Diamond-based heat-conducting optical cement preparation method, magnetic field temperature wide-field detection method and equipment

Abstract

The invention provides a diamond-based heat-conducting optical cement preparation method and device and a magnetic field temperature wide-field detection method and device. The method comprises the steps that an electron irradiation and annealing scheme is selected according to the diameter specification of diamond micro-powder; the annealed diamond micro-powder is subjected to acid pickling treatment; carrying out magnetic test and demagnetization treatment on the diamond micro-powder subjected to acid pickling treatment; performing drying treatment to obtain the quantum-grade diamond micro-powder heat-conducting filler; the quantum-grade diamond micro-powder heat-conducting filler is fully mixed into the ultraviolet light glue, and the diamond-based heat-conducting optical cement is obtained; preparing a chip sample to be tested based on the diamond-based heat-conducting optical cement; a chip sample to be detected is subjected to magnetic field / temperature detection based on magnetic field / temperature wide field detection equipment and method. By applying the technical scheme provided by the invention, the technical problems that the composite heat conduction material in the prior art generally only has heat conduction performance, does not have light transmission performance and does not have sensing characteristics, and magnetic field and temperature detection during chip operation cannot be realized while the heat dissipation performance of the chip is improved are solved.

Description

Technical Field

[0001] The present invention relates to the field of quantum precision measurement technology, and in particular to a preparation method and equipment for diamond-based thermal conductive optical adhesive and wide-field magnetic field temperature detection. Background Art

[0002] High-performance chips often have high heat generation power, and need to use heat dissipation devices to dissipate heat and keep the chip within a certain temperature range and operate normally. Affected by the physical structure of the chip, there is a gap in the contact interface between the chip and the heat dissipation device, which leads to reduced heat dissipation efficiency. Thermally conductive filling materials are needed to reduce contact thermal resistance. On the other hand, chip detection at the microscopic level can often only be achieved through observation under an optical microscope, and there is a lack of effective testing methods for physical quantities such as microcurrent and temperature of the microstructure inside the chip.

[0003] The conventional method for heat-conducting filling materials required for chip heat dissipation is to use composite thermal conductive materials. Composite thermal conductive materials are filled with thermal conductive fillers with high thermal conductivity coefficients, such as gold, silver, copper, aluminum nitride, etc., to improve the thermal conductivity of the material. However, existing composite thermal conductive materials usually only have thermal conductivity, not light transmittance, and even less sensing properties, and cannot detect the magnetic field and temperature of the chip while improving the chip's heat dissipation performance.

[0004] Currently, there are also technical solutions for detecting magnetic fields and temperatures during chip operation based on NV-color center quantum sensing. One type uses a diamond block containing an NV-color center ensemble diamond film layer as a sensor. This solution is limited by the rigid plane of the diamond block and is difficult to accurately detect for more complex special-shaped structures; one type is a probe scanning technology solution that combines NV-color center diamond particles with optical fiber. Its characteristic is that it can achieve high spatial resolution magnetic field measurement for a single point, but scanning the entire image takes a long time and cannot respond quickly; one type uses an optical fiber probe array to achieve rapid magnetic field detection within a certain range, but the diameter of the optical fiber probe itself limits the spatial resolution.

[0005] Therefore, it is necessary to break through the current technologies such as composite thermal conductive materials, rigid sensors, and optical fiber sensors, and realize high spatial resolution quantum sensing based on new thermal conductive materials to meet the needs of high-performance chips and various special-shaped structures for high thermal conductive materials as well as the needs for high spatial resolution magnetic field / temperature detection. Summary of the invention

[0006] The present invention provides a method and device for preparing diamond-based thermal conductive optical adhesive, and detecting a wide-field magnetic field and temperature, which can solve the technical problem in the prior art that composite thermal conductive materials usually only have thermal conductivity, no light transmittance, and no sensing characteristics, and cannot detect the magnetic field and temperature of the chip while improving the heat dissipation performance of the chip.

[0007] According to one aspect of the present invention, a method for preparing a diamond-based thermally conductive optical adhesive is provided, and the method for preparing a diamond-based thermally conductive optical adhesive comprises: step one, preparing diamond micropowder; step two, selecting whether to perform electron irradiation on the diamond micropowder or not according to the diameter specification of the diamond micropowder; if the diamond micropowder needs to be electron irradiated, then annealing the diamond micropowder after the electron irradiation; step three, judging whether there are impurities on the surface of the diamond micropowder, if there are impurities on the surface of the diamond micropowder, acid washing the annealed diamond micropowder; step four, performing a magnetic test on the diamond micropowder after the acid washing, if the magnetism of the diamond micropowder after the acid washing shows a magnetic field of the order of nT, demagnetizing the diamond micropowder; step five, drying the diamond micropowder to obtain a quantum-grade diamond micropowder thermally conductive filler; step six, fully mixing the quantum-grade diamond micropowder thermally conductive filler into the ultraviolet adhesive, and using ultrasonic vibration to fully disperse the diamond particles to obtain the diamond-based thermally conductive optical adhesive.

[0008] Furthermore, step 2 specifically includes: if the diameter specification of the diamond micropowder is nanometer-level diamond particles, the irradiation time of the diamond particles is less than 30 minutes, or no electron irradiation is performed; if the diameter specification of the diamond micropowder is micrometer-level diamond particles or the nitrogen concentration of the diamond micropowder is greater than 1ppm, the irradiation time of the diamond particles is not less than 30 minutes; if the irradiation time of the diamond micropowder exceeds 60 minutes, each 60 minutes is taken as a unit. After one electron irradiation unit, the diamond micropowder is taken out for annealing treatment, and then enters the next irradiation unit until the total irradiation time is completed.

[0009] Further, in step three, the diamond powder is subjected to acid washing treatment, which specifically includes: preparing a washing solution by mixing 30% concentration of hydrogen peroxide and concentrated sulfuric acid, mixing the diamond powder into the washing solution, stirring evenly for full reaction, heating to a set temperature, and then standing until the diamond powder is fully precipitated; removing excess acid solution from the upper layer, adding a large amount of deionized water to the remaining mixture of diamond powder and acid solution, and slowly adding sodium bicarbonate to the solution for neutralization; standing the solution, removing excess solution after the diamond powder is precipitated, and then adding a large amount of deionized water, and repeating this process for a set number of times; if the particle size of the diamond particles is less than 1 micron, the step of standing and settling can be omitted in the cleaning process after removing the acid solution, and the mixed solution can be directly filtered to obtain diamond powder, and repeatedly washed several times.

[0010] Furthermore, in step 4, the diamond powder is subjected to demagnetization treatment, which specifically includes: adding diamond particles to anhydrous ethanol and mixing them thoroughly, attaching a magnet to the bottom of a beaker containing the diamond-ethanol mixture, and placing the whole beaker in an ultrasonic cleaning machine water bath and oscillating it thoroughly, so that the diamond particles containing magnetic substances are attracted to the bottom of the beaker by the magnet; after the diamond-ethanol mixture is fully oscillated for a set time in the ultrasonic cleaning machine, pausing the ultrasound and quickly transferring the upper layer of the mixture to another clean beaker, and then injecting anhydrous ethanol into the original beaker, oscillating it again for a set time to absorb magnetic impurities, and then transferring the upper layer of the mixture after pausing the ultrasound, repeating this process until most of the non-magnetic diamond powder is transferred out, and finally filtering and evaporating the transferred mixture to obtain demagnetized diamond powder.

[0011] Furthermore, in step six, the quantum-grade diamond micro-powder thermal conductive filler is fully mixed into the ultraviolet adhesive, and the container sealed with the diamond-based thermal conductive optical adhesive mixture is placed in an ultrasonic water bath device, and the diamond particles are fully dispersed by ultrasonic vibration. The ultrasonic water bath time is 15-30 minutes.

[0012] According to another aspect of the present invention, a magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive is provided. The diamond-based thermal conductive optical adhesive is prepared using the preparation method of the diamond-based thermal conductive optical adhesive as described above. The magnetic field and temperature wide-field imaging detection device is used to realize magnetic field and temperature wide-field imaging detection of a sample to be tested. The diamond-based thermal conductive optical adhesive is coated on the sample to be tested. The magnetic field and temperature wide-field imaging detection device includes a sample test bench, a microwave antenna, an objective lens, an optical camera, a light source assembly, a lens assembly, a dichroic combination spectroscope, a filter assembly, a first permanent magnet, a second permanent magnet and a rotational translation stage assembly. The sample test bench is used to install the sample to be tested. The sample test bench includes a three-dimensional electric translation stage that can carry the sample to be tested to realize three-dimensional displacement. The first permanent magnet, the second permanent magnet and the rotary translation stage assembly are used to provide a bias magnetic field for the sample to be tested. The first permanent magnet and the second permanent magnet are symmetrically installed on both sides of the sample to be tested to form a uniform magnetic field at the sample to be tested. The microwave antenna is used to generate a uniform microwave magnetic field in the sample to be tested area. The light emitted by the light source assembly passes through the lens group and is split by the dichroic combination spectroscope. One beam of light passes through the objective lens and is irradiated onto the sample to be tested. The other beam passes through the lens assembly and is irradiated into the optical camera. The objective lens is used to image the diamond-based thermal conductive optical glue coated on the surface of the sample to be tested. After the fluorescence generated by the NV-color center in the diamond particles enters the optical lens, it passes through the color separation component and the filter component, and the optical camera performs light intensity detection, and the magnetic field and temperature are calculated according to the light intensity.

