CN117191924B - In-situ analysis and detection device for molecular pollutants with efficient separation and dynamic characterization - Google Patents
In-situ analysis and detection device for molecular pollutants with efficient separation and dynamic characterization Download PDFInfo
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Abstract
Description
技术领域Technical Field
本发明涉及一种高效分离和动态表征的分子污染物原位分析检测装置，属于分子污染物分析检测技术领域。The invention relates to an in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization, belonging to the technical field of molecular pollutant analysis and detection.
背景技术Background technique
近年来，我国完成了以月球探测、火星探测、空间站建造为代表的航天重大工程，中国航天科技不断到达新高度。在航天在轨期间，有机材料在高真空环境下释放的分子污染物沉积在敏感载荷表面，对航天器精密电子、光学仪器的效率和寿命构成重大威胁，使航天器在稳定性上遇到了艰巨的挑战。随着我国空间载荷向着高精密和高稳定性发展，实现航天器在轨分子污染防护与控制是航天器急需解决的重要问题之一。其中污染物成分组成的精确确定和挥发行为分析对于空间分子污染物防控研究至关重要。In recent years, my country has completed major aerospace projects represented by lunar exploration, Mars exploration, and space station construction, and China's aerospace technology has continued to reach new heights. During the in-orbit period of spaceflight, molecular pollutants released by organic materials in a high vacuum environment are deposited on the surface of sensitive payloads, posing a major threat to the efficiency and life of precision electronic and optical instruments in spacecraft, and making spacecraft face arduous challenges in stability. As my country's space payloads develop towards high precision and high stability, achieving in-orbit molecular contamination protection and control of spacecraft is one of the important issues that spacecraft urgently need to solve. Among them, the precise determination of pollutant composition and the analysis of volatilization behavior are crucial for the prevention and control of space molecular pollutants.
现阶段对分子污染物的组成研究常使用石英晶体微天平(QCM)、质谱仪(MS)和气相色谱(GC)。其中QCM只能研究总污染混合物的成分和挥发行为而不能确定实际不同污染物组成成分的单独贡献。尽管气质联用(GC/MS)能够将混合污染物实现一定程度的分离，但无法实现原位分离和实时动态分析。因此实现不同种类污染物分子的原位分离和检测具有重大意义。At present, the composition of molecular pollutants is often studied using quartz crystal microbalance (QCM), mass spectrometer (MS) and gas chromatography (GC). Among them, QCM can only study the composition and volatility of the total pollutant mixture but cannot determine the individual contributions of different pollutant components. Although gas chromatography-mass spectrometry (GC/MS) can achieve a certain degree of separation of mixed pollutants, it cannot achieve in-situ separation and real-time dynamic analysis. Therefore, it is of great significance to achieve in-situ separation and detection of different types of pollutant molecules.
研究空间分子污染物组成的方法有很多但各有不足。石英晶体微天平具有多温度步骤数据拟合的优势，但石英晶体微天平只能进行总污染混合物的成分研究，不能确定实际不同种类污染物的单独贡献。气-质联用(GC/MS)被广泛应用于复杂组分的分离与鉴定，但无论GC/MS物质分离的效率如何，都无法原位和实时实施。There are many methods to study the composition of spatial molecular pollutants, but each has its own shortcomings. Quartz crystal microbalance has the advantage of multi-temperature step data fitting, but quartz crystal microbalance can only study the composition of the total pollutant mixture and cannot determine the individual contributions of different types of pollutants. Gas chromatography-mass spectrometry (GC/MS) is widely used in the separation and identification of complex components, but no matter how efficient GC/MS material separation is, it cannot be implemented in situ and in real time.
发明内容Summary of the invention
本发明是为了解决上述技术问题，进而提供了一种高效分离和动态表征的分子污染物原位分析检测装置。The present invention aims to solve the above technical problems and further provides an in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization.
本发明为解决上述技术问题所采用的技术方案是：The technical solution adopted by the present invention to solve the above technical problems is:
一种高效分离和动态表征的分子污染物原位分析检测装置，包括真空仓体、质谱仪、温控仪、真空泵以及设置在真空仓体内的加热辐射板、分子污染物加热台、热防护罩、石英晶体微天平、污染物收集板、QCM温度控制器及安装架，其中，所述加热辐射板安装在真空仓体的内侧壁，所述安装架转动安装在真空仓体的上部，污染物收集板的数量为多个且铺设在安装架的底端，所述石英晶体微天平的数量至少为两个且均嵌装在多个污染物收集板之间，且石英晶体微天平、热防护罩及分子污染物加热台由上到下正对布置，所述石英晶体微天平与所述QCM温度控制器电连接，所述质谱仪固装在真空仓体外部且安装架水平状态下石英晶体微天平、污染物收集板及质谱仪三者等高设置，所述加热辐射板连接设置有温控仪，通过温控仪控制真空仓体内的温度，真空仓体外部连接设置有真空泵，通过真空泵控制真空仓体内的真空度。A molecular pollutant in-situ analysis and detection device for efficient separation and dynamic characterization comprises a vacuum chamber, a mass spectrometer, a temperature controller, a vacuum pump, a heating radiation plate, a molecular pollutant heating platform, a heat shield, a quartz crystal microbalance, a pollutant collecting plate, a QCM temperature controller and a mounting frame arranged in the vacuum chamber, wherein the heating radiation plate is mounted on the inner side wall of the vacuum chamber, the mounting frame is rotatably mounted on the upper part of the vacuum chamber, the number of pollutant collecting plates is multiple and laid on the bottom end of the mounting frame, the number of the quartz crystal microbalance is at least two and both are embedded between the multiple pollutant collecting plates, and the quartz crystal microbalance, the heat shield and the molecular pollutant heating platform are arranged opposite from top to bottom, the quartz crystal microbalance is electrically connected to the QCM temperature controller, the mass spectrometer is fixedly mounted outside the vacuum chamber, and the quartz crystal microbalance, the pollutant collecting plate and the mass spectrometer are arranged at the same height when the mounting frame is in a horizontal state, the heating radiation plate is connected to the temperature controller, and the temperature in the vacuum chamber is controlled by the temperature controller, the vacuum chamber is connected to the outside of the vacuum chamber with a vacuum pump, and the vacuum degree in the vacuum chamber is controlled by the vacuum pump.
