Microwave maser and preparation method thereof

Abstract

The invention discloses a microwave maser and a preparation method thereof. The preparation method comprises the following steps: grinding 1, 3, 5-tri (1-naphthyl) benzene powder and derivative material powder based on anthracene as a main body to be fully mixed, filling a quartz glass tube with the mixture for deoxidizing, and sealing the glass tube after deoxidizing; the quartz glass tube is subjected to high-temperature oil bath, the material in the quartz glass tube forms a glassy-state microwave gain medium, the quartz glass tube is sealed under the anaerobic condition, and the microwave laser is obtained. The microwave laser can perform optical excitation energy induction on a device at room temperature to form a highly-spin-polarized triplet state, so that the microwave stimulated emission intensity is enhanced; and the preparation process is simple.

Description

Technical Field

[0001] The present invention relates to the field of microwave technology, and in particular to a microwave laser and a preparation method thereof. Background Art

[0002] Microwave Amplification by Stimulated Emission of Radiation (MASER) has many extraordinary properties, such as generating electromagnetic waves with a single frequency and extremely low noise. It is widely used in atomic clocks, astronomical research, chemical and medical diagnosis, etc.

[0003] The microwave maser is based on the principle of stimulated radiation amplification of the gain medium. Existing microwave masers are mainly divided into gas microwave masers and solid microwave masers according to the type of stimulated radiation gain medium. The gain medium of traditional solid microwave masers is now mostly ruby ​​crystals or other paramagnetic crystals, but because ruby ​​crystals have strict requirements on the environment, they need to work in an environment of extremely low temperature and strong magnetic field, which greatly limits their application. Summary of the invention

[0004] In order to overcome the above-mentioned shortcomings and deficiencies of the prior art, the object of the present invention is to provide a method for preparing a microwave laser. The prepared microwave laser can optically excite the device at room temperature, can induce the formation of a highly spin-polarized triplet state, and achieve enhanced microwave stimulated emission intensity; and the preparation process is simple.

[0005] Another object of the present invention is to provide a microwave laser that is small in size and easy to carry, store and use.

[0006] The purpose of the present invention is achieved through the following technical solutions:

[0007] The present invention provides a method for preparing a microwave maser, comprising the following steps:

[0008] The 1,3,5-tri(1-naphthyl)benzene powder and the anthracene-based derivative material powder are ground until fully mixed, placed in a quartz glass tube for deoxygenation, and the quartz glass tube is sealed after deoxygenation; the quartz glass tube is subjected to a high-temperature oil bath at 155° C. to 165° C., and the material in the quartz glass tube forms a glassy microwave gain medium; the quartz glass tube is sealed under oxygen-free conditions to obtain a microwave maser;

[0009] The anthracene-based derivative material has one of the following structures:

[0010]

[0011] Wherein, R is bromo, naphthyl, phenyl or phenylvinyl, and X is hydrogen, methyl or bromo.

[0012] Preferably, the anthracene-based derivative material is one of the following compounds:

[0013]

[0014] Preferably, the mass of the derivative material based on anthracene as the main component is 0.15-0.25% of the mass of 1,3,5-tri(1-naphthyl)benzene.

[0015] Preferably, the 1,3,5-tri(1-naphthyl)benzene powder and the anthracene-based derivative material powder are ground until fully mixed, specifically:

[0016] The 1,3,5-tri(1-naphthyl)benzene powder and the anthracene-based derivative material powder were put into an agate mortar and ground until the powders were fully mixed.

[0017] Preferably, the quartz glass tube is a nuclear magnetic resonance tube.

[0018] Preferably, the deoxygenation is specifically performed by placing the NMR tube in a glove box filled with nitrogen for 8 to 12 hours for deoxygenation.

[0019] Preferably, the glass tube is sealed, specifically by putting a balloon on the opening of the nuclear magnetic resonance tube in a glove box and sealing the opening with a sealing film.

[0020] Preferably, the sealing of the quartz glass under oxygen-free conditions is specifically: placing the nuclear magnetic tube in a glove box and squeezing ultraviolet glue to seal the tube opening of the nuclear magnetic tube, and using an ultraviolet lamp to irradiate to cure the ultraviolet glue.

[0021] The present invention also provides a microwave maser, which is prepared by the microwave maser preparation method.

[0022] Preferably, the microwave laser operates at room temperature.

[0023] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0024] (1) The preparation method of the microwave laser of the present invention can induce the formation of a highly spin-polarized triplet state by light excitation at room temperature, thereby enhancing the intensity of microwave stimulated emission.

