A collection device for residual liquid samples in an ultrahigh vacuum chamber

Abstract

The application discloses a kind of collection devices of residual liquid sample in ultrahigh vacuum cavity, including liquid beam current trap upper end, residual liquid sample incident port, heating element, thermistor, liquid beam current trap lower end, standard vacuum flange, gate valve, vertical degree of freedom adjusting device, liquid sample cooling tank, liquid nitrogen input port, nitrogen output port, stainless steel tube, dewar flask.The device is condensed to liquid sample cooling tank by residual liquid sample using liquid nitrogen cooling collection device through liquid beam current trap upper end face incident port, realizes the recovery of residual liquid sample in ultrahigh vacuum cavity.The application is scientific and simple in design, easy to operate, and efficient in recovery, can quickly and quickly clean up the excess liquid sample in the cavity during the experiment, minimize the influence of excess liquid sample on the vacuum degree of vacuum cavity, and can be suitable for the research of different residual liquid sample experiments in ultrahigh vacuum cavity.

Description

Technical Field

[0001] This invention relates to a device for collecting residual liquid samples in an ultra-high vacuum chamber, used for scientific research using soft X-rays for liquid jetting methods. Background Technology

[0002] Electronic structure dynamics and energy transfer are key aspects of the study of liquid-phase functional materials in molecular bonds. Soft X-ray spectrometers have been found to detect local electrons and geometric structures through the K absorption edges of biological elements such as oxygen, carbon, and nitrogen, and the L absorption edges of transition elements such as iron and cobalt. However, due to the strong absorption of soft X-rays in air, experiments in the soft X-ray photon energy range require ultra-high vacuum conditions. The challenge of conducting basic research in situ using soft X-rays has always been the development of new experimental tools that meet this requirement. In recent years, soft X-ray spectrometers based on synchrotron radiation X-ray absorption spectroscopy, X-ray scattering spectroscopy, and resonant inelastic soft X-ray scattering have been developed into multifunctional tools for studying liquid samples and solution samples under ambient temperature and pressure conditions [1]. These tools can overcome the conflict between the ultra-high vapor pressure of liquid samples and the requirement for ultra-high vacuum in experiments. For liquid sample experiments in ultra-high vacuum, there are currently two commonly used methods: the first is the thin-film window method [2], which uses a thin-film cavity made of materials such as silicon nitride to separate the liquid sample under study from the ultra-high vacuum environment. The thin-film window consists of two small copper blocks with button-sized holes in the middle, a sealing ring, and a thin film. One copper block is used to fix the sealing ring, and the other copper block has holes on both sides to connect to a stainless steel tube for transferring the sample. The other end of the stainless steel tube is connected to a thin-film pump for injecting the sample outside the vacuum chamber. The advantage of the thin-film window method is that the liquid sample is close to thermodynamic equilibrium and the temperature of the liquid sample is easy to control. However, this method cannot use electronic detection, and the amount of liquid sample is affected by the interaction between the beam and the window, so that the detected spectrum cannot truly reflect the characteristics of the body fluid sample. At the same time, the absorption of the thin film can easily lead to signal attenuation, and the rupture of the thin film can easily lead to a rapid increase in the pressure risk inside the chamber. To this end, another liquid beam jet device has been developed, which can effectively avoid the problems encountered by the thin-film window [3], and is especially suitable for research using high-intensity vacuum ultraviolet light or X-ray free electron laser. The liquid jet method utilizes a high-performance liquid chromatography (HPLC) pump to inject liquid into an ultra-high vacuum chamber through a liquid nozzle. After the liquid sample undergoes mixing, degassing, and temperature control by the HPLC pump, it is injected into the liquid nozzle. The nozzle adjusts the sample flow rate to create a stable laminar flow region within the sample chamber. In this laminar flow region, the sample interacts with X-rays, scattering a strong liquid sample signal. Compared to the thin-film window method, the liquid jet method yields a more realistic and clearer sample signal. However, unlike the thin-film window method, the liquid jet method requires the recovery of the liquid sample flowing through the laminar flow region.

[0003] References:

[0004] 【1】S.Myneni,Y.Luo,L.-A.Naslund,M.Cavalleri,L. H.Ogasawara,A.Pelmenschikov,P.Wernet,P. C. Heske, Z. Hussain, L. G. MPettersson, A. Nilsson, J. Phys.: Condens. Matter 14 (2002) L213.

