CN102522490A - Preparation method for glass micro-needle thermocouple - Google Patents
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Abstract
本发明公开一种生物医学工程领域的玻璃微针热电偶的制备方法,包括:在玻璃微针表面沉积一层聚合物薄膜;将玻璃微针放入高温环境裂解,在玻璃微针上生成一层碳薄膜;往玻璃微针中注入金属液体并冷却;将玻璃微针尖端磨制出一定角度;最后在玻璃微针尖端沉积一层金属薄膜,形成热电偶热端接合点,得到最终所需要的玻璃微针热电偶。本发明制备玻璃微针热电偶工艺过程简单易操作。采用碳薄膜和生物相容性金属作为热电偶材料,热电性质稳定,有足够的物理化学稳定性,不易氧化或腐蚀;电阻温度系数小,导电率高,比热小;材料复制性好,机械强度高;生物相容性好,可以直接应用于生物医学领域。
The invention discloses a method for preparing a glass microneedle thermocouple in the field of biomedical engineering. carbon thin film; inject metal liquid into the glass microneedle and cool it; grind the tip of the glass microneedle to a certain angle; glass microneedle thermocouple. The process of preparing the glass microneedle thermocouple is simple and easy to operate. Carbon film and biocompatible metal are used as thermocouple materials, with stable thermoelectric properties, sufficient physical and chemical stability, and not easy to be oxidized or corroded; small temperature coefficient of resistance, high conductivity, and small specific heat; good material reproduction, mechanical High strength; good biocompatibility, can be directly applied to the field of biomedicine.
Description
技术领域 technical field
本发明涉及一种生物医学工程领域的玻璃微针热电偶制备方法,具体是一种以玻璃微针内部的金属和微针表面的碳薄膜作为导体的玻璃微针热电偶的制备方法。The invention relates to a method for preparing a glass microneedle thermocouple in the field of biomedical engineering, in particular to a method for preparing a glass microneedle thermocouple using metal inside the glass microneedle and a carbon film on the surface of the microneedle as conductors.
背景技术 Background technique
随着生物技术、半导体技术等在微纳观领域的高速发展,对微尺度结构和材料的研究受到越来越多的关注,尤其在实验技术领域,能对特征尺度在微纳尺度的检测对象进行直接、实时的检测和操纵成为微尺度研究领域的热点,也是研究者们面临的具有挑战性的研究课题。随着原子力显微镜、扫描电镜、超快光源的发展,使得材料的热学、机械、化学、电学、光学和声学性能的研究检测成为可能。With the rapid development of biotechnology and semiconductor technology in the field of micro-nano, more and more attention has been paid to the research on micro-scale structures and materials, especially in the field of experimental technology, which can detect objects with characteristic scales at the micro-nano scale Direct, real-time detection and manipulation has become a hot spot in the field of microscale research, and it is also a challenging research topic for researchers. With the development of atomic force microscope, scanning electron microscope and ultrafast light source, it is possible to study and detect the thermal, mechanical, chemical, electrical, optical and acoustic properties of materials.
微尺度检测技术在生物活动和其他很多物理过程研究中起着很重要的作用。例如,单个细胞的温度检测能在热疗法、癌症检测、代谢物的活动、甲状腺疾病诊断、核酸和蛋白质的热致变性中提供重要的数据。单个细胞温度的实时检测是一个热门研究领域,研究单个细胞在生物过程中的热反应能够提供重要的生理信息。Microscale detection technology plays an important role in the study of biological activities and many other physical processes. For example, temperature detection of single cells can provide important data in thermotherapy, cancer detection, activity of metabolites, thyroid disease diagnosis, heat-induced denaturation of nucleic acids and proteins. Real-time detection of individual cell temperature is a hot research field, and studying the thermal response of individual cells in biological processes can provide important physiological information.
