CN113735585A - 一种氧化铝/钛硅碳复合材料的制备方法 - Google Patents
一种氧化铝/钛硅碳复合材料的制备方法 Download PDFInfo
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- CN113735585A CN113735585A CN202110987687.2A CN202110987687A CN113735585A CN 113735585 A CN113735585 A CN 113735585A CN 202110987687 A CN202110987687 A CN 202110987687A CN 113735585 A CN113735585 A CN 113735585A
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- composite material
- titanium
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- alumina
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000010936 titanium Substances 0.000 title claims abstract description 30
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 20
- 239000002153 silicon-carbon composite material Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000002131 composite material Substances 0.000 claims abstract description 24
- -1 titanium aluminum carbon Chemical compound 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims description 29
- 238000000498 ball milling Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- DXZIFGZIQQRESB-UHFFFAOYSA-N [C].[Ti].[Si] Chemical compound [C].[Ti].[Si] DXZIFGZIQQRESB-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000919 ceramic Substances 0.000 abstract description 10
- 238000005452 bending Methods 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 14
- 229910000831 Steel Inorganic materials 0.000 description 12
- 239000010959 steel Substances 0.000 description 12
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 238000005498 polishing Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 4
- 229910009817 Ti3SiC2 Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于陶瓷复合材料的制备技术领域，具体涉及一种氧化铝/钛硅碳复合材料的制备方法。所述的复合材料由钛铝碳（Ti3AlC2），一氧化硅（SiO）均匀接触，真空烧结即可。本发明通过铝和硅的相互扩散，得到氧化铝/钛硅碳复合材料。本发明制备的复合材料具有高致密性，且性能稳定，复合材料中，氧化铝通过钛铝碳和一氧化硅反应生成的，能均匀包覆在钛硅碳晶体的表面，形成一种较为致密的氧化膜，阻碍了基体与外界的物质交换，提高了符合材料整体的抗氧化性能，钛硅碳又增强了复合材料的韧性，制备的复合材料纯度较高，烧结温度较低，并且具备较高的抗弯强度本发明工艺简单，易于工业化生产。
Description
技术领域
本发明属于陶瓷基复合材料领域，具体涉及一种以一氧化硅/钛铝碳(SiO/Ti3AlC2)为原料制备氧化铝/钛硅碳（Al2O3/Ti3SiC2）复合材料的制备方法。
背景技术
氧化铝因其高熔点，高强度，抗氧化，耐高温的优点，是一种极具前景的陶瓷基体材料。但是，氧化铝陶瓷的韧性较低，限制了在工业领域中的应用。MAX陶瓷，MAX相是指三元过渡族金属碳化物或氮化物，其化学通式为“Mn+1AXn”，其中M代表过渡族金属元素，A代表ⅢA或ⅣA族元素，X代表C或N, n=1～3，在陶瓷材料中具备较高韧性，而且MAX相陶瓷的热膨胀系数与氧化铝比较接近，适合与氧化铝陶瓷做结合使用，优势互补，以期获得的具备更好力学性能的新型结构材料。
