CN105565818B - 一种碳氮化钛致密陶瓷的烧结方法 - Google Patents

一种碳氮化钛致密陶瓷的烧结方法 Download PDF

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CN105565818B
CN105565818B CN201510999877.0A CN201510999877A CN105565818B CN 105565818 B CN105565818 B CN 105565818B CN 201510999877 A CN201510999877 A CN 201510999877A CN 105565818 B CN105565818 B CN 105565818B
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王群
洪祥云
李永卿
王澈
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Abstract

一种碳氮化钛致密陶瓷的烧结方法属于无机陶瓷体制备领域。采用制备得到的TiN(1‑x)Cx为基材，本发明通过化学法在TiN(1‑x)Cx粉体表面包覆一层微量铁源，将处理后的粉体置于1600～2000℃氩气气氛下保温烧结，最终得到气孔率少，径向收缩率达13％，致密度高达99％的TiNC陶瓷体。本方法工艺简单，制备出的陶瓷体致密度高。

Description

一种碳氮化钛致密陶瓷的烧结方法
技术领域
本发明属于无机陶瓷制备领域，具体涉及一种碳氮化钛致密陶瓷烧结制备新工艺的开发优化
背景技术
通过TiN掺C即可得到“零维”固溶体TiNC，TiNC为FCC型 NaCl结构，继承了TiN的高硬度和TiC的高强度，以及高熔点、高耐蚀耐磨和高的化学稳定性等优点，是一种优良的非氧化物陶瓷材料。优异的力学性能使其填补了传统陶瓷与WC系硬质合金之间的空白，被广泛应用于切削刀具、耐磨涂层、陶瓷结构件等领域。
TiNC因具有高熔点，很难直接烧结致密，一般作为硬质相用于金属陶瓷烧结。传统TiNC基金属陶瓷一般添加Ni作为润湿相，添加Mo提高 Ni在TiNC中的润湿性，从而烧结成型。但这类金属陶瓷因添加相的引入而大大降低TiNC的内禀特性，不利于广泛应用。
发明内容
本发明旨在结合传统TiNC体系烧结方法，提出一种新型低气孔率、高收缩率、高致密度的TiNC致密陶瓷烧结制备工艺方法，此方法特征在与制备条件要求低、操作简单、陶瓷体致密度高。
上述目标通过以下步骤实现：
(1)化学包覆：将制备得到的TiN(1-x)Cx粉体置于 Fe(NO3)2/Fe(NO3)3溶液中，铁盐中Fe的含量为TiN(1-x)Cx的1.5～8wt％。机械搅拌24h后旋转蒸发干燥，研磨过筛。
(2)旋转蒸发：将步骤(1)中处理后得到的 TiN(1-x)Cx-Fe(NO3)2/Fe(NO3)3混合溶液置于旋转蒸发器中，70℃真空蒸发3～5h，干燥后过筛。
(3)低温还原：将步骤(2)中处理后得到的粉体装入氧化铝坩锅，置于反应气氛炉中。通入氢气，以5℃～15℃/min的升温速度升至 600～900℃，保温2～5h。
(4)机械成型：将步骤(3)中处理后的粉体与1～5wt％的PVB 混合造粒，在4～10MPa压力下压制成型。
(5)低温排胶：将步骤(4)中压制得到的粘接体置于石墨坩埚 中，使用TiN(1-x)Cx进行埋粉，将坩埚 置于 碳管炉中。打开机械泵，抽真空达 10-1Pa后以5℃～15℃/min的升温速度升温至400～600℃保温0.5～2h进行排胶处理。
(6)高温烧结：步骤(5)排胶处理完成后，关闭机械泵，通入流动氩气保护，以5℃～15℃/min的升温速度升温至1600～2000℃，保温1～6h。
与传统TiNC烧结方法相比，本方法操作简单，成本低，实验条件要求低，可重复性高；与未经Fe包覆处理的TiNC系列陶瓷体相比，经过 Fe包覆的TiNC陶瓷体致密度显著提高。具体见附图3、5。
与传统TiNC烧结方法相比，本方法通过化学法包覆Fe使得TiNC 表面活化，引入液相烧结机制，且Fe与TiNC中C形成晶界富集稳定相Fe3C，降低了TiNC烧结活化能，促进烧结致密化。具体见图4。
附图说明
图1为TiNC致密烧结工艺简图
图2为TiNC系列陶瓷体的XRD，其中(a)实例1；(b)实例2； (c)实例3 图3为TiNC系列陶瓷体断面SEM，其中(A)实例1中 Fe-TiN0.7C0.3；(a)实例1中TiN0.7C0.3；(B)实例2中Fe-TiN0.7C0.3；(b) 实例2中TiN0.7C0.3；(C)实例3中Fe-TiN0.7C0.3；(c)实例3中TiN0.7C0.3
图4为TiNC系列陶瓷体断面EDS，其中(a)TiN0.7C0.3(b) Fe-TiN0.7C0.3
