Equipment and method for dispersing and spraying nano-diamond on surface

Abstract

The invention relates to the field of electrohydrodynamic atomization technology and quantum physics, and discloses a device and method for dispersedly spraying nano-diamond on the surface, the device comprises a transmission module, a fixing module and a high-pressure module, the transmission module continuously supplies preparation liquid required for preparing a sample, controls the preparation speed of the sample and ensures the preparation effect; the fixing module is used for fixing the spraying head to realize stable spraying; the high-pressure module is used for releasing high pressure and applying the high pressure to the tip of the electrospray sample spray head to generate spray, the injector is rotationally pushed by the electric control rotary stepping motor, so that liquid in the injector flows to push the preparation liquid in the sample spray pipe, and the spraying speed of the preparation liquid of the sample spray head is regulated and controlled; under the combined action of high voltage and the vertical lifting displacement table, a layer of nano-diamond particles is sprayed on the surface of the sample carrier by utilizing an atomization spraying method, and the nano-diamond sample prepared by the spraying method of the equipment has the advantages of uniformity and dispersion.

Description

Technical Field

[0001] The invention relates to the field of electrohydrodynamic atomization technology and quantum physics, and in particular to a device and a method for surface dispersion spraying of nano-diamonds. Background Art

[0002] Suspended mesoscopic nanoparticles serve as a transition between classical and quantum systems. Compared with the degree of control over suspended macroscopic objects, their dynamics and environmental coupling can be highly controlled, and they have phonon energy levels. Compared with more microscopic systems such as atoms and ions, they have smaller de Broglie wavelengths and are expected to further improve sensing sensitivity when used for precision measurements. However, the first step in using them for quantum sensing is to achieve isolation from the external environment, that is, stable suspension of the particles.

[0003] For the suspension process of nanoparticles, the first step is to separate the nanoparticle sample from the planar carrier to which it is attached and to support it. However, since the particle sample attached to the surface of the planar carrier is affected by adhesion forces such as van der Waals force, capillary force and electrostatic force, the support process needs to first overcome the above forces. There are currently three commonly used methods, piezoelectric ceramic vibration method, spray method and pulse laser separation method. Among them, the piezoelectric ceramic vibration method is not suitable for particles below the micron level; the uncontrollable random process in the spray method will cause pollution of the vacuum cavity, which is not conducive to repeated experiments; the pulse laser separation method overcomes the adhesion effect by bombarding the carrier with a pulse laser to achieve support capture, and it is expected to realize the controllable support suspension and reuse of single particles.

[0004] Pulse laser initiation requires that the nanoparticles on the planar carrier are sufficiently uniform and dispersed. The particles in the planar carrier samples sprayed with traditional atomizers often appear clumped and unevenly distributed, which greatly reduces the success rate of initiation. At present, there is still a lack of a spraying device that can evenly disperse nanoparticles to achieve stable pulse laser initiation and repeated use.

[0005] The diamond nitrogen vacancy center (NV color center) is a luminescent point defect in the diamond structure. It has stable spin characteristics and can be used as a probe for optical detection magnetic resonance (ODMR) technology. For the diamond NV color center sample required for ODMR, a planar carrier sample of dispersed NV color center nanodiamond particles is also required to facilitate the acquisition of operational NV color centers.

[0006] To solve the above problems, people have been looking for a spraying technology solution. Summary of the invention

[0007] In view of the shortcomings of the prior art, the present invention provides an apparatus and method for surface dispersed spraying of nano-diamonds, which solves the problem that particles in planar carrier samples sprayed with traditional atomizers often agglomerate and are unevenly distributed, thereby reducing the success rate of support.