MAX相陶瓷特别是钛硅碳陶瓷材料与氧化铝的结合已有研究，但是，目前，直接使用钛硅碳与氧化铝粉体制备致密的陶瓷复合材料所需烧结温度较高，约1450℃；钛硅碳与氧化铝界面处无明显反应；容易发生分解，产生碳化钛等杂质。
发明内容
针对现阶段氧化铝/钛硅碳陶瓷复合材料合成中存在的问题，本发明提供了一种氧化铝/钛硅碳复合材料的制备方法，该方法使用钛铝碳/一氧化硅为原材料制备出钛硅碳/氧化铝复合材料，具有较高的抗弯强度。
本发明为了实现上述目的所采用的技术方案为：
一种氧化铝/钛硅碳复合材料的制备方法，所述复合材料以钛铝碳Ti3AlC2粉和一氧化硅SiO粉为原料制备而成。
上述制备方法具体包括以下步骤：
（1）将原料钛铝碳Ti3AlC2粉和一氧化硅SiO粉采用混合均匀，得混合料；
（2）将混合料进行保温加压烧结，保温加压程序结束后随炉降温，降温后关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
进一步的，步骤（1）中，所述钛铝碳的粒径为3-15 μm，一氧化硅的粒径为0.5-5μm，纯度为99.9%。
进一步的，步骤（1）中，所述混合方法为将钛铝碳粉、一氧化硅粉混合，进行球磨混合。
上述混合方法中，钛铝碳与一氧化硅的摩尔比例为1：0.5-1.5。
进一步的，步骤（2）中，所述保温烧结为首先以1-10℃的升温速率升温至1200℃，然后以5-20℃/min的升温速率升温至1250 ℃-1350 ℃，保温1.5-3 h，烧结压力为25-35MPa。
本发明是通过化学反应使一种成本较低的MAX相材料（钛铝碳）转化为另一种MAX相（钛硅碳）材料，同时生成氧化铝的方法。
本发明的有益效果
1、本发明制备的复合材料具有高致密性，且性能稳定，复合材料中，氧化铝通过钛铝碳和一氧化硅反应生成的，能均匀包覆在钛硅碳晶体的表面，形成一种较为致密的氧化膜，阻碍了基体与外界的物质交换，提高了符合材料整体的抗氧化性能，钛硅碳又增强了复合材料的韧性，制备的复合材料纯度较高，烧结温度较低，并且具备较高的抗弯强度
2、本发明工艺简单，易于工业化生产。
附图说明
图1为本发明利用混合法烧结制备的钛硅碳/氧化铝复合材料的X射线衍射图谱。
图2为本发明利用混合法烧结制备的钛硅碳/氧化铝复合材料的微观图像。
图3为本发明利用混合法烧结制备的钛硅碳/氧化铝复合材料的元素分析图。
具体实施方式
下面通过实例对本发明做进一步地阐述，需要强调的是，下述说明仅是为了解释本发明，并不对其内容进行限定。
实施例1
（1）将称得44.22g的粒径10微米左右的钛铝碳（Ti3AlC2）和10.01g的粒径1-5微米的的氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约54.23g，用玻璃棒搅拌，使混合料更加均匀；然后放入108.81g的钢球，使得混合料与球的质量比大致为1：2；
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料；
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以10 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1300℃，在1300 ℃时保温120分钟，烧结压力为30 MPa，温度升至1300℃前开启加压程序，保压120分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
实施例2
（1）将称得43.92g的粒径8微米左右的钛铝碳（Ti3AlC2）和9.99g的粒径1-5微米一氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约53.91g，用玻璃棒搅拌，使混合料更加均匀。然后放入107.54g的钢球，使得混合料与球的质量比大致为1：2。
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料。
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以8 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1340℃，在1340 ℃时保温120分钟，烧结压力为30 MPa，温度升至1340℃前开启加压程序，保压120分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
实施例3
（1）将称得44.13g的粒径10微米左右的钛铝碳（Ti3AlC2）和10.82g的粒径1-5微米一氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约54.95g，用玻璃棒搅拌，使混合料更加均匀。然后放入110.69g的钢球，使得混合料与球的质量比大致为1：2。