[0005] 【2】J.-H.Guo,Y.Luo,A.Augustsson,J.-E.Rubensson,C. H. H. Siegbahn, and J. Nordgren, Phys. Rev. Lett. 89, 137402 (2002).

[0006] 【3】KRWilson,BSRude,J.Smith,C.Cappa,DTCo,RDSchaller,M.Larsson,T.Catalano,RJSaykally,Rev.Sci.Instrum.75(2004)725. Summary of the Invention

[0007] The purpose of this invention is to effectively recover liquid samples flowing through the X-ray zone and minimize their impact on the vacuum chamber.

[0008] To achieve the above objectives, the technical solution of this invention provides a collection device for residual liquid samples in an ultra-high vacuum chamber. The device comprises an upper end of a liquid beam trap, a residual liquid sample inlet, a heating element, a thermistor, a lower end of the liquid beam trap, a standard vacuum flange, a gate valve, a vertical degree-of-freedom adjustment device, a liquid sample cooling tank, a liquid nitrogen inlet, a nitrogen outlet, a stainless steel pipe, and a Dewar flask. The upper end of the liquid beam trap, the lower end of the liquid beam trap, the standard vacuum flange, the gate valve, the vertical degree-of-freedom adjustment device, and the liquid sample cooling tank are arranged sequentially along the flow direction of the residual liquid sample. The residual liquid sample flows into the upper end of the liquid beam trap from the residual liquid sample inlet, flows through the lower end of the liquid beam trap, the standard vacuum flange, the gate valve, and the vertical degree-of-freedom adjustment device, and then condenses into the liquid sample cooling tank.

[0009] The upper end of the liquid beam trap is a conical structure made of copper with a right-angled apex. The inlet for the residual liquid sample is located at the apex of the upper end of the liquid beam trap. A thermistor and a heating element are provided at the upper end of the liquid beam trap. The thermistor is used to monitor the temperature change at the upper end of the liquid beam trap in real time, and the heating element is used to eliminate water vapor condensed on the copper surface at the upper end of the liquid beam trap to prevent the inlet for the residual liquid sample from being blocked by supercooled droplets.

[0010] The lower end of the liquid beam trap is made of stainless steel. Its upper blade-shaped structure mates with the upper end of the liquid beam trap for installation. This blade-shaped structure achieves a vacuum seal between the lower and upper ends of the liquid beam trap while simultaneously creating a sufficient spatial gap to ensure adequate thermal decoupling between them. The lower end of the liquid beam trap is connected to the liquid sample cooling tank via a standard vacuum flange, a gate valve, and a vertical adjustment device.

[0011] The upper end of the liquid beam trap can be moved independently in the vertical direction by means of a vertical freedom direction adjustment device;

[0012] The liquid sample cooling tank is equipped with a liquid nitrogen inlet and a nitrogen outlet. The liquid nitrogen inlet is much lower in the vertical direction than the nitrogen outlet. The liquid nitrogen inlet is connected to the Dewar tank via a stainless steel connecting pipe.

[0013] Preferably, there are two thermistors, which are located on the outer side of the top surface of the liquid beam trap, and the two thermistors are respectively located at both ends of the residual liquid sample inlet.

[0014] Preferably, the heating element is located on the outer side of the upper top surface of the liquid beam trap.

[0015] Preferably, the liquid sample cooling tank is a double-walled cylindrical tank made of stainless steel.

[0016] Preferably, the upper end of the liquid beam trap, the heating element, the thermistor, the lower end of the liquid beam trap, and the liquid sample cooling tank are assembled into a single unit.

[0017] The device disclosed in this invention condenses residual liquid samples into a liquid sample cooling tank using a liquid nitrogen cooling collection device through the entrance port on the upper end face of a liquid beam trap, thereby achieving the recovery of residual liquid samples in an ultra-high vacuum chamber. This invention features a scientifically simple and scientifically designed structure, convenient operation, and high recovery efficiency. It can quickly and efficiently remove excess liquid samples from the chamber during experiments, minimizing the impact of excess liquid samples on the vacuum level of the vacuum chamber. It is applicable to research on different residual liquid samples in ultra-high vacuum chambers.

