CN111816753B - A kind of preparation method of paper-based bismuth telluride-based nanowire flexible thermocouple temperature sensor - Google Patents
A kind of preparation method of paper-based bismuth telluride-based nanowire flexible thermocouple temperature sensor Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 110
- 239000002070 nanowire Substances 0.000 title claims abstract description 107
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- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title claims abstract description 99
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- 239000000741 silica gel Substances 0.000 claims description 15
- 229910002027 silica gel Inorganic materials 0.000 claims description 15
- 229910052709 silver Inorganic materials 0.000 claims description 15
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- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 9
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- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims 1
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- 229910002908 (Bi,Sb)2(Te,Se)3 Inorganic materials 0.000 abstract description 72
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- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 4
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Abstract
Description
技术领域：Technical field:
本发明涉及柔性电子传感器件技术领域，具体涉及一种纸基底碲化铋基纳米线柔性热电偶型温度传感器的制备方法。The invention relates to the technical field of flexible electronic sensing devices, in particular to a preparation method of a paper-based bismuth telluride-based nanowire flexible thermocouple-type temperature sensor.
背景技术：Background technique:
温度传感器(temperature sensor)是指能感受温度并转换成可用输出信号的传感器。温度传感器是温度测量仪表的核心部分，品种繁多。按测量方式可分为接触式和非接触式两大类，按照传感器材料及电子元件特性分为热电阻和热电偶两类。A temperature sensor refers to a sensor that can sense temperature and convert it into a usable output signal. The temperature sensor is the core part of the temperature measuring instrument, and there are many varieties. According to the measurement method, it can be divided into two categories: contact type and non-contact type. According to the characteristics of sensor materials and electronic components, it can be divided into two categories: thermal resistance and thermocouple.
纸张因其柔性、来源丰富、性能可控、轻便、环保等优点，有望成为柔性电子器件的理想衬底材料。近年来很多研究者也利用纸作为基底制备了晶体管，超级电容器及锂电池等柔性电子器件。目前纸基底的柔性温度传感器研究还相对少，而柔性温度传感器在电子皮肤及机器人等领域具有广阔的应用前景。Paper is expected to be an ideal substrate material for flexible electronic devices due to its flexibility, abundant sources, controllable properties, lightness, and environmental protection. In recent years, many researchers have also used paper as a substrate to prepare flexible electronic devices such as transistors, supercapacitors and lithium batteries. At present, there are relatively few researches on flexible temperature sensors based on paper, and flexible temperature sensors have broad application prospects in the fields of electronic skin and robotics.
发明内容：Invention content:
本发明的目的是提供一种纸基底碲化铋基((Bi,Sb)2(Te,Se)3)纳米线柔性热电偶型温度传感器的制备方法，工艺简单，制备周期短，安全无污染、能耗低，得到的温度传感器响应时间短，灵敏度高，柔性良好。The purpose of the present invention is to provide a method for preparing a paper-based bismuth telluride-based ((Bi,Sb) 2 (Te, Se) 3 ) nanowire flexible thermocouple temperature sensor, which is simple in process, short in preparation period, safe and pollution-free , low energy consumption, the obtained temperature sensor has short response time, high sensitivity and good flexibility.
