CN108408727A - 一种易剥离陶瓷材料max相的合成及剥离方法 - Google Patents
一种易剥离陶瓷材料max相的合成及剥离方法 Download PDFInfo
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Abstract
一种易剥离陶瓷材料MAX相的合成及剥离方法,其主要是将合成原材料:M为Sc、Ti、V、Cr、Zr、Nb、Mo、Hf、Ta;A为A与Li、Na、K、Mg、Ca的合金粉,其中Li、Na、K、Mg、Ca的含量为10‑50at%;X为C或N;分别从上述M、A、X中各选取一种,按质量比M:A:X=2‑4:0.5‑1.1:1‑3,在氩气气氛下球磨12‑36h,得易剥离MAX相的粉状合成原料;将所得粉末在50MPa于磨具中预压成圆柱体,然后在2‑6GPa,800‑1600℃条件下烧结2‑4h,冷却至室温后卸压取出,将MAX材料粉碎,浸入腐蚀液中,40℃搅拌12h得到二维MXene陶瓷材料。本发明摆脱了MAX相剥离对高浓度HF的依赖,有助于二维MXene材料应用的推广。
Description
技术领域
本发明属于材料技术领域,特别涉及一种陶瓷材料MAX相的合成及剥离方法。
背景技术
三元层状陶瓷材料MAX是密排六方结构,通常用Mn+1AXn表示(n=1,2,3),其中,M代表过渡金属元素,A代表主族元素,X是碳或氮。M原子间以金属键相连、M与X间以强共价键结合此两种结合方式均较稳定;M与A之间的化学键较弱,A原子较易挣脱MX片层而得到二维层状的MX材料。目前用于剥离MAX相材料的主要是高浓度的氢氟酸。氢氟酸具有极强的腐蚀性、有剧毒。合成一种易于剥离或者取代氢氟酸作为腐蚀液的MAX相具有重要的意义。
目前MAX相的主要合成原料是M、A、X三种元素的单质、M元素的氢化物、化合物MX等。利用热压烧结、放电等离子烧结、氩气气氛无压烧结等工艺合成MAX相。利用以上工艺原料合成出的MAX相纯度很高,但是对它们的剥离条件要求比较苛刻,在二维材料的应用领域受到一定的限制。周爱国(Zhengyang Li,Libo Wang,Dandan Sun,Yude Zhang,BaozhongLiu,Qianku Hu,Aiguo Zhou。Synthesis and thermal stability of two-dimensionalcarbide MXene Ti3C2[J].Materials Science and Engineering B.2015,191:33-40)等研究的Ti3AlC2的剥离方法是以40%-49%的HF浸泡Ti3AlC2。该过程中使用的浓HF溶液具有强腐蚀性和毒性,致使该方法的推广大大受限。洪茂椿(Wang Kun,Zhou Youfu,Xu Wentao,Huang Decai,Wang Zhiguang,Hong Maochun.Fabrication and thermal stability oftwo-dimensional carbide Ti3C2nanosheets[J].Ceramics International.2016,42(7):8419-8424.)等研究的Ti3AlC2的剥离方法也是以高浓度的HF浸泡,与上述方法类似,并未摆脱浓HF的使用。
二维MXene材料的推广使用首先要解决其剥离试剂与剥离方法的无毒(低毒)、无害(低伤害)、操作难的问题。
发明内容
本发明的目的旨在提供一种工艺简单、无毒无害、容易剥离的易剥离陶瓷材料MAX相的合成及剥离方法。
本发明的合成及剥离方法如下:
(1)合成原材料:M为Sc、Ti、V、Cr、Zr、Nb、Mo、Hf、Ta;A为A与Li、Na、K、Mg、Ca的合金粉,其中Li、Na、K、Mg、Ca的含量为10-50at%;X为C或N;
分别从上述M、A、X中各选取一种,按质量比M:A:X=2-4:0.5-1.1:1-3,其中A的合金以A元素计量,按10-20:1的球料比加入直径6mm的不锈钢磨球,以300-400r/min的转速在氩气气氛下球磨12-36h,使之混合均匀,得易剥离MAX相的粉状合成原料;
(2)将步骤(1)所得粉末在50MPa的压力下于不锈钢磨具中预压成直径10mm高14mm的圆柱体,然后以高压烧结的方式在2-6GPa,800-1600℃条件下烧结2-4h,冷却至室温后卸掉压力取出样品,将其打磨干净得到易剥离的MAX相;
(3)把步骤(2)所得MAX材料粉碎,浸入腐蚀液中,40℃搅拌12h得二维MXene陶瓷材料。
所述腐蚀液为强碱:KOH、NaOH,强酸:盐酸、硝酸,弱酸:低浓度氢氟酸。