进一步地，石英晶体微天平与质谱仪之间的水平距离小于10cm。Furthermore, the horizontal distance between the quartz crystal microbalance and the mass spectrometer is less than 10 cm.
进一步地，分子污染物加热台的顶端面加工有弧形通槽。Furthermore, the top surface of the molecular pollutant heating stage is processed with an arc-shaped through groove.
进一步地，所述真空仓体连接设置有真空计。Furthermore, the vacuum chamber body is connected to a vacuum gauge.
进一步地，所述真空泵包括机械泵及分子泵。Furthermore, the vacuum pump includes a mechanical pump and a molecular pump.
进一步地，加热辐射板的数量为四个，且分别贴设在真空仓体的四个内侧壁上。Furthermore, there are four heating radiation panels, which are respectively attached to four inner side walls of the vacuum chamber body.
进一步地，所述真空仓体内固装有固定板，所述安装架转动安装在固定板上。Furthermore, a fixing plate is fixedly installed in the vacuum chamber body, and the mounting frame is rotatably mounted on the fixing plate.
进一步地，所述真空仓体上设置有仓门及放气阀门。Furthermore, the vacuum chamber body is provided with a chamber door and an air release valve.
一种采用上述装置的分子污染物原位分析检测方法，包括如下步骤：A method for in-situ analysis and detection of molecular pollutants using the above device comprises the following steps:
步骤一、将污染物源放置在分子污染物加热台上；Step 1: Place the contaminant source on the molecular contaminant heating table;
步骤二、采用真空泵对真空仓体进行抽真空至真空度为1×10-5Pa；Step 2: Use a vacuum pump to evacuate the vacuum chamber to a vacuum degree of 1×10 -5 Pa;
步骤三、将加热辐射板加热升温，通过温控仪控制真空仓体内的温度达到室温至400～500K；Step 3: Heat the heating radiation plate and control the temperature in the vacuum chamber to reach room temperature to 400-500K through a temperature controller;
步骤四、通过QCM温度控制器控制石英晶体微天平的温度为150～280K，与加热辐射板相比保持一个相对低温状态；Step 4: Control the temperature of the quartz crystal microbalance to 150-280K through the QCM temperature controller, maintaining a relatively low temperature state compared to the heating radiation plate;
步骤五、开启分子污染物加热台，使分子污染物释放，分子污染物加热台的温度与加热辐射板的温度相同或二者温度相差范围为0～5℃，脱气时间4～6天，污染物分子在石英晶体微天平及污染物收集板上沉积；Step 5: Turn on the molecular pollutant heating platform to release the molecular pollutants. The temperature of the molecular pollutant heating platform is the same as the temperature of the heating radiation plate or the temperature difference between the two is 0 to 5°C. The degassing time is 4 to 6 days. The pollutant molecules are deposited on the quartz crystal microbalance and the pollutant collection plate.
步骤六、沉积过程结束后，关闭加热辐射板及分子污染物加热台，待温控仪显示的温度接近室温后，关闭真空泵；Step 6: After the deposition process is completed, turn off the heating radiation plate and the molecular pollutant heating platform, and turn off the vacuum pump after the temperature displayed by the temperature controller is close to room temperature;
步骤七、打开放气阀门至真空仓体内的真空度为常压，关闭放气阀门，取出污染物材料；Step 7: Open the vent valve until the vacuum degree in the vacuum chamber is normal pressure, close the vent valve, and take out the pollutant material;
步骤八、转动安装架使石英晶体微天平及污染物收集板面向质谱仪；Step 8, rotating the mounting frame so that the quartz crystal microbalance and the contaminant collection plate face the mass spectrometer;
步骤九、依据所选用污染物源的性质确定起始温度和终止温度后，通过QCM温度控制器程序升温重新排放该沉积物，沉积的污染物向质谱仪释放；Step 9: After determining the starting temperature and the ending temperature according to the properties of the selected pollutant source, the QCM temperature controller is programmed to increase the temperature and then the sediment is re-emitted, and the deposited pollutants are released into the mass spectrometer;
步骤十、通过分析沉积物再排放过程中收集的质谱仪数据和石英晶体微天平数据，定量确定不同种类污染物的贡献，并在化学数据库中进行分子识别；通过分析梯度加热阶段收集的质谱仪数据，将检测到的总质量分成不同的种类，通过质谱仪的记录与现成的光谱数据库进行比较，定性识别释放的分子，重新释放污染物与分析过程完成。Step 10. By analyzing the mass spectrometer data and quartz crystal microbalance data collected during the sediment re-emission process, the contribution of different types of pollutants is quantitatively determined, and molecular identification is performed in the chemical database. By analyzing the mass spectrometer data collected during the gradient heating stage, the total detected mass is divided into different types, and the released molecules are qualitatively identified by comparing the mass spectrometer records with the existing spectral database. The re-release of pollutants and the analysis process are completed.
进一步地，步骤九中，QCM温度控制器程序升温速度为1～3K/min。Furthermore, in step nine, the temperature increase rate of the QCM temperature controller program is 1 to 3 K/min.