热电偶能直接测量温度,并把温度信号转换成热电动势信号,通过电气仪表转换成被测介质的温度。热电偶测温的基本原理是两种不同成份的导体(称为热电偶丝材或热电极)两端接合成回路,当两个接合点的温度不同时,在回路中就会产生电动势,这种现象称为热电效应,而这种电动势称为热电势。其中,直接用作测量介质温度的一端叫做工作端(也称为测量端),另一端叫做冷端(也称为补偿端),冷端与显示仪表或配套仪表连接,显示仪表会指出热电偶所产生的热电势。在热电偶实际测温应用中,常采用热端焊接、冷端开路的形式,冷端经连接导线与显示仪表连接构成测温系统。The thermocouple can directly measure the temperature, and convert the temperature signal into a thermal electromotive force signal, and convert it into the temperature of the measured medium through an electrical instrument. The basic principle of thermocouple temperature measurement is that two conductors with different components (called thermocouple wire or hot electrode) are connected into a loop at both ends. When the temperature of the two junctions is different, an electromotive force will be generated in the loop. This phenomenon is called thermoelectric effect, and this electromotive force is called thermoelectric force. Among them, the end directly used to measure the temperature of the medium is called the working end (also called the measuring end), and the other end is called the cold end (also called the compensation end). The resulting thermoelectric potential. In the actual temperature measurement application of thermocouples, the form of welding the hot end and opening the cold end is often used. The cold end is connected to the display instrument through the connecting wire to form a temperature measurement system.
从理论上讲,任何两种不同导体(或半导体)都可以配制成热电偶,但是作为实用的测温元件,对它的要求是多方面的。为了保证工程技术中的可靠性,以及足够的测量精度,并不是所有材料都能组成热电偶,一般对热电偶的电极材料,基本要求是:(1)、在测温范围内,热电性质稳定,不随时间而变化,有足够的物理化学稳定性,不易氧化或腐蚀;(2)、电阻温度系数小,导电率高,比热小;(3)、测温中产生热电势要大,并且热电势与温度之间呈线性或接近线性的单值函数关系;(4)、材料复制性好,机械强度高,制造工艺简单,价格便宜。Theoretically, any two different conductors (or semiconductors) can be formulated into thermocouples, but as a practical temperature measuring element, there are many requirements for it. In order to ensure the reliability of engineering technology and sufficient measurement accuracy, not all materials can form thermocouples. Generally, the basic requirements for electrode materials of thermocouples are: (1) Stable thermoelectric properties within the temperature measurement range , does not change with time, has sufficient physical and chemical stability, and is not easy to oxidize or corrode; (2), the temperature coefficient of resistance is small, the conductivity is high, and the specific heat is small; (3), the thermoelectric potential generated during temperature measurement is large, and The relationship between thermoelectric potential and temperature is a linear or nearly linear single-value function; (4), the material has good reproducibility, high mechanical strength, simple manufacturing process and low price.
经对现有技术文献的检索发现,R.Shrestha,T.Y.Choi,W.S.Chang等在《IEEE SENSORS 2010 Conference》(2010)p422-445撰文“Micropipette-BasedThermal Sensor for Biological Applications”(“基于微针的生物温度传感器”《2010年IEEE传感器会议》)。该文中采用玻璃微针内部通入的锡和玻璃微针表面沉积的镍作为热电偶材料。这种方法制作的热电偶探针由于使用了对细胞有毒害作用的金属镍,因此在应用上受到限制。After searching the prior art documents, it was found that R.Shrestha, T.Y.Choi, W.S.Chang et al wrote the article "Micropipette-Based Thermal Sensor for Biological Applications" ("Microneedle-based biological Temperature Sensors" "2010 IEEE Sensors Conference"). In this paper, tin injected into the glass microneedle and nickel deposited on the surface of the glass microneedle were used as thermocouple materials. The thermocouple probe made by this method is limited in application due to the use of metallic nickel, which is toxic to cells.
发明内容 Contents of the invention
本发明的目的在于克服现有技术的不足和缺陷,提出一种玻璃微针热电偶的制备方法,使得玻璃微针热电偶能够应用于生物医学微尺度领域的温度测量。由于采用生物相容性金属和碳薄膜作为热电偶材料,因此能够直接应用于测量单个细胞的温度。The purpose of the present invention is to overcome the deficiencies and defects of the prior art, and propose a method for preparing a glass microneedle thermocouple, so that the glass microneedle thermocouple can be applied to temperature measurement in the microscale field of biomedicine. Due to the use of biocompatible metal and carbon films as thermocouple materials, it can be directly applied to measure the temperature of single cells.
