CN114813670B - Low-temperature diamond nitrogen vacancy color center optical microscope - Google Patents
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G01N21/6456—Spatial resolved fluorescence measurements; Imaging
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- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
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Abstract
The invention discloses a low-temperature diamond nitrogen vacancy color center optical microscope, which aims to solve the problems that the current diamond nitrogen vacancy color center magnetic microscope is rarely researched, room-temperature experiments can only be carried out in an atmospheric environment, and research on magnetic materials in a low-temperature environment cannot be carried out; the optical platform is provided with a light path component which is used for making laser incident to the diamond nitrogen vacancy color center magnetic force microscope scanning head, focusing on the sample and receiving the original return fluorescence. The invention is especially suitable for the research of nano-scale magnetic materials in low-temperature environment, and has higher social use value and application prospect.
Description
Technical Field
The invention relates to the technical field of optical microscopes, in particular to a low-temperature diamond nitrogen vacancy color center optical microscope.
Background
Microscopic imaging and observation of magnetic materials are helpful for researching the microstructure and formation mechanism of the magnetic materials, and the scale of the magnetic material research tends to be submicron or even nanometer along with the development of scientific research technology. Therefore, ultra-high resolution and ultra-high sensitivity magnetic material testing has facilitated research into these nanoscale magnetic materials.
At present, the traditional microscopic observation equipment for magnetic material research mainly comprises a Kerr microscope (resolution is about 300 nm), a magnetic microscope MFM (resolution is about 50 nm) and the like, and the magnetic measurement technology and the scanning imaging technology of a diamond nitrogen vacancy color center are combined by the magnetic microscope of the diamond nitrogen vacancy color center, so that high-resolution magnetic imaging of about 30nm can be realized, quantitative magnetic analysis can be realized, and the magnetic microscopic observation equipment has remarkable advantages in magnetic microscopic imaging.
At present, few researches on a diamond nitrogen vacancy color center magnetic force microscope are carried out in China, room temperature experiments can be carried out only in an atmospheric environment, and researches on magnetic materials in a low-temperature environment can not be carried out. To this end, we propose a low temperature diamond nitrogen vacancy colour-centered optical microscope.
Disclosure of Invention
The present invention aims to solve or at least alleviate the problems of the prior art.
The invention provides a low-temperature diamond nitrogen vacancy color center optical microscope, which comprises an optical platform serving as a mounting matrix and a main chamber arranged on the optical platform, wherein the main chamber is provided with a cryostat for maintaining the low temperature in the main chamber and an ion pump for maintaining the ultra-high vacuum environment in the main chamber, and the main chamber is internally provided with a diamond nitrogen vacancy color center magnetic microscope scanning head for high-resolution magnetic imaging;
the optical platform is provided with a light path component which is used for making laser incident to the diamond nitrogen vacancy color center magnetic force microscope scanning head, focusing on the sample and receiving the original return fluorescence.
Optionally, one side of the main chamber is connected with a sample injection chamber through a transfer chamber in a penetrating way, a molecular pump for maintaining the vacuum state in the sample injection chamber is arranged on the sample injection chamber, and sample transmission rods for in-situ sample transmission without breaking the vacuum low-temperature environment of the main chamber are arranged on the transfer chamber and the sample injection chamber.
Optionally, the scanning head of the diamond nitrogen vacancy color center magnetic force microscope comprises an outer frame fixed on the inner wall of the main cavity, and an atomic force microscope for scanning a sample to obtain a sample surface morphology image, an objective lens component for converging excitation light and collecting fluorescence, and a microwave antenna component for performing microwave regulation and control on the nitrogen vacancy color center are arranged in the outer frame;
wherein the atomic force microscope comprises a needle tip assembly and a sample assembly.
Optionally, the needle point subassembly includes the diamond needle point that can dismantle the installation on the needle point holds in the palm through the needle point holds in the palm the preforming, and the positive and negative pole of diamond needle point is connected with the electrode that is used for needle point vibration control and surveys, and the needle point holds in the palm and installs on the output of X direction piezoceramics stepper motor, and X direction piezoceramics stepper motor installs on the output of first Y direction piezoceramics stepper motor, and first Y direction piezoceramics stepper motor is fixed in on the roof of outer frame.
