容易引入杂质，工艺繁琐，需要多次酸洗、水洗清除杂质。中国专利文件CN1371863A公开了一种二硼化钛纳米粉的制备方法：将平均粒径为5μm的二硼化钛粉末以球料比20:1高能球磨40～50h，于浓盐酸水溶液或浓硝酸、浓磷酸水溶液搅拌30min，静置10min后水洗2～3次，抽滤、烘干即得所需产品。该方法工艺简单、粉末均匀，适宜大规模生产，但其本质是二硼化钛自身的物理粉碎，原料成本较高。
因此，探究一种低成本、工艺简单、生产效率高的制备方法，制备一种纯度高，粒度均匀的二硼化钛粉体，是本发明的主要研究方向。
发明内容
本发明要解决的技术问题是通过改变生产工艺和生产条件，生产一种晶粒粒度分布均匀，纯度高达99.5％的二硼化钛粉体。本发明工艺简单、产物稳定、收率较高，得到的粉体纯度高，粒度分布均匀。
本发明要解决的技术问题的技术方案是：
该粉体由以下质量百分比的原料成分经混料、煅烧、精磨而成；碳化硼25～45wt.％,二氧化钛30～50wt.％，炭黑15～35wt.％，催化剂1～5wt.％，各成分用量之和为100％。
所述的碳化硼的平均粒径为1～50μm，富硼含量≥28％，进一步所选的，所述碳化硼的平均粒径为15～35μm,富硼含量≥50％。
所述的二氧化钛的平均粒径为3～8μm，纯度为≥99％，进一步所选的，所述二氧化钛的平均粒径为6～8μm，纯度≥99.9％。
所述的炭黑的平均粒径为0.1～1μm，进一步所选的，所述炭黑的平均粒径为0.1～0.5 μm。
所述的催化剂由以下组分组成及各组分的质量百分比如下：氧化锆10～35wt.％，氧化钇20～50wt.％，氧化铌30～50wt.％，各成分用量之和为100％。
高纯二硼化钛粉体的制备方法，包括步骤如下：
⑴按配比将原料放入刀型混料机的储料斗中干混30-60min；
⑵将干混后的原料直接装入带有隔层的坩埚中，进窑；
⑶利用中频加热炉进行烧结，升温速率为5～10℃/min，烧结温度2000～2200℃，高温烧结30～40小时，自然冷却出炉；
⑷将烧结后的产物经过气流磨精磨，根据调节气流磨的频率和研磨时间，得到需要的粒度范围。
进一步，所述的步骤⑴中的刀型混料机的储料斗采用不锈钢材质。
进一步，所述的步骤⑵中的隔层材质为一种高含量碳化钛或氮化钛高温耐火填料。
本发明的优异效果：
⑴混料过程中的刀型混料机，能够快速混料均匀，提高了3-10倍的效率；且混料机的储料斗为不锈钢材质，且混料过程中没有使用其他介质，所以，此工艺过程不会添入杂质。
⑵烧结载体中使用的高温耐火填料的隔层，避免了原料与坩埚直接接触，防止发生反应，减少了结晶体的污染；现在技术中，原料直接与坩埚接触烧结，烧结晶体收率仅有10-15％，此工艺方法收率能达50％以上，极大地提高了反应收率。
⑶2000～2200℃的烧结温度，30～40h的烧结时间，增大结晶体粒度，粒度可达300-1500 μm，结晶粒度增大，提高了二硼化钛晶体的纯度，同时硬度能够提高5倍左右，在本行业具有技术革命性创新。
⑷采用的气流磨精磨工艺过程，没有使用任何研磨介质，不会引入其他杂质，此工艺制备的二硼化钛粉体纯度高达99.5％；通过调节气流磨的速度和时间，能够研磨得到需要的 1-100μm不等的均匀粒度，做到粒度精准控制，保证后期制备的产品能有均匀的致密度和较高硬度。
(5)此制备工艺简单易操作，每个工艺过程均可做到精准控制，适用于工业大规模生产。
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明，但本发明所保护范围不限于此。
原料说明：
本发明所用的各型平均粒径不同的碳化硼微粉、二氧化钛微粉、炭黑微粉以及催化剂成分中氧化锆、氧化钇、氧化铌粉末均为市售原料。
实施例1
一种高纯二硼化钛粉体的制备方法，包括步骤如下：
(1)将B丰度为25％的碳化硼粉体(平均粒径为15～35μm)40kg，锐钛型二氧化钛(平均粒径为6～8μm)35kg，炭黑(平均粒径为0.1～0.5μm)24kg和氧化锆(平均粒径为10～20 μm)0.33kg，氧化钇(平均粒径为10～20μm)0.33kg，氧化铌(平均粒径为10～20μm)0.34g，在刀型混料机中混合60min；
(2)将干混后的原料转移至中频感应烧结炉，在氩气氛围中升温至2100℃，烧结时间为 35h，升温速率为8℃/min；
(3)将烧结后的产物用气流磨精磨2h，后得到粒径为1～5μm的粒度均匀的二硼化钛粉体。主晶相为TiB2相，纯度为99.5％。
实施例2