[0013] Further, the rotational translation stage assembly includes a first horizontal translation stage, a second horizontal translation stage, a vertical translation stage, a vertical rotation stage, a horizontal rotation stage and a base. The first permanent magnet is arranged on the first horizontal translation stage, and the first horizontal translation stage is used to drive the displacement of the first permanent magnet along the x direction. The second permanent magnet is arranged on the second horizontal translation stage, and the second horizontal translation stage is used to drive the displacement of the second permanent magnet along the x direction. The first horizontal translation stage and the second horizontal translation stage are arranged on the vertical rotation stage, and the vertical rotation stage is used to drive the rotation of the first permanent magnet and the second permanent magnet around the y axis. The vertical rotation stage is arranged on the vertical translation stage, and the vertical translation stage is used to drive the displacement of the first permanent magnet and the second permanent magnet along the z direction. The vertical translation stage is arranged on the horizontal rotation stage, and the horizontal rotation stage is used to drive the rotation of the first permanent magnet and the second permanent magnet around the z axis. The horizontal rotation stage is arranged on the base.

[0014] Furthermore, the dichroic film in the dichroic combination beam splitter is divided into two areas, including a dichroic coating part and a depolarizing beam splitting part, the dichroic coating part reflects 510nm-570nm green light, and the transmitted light wavelength is >650nm; the depolarizing beam splitting coating part has a reflection-transmission ratio of R / T=1; the filtering component includes a long-pass filter and a neutral filter, the starting wavelength of the long-pass filter is 650nm, the attenuation multiple of the neutral filter is 30dB-40dB, the neutral filter receives a light intensity reference signal corresponding to the camera frame, and the long-pass filter receives a diamond color center fluorescence signal corresponding to the camera frame.

[0015] According to another aspect of the present invention, a method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive is provided. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive uses the magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive as described above. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive comprises: irradiating a sample to be tested covered with diamond-based thermal conductive optical adhesive with green light, causing NV-color centers in quantum-level diamond particles to generate red fluorescence, performing wide-field imaging of the sample to be tested with an optical camera, and obtaining NV-color centers at different positions. The imaging area contains two parts: the first part is the excitation light intensity reference part, and the second part is the fluorescence signal detection part. The excitation light intensity reference part is used to correct the measurement error caused by the change of the fluorescence intensity due to the influence of the excitation light intensity. The sample to be tested is placed in a bias magnetic field, and microwave signals are uniformly radiated to the sample to be tested. The microwave frequency range is about 2.6GHz-3.2GHz. By scanning the microwave frequency, the optical magnetic resonance spectrum of each diamond particle can be detected by the camera, thereby obtaining the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles.

[0016] Furthermore, the optical magnetic resonance spectrum of each diamond particle is detected by a camera, so as to obtain the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles. Specifically, the green excitation light is reflected by the dichroic combination beam splitter and irradiated onto the sample to be tested through the objective lens. The NV-color centers in the diamond particles distributed on the sample to be tested emit fluorescence under the irradiation of the excitation light. The fluorescence is collected by the objective lens and then transmitted through the dichroic combination beam splitter, the long-pass filter and the neutral filter. The image is detected by the optical camera and processed to determine the diamond NV － The first magnetic field B1 is determined according to the distance and orientation between the first permanent magnet and the second permanent magnet, and the frequency is swept within the adjustable microwave frequency range. A frame of image is obtained at each frequency point, and each frame of image is processed. The specific processing method for each frame of image is: － The image processing unit i of the color center calculates the normalized signal s of its pixel with fluorescence signal i,j =F i,j / (k i R), j is the serial number of the frame image, corresponding to the microwave frequency f j , F i,j is the light intensity of the i-th image processing unit of the j-th frame image, which can eliminate the noise introduced by the change of the excitation light intensity. i}={s i,j} j＝1,2,3… , calculated by histogram {s i}, calculate the signal contrast {c i}={s i / s0}, with {c i} is the ordinate, frequency f j As the vertical axis, the NV in image processing unit i can be plotted. － The optical magnetic resonance spectrum of the color center; Based on the optical magnetic resonance spectrum, the microwave frequency is selected to use the 4-point method to measure the changes in the magnetic field / temperature during the test phase of the test product, and the magnetic field change δB and temperature change δT are obtained through 4 frames of images; During the normal operation of the test sample, each NV is monitored by the 4-point method － The changes of magnetic field and temperature at the color center are measured to complete the measurement under the bias magnetic field B1; the operation of the sample to be tested is stopped, and the external magnetic field is changed to the second magnetic field B2 and the third magnetic field B3 in turn, and the above optical magnetic resonance spectrum measurement process is repeated to complete the measurement of the magnetic field and temperature changes during the normal operation of the sample under different bias magnetic fields. The first magnetic field B1, the second magnetic field B2 and the third magnetic field B3 are orthogonal to each other, and the magnetic field amplitude B0 = |B1| = |B2| = |B3|; Based on the magnetic field measurement under the bias magnetic fields B1, B2 and B3, the NV corresponding to each diamond particle can be solved. － The axis of the color center, thus determining the NV during normal operation of the sample under test－ Vector projection change information of the magnetic field at the location of the color center.

[0017] Furthermore, the diamond NV － The color center position specifically includes: dividing the image into area A corresponding to the long-pass filter and area B corresponding to the neutral filter, area A is the area where fluorescence detection and positioning is required, and area B is the reference light area; for area B, taking the average value R of all pixel signals in area B as the reference light signal; for area A, setting the image processing unit area size to 5d×5d according to the diamond diameter d, and processing each unit area in area A at a step distance l; based on a given light intensity threshold S T Delineate the luminous area. If there is no fluorescent signal in the edge pixels of the processing unit area, it is determined that the unit contains NV. － Color center, if the edge pixel has a fluorescent signal, then determine whether its adjacent processing unit contains NV － Color center, finally, determine all the included NV － The image processing unit i of the color center records the maximum light intensity F in the luminous area mi , calculate the product coefficient k of the reference optical signal i =F mi / R.

[0018] Further, the microwave frequency is selected to perform a 4-point method to measure the changes in the magnetic field and temperature during the test phase of the sample to be tested, specifically including: selecting NV － Color center optical magnetic resonance spectrum corresponds to m s =-1, m s = +1, the microwave frequency corresponding to the maximum slope on both sides of the two resonance spectra is recorded as the first microwave frequency f a , the second microwave frequency f b , the third microwave frequency f c and the fourth microwave frequency f d , where m s For NV － The magnetic quantum number of the color center electron; the frequency difference between the two resonance spectra is 2γB, γ is the electron gyromagnetic ratio, when NV － When the color center senses the change of magnetic field, the two resonance peaks move in opposite directions. The first microwave frequency f a and the fourth microwave frequency f d The first signal contrast c corresponding to each a and the fourth signal contrast c d The change direction is consistent, the second microwave frequency f b and the third microwave frequency f c The second signal contrast c corresponding to each b Contrast with the third signal c c The change direction is consistent; when NV－ When the color center senses temperature changes, the two resonance peaks move in the same direction. The first microwave frequency f a and the third microwave frequency f c The first signal contrast c corresponding to each a and the third signal contrast c c The change direction is consistent, the second microwave frequency f b and the fourth microwave frequency f d The second signal contrast c of the corresponding signal b and the fourth signal contrast c d The direction of change is consistent; according to the first microwave frequency f a , the fourth microwave frequency f d , the second microwave frequency f b and the third microwave frequency f c The fluorescence changes are measured sequentially, and the first microwave frequency value f obtained by the previous measurement is combined a ', the fourth microwave frequency value f d ', the second microwave frequency value f b ' and the third microwave frequency value f c The corresponding fluorescence signals are subtracted in turn to obtain the first signal contrast difference δc a , the fourth signal contrast difference δc d , the second signal contrast difference δc b and the third signal contrast difference δc c , we can get the magnetic field change δB and temperature change δT, δB=[(δc a +δc d )-(δc b +δc c )]×k B ,δT=[(δc a +δc c )-(δc b +δc d )]×k T , where k B is the calibration coefficient corresponding to the magnetic field, k T is the calibration coefficient corresponding to temperature.

[0019] The technical solution of the present invention provides a method for preparing diamond-based thermal conductive optical adhesive. The method processes diamond micropowder and fully mixes the quantum-grade diamond micropowder thermal conductive filler into ultraviolet adhesive to obtain diamond-based thermal conductive optical adhesive. Since diamond is one of the materials with the highest thermal conductivity in nature, it can reach 1500-2200W / m·K, which is 4-5 times the thermal conductivity of other types of fillers such as silver. In theory, it can improve the thermal conductivity of the thermal conductive filling material. Based on artificial diamond particles, nitrogen-vacancy color centers are generated in the particles through irradiation, annealing and other technologies, and the negatively valenced nitrogen-vacancy (NV) in diamond is utilized. － ) color centers can achieve high-precision quantum sensing of physical quantities such as magnetic fields and temperature. At the same time, diamond particles themselves are not magnetic or conductive, but they are light-transmitting. When the chip is running, the diamond particles have little effect on it. If transparent optical glue is used as the matrix of the thermal conductive filling material, the effect on microscopic optical observation when it is applied to the chip is also limited. For large-scale rapid imaging detection based on diamond particles in the chip area, a wide-field imaging system can be used to use an optical camera to detect NV inside the diamond particles. － The optical signal of the color center can realize wide-field imaging of physical quantities such as magnetic field and temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The included drawings are used to provide a further understanding of the embodiments of the present invention, which constitute a part of the specification, are used to illustrate the embodiments of the present invention, and together with the text description, explain the principles of the present invention. Obviously, the drawings in the following description are only some embodiments of the present invention, and for ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0021] Figure 1 A flow chart of preparing a diamond-based thermally conductive optical adhesive according to a specific embodiment of the present invention is shown;

[0022] Figure 2 A schematic diagram of coating a sample to be tested with a diamond-based thermally conductive optical adhesive according to a specific embodiment of the present invention is shown;

[0023] Figure 3 A schematic diagram of a magnetic field / temperature wide-field imaging detection device based on a diamond-based thermally conductive optical adhesive provided according to a specific embodiment of the present invention is shown;

[0024] Figure 4 A schematic diagram of a sample to be tested and a microwave antenna provided according to a specific embodiment of the present invention is shown;

[0025] Figure 5a and Figure 5b A schematic diagram of a permanent magnet rotational translation stage provided according to a specific embodiment of the present invention is shown;

[0026] Figure 6 A schematic diagram of a dichroic mirror, a filter and an imaging area provided according to a specific embodiment of the present invention is shown;

[0027] Figure 7 A flow chart of a magnetic field / temperature wide-field imaging method provided according to a specific embodiment of the present invention is shown;

[0028] Figure 8 The method for determining the included NV according to a specific embodiment of the present invention is shown. － Schematic diagram of the image processing unit of the color center;

[0029] Fig. 9 A schematic diagram of optical magnetic resonance spectroscopy and 4-point magnetic field / temperature measurement provided according to a specific embodiment of the present invention is shown.