本发明与现有技术相比具有以下效果：Compared with the prior art, the present invention has the following effects:
为了在试验过程中石英晶体微天平上的污染物沉积量尽可能的多，本发明的高效分离和动态表征的分子污染物原位分析检测装置主要采取两个措施，一是通过将安装架、热防护罩及分子污染物加热台由上到下正对布置，所述石英晶体微天平与所述污染物收集板并列布置在所述安装架上，使得在放气过程中石英晶体微天平面对污染物源，收集污染物释放时的直接通量；二是通过设置热防护罩，使得脱气过程中气态污染物传输过程的损失率大幅度降低，一方面通过热防护罩对气态污染物传输路径提供了限制，另一方面在污染物源脱气过程中，热防护罩始终保持相当高的温度，使得任何污染物都不能吸附在其表面造成传输损失。In order to deposit as much pollutants as possible on the quartz crystal microbalance during the test, the in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention mainly adopts two measures. First, the mounting frame, the heat shield and the molecular pollutant heating platform are arranged opposite to each other from top to bottom, and the quartz crystal microbalance and the pollutant collection plate are arranged side by side on the mounting frame, so that the quartz crystal microbalance faces the pollutant source during the degassing process to collect the direct flux of the pollutants when released; second, by setting the heat shield, the loss rate of the gaseous pollutant transmission process during the degassing process is greatly reduced. On the one hand, the heat shield provides a restriction on the transmission path of the gaseous pollutants. On the other hand, during the degassing process of the pollutant source, the heat shield always maintains a relatively high temperature, so that any pollutants cannot be adsorbed on its surface to cause transmission losses.
本发明中通过在石英晶体微天平上增加污染物收集板，且污染物收集板与石英晶体微天平保持相同的温度，但是污染物收集板的表面积约是石英晶体微天平的十倍，实现在石英晶体微在平梯度加热过程中释放多达十倍的污染物，从而得以加强质谱仪中的信号，增加质谱仪的信噪比，提高测试的灵敏度；另外，通过将安装架转动安装在真空仓体内，使得在沉积过程结束、梯度加热开始之前，石英晶体微天平及污染物收集板会旋转面向质谱仪，沉积的污染物直接面向质谱仪释放，进一步增加质谱仪的信噪比，使得测试的灵敏度进一步提高。In the present invention, a pollutant collecting plate is added to the quartz crystal microbalance, and the pollutant collecting plate and the quartz crystal microbalance are kept at the same temperature, but the surface area of the pollutant collecting plate is about ten times that of the quartz crystal microbalance, so that up to ten times the pollutants can be released during the flat gradient heating process of the quartz crystal microbalance, thereby strengthening the signal in the mass spectrometer, increasing the signal-to-noise ratio of the mass spectrometer, and improving the sensitivity of the test; in addition, by rotating the mounting frame in the vacuum chamber, the quartz crystal microbalance and the pollutant collecting plate will rotate to face the mass spectrometer before the deposition process ends and the gradient heating begins, and the deposited pollutants are released directly facing the mass spectrometer, further increasing the signal-to-noise ratio of the mass spectrometer, so that the sensitivity of the test is further improved.
本发明的高效分离和动态表征的分子污染物原位分析检测装置，能够进行分子污染物的高效分离和原位动态检测，识别每个污染物成分种类，并定量确定每种污染物的含量来补充分析石英晶体微天平总质量损失的测试数据，高灵敏度石英晶体微天平原位梯度加热的质量损失数据和质谱仪数据结合分析来更好地理解不同种类的污染物分子脱气的过程。The in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention can perform high efficiency separation and in-situ dynamic detection of molecular pollutants, identify the type of each pollutant component, and quantitatively determine the content of each pollutant to supplement the analysis of the test data of the total mass loss of the quartz crystal microbalance. The mass loss data of in-situ gradient heating of the high-sensitivity quartz crystal microbalance and the mass spectrometer data are combined for analysis to better understand the degassing process of different types of pollutant molecules.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为本发明的高效分离和动态表征的分子污染物原位分析检测装置的主视示意图(沉积过程下)；FIG1 is a schematic front view of the in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention (under the deposition process);
图2为本发明的高效分离和动态表征的分子污染物原位分析检测装置的主视示意图(再释放过程下)。FIG. 2 is a schematic front view of the in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention (under the re-release process).
具体实施方式Detailed ways
对本发明实施方式中的技术方案进行清楚、完整地描述，显然，所描述的实施方式仅仅是本发明一部分实施方式，而不是全部的实施方式，基于本发明中的实施方式，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施方式，都属于本发明保护的范围。The technical solutions in the embodiments of the present invention are described clearly and completely. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
需要说明的是，本发明关于“左”、“右”、“左侧”、“右侧”、“上部”、“下部”“顶部”“底部”等方向上的描述均是基于附图所示的方位或位置的关系定义的，仅是为了便于描述本发明和简化描述，而不是指示或暗示所述的结构必须以特定的方位构造和操作，因此，不能理解为对本发明的限制。在本发明的描述中，“多个”的含义是两个以上，除非另有明确具体的限定。It should be noted that the descriptions of the present invention regarding directions such as "left", "right", "left side", "right side", "upper", "lower", "top", "bottom", etc. are all defined based on the relationship between the orientations or positions shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the structure must be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention. In the description of the present invention, the meaning of "multiple" is more than two, unless otherwise clearly and specifically defined.
