JPH03504894A - optical vacuum valve - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] optical vacuum valve Technical field TECHNICAL FIELD The present invention relates to optical research equipment, and more particularly to an optical vacuum valve.

Background technology Optical vacuum valves for studying the reactions of gases on the surfaces of hard materials are known ( L., L., “Infrared Spectrum of Absorbed Molecules J Page 45, Mil. Publisher, Moscow, 1969), this known optical vacuum valve has an optical window an air-tight chamber having an opening between which the retainer holds the It is arranged so that the measurement of the sample can be carried out on the path of the light beam incident from the light source. This known optical vacuum valve furthermore has a function for heating the sample and monitoring the temperature. system and an outlet that connects the valve to a vacuum system. This vacuum system is used to pull a vacuum on this valve. The vacuum system used in the valve is It is also an outlet for filling the mixture. In order to heat the sample, the latter That is, a gaseous mixture is placed in a position that blocks the incident light beam, and this gaseous mixture This gaseous mixture is introduced into the spectrometer's beam in order to position the spectrum of Can be put in. The advantage of this valve is that it can capture both the sample spectrum and the gas phase spectrum. The purpose is to provide favorable conditions for positioning. However, this trial The sample transfer system securely fixes the sample in the path of the light beam and sets it with high reproducibility. can't do something.

Additionally, the valve can perform spectral positioning of the sample at room temperature. Only in the case of The spectral emission at temperatures above room temperature is The optical part of the camera is heated directly and the position of the optical part is precisely fixed. (Applications of Surface Science, Volume 8, Page 11, 1980, N.H. C (Amsterdam), Earl Bowman, and I, L.

See “Study of in-situ Fourier transform infrared spectroscopy” by C., Frerichs. (see). A valve endowed with this construction is made of steel with an optical window held in the flange. The airtight optical chamber is rigidly attached to the lid, has an open cylindrical shape, and has an internal The sample holder of the crystal source is fitted with a heating device on the outside and a cooling window on the outside. a casing, and this outer casing is configured to admit a coolant, e.g. water. It has pipes for filling and draining. Sample position inside the valve The position of the sample is fixed, and in order to fix the position of this sample, the positioning of the gas phase spectrum is This prevents measurements from being performed independently of the sample spectrum. For gas phase absorption The fundamental thing to compensate for is the independent positioning of the sample being analyzed. It is carried out at the same pressure and temperature, but without a sample.

This lengthens the experimental manifold and reduces the precision of the results. Furthermore, this If a chemical reaction within the system generates reaction products in the gas phase, It is not possible to compensate for gas phase absorption and its composition analysis. the Alternatively, a sample holder in a fixed position can perform the analysis within a single experiment. There is only one sample. In other words, it is a series of trials. This means that each experiment must be performed independently to analyze the There is. A valve of the above construction can only be used for spectral positioning at temperatures above room temperature. You can do this. The cooling of the window in this structure is related to the cooling of the walls of the optical chamber. Therefore, when performing analysis at temperatures above room temperature, a temperature gradient is created in the gas phase. distribution occurs. In the latter case, i.e. when a temperature gradient occurs in the gas phase, The conventional valve obtains quantitative information about the absorption and catalytic reactions at the surface of the sample. It is not suitable for practical purposes. The reason is the thermodynamics and kinetics of chemical reactions. In order to measure physical properties, it is necessary to equalize the temperature gradients between the sample and the gas phase. It is from.

Disclosure of invention The present invention relates to the structure of a holder for a sample to be analyzed and the structure of a cooling device for an optical window of a chamber. The structure allows the sample to be moved relative to the spectrometer over the entire measurement temperature range. If possible, the structure should be designed to prevent the occurrence of gas phase gradients. Therefore, in order to study the thermodynamic and kinetic properties of the reaction between the gas phase and solid materials, Based on the problems to provide an optical vacuum valve that can provide favorable conditions. are doing.

This problem is solved by using airtight chambers with optical windows each held between flanges. one or more samples on the path of the light flux incident from the light source, which is equipped with a heating device and a heating device. an optical vacuum valve having a holder for accommodating a material; One flange of the has a groove which leads to the coolant supply system via a tube. In addition, the chamber is provided with an airtight casing, which casing allows the tube to a tube for introducing a heat transfer agent, the tube surrounding the vicinity of the chamber to be analyzed; and a tube for discharging the heat transfer agent, and a sample holder is provided in the chamber; The sample is moved relative to the light beam and fixed in the path of the light beam in this sample holder. The optical system is equipped with a mechanism for Eliminated by vacuum valve.

The sample holder is equipped with an additional fixing device, and with this additional fixing device several Placing the samples at the same time and fixing each sample alternately with respect to the path of the light beam is a convenient thing.

The proposed invention is capable of analyzing several samples within one experiment; Analyzing several samples within a single experiment is a convenient way to measure thermodynamic properties. To improve measurement accuracy by removing relative errors in temperature and pressure measurements when Furthermore, the time required for the experiment can be shortened. In addition, the surface Chemical treatments on compounds can be monitored and, along with this, gas phase It also becomes possible to monitor chemical treatments for Extends the working temperature range and Measurement of thermodynamic properties of chemical reactions by preventing the development of temperature gradients in the gas phase Accuracy can be improved.

Brief description of the drawing Fig. 1 is an overall view of the optical vacuum valve according to the present invention, and Fig. 2 is taken along the line ■-H in Fig. 1. FIG.

BEST MODE FOR CARRYING OUT THE INVENTION The invention will now be described in further detail with reference to the embodiments of the invention in connection with the attached drawings. explain.