[0018] Compared with the prior art, the present invention has the following significant features:

[0019] 1. The liquid beam trap described in this invention has a simple structure, a scientific and reasonable design, and efficient and thorough recovery.

[0020] 2. The upper end face of the liquid beam trap described in this invention is a cone shape with a right angle made of copper. The cone shape of the upper end of the liquid beam trap helps to eliminate the freezing of supercooled water vapor in the ultra-high vacuum cavity during the initial adjustment period.

[0021] 3. The present invention, through the thermistor and resistance heating element installed on the upper end face of the liquid beam trap, can accurately and timely monitor and remove water vapor condensed on the copper surface of the upper end face of the liquid beam trap, ensuring that the injection port of the upper end face of the liquid beam trap is unobstructed.

[0022] 4. The upper part of the lower end of the liquid beam trap described in this invention is designed in the shape of a knife blade. This design is ingenious and scientific, which can effectively ensure the vacuum seal between the upper end and the lower end of the liquid beam trap, and also enable sufficient thermal decoupling between the two. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of a device for collecting residual liquid samples in an ultra-high vacuum chamber, as disclosed in this invention. Detailed Implementation

[0024] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0025] like Figure 1 As shown, the present invention discloses a collection device for residual liquid samples in an ultra-high vacuum chamber, comprising: an upper end of a liquid beam trap 1, a residual liquid sample inlet 2, a heating element 3, a thermistor 4, a lower end of the liquid beam trap 5, a standard vacuum flange 6, a gate valve 7, a vertical degree of freedom adjustment device 8, a liquid sample cooling tank 9, a liquid nitrogen inlet 10, a nitrogen outlet 11, a stainless steel pipe 12, and a Dewar jar 13.

[0026] Along the flow direction of the residual liquid sample, the following components are sequentially arranged: upper end 1 of the liquid beam trap, lower end 5 of the liquid beam trap, standard vacuum flange 6, gate valve 7, vertical degree of freedom adjustment device 8, and liquid sample cooling tank 9. The residual liquid sample flows into the upper end 1 of the liquid beam trap from the residual liquid sample inlet 2, flows through the lower end 5 of the liquid beam trap, standard vacuum flange 6, gate valve 7, and vertical degree of freedom adjustment device 8, and finally condenses into the liquid sample cooling tank 9.

[0027] The upper part 1 of the liquid beam trap is made of copper and has a cone shape with a right-angled apex. A residual liquid sample inlet 2 is located at the apex of the upper part 1. Small holes are located at both ends of the outer surface of the upper part 1, and thermistors 4 are installed in these holes to monitor the temperature changes of the upper part 1 in real time. A resistance heating element 3 is installed on the outer surface of the upper part 1 to promptly eliminate water vapor condensation on the copper surface of the upper part 1, preventing the residual liquid sample inlet 2 from being blocked by supercooled droplets condensing upon contact.

[0028] The lower end 5 of the liquid beam trap is made of stainless steel. The upper part of the lower end 5 is designed in a blade shape. This design helps to create a vacuum seal between the upper end 1 and the lower end 5 of the liquid beam trap when they are tightened with screws. On the other hand, it creates a relatively wide gap between the upper end 1 and the lower end 5 of the liquid beam trap, thereby ensuring sufficient thermal decoupling between them. The bottom end of the lower end 5 of the liquid beam trap is connected to the liquid sample cooling tank 9 through a standard vacuum flange 6, a gate valve 7, and a vertical degree of freedom adjustment device 8.

[0029] The standard vacuum flange 6 and gate valve 7 are used to maintain the vacuum level in the ultra-high vacuum chamber during the collection of residual liquid samples.

[0030] The liquid sample cooling tank 9 is made of stainless steel and has a double-layered cylindrical shape. The bottom of the liquid sample cooling tank 9 has a liquid nitrogen inlet 10, and the top side has a nitrogen outlet 11. A nitrogen valve is installed on the end face of the nitrogen outlet 11. The liquid nitrogen inlet 10 is connected to the Dewar flask 13 via a stainless steel connecting pipe 12. Inside the liquid sample cooling tank 9, the liquid nitrogen inlet 10 is vertically much lower than the nitrogen outlet 11; this design effectively improves the cooling effect of the liquid sample cooling tank 9.