[0008] To achieve the above objectives, the present invention is implemented by the following technical solutions: a device for surface dispersion spraying of nano-diamonds, comprising:

[0009] The transmission module comprises a syringe placement platform with a syringe fixed on the upper part, an electrically controlled rotary stepping motor for pushing the syringe piston to eject the sample liquid is installed on one side of the top of the syringe placement platform, a liquid conduit is installed at the liquid outlet of the syringe, and one end of the liquid conduit is connected to the sample nozzle;

[0010] A fixing module, comprising a vertical lifting displacement platform, used to fix the sample nozzle in a spray environment component filled with nitrogen and enable it to move vertically, wherein a plastic piston is arranged inside the sample nozzle, a displacement knob is arranged on one side of the vertical lifting displacement platform, a sample nozzle is installed at the front end of the sample nozzle, a spray bracket is also installed on the moving platform of the vertical lifting displacement platform, the spray bracket comprises a plurality of threaded rods, and a plurality of the threaded rods are equipped with a grounding electrode through plastic nuts to form a fixed whole, a rubber-headed buffer screw is used above the spray bracket to align the sample nozzle with the center of the grounding electrode, the spray is sprayed downward, and the spray is sprayed downward on the surface of the sample carrier above the grounding electrode, and the distance between the sample nozzle and the grounding electrode is 15 mm to 20 mm;

[0011] A high voltage module is used to generate a high voltage of 5 kV to 10 kV, which is applied between the sample nozzle and the ground electrode to change the spray shape;

[0012] The liquid in the syringe is guided to the piston at the rear end of the sample nozzle through a liquid conduit, and the syringe is rotated and pushed by an electrically controlled rotary stepping motor to cause the internal liquid to flow to push the preparation liquid inside the sample nozzle, thereby realizing the regulation of the sample nozzle preparation liquid ejection speed. Under the joint action of high voltage electricity and a vertical lifting and displacement stage, a layer of nano-diamond particles is sprayed on the surface of the sample carrier by using an atomization spray method.

[0013] Preferably, the syringe placement platform is composed of three plastic blocks and two guide rails. The plastic blocks at both ends are used to fix the guide rails and the syringe. The output end of the electric-controlled rotary stepper motor is fixedly installed with a threaded column threadedly connected to the outer wall of the guide rail of the middle plastic block. The two guide rails are arranged on both sides of the middle plastic block.

[0014] Preferably, the sample nozzle is made of an insulating transparent plastic material, the front and rear ends of the nozzle are separated by a piston, the front end of the nozzle is equipped with a sample, and the rear end is connected to a syringe; the sample nozzle is made of a conductive stainless steel metal material, connected to the front end of the sample nozzle, and has an inner diameter of 0.35 mm; the grounding electrode is made of a conductive aluminum metal material, forming a small platform with a thickness of 2 mm 20 mm below the sample nozzle, and is grounded using a wire, and the ground wire is placed close to the outside of the spray environment component.

[0015] Preferably, the spray environment component is an acrylic box composed of five acrylic plates, and the sides have holes for entering the liquid conduit, the high-voltage line, the grounding line, and the nitrogen pipe.

[0016] A method for surface dispersion spraying of nano-diamonds, using the above-mentioned device for surface dispersion spraying of nano-diamonds, comprises the following method steps:

[0017] S1. Sample solution preparation: dilute 1 mg / ml nanodiamond stock solution with anhydrous ethanol to 0.025-0.1 mg / ml and then ultrasonically vibrate for 15-20 min;

[0018] S2, loading solution: inject the nano-diamond dilution after ultrasound into the front end of the sample nozzle and separate it from the rear end of the sample nozzle using a plastic piston, connect the rear end of the sample nozzle to a liquid conduit, connect the liquid conduit to a syringe, fill the syringe with anhydrous ethanol, then start the transmission module to fill the front end of the sample nozzle with the nano-diamond dilution;

[0019] S3. Sample carrier preset: Place the sample carrier to be sprayed on the upper part of the ground electrode, and adjust the distance between the ground electrode and the sample nozzle to 15mm-20mm. Then turn on the nitrogen, and use the nitrogen pipe to pass the nitrogen into the spray environment component through the side hole of the spray environment component for a period of time until the wooden stick with sparks cannot be rekindled at the hole. Then turn off the nitrogen and use plasticine to block the hole.