[0025] (2) The preparation method of the microwave laser of the present invention has a simple preparation process for the microwave gain medium material, and the microwave gain material is in a glassy state, which makes the manufacturing process of the microwave laser also simpler.

[0026] (3) The microwave laser of the present invention is small in size and easy to carry, store and use. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the principle of generating spin polarization under light excitation induction in the microwave gain medium of an embodiment of the present invention.

[0028] Figure 2 This is the absorption and emission spectrum of the microwave laser of Example 1 of the present invention tested at room temperature.

[0029] Figure 3 This is the absorption and emission spectrum of the microwave laser of Example 2 of the present invention tested at room temperature.

[0030] Figure 4 This is the absorption and emission spectrum of the microwave laser of Example 3 of the present invention tested at room temperature.

[0031] Figure 5 This is the absorption and emission spectrum of the microwave laser of Example 4 of the present invention tested at room temperature.

[0032] Figure 6 This is the absorption and emission spectrum of the microwave laser of Example 5 of the present invention tested at room temperature.

[0033] Figure 7 This is the absorption and emission spectrum of the microwave laser of Example 6 of the present invention tested at room temperature.

[0034] Figure 8 This is the absorption and emission spectrum of the microwave laser of Example 7 of the present invention tested at room temperature. DETAILED DESCRIPTION

[0035] The present invention will be further described in detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.

[0036] Example 1

[0037] Weigh 1 mg of 9,10-dibromoanthracene (molecular weight 336.02 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% wt and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and put it in a glove box filled with nitrogen for one night for deoxygenation. Put a balloon on the nuclear magnetic tube in the glove box and seal the mouth with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0038] The molecular structure of 9,10-dibromoanthracene in this example is as follows:

[0039]

[0040] The molecular structure of 1,3,5-tri(1-naphthyl)benzene in this embodiment is as follows:

[0041]

[0042] Example 2

[0043] Weigh 1 mg of 2,6-dibromoanthracene (molecular weight 336.03 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% wt and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and place it in a glove box filled with nitrogen for one night for deoxygenation. In the glove box, put a balloon on the nuclear magnetic tube and seal the mouth with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0044] The molecular structure of 2,6-dibromoanthracene in this example is as follows:

[0045]

[0046] Example 3

[0047] Weigh 1 mg of 2,6-diphenylanthracene (molecular weight 330.43 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% wt and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and place it in a glove box filled with nitrogen for one night for deoxygenation. In the glove box, put a balloon on the nuclear magnetic tube and seal the mouth with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0048] The molecular structure of 2,6-diphenylanthracene in this embodiment is as follows:

[0049]

[0050] Example 4

[0051] Weigh 1 mg of 2,6-di(phenylvinyl)anthracene (molecular weight 382.5 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% wt and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and put it in a glove box filled with nitrogen for one night for deoxygenation. In the glove box, put a balloon on the nuclear magnetic tube and seal the mouth with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0052] The molecular structure of 2,6-di(phenylvinyl)anthracene in this embodiment is as follows:

[0053]

[0054] Example 5

[0055] Weigh 1 mg of 9,10-di(2-naphthyl)anthracene (molecular weight 430.54 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% wt and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and put it in a glove box filled with nitrogen for one night for deoxygenation. Put a balloon on the nuclear magnetic tube in the glove box and seal the mouth with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0056] The molecular structure of 9,10-di(2-naphthyl)anthracene in this example is as follows:

[0057]

[0058] Example 6

[0059] Weigh 1 mg of 2-methyl-9,10-di(2-naphthyl)anthracene (molecular weight 444.58 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% wt and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and put it in a glove box filled with nitrogen for one night for deoxygenation. In the glove box, put a balloon on the nuclear magnetic tube and seal the mouth with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0060] The molecular structure of 2-methyl-9,10-di(2-naphthyl)anthracene in this embodiment is as follows:

[0061]

[0062] Example 7

[0063] Weigh 1 mg of 2-bromo-9,10-dinaphthyl anthracene (molecular weight 509.45 g / mol) powder into an agate mortar, then weigh 500 mg of 1,3,5-tri(1-naphthyl)benzene (molecular weight 456.59 g / mol) at a ratio of 0.2% and grind into an agate mortar until the solid powder is fully mixed, put the solid powder into a 5 mm diameter nuclear magnetic tube, the powder height is about 2 cm, and put it in a glove box filled with nitrogen for one night for deoxygenation. Put a balloon on the nuclear magnetic tube in the glove box and seal the mouth of the tube with a sealing film, and put the nuclear magnetic tube in a high-temperature oil bath of about 160°C to form a uniform amorphous solid, that is, a glassy microwave gain medium. Put the nuclear magnetic tube in a glove box and squeeze 1-2 cm of ultraviolet glue to seal the nuclear magnetic tube, use an ultraviolet lamp to irradiate the ultraviolet glue to solidify it, and obtain a microwave laser.