[0030] The above drawings include the following reference numerals:

[0031] 1. Optical camera; 2. Long-pass filter; 3. Neutral filter; 4. Dichroic combination spectrometer; 5. Lens group; 6. Excitation light source; 7. Objective lens; 8. First permanent magnet; 9. Second permanent magnet; 10. Sample to be tested; 11. Microwave antenna; 12. Sample test bench; 13. First horizontal translation stage; 14. Second horizontal translation stage; 15. Vertical rotation stage; 16. Vertical translation stage; 17. Horizontal rotation stage; 18. Base. DETAILED DESCRIPTION

[0032] like Figure 1 As shown, according to a specific embodiment of the present invention, a method for preparing a diamond-based thermal conductive optical adhesive is provided, and the method for preparing a diamond-based thermal conductive optical adhesive includes: step one, preparing diamond micropowder; step two, selecting whether to perform electron irradiation on the diamond micropowder or not according to the diameter specification of the diamond micropowder; if the diamond micropowder needs to be irradiated with electrons, then annealing the diamond micropowder after the electron irradiation; step three, judging whether there are impurities on the surface of the diamond micropowder, if there are impurities on the surface of the diamond micropowder, acid washing the annealed diamond micropowder; step four, performing a magnetic test on the diamond micropowder after the acid washing, if the magnetism of the diamond micropowder after the acid washing shows a magnetic field of the order of nT, demagnetizing the diamond micropowder; step five, drying the diamond micropowder to obtain a quantum-grade diamond micropowder thermal conductive filler; step six, fully mixing the quantum-grade diamond micropowder thermal conductive filler into the ultraviolet adhesive, and using ultrasonic vibration to fully disperse the diamond particles to obtain the diamond-based thermal conductive optical adhesive.

[0033] This configuration method is used to provide a method for preparing diamond-based thermal conductive optical adhesive. The method processes diamond micropowder and fully mixes the quantum-grade diamond micropowder thermal conductive filler into ultraviolet adhesive to obtain diamond-based thermal conductive optical adhesive. Diamond is one of the materials with the highest thermal conductivity in nature, which can reach 1500-2200W / m·K, which is 4-5 times the thermal conductivity of other types of fillers such as silver. In theory, it can improve the thermal conductivity of thermal conductive filling materials. Based on artificial diamond particles, nitrogen-vacancy color centers are generated in the particles through irradiation, annealing and other technologies, and the negatively valenced nitrogen-vacancy (NV) in diamond is used. － ) color centers can achieve high-precision quantum sensing of physical quantities such as magnetic fields and temperature. At the same time, diamond particles themselves are not magnetic or conductive, but they are light-transmitting. When the chip is running, the diamond particles have little effect on it. If transparent optical glue is used as the matrix of the thermal conductive filling material, the effect on microscopic optical observation when it is applied to the chip is also limited. For large-scale rapid imaging detection based on diamond particles in the chip area, a wide-field imaging system can be used to use an optical camera to detect NV inside the diamond particles. － The optical signal of the color center can realize wide-field imaging of physical quantities such as magnetic field and temperature. Therefore, the preparation method of diamond-based thermal conductive optical adhesive provided by the present invention can effectively solve the technical problem that various composite thermal conductive materials in the prior art usually only have thermal conductivity, no light transmittance, and no sensing characteristics, and cannot realize the detection of the chip operation magnetic field and temperature while improving the chip heat dissipation performance.

[0034] Furthermore, in the present invention, in order to form atomic vacancies in diamond particles so as to combine with nitrogen atoms in diamond to form NV － Color center, step 2 specifically includes: if the diameter specification of the diamond micropowder is nanometer-level diamond particles, the irradiation time of the diamond particles is less than 30 minutes, or no electron irradiation is performed; if the diameter specification of the diamond micropowder is micrometer-level diamond particles or the nitrogen concentration of the diamond micropowder is greater than 1ppm, the irradiation time of the diamond particles is not less than 30 minutes; if the irradiation time of the diamond micropowder exceeds 60 minutes, each 60 minutes is taken as a unit. After one electron irradiation unit, the diamond micropowder is taken out for annealing treatment, and then enters the next irradiation unit until the total irradiation time is completed.

[0035] As a specific embodiment of the present invention, the electron irradiation energy is 1MeV-10MeV, and the electron irradiation time is 0-300 minutes. Since electron irradiation generates a large amount of heat, in order to avoid overheating and causing diamond combustion and oxidation, the vessel containing diamond micropowder should be liquid-cooled. For nano-scale diamond particles, the irradiation time should be shorter (the time range is less than 30 minutes), or no irradiation, and only the vacancies of the diamond particles themselves can be used. For diamond particles with larger particle sizes (i.e., micron size specifications), a longer irradiation time (time range is greater than or equal to 30 minutes) should be used to fully generate vacancies. On the other hand, for diamond micropowders with higher nitrogen concentrations (nitrogen concentration range is greater than 1ppm), a longer irradiation time is used so that the number of vacancies is equivalent to the number of nitrogen atoms. For longer irradiation times, the diamond micropowder should be taken out for annealing treatment every 60 minutes as a unit, and then enter the next irradiation unit until the total time required for irradiation is completed.

[0036] Furthermore, in the present invention, in order to remove impurities such as oxides on the surface of diamond particles, the acid washing treatment of diamond powder specifically includes: preparing a washing solution by mixing 30% concentration of hydrogen peroxide and concentrated sulfuric acid, mixing the diamond powder into the washing solution, stirring evenly for full reaction, heating to a set temperature, and then standing until the diamond powder is fully precipitated; removing excess acid solution from the upper layer, adding a large amount of deionized water to the remaining mixture of diamond powder and acid solution, and slowly adding sodium bicarbonate to the solution for neutralization; standing the solution, removing excess solution after the diamond powder is precipitated, and then adding a large amount of deionized water, and repeating this process for a set number of times; if the particle size of the diamond particles is less than 1 micron, the step of standing and settling can be omitted in the cleaning process after removing the acid solution, and the mixed solution can be directly filtered to obtain diamond powder, and repeatedly washed several times.

[0037] In addition, in the present invention, in order to avoid the influence of magnetic impurities on the sample to be tested and the test signal, in step 4, the demagnetization treatment of the diamond powder specifically includes: adding diamond particles to anhydrous ethanol and mixing and stirring them fully, attaching a magnet to the bottom of the beaker containing the diamond-ethanol mixed solution, and placing the whole beaker in an ultrasonic cleaning machine water bath and oscillating it fully, so that the diamond particles containing magnetic substances are attracted to the bottom of the beaker by the magnet; after the diamond-ethanol mixed solution is fully oscillated for a set time in the ultrasonic cleaning machine, pausing the ultrasound and quickly transferring the upper mixed solution to another clean beaker, and then injecting anhydrous ethanol into the original beaker, oscillating it again to absorb the magnetic impurities for a set time, and then transferring the upper mixed solution after pausing the ultrasound, repeating this process until most of the non-magnetic diamond powder is transferred out, and finally filtering and evaporating the transferred mixed solution to obtain demagnetized diamond powder.

[0038] Furthermore, in the present invention, in order to avoid agglomeration of diamond powder in ultraviolet adhesive, in step six, the quantum-grade diamond powder thermal conductive filler is fully mixed into the ultraviolet adhesive, and the container sealed with the diamond-based thermal conductive adhesive mixture is placed in an ultrasonic water bath device, and ultrasonic vibration is used to fully disperse the diamond particles, and the ultrasonic water bath time is 15-30 minutes.

[0039] According to another aspect of the present invention, a magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive is provided. The diamond-based thermal conductive optical adhesive is prepared using the preparation method of the diamond-based thermal conductive optical adhesive as described above. The magnetic field and temperature wide-field imaging detection device is used to realize magnetic field and temperature wide-field imaging detection of a sample to be tested. The diamond-based thermal conductive optical adhesive is coated on the sample to be tested. The magnetic field and temperature wide-field imaging detection device includes a sample test bench, a microwave antenna, an objective lens, an optical camera, a light source assembly, a lens assembly, a dichroic combination spectroscope, a filter assembly, a first permanent magnet, a second permanent magnet and a rotational translation stage assembly. The sample test bench is used to install the sample to be tested. The sample test bench includes a three-dimensional electric translation stage that can carry the sample to be tested to realize three-dimensional displacement. The first permanent magnet, the second permanent magnet and the rotary translation stage assembly are used to provide a bias magnetic field for the sample to be tested. The first permanent magnet and the second permanent magnet are symmetrically installed on both sides of the sample to be tested to form a uniform magnetic field at the sample to be tested. The microwave antenna is used to generate a uniform microwave magnetic field in the sample to be tested area. The light emitted by the light source assembly passes through the lens group and is split by the dichroic combination spectroscope. One beam of light passes through the objective lens and is irradiated onto the sample to be tested. The other beam passes through the lens assembly and is irradiated into the optical camera. The objective lens is used to image the diamond-based thermal conductive optical glue coated on the surface of the sample to be tested. After the fluorescence generated by the NV-color center in the diamond particles enters the optical lens, it passes through the color separation component and the filter component, and the optical camera performs light intensity detection, and the magnetic field and temperature are calculated according to the light intensity.