[0020] S4, test spraying: ground the fixed module, connect the high-voltage module to the fixed module, start the high-voltage module, adjust the voltage within 5kv-10kv, use a red laser light to illuminate the bottom of the sample nozzle (3), and stop when the spray is observed to be a stable single cone, and stop the high-voltage module;

[0021] S5. Start spraying: Use atomizing spray method, turn on the transmission module and the high-voltage module, control the spraying time, obtain a layer of nano-diamond coating, and complete the production of nano-diamond coating.

[0022] Preferably, in step S1, the steps of preparing the nano-diamond dilution solution specifically include:

[0023] First, a nano-diamond solution containing NV color centers with an average particle size of 40 nm and a concentration of 1 mg / ml is diluted to 0.025 mg / ml with anhydrous ethanol, and then the diluted suspension is placed in an ultrasonic device for ultrasonic oscillation treatment for 15 minutes to 20 minutes to obtain a nano-diamond diluted solution.

[0024] Preferably, in step S5, the atomization spray method is an electrohydrodynamic atomization method.

[0025] Preferably, the specific process of the electrohydrodynamic atomization method is: under the conditions of a flow rate of 3 ml / h and a voltage of 5 kv to 10 kv, the electrohydrodynamic atomization method is used, and the nano-diamond dilution liquid is decomposed into fine droplets under the influence of an external electric field and sprayed vertically downward in a cone shape onto the surface of the sample carrier above the ground electrode.

[0026] The invention provides a device and a method for surface dispersion spraying of nano-diamonds.

[0027] It has the following beneficial effects:

[0028] 1. The nano-diamond coating prepared by the present invention utilizes the characteristics of dispersed distribution of particles to provide sample materials for using pulsed laser to support in vacuum to achieve stable confinement of nano-particles in optical tweezers or ion traps, and also provides sample materials for stable ODMR detection.

[0029] 2. The dispersed nano-diamond coating prepared by the equipment and method provided by the present invention was subjected to SEM testing to analyze the spraying effect of the nano-diamond coating from three aspects: particle agglomeration, dispersion degree, and uniform distribution. A pulsed laser support test of mesoscopic particles suspended in an ion trap in a vacuum was also performed to achieve stable suspension of nano-diamond particles. At the same time, the nano-diamond coating prepared by the present invention was subjected to ODMR detection, and a suitable ODMR signal was successfully found.

[0030] 3. The equipment and method provided by the present invention, through the structure of the fixed module, cooperate with the optimal operation of the equipment, the selection of required items, and the equipment parameters, effectively improve the adaptation problem of voltage, spray size and particle size in the process of nanodiamond electrospray spraying, and stably realize the preparation of samples required for mesoscopic quantum sensing, and solve the problem that particles prepared by traditional atomization methods are easy to agglomerate, uneven, and cannot effectively disperse nanoparticles. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0032] Figure 2 It is a schematic diagram of the internal structure of the present invention;

[0033] Figure 3This is a schematic diagram of the overall structure of the fixed module in the present invention;

[0034] Figure 4 This is a schematic diagram of the internal structure of the syringe in the present invention;

[0035] Figure 5 It is a schematic diagram of the overall structure of the transmission module of the present invention;

[0036] Figure 6 It is the overall structure layout diagram and structure relationship diagram of the present invention;

[0037] Figure 7 The SEM results of the sample coating prepared by the device and method of the present invention;

[0038] Figure 8 A physical picture of the nano-diamond particles suspended in the vacuum ion trap as demonstrated by the experiment of the present invention;

[0039] Fig. 9 This is the ODMR detection result proved by the experiment of the present invention.