在本发明的描述中，除非另有明确规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。In the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected" and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
具体实施方式一：结合图1及图2说明本实施方式，一种高效分离和动态表征的分子污染物原位分析检测装置，包括真空仓体1、质谱仪2、温控仪3、真空泵以及设置在真空仓体1内的加热辐射板5、分子污染物加热台6、热防护罩7、石英晶体微天平8、污染物收集板9、QCM温度控制器10及安装架，其中，所述加热辐射板5安装在真空仓体1的内侧壁，所述安装架转动安装在真空仓体1的上部，污染物收集板9的数量为多个且铺设在安装架的底端，所述石英晶体微天平8的数量至少为两个且均嵌装在多个污染物收集板9之间，且石英晶体微天平8、热防护罩7及分子污染物加热台6由上到下正对布置，所述石英晶体微天平8与所述QCM温度控制器10电连接，所述质谱仪2固装在真空仓体1外部且安装架水平状态下石英晶体微天平8、污染物收集板9及质谱仪2三者等高设置，所述加热辐射板5连接设置有温控仪3，通过温控仪3控制真空仓体1内的温度，真空仓体1外部连接设置有真空泵，通过真空泵控制真空仓体1内的真空度。Specific implementation method 1: Combined with Figures 1 and 2, this implementation method is described. An in-situ analysis and detection device for molecular pollutants with efficient separation and dynamic characterization includes a vacuum chamber 1, a mass spectrometer 2, a temperature controller 3, a vacuum pump, a heating radiation plate 5, a molecular pollutant heating platform 6, a heat protection cover 7, a quartz crystal microbalance 8, a pollutant collecting plate 9, a QCM temperature controller 10 and a mounting frame arranged in the vacuum chamber 1, wherein the heating radiation plate 5 is installed on the inner side wall of the vacuum chamber 1, the mounting frame is rotatably installed on the upper part of the vacuum chamber 1, the number of pollutant collecting plates 9 is multiple and laid on the bottom end of the mounting frame, and the quartz crystal microbalance 8 is arranged on the inner side wall of the vacuum chamber 1. There are at least two balances 8, which are embedded between a plurality of pollutant collecting plates 9, and the quartz crystal microbalance 8, the heat protection cover 7 and the molecular pollutant heating platform 6 are arranged opposite to each other from top to bottom, the quartz crystal microbalance 8 is electrically connected to the QCM temperature controller 10, the mass spectrometer 2 is fixedly mounted on the outside of the vacuum chamber 1 and the quartz crystal microbalance 8, the pollutant collecting plate 9 and the mass spectrometer 2 are arranged at the same height when the mounting frame is in a horizontal state, the heating radiation plate 5 is connected to a temperature controller 3, and the temperature in the vacuum chamber 1 is controlled by the temperature controller 3, and a vacuum pump is connected to the outside of the vacuum chamber 1, and the vacuum degree in the vacuum chamber 1 is controlled by the vacuum pump.
本发明提出一种模拟高温400～600K和高真空度1×10-4～1×10-5Pa空间环境条件下，对空间分子污染物进行高效分离和动态表征的原位分析测试装置。其中分子污染物包括不限于室温固化结构胶、硅油、泵油、烃类、酯类等。The present invention proposes an in-situ analysis and testing device for efficiently separating and dynamically characterizing space molecular pollutants under simulated space environment conditions of high temperature 400-600K and high vacuum 1×10 -4 ～1×10 -5 Pa. The molecular pollutants include but are not limited to room temperature curing structural adhesives, silicone oil, pump oil, hydrocarbons, esters, etc.
采用本发明的高效分离和动态表征的分子污染物原位分析检测装置，在脱气过程中，通过真空泵及加热辐射板5设置高温高真空条件，使得对污染材料脱气时所处的空间环境模拟的更加真实。The in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention is used. During the degassing process, high temperature and high vacuum conditions are set through a vacuum pump and a heating radiation plate 5, so that the simulation of the space environment in which the contaminated material is located during degassing is more realistic.
石英晶体微天平8的数量优选为两个以上，以取多个测量结果的平均值。The number of quartz crystal microbalances 8 is preferably two or more so as to obtain an average value of a plurality of measurement results.
为了在试验过程中石英晶体微天平8上的污染物沉积量尽可能的多，本发明的高效分离和动态表征的分子污染物原位分析检测装置主要采取两个措施，一是通过将安装架、热防护罩7及分子污染物加热台6由上到下正对布置，所述石英晶体微天平8与所述污染物收集板9并列布置在所述安装架上，使得在放气过程中石英晶体微天平8面对污染物源，收集污染物释放时的直接通量；二是通过设置热防护罩7，使得脱气过程中气态污染物传输过程的损失率大幅度降低，一方面通过热防护罩7对气态污染物传输路径提供了限制，另一方面在污染物源脱气过程中，热防护罩7始终保持相当高的温度，使得任何污染物都不能吸附在其表面造成传输损失。In order to deposit as much pollutants as possible on the quartz crystal microbalance 8 during the test, the in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention mainly adopts two measures. First, the mounting frame, the heat shield 7 and the molecular pollutant heating platform 6 are arranged opposite to each other from top to bottom, and the quartz crystal microbalance 8 and the pollutant collecting plate 9 are arranged side by side on the mounting frame, so that during the degassing process, the quartz crystal microbalance 8 faces the pollutant source and collects the direct flux of the pollutants when they are released; second, by setting the heat shield 7, the loss rate of the gaseous pollutant transmission process during the degassing process is greatly reduced. On the one hand, the heat shield 7 provides a restriction on the transmission path of the gaseous pollutants. On the other hand, during the degassing process of the pollutant source, the heat shield 7 always maintains a relatively high temperature, so that any pollutants cannot be adsorbed on its surface to cause transmission losses.