一种高纯二硼化钛粉体的制备方法，包括步骤如下：
(1)将B丰度为50％的碳化硼粉体(平均粒径为1～35μm)45kg，锐钛型二氧化钛(平均粒径为6～8μm)30kg，炭黑(平均粒径为0.1～0.5μm)20kg和氧化锆(平均粒径为10～20 μm)1.25kg，氧化钇(平均粒径为10～20μm)2.5kg，氧化铌(平均粒径为10～20μm)1.25g，在刀型混料机中混合60min；
(2)将干混后的原料转移至中频感应烧结炉，在氩气氛围中升温至2000℃，烧成时间为 40h，升温速率为5℃/min；
(3)将烧结后的产物用气流磨精磨1h，后得到粒径为3～8μm的粒度均匀的二硼化钛粉体。主晶相为TiB2相，纯度为99％。
实施例3
一种高纯二硼化钛粉体的制备方法，包括步骤如下：
(1)将B丰度为60％的碳化硼粉体(平均粒径为1～35μm)25kg，锐钛型二氧化钛(平均粒径为6～8μm)50kg，炭黑(平均粒径为0.1～0.5μm)24kg和氧化锆(平均粒径为10～20 μm)0.3kg，氧化钇(平均粒径为10～20μm)0.2kg，氧化铌(平均粒径为10～20μm)0.5g，在刀型混料机中混合60min；
(2)将干混后的原料转移至中频感应烧结炉，在氩气氛围中升温至2200℃，烧成时间为 30h，升温速率为10℃/min；
(3)将烧结后的产物用气流磨精磨30min，后得到粒径为30-50μm的粒度均匀的二硼化钛粉体。主晶相为TiB2相，纯度为99.3％。
对比例1：
如实施例1所述，不同的是步骤(2)中烧结温度为1900℃。所得产品主晶相为TiB2和TiB相，TiB2纯度为90％。
对比例2：
如实施例1所述，不同的是步骤(1)中原料不使用催化剂。所得产品主晶相为TiB2和 TiC相，TiB2纯度为95％。
通过对比实施例1和对比例1-2可知，当烧结温度为1900℃时，碳热还原反应不够彻底，生成物是二硼化钛和一硼化钛的混合物，目标产物的纯度明显降低。当没有催化剂引入时，反应程度有所下降，生成物是二硼化钛和碳化钛的混合物，目标产物的纯度也有一定程度的降低。
需要说明的是，以上列举的仅是本发明的若干个具体实施例，显然本发明不仅仅限于以上实施例，还可以有其他变形。本领域的技术人员从本发明公开内容直接导出或间接引申的所有变形，均应认为是本发明的保护范围。

Claims (7)

1.一种高纯二硼化钛粉体，其特征在于，该粉体由以下质量百分比的原料成分经混料、煅烧、精磨而成，其组分为：
碳化硼25～45wt.％
二氧化钛30～50wt.％
炭黑15～35wt.％
催化剂1～5wt.％，各成分用量之和为100％；
所述的催化剂由以下组分组成且各组分的质量百分比如下：
氧化锆10～35wt.％
氧化钇20～50wt.％
氧化铌30～50wt.％，各成分用量之和为100％；
所述高纯二硼化钛粉体的制备方法，包括步骤如下：
⑴按配比将原料放入刀型混料机的储料斗中干混30-60min；
⑵将干混后的原料直接装入带有隔层的坩埚中，进窑；
⑶利用中频加热炉进行烧结，升温速率为5～10℃/min，烧结温度2000～2200℃，高温烧结30～40小时，自然冷却出炉；
⑷将烧结后的产物经过气流磨精磨，根据调节气流磨的频率和研磨时间，得到需要的粒度范围。
2.根据权利要求1所述的高纯二硼化钛粉体，其特征在于，所述的碳化硼的平均粒径为1～50μm，富硼含量≥28％。
3.根据权利要求1所述的高纯二硼化钛粉体，其特征在于，所述的二氧化钛的平均粒径为3～8μm，纯度为≥99％。
4.根据权利要求1所述的高纯二硼化钛粉体，其特征在于，所述的炭黑的平均粒径为0.1～1μm。
5.一种权利要求1-4任一项所述的高纯二硼化钛粉体的制备方法，包括步骤如下：
⑴按配比将原料放入刀型混料机的储料斗中干混30-60min；
⑵将干混后的原料直接装入带有隔层的坩埚中，进窑；
⑶利用中频加热炉进行烧结，升温速率为5～10℃/min，烧结温度2000～2200℃，高温烧结30～40小时，自然冷却出炉；
⑷将烧结后的产物经过气流磨精磨，通过调节气流磨的频率和研磨时间，得到需要的粒度范围。
6.根据权利要求5所述的高纯二硼化钛粉体 的制备方法，其特征在于，步骤⑴中的刀型混料机的储料斗采用不锈钢材质。
7.根据权利要求5所述的高纯二硼化钛粉体 的制备方法，其特征在于，所述的步骤⑵中的隔层材质为一种高含量碳化钛或氮化钛高温耐火填料。
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