Optionally, the sample subassembly is including the sample frame that is used for the sample to deposit, and the sample frame is installed on XY direction coupling piezoelectric stepper motor's output through pluggable sample frame preforming, still installs the piezoelectric scanning platform that is used for realizing needle feeding operation and high accuracy scanning sample on XY direction coupling piezoelectric stepper motor's the output, XY direction coupling piezoelectric stepper motor is fixed in on the output of first Z direction piezoelectric stepper motor, and first Z direction piezoelectric stepper motor passes through the adaptor and installs on the roof of outer frame.
Optionally, the objective lens assembly includes an objective lens, the objective lens is mounted on an output end of the second Z-direction piezoelectric stepper motor through an adapter to adjust a Z-direction position of the objective lens so that a laser focus converged by the objective lens coincides with a nitrogen vacancy color center in the diamond needle point, and the second Z-direction piezoelectric stepper motor is fixed on a bottom wall of the outer frame.
Optionally, the microwave antenna assembly includes a microwave antenna, and the microwave antenna is installed on the output end of the second Y-direction piezoelectric stepper motor through the adapter, the second Y-direction piezoelectric stepper motor is installed on the output end of the Z-direction piezoelectric stepper motor, and the Z-direction piezoelectric stepper motor is installed on the bottom wall of the outer frame.
Optionally, the microwave antenna assembly further comprises a microwave source for generating a microwave signal and an amplifier for amplifying the microwave signal.
Optionally, the distance between the microwave antenna and the diamond needle point is 90-110um.
The invention has the following advantages:
1. the invention can realize vacuum degree better than 5x10 by arranging the low-temperature thermostat and the ion pump on the main chamber -8 The working temperature in the main chamber is between 10K and 300K under the ultra-high vacuum low-temperature working environment with the Pa and the temperature of about 10K, so that the magnetic properties of the sample in the low-temperature environment can be tested, the diamond needle tip and the sample can be replaced in situ, and the experimental efficiency is effectively improved.
2. The invention realizes quantitative nondestructive imaging of magnetic properties through the arrangement of the diamond nitrogen vacancy color center magnetic force microscope scanning head, has high spatial resolution of about 30nm and ultrahigh detection sensitivity of single spin, realizes high resolution magnetic imaging of about 30nm, provides technical support for the research of nano-scale magnetic materials in low-temperature environment, and has wide application prospect in the fields of magnetic domain imaging, two-dimensional materials, topological magnetic structures and the like.
Drawings
The foregoing features, technical features, advantages and implementation of a low temperature diamond nitrogen vacancy color center optical microscope will be further described in a clear and understandable manner by describing preferred embodiments with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic diagram of a scanning head of a diamond nitrogen vacancy color center magnetic force microscope in accordance with the present invention;
FIG. 3 is a schematic view of a needle tip assembly according to the present invention;
FIG. 4 is a schematic view of a sample assembly according to the present invention;
FIG. 5 is a schematic view of an objective lens assembly according to the present invention;
fig. 6 is a schematic structural diagram of a microwave antenna assembly according to the present invention;
fig. 7 is a flow chart of a low temperature diamond nitrogen vacancy color center optical microscope imaging of the present invention.
In the figure: cryostat 10, ion pump 20, main chamber 30, transfer chamber 301, diamond nitrogen vacancy color center magnetic force microscope scanning head 40, outer frame 41, needle tip assembly 42, X-direction piezoelectric stepper motor 421, first Y-direction piezoelectric stepper motor 422, needle tip holding piece 423, electrode 424, needle tip holding 425, diamond needle tip 426, and,
The microwave antenna assembly 45, the microwave antenna 451, the second Y-direction piezoelectric stepper motor 452, the adaptor 453, the Z-direction piezoelectric stepper motor 454, the sample rod 50, the light path member 60, the sample chamber 70, the molecular pump 80 and the optical platform 90;
in fig. 7: laser 001, coupler 002, single mode fiber 003, collimator 004, long-pass dichroic mirror 005, scanning galvanometer 006, first lens 007, second lens 008, objective lens 009, microwave antenna 010, diamond probe 011, sample 012, amplifier 013, microwave source 014, displacement stage 015, third lens 016, long-pass filter 017, multimode fiber 018, photon counter 019, beam splitting mirror 020, infinity barrel 021, CCD 022, flexible fiber light guide 023, fiber illuminator 024, three-dimensional displacement stage 025.