[0040] This configuration is used to provide a wide-field imaging detection device for magnetic field and temperature based on diamond-based thermal conductive optical adhesive. Diamond-based thermal conductive optical adhesive is used as a composite thermal conductive material applied to the surface of the sample to be tested. The sample to be tested is placed in a bias magnetic field, and microwave signals are uniformly radiated to the sample to be tested. The microwave frequency is scanned, and the optical magnetic resonance spectrum of each diamond particle can be detected by the camera, thereby obtaining the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles. This method can be used for imaging the magnetic field and temperature generated by the sample during operation in sample testing.

[0041] Further, in the present invention, in order to enable a pair of permanent magnets to generate magnetic fields of different directions and sizes at the sample, the direction of the bias magnetic field is adjusted to achieve alignment of the magnetic field with different color center orientations. Specifically, the rotation translation stage assembly includes a first horizontal translation stage, a second horizontal translation stage, a vertical translation stage, a vertical rotation stage, a horizontal rotation stage and a base. The first permanent magnet is arranged on the first horizontal translation stage, and the first horizontal translation stage is used to drive the displacement of the first permanent magnet along the x direction. The second permanent magnet is arranged on the second horizontal translation stage, and the second horizontal translation stage is used to drive the displacement of the second permanent magnet along the x direction. The first horizontal translation stage and the second horizontal translation stage are arranged on the vertical rotation stage, and the vertical rotation stage is used to drive the rotation of the first permanent magnet and the second permanent magnet around the y axis. The vertical rotation stage is arranged on the vertical translation stage, and the vertical translation stage is used to drive the displacement of the first permanent magnet and the second permanent magnet along the z direction. The vertical translation stage is arranged on the horizontal rotation stage, and the horizontal rotation stage is used to drive the rotation of the first permanent magnet and the second permanent magnet around the z axis. The horizontal rotation stage is arranged on the base.

[0042] Furthermore, in the present invention, in order to satisfy the requirement that the reference light and the fluorescence signal are irradiated to different areas of the camera frame, the dichroic film in the dichroic combination beam splitter is divided into two areas, including a dichroic coating part and a depolarizing beam splitting part, the dichroic coating part reflects 510nm-570nm green light, and the wavelength of the transmitted light is >650nm; the depolarizing beam splitting coating part has a reflection-transmittance ratio of R / T=1; in order to achieve filtering in different areas, the filtering component includes a long-pass filter and a neutral filter, the starting wavelength of the long-pass filter is 650nm, the attenuation multiple of the neutral filter is 30dB-40dB, the neutral filter corresponds to the camera frame to receive the light intensity reference signal, and the long-pass filter corresponds to the camera frame to receive the diamond color center fluorescence signal.

[0043] According to another aspect of the present invention, a method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive is provided. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive uses the magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive as described above. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive comprises: irradiating a sample to be tested covered with diamond-based thermal conductive optical adhesive with green light, so that NV- color centers in quantum-level diamond particles generate red fluorescence, performing wide-field imaging of the sample to be tested by an optical camera, and obtaining NV- at different positions. The quantum information of the color center, the imaging area contains two parts, the first part is the excitation light intensity reference part, the second part is the fluorescence signal detection part, the excitation light intensity reference part is used to correct the measurement error caused by the fluorescence intensity being affected by the change of the excitation light intensity; the sample to be tested is placed in a bias magnetic field, and microwave signals are uniformly radiated to the sample to be tested. The microwave frequency range is about 2.6GHz-3.2GHz. By scanning the microwave frequency, the optical magnetic resonance spectrum of each diamond particle can be detected by the camera, thereby obtaining the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles.

[0044] This configuration method is used to provide a wide-field imaging detection method for magnetic field and temperature based on diamond-based thermal conductive optical adhesive. Diamond-based thermal conductive optical adhesive is used as a composite thermal conductive material applied to the surface of the sample to be tested. The sample to be tested is placed in a bias magnetic field, and microwave signals are uniformly radiated to the sample to be tested. The microwave frequency is scanned, and the optical magnetic resonance spectrum of each diamond particle can be detected by the camera, thereby obtaining the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles. This method can be used for imaging the magnetic field and temperature generated by the sample during operation in sample testing.

[0045] Furthermore, in the present invention, the optical magnetic resonance spectrum of each diamond particle is detected by a camera, thereby obtaining the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles. Specifically, the green excitation light is reflected by the dichroic combination beam splitter and irradiated onto the sample to be tested through the objective lens, and the NV-color centers in the diamond particles distributed on the sample to be tested emit fluorescence under the irradiation of the excitation light. The fluorescence is collected by the objective lens and then transmitted through the dichroic combination beam splitter, the long-pass filter and the neutral filter, and the image is obtained by the optical camera and processed to determine the diamond NV － The first magnetic field B1 is determined according to the distance and orientation between the first permanent magnet and the second permanent magnet, and the frequency is swept within the adjustable microwave frequency range. A frame of image is obtained at each frequency point, and each frame of image is processed. The specific processing method for each frame of image is: － The image processing unit i of the color center calculates the normalized signal s of its pixel with fluorescence signal i,j =Fi,j / (k i R), j is the serial number of the frame image, corresponding to the microwave frequency f j , F i,j is the light intensity of the i-th image processing unit of the j-th frame image, which can eliminate the noise introduced by the change of the excitation light intensity. i}={s i,j} j＝1,2,3… , calculated by histogram {s i}, calculate the signal contrast {c i}={s i / s0}, with {c i} is the ordinate, frequency f j As the vertical axis, the NV in image processing unit i can be plotted. － The optical magnetic resonance spectrum of the color center; Based on the optical magnetic resonance spectrum, the microwave frequency is selected to use the 4-point method to measure the changes in the magnetic field / temperature during the test phase of the test product, and the magnetic field change δB and temperature change δT are obtained through 4 frames of images; During the normal operation of the test sample, each NV is monitored by the 4-point method － The changes of magnetic field and temperature at the color center are measured to complete the measurement under the bias magnetic field B1; the operation of the sample to be tested is stopped, and the external magnetic field is changed to the second magnetic field B2 and the third magnetic field B3 in turn, and the above optical magnetic resonance spectrum measurement process is repeated to complete the measurement of the magnetic field and temperature changes during the normal operation of the sample under different bias magnetic fields. The first magnetic field B1, the second magnetic field B2 and the third magnetic field B3 are orthogonal to each other, and the magnetic field amplitude B0 = |B1| = |B2| = |B3|; Based on the magnetic field measurement under the bias magnetic fields B1, B2 and B3, the NV corresponding to each diamond particle can be solved. － The axis of the color center, thus determining the NV during normal operation of the sample under test － Vector projection change information of the magnetic field at the location of the color center.

[0046] Furthermore, in the present invention, the diamond NV is determined － The color center position specifically includes: dividing the image into area A corresponding to the long-pass filter and area B corresponding to the neutral filter, area A is the area where fluorescence detection and positioning is required, and area B is the reference light area; for area B, taking the average value R of all pixel signals in area B as the reference light signal; for area A, setting the image processing unit area size to 5d×5d according to the diamond diameter d, and processing each unit area in area A at a step distance l; based on a given light intensity threshold S T Delineate the luminous area. If there is no fluorescent signal in the edge pixels of the processing unit area, it is determined that the unit contains NV. － Color center, if the edge pixel has a fluorescent signal, then determine whether its adjacent processing unit contains NV －Color center, finally, determine all the included NV － The image processing unit i of the color center records the maximum light intensity F in the luminous area mi , calculate the product coefficient k of the reference optical signal i =F mi / R.

[0047] Further, the microwave frequency is selected to perform a 4-point method to measure the changes in the magnetic field and temperature during the test phase of the sample to be tested, specifically including: selecting NV － Color center optical magnetic resonance spectrum corresponds to m s =-1, m s = +1, the microwave frequency corresponding to the maximum slope on both sides of the two resonance spectra is recorded as the first microwave frequency f a , the second microwave frequency f b , the third microwave frequency f c and the fourth microwave frequency f d , where m s For NV － The magnetic quantum number of the color center electron; the frequency difference between the two resonance spectra is 2γB, γ is the electron gyromagnetic ratio, when NV － When the color center senses the change of magnetic field, the two resonance peaks move in opposite directions. The first microwave frequency f a and the fourth microwave frequency f d The first signal contrast c corresponding to each a and the fourth signal contrast c d The change direction is consistent, the second microwave frequency f b and the third microwave frequency f c The second signal contrast c corresponding to each b Contrast with the third signal c c The change direction is consistent; when NV － When the color center senses temperature changes, the two resonance peaks move in the same direction. The first microwave frequency f a and the third microwave frequency f c The first signal contrast c corresponding to each a and the third signal contrast c c The change direction is consistent, the second microwave frequency f b and the fourth microwave frequency f d The second signal contrast c of the corresponding signal b and the fourth signal contrast c d The direction of change is consistent; according to the first microwave frequency f a , the fourth microwave frequency f d , the second microwave frequency f b and the third microwave frequency f cThe fluorescence changes are measured sequentially, and the first microwave frequency value f obtained by the previous measurement is combined a ', the fourth microwave frequency value f d ', the second microwave frequency value f b ' and the third microwave frequency value f c The corresponding fluorescence signals are subtracted in turn to obtain the first signal contrast difference δc a , the fourth signal contrast difference δc d , the second signal contrast difference δc b and the third signal contrast difference δc c , we can get the magnetic field change δB and temperature change δT, δB=[(δc a +δc d )-(δc b +δc c )]×k B ,δT=[(δc a +δc c )-(δc b +δc d )]×k T , where k B is the calibration coefficient corresponding to the magnetic field, k T is the calibration coefficient corresponding to temperature, δc a＝ c a -c a ',δc d＝ c d -c d ',δc b =c b -c b ',δc c＝ c c -c c ',c a ' is the previous value of the first signal contrast, c d ' is the fourth signal contrast value before, c b ' is the previous value of the second signal contrast, c c ' is the previous value of the third signal contrast.