[0031] The upper end 1 of the liquid beam trap, the heating element 3, the thermistor 4, the lower end 5 of the liquid beam trap, and the liquid sample cooling tank 9 are assembled into a whole. The upper end 1 of the liquid beam trap can be moved independently in the vertical direction by the vertical degree of freedom adjustment device 8.

[0032] The Dewar jar 13 is connected to the liquid sample cooling tank 9 via a stainless steel pipe 12 and a liquid nitrogen inlet 10, thereby enabling the condensation and collection of liquid samples.

[0033] This invention features a simple structure, scientific and rational design, and convenient operation. By utilizing a heating resistance wire on the upper surface of the beam trap, the upper entrance of the beam trap can be kept unobstructed. By adjusting the vertical degree-of-freedom adjustment device, the vertical relative position of the residual liquid entrance at the upper end of the liquid beam trap can be precisely adjusted, thereby achieving effective recovery of residual liquid samples. This invention patent essentially belongs to the field of liquid sample jetting technology in X-ray ultra-high vacuum cavities, and is particularly suitable for basic and applied research using soft X-rays under in-situ conditions for droplet sample analysis.

Claims

1. A device for collecting residual liquid samples in an ultra-high vacuum chamber, used for experimental research on different residual liquid samples in an ultra-high vacuum chamber, characterized in that, The system includes an upper liquid beam trap, a residual liquid sample inlet, a heating element, a thermistor, a lower liquid beam trap, a standard vacuum flange, a gate valve, a vertical degree-of-freedom adjustment device, a liquid sample cooling tank, a liquid nitrogen inlet, a nitrogen outlet, a stainless steel pipe, and a Dewar flask. The upper and lower liquid beam traps, standard vacuum flange, gate valve, vertical degree-of-freedom adjustment device, and liquid sample cooling tank are arranged sequentially along the flow direction of the residual liquid sample. The residual liquid sample flows into the upper surface of the liquid beam trap from the residual liquid sample inlet, passes through the lower liquid beam trap, standard vacuum flange, gate valve, and vertical degree-of-freedom adjustment device, and then condenses in the liquid sample cooling tank. The upper end of the liquid beam trap is a conical structure made of copper with a right-angled apex. The residual liquid sample inlet is located at the apex of the upper end of the liquid beam trap. A thermistor and a heating element are provided at the upper end of the liquid beam trap. The thermistor is used to monitor the temperature change at the upper end of the liquid beam trap in real time. The heating element is used to eliminate water vapor condensed on the copper surface at the upper end of the liquid beam trap to prevent the residual liquid sample inlet from being blocked by supercooled droplets. There are two thermistors, which are located on the outer side of the top surface of the upper end of the liquid beam trap. The two thermistors are located at both ends of the residual liquid sample inlet. The lower end of the liquid beam trap is made of stainless steel. Its upper blade-shaped structure mates with the upper end of the liquid beam trap for installation. This blade-shaped structure achieves a vacuum seal between the lower and upper ends of the liquid beam trap while simultaneously creating a sufficient spatial gap to ensure adequate thermal decoupling between them. The lower end of the liquid beam trap is connected to the liquid sample cooling tank via a standard vacuum flange, a gate valve, and a vertical adjustment device. The upper end of the liquid beam trap can be moved independently in the vertical direction by means of a vertical freedom direction adjustment device; The liquid sample cooling tank is equipped with a liquid nitrogen inlet and a nitrogen outlet. The liquid nitrogen inlet is much lower in the vertical direction than the nitrogen outlet. The liquid nitrogen inlet is connected to the Dewar tank via a stainless steel connecting pipe.

2. The device for collecting residual liquid samples in an ultra-high vacuum chamber as described in claim 1, characterized in that, The heating element is located on the outer side of the top surface of the liquid beam trap.

3. The device for collecting residual liquid samples in an ultra-high vacuum chamber as described in claim 1, characterized in that, The liquid sample cooling tank is a double-walled cylindrical tank made of stainless steel.

4. The device for collecting residual liquid samples in an ultra-high vacuum chamber as described in claim 1, characterized in that, The upper end of the liquid beam trap, the heating element, the thermistor, the lower end of the liquid beam trap, and the liquid sample cooling tank are assembled into a single unit.

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