本发明是通过以下技术方案予以实现的：The present invention is achieved through the following technical solutions:
一种纸基底碲化铋基((Bi,Sb)2(Te,Se)3)纳米线柔性热电偶型温度传感器的制备方法，该方法包括以下步骤：A preparation method of a paper-based bismuth telluride-based ((Bi,Sb) 2 (Te, Se) 3 ) nanowire flexible thermocouple temperature sensor, the method comprising the following steps:
(1)将P型及N型的碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末分别置于管式炉中，在氢/氩混合气氛中200℃～400℃退火120～420分钟分别得到退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末；(1) The P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were placed in a tube furnace respectively, and annealed at 200°C to 400°C in a hydrogen/argon mixed atmosphere The annealed P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders are respectively obtained in 120 to 420 minutes;
(2)将步骤(1)得到的退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末分别与聚乙烯吡咯烷酮混合，分别超声分散在乙二醇溶剂中得到P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液；P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线的浓度分别为30～80mg/mL，聚乙烯吡咯烷酮浓度为0.3～2mg/mL；(2) The annealed P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders obtained in step (1) are respectively mixed with polyvinylpyrrolidone, and ultrasonically dispersed in ethylene glycol respectively. P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions were obtained in a solvent; P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 The concentrations of nanowires are 30-80 mg/mL, respectively, and the concentration of polyvinylpyrrolidone is 0.3-2 mg/mL;
(3)在真空抽滤辅助的条件下，将步骤(2)得到的P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液分别均匀滴涂在玻璃纤维滤膜上；P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液的滴涂量分别为0.2-1.2mL/cm2，滴涂完成后80℃真空干燥得到粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜；(3) Under the assisted condition of vacuum filtration, the P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersion liquids obtained in step (2) were uniformly drop-coated on glass. On the fiber filter membrane; the drop coating amount of P-type and N-type bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire dispersions is 0.2-1.2mL/cm 2 respectively, and the drop coating is completed at 80℃ The bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire film was obtained by vacuum drying and adhered to the glass fiber membrane;
(4)将步骤(3)中得到的粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜按照一定的间距垂直交错排列，薄膜之间的间距为1mm～30mm，并夹在两张复印纸之间，放置于压片机中10-40Mpa下挤压成型，然后取出，先去掉玻璃纤维滤膜背面的复印纸，再用刷子去掉碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜背面的玻璃纤维滤膜碎片，得到以复印纸为基底的P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜的垂直交叉阵列；(4) The bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire films obtained in the step (3) and adhered to the glass fiber filter membrane are vertically staggered according to a certain spacing, and the films are arranged in a staggered manner. The distance is 1mm~30mm, and it is sandwiched between two copies of paper, placed in a tablet press under 10-40Mpa and extruded, and then taken out, first remove the copy paper on the back of the glass fiber filter, and then remove the tellurium with a brush Fragments of glass fiber filter membranes on the back of bismuth (Bi,Sb) 2 (Te,Se) 3 nanowire films to obtain P-type and N-type bismuth telluride-based (Bi,Sb) 2 (Te ,Se) 3 vertical cross array of nanowire films;
(5)在步骤(4)得到的以复印纸为基底的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列交叉节点处涂覆导电银胶作为电极及传热层，在薄膜两端也涂覆上导电银胶作为电极，导电银胶的涂覆厚度为0.5μm～20μm，涂覆完成后真空烘箱中60℃干燥30分钟使银胶固化；(5) Coating conductive silver paste as electrodes and heat transfer layers at the intersection nodes of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film arrays based on copy paper obtained in step (4) , the two ends of the film are also coated with conductive silver glue as electrodes. The coating thickness of the conductive silver glue is 0.5 μm to 20 μm. After the coating is completed, it is dried in a vacuum oven at 60 ° C for 30 minutes to cure the silver glue;
(6)在步骤(5)中得到的以复印纸为基底的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜两端的银胶电极上用空心小铆钉及连接端子连接上导线，再采用刮涂法在整个复印纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列表面涂覆一层导热硅胶作为封装层，使整个纳米线薄膜阵列及电极区域都完全被覆盖，导热硅胶涂覆厚度为1μm～100μm；然后放置在真空烘箱中于60℃真空烘干得到纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线柔性热电偶型温度传感器。(6) The silver glue electrodes at both ends of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire film based on copy paper obtained in step (5) are connected with small hollow rivets and connecting terminals Then use the blade coating method to coat the entire surface of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array on the copy paper substrate with a layer of thermally conductive silica gel as an encapsulation layer, so that the entire nanowire thin film array and the electrode area are completely covered, and the thickness of thermally conductive silica gel coating is 1 μm ~ 100 μm; and then placed in a vacuum oven at 60 ℃ vacuum drying to obtain paper-based bismuth telluride (Bi, Sb) 2 (Te, Se) 3 nm Wire flexible thermocouple type temperature sensor.