Detailed Description
The invention is further illustrated by the following examples in connection with figures 1-7:
example 1
The invention provides a low-temperature diamond nitrogen vacancy color center optical microscope, referring to fig. 1-2, comprising an optical platform 90 serving as a mounting matrix and a main chamber 30 arranged on the optical platform 90, wherein the main chamber 30 is provided with a cryostat 10 for maintaining the low temperature in the main chamber 30 and an ion pump 20 for maintaining the ultra-high vacuum environment in the main chamber 30;
the main chamber 30 is internally provided with a diamond nitrogen vacancy color core magnetic force microscope scanning head 40 for high resolution magnetic imaging, and the optical platform 90 is provided with a light path component 60 for making laser incident on the diamond nitrogen vacancy color core magnetic force microscope scanning head 40 and focusing on a sample and receiving return fluorescence of a primary path.
The scanning head 40 of the diamond nitrogen vacancy color center magnetic force microscope comprises an outer frame 41 fixed on the inner wall of the main chamber 30, and an atomic force microscope for scanning a sample to obtain a sample surface morphology image, an objective lens assembly 44 for converging excitation light and collecting fluorescence, and a microwave antenna assembly 45 for performing microwave regulation and control on the nitrogen vacancy color center are arranged in the outer frame 41;
wherein the atomic force microscope comprises a tip assembly 42 and a sample assembly 43; in this embodiment, the diamond nitrogen vacancy color center magnetic force microscope scanning head 40 is all made of nonmagnetic materials such as pure titanium, and is suitable for experiments in a strong magnetic vacuum low-temperature environment.
In this embodiment, the light path member 60 emits a collimated gaussian beam and enters the objective lens assembly 44 of the diamond nitrogen-vacancy color center magnetic force microscope scanning head 40, the objective lens assembly 44 converges excitation light to be collected at the diamond needle point 426 of the needle point assembly 42, the nitrogen-vacancy color center in the diamond needle point 426 generates a fluorescence primary path to return through the objective lens assembly 44, the objective lens assembly 44 collects fluorescence and the emitted fluorescence primary path returns to the light path member 60, and the photon counter built in the light path member 60 receives detection.
In this embodiment, as shown in fig. 3, the tip assembly 42 includes a diamond tip 426 detachably mounted on a tip holder 425 through a tip holding piece 423, the tip amplitude is not required to be detected by an additional optical path, the color center fluorescence collection efficiency of a special optical coupling structure is high, the positive and negative electrodes of the diamond tip 426 are connected with electrodes 424 for controlling and detecting the tip vibration, the tip holder 425 is mounted on the output end of an X-direction piezoelectric ceramic stepper motor 421, the X-direction piezoelectric ceramic stepper motor 421 is mounted on the output end of a first Y-direction piezoelectric stepper motor 422, and the first Y-direction piezoelectric stepper motor 422 is fixed on the top wall of the outer frame 41, thereby effectively ensuring the adjustment of the diamond tip 426 in the X-direction and the Y-direction, and further adjusting the position of the diamond tip 426 to move the nitrogen vacancy color center to the focal point of the objective lens 441.
