CN114956196B - 一种丙酮传感材料及其快速制备方法 - Google Patents
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Abstract
本发明公开了一种丙酮传感材料及其快速制备方法,属于半导体金属氧化物气体传感器技术领域。采用快速固相合成法,通过研磨和煅烧来合成珊瑚状形貌的Co3O4纳米材料,将其制备成气敏元件,在160℃最佳操作温度下,基于制备的珊瑚状Co3O4材料组装的气敏元件对50 ppm丙酮灵敏度最高,能达到17.8,响应时间为160 s,恢复时间为28 s,该传感材料对丙酮有着优异的选择性,具有较好的实际应用价值。
Description
技术领域
本发明属于半导体金属氧化物气体传感器技术领域,具体涉及开发了一种固相合成法快速制备珊瑚状四氧化三钴纳米材料,由该纳米材料组装的气体传感器对丙酮具有优异的传感性能。
背景技术
半导体金属氧化物因为具有灵敏度高、稳定性好、易于制备等优点,在检测有毒有害气体方面有极大的优势,所以在气体传感领域被广泛使用。丙酮是重要的有机合成原料,有易燃、易挥发,化学性质较活泼等基本性质,但其具有剧毒,对人体危害非常大,吸入过量丙酮会麻痹神经,导致恶心、头晕、甚至昏迷等健康危害,所以迫切需要制备出一种灵敏度高且选择性好的丙酮气体传感器。目前用于检测丙酮的气体传感器有较多报道,发明专利“一种基于晶相改进的CdSnO3纳米半导体敏感材料的丙酮气体传感器及其制备方法”(CN114062446A)制备的CdSnO3基丙酮气体传感器在300℃温度下对100 ppm丙酮气体的响应值为17.78;专利“基于分枝状异质结阵列丙酮气体传感器、制备方法及应用”(CN112255277B)制备了TiO2/α-Fe2O3基分支状丙酮气体传感器,其在225℃温度下对100ppm丙酮气体的响应值为21.9;专利“一维α-Fe2O3纳米棒的制备方法及基于α-Fe2O3纳米棒的丙酮传感器”(CN108776156B)将Fe(NO3)2·9H2O溶于去离子水,用氢氧化钠调pH值,经水热、洗涤和干燥后,得到α-Fe2O3纳米棒,基于该纳米棒组装的传感器,其在225℃温度下对100 ppm丙酮气体的响应值为4.56。虽然在半导体氧化物气体传感器的研究上已取得了很大进步,但进一步提高丙酮传感器的灵敏度、选择性和降低最佳操作温度等技术参数是非常有必要的。
四氧化三钴(Co3O4)是典型的p型半导体金属氧化物,由于其禁带宽度接近可见光能量,且无毒、具有强耐腐蚀性,在光催化剂、超级电容器和气体传感器等领域引起了广泛关注。调控形貌是增强气体传感器的气敏性能一种方法。如专利“一种四氧化三钴纳米材料的制备方法及其产品和应用”(CN111003732A)用溶剂热法制备Co前驱体材料,然后将其均匀分散在Co盐溶液中,经过冷冻干燥去除溶剂,煅烧后得到四氧化三钴,用该材料制备的传感器在150℃温度下对50 ppm甲醛气体的响应值高达18.7,但其制备方法较复杂。本发明的反应物前驱体是醋酸钴,经过研磨和煅烧获得了珊瑚状Co3O4纳米结构粉末,该方法制备时间较短,且无毒环保,使用该材料制备的气体传感器对丙酮的响应高,选择性好,操作简便。
发明内容
本发明提供了一种快速制备丙酮传感材料的方法,制备方法快速简便且无毒环保,通过研磨和煅烧合成了珊瑚状Co3O4纳米材料,将该材料制备成传感器用于丙酮检测,灵敏度高,选择性好。
本发明所述的一种高响应的珊瑚状Co3O4纳米材料的丙酮传感器,由外表面带有两条平行、环状且彼此分立的金电极的陶瓷管衬底,涂覆在陶瓷管外表面、金电极上的纳米敏感材料和置于陶瓷管内的镍镉加热线圈组成,制备步骤如下:
1、珊瑚状Co3O4纳米材料的制备方法:
(1)将0.01~0.03 mmolCo(CH3COO)2·4H2O和0.01~0.03 mmol的H2C2O4·2H2O在研钵中均匀研磨20~40 min,同时在研磨的过程中滴加少许无水乙醇;
(2)将上述样品转移至50℃~70℃的烘箱中干燥,得到粉红色的粉末;
(3)将得到的粉红色粉末放入马弗炉中在400~600℃温度下煅烧1~3 h,得到最终产物,珊瑚状Co3O4纳米材料,为黑色粉末。
2、基于Co3O4纳米材料传感器的制备方法:
本发明所涉及的传感器采用的是旁热式结构,具体工艺如下:将制好的30~60 mg粉末与2~3滴松油醇混合,在玛瑙研钵中顺时针研磨20~40 min均匀形成浆液,再用刷子将浆液均匀涂在陶瓷管表面,以形成薄的传感材料涂层,在基座上焊接好后,老化2~3天,制成旁热式烧结型气敏元件。