MAX相是三元层状陶瓷材料,其中A元素独立成层,以较弱的共价键与M原子相连。显然,按上述配比配料A元素不足,不足以完全生成MAX相,缺少A元素的位置会随机产生。由于高压反应限制了L元素的逸出,迫使它占据A元素的位置(无化学键的形成)或者使键能较弱的化学键。因为L元素与其他元素间并无化学键的生成且L元素是非常活泼的金属元素,当这种含有均匀分散的Li、Na、K、Mg或Ca元素的MAX相被剥离时,首先是MAX相表面(层)的Li、Na、K、Mg或Ca元素与腐蚀液反应生成微小孔洞,此反应过程中会短时间内放出较多的热量且生成强碱,这一脉冲热量会机械性的扩张L原子所占据的微小孔洞,辅助腐蚀液接触MAX相中的A原子及其它Li、Na、K、Mg或Ca原子,有助于进一步腐蚀。同时这一热量也会提高腐蚀液与MAX的反应活性,在无HF的腐蚀液或低浓度的HF腐蚀液中,实现MAX的剥离。当腐蚀液为强酸时,溶液中氢离子浓度较高,对活泼金属的反应活性高且反应剧烈,在反应过程中不仅放出大量热量还生成氢气,这一热量和气体机械的扩张MXene的层间距,利于MAX的剥离。另外由于此法合成的MAX中含有活泼的金属单质,在活泼金属被剥离的过程中有利于HF对MAX的腐蚀。所以在低浓度的HF中会被剥离(比浓度的HF相较于高浓度的HF活性低)。
本发明与现有技术相比具有如下优点:
1、合成的MAX相易于剥离,避免了高浓度HF溶液的使用;
2、利用高压限域的作用将样品全面压实封住限制Li、Na、K、Mg或Ca元素的损失(相对于放电等离子烧结、热压烧结、气氛无压烧结);
3、利用活泼金属元素占位,再将其去除的方法达到了合成易剥离MAX相的目的;
4、避免了对人体危害巨大的高浓度HF的使用实现MAX相的剥离,具有广阔的应用前景。
具体实施例
实施例1
按铝和锂的质量之比为5:1,于真空非自耗电弧炉中熔炼铝锂合金,待冷却后翻转再次熔炼,重复熔炼五次,利用浓差扩散使二者混合均匀。将熔炼好的铝锂合金粉碎,筛选500目以下的细粉备用,按质量比钛:铝锂合金(以铝计):碳=3:1.1:2配料,按10:1的球料比加入直径6mm的不锈钢磨球,400r/min在氩气气氛下每球磨60min冷却30min,循环12次得易剥离MAX相的合成原料;将上述原料在不锈钢磨具中以50MPa压力预压成直径10mm、高14mm的圆柱体,之后在六面顶压机中烧结,压力2GPa,温度1300℃,烧结2h后冷却至室温,把样品取出打磨干净、粉碎备用;取烧结后的粉末1g浸泡于20mL 2mol L-1的NaOH溶液中,40℃搅拌12h后离心洗涤干燥得到二维MXene(Ti3C2Tx)。(T为-OH/-F/-O-中的一种或多种,x为其含量。下同)
实施例2
按铝镁的质量比为1:1,于真空非自耗电弧炉中熔炼铝镁合金,待冷却后翻转再次熔炼,重复熔炼五次,利用浓差扩散使二者混合均匀。将熔炼好的铝锂合金粉碎,筛选500目以下的细粉备用,按质量比钛:铝锂合金(以铝计):碳=4:0.5:3配料,按10:1的球料比加入直径6mm的不锈钢磨球,300r/min在氩气气氛下每球磨60min冷却30min,循环24次得易剥离MAX相的合成原料;将上述原料在不锈钢磨具中以50MPa压力预压成直径10mm,高14mm的圆柱体,之后在六面顶压机中烧结,压力4GPa,温度1200℃,烧结2h后冷却至室温,把样品取出打磨干净、粉碎备用;取烧结后的粉末1g浸泡于20mL 2mol L-1的HCl溶液中,40℃搅拌12h后离心洗涤干燥得到二维MXene(Ti2CTx)。
实施例3
按硅钙的质量比为9:1,于真空非自耗电弧炉中熔炼硅钙合金,待冷却后翻转再次熔炼,重复熔炼五次,利用浓差扩散使二者混合均匀。将熔炼好的铝锂合金粉碎,筛选500目以下的细粉备用,按质量比钛:铝锂合金(以铝计):碳=3:0.5:2配料,按20:1的球料比加入直径6mm的不锈钢磨球,350r/min在氩气气氛下每球磨60min冷却30min,循环12次得易剥离MAX相的合成原料;将上述原料在不锈钢磨具中以50MPa压力预压成直径10mm,高14mm的圆柱体,之后在六面顶压机中烧结,压力3GPa,温度1350℃,烧结2h后冷却至室温,把样品取出打磨干净、粉碎备用;取烧结后的粉末1g浸泡于20mL 4mol L-1的KOH溶液中,40℃搅拌12h后离心洗涤干燥得到二维MXene(Ti3C2Tx)。
实施例4
按镓钠的质量比为1:1,于真空非自耗电弧炉中熔炼镓钠合金,待冷却后翻转再次熔炼,重复熔炼五次,利用浓差扩散使二者混合均匀。将熔炼好的铝锂合金粉碎,筛选500目以下的细粉备用,按质量比钛:铝锂合金(以铝计):碳=2:1.1:1配料,按20:1的球料比加入直径6mm的不锈钢磨球,400r/min在氩气气氛下每球磨60min冷却30min,循环36次得易剥离MAX相的合成原料;将上述原料在不锈钢磨具中以50MPa压力预压成直径10mm,高14mm的圆柱体,之后在六面顶压机中烧结,压力4GPa,温度1100℃,烧结2h后冷却至室温,把样品取出打磨干净、粉碎备用;取烧结后的粉末1g浸泡于20mL 2mol L-1的NaOH溶液中,40℃搅拌12h后离心洗涤干燥得到二维MXene(Ga2CTx)。