本发明中通过在石英晶体微天平8上增加污染物收集板9，且污染物收集板9与石英晶体微天平8保持相同的温度，但是污染物收集板9的表面积约是石英晶体微天平8的十倍，实现在石英晶体微在平梯度加热过程中释放多达十倍的污染物，从而得以加强质谱仪2中的信号，增加质谱仪2的信噪比，提高测试的灵敏度；另外，通过将安装架转动安装在真空仓体1内，使得在沉积过程结束、梯度加热开始之前，石英晶体微天平8及污染物收集板9会旋转面向质谱仪2，沉积的污染物直接面向质谱仪2释放，进一步增加质谱仪2的信噪比，使得测试的灵敏度进一步提高。In the present invention, a pollutant collecting plate 9 is added to the quartz crystal microbalance 8, and the pollutant collecting plate 9 and the quartz crystal microbalance 8 are kept at the same temperature, but the surface area of the pollutant collecting plate 9 is about ten times that of the quartz crystal microbalance 8, so that up to ten times of pollutants can be released during the flat gradient heating process of the quartz crystal microbalance, thereby strengthening the signal in the mass spectrometer 2, increasing the signal-to-noise ratio of the mass spectrometer 2, and improving the sensitivity of the test; in addition, by rotating the mounting frame in the vacuum chamber 1, the quartz crystal microbalance 8 and the pollutant collecting plate 9 will rotate to face the mass spectrometer 2 before the deposition process ends and the gradient heating begins, and the deposited pollutants are released directly facing the mass spectrometer 2, further increasing the signal-to-noise ratio of the mass spectrometer 2, so that the sensitivity of the test is further improved.
本发明的高效分离和动态表征的分子污染物原位分析检测装置，能够进行分子污染物的高效分离和原位动态检测，识别每个污染物成分种类，并定量确定每种污染物的含量来补充分析石英晶体微天平8总质量损失的测试数据，高灵敏度石英晶体微天平8原位梯度加热的质量损失数据和质谱仪2数据结合分析来更好地理解不同种类的污染物分子脱气的过程。The in-situ analysis and detection device for molecular pollutants with high efficiency separation and dynamic characterization of the present invention can perform high efficiency separation and in-situ dynamic detection of molecular pollutants, identify the type of each pollutant component, and quantitatively determine the content of each pollutant to supplement the analysis of the test data of the total mass loss of the quartz crystal microbalance 8. The mass loss data of the in-situ gradient heating of the high-sensitivity quartz crystal microbalance 8 and the data of the mass spectrometer 2 are combined for analysis to better understand the degassing process of different types of pollutant molecules.
质谱仪与真空仓体之间设置有质谱仪控制阀门17。A mass spectrometer control valve 17 is provided between the mass spectrometer and the vacuum chamber.
石英晶体微天平8与质谱仪2之间的水平距离小于10cm。如此设计，使石英晶体微天平8与质谱仪2在空间上彼此非常接近，利用两者足够近的空间使气体杂乱扩散导致的损失量忽略不计。The horizontal distance between the quartz crystal microbalance 8 and the mass spectrometer 2 is less than 10 cm. With such a design, the quartz crystal microbalance 8 and the mass spectrometer 2 are very close to each other in space, and the loss caused by the disorderly diffusion of the gas is negligible by utilizing the space close enough between the two.
分子污染物加热台6的顶端面加工有弧形通槽。如此设计，便于放置污染物源。The top surface of the molecular pollutant heating platform 6 is processed with an arc-shaped through groove. Such a design facilitates the placement of the pollutant source.
所述真空仓体1连接设置有真空计11。The vacuum chamber body 1 is connected to a vacuum gauge 11 .
所述真空泵包括机械泵12及分子泵13。如此设计，通过设置机械泵12及分子泵13，便于调节真空仓体1内的真空度，满足实验中对较高真空条件要求。机械泵12与真空仓体1之间的连接管路上以及分子泵13与真空仓体1之间的连接管路上分别设置有控制阀门。The vacuum pump includes a mechanical pump 12 and a molecular pump 13. In this design, by setting the mechanical pump 12 and the molecular pump 13, it is convenient to adjust the vacuum degree in the vacuum chamber 1 to meet the requirements of higher vacuum conditions in the experiment. Control valves are respectively provided on the connecting pipeline between the mechanical pump 12 and the vacuum chamber 1 and on the connecting pipeline between the molecular pump 13 and the vacuum chamber 1.
加热辐射板5的数量为四个，且分别贴设在真空仓体1的四个内侧壁上。如此设计，使真空仓体1内部温度更均匀。There are four heating radiation plates 5, which are respectively attached to the four inner side walls of the vacuum chamber body 1. Such a design makes the temperature inside the vacuum chamber body 1 more uniform.
所述真空仓体1内固装有固定板14，所述安装架转动安装在固定板14上。如此设计，通过固定板14实现安装架在真空仓体1内的转动安装，进而实现安装架上石英晶体微天平8及污染物收集板9的位置转动。The vacuum chamber 1 is fixed with a fixing plate 14, and the mounting frame is rotatably mounted on the fixing plate 14. With such a design, the mounting frame is rotatably mounted in the vacuum chamber 1 through the fixing plate 14, thereby realizing the position rotation of the quartz crystal microbalance 8 and the pollutant collecting plate 9 on the mounting frame.
所述真空仓体1上设置有仓门15及放气阀门16。如此设计，通过设置仓门15，便于污染物源的取放操作。The vacuum chamber body 1 is provided with a chamber door 15 and a deflation valve 16. With such a design, the chamber door 15 is provided to facilitate the operation of taking and placing the pollutant source.
