CN110241440B - 一种硼基电化学非晶态固体的快速制备方法 - Google Patents
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- 229910052796 boron Inorganic materials 0.000 title claims abstract description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000007787 solid Substances 0.000 title abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 16
- 238000007747 plating Methods 0.000 claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- -1 alkali metal silicon boron hydrogen salt Chemical class 0.000 claims abstract description 12
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229960000583 acetic acid Drugs 0.000 claims abstract description 6
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 6
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000008139 complexing agent Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 4
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 4
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000010959 steel Substances 0.000 claims abstract description 4
- 229940095064 tartrate Drugs 0.000 claims abstract description 4
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 3
- 230000005587 bubbling Effects 0.000 claims 1
- 238000007733 ion plating Methods 0.000 abstract description 6
- 150000003839 salts Chemical class 0.000 abstract description 6
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229940001468 citrate Drugs 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229940039748 oxalate Drugs 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
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- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 1
- 229960001860 salicylate Drugs 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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Abstract
本发明提供的一种硼基电化学非晶态固体的快速制备方法,包括如下步骤:步骤一、以碱金属硅硼氢盐为原料,溶解于DMAC(N,N'‑二甲基乙酰胺)溶液;步骤二、将溶有冰醋酸的DMAC(N,N'‑二甲基乙酰胺)溶液滴加至上述溶液中,真空蒸馏提纯;步骤三、磁力搅拌水浴恒温锅中,以乙醇作为溶剂,以碱金属醋酸硅硼氢盐以及Cu、Ni或Co醋酸盐为主要成分,四正丁基溴化铵作为导电盐,以碱金属草酸盐、柠檬酸盐、酒石酸盐或EDTA为络合剂,以适合钢铁板作为极板,在一定的电流密度下,在一定的温度下,施镀。由上,可以采用溶液离子镀制备硼基电化学非晶态合金。
Description
技术领域
本发明涉及电化学非晶固体技术领域,特别是指一种硼基电化学非晶态固体。