实施例5
按铝钠的质量比为1:1,于真空非自耗电弧炉中熔炼铝钠合金,待冷却后翻转再次熔炼,重复熔炼五次,利用浓差扩散使二者混合均匀。将熔炼好的铝锂合金粉碎,筛选500目以下的细粉备用,按质量比铌:铝锂合金(以铝计):碳=3:1.1:2配料,按20:1的球料比加入直径6mm的不锈钢磨球,400r/min在氩气气氛下每球磨60min冷却30min,循环24次得易剥离MAX相的合成原料;将上述原料在不锈钢磨具中以50MPa压力预压成直径10mm,高14mm的圆柱体,之后在六面顶压机中烧结,压力6GPa,温度1600℃,烧结4h后冷却至室温,把样品取出打磨干净、粉碎备用。取烧结后的粉末1g浸泡于20mL 10%的HF溶液中,40℃搅拌12h后离心洗涤干燥得到二维MXene(Nb2CTx)。
实施例6
按硅锂的质量比为1:1,于真空非自耗电弧炉中熔炼铝钠合金,待冷却后翻转再次熔炼,重复熔炼五次,利用浓差扩散使二者混合均匀。将熔炼好的铝锂合金粉碎,筛选500目以下的细粉备用,按质量比铌:铝锂合金(以铝计):碳=3:1.1:2配料,按20:1的球料比加入直径6mm的不锈钢磨球,400r/min在氩气气氛下每球磨60min冷却30min,循环24次得易剥离MAX相的合成原料;将上述原料在不锈钢磨具中以50MPa压力预压成直径10mm,高14mm的圆柱体,之后在六面顶压机中烧结,压力6GPa,温度800℃,烧结4h后冷却至室温,把样品取出打磨干净、粉碎备用。取烧结后的粉末1g浸泡于20mL 2mol L-1的NaOH溶液中,40℃搅拌12h后离心洗涤干燥得到二维MXene(Nb2CTx)。
Claims (2)
1.一种易剥离陶瓷材料MAX相的合成及剥离方法,其特征在于:
(1)合成原材料:M为Sc、Ti、V、Cr、Zr、Nb、Mo、Hf、Ta;A为A与Li、Na、K、Mg、Ca的合金粉,其中Li、Na、K、Mg、Ca的含量为10-50at%;X为C或N;
分别从上述M、A、X中各选取一种,按质量比M:A:X=2-4:0.5-1.1:1-3,其中A的合金以A元素计量,按10-20:1的球料比加入直径6mm的不锈钢磨球,以300-400r/min的转速在氩气气氛下球磨12-36h,使之混合均匀,得易剥离MAX相的粉状合成原料;
(2)将步骤(1)所得粉末在50MPa的压力下于不锈钢磨具中预压成直径10mm高14mm的圆柱体,然后以高压烧结的方式在2-6GPa,800-1600℃条件下烧结2-4h,冷却至室温后卸掉压力取出样品,将其打磨干净得到易剥离的MAX相;
(3)把步骤(2)所得MAX材料粉碎,浸入腐蚀液中,40℃搅拌12h得到二维MXene陶瓷材料。
2.根据权利要求1所述的易剥离陶瓷材料MAX相的合成及剥离方法,其特征在于:所述腐蚀液为强碱:KOH、NaOH,强酸:盐酸、硝酸,弱酸:低浓度氢氟酸。
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CN109231988A (zh) * | 2018-11-01 | 2019-01-18 | 燕山大学 | 一种大空位非计量比活性Ti3AlC2陶瓷材料的制备方法 |
CN113066965A (zh) * | 2021-03-22 | 2021-07-02 | 宁波杉杉新材料科技有限公司 | MXene-硅复合负极材料、含其的电池及其制备方法和应用 |
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CN109231989A (zh) * | 2018-11-01 | 2019-01-18 | 燕山大学 | 一种高活性合金插层Ti3AlMC2陶瓷材料的制备方法 |
CN109231988A (zh) * | 2018-11-01 | 2019-01-18 | 燕山大学 | 一种大空位非计量比活性Ti3AlC2陶瓷材料的制备方法 |
CN109231988B (zh) * | 2018-11-01 | 2020-09-22 | 燕山大学 | 一种大空位非计量比活性Ti3AlC2陶瓷材料的制备方法 |
CN113066965A (zh) * | 2021-03-22 | 2021-07-02 | 宁波杉杉新材料科技有限公司 | MXene-硅复合负极材料、含其的电池及其制备方法和应用 |
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