具体实施方式二：结合图1及图2说明本实施方式，一种采用上述装置的分子污染物原位分析检测方法，包括如下步骤：Specific implementation method 2: This implementation method is described in conjunction with FIG. 1 and FIG. 2 . A method for in-situ analysis and detection of molecular contaminants using the above-mentioned device includes the following steps:
步骤一、将污染物源放置在分子污染物加热台6上；Step 1: placing the pollutant source on the molecular pollutant heating platform 6;
步骤二、采用真空泵对真空仓体1进行抽真空至真空度为1×10-5Pa；采用机械泵12对真空仓体1进行粗抽气至真空度为1×10-1Pa，此过程需要时间20～40min；采用分子泵13对真空仓体1进行主抽气至真空度为1×10-5Pa，此过程需要时间2～4h；Step 2: Use a vacuum pump to evacuate the vacuum chamber body 1 to a vacuum degree of 1×10 -5 Pa; use a mechanical pump 12 to roughly evacuate the vacuum chamber body 1 to a vacuum degree of 1×10 -1 Pa, and this process takes 20 to 40 minutes; use a molecular pump 13 to mainly evacuate the vacuum chamber body 1 to a vacuum degree of 1×10 -5 Pa, and this process takes 2 to 4 hours;
步骤三、将加热辐射板5加热升温，通过温控仪3控制真空仓体1内的温度达到室温至400～500K；根据所测分子污染物的不同，真空仓体1内的温度设定变动很大，所设定的温度是为了匹配污染材料在航天任务期间所经历的温度。Step 3: Heat the heating radiation plate 5 and control the temperature in the vacuum chamber 1 to reach room temperature to 400-500K through the temperature controller 3; the temperature setting in the vacuum chamber 1 varies greatly depending on the molecular pollutants being measured, and the set temperature is to match the temperature experienced by the contaminated material during the space mission.
步骤四、通过QCM温度控制器10控制石英晶体微天平8的温度为150～280K，与加热辐射板5相比保持一个相对低温状态；实验选定不同的温度，应至少有三个不同的石英晶体微天平8收集污染物，根据污染物沉积量再选定最佳沉积温度。QCM适宜低温的温度需要测试得出，多次实验选出污染物沉积量最大的温度为最佳设定温度Step 4: Use the QCM temperature controller 10 to control the temperature of the quartz crystal microbalance 8 to 150-280K, maintaining a relatively low temperature compared to the heating radiation plate 5; select different temperatures for the experiment, and at least three different quartz crystal microbalances 8 should collect pollutants, and then select the optimal deposition temperature based on the amount of pollutant deposition. The temperature suitable for QCM low temperature needs to be tested, and the temperature with the largest amount of pollutant deposition is selected as the optimal setting temperature after multiple experiments.
步骤五、开启分子污染物加热台6，使分子污染物释放，分子污染物加热台6的温度与加热辐射板5的温度相同或二者温度相差范围为0～5℃，脱气时间4～6天，污染物分子在石英晶体微天平8及污染物收集板9上沉积；Step 5: Turn on the molecular pollutant heating platform 6 to release the molecular pollutants. The temperature of the molecular pollutant heating platform 6 is the same as the temperature of the heating radiation plate 5 or the temperature difference between the two is in the range of 0 to 5° C. The degassing time is 4 to 6 days. The pollutant molecules are deposited on the quartz crystal microbalance 8 and the pollutant collecting plate 9.
步骤六、沉积过程结束后，关闭加热辐射板5及分子污染物加热台6，待温控仪3显示的温度接近室温后，关闭真空泵；真空泵关闭顺序为先关闭分子泵13，再关闭机械泵12。Step 6: After the deposition process is completed, turn off the heating radiation plate 5 and the molecular pollutant heating platform 6, and turn off the vacuum pump after the temperature displayed by the temperature controller 3 is close to room temperature; the vacuum pump is turned off in the order of first turning off the molecular pump 13 and then turning off the mechanical pump 12.
步骤七、打开放气阀门16至真空仓体1内的真空度为常压，关闭放气阀门16，取出污染物材料；进行到此步骤时QCM及污染物收集板9沉积污染物步骤完成。Step 7: Open the vent valve 16 until the vacuum degree in the vacuum chamber 1 reaches normal pressure, close the vent valve 16, and remove the pollutant material; at this step, the step of depositing pollutants on the QCM and the pollutant collecting plate 9 is completed.
步骤八、转动安装架使石英晶体微天平8及污染物收集板9面向质谱仪2；使沉积的污染物直接面向质谱仪2释放。Step 8: Rotate the mounting frame so that the quartz crystal microbalance 8 and the pollutant collecting plate 9 face the mass spectrometer 2 ; and release the deposited pollutants directly toward the mass spectrometer 2 .
步骤九、依据所选用污染物源的性质确定起始温度和终止温度后，通过QCM温度控制器10程序升温重新排放该沉积物，沉积的污染物向质谱仪2释放；程序升温：设置的程序连续地随时间线性或非线性逐渐升高。材料再释放时的起始温度和终止温度根据污染物源的性质以及材料使用时所经历的空间环境温度所确定。例如：黑色聚酰亚胺薄膜材料，长期使用温度范围73～573K，沸点高于180K,其耐高温达673K以上。QCM控制起始温度160～180K，终止温度340～360K；704硅橡胶胶黏剂，一般沸点都高过375K,高温硅油使用温度是288～588K，密度为1.070g/mL，温度系数是0.00053，25℃时的粘度44～50mpa.s，QCM控制起始温度288～390K，终止温度580～600K；J-133室温固化结构胶，固化时不需加热加压，胶层厚度达到1.6mm时仍具有高强度，耐疲劳、耐振动、耐湿热老化，使用温度193～373K，QCM控制起始温度180～200K，终止温度380～400K。QCM及污染物收集板9程序升温过程中沉积在其上的污染物受热重新排放。Step 9: After determining the starting temperature and the ending temperature according to the properties of the selected pollutant source, the QCM temperature controller 10 is used to program the temperature and re-discharge the sediment, and the deposited pollutants are released to the mass spectrometer 2; Program temperature rise: The set program continuously increases linearly or nonlinearly over time. The starting temperature and the ending temperature when the material is released again are determined according to the properties of the pollutant source and the space environment temperature experienced when the material is used. For example: the black polyimide film material has a long-term use temperature range of 73 to 573K, a boiling point higher than 180K, and a high temperature resistance of more than 673K. QCM controls the starting temperature at 160-180K and the ending temperature at 340-360K; 704 silicone rubber adhesive, generally the boiling point is higher than 375K, the high temperature silicone oil is used at 288-588K, the density is 1.070g/mL, the temperature coefficient is 0.00053, the viscosity at 25°C is 44-50mpa.s, QCM controls the starting temperature at 288-390K and the ending temperature at 580-600K; J-133 room temperature curing structural adhesive, no heating and pressurization is required during curing, the adhesive layer still has high strength when the thickness reaches 1.6mm, fatigue resistance, vibration resistance, and heat and humidity aging resistance, the use temperature is 193-373K, QCM controls the starting temperature at 180-200K and the ending temperature at 380-400K. During the program heating process of QCM and pollutant collection plate 9, the pollutants deposited on it are heated and discharged again.