[0040] Among them, 1. vertical lifting platform; 2. sample nozzle; 3. sample nozzle; 4. ground electrode; 5. spray bracket; 6. syringe placement platform; 7. electric control rotary stepper motor; 8. displacement knob; 9. plastic piston; 10. rubber head buffer screw; 11. plastic nut; 12. threaded rod; 13. syringe; 14. threaded column; 15. guide rail; 16. liquid conduit; 17. spray environment components. DETAILED DESCRIPTION

[0041] The following will be combined with the drawings in the specification of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0042] Please refer to the attached Figure 1 -Attached Fig. 9 The present invention provides a device and method for surface dispersion spraying of nano-diamonds. The device comprises three main parts, namely a transmission module, a fixing module and a high-voltage module, wherein:

[0043] Please refer to the attached Figure 1 -Attached Figure 5As shown, the transmission module includes a syringe placement platform 6 with a syringe 13 fixed on the upper part, an electrically controlled rotary stepping motor 7 for pushing the syringe 13 piston to eject the sample liquid is installed on one side of the top of the syringe placement platform 6, a liquid conduit 16 is installed at the liquid outlet of the syringe 13, one end of the liquid conduit 16 is connected to a sample nozzle 2, the sample nozzle 2 is formed of at least one of vinyl chloride resin, polyphenylene sulfide resin, polyurethane resin, and polytetrafluoroethylene resin as an insulating material, the sample nozzle 2 stores nano-diamond diluent, the storage position is on the side close to the sample nozzle 3, and the nano-diamond diluent is separated from the rear end anhydrous ethanol propellant by a plastic piston 9;

[0044] In the above structure, the syringe placement platform 6 is composed of three plastic blocks and two guide rails 15. The plastic blocks at both ends are used to fix the guide rails 15 and the syringe 13. The output end of the electric-controlled rotary stepper motor 7 is fixedly installed with a threaded column 14 threadedly connected to the outer wall of the guide rail 15 of the middle plastic block. The two guide rails 15 are arranged on both sides of the middle plastic block.

[0045] The fixing module includes a vertical lifting displacement platform 1, which is used to fix the sample nozzle 2 in a spray environment component 17 filled with nitrogen and enable it to move vertically. A plastic piston 9 is arranged inside the sample nozzle 2. A displacement knob 8 is arranged on one side of the vertical lifting displacement platform 1. The knob has a scale for quantitative control and a measuring range of 200 mm. A sample nozzle 3 is installed at the front end of the sample nozzle 2. The sample nozzle 3 is a hollow cylindrical needle formed by a metal stainless steel conductor with a hollow inner diameter of 0.35 mm. The sample is squeezed from the sample nozzle 2 into the sample nozzle 3. A spray bracket 5 is also installed on the moving platform of the vertical lifting displacement platform 1. The spray bracket 5 includes a plurality of threaded rods 12, and the plurality of threaded rods 12 are equipped with a grounding electrode 4 through a plastic nut 11 to form a fixed whole. The grounding The electrode 4 is made of conductive aluminum metal, and a small platform with a thickness of 2 mm is formed 20 mm below the sample nozzle 3. There are three small holes for threading a threaded rod 12 for fixing. The electrode 4 is connected to the ground wire using a wire. The ground wire is extended with a copper braid to fit closely to the external spray environment component 17. The spray environment component 17 is a bottomless box composed of five acrylic plates. There are holes on the sides of the box to enter the liquid conduit 16, the high-voltage wire, the ground wire, and the nitrogen pipe. The liquid conduit 16 is made of PEEK material, one end of which is connected to the syringe 13 by a Luer male head, and the other end is connected to the sample nozzle 2 by an adapter. The ground electrode 4 is also used as a spray platform to place the sample carrier. A rubber-headed buffer screw 10 is used above the spray bracket 5 to align the sample nozzle 3 with the center of the ground electrode 4, and the spray is sprayed downward;

[0046] Specifically, the upper end of the spray bracket 5 is made of aluminum alloy, and three plastic threaded rods 12 are fixed at the lower end. The upper end is fixed to the vertical lifting platform 1, and is equipped with a rubber head buffer screw 10 for fixing the sample nozzle 2 to achieve the alignment of the sample nozzle 3. Six plastic nuts 11 are used at the lower end to fix the ground electrode 4 on the threaded rod 12. The distance between the sample nozzle 3 and the ground electrode 4 is 15mm to 20mm.