P型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末的制备方法参见专利号200910096585.0发明名称为一种锑掺杂碲化铋纳米线的制备方法或论文Aqueoussolution synthesis of(Sb,Bi)2(Te,Se)3nanocrystals with controllablecomposition and morphology(Z.Y.Lu,et al.J.Mater.Chem.C,2013,1,6271–6277)，；N型的碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末的制备方法参见论文Aqueous solutionsynthesis of(Sb,Bi)2(Te,Se)3nanocrystals with controllable composition andmorphology(Z.Y.Lu,et al.J.Mater.Chem.C,2013,1，6271–6277)。For the preparation method of P-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powder, please refer to Patent No. 200910096585.0 The title of the invention is a preparation method of antimony-doped bismuth telluride nanowires or the paper Aqueoussolution synthesis of ( Sb,Bi) 2 (Te,Se) 3 nanocrystals with controllablecomposition and morphology(ZYLu, et al.J.Mater.Chem.C,2013,1,6271–6277),; N-type bismuth telluride-based (Bi, For the preparation method of Sb) 2 (Te,Se) 3 nanowire powder, please refer to the paper Aqueous solution synthesis of (Sb, Bi) 2 (Te, Se) 3 nanocrystals with controllable composition and morphology (ZYLu, et al.J.Mater.Chem.C , 2013, 1, 6271–6277).
优选地，步骤(1)中，退火温度为250℃～350℃，退火时间为120～300分钟。Preferably, in step (1), the annealing temperature is 250°C to 350°C, and the annealing time is 120 to 300 minutes.
优选地，步骤(2)中P型或N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线的浓度为40～60mg/mL；聚乙烯吡咯烷酮浓度为0.4～0.8mg/mL。Preferably, in step (2), the concentration of P-type or N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowires is 40-60 mg/mL; the concentration of polyvinylpyrrolidone is 0.4-0.8 mg/mL mL.
优选地，步骤(3)中玻璃纤维滤膜的大小为1mm*20mm～20mm*100mm，更优选为2mm*20mm～20mm*100mm，P型或N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液的滴涂量均为0.6-1mL/cm2。Preferably, in step (3), the size of the glass fiber filter membrane is 1mm*20mm～20mm*100mm, more preferably 2mm*20mm～20mm*100mm, P-type or N-type bismuth telluride-based (Bi, Sb) 2 ( The drop coating amount of the Te,Se) 3 nanowire dispersion liquid is 0.6-1mL/cm 2 .
优选地，步骤(4)中挤压成型压力为20～40MPa，薄膜之间的距离为2mm～20mm。Preferably, in step (4), the extrusion molding pressure is 20-40 MPa, and the distance between the films is 2 mm-20 mm.
优选地，步骤(5)中导电银胶的涂覆厚度为1μm～10μm。Preferably, the coating thickness of the conductive silver paste in step (5) is 1 μm˜10 μm.
优选地，步骤(6)中导热硅胶涂覆厚度为10μm～50μm。Preferably, in step (6), the coating thickness of the thermally conductive silica gel is 10 μm˜50 μm.
本发明的有益效果如下：The beneficial effects of the present invention are as follows:
本发明通过设计P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜的垂直交叉阵列(m条P型及n条N型热电薄膜相互交叉)结构，使得一张薄膜上共有m*n个交叉节点可以用于感应薄膜上温度的变化，增加了单位面积上的温度测量节点数用于感应薄膜上温度的变化，能够输出更大的电压信号，由此准确而灵敏地测量温度，得到的温度传感器响应时间短，灵敏度高，柔性良好。The present invention designs a vertical cross array (m pieces of P-type and n pieces of N-type thermoelectric films intersect each other) structure of P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire films, so that A total of m*n cross nodes on a film can be used to sense the temperature change on the film, and the number of temperature measurement nodes per unit area is increased to sense the temperature change on the film, which can output a larger voltage signal, thus The temperature is measured accurately and sensitively, and the obtained temperature sensor has short response time, high sensitivity and good flexibility.
附图说明：Description of drawings:
图1是本发明实施例1步骤(5)所得到的涂覆有导电银胶的纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列示意图。1 is a schematic diagram of a paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array obtained by step (5) of Example 1 of the present invention and coated with conductive silver paste.