[0048] In order to further understand the present invention, the following Figures 1 to 9 The preparation method of the diamond-based thermal conductive optical adhesive provided by the present invention, and the magnetic field and temperature wide-field imaging detection equipment and method based on the diamond-based thermal conductive optical adhesive are described in detail.

[0049] like Figures 1 to 9As shown, the present invention provides a preparation of diamond-based thermal conductive optical adhesive, magnetic field / temperature wide-field imaging detection equipment and method. The diamond-based thermal conductive optical adhesive can be used as a composite thermal conductive material applied to the surface of the chip to improve the heat dissipation performance of the chip. At the same time, it can be used for imaging the magnetic field and temperature generated by the chip during operation during chip testing.

[0050] A first aspect of an embodiment of the present application provides a diamond-based thermally conductive optical adhesive composite thermally conductive material, comprising: a quantum-grade diamond micro-powder thermally conductive filler and an optical adhesive matrix.

[0051] The quantum-grade diamond micropowder thermal conductive filler is obtained by irradiating, annealing, pickling, demagnetizing, drying and other processes of nano-micron-scale diamond micropowder. The diamond micro-nano particles contain NV － Diamond micro powder material with color center.

[0052] The diameter of the diamond micropowder particles is between 50nm and 10μm, usually including 50nm, 100nm, 200nm, 500nm, 1μm, 1.5μm, 2.5μm, 3.5μm, 5μm, 7μm, 10μm and other diameter specifications. In the specific embodiment, the same diameter specification should be used to prepare the thermal conductive filler. Diamond particles with larger particle sizes have higher thermal conductivity, but the spatial resolution of magnetic / thermal imaging is poor, and are used in scenarios with high requirements for heat dissipation but low requirements for imaging resolution; nano-scale diamond particles can achieve extremely high spatial resolution magnetic / thermal imaging, and compared with large-diameter diamond particles, they can increase the rheological properties and stability of thermal conductive optical adhesive materials. On the other hand, it may cause larger gaps between thermal conductive fillers and reduce thermal conductivity, but low thermal conductivity is also conducive to the realization of local thermal imaging.

[0053] The nitrogen content of the diamond micropowder particles should be below 50ppm and higher than 1ppm. The lower the nitrogen content, the more conducive it is to improving the thermal conductivity; the higher the nitrogen content, the more conducive it is to forming sufficient NV － Lustful heart.

[0054] The diamond powder is irradiated with electrons to form atomic vacancies in the diamond particles so as to combine with nitrogen atoms in the diamond to form NV. －Color center. The electron irradiation energy is 1MeV-10MeV, and the electron irradiation time is 30-300 minutes. Since electron irradiation generates a lot of heat, in order to avoid overheating and causing diamond combustion and oxidation, the container containing diamond micropowder should be liquid cooled. For nano-scale diamond particles, the irradiation time should be shorter (the time range is less than 30 minutes) or no irradiation (if electron irradiation is not performed, no subsequent annealing treatment is required), and only the vacancies of the diamond particles themselves can be used. For diamond particles with larger particle sizes (i.e., micron size specifications), a longer irradiation time (the time range is not less than 30 minutes) should be used to fully generate vacancies. On the other hand, for diamond micropowders with higher nitrogen concentrations (concentration range greater than 1ppm), a longer irradiation time is used so that the number of vacancies is equivalent to the number of nitrogen atoms. For longer irradiation times, the diamond micropowder should be taken out for annealing every 60 minutes as a unit, and then enter the next irradiation unit until the total time required for irradiation is completed.

[0055] The annealing treatment of the diamond powder is used to migrate the vacancies in the diamond particles and combine with nitrogen atoms to form NV － Color center. Use vacuum tube furnace, vacuum degree is 10 -5 mbar, uniformly heat to 800℃-900℃, keep the temperature stable for 60 minutes, stop heating, let the diamond powder cool naturally to room temperature. Take out the diamond powder and irradiate it again or proceed to the next step.

[0056] The acid washing treatment of the diamond powder is used to remove impurities such as oxides on the surface of the diamond particles. Before acid washing, the diamond powder can be observed under a microscope to see if it contains impurities. If there are no impurities, this step can be omitted. A washing solution is prepared by mixing 30% hydrogen peroxide and concentrated sulfuric acid, and the diamond powder is mixed into the washing solution, stirred evenly and fully reacted, and then heated to 100°C appropriately, and then allowed to stand until the diamond powder is fully precipitated. Remove the excess acid solution from the upper layer as much as possible, add a large amount of deionized water to the remaining mixture of diamond powder and acid solution, and then slowly add sodium bicarbonate to the solution to neutralize it. The solution is allowed to stand, and after the diamond powder is precipitated, the excess solution is removed, and then a large amount of deionized water is added, and this process is repeated several times. For diamond particles with larger particle sizes (particle size range is greater than 1 micron), the step of standing and settling can be omitted in the cleaning process after removing the acid solution, and the mixed solution can be directly filtered to obtain diamond powder, and the diamond powder is repeatedly washed several times.

[0057] The demagnetization treatment of the diamond micropowder is used to remove diamond particles containing catalyst impurities such as nickel. Before the demagnetization step, a high-sensitivity magnetometer can be used to test the magnetic properties of the micropowder. If the micropowder exhibits a magnetic field of the order of nT, the magnetic impurities therein should be removed as much as possible to avoid affecting the chip to be tested and the test signal. The specific method of the demagnetization treatment is to add the diamond particles to anhydrous ethanol and mix and stir them thoroughly, attach a magnet to the bottom of the beaker containing the diamond ethanol mixture, and place the whole in an ultrasonic cleaning machine water bath and oscillate it sufficiently so that the diamond particles containing magnetic substances are attracted to the bottom of the beaker by the magnet. After the diamond ethanol mixed liquid is fully oscillated in an ultrasonic cleaning machine for 15-30 minutes, the ultrasound is paused and 30% of the upper mixed liquid is quickly transferred to another clean beaker, and then anhydrous ethanol is injected into the original beaker, and the magnetic impurities are absorbed again by oscillation for 15-30 minutes, and then 30% of the upper mixed liquid is transferred out after the ultrasound is paused. This process is repeated for no less than 5 times until more than 80% of the non-magnetic diamond powder is transferred out, and finally the transferred mixed liquid is filtered and evaporated to obtain demagnetized diamond micropowder.

[0058] The drying treatment of the diamond powder is used to remove water, ethanol and other components from the pure diamond powder obtained after the steps of pickling and demagnetization. The diamond powder can be placed in a tubular annealing furnace again for 10 -5 mbar vacuum is heated to 100℃-120℃ until no more water molecules are extracted. The diamond powder is taken out after cooling down and used as quantum grade diamond powder thermal conductive filler.

[0059] The optical adhesive matrix is ​​made of ultraviolet adhesive, such as NOA61 ultraviolet adhesive from Norland, which is easy to mix with the thermal conductive filler due to its low viscosity, and is pre-cured and cured under ultraviolet light.

[0060] The diamond-based thermally conductive optical adhesive is a composite thermally conductive material with certain thermal conductivity and quantum sensing performance obtained by fully mixing quantum-grade diamond micropowder thermal conductive filler into ultraviolet adhesive. Among them, the mass proportion of diamond micropowder is 10% to 80%. The higher the required thermal conductivity, the higher the filling mass proportion of diamond micropowder should be. When the filling amount of diamond micropowder is higher than 50%, agglomeration is prone to occur. The diamond micropowder should be fully dispersed in the optical adhesive before use.

[0061] The method for breaking up the diamond micropowder in the diamond-based thermal conductive optical adhesive is to place a container sealed with the diamond-based thermal conductive optical adhesive mixture in an ultrasonic water bath device, and use ultrasonic vibration to fully break up the diamond particles. The ultrasonic water bath time is 15-30 minutes. Due to gravity, the concentration of diamond micropowder in the lower part of the container is higher than that in the upper part. After the ultrasonic water bath ends, the diamond optical adhesive mixture in the lower middle part of the container is quickly taken out and spin-coated on the chip to be tested, so that the diamond particles are distributed as evenly as possible on the object to be tested.

[0062] A second aspect of the present application provides a magnetic field / temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive. The detection device is as follows: Figure 3 , Figure 4 As shown, it is composed of a sample test table 12, a microwave antenna 11, an objective lens 7, an optical camera 1, an excitation light source 6, a lens group 5, a dichroic mirror 4, a filter 2, a first permanent magnet 8, a second permanent magnet 9 and a rotational displacement stage assembly. The rotational displacement stage assembly is shown in FIG5 , and includes a first horizontal displacement stage 13 and a second horizontal displacement stage 14, which are used to achieve the x-direction displacement of the first permanent magnet 8 and the second permanent magnet 9; a vertical displacement stage 16, which is used to achieve the z-direction displacement of the permanent magnet; a vertical rotation stage 15, which is used to achieve the rotation of the permanent magnet around the y-axis; a horizontal rotation stage 17, which is used to achieve the rotation of the permanent magnet around the z-axis; and a base 18.