[0047] A high voltage module, which is used to generate a high voltage of 5 kV to 10 kV, and is applied between the sample nozzle 3 and the ground electrode 4 to generate a spray;

[0048] The basic working principle of the device is as follows: firstly, the sample carrier to be sprayed is placed on the upper part of the ground electrode 4, and at the same time, the distance between the ground electrode 4 and the sample nozzle 3 is adjusted. The propulsion liquid in the syringe 13 is guided to the piston at the rear end of the sample nozzle 2 through the liquid conduit 16. The syringe 13 is rotated and propelled by the electronically controlled rotary stepper motor 7 to make the internal liquid flow to push the preparation liquid inside the sample nozzle 2, so as to realize the regulation of the spraying speed of the preparation liquid of the sample nozzle 3. Then, the high voltage generated by the high-voltage module between the sample nozzle 3 and the ground electrode 4 is adjusted to adjust the spraying cone shape of the nano-diamond diluent, and a layer of nano-diamond particles is sprayed on the surface of the sample carrier by using the atomization spray method.

[0049] Furthermore, the present invention also provides a method for surface dispersion spraying of nano-diamonds, comprising the following method steps:

[0050] S1. Sample solution preparation: dilute the nanodiamond stock solution with anhydrous ethanol to 0.025 mg / ml and then ultrasonically vibrate for 15 min to 20 min;

[0051] S2, loading solution: inject the nano-diamond dilution after ultrasound into the front end of the sample nozzle 2 and separate it from the rear end of the sample nozzle 2 using a plastic piston 9, the rear end of the sample nozzle 2 is connected to a liquid conduit 16, the liquid conduit 16 is connected to a syringe 13, the inside of the syringe 13 is filled with anhydrous ethanol, and then the transmission module is started to fill the front end of the sample nozzle 2 with the nano-diamond dilution;

[0052] S3, sample carrier preset: place the sample carrier to be sprayed on the upper part of the ground electrode 4, and adjust the distance between the ground electrode 4 and the sample nozzle 3, the distance value is 15mm-20mm, then turn on the nitrogen, use the nitrogen pipe to pass the nitrogen into the spray environment component 17 through the side hole of the spray environment component 17 for a period of time, until the wooden stick with sparks cannot be rekindled at the hole, turn off the nitrogen, and use plasticine to block the hole;

[0053] S4, test spraying: ground the fixed module, connect the high-voltage module to the fixed module, start the high-voltage module, adjust the voltage within 5kv~10kv, use the red laser light to illuminate the sample nozzle 3, and observe that the spray sprayed from the sample nozzle 3 is a stable single cone, turn off the high-voltage power output, and stop running the high-voltage module;

[0054] S5. Start spraying: Use atomization spraying method, turn on the transmission module and the high-pressure module, so that the sample nozzle 3 sprays the surface of the sample carrier. After a certain period of time, a layer of nano-diamond coating is obtained on the surface of the sample carrier, and the production of the nano-diamond coating is completed.

[0055] The present invention will be further described below in conjunction with specific embodiments:

[0056] Embodiment 1:

[0057] This embodiment provides a method for surface dispersion spraying of nano-diamonds, using the above-mentioned device for surface dispersion spraying of nano-diamonds, specifically comprising the following steps:

[0058] S1. Dilute the original nanoparticle solution to 0.025 mg / ml with anhydrous ethanol solvent, separate the front and rear ends of the sample nozzle 2 with a plastic piston 9, and then put the prepared suspension into an ultrasonic machine for ultrasonic vibration for 15 min to 20 min to obtain a nanodiamond dilution solution;

