Detection equipment and method for laser confocal Raman spectrometer

Abstract

The invention discloses detection equipment and method for a laser confocal Raman spectrometer in the technical field of Raman spectrometers. The detection equipment comprises a detector, a sample chamber and a refrigerator which are sequentially arranged from left to right, a light path system for detecting a to-be-detected sample in the sample chamber is arranged in the detector; a cooling pipe is communicated between the sample chamber and the refrigerator, a protective pipe and a connecting pipe are sequentially arranged outside the cooling pipe, a filling layer is arranged between the connecting pipe and the protective pipe, the ends, away from the sample chamber, of the cooling pipe and the protective pipe are both communicated with the refrigerator, and a plurality of movable dust is arranged in the protective pipe; a damping mechanism used for absorbing vibration generated in the working process of the refrigerator is arranged between the refrigerator and the cooling pipe, a pressure sensor is arranged at the bottom of the damping mechanism, and the pressure sensor is electrically connected with a control panel. The control panel controls the working condition of the detector based on the real-time pressure data measured by the pressure sensor, controls the vibration generated by the refrigerator, and guarantees the precision and reliability of the test data of the detector.

Description

Technical Field

[0001] The invention belongs to the technical field of Raman spectrometers, and in particular relates to detection equipment and a method for a laser confocal Raman spectrometer. Background Art

[0002] Laser confocal Raman spectrometer is a scientific instrument used in the field of materials science. It uses Raman scattering that occurs when laser irradiates the surface of the sample body, and generates a Raman spectrum by changing the energy of Raman scattered photons to provide information about the structure, chemical composition, crystal structure, etc. of the sample molecules. It can be used to analyze different types of samples such as solids, liquids, and gases, and is widely used in materials physics, petrochemicals, life sciences and other fields.

[0003] In recent years, with the emergence of new electromagnetic functional materials such as high-temperature superconductors and topological insulators, the study of material properties at different temperatures, especially low temperatures, has become a hot topic, and variable-temperature laser microscopy confocal Raman technology has become one of the best methods to study the structural properties of materials at different temperatures.

[0004] Existing laser confocal Raman spectrometers with variable temperature function usually use cryogenic liquids (liquid nitrogen, liquid helium, etc.) as cooling sources. Since cryogenic liquids have volatilization problems and are expensive, refrigerators are usually used for cooling. However, the vibrations generated by the refrigerator during operation will be transmitted to the sample, affecting the measurement accuracy of the laser confocal Raman spectrometer. Summary of the invention

[0005] The purpose of the present invention is to provide a detection device and method for a laser confocal Raman spectrometer, which is convenient for controlling the vibration generated by a refrigerator and ensuring the accuracy and reliability of the test data of the detector.

[0006] In order to achieve the above object, the technical solution of the present invention is as follows:

[0007] A detection device of a laser confocal Raman spectrometer comprises a detector, a sample chamber and a refrigerator which are arranged in sequence from left to right;

[0008] The detector is provided with an optical path system for detecting the sample to be detected in the sample chamber; a cooling pipe is connected between the sample chamber and the refrigerator, a protective pipe and a connecting pipe are arranged outside the cooling pipe in sequence, and a filling layer is arranged between the connecting pipe and the protective pipe, and the ends of the cooling pipe and the protective pipe away from the sample chamber are both connected to the refrigerator, and a plurality of adsorbent dusts are arranged in the protective pipe;

[0009] A shock-absorbing mechanism is provided between the refrigerator and the cooling pipe for absorbing the vibration generated during the operation of the refrigerator. A pressure sensor is provided on the side of the shock-absorbing mechanism away from the refrigerator. The pressure sensor is electrically connected to a control panel. The control panel controls the working condition of the detector based on real-time pressure data measured by the pressure sensor.

[0010] The following beneficial effects are achieved by adopting the above scheme:

[0011] During the operation of the refrigerator, a buffer is formed by the shock-absorbing mechanism to weaken the vibration transmitted by the refrigerator to the cooling pipe. At the same time, the vibration of the refrigerator after attenuation is tested by the pressure sensor at the shock-absorbing mechanism to control the sampling time of the Raman spectrum detection during the operation of the detector, so as to ensure the accuracy and reliability of the test data of the detector.

[0012] At the same time, the protection and isolation formed by the protective tube and the connecting tube can reduce the heat exchange between the cooling tube and the outside world, and the gas flow in the transmission process through the protective tube drives some dust to move on the tube wall. According to the restraint of the flue gas flow wall effect, the dust can easily form a shell on the inner wall of the protective tube to protect the protective tube. When the protective tube is damaged or gaps appear at the connection of the refrigeration tube, the gaps are bonded and blocked by dust to reduce the interference of outside air on the heat exchange of the refrigeration tube.