[0063] The sample test table 12 is used to install or hold the chip sample to be tested, and can realize the power-on test function of the chip. The chip sample is coated with the diamond-based thermal conductive optical glue. The test table includes a three-dimensional electric displacement table, which can carry the sample to be tested to achieve three-dimensional movement, so as to adjust the imaging area and imaging plane of the system.

[0064] The permanent magnet and its rotating stage are used to provide a bias magnetic field for the test sample. The permanent magnet is symmetrically installed on both sides of the test sample to form a uniform magnetic field at the sample, and the magnitude of the magnetic field is controlled to be about 10 Gauss. The rotating displacement stage assembly on which the permanent magnet is installed can realize a pair of permanent magnets to generate magnetic fields of different directions and magnitudes at the sample, and the magnetic field is aligned with different color center orientations by adjusting the direction of the bias magnetic field.

[0065] The microwave antenna 11 is a ring-shaped microwave coil, which is used to generate a uniform microwave magnetic field in the sample area to be tested. The microwave antenna is connected to the microwave signal by a coaxial cable, and the microwave signal is input through the coaxial cable.

[0066] The wavelength range of the light emitted by the excitation light source is 510nm-570nm green light. In one embodiment, a laser light source is used, which is expanded by a lens group 5 and then reflected by a dichroic combination beam splitter 4 to irradiate the chip sample, so as to excite the NV of the diamond particles in the thermal conductive optical glue. －In another embodiment, a green LED light source is used, which is focused by a lens group 5 after being emitted and reflected by a dichroic combination beam splitter 4 before being irradiated onto the sample to be tested.

[0067] The dichroic film in the dichroic combined beam splitter 4 is divided into two areas, including a dichroic coating part and a depolarizing beam splitting part. The dichroic coating part reflects 510nm-570nm green light, and the wavelength of the transmitted light is greater than 650nm; the depolarizing beam splitting coating part has a reflection-transmission ratio R / T=1. This satisfies the requirement that the reference light and the fluorescent signal are irradiated to different areas of the camera frame.

[0068] The objective lens 7 is used to image the diamond-based thermal conductive optical glue coated on the surface of the sample to be tested, and is vertically aligned with the sample to be tested. The magnification of the objective lens 7 is determined by the size of the area to be tested. The larger the area to be tested, the smaller the required lens magnification should be. The imaging area corresponding to the camera frame should be included in the area where the diamond-based thermal conductive optical glue is coated on the sample to be tested. A color separation mirror 4 and a filter are installed between the lens and the camera.

[0069] The filter is a combination of a long-pass filter 2 and a neutral filter 3. The starting wavelength of the long-pass filter part is 650nm (the long-pass filter part corresponds to the dichroic coating part, i.e., area A); the attenuation multiple of the neutral filter part is about 30dB-40dB (the neutral filter part corresponds to the depolarization splitting part, i.e., area B), corresponding to different areas of the camera frame. The neutral filter part corresponds to the camera frame to receive the light intensity reference signal, and the long-pass filter part corresponds to the camera frame to receive the diamond color center fluorescence signal.

[0070] The optical camera 1 can be a CCD camera or a CMOS camera. For applications with higher measurement sensitivity requirements, a CCD camera should be used to obtain a higher signal-to-noise ratio, and an EMCCD camera can be used to achieve single-photon level fluorescence signal detection; for applications with higher time resolution requirements, a CMOS camera should be used to obtain a higher image acquisition speed.

[0071] The diamond particles in the diamond-based thermal conductive optical adhesive are coated on the sample to be tested, and the NV in the diamond particles － After the fluorescence generated by the color center enters the optical lens, it passes through the dichroic mirror 4, the long-pass filter 2 and the neutral filter 3, and the optical camera 1 performs light intensity detection, and the magnetic field and temperature are calculated through the light intensity signal.

[0072] Based on the detection device described in the embodiments of the present application, a third aspect of the embodiments of the present application provides a magnetic field / temperature wide-field imaging method based on diamond-based thermally conductive optical glue. The method is applied to the sensing test of the magnetic field / temperature generated during the operation of the chip. In the embodiments of the present application, the newly prepared diamond-based thermally conductive optical glue is quickly spin-coated on the chip to be tested. A relatively large amount of glue liquid is required during spin-coating to facilitate the full flow of the glue liquid containing diamond micropowder. The film thickness of the glue liquid is controlled by the rotation speed. When the particle size of the diamond particles is d, the film thickness h of the glue liquid should satisfy 1.1d < h < 1.9d to ensure that only one diamond particle is contained at different positions in the film layer.

[0073] The chip to be tested in the embodiments of the present application can also be other components or materials, which are characterized by the need for heat exchange with the outside world, the presence of special-shaped structures that are difficult to fully contact with the heat dissipation plane, and the need to achieve high-spatial-resolution magnetic field or temperature measurement.

[0074] After the spin-coating of the thermally conductive glue film layer in the embodiments of the present application is completed, pre-curing should be carried out. One method of pre-curing is to use a 100-watt mercury lamp to irradiate at a distance of 6 inches from the glue layer for 10 seconds. After the pre-curing is completed, the magnetic field / temperature measurement can be carried out. If the thermally conductive optical glue is not required in subsequent use, it can be quickly removed with solvents such as methylene chloride. If the thermally conductive optical glue is required, the magnetic field / temperature measurement can be carried out after the curing is completed.

[0075] After the test of the fully cured chip is completed, the heat dissipation element can be further installed. The plane formed by the thermally conductive optical glue is in full contact with other heat dissipation materials or components to achieve a better heat dissipation effect.

[0076] The magnetic field / temperature wide-field imaging method is as follows: The chip element coated with diamond-based thermally conductive optical glue is irradiated with green light. The NV － color centers in the quantum-level diamond particles will generate red fluorescence. The chip element is imaged in a wide field by an optical camera 1 to obtain the quantum information of the NV － color centers at different positions. The imaging area includes two parts. The first part is the excitation light intensity reference part, and the second part is the fluorescence signal detection part. The excitation light intensity reference part is used to correct the measurement error caused by the change in the fluorescence intensity affected by the excitation light intensity.

[0077] The chip element to be tested is placed in a bias magnetic field, and a microwave signal is uniformly radiated to the chip element. The microwave frequency range is about 2.6 GHz - 3.2 GHz. By scanning the microwave frequency, the electron paramagnetic resonance spectrum of each diamond particle can be detected by the camera, so as to obtain the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles.

[0078] The process of the magnetic field / temperature wide-field imaging method is as Figure 7The specific method is as follows. First, the position of the diamond is determined. The green excitation light (in other embodiments, it can also be a green LED light source) is reflected by the dichroic mirror 4 and then irradiated onto the sample to be tested through the objective lens 7. The NV in the diamond particles distributed on the sample to be tested － The color center emits fluorescence under the irradiation of the excitation light. The fluorescence is collected by the objective lens and then transmitted through the dichroic mirror 4, the long-pass filter 2 and the neutral filter 3. The optical camera detects and obtains the image and processes it. The image obtained should be the average of several images with a sufficiently long exposure time to maximize the signal-to-noise ratio.

[0079] Specific Diamond NV － The processing method for determining the color center position is to divide the image into area A corresponding to the long-pass filter 2 and area B corresponding to the neutral filter 3. Area A is the area where fluorescence detection and positioning is required, and area B is the reference light area. For area B, the average value R of all pixel signals in area B is taken as the reference light signal. For area A, the image processing unit area size is set to 5d×5d according to the diamond diameter d, and the processing is performed unit by unit area in area A at a step distance l. The processing method for the image processing unit is based on a given light intensity threshold S T Delineate the luminous area (i.e., if the pixel luminous intensity is greater than or equal to the light intensity threshold, it is considered that there is a fluorescent signal). If there is no fluorescent signal in the edge pixels of the processing unit area, it is determined that the unit contains NV. － Color center, if the edge pixel has a fluorescent signal, then determine whether its adjacent processing unit contains NV － Color center, such as Figure 8 Finally, all the NV － The image processing unit i of the color center records the maximum light intensity F in the luminous area mi , calculate the product coefficient k of the reference optical signal i =F mi / R, R is the average value of all pixel signals in area B.

[0080] Determine the NV in the image － After the color center distribution position is determined, the optical magnetic resonance spectrum test is performed. The specific method is to determine the magnetic field B1 by the distance and orientation of the permanent magnet, sweep the frequency within the adjustable microwave frequency range, and obtain a frame of image at each frequency point. The specific processing method for each frame of image is to － The image processing unit i of the color center calculates the normalized signal s of its pixel with fluorescence signal i,j =F i,j / (k i R), j is the serial number of the frame image, corresponding to the microwave frequency f j , F i,jis the light intensity of the i-th image processing unit of the j-th frame image, which can eliminate the noise introduced by the change of the excitation light intensity. i}={s i,j} j＝1,2,3… , calculated by histogram {s i}, calculate the signal contrast {c i}={s i / s0}, with {c i} is the ordinate, frequency f j As the vertical axis, the NV in image processing unit i can be plotted. － The optical magnetic resonance spectrum of the color center (i.e. Fig. 9 ). Based on the optical magnetic resonance spectrum, the microwave frequency is selected to perform a 4-point method to measure the change of magnetic field / temperature during the test phase of the product under test, such as Fig. 9 shown.