步骤十、通过分析沉积物再排放过程中收集的质谱仪2数据和石英晶体微天平8数据，定量确定不同种类污染物的贡献，并在化学数据库中进行分子识别；通过分析梯度加热阶段收集的质谱仪2数据，将检测到的总质量分成不同的种类，通过质谱仪2的记录与现成的光谱数据库进行比较，定性识别释放的分子，重新释放污染物与分析过程完成。一旦识别出单个分子，就可以更容易地在MS数据中找到特定片段。Step 10: By analyzing the mass spectrometer 2 data and quartz crystal microbalance 8 data collected during the sediment re-discharge process, the contribution of different types of pollutants is quantitatively determined and molecular identification is performed in the chemical database; by analyzing the mass spectrometer 2 data collected during the gradient heating stage, the total mass detected is divided into different types, and the released molecules are qualitatively identified by comparing the records of the mass spectrometer 2 with the ready-made spectral database, and the re-release of pollutants is completed with the analysis process. Once individual molecules are identified, it is easier to find specific fragments in the MS data.
步骤九中，QCM温度控制器10程序升温速度为1～3K/min。In step nine, the QCM temperature controller 10 is programmed to increase the temperature at a rate of 1 to 3 K/min.
具体实施方式三：结合图1及图2说明本实施方式，模拟真空度为1×10-5Pa和温度为378K条件下，黑色聚酰亚胺薄膜材料脱气的有机物成分定量与定性分析。Specific implementation method three: This implementation method is described in conjunction with FIG. 1 and FIG. 2 , and quantitative and qualitative analysis of organic components of degassing of black polyimide film material is performed under simulated vacuum conditions of 1×10 −5 Pa and temperature of 378K.
步骤一、将仓门打开，将黑色聚酰亚胺薄膜材料放在分子污染物加热台上，所用的黑色卡普顿样品是一块厚度为40.48cm×30.88cm×0.00198cm的单张材料。所用的整张材料用4.02厘米宽的褶皱折叠起来，并用预先清洗过的金属夹子固定，关闭仓门；Step 1: Open the door and place the black polyimide film material on the molecular contaminant heating table. The black Kapton sample used is a single sheet of material with a thickness of 40.48cm×30.88cm×0.00198cm. The entire sheet of material used is folded with 4.02 cm wide folds and fixed with pre-cleaned metal clips, and the door is closed;
步骤二、打开机械泵阀门，使用机械泵对真空仓体进行抽真空，直至真空计显示真空度为1×10-1Pa，此过程需要时间30min；关闭机械泵阀门和机械泵，打开分子泵和分子泵阀门，直至真空计显示真空度达到1×10-5Pa,此过程需要时间4h；Step 2: Open the valve of the mechanical pump and use the mechanical pump to evacuate the vacuum chamber until the vacuum gauge shows a vacuum degree of 1×10 -1 Pa. This process takes 30 minutes. Close the valve of the mechanical pump and the mechanical pump, and open the molecular pump and the molecular pump valve until the vacuum gauge shows a vacuum degree of 1×10 -5 Pa. This process takes 4 hours.
步骤三、将加热辐射板加热升温，通过温控仪控制真空仓体的温度达到室温至378K；Step 3: Heat the heating radiation plate and control the temperature of the vacuum chamber to reach room temperature to 378K through a temperature controller;
步骤四、通过QCM温度控制器10控制温度150K，与加热辐射板相比保持一个相对低温状态；Step 4: Control the temperature to 150K by the QCM temperature controller 10 to maintain a relatively low temperature compared to the heating radiation plate;
步骤五、开启分子污染物加热台，使分子污染物释放，分子污染物加热台的温度尽量保持378K左右，脱气时间6天，污染物分子在QCM及收集板上沉积；Step 5: Turn on the molecular contaminant heating stage to release the molecular contaminants. The temperature of the molecular contaminant heating stage is kept at around 378K as much as possible. The degassing time is 6 days. The contaminant molecules are deposited on the QCM and the collection plate.