[0013] Furthermore, a sample stage for placing samples to be tested is fixedly connected in the sample chamber, and a cooling tube is wrapped around the sample stage; an observation port is also opened at the bottom of the sample chamber, the observation port is located above the sample stage, and the observation port is filled with a glass layer for support.

[0014] Beneficial effect: The cooling tube is wound around the sample table so that the cooling tube can cool down the sample chamber and provide a placement space for the sample to be tested, so that the detector can test the sample to be tested.

[0015] Furthermore, the shock absorbing mechanism includes a deformable body and a plurality of buffer blocks. The deformable body is located between adjacent buffer blocks. A plurality of buffer channels are opened in the deformable body. A pressure rod and a plurality of support rods are provided in the buffer channels. The pressure rod is fixedly connected to the refrigerator. The length of the support rod decreases from the inside to the outside, and the distance between the support rod and the pressure rod increases from the inside to the outside. The pressure sensor is located at the end of the support rod away from the refrigerator.

[0016] Beneficial effect: The buffer block is supported by a number of support rods. During the operation of the refrigerator, the support rod is gradually pressurized by the pressure rod, and the deformation of the support rod provides a buffer space to reduce the vibration of the refrigerator. At the same time, during the gradual downward movement of the pressure rod, the support effect of the support rod is improved through the support of the support rods in multiple buffer channels. At the same time, vibration is absorbed through the deformation bodies between the multiple buffer channels to reduce the external vibration generated during the operation of the refrigerator from being transmitted to the cooling pipe.

[0017] Furthermore, the connecting pipe is a corrugated pipe.

[0018] Beneficial effect: By connecting the sample chamber and the refrigerator through the bellows, the external vibration generated during the operation of the refrigerator can be effectively reduced and directly transmitted to the sample chamber through the cooling pipe, so as to ensure the accuracy and reliability of the test data of the detector.

[0019] Furthermore, the cooling pipe is a multi-section pipe.

[0020] Beneficial effect: The cooling pipe is divided into multiple sections to reduce the vibration generated during the operation of the refrigerator and directly transmit the vibration to the sample chamber through the complete cooling pipe, thereby ensuring the accuracy and reliability of the test data of the detector.

[0021] Furthermore, one end of the cooling tube close to the sample chamber is connected to a Tesla valve-type tube.

[0022] Beneficial effect: The Tesla valve tube is used to slow down the gas flow rate of the cold air when the cooling tube enters the sample chamber, thereby extending the heat exchange time between the cooling tube and the sample chamber, so that the sample chamber can be fully cooled.

[0023] Furthermore, the protection tube is also located on the inner wall of the sample chamber, and the protection tube is ring-shaped.

[0024] Beneficial effect: The inner wall of the sample chamber is protected by the annular protective tube, which plays a role in isolating the sample chamber from the outside world, thereby reducing the heat exchange between the outside air and the inside of the sample chamber, thereby facilitating the maintenance of a stable temperature in the sample chamber.

[0025] Furthermore, temperature sensors are respectively provided in the sample chamber and the protection tube, and the temperature sensors are used to detect the temperature data in the sample chamber and the protection tube in real time, and send the temperature data to the control panel;

[0026] The control panel compares the temperature data in the sample chamber and the protection tube for consistency. If the temperature data in the sample chamber and the protection tube are consistent, a maintenance instruction is sent to the refrigerator and the detector. If the temperature data in the sample chamber and the protection tube are inconsistent, a stop instruction is sent to the refrigerator and the detector.

[0027] Beneficial effect: By stopping the sending of instructions and maintaining the sending of instructions, the erroneous execution of the connecting pipe when it is damaged is reduced, thereby ensuring the test accuracy and reliability of the laser confocal Raman spectrometer.

[0028] Further, a detection method of a laser confocal Raman spectrometer, according to the detection device method of the laser confocal Raman spectrometer, comprises the following steps: step 1, installing the detector, the sample chamber and the refrigerator on the ground, so that the sample chamber is located below the eyepiece of the optical path system in the detector, and installing a base between the ground and the detector, the sample chamber and the refrigerator for support;

[0029] Step 2, connecting the sample chamber and the refrigerator in the order of the cooling tube, the protection tube and the connecting tube from inside to outside, and arranging a shock absorbing mechanism between the refrigerator and the cooling tube, and making the number of supporting rods of the shock absorbing mechanism decrease in sequence from inside to outside;

[0030] Step 3: The control panel controls the operation of the detector through the measurement of the pressure sensor and the temperature sensor.