[0081] The 4-point magnetic field / temperature measurement method is to select NV － Color center optical magnetic resonance spectrum corresponds to m s =-1, m s =+1(m s For NV － The microwave frequency corresponding to the maximum slope of the two resonance spectra of the color center electron) is denoted as f a 、f b 、f c 、f d . By NV － The quantum precision measurement characteristics of the color center show that the two resonance spectra are symmetrical about the frequency D corresponding to the zero-field splitting energy, which is about 2.87 GHz at room temperature; the frequency difference between the two resonance spectra is 2γB, where γ is the electron gyromagnetic ratio, which is about 28 Hz / nT. － When the magnetic field felt by the color center changes, the two resonance peaks move in opposite directions, f a With f d The corresponding signal c a 、c d The change direction is consistent, f b With f c The corresponding signal c b 、c c The change direction is consistent; when NV － When the temperature changes felt by the color center, the two resonance peaks move in the same direction, f a With f c The corresponding signal c a 、c c The change direction is consistent, f b With f d The corresponding signal c b 、cd The change direction is consistent. Therefore, according to f a 、f d 、f b 、f c The fluorescence changes are measured sequentially, and the binding pre-value is obtained as δc a ,δc d ,δc b ,δc c , we can get the changes of magnetic field and temperature.

[0082] δB=[(δc a +δc d )-(δc b +δc c )]×k B

[0083] δT=[(δc a +δc c )-(δc b +δc d )]×k T

[0084] This method obtains the changes of magnetic field and temperature through 4 frames of images, k B is the calibration coefficient corresponding to the magnetic field, k T is the calibration coefficient corresponding to temperature.

[0085] The microwave frequency f i It can be a single frequency, and in some embodiments, it represents a frequency including f i 、f i ±f hpl Three frequencies of microwave signals, among which f hpl Corresponding to NV － The electron spin and 14 Hyperfine interaction of N nuclear spins, about 2.16MHz.

[0086] Each NV is monitored by a 4-point method during normal operation of the test sample － The changes in magnetic field and temperature at the color center complete the measurement under the bias magnetic field B1 condition.

[0087] Stop the operation of the sample to be tested, change the external magnetic field to B2 and B3 in turn, repeat the above optical magnetic resonance spectrum measurement process, and complete the measurement of magnetic field and temperature changes during normal operation of the sample under different bias magnetic fields. The B1, B2, and B3 are mutually orthogonal, |B1|=|B2|=|B3|=B0, and the magnetic field amplitude is about 10G.

[0088] Based on the magnetic field measurement under the bias magnetic fields B1, B2, and B3, the NV corresponding to each diamond particle can be calculated. －The axis of the color center can determine the direction of the projection of the magnetic field change during the operation of the sample to be tested. According to the resonance peak position f of the measured optical magnetic resonance spectrum － 、f + , the projection size of the bias magnetic field on the NV axis can be calculated, and the calculation method is B p =(f + -f － ) / 2γ, the three projection sizes are calculated to be B 1p , B 2p , B 3p , then in the coordinate system composed of (B1, B2, B3), NV － The unit vector about the color center axis is denoted as (B 1p ,B 2p ,B 3p ) / B0, thus we can get NV during the normal operation test of the sample to be tested － Vector projection change information of the magnetic field at the location of the color center.

[0089] In summary, the present invention provides a method and device for preparing diamond-based thermal conductive optical adhesive, detecting a wide field of magnetic field and temperature, which can improve the heat dissipation performance of the chip by using the diamond-based thermal conductive optical adhesive as a composite thermal conductive material applied to the surface of the chip, and can also be used for imaging the magnetic field and temperature generated when the chip is running during chip testing. The method and device realize high spatial resolution quantum sensing based on diamond-based thermal conductive optical adhesive, meeting the needs of high-performance chips and various special-shaped structures for high thermal conductivity materials and the needs for high spatial resolution magnetic field / temperature detection.

[0090] For ease of description, spatially relative terms such as "above", "above", "on the upper surface of", "above", etc. may be used here to describe the spatial positional relationship between a device or feature and other devices or features as shown in the figure. It should be understood that spatially relative terms are intended to include different orientations of the device in use or operation in addition to the orientation described in the figure. For example, if the device in the accompanying drawings is inverted, the device described as "above other devices or structures" or "above other devices or structures" will be positioned as "below other devices or structures" or "below other devices or structures". Thus, the exemplary term "above" can include both "above" and "below". The device can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatially relative descriptions used here are interpreted accordingly.

[0091] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. If not otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the present invention.

[0092] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing a diamond-based thermally conductive optical adhesive, characterized in that: The preparation method of the diamond-based thermally conductive optical adhesive comprises: Step 1, prepare diamond powder; Step 2: According to the diameter specification of the diamond micropowder, the diamond micropowder is subjected to electron irradiation or not; if the diamond micropowder needs to be subjected to electron irradiation, the diamond micropowder is subjected to annealing treatment after the electron irradiation; Step 3, determining whether there are impurities on the surface of the diamond micropowder, if there are impurities on the surface of the diamond micropowder, performing pickling treatment on the annealed diamond micropowder; Step 4: Perform a magnetic test on the diamond powder after pickling. If the magnetism of the diamond powder after pickling shows a magnetic field of nT order, demagnetize the diamond powder. Step 5, drying the diamond micropowder to obtain quantum grade diamond micropowder thermal conductive filler; Step six, fully mix the quantum-grade diamond micro-powder thermal conductive filler into the ultraviolet adhesive, and use ultrasonic vibration to fully disperse the diamond particles to obtain the diamond-based thermal conductive optical adhesive.

2. The method for preparing the diamond-based thermally conductive optical adhesive according to claim 1, characterized in that: The step 2 specifically includes: if the diameter specification of the diamond micropowder is nano-scale diamond particles, the irradiation time of the diamond particles is less than 30 minutes, or no electron irradiation is performed; if the diameter specification of the diamond micropowder is micron-scale diamond particles or the nitrogen concentration of the diamond micropowder is greater than 1ppm, the irradiation time of the diamond particles is not less than 30 minutes; if the irradiation time of the diamond micropowder exceeds 60 minutes, each 60 minutes is taken as a unit, and after one electron irradiation unit, the diamond micropowder is taken out for annealing treatment, and then enters the next irradiation unit until the total irradiation time is completed.

3. The method for preparing the diamond-based thermally conductive optical adhesive according to claim 1, characterized in that: In the step 3, the diamond powder is subjected to acid washing treatment, which specifically includes: preparing a washing solution by mixing 30% concentration of hydrogen peroxide and concentrated sulfuric acid, mixing the diamond powder into the washing solution, stirring evenly for full reaction, heating to a set temperature, and then standing until the diamond powder is fully precipitated; removing excess acid solution from the upper layer, adding a large amount of deionized water to the remaining mixture of diamond powder and acid solution, and slowly adding sodium bicarbonate to the solution for neutralization; standing the solution, removing excess solution after the diamond powder is precipitated, and then adding a large amount of deionized water, and repeating this process for a set number of times; if the particle size of the diamond particles is less than 1 micron, the step of standing and settling can be omitted in the cleaning process after removing the acid solution, and the mixed solution can be directly filtered to obtain diamond powder, and the cleaning is repeated several times.

4. The method for preparing the diamond-based thermally conductive optical adhesive according to claim 3, characterized in that: In the step 4, the demagnetization treatment of the diamond powder specifically includes: adding diamond particles to anhydrous ethanol and mixing and stirring them fully, attaching a magnet to the bottom of a beaker containing the diamond-ethanol mixture, and placing the whole beaker in an ultrasonic cleaning machine water bath and oscillating it fully, so that the diamond particles containing magnetic substances are attracted to the bottom of the beaker by the magnet; after the diamond-ethanol mixture is fully oscillated in the ultrasonic cleaning machine for a set time, pausing the ultrasound and quickly transferring the upper layer of the mixture to another clean beaker, and then injecting anhydrous ethanol into the original beaker, oscillating it again to absorb magnetic impurities for a set time, and then transferring the upper layer of the mixture after pausing the ultrasound, repeating this process until most of the non-magnetic diamond powder is transferred out, and finally filtering and evaporating the transferred mixture to obtain demagnetized diamond powder.

5. The method for preparing the diamond-based thermally conductive optical adhesive according to claim 4, characterized in that: In step six, the quantum-grade diamond micro-powder thermal conductive filler is fully mixed into the ultraviolet adhesive, and the container sealed with the diamond-based thermal conductive optical adhesive mixture is placed in an ultrasonic water bath device, and the diamond particles are fully dispersed by ultrasonic vibration. The ultrasonic water bath time is 15-30 minutes.

6. A magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive, characterized in that: The diamond-based thermal conductive optical adhesive is prepared using the preparation method of the diamond-based thermal conductive optical adhesive as described in any one of claims 1 to 5; the magnetic field and temperature wide-field imaging detection equipment is used to realize magnetic field and temperature wide-field imaging detection of the sample to be tested; the diamond-based thermal conductive optical adhesive is coated on the sample to be tested; the magnetic field and temperature wide-field imaging detection equipment comprises a sample test bench, a microwave antenna, an objective lens, an optical camera, a light source assembly, a lens assembly, a dichroic combination spectroscope, a filter assembly, a first permanent magnet, a second permanent magnet and a rotational displacement stage assembly; the sample test bench is used to install the sample to be tested; the sample test bench comprises a three-dimensional electric displacement stage, which can carry the sample to be tested to achieve three-dimensional movement; the first permanent magnet, the second permanent magnet and the rotational displacement stage assembly The stage assembly is used to provide a bias magnetic field for the sample to be tested. The first permanent magnet and the second permanent magnet are symmetrically installed on both sides of the sample to be tested to form a uniform magnetic field at the sample to be tested. The microwave antenna is used to generate a uniform microwave magnetic field in the sample to be tested area. The light emitted by the light source assembly passes through the lens group and is split by the dichroic combination spectroscope. One beam of light passes through the objective lens and is irradiated onto the sample to be tested. The other beam passes through the lens assembly and is irradiated into the optical camera. The objective lens is used to image the diamond-based thermal conductive optical glue coated on the surface of the sample to be tested. After the fluorescence generated by the NV-color center in the diamond particles enters the optical lens, it passes through the color separation component and the filter component, and the optical camera performs light intensity detection, and the magnetic field and temperature are calculated according to the light intensity.