图5为TiNC系列陶瓷体致密度及收缩率，其中(a)密度ρ(b) 径向收缩率(c)致密度Δρ
具体实施方式
碳氮化钛陶瓷材料烧结方法采用TiN(1-x)Cx(0＜x≤0.9)为基材，由于碳含量对烧结方法基本无影响，且不具工艺研究价值，因此实验实例采用TiN0.7C0.3为烧结基材。下面结合具体实例与上述附图对发明内容进行详细解释说明：
实例1：
(1)称取6g制备得到的TiN0.7C0.3粉体，置于含0.39g Fe(NO3)3的水溶液中，机械搅拌24h。
(2)将处理后的TiN0.7C0.3-Fe(NO3)3混合溶液置于 旋转蒸发器中，70℃真空蒸发3h，干燥后过筛。
(3)将(2)中处理的粉体装入氧化铝坩埚 ，置于 反应气氛炉中，通入氢气，以5℃/min的升温速度升至600℃，保温5h。
(4)将0.06g的PVB滴加到(3)步骤还原后得到的粉体中进行混合造粒，在4MPa压力下压制成圆片型粘接体。
(5)将(4)中压制得到的粘接体置于 石墨坩埚 中，使用TiN0.7C0.3粉进行埋粉。将坩埚 置于 碳管炉中，打开机械泵，抽真空达0.5×10-1Pa后以10℃ /min的升温速度升温至400℃保温0.5h进行排胶。
(6)排胶处理完成后，关闭机械泵，通入氩气保护，以5℃/min的升温速度升温至1600℃，保温1h后记得TiN0.7C0.3陶瓷材料。
(7)将此工艺下烧结得到的TiN0.7C0.3陶瓷材料进行致密度测试， SEM/EDS测试。可以看出未进行任何处理的TiN0.7C0.3陶瓷体密度为 3.481g/cm3，径向收缩率仅1.74％，致密度为65.31％；而进行Fe包覆处理的 Fe-TiN0.7C0.3陶瓷体密度为4.869g/cm3，径向收缩率为9.56％，致密度达 91.35％。
实例2：
(1)称取6g制备得到的TiN0.7C0.3粉体，置于 含1.04g Fe(NO3)3的水溶液中，机械搅拌24h。
(2)将处理后的TiN0.7C0.3-Fe(NO3)2混合溶液置于 旋转蒸发器中，70℃真空蒸发4h，干燥后过筛。
(3)将(2)中处理的粉体装入氧化铝坩埚 ，置于 反应气氛炉中，通入氢气，以10℃/min的升温速度升至700℃，保温3.5h。
(4)将0.12g的PVB滴加到(3)步骤还原后得到的粉体中进行混合造粒，在6MPa压力下压制成圆片型粘接体。
(5)将(4)中压制得到的粘接体置于 石墨坩埚 中，使用TiN0.7C0.3粉进行埋粉。将坩埚 置于 碳管炉中，打开机械泵，抽真空达0.5×10-1Pa后以15℃ /min的升温速度升温至500℃保温1h进行排胶。
(6)排胶处理完成后，关闭机械泵，通入流动氩气保护，以10℃/min 的升温速度升温至1800℃，保温3h后得TiN0.7C0.3/Fe-TiN0.7C0.3陶瓷体。
(7)将此工艺下烧结得到的TiN0.7C0.3陶瓷体进行致密度测试，SEM/EDS 测试。可以看出未经过处理的TiN0.7C0.3陶瓷体密度为3.585g/cm3，径向收缩率仅2.26％，致密度为68.55％；而进行Fe包覆处理的Fe-TiN0.7C0.3陶瓷体密度为5.018g/cm3，径向收缩率为10.78％，致密度达95.95％。 TiN0.7C0.3/Fe-TiN0.7C0.3陶瓷体致密度较实例1中陶瓷体有所提升，说明烧结温度和时间的提升有助于陶瓷体致密化。
实例3：
(1)称取6g制备得到的TiN0.7C0.3粉体，置于 含1.54g Fe(NO3)2的水溶液中，机械搅拌24h。
(2)将处理后的TiN0.7C0.3-Fe(NO3)3混合溶液置于 旋转蒸发器中，70℃真空蒸发5h，干燥后过筛。
(3)将(2)中处理的粉体装入氧化铝坩埚 ，置于 反应气氛炉中，通入氢气，以15℃/min的升温速度升至900℃，保温2h。
(4)将0.3g的PVB滴加到(3)步骤还原后得到的粉体中进行混合造粒，在10MPa压力下压制成圆片型粘接体。
(5)将(4)中压制得到的粘接体置于 石墨坩埚 中，使用TiN0.7C0.3粉进行埋粉。将坩埚 置于 碳管炉中，打开机械泵，抽真空达0.5×10-1Pa后以20℃ /min的升温速度升温至600℃保温2h进行排胶。
(6)排胶处理完成后，关闭机械泵，通入流动氩气保护，以15℃/min 的升温速度升温至2000℃，保温6h后得TiN0.7C0.3/Fe-TiN0.7C0.3陶瓷体。
(7)将此工艺下烧结得到的TiN0.7C0.3陶瓷体进行致密度测试，SEM/EDS 测试。可以看出未经过任何处理的TiN0.7C0.3陶瓷体密度为3.626g/cm3，径向收缩率为2.96％，致密度为72.09％；而进行Fe包覆处理的Fe-TiN0.7C0.3陶瓷体密度为5.025g/cm3，径向收缩率达13.04％，致密度高达99.9％。TiN0.7C0.3/ Fe-TiN0.7C0.3陶瓷体致密度较实例1、2中陶瓷体有所提升，说明温度和时间的提升有助于TiNC陶瓷体致密化。