步骤六、沉积过程结束后关闭加热辐射板，关闭分子污染物加热台，待温控仪显示的温度接近室温后，关闭分子泵阀门和分子泵，再关闭机械泵阀门和机械泵；Step 6: After the deposition process is completed, turn off the heating radiation plate, turn off the molecular pollutant heating platform, and when the temperature displayed by the temperature controller is close to room temperature, turn off the molecular pump valve and the molecular pump, and then turn off the mechanical pump valve and the mechanical pump;
步骤七、打开放气阀门直至真空计显示真空度为常压，关闭放气阀门，开启仓门，取出黑色聚酰亚胺薄膜材料，关闭仓门；Step 7: Open the vent valve until the vacuum gauge shows that the vacuum degree is normal pressure, close the vent valve, open the door, take out the black polyimide film material, and close the door;
步骤八、转动安装架使石英晶体微天平及污染物收集板面向质谱仪；Step 8, rotating the mounting frame so that the quartz crystal microbalance and the contaminant collection plate face the mass spectrometer;
步骤九、通过QCM温度控制器10以180K为起始温度程序升温2K/min至350K，重新排放该沉积物然后将其输送到质谱仪；Step 9: Using the QCM temperature controller 10 to program the temperature at 2K/min from 180K to 350K, the sediment is discharged again and then transported to the mass spectrometer;
步骤十、污染物再释放的QCM数据和质谱的数据综合分析可知有二种有机污染物被重新释放:N,N-二甲基羟胺以及可能的丙烷，温度分别在190K和280K，这表明该设备成功实现了两个有机分子污染物的分离与鉴定。Step 10. Comprehensive analysis of the QCM data and mass spectrometry data of pollutant re-release shows that two organic pollutants are re-released: N,N-dimethylhydroxylamine and possible propane, at temperatures of 190K and 280K, respectively. This indicates that the equipment has successfully achieved the separation and identification of two organic molecular pollutants.
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004014981A (en) * | 2002-06-11 | 2004-01-15 | Hitachi Kokusai Electric Inc | Substrate processing equipment |
| CN101776557A (en) * | 2009-12-17 | 2010-07-14 | 中国航天科技集团公司第五研究院第五一○研究所 | Device for testing grease evaporation rate in vacuum environment |
| CN101852707A (en) * | 2010-05-20 | 2010-10-06 | 中国科学院化学研究所 | A signal amplification method of quartz crystal microbalance using polystyrene sphere as template |
| CN101876614A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | An in-situ monitoring device for air pollution from non-metallic materials on the optical surface of spacecraft |
| CN101876613A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | A method for monitoring the contamination of sensitive cryogenic surfaces of spacecraft |
| CN101876612A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | An in-situ monitoring method for outgassing pollution of non-metallic materials on the optical surface of spacecraft |
| DE102013021489A1 (en) * | 2013-12-13 | 2015-01-08 | Carl Zeiss Sms Gmbh | Contamination determination in a vacuum chamber |
| CN108717029A (en) * | 2018-05-31 | 2018-10-30 | 北京航空航天大学 | Low-temperature control system and control method for vacuum QCM |
| CN113758947A (en) * | 2021-08-11 | 2021-12-07 | 中国科学院上海光学精密机械研究所 | A test device and method for inducing molecular contamination in spacecraft cabin by total ionizing dose |
| CN114112308A (en) * | 2021-11-01 | 2022-03-01 | 中国科学院上海光学精密机械研究所 | A kind of measuring device and method for surface contamination of optical parts |
| CN114112774A (en) * | 2021-11-16 | 2022-03-01 | 哈尔滨工业大学 | Device and method for analyzing and testing adsorption and desorption performances of molecular pollutants |
| CN115698374A (en) * | 2020-05-01 | 2023-02-03 | 应用材料公司 | Quartz Crystal Microbalance Concentration Monitoring |
| CN115683291A (en) * | 2022-11-16 | 2023-02-03 | 兰州空间技术物理研究所 | Integrated type difference frequency quartz crystal microbalance |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070028669A1 (en) * | 2003-09-26 | 2007-02-08 | Brewster Barrie D | Detection of contaminants within fluid pumped by a vacuum pump |
| EP2490006A4 (en) * | 2009-10-14 | 2018-05-02 | Nippon Paper Industries Co., Ltd. | Method for measuring degree of contaminant deposition |
-
2023
- 2023-08-03 CN CN202310969383.2A patent/CN117191924B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004014981A (en) * | 2002-06-11 | 2004-01-15 | Hitachi Kokusai Electric Inc | Substrate processing equipment |
| CN101776557A (en) * | 2009-12-17 | 2010-07-14 | 中国航天科技集团公司第五研究院第五一○研究所 | Device for testing grease evaporation rate in vacuum environment |
| CN101876614A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | An in-situ monitoring device for air pollution from non-metallic materials on the optical surface of spacecraft |
| CN101876613A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | A method for monitoring the contamination of sensitive cryogenic surfaces of spacecraft |
| CN101876612A (en) * | 2009-12-17 | 2010-11-03 | 中国航天科技集团公司第五研究院第五一○研究所 | An in-situ monitoring method for outgassing pollution of non-metallic materials on the optical surface of spacecraft |
| CN101852707A (en) * | 2010-05-20 | 2010-10-06 | 中国科学院化学研究所 | A signal amplification method of quartz crystal microbalance using polystyrene sphere as template |
| DE102013021489A1 (en) * | 2013-12-13 | 2015-01-08 | Carl Zeiss Sms Gmbh | Contamination determination in a vacuum chamber |
| CN108717029A (en) * | 2018-05-31 | 2018-10-30 | 北京航空航天大学 | Low-temperature control system and control method for vacuum QCM |
| CN115698374A (en) * | 2020-05-01 | 2023-02-03 | 应用材料公司 | Quartz Crystal Microbalance Concentration Monitoring |
| CN113758947A (en) * | 2021-08-11 | 2021-12-07 | 中国科学院上海光学精密机械研究所 | A test device and method for inducing molecular contamination in spacecraft cabin by total ionizing dose |
| CN114112308A (en) * | 2021-11-01 | 2022-03-01 | 中国科学院上海光学精密机械研究所 | A kind of measuring device and method for surface contamination of optical parts |
| CN114112774A (en) * | 2021-11-16 | 2022-03-01 | 哈尔滨工业大学 | Device and method for analyzing and testing adsorption and desorption performances of molecular pollutants |
| CN115683291A (en) * | 2022-11-16 | 2023-02-03 | 兰州空间技术物理研究所 | Integrated type difference frequency quartz crystal microbalance |
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|---|---|
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