附图说明:
图1为实施例1所得样品扫描电镜图(SEM);
图2为实施例1、2、3制备的气敏元件对50 ppm丙酮的响应值随工作温度变化的曲线图;
图3为实施例1所制备的样品的响应恢复时间图;
图4为实施例1制备的气敏元件在最佳操作温度对50 ppm的不同有机气体的敏感性能测试图;
具体实施方式:
以下结合实施例对本发明做具体的说明,使熟悉本领域的技术人在研读本说明书之后能据以实施,其中实施例1为最佳制备条件。应当理解,此处所描述的具体实施案例仅用以解释本发明专利,并不用于限定本发明专利。
实施例1:一种丙酮传感材料及其快速制备方法
(1)将0.02 mmol Co(CH3COO)2·4H2O和0.02 mmol H2C2O4·2H2O在研钵中均匀研磨30 min,同时在研磨的过程中滴加少许无水乙醇;
(2)将上述样品转移至60℃的烘箱中干燥,得到粉红色的粉末;
(3)将得到的粉红色粉末放入马弗炉中在400℃下煅烧2 h,得到最终产物,图1显示该样品是由大量的纳米粒子组成的珊瑚状形貌,粒子尺寸为10~20 nm;
(4)取30 mg制得的黑色粉末放入玛瑙研钵中,滴加1~2滴松油醇后顺时针研磨30min形成浆液,用毛刷取适量浆液涂覆在市售陶瓷管外表面,静置2天,在基座上先用高性能焊锡丝焊接陶瓷管,再将加热丝穿过陶瓷管用锡丝焊上;
(5)将制备好的传感器置于老化台在200℃的条件下老化72 h,得到基于400℃煅烧Co3O4纳米材料的气敏元件。
实施例2:一种丙酮传感材料及其快速制备方法
(1)将0.02 mmol Co(CH3COO)2·4H2O和0.02 mmol H2C2O4·2H2O在研钵中均匀研磨30 min,同时在研磨的过程中滴加少许无水乙醇;
(2)将上述样品转移至60℃的烘箱中干燥,得到粉红色的粉末;
(3)将得到的粉红色粉末放入马弗炉中在500℃下煅烧2 h,得到最终产物;
(4)气敏元件制备步骤同实施例1的方法,得到基于500℃煅烧Co3O4纳米材料的气敏元件。
实施例3:一种丙酮传感材料及其快速制备方法
(1)将0.02 mmol Co(CH3COO)2·4H2O和0.02 mmol H2C2O4·2H2O在研钵中均匀研磨30 min,同时在研磨的过程中滴加少许无水乙醇;
(2)将上述样品转移至60℃的烘箱中干燥,得到粉红色的粉末;
(3)将得到的粉红色粉末放入马弗炉中在600℃下煅烧2 h,得到最终产物;
(4)气敏元件制备步骤同实施例1的方法,得到基于600 ℃煅烧Co3O4纳米材料的气敏元件。
实施例4:Co3O4纳米材料的气敏元件传感性能测试
气敏元件特性的测试采用静态配气法,通过WS-30A型气敏元件测试系统在5.0 V的加热电压下测试80℃到240℃工作温度范围内,不同煅烧温度的Co3O4材料制备的气敏元件对50 ppm丙酮的响应值随工作温度变化曲线如图2,从图2中可以看出煅烧温度为400℃的Co3O4气敏元件在160℃的工作温度下,对丙酮有优良的响应值为17.8,其响应恢复时间如图3所示,响应时间为160 s,恢复时间为28 s;同样的,采用静态配气法,通过WS-30A型气敏元件测试系统在5.0 V的加热电压下测试煅烧温度为400℃的Co3O4材料制备的气敏元件对其他有机化合物的响应值,如图4显示了在160℃温度下对50 ppm的甲醛、甲醇、丙酮、异丙醇、乙醇、三乙胺的响应值分别为1.7、2.1、17.8、3.6、2.7、4.3,从图4的测试结果可以看出煅烧温度为400℃的Co3O4气敏元件对丙酮检测具有良好的选择性。
Claims (1)
1.一种丙酮传感材料的快速制备方法,其特征在于,包括以下工艺步骤:
(a)将0.02mmol Co(CH3COO)2·4H2O和0.02mmol H2C2O4·2H2O在研钵中均匀研磨30min,同时在研磨的过程中滴加少许无水乙醇;
(b)将上述样品转移至60℃的烘箱中干燥,得到粉红色的粉末;
(c)将得到的粉红色粉末放入马弗炉中在400℃下煅烧2h,得到最终产物,珊瑚状Co3O4纳米材料,为黑色粉末;
上述制备方法获得的珊瑚状Co3O4纳米材料组装成的气体传感器,在160℃的工作温度下,对丙酮的响应值为17.8,其响应时间为160s,恢复时间为28s。
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