本发明是通过以下技术方案实现的,本发明首先在玻璃微针上沉积一层聚合物薄膜,其次将玻璃微针放入高温环境裂解,在玻璃微针上生成一层碳薄膜,然后往玻璃微针中注入金属液体并冷却,接着将玻璃微针尖端磨制出一定角度,最后在玻璃微针尖端沉积一层金属,得到最终所需要的玻璃微针热电偶。The present invention is achieved through the following technical solutions. The present invention firstly deposits a layer of polymer film on the glass microneedle, and then puts the glass microneedle into a high-temperature environment for cracking to form a layer of carbon film on the glass microneedle, and then deposits a layer of polymer film on the glass microneedle. The metal liquid is injected into the microneedle and cooled, then the tip of the glass microneedle is ground to a certain angle, and finally a layer of metal is deposited on the tip of the glass microneedle to obtain the final required glass microneedle thermocouple.
本发明包括以下步骤:The present invention comprises the following steps:
第一步、在玻璃微针表面沉积一层聚合物薄膜。The first step is to deposit a polymer film on the surface of the glass microneedles.
所述的玻璃微针为石英玻璃微针。The glass microneedles are quartz glass microneedles.
所述的玻璃微针尖端尺寸为微米到纳米级。The size of the tip of the glass microneedle is from micrometer to nanometer.
所述的沉积是化学气相沉积。Said deposition is chemical vapor deposition.
所述的聚合物薄膜厚度为微米到纳米级。The thickness of the polymer film is micron to nanometer.
第二步、将玻璃微针放入高温环境裂解,在玻璃微针上生成一层碳薄膜。In the second step, the glass microneedles are cracked in a high-temperature environment, and a layer of carbon film is formed on the glass microneedles.
所述的高温裂解是指将聚合物薄膜放入充满保护气氛的裂解炉中,以150~1400℃温度加热0.5~6小时。The high-temperature cracking refers to putting the polymer film into a cracking furnace filled with a protective atmosphere, and heating at a temperature of 150-1400° C. for 0.5-6 hours.
第三步、往玻璃微针中注入金属液体并冷却。The third step is to inject the metal liquid into the glass microneedle and cool it down.
所述的金属液体为低熔点生物相容性金属及其合金。The metal liquid is a biocompatible metal with a low melting point and its alloy.
第四步、将玻璃微针尖端磨制出角度。The fourth step is to grind the tip of the glass microneedle into an angle.
所述的磨制为在磨针仪下将玻璃微针尖端磨制出所需角度。The grinding is to grind the tip of the glass microneedle to a desired angle under a needle grinder.
第五步、玻璃微针尖端沉积一层金属薄膜,形成热电偶热端接合点,得到最终所需要的玻璃微针热电偶。The fifth step is to deposit a layer of metal film on the tip of the glass microneedle to form the thermocouple hot end junction, and obtain the final required glass microneedle thermocouple.
所述的金属为生物相容性金属,厚度为微米到纳米级。The metal is a biocompatible metal with a thickness ranging from micron to nanometer.
与现有技术相比,本发明制备玻璃微针热电偶工艺过程简单易操作。采用碳薄膜和生物相容性金属作为热电偶材料,热电性质稳定,有足够的物理化学稳定性,不易氧化或腐蚀;电阻温度系数小,导电率高,比热小;材料复制性好,机械强度高;生物相容性好,可以直接应用于生物医学领域。Compared with the prior art, the process of preparing glass microneedle thermocouples in the present invention is simple and easy to operate. Carbon film and biocompatible metal are used as thermocouple materials, with stable thermoelectric properties, sufficient physical and chemical stability, and not easy to be oxidized or corroded; small temperature coefficient of resistance, high conductivity, and small specific heat; good material reproduction, mechanical High strength; good biocompatibility, can be directly applied to the field of biomedicine.