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料。
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以12 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1280℃，在1280 ℃时保温120分钟，烧结压力为35 MPa，温度升至1280℃前开启加压程序，保压120分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
实施例4
（1）将称得44.03g的粒径12微米左右的钛铝碳（Ti3AlC2）和10.55g的粒径0.5-3微米一氧化硅（SiO）加入到行星式球磨机钢罐中，形成钛铝碳与一氧化硅摩尔比1：1左右的混合料，共计约54.58g，用玻璃棒搅拌，使混合料更加均匀。然后放入109.9g的钢球，使得混合料与球的质量比大致为1：2。
（2）将步骤（1）中装有混合料的行星式球磨机钢罐放入行星式球磨机，设置球磨速度70r/min，每30 min暂停10 min，共计球磨时间2 h，暂停时间30 min。球磨完成后，取出混合料。
（3）将步骤（2）中得到得混合料，以下“压头-垫片-碳纸-混合料-碳纸-垫片-上压头”的结构，全部装入直径约45 mm 空心圆柱型石墨模具，放入真空热压炉，打开真空系统抽真空，然后以1 ℃/分钟的升温速率升至1200 ℃，再以5℃ /分钟的升温速率升至1280℃，在1280 ℃时保温100分钟，烧结压力为30 MPa，温度升至1280℃前开启加压程序，保压100分钟。保温加压程序结束后随炉降温，降温至200 ℃时，关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
（4）使用砂纸和抛光机将步骤（3）中的薄饼状氧化铝/钛硅碳复合材料的表面抛光去除与样品表面结合的碳纸，得到可用的样品。
效果实施例
（一）将实施例1-4制备的复合材料进行抗弯强度检测，具体检测结果见表1。
抗弯强度检测使用三点弯曲法测试试样的弯曲强度。首先将烧结后的陶瓷圆片放到磨床上粗磨，目的是除去样品表面覆盖的石墨纸和杂质，并将样品表面大致磨平；然后将大致磨平的样品进行抛光，最后将抛光后的试样用线切割机切成所需要的试样条，试样条的表面光滑，无肉眼可见缺陷，尺寸为长36mm，宽4mm，高3mm。试样测试实际跨距为30mm。利用电子万能材料试验机对制得的试样进行弯曲强度测试，测试时试验机上压头下压的速度为0.5 mm/min。记录载荷P，计算出抗弯强度。每个样品制备三个试样条测试三次，最后计算均值。
抗弯强度根据以下材料的弯曲强度公式计算：
表1
（二）本发明制备的钛铝碳/一氧化硅球磨混合烧结制备的钛硅碳/氧化铝复合材料的X射线衍射图谱，如图1所示，微观图像及元素分析如图2和图3所示。
图 1为钛铝碳/一氧化硅球磨混合烧结制备的钛硅碳/氧化铝复合材料的X射线衍射图谱。其中的X射线峰揭示了复合材料中的 Ti3SiC2相（*）、Al2O3 相（◆）和非晶相（△）。非晶相对应于图 1 左侧的突起。Ti3SiC2相、Al2O3 相有明确的XRD峰。
图2为钛铝碳/一氧化硅球磨混合烧结制备的钛硅碳/氧化铝复合材料，在抗弯强度测试产生的断面于扫描电子显微镜下的显示出的微观图像。抗弯强度测试产生断面的SEM显微照片，包含长度约10μm的层状晶体结构，和围绕在四周的其他形状的晶体结构。一氧化硅相可能在断裂测试和超声处理过程中被去除。
图3为与图2对应的元素分布图。Ti-Si-C和Al-O的分布是一致的，并且发现来自分解的 Ti3-C2 层的碳。 因此，在 SEM 显微照片中确定多层 Ti3SiC2 被 Al2O3 紧紧包围（图2）。 破碎的 MAX 晶粒中没有明显 Al 信号，这意味着 SiO 可以将粒径为 10 μm 的Ti3AlC2 转化为层状Ti3SiC2。
Claims (6)
1.一种氧化铝/钛硅碳复合材料的制备方法，其特征在于，所述复合材料以钛铝碳Ti3AlC2粉和一氧化硅SiO粉为原料制备而成。
2.根据权利要求1所述的制备方法，其特征在于，具体包括以下步骤：
（1）将原料钛铝碳Ti3AlC2粉和一氧化硅SiO粉混合均匀，得混合料；
（2）将混合料进行保温加压烧结，保温加压程序结束后随炉降温，降温后关闭真空系统，得到薄饼状氧化铝/钛硅碳复合材料。
3.根据权利要求1或2所述的制备方法，其特征在于，步骤（1）中，所述钛铝碳的粒径为3-15 μm，一氧化硅的粒径为0.5-5μm，纯度为99.9%。
4.根据权利要求2或3所述的制备方法，其特征在于，步骤（1）中，所述混合料采用球磨法进行混合。
5.根据权利要求3所述的制备方法，其特征在于，所述钛铝碳与一氧化硅的摩尔比例为1：0.5-1.5。
6.根据权利要求2-5任一项所述的制备方法，其特征在于，步骤（2）中，所述保温烧结为首先以1-10℃的升温速率升温至1200℃，然后以5-20℃/min的升温速率升温至1250 ℃-1350 ℃，保温1.5-3 h，烧结压力为25-35MPa。
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