[0064] The molecular structure of 2-bromo-9,10-dinaphthylanthracene in this example is as follows:

[0065]

[0066] In the above embodiment, the microwave gain medium in the microwave maser is mainly anthracene, and substituents are substituted at different positions, mainly including bromine, phenyl, methyl and naphthyl substituents, and the resulting derivative material is doped in 1,3,5-tri(1-naphthyl)benzene. The principle of the microwave gain medium of this embodiment to generate spin polarization under light excitation is as follows Figure 1As shown, under the excitation of short laser pulse light, anthracene derivatives transition from the S0 ground state singlet to the S1 excited singlet state, and then rapidly undergo intersystem crossing (ISC) to reach the excited triplet state under the action of spin-orbit coupling. During this period, the intersystem crossing causes spin-selective spin polarization between the triplet sub-energy levels, which is reflected in the different spin proportions on the three sub-energy levels (the number of black dots indicates the proportion).

[0067] The microwave lasers prepared in the above Examples 1 to 7 were tested by using electron paramagnetic resonance spectroscopy in pulse mode, using 355 nm wavelength light excitation, a laser frequency of 10 Hz, a laser energy of about 1 mJ, and a test temperature of room temperature.

[0068] The absorption and emission spectra of the microwave masers of Examples 1 to 7 obtained by testing are as follows: Figures 2 to 8 As shown in the figure, the microwave gain materials of the microwave masers of Examples 1 to 7 can all generate triplet states through intersystem crossing to enhance the microwave stimulated emission intensity. However, compared with the microwave masers of Examples 3 to 6, the microwave masers of Examples 1, 2, and 7 have higher signal intensity, smoother spectrum curves, and better signal-to-noise ratios, indicating that their intersystem crossing generates triplet states faster and has better performance.

[0069] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A method for preparing a microwave maser, characterized in that: The following steps are involved: The 1,3,5-tri(1-naphthyl)benzene powder and the anthracene-based derivative material powder are ground until fully mixed, placed in a quartz glass tube for deoxygenation, and the quartz glass tube is sealed after deoxygenation; the quartz glass tube is subjected to a high-temperature oil bath at 155° C. to 165° C., and the material in the quartz glass tube forms a glassy microwave gain medium; the quartz glass tube is sealed under oxygen-free conditions to obtain a microwave maser; The anthracene-based derivative material has one of the following structures: Wherein, R is bromo, naphthyl, phenyl or phenylvinyl, and X is hydrogen, methyl or bromo.

2. The method for preparing a microwave maser according to claim 1, characterized in that: The anthracene-based derivative material is one of the following compounds:

3. The method for preparing a microwave maser according to claim 1, characterized in that: The mass of the derivative material based on anthracene as the main component is 0.15 to 0.25% of the mass of 1,3,5-tri(1-naphthyl)benzene.

4. The method for preparing a microwave maser according to claim 1, characterized in that: The 1,3,5-tri(1-naphthyl)benzene powder and the anthracene-based derivative material powder are ground until fully mixed, specifically: The 1,3,5-tri(1-naphthyl)benzene powder and the anthracene-based derivative material powder were put into an agate mortar and ground until the powders were fully mixed.

5. The method for preparing a microwave maser according to claim 1, characterized in that: The quartz glass tube is a nuclear magnetic tube.

6. The method for preparing a microwave maser according to claim 5, characterized in that: The deoxygenation is specifically performed by placing the NMR tube in a glove box filled with nitrogen for 8 to 12 hours for deoxygenation.

7. The method for preparing a microwave maser according to claim 5, characterized in that: The glass tube is sealed by putting a balloon on the mouth of the nuclear magnetic resonance tube in a glove box and sealing the mouth with a sealing film.

8. The method for preparing a microwave maser according to claim 5, characterized in that: The method of sealing the quartz glass under oxygen-free conditions specifically comprises: placing the nuclear magnetic tube in a glove box, squeezing ultraviolet glue on the tube opening of the nuclear magnetic tube, and using an ultraviolet lamp to irradiate and solidify the ultraviolet glue.

9. A microwave maser, characterized in that: The microwave laser is prepared by the method for preparing the microwave laser according to any one of claims 1 to 8.

10. The microwave maser according to claim 9, characterized in that Its operating temperature is room temperature.

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