背景技术
电化学非晶固体由于具有低成本、可大面积镀覆以及可以获得冶金法无望的新合金的特点,其快速制备研究备受关注。但是,目前主要集中于第八族元素与(P、B、C、S)等元素的合金化上,B与其它元素因其单盐或者络盐因还原电位差异及镀液稳定性不高而难以快速共沉积获得相应的硼基电化学非晶态固体。过渡金属硼化物为新型超硬材料的热点研究对象,其硼基电化学非晶态固体具有重要的理论与实际意义。
鉴于此,基于碱金属硼氢与其他元素再键合复合盐的有机沉积,研究电化学非晶态固体的快速制备方法。
发明内容
有鉴于此,本发明的主要目的在于提供一种硼基电化学非晶态固体的快速制备方法,以填补溶液离子镀制备B基非晶态固体镀层以及快速制备易于块体非晶化的空白。
本发明提供的一种硼基电化学非晶态固体的快速制备方法,包括如下步骤:
步骤一、以碱金属硅硼氢盐为原料,溶解于DMAC(N,N'-二甲基乙酰胺)溶液;
步骤二、将溶有冰醋酸的DMAC(N,N'-二甲基乙酰胺)溶液滴加至上述溶液中,真空蒸馏提纯;
步骤三、磁力搅拌水浴恒温锅中,以乙醇作为溶剂,四正丁基溴化铵作为导电盐,以碱金属醋酸硅硼氢盐以及Cu、Ni或Co醋酸盐为主分,以碱金属草酸盐、柠檬酸盐、酒石酸盐或EDTA为络合剂,以选定钢板作为极板,在一定的电流密度下,在一定的温度下,施镀。
由上,可以采用溶液离子镀快速制备硼基电化学非晶态固体,例如镀层以及块体非晶。
优选地,将溶有冰醋酸的DMAC(N,N'-二甲基乙酰胺)溶液缓慢滴加至上述溶液中,边滴加边搅拌,直到不冒气泡为止,防止滴加过程中因产生大量的氢气,发生危险。
优选地,导电盐四正丁基溴化铵的浓度为0.01~0.05mol/L。
优选地,碱金属醋酸硅硼氢盐的浓度为1~6g/L。
优选地,Cu、Ni或Co醋酸盐的浓度为0.1~2g/L。
优选地,作为络合剂的碱金属草酸盐、酒石酸盐、柠檬酸盐、水杨酸盐或EDTA的浓度为0.05~2g/L。
优选地,电流密度为0.1A/dm2~15A/dm2。
优选地,施镀的温度为25~45℃。
优选地,施镀的时间为0.5~2小时。
由上,可以降低生产成本,提高效率。
附图说明
图1为硼基电化学非晶态固体的快速制备方法流程图;
图2为样品8的XRD图谱。
具体实施方式
如图1所示,具体的使用碱金属硅硼氢盐作为主分,在此基础上通过溶液离子镀制备B基非晶固体镀层。具体步骤为:
步骤一、以碱金属硅硼氢盐为原料,溶解于DMAC(N,N'-二甲基乙酰胺)溶液;
步骤二、将溶有冰醋酸的DMAC(N,N'-二甲基乙酰胺)溶液滴加至上述溶液中;
具体操作为,滴加要缓慢,因为有大量氢气放出,边滴加边搅拌,直到不冒气泡,真空蒸馏提纯;
步骤三、磁力搅拌水浴恒温锅中,以乙醇作为溶剂,四正丁基溴化铵(0.01~0.03mol/L)作为导电盐,以碱金属醋酸硅硼氢盐(1~5g/L)以及醋酸镍(0.1~2g/L)为主分,以草酸钠、酒石酸盐或EDTA(总浓度0.05~2g/L)为络合剂,以适合钢铁板作为极板,在0.2A/dm2~3.2A/dm2的电流密度下,25~45℃施镀2小时。
本发明为基于碱金属硅硼氢盐的新型主分,提供一种溶液离子镀制备B基非晶合金镀层的方法。通过此方法,可以溶液离子镀制得硼基非晶态固体镀层,具有快速制备特性。
本发明对镀速进行检测分析。表1为正交实验因素水平表,表2为各因素正交实验结果分析。如表1和表2所示,最大镀速可达约150μm·h-1,属于快速制备,可以用于制备块体材料。
表1正交实验因素水平表
表2各因素正交实验结果分析
对样品8进行X射线衍射,如图2为样品8的XRD图谱。分析其衍射图谱,为漫散衍射峰,为典型的非晶特征,证明该方法可以用于块体非晶化。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.一种硼基电化学非晶态合金的快速制备方法,其特征在于,包括如下步骤:
步骤一、以碱金属硅硼氢盐为原料,溶解于DMAC(N,N'-二甲基乙酰胺)溶液;
步骤二、将溶有冰醋酸的DMAC(N,N'-二甲基乙酰胺)溶液滴加至上述溶液中,真空蒸馏提纯;
步骤三、磁力搅拌水浴恒温锅中,具有溶剂乙醇,浓度为0.01~0.05mol/L的导电盐四正丁基溴化铵,浓度为1~6g/L的碱金属醋酸硅硼氢盐以及浓度为0.1~2g/L的Cu、Ni或Co醋酸盐,总浓度为0.05~2g/L的络合剂碱金属草酸盐、柠檬酸盐、酒石酸盐或EDTA,以钢铁板作为极板,在0.1A/dm2~15A/dm2的电流密度下,25~45℃温度下,施镀0.5~2小时。
2.根据权利要求1所述的一种硼基电化学非晶态合金的快速制备方法,其特征在于,所述步骤二具体包括:
将溶有冰醋酸的DMAC(N,N'-二甲基乙酰胺)溶液缓慢滴加至上述溶液中,边滴加边搅拌,直到不冒气泡为止。
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