图2为本发明实施例1步骤(5)所得到的柔性薄膜器件实物图。FIG. 2 is a physical diagram of the flexible thin film device obtained in step (5) of Example 1 of the present invention.
图3为步骤(5)所得到的柔性薄膜器件柔性测试结果图。FIG. 3 is a graph showing the result of the flexibility test of the flexible thin film device obtained in step (5).
图4为步骤(6)中碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜两端导线引出设计示意图。FIG. 4 is a schematic diagram of the design of the lead-out design of both ends of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire film in step (6).
图5为本发明实施例1得到的涂覆有导热硅胶封装层的纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线柔性热电偶型温度传感器示意图。5 is a schematic diagram of a paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire flexible thermocouple temperature sensor coated with a thermally conductive silica gel encapsulation layer obtained in Example 1 of the present invention.
图6为实施例1得到的传感器所测量的温差与相应输出电压曲线。FIG. 6 is a curve of the temperature difference measured by the sensor obtained in Example 1 and the corresponding output voltage.
具体实施方式：Detailed ways:
以下是对本发明的进一步说明，而不是对本发明的限制。The following is a further description of the present invention, rather than a limitation of the present invention.
实施例1：Example 1:
(1)分别取500mg P型及500mgN型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末置于管式炉中，在氢/氩混合气氛中于350℃退火120分钟分别得到退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末；(1) 500 mg of P-type and 500 mg of N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were taken and placed in a tube furnace, and annealed at 350 °C for 120 minutes in a hydrogen/argon mixed atmosphere P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were respectively obtained after annealing;
(2)将退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末分别与4mg的聚乙烯吡咯烷酮混合超声分散在10mL乙二醇溶剂中得到P型及N型的碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液；P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线的浓度分别为50mg/mL，聚乙烯吡咯烷酮浓度为0.4mg/mL；(2) The annealed P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were respectively mixed with 4 mg of polyvinylpyrrolidone and ultrasonically dispersed in 10 mL of ethylene glycol solvent to obtain P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions; the concentration of P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowires 50mg/mL respectively, the concentration of polyvinylpyrrolidone is 0.4mg/mL;
(3)在真空抽滤辅助的条件下，将P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液分别均匀滴涂在玻璃纤维滤膜上，玻璃纤维滤膜的大小为2mm*20mm。P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液的滴涂量分别为0.4mL/cm2，滴涂完成后将玻璃纤维滤膜转移到真空烘箱中于80℃真空干燥得到粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜；(3) P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions were uniformly drop-coated on glass fiber filter membranes under the assistance of vacuum filtration, respectively. The size of the fiber filter membrane is 2mm*20mm. P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions were applied with a drop coating volume of 0.4 mL/cm 2 respectively. After the drop coating was completed, the glass fiber filter was transferred to a vacuum oven. The bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire film was obtained by vacuum drying at 80° C.
(4)将粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜按照一定的间距垂直交错排列，并夹在两张复印纸之间，薄膜之间的间距大小为2mm。将夹有玻璃纤维滤膜的两张复印纸放置于压片机中以40Mpa的压力挤压后取出，去掉玻璃纤维滤膜背面的复印纸，再用刷子去掉碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜背面的玻璃纤维滤膜碎片，得到以复印纸为基底的P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜垂直交叉阵列；(4) The bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire films adhered to the glass fiber filter membrane are vertically staggered according to a certain spacing, and sandwiched between two copy papers, The gap size between the films is 2mm. Place two copy papers sandwiched with glass fiber filter in a tablet press and squeeze them out at a pressure of 40Mpa, remove the copy paper on the back of the glass fiber filter, and then remove the bismuth telluride base (Bi, Sb) with a brush. 2 (Te,Se) 3 nanowire film on the back of the glass fiber filter fragments, obtained P-type and N-type bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire film vertical on copy paper cross array;