[0059] S2. Use anhydrous ethanol to clean the syringe 13, liquid conduit 16, sample nozzle 2, sample nozzle head 3, and plastic piston 9. Use a Luer male connector to connect the syringe 13 and the liquid conduit 16. Then fill the syringe 13 and the liquid conduit 16 with anhydrous ethanol. Reset the position of the plastic block in the middle of the transmission module, fix the syringe 13, and inject to the front end of the sample nozzle 2. The other end of the liquid conduit 16 enters the fixed module from the side hole of the spray environment component 17. After the rear end of the sample nozzle 2 is filled with anhydrous ethanol, it is connected to the liquid conduit 16 entering the fixed module using an adapter. Start the electronically controlled rotary stepper motor 7 in the transmission module, adjust the propulsion flow rate to 3 ml / m, and pause the propulsion when liquid begins to flow out of the nozzle. Wipe the ground electrode 4 to keep the ground electrode 4 dry, and change the propulsion flow rate to 3 ml / h.

[0060] S3. If the sample is used for pulsed laser of vacuum suspended mesoscopic particles, use 0.3mm thick aluminum sheet as the plane carrier. If the sample is used for quantum sensing research of nanodiamond system, use 1mm thick glass slide as the plane carrier. Clamp the sample carrier to be sprayed, such as aluminum sheet or glass slide, with tweezers and directly send it to the ground electrode 4 under the sample nozzle 3. Align the geometric center of the plane carrier with the sample nozzle 3. Turn on the nitrogen. Use a nitrogen pipe to pass nitrogen through the side hole of the spray environment component 17 into the spray environment component 17 for a period of time until the wooden stick with sparks cannot be reignited at the hole. Turn off the nitrogen and use plasticine to block the hole.

[0061] S4, turn on the electronically controlled rotary stepper motor 7, set the voltage to 5kv and turn on the high voltage power supply, use a red laser light to observe the spray shape and slowly increase the voltage until the spray is observed to be a stable single cone jet, then stop increasing the voltage and turn off the high voltage power supply.

[0062] S5, turning on the high voltage and the stepping electrode 7 to start spraying, and controlling the spraying time as needed within 2 minutes to obtain a dispersed nano-diamond coating.

[0063] Embodiment 2:

[0064] Example 2 provides a method for preparing a nano-diamond coating, which is different from the method provided in Example 1 above in that:

[0065] The solvent used to dilute the nano-diamond stock solution is dichloromethane.

[0066] Since methylene chloride and anhydrous ethanol are immiscible, the front and rear ends of the sample nozzle 2 are not separated by a plastic piston 9 .

[0067] The nano-diamond coating prepared in Example 1 was subjected to SEM testing in the same manner as in Example 1. The test results showed that the nano-diamond coating prepared in Example 2 was more concentrated and had an irregular texture in its distribution.

[0068] Comparative test example 1:

[0069] Comparative Test Example 1 provides a method for preparing a nano-diamond coating, which is basically the same as the preparation method provided in Example 1, except that: Comparative Test 1 does not include the above-mentioned ultrasonic oscillation step, and the nano-diamond stock solution is directly added to the front end of the sample nozzle 2 after being diluted.

[0070] Comparative test example 2:

[0071] Comparative Test Example 2 provides a method for preparing a nano-diamond coating, which is basically the same as the method provided in Example 1, except that: Comparative Test 2 does not include the step of introducing nitrogen into the spray environment component 17 .

[0072] Comparative test example 3:

[0073] Comparative Test Example 3 provides a method for preparing a nano-diamond coating, which is basically the same as the method provided in Example 1, except that the ground wire connected to the ground electrode 4 in Comparative Test 3 is farther away from the fixed module.

[0074] Experiments have shown that: a scanning electron microscope was used to perform SEM testing on the dispersed nano-diamond coating prepared by the device and method provided by this embodiment, and the spraying effect of the nano-diamond coating was analyzed from three aspects: particle agglomeration, dispersion degree, and uniform distribution; a pulsed laser loading test of mesoscopic particles suspended in an ion trap in a vacuum was performed on the nano-diamond coating prepared by the device and method provided by the present invention; and an ODMR test was performed on the nano-diamond coating prepared by the device and method provided by the present invention.