附图说明 Description of drawings
图1为本发明实施例1实施过程示意图。Fig. 1 is a schematic diagram of the implementation process of
图2为本发明实施例2实施过程示意图。Fig. 2 is a schematic diagram of the implementation process of
图3为本发明实施例3实施过程示意图。Fig. 3 is a schematic diagram of the implementation process of
具体实施方式 Detailed ways
下面结合附图对本发明的实施例做详细说明:本实施例以本发明技术方案为前提进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。Embodiments of the present invention are described in detail below in conjunction with the accompanying drawings: the present embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to the following Example.
实施例1Example 1
如图1所示,本实施例通过以下步骤进行制备:As shown in Figure 1, the present embodiment is prepared through the following steps:
第一步、在尖端外径0.5微米的玻璃微针表面化学气相沉积一层厚度为5微米的Parylene C(聚一氯对二甲苯)薄膜,如图1a所示,1是Parylene C薄膜,2是石英玻璃微针。The first step, on the surface of the glass microneedle with a tip outer diameter of 0.5 micron, the chemical vapor deposition layer is a 5 micron Parylene C (polychloroparaxylylene) film, as shown in Figure 1a, 1 is the Parylene C film, 2 It is a quartz glass microneedle.
第二步、将表面沉积有Parylene C薄膜的玻璃微针放入充满氮气保护气氛的裂解炉中,以900℃温度加热1小时(此操作在150~1400℃温度加热0.5~6小时范围内均能实施),裂解Parylene C薄膜,在玻璃微针上生成一层碳薄膜,如图1b所示,1为碳薄膜,2为石英玻璃微针。The second step is to put the glass microneedle with the Parylene C film deposited on the surface into a cracking furnace filled with a nitrogen protective atmosphere, and heat it at 900°C for 1 hour (this operation can be performed at a temperature of 150-1400°C for 0.5-6 hours). can implement), crack Parylene C thin film, generate one layer of carbon thin film on glass microneedle, as shown in Figure 1b, 1 is carbon thin film, 2 is quartz glass microneedle.
第三步、往玻璃微针中注入无铅焊锡液体并冷却,如图1c所示,1是碳薄膜,2是石英玻璃微针,3是无铅焊锡。The third step is to inject lead-free solder liquid into the glass microneedle and cool it down, as shown in Figure 1c, 1 is a carbon film, 2 is a quartz glass microneedle, and 3 is lead-free solder.
第四步、使用磨针仪将玻璃微针尖端磨制出45°,如图1d所示,1是碳薄膜,2是石英玻璃微针,3是无铅焊锡。The fourth step is to use a needle grinder to grind the tip of the glass microneedle to 45°, as shown in Figure 1d, 1 is a carbon film, 2 is a quartz glass microneedle, and 3 is lead-free solder.
第五步、玻璃微针尖端沉积一层200纳米厚的金薄膜,形成热电偶热端接合点,得到最终所需要的玻璃微针热电偶,如图1e所示,1是碳薄膜,2是石英玻璃微针,3是无铅焊锡,4是金薄膜。In the fifth step, a 200-nm-thick gold film is deposited on the tip of the glass microneedle to form a thermocouple hot-end junction to obtain the final required glass microneedle thermocouple. As shown in Figure 1e, 1 is a carbon film, and 2 is a Quartz glass microneedle, 3 is lead-free solder, 4 is gold film.
实施例2Example 2
如图2所示,本实施例通过以下步骤进行制备:As shown in Figure 2, the present embodiment is prepared through the following steps:
第一步、在尖端外径1微米的玻璃微针表面化学气相沉积一层厚度为8微米的PP(聚丙烯)薄膜,如图2a所示,1是PP薄膜,2是石英玻璃微针。The first step is to chemical vapor deposit a layer of PP (polypropylene) film with a thickness of 8 microns on the surface of the glass microneedle with a tip outer diameter of 1 micron, as shown in Figure 2a, 1 is the PP film, and 2 is the quartz glass microneedle.