(5)在以复印纸为基底的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列交叉节点处涂覆导电银胶作为电极及传热层，在薄膜两端也涂覆上导电银胶作为电极，导电银胶的涂覆厚度为10μm，涂覆完成后将纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列置于真空烘箱中于60℃干燥30分钟使银胶固化，得到柔性薄膜器件(其示意图如图1所示，实物如图2所示)。以5毫米的弯折半径对器件进行弯折测试，图3所示的测试结果表明弯折400次后器件电阻增加约23％；(5) Coating conductive silver paste as electrode and heat transfer layer at the intersection of bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array based on copy paper, and also on both ends of the thin film. Coated with conductive silver paste as electrodes, the coating thickness of conductive silver paste is 10 μm, after coating, the paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array is placed in a vacuum oven The silver glue was cured by drying at 60° C. for 30 minutes to obtain a flexible thin-film device (the schematic diagram is shown in FIG. 1 , and the real object is shown in FIG. 2 ). The device is subjected to a bending test with a bending radius of 5 mm. The test results shown in Figure 3 show that the resistance of the device increases by about 23% after 400 times of bending;
(6)在纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜两端的银胶电极上用空心小铆钉及连接端子连接上导线(如图4所示)，再采用刮涂法在整个纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列表面涂覆一层导热硅胶作为封装层，使整个纳米线薄膜阵列及电极区域都完全被覆盖，导热硅胶涂覆厚度为10μm；(6) Use small hollow rivets and connecting terminals to connect wires (as shown in Figure 4) on the silver glue electrodes at both ends of the paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire film (as shown in Figure 4), and then A layer of thermally conductive silica gel was coated on the surface of the entire paper substrate bismuth telluride-based (Bi,Sb) 2 (Te, Se) 3 nanowire thin film array by the blade coating method as an encapsulation layer, so that the entire nanowire thin film array and the electrode area were completely is covered, and the thickness of thermally conductive silica gel coating is 10 μm;
(7)最后将涂覆导热硅胶的纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列放置在真空烘箱中于60℃真空烘干3小时即得到纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线柔性热电偶型温度传感器(如图5所示)。(7) Finally, the paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array coated with thermally conductive silica gel was placed in a vacuum oven at 60 °C for vacuum drying for 3 hours to obtain paper-based tellurium Bismuth (Bi, Sb) 2 (Te, Se) 3 nanowire flexible thermocouple temperature sensor (shown in Figure 5).
测试碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜的厚度约为10微米，其温度响应时间约100微秒。传感器所测量的温差与相应输出电压曲线如图6所示，可以看出温差每提高5度，传感器输出电压约提升0.5毫伏，具有较好的灵敏度。The thickness of the tested bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire film is about 10 microns, and its temperature response time is about 100 microseconds. The temperature difference measured by the sensor and the corresponding output voltage curve are shown in Figure 6. It can be seen that every time the temperature difference increases by 5 degrees, the output voltage of the sensor increases by about 0.5 mV, which has better sensitivity.
实施例2：Example 2:
(1)分别取400mg P型及400mgN型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末置于管式炉中，在氢/氩混合气氛中于280℃退火150分钟得到退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末；(1) 400 mg of P-type and 400 mg of N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were taken and placed in a tube furnace, and annealed at 280 °C for 150 minutes in a hydrogen/argon mixed atmosphere P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders are obtained after annealing;
(2)将退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末分别与6mg的聚乙烯吡咯烷酮混合超声分散在10mL乙二醇溶剂中得到P型及N型的碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液；P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线的浓度分别为40mg/mL，聚乙烯吡咯烷酮浓度为0.6mg/mL；(2) The annealed P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were respectively mixed with 6 mg of polyvinylpyrrolidone and ultrasonically dispersed in 10 mL of ethylene glycol solvent to obtain P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions; the concentration of P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowires 40mg/mL respectively, the concentration of polyvinylpyrrolidone is 0.6mg/mL;
(3)在真空抽滤辅助的条件下，将P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液分别均匀滴涂在玻璃纤维滤膜上，玻璃纤维滤膜的大小为20mm*100mm。P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液的滴涂量分别为0.6mL/cm2，滴涂完成后将玻璃纤维滤膜转移到真空烘箱中于80℃真空干燥得到粘附在玻璃纤维滤膜上的(碲化铋基Bi,Sb)2(Te,Se)3纳米线薄膜；(3) P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions were uniformly drop-coated on glass fiber filter membranes under the assistance of vacuum filtration, respectively. The size of the fiber filter membrane is 20mm*100mm. The amount of P-type and N-type bismuth telluride based (Bi,Sb) 2 (Te,Se) 3 nanowire dispersions was respectively 0.6mL/cm 2 , and the glass fiber filter membrane was transferred to a vacuum oven after the drop coating was completed. The (bismuth telluride-based Bi, Sb) 2 (Te, Se) 3 nanowire film was obtained by vacuum drying at 80° C.