In this embodiment, as shown in fig. 4, the sample assembly 43 includes a sample holder 435 for storing samples, the sample holder 435 is mounted on an output end of an XY-direction coupled piezoelectric stepper motor 433 through a pluggable sample holder pressing sheet 436, a piezoelectric scanning table 434 for implementing a needle insertion operation and scanning samples with high precision is further mounted on the output end of the XY-direction coupled piezoelectric stepper motor 433, the XY-direction coupled piezoelectric stepper motor 433 is fixed on an output end of the first Z-direction piezoelectric stepper motor 432, and the first Z-direction piezoelectric stepper motor 432 is mounted on a top wall of the outer frame 41 through an adaptor 431, and the positions of the sample holder 435 can be adjusted in three dimensions by the first Z-direction piezoelectric stepper motor 432 and the XY-direction coupled piezoelectric stepper motor 433, so as to adjust the position of the sample to be detected to move to the diamond probe tip 426 for testing.
In this embodiment, as shown in fig. 5, the objective lens assembly 44 includes an objective lens 441, the objective lens 441 is mounted on an output end of a second Z-direction piezoelectric stepper motor 443 via an adapter 442 to adjust the Z-direction position of the objective lens 441 so that the converging laser focus of the objective lens 441 coincides with the nitrogen vacancy color center in the diamond tip 426, and the second Z-direction piezoelectric stepper motor 443 is fixed on the bottom wall of the outer frame 41.
In this embodiment, as shown in fig. 6, the microwave antenna assembly 45 includes a microwave antenna 451, a microwave source 014 for generating microwave signals, and an amplifier 013 for amplifying the microwave signals, wherein the microwave antenna 451 is mounted on the output end of the second Y-direction piezoelectric stepper motor 452 through an adaptor 453, the second Y-direction piezoelectric stepper motor 452 is mounted on the output end of the Z-direction piezoelectric stepper motor 454, the Z-direction piezoelectric stepper motor 454 is mounted on the bottom wall of the outer frame 41, and the second Y-direction piezoelectric stepper motor 452 and the Z-direction piezoelectric stepper motor 454 can two-dimensionally adjust the position of the microwave antenna 451 in the Y-direction and the Z-direction so that the distance between the microwave antenna 451 and the diamond tip 426 is 90-110um;
in this embodiment, the microwave source generates microwaves and emits the microwaves after being amplified, the microwave antenna 451 is located near the diamond tip 426, the spin state of the nitrogen-free color center can be operated and detected by laser and microwaves, the externally applied magnetic field is measured by an Optical Detection Magnetic Resonance (ODMR) method, and the magnetic field distribution imaging diagram of the sample surface can be obtained after the magnetic field on the sample surface is continuously detected by the scanning probe.
In the present embodiment, the arrangement of the cryostat 10 and the ion pump 20 on the main chamber 30 can realize the vacuum degree better than 5x10 -8 The working temperature in the main chamber 30 is between 10K and 300K in the ultra-high vacuum low-temperature working environment with Pa and about 10K, so that the magnetic property of a sample in the low-temperature environment can be tested; meanwhile, the arrangement of the diamond nitrogen vacancy color center magnetic force microscope scanning head 40 realizes quantitative nondestructive imaging of magnetic properties, has high spatial resolution of about 30nm and ultrahigh detection sensitivity of single spin, realizes high-resolution magnetic imaging of about 30nm, provides technical support for the research of nano-scale magnetic materials in a low-temperature environment, and has wide application prospects in the fields of magnetic domain imaging, two-dimensional materials, topological magnetic structures and the like.
Example 2
The difference between this embodiment and embodiment 1 is that, as shown in fig. 6, one side of the main chamber 30 is connected with the sample injection chamber 70 through the transfer chamber 301, the sample injection chamber 70 is installed with the molecular pump 80 for maintaining the vacuum state in the sample injection chamber 70, the transfer chamber 301 and the sample injection chamber 70 are provided with the sample transmission rod 50 for in-situ sample transmission without breaking the vacuum low-temperature environment of the main chamber 30, and the sample and the diamond needle point 426 in the sample frame 435 are matched with the diamond needle point 426 detachably installed on the needle point 425 through the needle point supporting piece 423 and the sample frame 435 installed on the output end of the XY-direction coupled piezoelectric stepping motor 433 through the pluggable sample frame pressing piece 436, so that the sample and the diamond needle point 426 in the sample frame 435 can be replaced in situ through the operation of the sample transmission rod 50.