[0031] Beneficial effect: The base supports the detector, the sample chamber and the refrigerator, provides a buffer and adjusts the support height of the detector, the sample chamber and the refrigerator to facilitate detection.

[0032] The support of the shock absorbing mechanism can reduce the vibration transmission during the operation of the refrigerator. At the same time, the number of support rods is changed to facilitate the shock absorbing mechanism to perform deformation support during the support process, gradually provide a supporting effect, and make the refrigerator more stable.

[0033] The control panel is used to reduce the interference of the refrigerator to the detector during operation, so as to ensure the test accuracy and reliability of the laser confocal Raman spectrometer.

[0034] Furthermore, in step 1 and step 2, the inner wall of the sample chamber and the inner wall of the protective tube are polished, and the sample chamber is vacuumed.

[0035] Beneficial effect: The inner wall of the light ring and the vacuum environment are used to reduce the radiation heat leakage changes caused by the air flow in the sample room, so as to ensure the test accuracy and reliability of the laser confocal Raman spectrometer. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 It is a cross-sectional view of a detector of a detection device of a laser confocal Raman spectrometer according to an embodiment of the present invention.

[0037] Figure 2 for Figure 1 Schematic diagram of the sample chamber connections.

[0038] Figure 3 for Figure 2 sectional view of .

[0039] Figure 4 for Figure 2 Partial cross-sectional view of the cooling pipe. DETAILED DESCRIPTION

[0040] The following is further described in detail through specific implementation methods:

[0041] The figure marks in the drawings of the specification include: detector 1, base 10, CCD sensor 11, grating 12, focusing lens 13, light source 14, beam expander 15, reflector 16, filter 17, eyepiece 18, sample chamber 2, observation port 21, sample stage 22, temperature sensor 23, cooling tube 3, connecting tube 31, protective tube 32, filling layer 33, Tesla valve type tube 34, shock absorbing mechanism 4, buffer block 41, pressure rod 42, support rod 43, pressure sensor 44, refrigerator 5.

[0042] Example 1

[0043] The embodiment is basically as shown in the attached Figures 1 to 4 As shown: a detection device of a laser confocal Raman spectrometer, comprising a detector 1, a sample chamber 2 and a refrigerator 5 arranged in sequence from left to right; an optical path system for detecting a sample to be detected in the sample chamber 2 is arranged in the detector 1; the optical path system comprises a light source 14, a beam expander 15, a filter 17 and an eyepiece 18 arranged in sequence along the light transmission direction, a plurality of reflectors 16 for converting directions are arranged between the eyepiece 18 and the light source 14, and a CCDCCD sensor 11 is also included, and a focusing lens 13 and a grating 12 are arranged between the CCDCCD sensor 11 and the eyepiece 18 for connection;

[0044] A cooling pipe 3 is connected between the sample chamber 2 and the refrigerator 5. A sample table 22 for placing the sample to be tested is welded in the sample chamber 2, and the cooling pipe 3 is wrapped around the sample table 22. An observation port 21 is also opened at the bottom of the sample chamber 2. The observation port 21 is located above the sample table 22, and the observation port 21 is filled with a glass layer for support. A protective tube 32 and a connecting tube 31 are arranged in sequence outside the cooling tube 3. The connecting tube 31 is a corrugated tube. The cooling tube 3 is a multi-section pipe, and a filling layer 33 is arranged between the connecting tube 31 and the protective tube 32. The filling layer 33 includes but is not limited to foam. In addition to supporting the sample stage 22, the filling layer 33 further reduces vibration interference. The cooling tube 3 and the protective tube 32 are connected to the refrigerator 5 at one end away from the sample chamber 2. Some movable dust is arranged in the protective tube 32. The protective tube 32 is also located on the inner wall of the sample chamber 2, and the protective tube 32 is annular. The cooling tube 3 and the protective tube 32 constitute a three-pronged tube. The end of the cooling tube 3 close to the sample chamber 2 is connected to a Tesla valve-type tube 34. The material of the cooling tube 3 is pure copper.

[0045] For example, pure copper has a good thermal conductivity, so as to facilitate the rapid transfer of cold air between the sample chamber 2 and the refrigerator 5 .

[0046] A shock absorbing mechanism 4 for absorbing the vibration generated during the operation of the refrigerator 5 is provided between the refrigerator 5 and the cooling tube 3. The shock absorbing mechanism 4 includes a deformable body and a plurality of buffer blocks 41. The deformable body is located between adjacent buffer blocks 41. A plurality of buffer channels are opened in the deformable body. A pressure rod 42 and a plurality of support rods 43 are provided in the buffer channels. The pressure rod 42 is fixedly connected to the refrigerator 5. The length of the support rod 43 decreases from the inside to the outside, and the distance between the support rod 43 and the pressure rod 42 increases from the inside to the outside. A pressure sensor 44 is also fixedly connected to the buffer block 41. The pressure sensor 44 is located at one end of the support rod 43 away from the refrigerator 5. The pressure sensor 44 is electrically connected to the control panel.

[0047] The pressure sensor 44 is used to measure the pressure data applied by the shock absorbing mechanism 4 in real time, and send the pressure data to the control panel. The control panel is used to calculate the difference between the pressure data before and after the current time, and compare the difference with the set standard value. If the difference is greater than the standard value, an interval work instruction is sent to the detector 1, and the control panel will record the pressure data of the current time and add an abnormal mark. If the difference is less than the standard value, a detection pass instruction is sent to the detector 1, and the control panel records the pressure data of the current time.

[0048] Temperature sensors 23 are respectively provided in the sample chamber 2 and the protective tube 32, and the temperature sensors 23 are used to detect the temperature data in the sample chamber 2 and the protective tube 32 in real time, and send the temperature data to the control panel; the control panel compares the temperature data in the sample chamber 2 and the protective tube 32 for consistency, and if the temperature data in the sample chamber 2 and the protective tube 32 are consistent, a maintenance instruction is sent to the refrigerator 5 and the detector 1; if the temperature data in the sample chamber 2 and the protective tube 32 are inconsistent, a stop instruction is sent to the refrigerator 5 and the detector 1.

[0049] The specific implementation process is as follows: during the operation of the refrigerator 5, the vibration of the refrigerator 5 is transmitted to the cooling tube 3 through the shock absorbing mechanism 4, and the support rod 43 is gradually pressurized by the pressure rod 42, and a buffer space is provided by the deformation of the support rod 43. During the contact between the pressure rod 42 and multiple support rods 43, multiple buffers are formed by the support rods 43 in different buffer channels to reduce the vibration of the refrigerator 5; at the same time, during the gradual downward movement of the pressure rod 42, the support effect of the support rod is improved by the support of the support rods 43 in multiple buffer channels, and at the same time, vibration absorption is performed by the deformation body between the multiple buffer channels to reduce the external vibration generated during the operation of the refrigerator 5 from being transmitted to the cooling tube 3.

[0050] At the same time, the pressure sensor 44 measures the pressure applied by the shock absorbing mechanism 4, and tests the vibration of the refrigerator 5 after it is reduced through the pressure sensor 44, so as to control the sampling time of the Raman spectrum detection process during the operation of the detector 1, reduce the light movement changes caused by the vibration of the optical path system in the detector 1, and ensure the accuracy and reliability of the test data of the detector 1.

[0051] At the same time, the protection and isolation formed by the protective tube 32 and the connecting tube 31 can reduce the heat exchange between the cooling tube 3 and the outside world, and the gas flow in the protective tube 32 during the transmission process drives some dust to move on the tube wall. According to the restraint of the flue gas flow wall effect, the dust can easily form a shell on the inner wall of the protective tube 32 to protect the protective tube 32. When the protective tube 32 is damaged or a gap appears at the connection of the refrigeration tube, the gap is bonded and blocked by the dust to reduce the interference of the outside air on the heat exchange of the refrigeration tube; and the temperature data in the sample chamber 2 and the protective tube 32 are compared for consistency through the control panel to reduce the erroneous execution of the connecting tube 31 when it is damaged, thereby ensuring the test accuracy and reliability of the laser confocal Raman spectrometer.

[0052] Example 2

[0053] The difference from the above embodiment is that a detection method of a laser confocal Raman spectrometer comprises the following steps:

[0054] Step 1: Install the detector 1, sample chamber 2 and refrigerator 5 on the ground, so that the sample chamber 2 is located below the eyepiece 18 of the optical path system in the detector 1, and install a base 10 between the ground and the detector 1, sample chamber 2 and refrigerator 5 for support; first polish the inner wall of the sample chamber 2 and the inner wall of the protective tube 32, and then support them with the base 10 to provide a buffer while adjusting the support height of the detector 1, sample chamber 2 and refrigerator 5 to facilitate detection.

[0055] Step 2: Connect the sample chamber 2 and the refrigerator 5 in the order of the cooling tube 3, the protective tube 32 and the connecting tube 31 from the inside to the outside, and arrange the shock absorbing mechanism 4 between the refrigerator 5 and the cooling tube 3, and make the number of the supporting rods 43 of the shock absorbing mechanism 4 decrease in sequence from the inside to the outside, and evacuate the sample chamber 2; through the support of the shock absorbing mechanism 4, the vibration transmission of the refrigerator 5 during operation is reduced, and at the same time, the number of the supporting rods 43 is changed to facilitate the deformation support of the shock absorbing mechanism 4 during the supporting process.

[0056] Step 3: The control panel controls the operation of the detector 1 through the measurement of the pressure sensor 44 and the temperature sensor 23, so as to reduce the interference of the refrigerator 5 on the detector 1 during operation and ensure the test accuracy and reliability of the laser confocal Raman spectrometer.

[0057] The above is only an embodiment of the present invention, and the common knowledge such as the known specific structure and / or characteristics in the scheme is not described in detail here. It should be pointed out that for those skilled in the art, several deformations and improvements can be made without departing from the structure of the present invention, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. A detection device for a laser confocal Raman spectrometer, characterized in that: It includes a detector, a sample chamber and a refrigerator which are arranged from left to right; The detector is provided with an optical path system for detecting the sample to be detected in the sample chamber; a cooling pipe is connected between the sample chamber and the refrigerator, a protective pipe and a connecting pipe are arranged outside the cooling pipe in sequence, and a filling layer is arranged between the connecting pipe and the protective pipe, and the ends of the cooling pipe and the protective pipe away from the sample chamber are both connected to the refrigerator, and a plurality of adsorbent dusts are arranged in the protective pipe; A shock-absorbing mechanism is provided between the refrigerator and the cooling pipe for absorbing the vibration generated during the operation of the refrigerator. A pressure sensor is provided on the side of the shock-absorbing mechanism away from the refrigerator. The pressure sensor is electrically connected to a control panel. The control panel controls the working condition of the detector based on real-time pressure data measured by the pressure sensor.

2. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: A sample stage for placing the sample to be tested is fixedly connected in the sample chamber, and a cooling tube is wrapped around the sample stage; an observation port is also opened at the bottom of the sample chamber, the observation port is located above the sample stage, and the observation port is filled with a glass layer for support.

3. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: The shock absorbing mechanism includes a deformable body and a plurality of buffer blocks. The deformable body is located between adjacent buffer blocks. A plurality of buffer channels are opened in the deformable body. A pressure rod and a plurality of support rods are provided in the buffer channels. The pressure rod is fixedly connected to the refrigerator. The length of the support rod decreases from the inside to the outside, and the distance between the support rod and the pressure rod increases from the inside to the outside. The pressure sensor is located at the end of the support rod away from the refrigerator.

4. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: The connecting pipe is a bellows.

5. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: The cooling pipe is a multi-section pipe.

6. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: One end of the cooling tube close to the sample chamber is connected with a Tesla valve-type tube.

7. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: The protection tube is also located on the inner wall of the sample chamber, and the protection tube is annular.

8. The detection device of laser confocal Raman spectrometer according to claim 1, characterized in that: The sample chamber and the protection tube are respectively provided with temperature sensors, which are used to detect the temperature data in the sample chamber and the protection tube in real time and send the temperature data to the control panel; The control panel compares the temperature data in the sample chamber and the protection tube for consistency. If the temperature data in the sample chamber and the protection tube are consistent, a maintenance instruction is sent to the refrigerator and the detector. If the temperature data in the sample chamber and the protection tube are inconsistent, a stop instruction is sent to the refrigerator and the detector.

9. A detection method of laser confocal Raman spectrometer, characterized in that: The method for detecting equipment of a laser confocal Raman spectrometer according to any one of claims 1 to 8 comprises the following steps: Step 1, installing the detector, the sample chamber and the refrigerator on the ground, so that the sample chamber is located below the eyepiece of the optical path system in the detector, and installing a base between the ground and the detector, the sample chamber and the refrigerator for support; Step 2, connecting the sample chamber and the refrigerator in the order of the cooling tube, the protection tube and the connecting tube from inside to outside, and arranging a shock absorbing mechanism between the refrigerator and the cooling tube, and making the number of supporting rods of the shock absorbing mechanism decrease in sequence from inside to outside; Step 3: The control panel controls the operation of the detector through the measurement of the pressure sensor and the temperature sensor.

10. The detection method of laser confocal Raman spectrometer according to claim 9, characterized in that: In step 1 and step 2, the inner wall of the sample chamber and the inner wall of the protective tube are polished, and the sample chamber is evacuated at the same time.

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