(4)将粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜按照一定的间距垂直交错排列，并夹在两张复印纸之间，薄膜之间的间距大小为20mm。将夹有玻璃纤维滤膜的两张复印纸放置于压片机中以30Mpa的压力挤压后取出，去掉玻璃纤维滤膜背面的复印纸，再用刷子去掉碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜背面的玻璃纤维滤膜碎片，得到以复印纸为基底的P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜垂直交叉阵列；(4) The bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire films adhered to the glass fiber filter membrane are vertically staggered according to a certain spacing, and sandwiched between two copy papers, The gap size between the films is 20mm. Place two copy papers sandwiched with glass fiber membrane in a tablet press and squeeze them out at a pressure of 30Mpa, remove the copy paper on the back of the glass fiber membrane, and then remove the bismuth telluride base (Bi, Sb) with a brush. 2 (Te,Se) 3 nanowire film on the back of the glass fiber filter fragments, obtained P-type and N-type bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire film vertical on copy paper cross array;
(5)在以复印纸为基底的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列交叉节点处涂覆导电银胶作为电极及传热层，在薄膜两端也涂覆上导电银胶作为电极，导电银胶的涂覆厚度为1μm，涂覆完成后将纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列置于真空烘箱中于60℃干燥30分钟使银胶固化；(5) Coating conductive silver paste as electrode and heat transfer layer at the intersection of bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array based on copy paper, and also on both ends of the thin film. Coated with conductive silver paste as electrodes, the coating thickness of conductive silver paste was 1 μm, after coating, the paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array was placed in a vacuum oven Dry at 60°C for 30 minutes to cure the silver glue;
(6)在纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜两端的银胶电极上用空心小铆钉及连接端子连接上导线，再采用刮涂法在整个纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列表面涂覆一层导热硅胶作为封装层，使整个纳米线薄膜阵列及电极区域都完全被覆盖，导热硅胶涂覆厚度为20μm；(6) Connect the wires with small hollow rivets and connecting terminals on the silver glue electrodes at both ends of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire film on the paper substrate, and then use the blade coating method to coat the entire paper. The surface of the base bismuth telluride-based (Bi,Sb) 2 (Te, Se) 3 nanowire thin film array is coated with a layer of thermally conductive silica gel as an encapsulation layer, so that the entire nanowire thin film array and the electrode area are completely covered, and the thermal conductive silica gel is coated The thickness is 20μm;
(7)最后将涂覆导热硅胶的纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列放置在真空烘箱中于60℃真空烘干3小时即得到纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线柔性热电偶型温度传感器。(7) Finally, the paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array coated with thermally conductive silica gel was placed in a vacuum oven at 60 °C for vacuum drying for 3 hours to obtain paper-based tellurium Bismuth (Bi,Sb) 2 (Te,Se) 3 nanowire flexible thermocouple temperature sensor.