Claims (4)

1.一种碳氮化钛致密陶瓷的烧结方法，其特征在于：采用TiN(1-x)Cx以及铁盐为原料，TiN(1-x)Cx中0＜x＜1，通过化学法在TiN(1-x)Cx粉体表面包覆一层铁盐，Fe的含量为TiN(1-x)Cx的1.5～8at％；还原铁盐后，置于1600～2000℃氩气气氛下保温烧结，最终得到TiNC致密陶瓷体；
步骤如下：(1)化学包覆：将TiN(1-x)Cx粉体置于 铁盐溶液中，铁盐中Fe的含量为TiN(1-x)Cx的1.5～8at％；机械搅拌12-24h后旋转蒸发干燥，研磨过筛；
(2)低温还原：将经过步骤(1)处理后的粉体平铺于氧化铝坩埚 ，置于反应气氛炉中，通入氢气，以5～15℃/min的升温速度升温至600～900℃，保温2～5h还原铁盐；
(3)高温烧结：将经过步骤(2)还原后的粉体加入粘接剂后压制成型，将压制成型的粘接体埋入TiNC粉体内，置于反应气氛炉中，通入流动的氩气，排胶后以5～15℃/min的升温速度升高温度至1600～2000℃，保温1～6h。
2.根据权利要求1中所述的方法，其特征在于：步骤(1)中铁盐为Fe(NO3)2或Fe(NO3)3。
3.根据权利要求1中所述的方法，其特征在于：步骤(3)中使用的 粘接剂为石蜡、PVB或者PVA，加入量为TiNC粉体的1～5wt％。
4.根据权利要求1中所述的方法，步骤(3)中其特征在于：排胶温度400～600℃，时间0.5～2h。
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