Other undescribed structures refer to embodiment 1.
In the imaging process of the low-temperature diamond nitrogen vacancy color center optical microscope of the embodiment, referring to fig. 7, laser 001 emits 532nm laser light into a single-mode optical fiber 003 through a coupler 002 and emits the laser light into a collimated Gaussian beam from a collimator 004, the collimated Gaussian beam enters a scanning galvanometer 006 after being reflected by a long-wave-pass dichroic mirror 005 and then enters an entrance pupil of an objective lens 009 to be focused at a needle point of a diamond probe 011 after passing through a 4F optical system, the nitrogen vacancy color center in the diamond probe 011 generates a fluorescence primary path, and the fluorescence primary path returns to the objective lens 009, the 4F optical system, the scanning galvanometer 006 and the long-wave-pass dichroic mirror 005, and finally enters a multimode optical fiber 018 through a third lens 016 to be received and detected by a photon counter 019 after being focused by a long-wave-pass filter 017, wherein the angle of the third lens 016 can be adjusted through a displacement table 015 to focus fluorescence;
in which a 4F optical system for scanning and positioning the nitrogen-vacancy color center together with the scanning galvanometer 006 is provided in the light path member 60, in fig. 7, the first lens 007 and the second lens 008 constitute the 4F optical system in the present embodiment.
Early debugging stage: a beam splitter 020 is arranged between a 4F optical system and an objective 009, white light emitted by an optical fiber illuminator 024 is reflected to the objective 009 by the beam splitter 020 through a flexible optical fiber light guide 023 and an infinite lens barrel 021 and is focused on a diamond probe 011 tip and a sample 012, a reflected light primary path returns to enter the CCD 022 for imaging, the laser focus and a nitrogen vacancy color center can be aligned and the sample 012 is positioned through the adjustment, wherein the infinite lens barrel 021 and the CCD 022 can realize position adjustment through a three-dimensional displacement table 025, the white light is ensured to be focused on the diamond probe 011 tip and the sample 012, and the reflected light enters the CCD 022 for imaging;
According to the cryogenic diamond nitrogen vacancy color center optical microscope of the embodiment of the invention, the arrangement of the cryostat 10 and the ion pump 20 on the main chamber 30 can realize the vacuum degree better than 5x10 -8 The working temperature in the main chamber 30 is 10K-300K in the ultra-high vacuum low-temperature working environment with Pa and temperature of about 10K, and the magnetic property of the sample in the low-temperature environment can be testedThe diamond needle tip and the sample can be replaced in situ, so that the experimental efficiency is effectively improved;
meanwhile, the arrangement of the diamond nitrogen vacancy color center magnetic force microscope scanning head 40 realizes quantitative nondestructive imaging of magnetic properties, has high spatial resolution of about 30nm and ultrahigh detection sensitivity of single spin, realizes high-resolution magnetic imaging of about 30nm, provides technical support for the research of nano-scale magnetic materials in a low-temperature environment, and has wide application prospects in the fields of magnetic domain imaging, two-dimensional materials, topological magnetic structures and the like.