实施例3：Example 3:
(1)分别取600mg P型及600mgN型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末置于管式炉中，在氢/氩混合气氛中于250℃退火300分钟得到退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末；(1) 600 mg of P-type and 600 mg of N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were taken and placed in a tube furnace, and annealed at 250 °C for 300 minutes in a hydrogen/argon mixed atmosphere P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders are obtained after annealing;
(2)将退火后P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线粉末分别与8mg的聚乙烯吡咯烷酮混合超声分散在10mL乙二醇溶剂中得到P型及N型的碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液；P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线的浓度分别为60mg/mL，聚乙烯吡咯烷酮浓度为0.8mg/mL；(2) The annealed P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire powders were respectively mixed with 8 mg of polyvinylpyrrolidone and ultrasonically dispersed in 10 mL of ethylene glycol solvent to obtain P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions; the concentration of P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowires 60mg/mL respectively, and the concentration of polyvinylpyrrolidone was 0.8mg/mL;
(3)在真空抽滤辅助的条件下，将P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液分别均匀滴涂在玻璃纤维滤膜上，玻璃纤维滤膜的大小为15mm*50mm。P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线分散液的滴涂量分别为1mL/cm2，滴涂完成后将玻璃纤维滤膜转移到真空烘箱中于80℃真空干燥得到粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜；(3) P-type and N-type bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire dispersions were uniformly drop-coated on glass fiber filter membranes under the assistance of vacuum filtration, respectively. The size of the fiber filter membrane is 15mm*50mm. The amount of P-type and N-type bismuth telluride based (Bi,Sb) 2 (Te,Se) 3 nanowire dispersions was 1mL/cm 2 , respectively. After the drop coating was completed, the glass fiber filter was transferred to a vacuum oven. The bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire film was obtained by vacuum drying at 80°C and adhered to the glass fiber membrane;
(4)将粘附在玻璃纤维滤膜上的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜按照一定的间距垂直交错排列，并夹在两张复印纸之间，薄膜之间的间距大小为5mm。将夹有玻璃纤维滤膜的两张复印纸放置于压片机中以20Mpa的压力挤压后取出，去掉玻璃纤维滤膜背面的复印纸，再用刷子去掉碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜背面的玻璃纤维滤膜碎片，得到以复印纸为基底的P型及N型碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜垂直交叉阵列；(4) The bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire films adhered to the glass fiber filter membrane are vertically staggered according to a certain spacing, and sandwiched between two copy papers, The gap size between the films is 5mm. Place two copy papers sandwiched with glass fiber filter in a tablet press and squeeze them out at a pressure of 20Mpa, remove the copy paper on the back of the glass fiber filter, and remove the bismuth telluride base (Bi, Sb) with a brush. 2 (Te,Se) 3 nanowire film on the back of the glass fiber filter fragments, obtained P-type and N-type bismuth telluride-based (Bi,Sb) 2 (Te,Se) 3 nanowire film vertical on copy paper cross array;
(5)在以复印纸为基底的碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列交叉节点处交叉节点处涂覆导电银胶作为电极及传热层，在薄膜两端也涂覆上导电银胶作为电极，导电银胶的涂覆厚度为3μm，涂覆完成后将纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列置于真空烘箱中于60℃干燥30分钟使银胶固化；(5) Coating conductive silver paste as electrodes and heat transfer layers at the intersection nodes of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film arrays based on copy paper. Both ends are also coated with conductive silver paste as electrodes, and the coating thickness of the conductive silver paste is 3 μm. Dry the silver glue in a vacuum oven at 60°C for 30 minutes;
(6)在纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜两端的银胶电极上用空心小铆钉及连接端子连接上导线，再采用刮涂法在整个纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列表面涂覆一层导热硅胶作为封装层，使整个纳米线薄膜阵列及电极区域都完全被覆盖，导热硅胶涂覆厚度为50μm；(6) Connect the wires with small hollow rivets and connecting terminals on the silver glue electrodes at both ends of the bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire film on the paper substrate, and then use the blade coating method to coat the entire paper. The surface of the base bismuth telluride-based (Bi,Sb) 2 (Te, Se) 3 nanowire thin film array is coated with a layer of thermally conductive silica gel as an encapsulation layer, so that the entire nanowire thin film array and the electrode area are completely covered. The thickness is 50μm;
(7)最后将涂覆导热硅胶的纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线薄膜阵列放置在真空烘箱中于60℃真空烘干3小时即得到纸基底碲化铋基(Bi,Sb)2(Te,Se)3纳米线柔性热电偶型温度传感器。(7) Finally, the paper-based bismuth telluride-based (Bi, Sb) 2 (Te, Se) 3 nanowire thin film array coated with thermally conductive silica gel was placed in a vacuum oven at 60 °C for vacuum drying for 3 hours to obtain paper-based tellurium Bismuth (Bi,Sb) 2 (Te,Se) 3 nanowire flexible thermocouple temperature sensor.
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