第二步、将表面沉积有PP薄膜的玻璃微针放入充满氮气保护气氛的裂解炉中,以700℃温度加热1小时,裂解PP薄膜,在玻璃微针上生成一层碳薄膜,如图2b所示,1为碳薄膜,2为石英玻璃微针。The second step is to put the glass microneedle with PP film deposited on the surface into a pyrolysis furnace filled with nitrogen protection atmosphere, heat it at 700°C for 1 hour, crack the PP film, and form a layer of carbon film on the glass microneedle, as shown in the figure As shown in 2b, 1 is a carbon film, and 2 is a quartz glass microneedle.
第三步、在保护气氛中往玻璃微针里注入锌镁合金液体并冷却,如图2c所示,1是碳薄膜,2是石英玻璃微针,3是锌镁合金。The third step is to inject zinc-magnesium alloy liquid into the glass microneedle in a protective atmosphere and cool it down, as shown in Figure 2c, 1 is a carbon film, 2 is a quartz glass microneedle, and 3 is a zinc-magnesium alloy.
第四步、使用磨针仪将玻璃微针尖端磨制出45°,如图2d所示,1是碳薄膜,2是石英玻璃微针,3是锌镁合金。The fourth step is to use a needle grinder to grind the tip of the glass microneedle to 45°, as shown in Figure 2d, 1 is a carbon film, 2 is a quartz glass microneedle, and 3 is a zinc-magnesium alloy.
第五步、玻璃微针尖端沉积一层150纳米厚的金薄膜,形成热电偶热端接合点,得到最终所需要的玻璃微针热电偶,如图2e所示,1是碳薄膜,2是石英玻璃微针,3是锌镁合金,4是金薄膜。In the fifth step, deposit a 150-nm-thick gold film on the tip of the glass microneedle to form a thermocouple hot-end junction to obtain the final required glass microneedle thermocouple. As shown in Figure 2e, 1 is a carbon film and 2 is a Quartz glass microneedle, 3 is a zinc-magnesium alloy, and 4 is a gold film.
实施例3Example 3
如图3所示,本实施例通过以下步骤进行制备:As shown in Figure 3, the present embodiment is prepared through the following steps:
第一步、在尖端外径1微米的玻璃微针表面化学气相沉积一层厚度为8微米的GDP(辉光放电聚合物)薄膜,如图3a所示,1是GDP薄膜,2是石英玻璃微针。The first step is to chemical vapor deposit a layer of GDP (glow discharge polymer) film with a thickness of 8 microns on the surface of the glass microneedle with a tip outer diameter of 1 micron, as shown in Figure 3a, 1 is the GDP film, and 2 is the quartz glass Microneedles.
第二步、将表面沉积有GDP薄膜的玻璃微针放入充满氮气保护气氛的裂解炉中,以500℃温度加热1小时,裂解GDP薄膜,在玻璃微针上生成一层碳薄膜,如图3b所示,1为碳薄膜,2为石英玻璃微针。The second step is to put the glass microneedle with the GDP film deposited on the surface into a pyrolysis furnace filled with nitrogen protection atmosphere, heat at 500°C for 1 hour, crack the GDP film, and form a layer of carbon film on the glass microneedle, as shown in the figure As shown in 3b, 1 is a carbon film, and 2 is a quartz glass microneedle.
第三步、在保护气氛中往玻璃微针里注入镁金属液体并冷却,如图3c所示,1是碳薄膜,2是镁,3是玻璃微针。The third step is to inject magnesium metal liquid into the glass microneedle in a protective atmosphere and cool it down, as shown in Figure 3c, 1 is a carbon film, 2 is magnesium, and 3 is a glass microneedle.
第四步、使用磨针仪将玻璃微针尖端磨制出30°,如图3d所示,1是碳薄膜,2是石英玻璃微针,3是镁金属。The fourth step is to use a needle grinder to grind the tip of the glass microneedle to 30°, as shown in Figure 3d, 1 is a carbon film, 2 is a quartz glass microneedle, and 3 is magnesium metal.
第五步、玻璃微针尖端沉积一层200纳米厚的金薄膜,形成热电偶热端接合点,如图3e所示,1是碳薄膜,2是石英玻璃微针,3是镁金属,4是金薄膜。Step 5: Deposit a 200nm-thick gold film on the tip of the glass microneedle to form the thermocouple hot junction, as shown in Figure 3e, 1 is a carbon film, 2 is a quartz glass microneedle, 3 is magnesium metal, 4 It's a gold film.