[0075] The test results show that:

[0076] The nano-diamond coating particles obtained by comparative experiment 1 were severely agglomerated in the SEM image, the success rate of pulsed laser support in the vacuum ion trap was slightly reduced, and the detected ODMR signal was partially overexposed;

[0077] The nano-diamond coating particles obtained by comparative experiment 2 have uneven particle distribution in the SEM image, the success rate of pulsed laser support of the vacuum ion trap is reduced, and the detected ODMR signal is unstable;

[0078] The nano-diamond coating particles prepared by comparative experiment 3 have too dispersed particle spraying range in the SEM image, and the success rate of pulse laser support in vacuum ion trap is seriously reduced, and the ODMR signal is difficult to scan out;

[0079] like Figure 7 As shown in FIG. 1 , the nano-diamond coating particles prepared in Example 1 have no obvious agglomeration in the SEM image, and the dispersion degree is appropriate and the distribution is relatively uniform; Figure 8 As shown, the nano-diamond coating particles prepared in Example 1 have a high success rate in realizing pulsed laser support of an ion trap in a vacuum;

[0080] like Fig. 9 As shown, the nano-diamond coating particles prepared in Example 1 can detect obvious ODMR signals. It can be seen that the nano-diamond coating preparation method provided in Example 1 can significantly improve the spraying effect of dispersed nano-particles.

[0081] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A device for surface dispersion spraying of nano-diamonds, characterized in that: include: The transmission module comprises a syringe placement platform (6) on which a syringe (13) is fixed, an electrically controlled rotary stepping motor (7) for pushing the piston of the syringe (13) to eject the sample liquid is installed on one side of the top of the syringe placement platform (6), a liquid conduit (16) is installed at the liquid outlet of the syringe (13), and one end of the liquid conduit (16) is connected to the sample nozzle (2); A fixing module, comprising a vertical lifting displacement platform (1), used to fix a sample nozzle (2) in a spray environment component (17) filled with nitrogen and enable it to move vertically, wherein a plastic piston (9) is arranged inside the sample nozzle (2), a displacement knob (8) is arranged on one side of the vertical lifting displacement platform (1), a sample nozzle (3) is installed at the front end of the sample nozzle (2), and a spray bracket (5) is also installed on the moving platform of the vertical lifting displacement platform (1), wherein the spray bracket (5) comprises a plurality of threaded rods (12), and the plurality of threaded rods (12) are matched with a grounding electrode (4) through a plastic nut (11) to form a fixed whole, a rubber head buffer screw (10) is used above the spray bracket (5) to align the sample nozzle (3) with the center of the grounding electrode (4), and the spray is sprayed downward on the surface of the sample carrier above the grounding electrode (4), and the distance between the sample nozzle (3) and the grounding electrode (4) is 15 mm to 20 mm; A high voltage module, which is used to generate a high voltage of 5 kV to 10 kV and is applied between the sample nozzle (3) and the ground electrode (4) to change the spray shape; The liquid in the syringe (13) is guided to the piston at the rear end of the sample nozzle (2) through a liquid conduit (16), and the syringe (13) is rotated and pushed by an electrically controlled rotary stepping motor (7), so that the liquid inside the syringe flows to push the prepared liquid inside the sample nozzle (2), thereby realizing the regulation of the spraying speed of the prepared liquid from the sample nozzle (3). Under the joint action of high voltage electricity and the vertical lifting and displacement stage (1), a layer of nano-diamond particles is sprayed on the surface of the sample carrier by using an atomization spray method.

2. The device for surface dispersion spraying of nano-diamonds according to claim 1, characterized in that: The syringe placement platform (6) is composed of three plastic blocks and two guide rails (15). The plastic blocks at both ends are used to fix the guide rails (15) and the syringe (13). The output end of the electric-controlled rotary stepping motor (7) is fixedly mounted with a threaded column (14) threadedly connected to the outer wall of the guide rail (15) of the middle plastic block. The two guide rails (15) are arranged through both sides of the middle plastic block.