According to the invention, the optical vacuum valve comprises a gas-tight chamber 1 (FIG. 1). The chamber has an optical window 2, which is held between flanges 3.4. Airtight The chamber 1 is connected to a vacuum device (not shown) using a flange 5. . One flange of the housing 2, for example flange 3, has an annular groove 6, which groove 6 Via a pipe 7 it is connected to a device for supplying a coolant, for example water.

The lid 8 of the chamber 1 is connected to a sample holder 10 via a bellows 9. The lower part of the holder 10 is connected to a sample fixing device 11 in the form of a cylindrical hole. sample The cooling device is represented by two tubes 12, which are connected to the sample holder 1. A coolant inlet and a coolant outlet of 0, which are separated by a partition member 13. There is. In addition, the lower part of the sample holder 10 is equipped with a heating device 14 (Fig. 2) and a temperature pick. It houses an up device 15.

In the vicinity of the sample fixation device, the chamber 1 is surrounded by a gas-tight casing 16. The casing 16 has pipes 17 for inflowing and discharging the heat transfer agent.

The outer wall of the chamber 1 is located inside the casing 16 and is heated inside the casing 16. It surrounds a transducer 18 for measuring and monitoring the temperature. casing 16, a part near the sample position is a pickup member 1 for detecting the temperature of the sample. 9, which pick-up member 19 is moved into the chamber by means of the flange 20. It is connected to the main body of 1. In addition, a compensator 21 is provided in the chamber 1, which The compensator 21 compensates for changes in volume when the sample holder 10 is moving. Ru.

The positioning of the sample is performed as follows with the aid of the proposed optical vacuum valve.

A compressed disk-shaped sample is placed inside a device 11 that fixes a sample holder 1o. The latter, that is, the fixing device 11 of the sample holder, is located inside the chamber 1. installed and with the help of the lid 8, this cham held in the chamber. Chamber 1 is evacuated using a vacuum device. window 2 For cooling, water circulating through the outer thermostat enters the groove 6 of the flange 3. is supplied to the interior of the sample holder 10, and then heated internally in the lower part of the sample holder 10. Device 14 begins heating. At the same time, heated air flows through the tube 17. , into the casing 16. In this state, the sample is heated and vacuum-treated. This heating and vacuum treatment is extremely important to clean the surface of this sample. Yes, the temperature of this process was measured using a temperature pick-up device 15.18.19. and monitored. After processing of the preceding sample is completed, chamber 1 and case are The temperature inside the thing 16 is brought to the required temperature and the sample is exposed to light with the aid of the mechanism 9. are arranged alternately on the path of the bundle and the spectral positioning of this sample is performed. Ru.

When no sample is inserted and the fixing device 11 is placed on the path of the light beam, the ratio is A reference sample is positioned for comparison. Thereafter, the gaseous reaction mixture is From the vacuum device, the sample and gaseous reaction mixture are fed through tube 5 and Positioning of the torque is done using the method already described. The volume of chamber l is In order to maintain a constant value, the compensator 21 is used when the sample holder 10 is moving. used.

If measurements are to be made at room temperature, liquid or vaporized nitrogen coolant is supplied to the case through tube 17. It is necessary to feed it into the thing 16 and then into the lower part of the sample holder 10.

The temperature inside the chamber 1 and the casing 16 is maintained constant and a temperature pick-up is used. measured and monitored using tap equipment 15.18.19.

In this way, the sample holder 10 can be passed through the moving mechanism 9 and held on the M8 without being rigid. It is possible to measure both the spectrum of the solid sample and the spectrum of the gas phase. , Furthermore, several samples can be analyzed in one experiment.

Measurement of dynamic thermal properties by absorption method when there are several samples is based on gas pressure and temperature. Overall, relative errors in measurements are eliminated, resulting in improved accuracy. Furthermore, all sample surfaces are thermally vacuum cleaned at the same time, reducing the time required for the experiment. Can be shortened. Further, a sample cooling device is built into the sample holder 10. Therefore, the range of measurement temperatures is expanded to the lower temperature side (to 196 degrees below zero Celsius). Keishi [6] evacuates the area near the sample in chamber 1, and this reduced pressure causes the gas to evacuate. This makes it possible to prevent temperature gradients from occurring in the gas phase. Expanding the temperature range to be measured Large and chemical reactions that prevent the occurrence of temperature gradients in the gas phase and the spectrum of the gas phase The ability to follow the progress of the experiment provides benefits when conducting experiments. This increases the amount of information that can be obtained and improves the accuracy of kinematic parameters.

Industrial applicability The present invention can be used for spectroscopic analysis of solid substances, and even in contact with gases. , i.e. used for research methods involving absorption, heterogeneous catalysis, corrosion, and surface modification. It is also possible to do so.

count international search report -111111-mpCT15u89100076

Claims (2)

[Claims] 1. air having an optical window (2) held between flanges (3, 4) respectively; Light incident from a light source in which a dense chamber (1) and a heating device (14) are provided. an optical vacuum valve comprising a holder (10) for containing one or more samples on the path of the bundle; one flange (3) of each optical window (2) is connected to the coolant supply via a tube (7). The chamber (1) has a groove (6) connected to the supply system, and the chamber (1) has a groove (6) connected to the supply system. A tube (17) for inflowing and discharging the heat transfer agent surrounding the chamber (1) during application. ) and a gas-tight casing (16) for moving the sample relative to the light beam. and a mechanism (9) for fixing the sample on the path of the light beam. An optical vacuum valve comprising a holder (10) and a sample cooling device. 2. A sample holder (10) is used for placing several samples at the same time and for holding each sample. having additional fixing devices (11) for fixing alternately on the path of the light beam; The optical vacuum valve according to claim 1, characterized in that: