CN110286100B - Infrared reflection and transmission measurement system and method - Google Patents
Infrared reflection and transmission measurement system and method Download PDFInfo
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- CN110286100B CN110286100B CN201910610537.2A CN201910610537A CN110286100B CN 110286100 B CN110286100 B CN 110286100B CN 201910610537 A CN201910610537 A CN 201910610537A CN 110286100 B CN110286100 B CN 110286100B
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
The invention discloses an infrared reflection and transmission measurement system and method, aiming at the characterization problem of the physical property of magnetic field regulation, the technical scheme of the invention combines infrared spectroscopy measurement and a magnetic field, can realize variable low-temperature infrared reflection and transmission measurement under the magnetic field, and can simultaneously measure the reflection and transmission spectrums of a sample which can reflect and transmit infrared light without changing a light path or reloading the sample when the measurement system carries out reflection and transmission measurement.
Description
Technical Field
The invention relates to the technical field of spectral measurement, in particular to an infrared reflection and transmission measurement system and method.
Background
Infrared spectroscopy is a powerful method for studying the optical properties, molecular vibration and the dynamic behavior of low-energy charges in materials with quantum functions, and is widely applied in the fields of material science, physics, chemistry, polymer science, biology, life science and the like. By measuring the infrared reflection spectrum or the transmission spectrum of the sample, important information such as the optical coefficient (dielectric coefficient, photoconduction, refractive index and the like), the molecular structure, various basic excitations (electrons, phonons, spins, plasmons and the like) and the interaction between the basic excitations can be obtained.
Magnetic fields can couple electron charges with the proton, neutron, and electron magnetic moments of the constituent species, and are a powerful tool for studying material properties. The superconductor, the magnetic material and the quantum Hall device can generate coupled spin under the action of a strong magnetic field, establish or remove the phenomena of correlation, resonance, local electrons, breaking time reversal symmetry and the like, and the properties of the materials are obviously influenced. Therefore, the magnetic field is an important thermodynamic parameter as well as the temperature and the pressure.
At present, a common reflection spectrum measurement accessory or a transmission spectrum measurement mode configured for an infrared spectrometer cannot be coupled with a low temperature superconducting magnet for measurement. Even when the measurement is not carried out at low temperature or in a magnetic field, the measurement of reflection spectrum and transmission spectrum can not be carried out simultaneously, the corresponding reflection accessory must be arranged on a spectrometer for measurement when the reflection spectrum is measured, the reflection accessory must be removed for measurement when the transmission spectrum is measured, and a sample also needs to be reloaded.
Disclosure of Invention
In view of this, the technical solution of the present invention provides an infrared reflection and transmission measurement system and method, which combine infrared spectroscopy measurement and a magnetic field to realize variable low-temperature infrared reflection and transmission spectroscopy measurement under the magnetic field without changing a light path and reloading a sample.
In order to achieve the above purpose, the invention provides the following technical scheme:
an infrared reflection and transmission measurement system, the measurement system comprising:
the superconducting magnet chamber is provided with a first flange port and a second flange port which are opposite, the sample to be detected is placed between the first flange port and the second flange port, and the superconducting magnet chamber is used for providing a magnetic field environment for the sample to be detected;
the reflection spectrum measuring device is used for irradiating infrared light emitted by an infrared spectrometer onto the sample to be measured through the first flange opening, acquiring the infrared light reflected by the sample to be measured through the first flange opening, and measuring infrared reflection spectrum information of the sample;
and the transmission measuring device is used for acquiring the infrared light transmitted by the sample to be measured through the second flange port and measuring the infrared transmission spectrum information of the sample.
Preferably, in the above measurement system, the superconducting magnet chamber includes:
the magnetic field vacuum chamber comprises a room temperature hole penetrating through a magnet, and the two ends of one room temperature hole are respectively provided with the first flange port and the second flange port;
and the sample holder is used for loading the sample to be detected.
Preferably, in the above measuring system, the sample holder includes: the device comprises a sample rod, a sample support and a three-dimensional translation table;
the sample support is fixed on the sample rod and used for placing the sample to be detected;
one end of the sample rod, which is fixed with the sample support, is used for being arranged in the magnetic field vacuum chamber through one end of the other room temperature hole and is connected with the three-dimensional translation stage in the magnetic field vacuum chamber;
the three-dimensional translation stage is used for adjusting the position of the sample to be measured.
Preferably, in the above measuring system, the other end of the sample rod is used for inserting a transmission line, and one end of the transmission line, which is far away from the sample rod, is inserted into a liquid nitrogen tank or a liquid helium tank, so that the sample is supported in a set temperature environment.
Preferably, in the above measurement system, the reflection spectrum measurement apparatus includes:
the reflecting vacuum cavity is provided with a third flange port used for being connected with the infrared spectrometer and a fourth flange port used for being arranged opposite to the first flange port;
the first light path component is used for irradiating infrared light obtained through the third flange opening onto the sample to be detected sequentially through the fourth flange opening and the first flange opening, obtaining the infrared light reflected by the sample to be detected sequentially through the first flange opening and the fourth flange opening, and transmitting the obtained reflected light to the reflection detector.
Preferably, in the above measurement system, the first optical path member includes:
the first optical lens group is used for transmitting infrared light incident through the third flange port to the fourth flange port for emergent emission so as to irradiate the sample to be detected;
the second optical lens group is used for acquiring infrared light incident through the fourth flange port and transmitting the acquired infrared light to the reflection detector; the reflection detector comprises a first reflection detector positioned in the reflection vacuum cavity and a second reflection detector positioned outside the reflection vacuum cavity;
the second optical lens group can enable infrared light to be transmitted to the first reflection detector through a first path, or enable the infrared light to be transmitted to the second reflection detector through a second path and a fifth flange port located on the reflection vacuum cavity.
Preferably, in the above measurement system, the transmission measurement device includes:
a transmission vacuum chamber having a sixth flange port for opposing the second flange port;
and the second light path component is used for acquiring the infrared light transmitted by the sample to be detected sequentially through the second flange port and the sixth flange port and transmitting the acquired infrared light to the transmission detector.
Preferably, in the above measurement system, the transmission detector includes: a first transmission detector located within the transmission vacuum chamber and a second transmission detector located outside the transmission vacuum chamber;
the second optical path component comprises: the third optical lens group can enable infrared light to be transmitted to the first transmission detector through a third path, or enable the infrared light to be transmitted to the second transmission detector through a fourth path and a seventh flange port located on the transmission vacuum cavity.
In the above measurement system, it is preferable that each of the superconducting magnet chamber, the reflection spectrum measuring device, and the transmission spectrum measuring device has a vacuum chamber in which a degree of vacuum is independently controlled.
The invention also provides an infrared reflection and transmission measurement method, and the reflection spectrum information and the transmission spectrum information of the sample to be measured are measured by the measurement system.
It can be known from the above description that in the infrared reflection and transmission measurement system and method provided in the technical solution of the present invention, the infrared spectroscopy measurement and the magnetic field are combined to achieve variable low temperature infrared reflection and transmission measurement under the magnetic field, and when the measurement system performs reflection and transmission measurement, the light path does not need to be changed, and the sample does not need to be reloaded, so that the reflection and transmission spectrum of the sample which can reflect and transmit infrared light can be measured at the same time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an infrared reflection and transmission measurement system according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of another infrared reflection and transmission measurement system according to an embodiment of the present invention;
FIG. 3 is an equivalent optical path diagram of the measuring apparatus shown in FIG. 2;
FIG. 4 is a reflection line provided by an embodiment of the present invention;
fig. 5 is a transmission line according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1, fig. 1 is a schematic structural diagram of an infrared reflection and transmission measurement system provided in an embodiment of the present invention, where the measurement system includes: a superconducting magnet chamber 12, wherein the superconducting magnet chamber 12 has a first flange opening and a second flange opening which are opposite to each other, the sample 14 to be tested is placed between the first flange opening and the second flange opening, and the superconducting magnet chamber 12 is used for providing a magnetic field environment for the sample 14 to be tested; the reflection spectrum measuring device 11 is used for irradiating infrared light emitted by an infrared spectrometer 15 onto the sample 14 to be measured through the first flange opening, acquiring the infrared light reflected by the sample 14 to be measured through the first flange opening, and measuring infrared reflection spectrum information of the sample; and the transmission measuring device 13 is used for acquiring the infrared light transmitted by the sample 14 to be measured through the second flange port and measuring the infrared transmission spectrum information of the sample 13.
The infrared spectrometer 15 may be a fourier transform infrared spectrometer. The measurement system can be coupled with a Fourier transform infrared spectrometer and a superconducting magnet to realize a controllable low-temperature infrared reflection and transmission spectrum measurement system in a magnetic field.
The superconducting magnet chamber 12, the reflection spectrum measuring device 11 and the transmission measuring device 13 may be implemented as shown in fig. 2 and 3, where fig. 2 is a schematic structural diagram of another infrared reflection and transmission measuring system provided by an embodiment of the present invention, and fig. 3 is an equivalent optical path diagram of the measuring device shown in fig. 2.
As shown in fig. 2 and 3, the superconducting magnet chamber 12 includes: the magnetic field vacuum chamber 21 comprises two room temperature holes penetrating through the magnet, the two ends of one room temperature hole are respectively provided with the first flange port and the second flange port, and the magnetic field vacuum chamber 21 and the superconducting magnet 22 inside the magnetic field vacuum chamber jointly form a superconducting magnet chamber; a sample holder 23, wherein the sample holder 23 is used for loading the sample 14 to be tested. The sample holder 23 is used for providing a preset low-temperature environment for the sample 14 to be measured, and selecting and adjusting the position of the sample 14 to be measured. The measurement system can be used with a superconducting magnet with two horizontal room temperature bores. The aperture of one room temperature hole is 80mm, the aperture of the other room temperature hole is 50mm, and the aperture of the room temperature hole can be set by combining a light path, the size of a sample rack and the model of equipment, and is not particularly limited.
Optionally, the sample holder 23 comprises: a sample rod 24, a sample holder and a three-dimensional translation stage; the sample holder and the three-dimensional translation stage are not shown in fig. 2. The sample holder is fixed on the sample rod 24 and is used for placing the sample 14 to be detected; one end of the sample rod 24, to which the sample holder is fixed, is used for being placed in the magnetic field vacuum chamber 21 through the other end, and is connected with the three-dimensional translation stage in the magnetic field vacuum chamber 21; the three-dimensional translation stage is used for adjusting the position of the sample 14 to be measured. The three-dimensional translation stage comprises a two-dimensional short-distance translation adjusting platform and a one-dimensional long-distance translation stage with a corrugated pipe. The sample rod 24 is adapted to be mounted on a three-dimensional translation stage, and is connected to the superconducting magnet 22 via the bellows. The sample holder was made of copper. The sample holder is removably mounted on the sample rod 24. The sample holder can be two types of sample holders with holes and sample holders without holes, wherein the sample holder with holes is used for measuring reflection spectrums and transmission spectrums, and the sample holder without holes is used for measuring the reflection spectrums. The sample holder has a position for simultaneously placing three samples 14 to be measured of 10mm × 10mm size, and switching measurement of multiple samples can be performed without breaking vacuum.
The other end of the sample rod 24 is used for inserting a transmission line, and one end of the transmission line, which is far away from the sample rod, is inserted into a liquid nitrogen tank or a liquid helium tank, so that the sample holder is in a set temperature environment. The transfer line and the liquid nitrogen or liquid helium tank are not shown in fig. 2.
As shown in fig. 2 and 3, the reflection spectrum measuring apparatus 11 includes: the reflecting vacuum cavity 31 is provided with a third flange port used for being connected with the infrared spectrometer and a fourth flange port used for being arranged opposite to the first flange port; the first light path component is used for acquiring infrared light through the third flange opening, irradiating the infrared light onto the sample to be detected sequentially through the fourth flange opening and the first flange opening, acquiring the infrared light reflected by the sample to be detected sequentially through the first flange opening and the fourth flange opening, and transmitting the acquired reflected light to the reflection detector. The third flange port can be coupled with the infrared spectrometer through the set parallel light path 32, so that the third flange port can be coupled with the leading-out light path of most Fourier transform infrared spectrometers, and the third flange port can be conveniently used among spectrometers of different models without changing the light path.
The reflection spectrum measuring device 11 includes a reflection vacuum cavity 31 and a first light path component having a set light path, and the reflection spectrum measuring device 11 can focus infrared light guided by an infrared spectrometer onto the sample 14 to be measured, receive infrared light reflected by the sample 14 to be measured, and transmit the received infrared light to a reflection detector. The reflective vacuum cavity 31 is used to communicate the spectrometer with the superconducting magnet chamber 12.
The first light path component comprises octahedral optics M1-M8. The optical mirrors M1-M8 constitute a reflection optical path between the reflection spectrum measuring apparatus 11 and the superconducting magnet chamber 12. Optic M2, M5 and M6 are flat mirrors, and optic M1, M3, M4, M7 and M8 are ellipsoidal mirrors.
Optionally, the first optical path component includes: the first optical lens group is used for transmitting the infrared light incident through the third flange port to the fourth flange port for emergent so as to irradiate the sample to be detected, and for example, optical lenses M1-M3 form the first optical lens group; the second optical lens group is used for acquiring infrared light incident through the fourth flange port and transmitting the acquired infrared light to the reflection detector; the reflection detector comprises a first reflection detector 33 positioned in the reflective vacuum chamber 31 and a second reflection detector 34 positioned outside the reflective vacuum chamber 31, such as optical mirrors M4-M8 forming a second optical mirror group. The second optical lens group can transmit infrared light to the first reflective detector 33 through a first path, or transmit infrared light to the second reflective detector 34 through a second path and a fifth flange port located on the reflective vacuum cavity.
Optic M1 acts as a focusing mirror to receive collimated infrared light exiting the spectrometer and focus it to a focal point P1. The optical mirror M1 can focus the infrared light to the focal point P1 after being reflected by the optical mirror M1. The focused infrared light travels from the focal point P1 to the optic M3 at a preset distance. The optical mirrors M3 and M4 are a pair of focusing mirrors, the optical mirror M3 is configured to focus the incident infrared light onto the sample 14 to be measured, and the optical mirror M4 is configured to receive the infrared light reflected by the sample 14 to be measured, and transmit the infrared light to the optical mirror M5. The optic M5 is a position adjustable planar mirror that, at position a1, reflects incident infrared light to the optic M7, which transmits the infrared light to the first reflective detector 33 through the optic M7. When the optic M5 is at position a2, the incident infrared light may be reflected to the optic M8, and transmitted to the second reflective detector 34 through the optic M8. The infrared light from the optic M5 may be configured to be reflected by the optic M6 to the optic M7. The optical mirrors M7 and M8 are both focusing lenses and are respectively used for focusing incident infrared light to different reflection detectors so as to realize the reflection spectrum measurement of different infrared wave bands.
Wherein the optic M5 can be placed on a guide rail, the position of the optic M5 can be changed by a vacuum feed-in lever without breaking vacuum, so that it switches between positions a1 and a2 to select its outgoing infrared light to be transmitted to the optic M7 or M8.
As shown in fig. 2 and 3, the transmission measurement device 13 includes: a transmission vacuum chamber 41, wherein the transmission vacuum chamber 41 is provided with a sixth flange port opposite to the second flange port; and the second light path component is used for acquiring the infrared light transmitted by the sample to be detected 14 sequentially through the second flange port and the sixth flange port and transmitting the acquired infrared light to the transmission detector.
The transmission measuring device 13 includes a transmission vacuum chamber 41 and a second optical path component having a set optical path, and the transmission measuring device 13 is configured to receive the infrared light transmitted by the sample 14 to be measured after being absorbed and transmit the infrared light to the transmission detector.
The second light path component comprises five optical mirrors M9-M13, the optical mirrors M10 and M11 are plane mirrors, and the optical mirrors M9, M12 and M13 are ellipsoidal mirrors. Optics M1-M3 and M9-M13 constitute the transmission optical path. The reflection optical path and the transmission optical path share the optical mirrors M1-M3. After the optical mirror M1-M3 focuses the infrared light extracted by the infrared spectrometer on the sample 14 to be measured, the infrared light absorbed by the sample 14 to be measured is received by the optical mirror M9, and the optical mirror M9 is a focusing mirror. The optic M9 transmits the incident infrared light to the optic M12 or the optic M13 through the optic M10. The position of the optic M10 is adjustable, and when it is in position B1, it transmits the incident infrared light to the optic M12, and transmits the infrared light to the first transmission detector 42 through the optic M12. When the optic M10 is at position B2, the incident infrared light is transmitted to the optic M13, and the infrared light is transmitted to the second transmission detector 43 through the optic M13. The infrared light beyond the exit of optic M10 at position B1 may be arranged to be reflected by optic M11 to optic M12. The optical mirrors M12 and M13 are both focusing lenses and are respectively used for focusing incident infrared light to different transmission detectors so as to realize transmission spectrum measurement of different infrared wave bands.
Optionally, the transmission detector comprises: a first transmission detector 42 located within the transmissive vacuum chamber 41 and a second transmission detector 43 located outside the transmissive vacuum chamber 41; the second light path component includes: a third optical lens group, which can transmit the infrared light to the first transmission detector 42 through a third path, or transmit the infrared light to the second transmission detector 43 through a fourth path and a seventh flange port located on the transmission vacuum chamber 41.
In the embodiment of the present invention, the superconducting magnet chamber 12, the reflection spectrum measuring apparatus 11, and the transmission spectrum measuring apparatus 13 each have a vacuum chamber in which the degree of vacuum is independently controlled. Thus, the superconducting magnet chamber 12, the reflection spectrum measuring device 11 and the transmission spectrum measuring device 13 are respectively provided with independent vacuum chambers, and the measuring system works in a vacuum state to carry out spectrum measurement, so that water vapor and CO in the air can be effectively eliminated2And the like, and the three can be respectively vacuumized, so that the vacuum environment of the reflection spectrum measuring device 11 and the transmission spectrum measuring device 13 cannot be damaged when the sample 14 to be measured in the superconducting magnet chamber 12 is replaced. The reflection spectrum measuring device 11 may be connected to the superconducting magnet chamber 12 through a vacuum pipeline, and the two may be sealed by a window to maintain respective vacuum, and the transmission spectrum measuring device 13 may be connected to the superconducting magnet chamber 12 through a vacuum pipeline, and both may be connected to each otherThe chambers are maintained at their respective vacuums by the louver seals.
The number and arrangement of the optical mirrors in the reflection spectrum measuring device 11 and the transmission spectrum measuring device 13 are not limited to those shown in fig. 2 and 3, and the sizes of the reflection spectrum measuring device 11 and the transmission spectrum measuring device 13 in the length and width may be adjusted based on the need or the reduction of the number of plane mirrors. The light path is optimized by comprehensively considering different measurement modes, different detector switching and reducing the volume of the vacuum cavity as much as possible, and the number and the layout of optical mirrors in the reflection spectrum measuring device 11 and the transmission spectrum measuring device 13 are designed.
When the sample that awaits measuring 14 reflection infrared light and do not pass through infrared light and/or the sample frame is placed the sample that awaits measuring 14 regional not passing through infrared light, detecting system can be used for detecting the infrared reflection spectrum information of the sample that awaits measuring 14 alone, works as the sample that awaits measuring 14 reflection infrared light and transmission infrared light just the sample frame is placed the sample that awaits measuring 14 regional passing through infrared light, measuring system can measure the infrared reflection spectrum information and the reflection spectrum information of the sample that awaits measuring 14 simultaneously.
In the embodiment of the invention, all the optical elements, the optical element adjusting frame and the supporting and fixing piece are made of aluminum materials, and the spring of the mirror frame is made of nonmagnetic copper so as to eliminate the influence of a magnetic field and ensure the stability of an optical path.
As can be seen from the above description, the detection system according to the embodiment of the present invention has the following advantages:
the detection system can be coupled with a superconducting magnet and a sample rack with variable low temperature, so that the infrared reflectance spectrum or the infrared reflectance spectrum and the transmission spectrum under controllable low temperature and magnetic field can be measured simultaneously;
the light path design of the detection system adopts the infrared light which is introduced into the spectrometer by parallel light, and the detection system can be used together with most common Fourier transform infrared spectrometers without changing the light path, so that the detection system is convenient to transplant to different spectrometer systems;
for a sample to be measured which can transmit and reflect infrared light, the measuring system can simultaneously measure a reflection spectrum and a transmission spectrum without reloading the sample, and is very convenient for measurement under the conditions of low temperature and magnetic field.
The measurement of the reflection spectrum and the transmission spectrum by the measuring system of the present invention will be described below in specific experimental examples.
Experimental example 1
This example was conducted by measuring SrTiO3Reflection spectrum of single crystal sample, illustrating the embodiment of reflection spectrum measurement. Firstly, magnet excitation work is performed in advance according to the requirement of the superconducting magnet 22 until the magnet meets the working state. Taking out the low temperature sample rod 24 from the temperature hole, and mixing SrTiO 5mm × 5mm × 0.5mm3The single crystal sample and the reference gold-plated mirror are mounted on the two sample positions of the reflective sample holder at the front of the sample rod 24, respectively. The sample rod 24 is inserted into the room temperature hole and the reference golden mirror position is adjusted to the optical path center. The light is selectively transmitted to different reflective detectors by changing the optical mirror M5 according to the desired wavelength band to be measured. The signal measured by the reflection detector is monitored by the spectrometer in real time, and the position and the angle of the reference mirror (or the sample) can be finely adjusted according to the signal intensity until the signal is strongest. And starting a vacuum pump, and vacuumizing by opening an angle valve connected to the reflective vacuum cavity and the room-temperature hole until the vacuum meets the requirement. One end of the transmission line is inserted into the liquid nitrogen (or liquid helium) tank, the other end of the transmission line is inserted into the low-temperature sample rod 24, the liquid nitrogen (or liquid helium) is transmitted into the low-temperature sample rod through the transmission line, the temperature controller is used for setting the measurement temperature to be 78K, and the specific low-temperature environment can be set based on requirements and is not limited to be 78K. The magnetic field is applied to 3Tesla (Tesla) by a magnet control power supply, and the specific magnetic field environment can be set based on requirements and is not limited to 3 Tesla. Setting acquisition parameters by using a spectrometer acquisition program, acquiring a single-channel spectrum of a reference golden mirror as a reference spectrum, and then setting SrTiO through a sample rod 243The single crystal sample is moved to a measurement position and its single channel spectrum is acquired. SrTiO3The single channel spectrum of the single crystal sample is divided by the single channel spectrum of the gold mirror to obtain the reflection spectrum of the sample, as shown in fig. 4, fig. 4 is a reflection spectrum provided by an embodiment of the present invention, and fig. 4 is SrTiO3And (3) the reflection spectrum of the single crystal sample under the environment of 78K low temperature and the environment of 3Tesla magnetic field.
Experimental example 2
This example is obtained by measuring ZnO/HfO2Transmission spectra of the/Si thin film samples, illustrating embodiments of transmission spectrum measurements. Firstly, magnet excitation work is made in advance according to the requirement of the superconducting magnet until the magnet meets the working state. The cryogenic sample bar 24 was removed from the room temperature well, the transmissive sample holder was installed, and the ZnO/HfO2/Si thin film sample was placed in one of the sample positions of the transmissive sample holder (sample mounted in the center of the well) while the other sample position was left free of sample. The sample rod 24 is inserted into the room-temperature well, and the center of the well at the position where the sample is not placed is adjusted to the center of the optical path. The light is selectively transmitted to different transmission detectors by changing the optical mirror M10 according to the wavelength band to be measured. And monitoring the signals measured by the detector in real time by using a spectrometer, and finely adjusting the positions of the holes at the positions where the samples are not placed according to the signal intensity until the signals are strongest. And starting a vacuum pump, and vacuumizing by opening an angle valve connected to the transmission vacuum cavity and the room temperature hole until the vacuum meets the requirement. One end of the transmission line is inserted into the liquid nitrogen (or liquid helium) tank, the other end of the transmission line is inserted into the low-temperature sample rod, the liquid nitrogen (or liquid helium) is transmitted into the low-temperature sample rod 24 through the transmission line, the temperature controller is used for setting the measurement temperature to be 78K, and the specific low-temperature environment can be set based on requirements and is not limited to 78K. The magnetic field is applied to 3tesla by the magnet control power supply, and the specific magnetic field environment can be set based on requirements and is not limited to 3 tesla. Setting acquisition parameters by using a spectrometer acquisition program, acquiring an empty light path single-channel transmission spectrum of a position where a sample is not placed, moving a film sample to the center of a light path, and acquiring a single-channel transmission spectrum of the sample, wherein the ratio of the single-channel transmission spectrum of the sample to the empty light path single-channel spectrum is the transmission spectrum of the sample, as shown in fig. 5, fig. 5 is a transmission spectrum line provided by the embodiment of the invention. ZnO/HfO in FIG. 52The transmission spectrum of the/Si film sample under the environment of 78K low temperature and the environment of 3Tesla magnetic field.
Based on the embodiment of the measurement system, another embodiment of the present invention further provides an infrared reflection and transmission measurement method, which can measure reflection spectrum information and transmission spectrum information of a sample to be measured by using the measurement system described in the embodiment. The measurement method combines infrared spectroscopy measurement and a magnetic field aiming at the characterization problem of the physical property of magnetic field regulation, can realize variable low-temperature infrared reflection and transmission measurement under the magnetic field, does not need to change a light path or reload a sample when the measurement system carries out reflection and transmission measurement, and can simultaneously measure the reflection and transmission spectrums of the sample which can reflect and transmit infrared light.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The measuring method disclosed by the embodiment corresponds to the measuring device disclosed by the embodiment, so that the description is simple, and relevant points can be referred to the corresponding part of the measuring device for description.
It is further noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such article or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in an article or device that comprises the element.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. An infrared reflection and transmission measurement system, the measurement system comprising:
the superconducting magnet chamber is provided with a first flange opening and a second flange opening which are opposite, a sample to be detected is placed between the first flange opening and the second flange opening, and the superconducting magnet chamber is used for providing a magnetic field environment for the sample to be detected;
the reflection spectrum measuring device is used for irradiating infrared light emitted by an infrared spectrometer onto the sample to be measured through the first flange opening, acquiring the infrared light reflected by the sample to be measured through the first flange opening, and measuring infrared reflection spectrum information of the sample;
the transmission measuring device is used for acquiring infrared light transmitted by the sample to be measured through the second flange port and measuring infrared transmission spectrum information of the sample;
the superconducting magnet chamber includes:
the magnetic field vacuum chamber comprises two room temperature holes penetrating through the magnet, and the two ends of one room temperature hole are respectively provided with the first flange port and the second flange port
The sample holder is used for loading the sample to be detected;
the sample holder includes: the device comprises a sample rod, a sample support and a three-dimensional translation table;
the sample support is fixed on the sample rod and used for placing the sample to be detected;
one end of the sample rod, which is fixed with the sample support, is used for being arranged in the magnetic field vacuum chamber through one end of the other room temperature hole and is connected with the three-dimensional translation stage in the magnetic field vacuum chamber; the other end of the sample rod is used for inserting a transmission line, and one end of the transmission line, which is far away from the sample rod, is inserted into a liquid nitrogen tank or a liquid helium tank, so that the sample holder is in a set temperature environment;
the three-dimensional translation stage is used for adjusting the position of the sample to be measured.
2. The measuring system according to claim 1, wherein the other end of the sample rod is used for inserting a transmission line, and one end of the transmission line, which faces away from the sample rod, is inserted into a liquid nitrogen tank or a liquid helium tank, so that the sample holder is in a set temperature environment.
3. The measurement system of claim 1, wherein the reflectance spectrum measurement device comprises:
the reflecting vacuum cavity is provided with a third flange port used for being connected with the infrared spectrometer and a fourth flange port used for being arranged opposite to the first flange port;
the first light path component is used for acquiring infrared light through the third flange port, irradiating the infrared light onto the sample to be detected through the fourth flange port and the first flange port in sequence, acquiring the infrared light reflected by the sample to be detected through the first flange port and the fourth flange port in sequence, and transmitting the acquired reflected light to the reflection detector.
4. The measurement system of claim 3, wherein the first optical path component comprises:
the first optical lens group is used for transmitting infrared light incident through the third flange port to the fourth flange port for emergent emission so as to irradiate the sample to be detected;
the second optical lens group is used for acquiring infrared light incident through the fourth flange port and transmitting the acquired infrared light to the reflection detector; the reflection detector comprises a first reflection detector positioned in the reflection vacuum cavity and a second reflection detector positioned outside the reflection vacuum cavity;
the second optical lens group can enable infrared light to be transmitted to the first reflection detector through a first path, or enable the infrared light to be transmitted to the second reflection detector through a second path and a fifth flange port located on the reflection vacuum cavity.
5. The measurement system of claim 1, wherein the transmission measurement device comprises:
the transmission vacuum cavity is provided with a sixth flange port which is used for being arranged opposite to the second flange port;
and the second light path component is used for acquiring the infrared light transmitted by the sample to be detected sequentially through the second flange port and the sixth flange port and transmitting the acquired infrared light to a transmission detector.
6. The measurement system of claim 5, wherein the transmission detector comprises: a first transmission detector located within the transmission vacuum chamber and a second transmission detector located outside the transmission vacuum chamber;
the second optical path component comprises: the third optical lens group can enable infrared light to be transmitted to the first transmission detector through a third path, or enable the infrared light to be transmitted to the second transmission detector through a fourth path and a seventh flange port located on the transmission vacuum cavity.
7. The measurement system according to any one of claims 1 to 6, wherein the superconducting magnet chamber, the reflection spectrum measurement apparatus and the transmission spectrum measurement apparatus each have a vacuum chamber with independently controlled vacuum degrees.
8. An infrared reflection and transmission measuring method, characterized in that reflection spectrum information and transmission spectrum information of a sample to be measured are measured by the measuring system according to any one of claims 1 to 7.
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| CN102492939A (en) * | 2011-12-29 | 2012-06-13 | 中国科学院半导体研究所 | Atomic layer deposition apparatus integrated with Fourier transform infrared in-situ monitoring system |
| CN204262594U (en) * | 2014-10-22 | 2015-04-15 | 武汉辉科光电有限公司 | Flexible accurate panel beating laser cutting unit |
| CN108844926A (en) * | 2018-06-12 | 2018-11-20 | 中国科学院上海技术物理研究所 | Magneto-optic luminescence generated by light Photoreflectance and light modulation transmitted spectrum combined test system |
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| CN102492939A (en) * | 2011-12-29 | 2012-06-13 | 中国科学院半导体研究所 | Atomic layer deposition apparatus integrated with Fourier transform infrared in-situ monitoring system |
| CN204262594U (en) * | 2014-10-22 | 2015-04-15 | 武汉辉科光电有限公司 | Flexible accurate panel beating laser cutting unit |
| CN108844926A (en) * | 2018-06-12 | 2018-11-20 | 中国科学院上海技术物理研究所 | Magneto-optic luminescence generated by light Photoreflectance and light modulation transmitted spectrum combined test system |
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