7. The magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive according to claim 6, characterized in that: The rotation translation stage assembly includes a first horizontal translation stage, a second horizontal translation stage, a vertical translation stage, a vertical rotation stage, a horizontal rotation stage and a base. The first permanent magnet is arranged on the first horizontal translation stage, and the first horizontal translation stage is used to drive the first permanent magnet to move along the x direction. The second permanent magnet is arranged on the second horizontal translation stage, and the second horizontal translation stage is used to drive the second permanent magnet to move along the x direction. The first horizontal translation stage and the second horizontal translation stage are arranged on the vertical rotation stage, and the vertical rotation stage is used to drive the first permanent magnet and the second permanent magnet to rotate around the y axis. The vertical rotation stage is arranged on the vertical translation stage, and the vertical translation stage is used to drive the first permanent magnet and the second permanent magnet to move along the z direction. The vertical translation stage is arranged on the horizontal rotation stage, and the horizontal rotation stage is used to drive the first permanent magnet and the second permanent magnet to rotate around the z axis. The horizontal rotation stage is arranged on the base.

8. The magnetic field and temperature wide-field imaging detection device based on diamond-based thermally conductive optical adhesive according to claim 7, characterized in that: The dichroic film in the dichroic combination beam splitter is divided into two areas, including a dichroic coating part and a depolarizing beam splitting part, the dichroic coating part reflects 510nm-570nm green light, and the transmitted light wavelength is>650nm; the depolarizing beam splitting coating part has a reflection-transmission ratio R / T=1; the filtering component includes a long-pass filter and a neutral filter, the starting wavelength of the long-pass filter is 650nm, the attenuation multiple of the neutral filter is 30dB-40dB, the neutral filter receives a light intensity reference signal corresponding to the camera frame, and the long-pass filter receives a diamond color center fluorescence signal corresponding to the camera frame.

9. A magnetic field and temperature wide-field imaging detection method based on diamond-based thermal conductive optical adhesive, characterized in that: The magnetic field and temperature wide-field imaging detection method based on diamond-based thermal conductive optical adhesive uses a magnetic field and temperature wide-field imaging detection device based on diamond-based thermal conductive optical adhesive as described in any one of claims 6 to 8, and the magnetic field and temperature wide-field imaging detection method based on diamond-based thermal conductive optical adhesive includes: Green light is used to irradiate the sample to be tested, which is coated with diamond-based thermal conductive optical adhesive. The NV-color center in the quantum-level diamond particles produces red fluorescence. The sample to be tested is imaged in a wide field by an optical camera to obtain the quantum information of the NV-color center at different positions. The imaging area includes two parts, the first part is the excitation light intensity reference part, and the second part is the fluorescence signal detection part. The excitation light intensity reference part is used to correct the measurement error caused by the change of the excitation light intensity. The sample to be tested is placed in a bias magnetic field, and microwave signals are uniformly radiated to the sample to be tested. The microwave frequency range is about 2.6GHz-3.2GHz. By scanning the microwave frequency, the optical magnetic resonance spectrum of each diamond particle can be detected by a camera, thereby obtaining the magnetic field information at the diamond particles and the temperature distribution at different positions of the diamond particles.

10. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermally conductive optical adhesive according to claim 9, characterized in that: The optical magnetic resonance spectrum of each diamond particle is detected by the camera, so as to obtain the magnetic field information at the diamond particle and the temperature distribution at different positions of the diamond particles, including: The green excitation light is reflected by the dichroic beam splitter and then irradiated onto the sample to be tested through the objective lens. The NV-color centers in the diamond particles distributed on the sample to be tested emit fluorescence under the irradiation of the excitation light. The fluorescence is collected by the objective lens and then transmitted through the dichroic beam splitter, long-pass filter and neutral filter. The image is detected by the optical camera and processed to determine the diamond NV － Color center position; The first magnetic field B1 is determined according to the distance and orientation between the first permanent magnet and the second permanent magnet, and the frequency is swept within the adjustable microwave frequency range. A frame of image is acquired at each frequency point, and each frame of image is processed. The specific processing method for each frame of image is as follows: － The image processing unit i of the color center calculates the normalized signal s of its pixel with fluorescence signal i,j =F i,j / (k i R), j is the serial number of the frame image, corresponding to the microwave frequency f j , F i,j is the light intensity of the i-th image processing unit of the j-th frame image, which can eliminate the noise introduced by the change of the excitation light intensity. i }={s i,j } j＝1,2,3… , calculated by histogram {s i }, calculate the signal contrast {c i }={s i / s0}, with {c i } is the ordinate, frequency f j As the vertical axis, the NV in image processing unit i can be plotted. － The optical magnetic resonance spectrum of the color center; based on the optical magnetic resonance spectrum, the microwave frequency is selected to use the 4-point method to measure the changes in the magnetic field and temperature during the test phase of the sample to be tested, and the magnetic field change δB and temperature change δT are obtained through 4 frames of images; Each NV is monitored by a 4-point method during normal operation of the test sample － The changes of magnetic field and temperature at the color center complete the measurement under the bias magnetic field B1 condition; Stop the operation of the sample to be tested, change the external magnetic field to the second magnetic field B2 and the third magnetic field B3 in turn, repeat the above optical magnetic resonance spectrum measurement process, and complete the measurement of the magnetic field and temperature changes during the normal operation of the sample under different bias magnetic fields, the first magnetic field B1, the second magnetic field B2 and the third magnetic field B3 are orthogonal to each other, and the magnetic field amplitude B0 = |B1| = |B2| = |B3|; Based on the magnetic field measurement under the bias magnetic fields B1, B2 and B3, the NV corresponding to each diamond particle can be calculated. － The axis of the color center, thus determining the NV during normal operation of the sample under test － Vector projection change information of the magnetic field at the location of the color center.

11. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermal conductive optical adhesive according to claim 10, characterized in that: Determine Diamond NV － The color center position specifically includes: dividing the image into area A corresponding to the long-pass filter and area B corresponding to the neutral filter, area A is the area where fluorescence detection and positioning is required, and area B is the reference light area; for area B, taking the average value R of all pixel signals in area B as the reference light signal; for area A, setting the image processing unit area size to 5d×5d according to the diamond diameter d, and processing each unit area in area A at a step distance l; based on a given light intensity threshold S T Delineate the luminous area. If there is no fluorescent signal in the edge pixels of the processing unit area, it is determined that the unit contains NV. － Color center, if the edge pixel has a fluorescent signal, then determine whether its adjacent processing unit contains NV － Color center, finally, determine all the included NV － The image processing unit i of the color center records the maximum light intensity F in the luminous area mi , calculate the product coefficient k of the reference optical signal i =F mi / R.

12. The method for wide-field imaging detection of magnetic field and temperature based on diamond-based thermally conductive optical adhesive according to claim 10, characterized in that: The changes of the magnetic field and temperature during the test phase of the sample to be tested are specifically selected by using the 4-point method to measure the microwave frequency: Select NV － Color center optical magnetic resonance spectrum corresponds to m s =-1, m s = +1, the microwave frequency corresponding to the maximum slope on both sides of the two resonance spectra is recorded as the first microwave frequency f a , the second microwave frequency f b , the third microwave frequency f c and the fourth microwave frequency f d , where m s For NV － The magnetic quantum number of the color center electron; the frequency difference between the two resonance spectra is 2γB, γ is the electron gyromagnetic ratio, when NV － When the color center senses the change of magnetic field, the two resonance peaks move in opposite directions. The first microwave frequency f a and the fourth microwave frequency f d The first signal contrast c corresponding to each a and the fourth signal contrast c d The change direction is consistent, the second microwave frequency f b and the third microwave frequency f c The second signal contrast c corresponding to each b Contrast with the third signal c c The change direction is consistent; when NV － When the color center senses temperature changes, the two resonance peaks move in the same direction. The first microwave frequency f a and the third microwave frequency f c The first signal contrast c corresponding to each a and the third signal contrast c c The change direction is consistent, the second microwave frequency f b and the fourth microwave frequency f d The second signal contrast c of the corresponding signal b and the fourth signal contrast c d The direction of change is consistent; according to the first microwave frequency f a , the fourth microwave frequency f d , the second microwave frequency f b and the third microwave frequency f c The fluorescence changes are measured sequentially, and the first microwave frequency value f obtained by the previous measurement is combined a ', the fourth microwave frequency value f d ', the second microwave frequency value f b ' and the third microwave frequency value f c The corresponding fluorescence signals are subtracted in turn to obtain the first signal contrast difference δc a , the fourth signal contrast difference δc d , the second signal contrast difference δc b and the third signal contrast difference δc c , we can get the magnetic field change δB and temperature change δT, δB=[(δc a +δc d )-(δc b +δc c )]×k B δT=[(δc a +δc c )-(δc b +δc d )]×k T Among them, k B is the calibration coefficient corresponding to the magnetic field, k T is the calibration coefficient corresponding to temperature.

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