3. The device for surface dispersion spraying of nano-diamonds according to claim 1, characterized in that: The sample nozzle (2) is made of an insulating transparent plastic material, the front and rear ends of the nozzle are separated by a piston, the front end of the nozzle is loaded with a sample, and the rear end is connected to a syringe (13); the sample nozzle (3) is made of a conductive stainless steel metal material, connected to the front end of the sample nozzle (2), and has an inner diameter of 0.35 mm; the grounding electrode (4) is made of a conductive aluminum metal material and is grounded using a wire, and the grounding wire is placed close to the outside of the spray environment component (17).

4. The device for surface dispersion spraying of nano-diamonds according to claim 1, characterized in that: The spray environment component (17) is an acrylic box composed of five acrylic plates, and has holes on the sides for entering the liquid conduit (16), the high-voltage wire, the ground wire, and the nitrogen pipe.

5. A method for surface dispersion spraying of nanodiamonds, characterized in that: The device for surface dispersion spraying of nano-diamonds according to any one of claims 1 to 4 comprises the following steps: S1. Sample solution preparation: dilute 1 mg / ml nanodiamond stock solution with anhydrous ethanol, and then ultrasonically vibrate for 15 min to 20 min after dilution; S2, loading solution: inject the nano-diamond dilution solution after ultrasound into the front end of the sample nozzle (2) and separate it from the rear end of the sample nozzle (2) using a plastic piston (9), the rear end of the sample nozzle (2) is connected to a liquid conduit (16), the liquid conduit (16) is connected to a syringe (13), the interior of the syringe (13) is filled with anhydrous ethanol, and then the transmission module is started to fill the front end of the sample nozzle (2) with the nano-diamond dilution solution; S3, sample carrier preset: place the sample carrier to be sprayed on the upper part of the ground electrode (4), and adjust the distance between the ground electrode (4) and the sample nozzle (3) to 15 mm to 20 mm, then turn on the nitrogen, and use a nitrogen pipe to pass the nitrogen into the spray environment component (17) through the side hole of the spray environment component (17) for a period of time until the wooden stick with sparks cannot be rekindled at the hole, turn off the nitrogen, and use plasticine to block the hole; S4, test spraying: ground the fixed module, connect the high-voltage module to the fixed module, start the high-voltage module, adjust the voltage within 5kv-10kv, use a red laser light to illuminate the bottom of the sample nozzle (3), and stop when the spray is observed to be a stable single cone, and stop the high-voltage module; S5. Start spraying: Use atomizing spray method, turn on the transmission module and the high-voltage module, control the spraying time, obtain a layer of nano-diamond coating, and complete the production of nano-diamond coating.

6. A method for surface dispersion spraying of nano-diamonds according to claim 5, characterized in that: In step S1, the steps of preparing the nano-diamond dilution solution specifically include: First, a nano-diamond solution with an average particle size of 40 nm and a concentration of 1 mg / ml is diluted to 0.025 mg / ml by adding anhydrous ethanol, and then the diluted suspension is placed in an ultrasonic device for ultrasonic oscillation treatment for 15 minutes to 20 minutes to obtain a nano-diamond diluted solution.

7. The method for surface dispersion spraying of nano-diamonds according to claim 5, characterized in that: In the step S5, the atomization spray method is an electrohydrodynamic atomization method.

8. A method for surface dispersion spraying of nano-diamonds according to claim 7, characterized in that: The specific process of the electrohydrodynamic atomization method is as follows: under the conditions of a flow rate of 3 ml / h and a voltage of 5 kv to 10 kv, the electrohydrodynamic atomization method is used, and the nano-diamond dilution liquid is jet-decomposed into fine droplets under the influence of an external electric field, and sprayed vertically downward in a cone shape onto the surface of the sample carrier above the ground electrode (4).

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