In the description of the present invention, it should be noted that the terms "first," "second," and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Finally, it should be noted that: the above examples are only specific embodiments of the present invention, and are not intended to limit the scope of the present invention, but it should be understood by those skilled in the art that the present invention is not limited thereto, and that the present invention is described in detail with reference to the foregoing examples: any person skilled in the art may modify or easily conceive of the technical solution described in the foregoing embodiments, or perform equivalent substitution of some of the technical features, while remaining within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (5)
1. The low-temperature diamond nitrogen vacancy color center optical microscope comprises an optical platform (90) serving as a mounting substrate and a main chamber (30) arranged on the optical platform (90), and is characterized in that the main chamber (30) is provided with a cryostat (10) for maintaining low temperature in the main chamber (30), an ion pump (20) for maintaining an ultrahigh vacuum environment in the main chamber (30), and a diamond nitrogen vacancy color center magnetic microscope scanning head (40) for high-resolution magnetic imaging is arranged in the main chamber (30); the optical platform (90) is provided with a light path component (60) which is used for making laser incident to the diamond nitrogen vacancy color center magnetic force microscope scanning head (40) and focusing on the sample and receiving the original return fluorescence;
the diamond nitrogen vacancy color center magnetic force microscope scanning head (40) comprises an outer frame (41) fixed on the inner wall of the main cavity (30), and an atomic force microscope for scanning a sample to obtain a sample surface morphology image, an objective lens assembly (44) for converging excitation light and collecting fluorescence and a microwave antenna assembly (45) for performing microwave regulation and control on the nitrogen vacancy color center are arranged in the outer frame (41);
wherein the atomic force microscope comprises a needle tip assembly (42) and a sample assembly (43);
the needle point component (42) comprises a diamond needle point (426) detachably arranged on a needle point holder (425) through a needle point holding sheet (423), the anode and the cathode of the diamond needle point (426) are connected with electrodes (424) for controlling and detecting needle point vibration, the needle point holder (425) is arranged on the output end of an X-direction piezoelectric ceramic stepping motor (421), the X-direction piezoelectric ceramic stepping motor (421) is arranged on the output end of a first Y-direction piezoelectric stepping motor (422), and the first Y-direction piezoelectric stepping motor (422) is fixed on the top wall of an outer frame (41);
the sample assembly (43) comprises a sample rack (435) for storing samples, the sample rack (435) is arranged on the output end of an XY direction coupling piezoelectric stepping motor (433) through a pluggable sample rack pressing sheet (436), a piezoelectric scanning table (434) for realizing needle insertion operation and high-precision sample scanning is further arranged on the output end of the XY direction coupling piezoelectric stepping motor (433), the XY direction coupling piezoelectric stepping motor (433) is fixed on the output end of a first Z direction piezoelectric stepping motor (432), and the first Z direction piezoelectric stepping motor (432) is arranged on the top wall of the outer frame (41) through an adapter (431);
one side of the main chamber (30) is connected with a sample injection chamber (70) in a penetrating way through a transfer chamber (301), a molecular pump (80) for maintaining the vacuum state in the sample injection chamber (70) is installed on the sample injection chamber (70), and sample transmission rods (50) for in-situ sample transmission without breaking the vacuum low-temperature environment of the main chamber (30) are arranged on the transfer chamber (301) and the sample injection chamber (70).
2. A cryogenic diamond nitrogen vacancy color-centered optical microscope as in claim 1, wherein: the objective lens assembly (44) comprises an objective lens (441), the objective lens (441) is arranged on the output end of a second Z-direction piezoelectric stepping motor (443) through a connecting piece (442) so as to adjust the Z-direction position of the objective lens (441) to enable the focus of converging laser of the objective lens (441) to coincide with the color center of nitrogen vacancy in the diamond needle point (426), and the second Z-direction piezoelectric stepping motor (443) is fixed on the bottom wall of the outer frame (41).
3. A cryogenic diamond nitrogen vacancy color-centered optical microscope as in claim 1, wherein: the microwave antenna assembly (45) comprises a microwave antenna (451), the microwave antenna (451) is mounted on the output end of a second Y-direction piezoelectric stepping motor (452) through an adapter (453), the second Y-direction piezoelectric stepping motor (452) is mounted on the output end of a Z-direction piezoelectric stepping motor (454), and the Z-direction piezoelectric stepping motor (454) is mounted on the bottom wall of the outer frame (41).
4. A cryogenic diamond nitrogen vacancy color-centered optical microscope as in claim 3, wherein: the microwave antenna assembly (45) further comprises a microwave source (014) for generating a microwave signal and an amplifier (013) for amplifying the microwave signal.
5. A cryogenic diamond nitrogen vacancy color-centered optical microscope as in claim 3, wherein: the distance between the microwave antenna (451) and the diamond needle point (426) is 90-110um.
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