上述实施例的工艺简单、易操作。采用碳薄膜和生物相容性金属作为热电偶材料,热电性质稳定,有足够的物理化学稳定性,不易氧化或腐蚀;电阻温度系数小,导电率高,比热小;材料复制性好,机械强度高;生物相容性好,可以直接应用于生物医学领域。应当理解的是,上述实施例只是本发明的优选实施,本发明还可以是其他的实施方式,如变换其中的参数(如高温裂解温度150~1400℃,角度以及时间等参数)。The process of the above embodiment is simple and easy to operate. Carbon film and biocompatible metal are used as thermocouple materials, with stable thermoelectric properties, sufficient physical and chemical stability, and not easy to be oxidized or corroded; small temperature coefficient of resistance, high conductivity, and small specific heat; good material reproduction, mechanical High strength; good biocompatibility, can be directly applied to the field of biomedicine. It should be understood that the foregoing embodiments are only preferred implementations of the present invention, and the present invention can also be other implementations, such as changing parameters therein (such as high temperature cracking temperature 150-1400° C., parameters such as angle and time).
尽管本发明的内容已经通过上述优选实施例作了详细介绍,但应当认识到上述的描述不应被认为是对本发明的限制。在本领域技术人员阅读了上述内容后,对于本发明的多种修改和替代都将是显而易见的。因此,本发明的保护范围应由所附的权利要求来限定。Although the content of the present invention has been described in detail through the above preferred embodiments, it should be understood that the above description should not be considered as limiting the present invention. Various modifications and alterations to the present invention will become apparent to those skilled in the art upon reading the above disclosure. Therefore, the protection scope of the present invention should be defined by the appended claims.
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CN106768445A (en) * | 2016-12-29 | 2017-05-31 | 北京航空航天大学 | A kind of quick response temperature thermocouple |
CN108387320A (en) * | 2018-02-08 | 2018-08-10 | 北京航空航天大学 | A kind of permanent mold casting quick response temperature thermocouple |
CN108414106A (en) * | 2018-02-08 | 2018-08-17 | 北京航空航天大学 | A kind of casting mould quick response temperature thermocouple |
CN111076836A (en) * | 2019-12-12 | 2020-04-28 | 西安交通大学 | Metal-oxide type thin film thermocouple and preparation method thereof |
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CN1357930A (en) * | 2000-12-08 | 2002-07-10 | 中国科学院长春光学精密机械与物理研究所 | New-type thermocouple produced by means of photoetching techn and gas-phase deposition techn |
CN101493360A (en) * | 2009-01-05 | 2009-07-29 | 东南大学 | Thermocouple with micron or nanometer grade tip curvature radius and method for producing the same |
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CN1357930A (en) * | 2000-12-08 | 2002-07-10 | 中国科学院长春光学精密机械与物理研究所 | New-type thermocouple produced by means of photoetching techn and gas-phase deposition techn |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106768445A (en) * | 2016-12-29 | 2017-05-31 | 北京航空航天大学 | A kind of quick response temperature thermocouple |
CN106768445B (en) * | 2016-12-29 | 2018-10-30 | 北京航空航天大学 | A kind of quick response temperature thermocouple |
CN108387320A (en) * | 2018-02-08 | 2018-08-10 | 北京航空航天大学 | A kind of permanent mold casting quick response temperature thermocouple |
CN108414106A (en) * | 2018-02-08 | 2018-08-17 | 北京航空航天大学 | A kind of casting mould quick response temperature thermocouple |
CN108414106B (en) * | 2018-02-08 | 2019-07-12 | 北京航空航天大学 | A fast-response temperature measuring thermocouple for casting molds |
CN111076836A (en) * | 2019-12-12 | 2020-04-28 | 西安交通大学 | Metal-oxide type thin film thermocouple and preparation method thereof |
CN111076836B (en) * | 2019-12-12 | 2020-10-27 | 西安交通大学 | Metal-oxide type thin film thermocouple and preparation method thereof |
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