Size-adjustable cluster preparation equipment and method

Abstract

The invention discloses size-adjustable cluster preparation equipment and a size-adjustable cluster preparation method. The size-adjustable cluster preparation equipment comprises a control device, a gas cylinder fixing frame and a control device, the cluster generation device comprises a power supply, a generation cavity, a first stepping motor, a second stepping motor, a first electrode and a second electrode, the gas cylinder fixing frame is arranged on one side of the internal bracket; the power source is arranged below the inner support, a first stepping motor and a second stepping motor are arranged on the two sides of the generating cavity respectively, the output end of the first stepping motor is connected with the first electrode, and the output end of the second stepping motor is connected with the second electrode; openings matched with the first electrode and the second electrode are formed in the two sides of the generating cavity respectively. According to the invention, the stepping motor drives the electrode to move, the electrode generates spark ablation through the pulse voltage, and the deposition distance is adjusted to realize the regulation and control of the cluster size.

Description

Technical Field

[0001] The present invention relates to the technical field of nanoclusters, and particularly to a cluster preparation device and method with adjustable size. Background Art

[0002] Nanoclusters are nanoscale structures composed of several atoms or molecules. Due to their unique properties in size effect, quantum effect, and surface activity, they have broad application potential in multiple fields such as catalysis, sensors, electronic devices, biomedicine, etc. Their advantages are mainly reflected in high surface energy, good catalytic activity, and quantum characteristics in specific fields. For example, in the field of catalysis, nanoclusters can provide higher catalytic activity than bulk materials and are widely used in chemical reactions such as hydrogenation, oxidation, and desulfurization.

[0003] In the field of sensors, due to their highly sensitive reaction performance, nanoclusters become ideal materials in gas sensors and biosensors; in addition, nanoclusters also show great potential in electronic and optoelectronic devices, drug delivery, etc.

[0004] However, the existing methods for preparing nanoclusters still face some challenges. Conventional preparation methods such as chemical vapor deposition, solution method, laser evaporation method, and electrochemical method usually need to be carried out under harsh conditions such as high temperature and high pressure, and it is difficult to precisely control the size and dispersion of nanoclusters. The operation is complex and the energy consumption is high. Summary of the Invention

[0005] The purpose of the present invention is to provide a cluster preparation device and method with adjustable size, which can produce elemental metals, metal oxides, alloys, and semiconductor materials with particle sizes ranging from atomic level to 20 nanometers by generating spark ablation on the electrode through pulsed voltage at room temperature and standard atmospheric pressure.

[0006] To solve the above technical problems, the present invention provides the following technical solutions:

[0007] A cluster preparation device with adjustable size, comprising:

[0008] A control device, which belongs to the total control center and is used to monitor and control the operating state of the cluster preparation device;

[0009] A gas cylinder fixing rack for fixing and carrying the gas cylinder containing carrier gas, and the gas cylinder fixing rack is arranged on one side of the inner bracket;

[0010] A cluster generation device for preparing clusters, and the cluster generation device includes: a power supply, a generation cavity, a first stepping motor, a second stepping motor, a first electrode, and a second electrode;

[0011] The power supply is arranged below the inner bracket. A first stepping motor and a second stepping motor are respectively arranged on both sides of the generating cavity. The output end of the first stepping motor is connected to the first electrode through a copper pipe, and the output end of the second stepping motor is connected to the second electrode through a copper pipe. Openings matching the first electrode and the second electrode are respectively formed on both sides of the generating cavity.

[0012] According to the above technical solution, a window flange is arranged above the generating cavity.

[0013] According to the above technical solution, the gas cylinder fixing rack fixes 4 gas cylinders carrying carrier gas. 4 gas flow meters are arranged above the inner bracket, and the 4 gas flow meters are respectively connected to the 4 gas cylinders carrying carrier gas; the carrier gas in the 4 gas cylinders carrying carrier gas can be different.

[0014] The gas flow meter transmits the monitored gas flow data to the control device, and the control device controls the gas flow meter according to the received gas flow data to control the gas flow so that the gas outputs at a rated flow.

[0015] According to the above technical solution, 4 pressure reducing valves are arranged on one side of the inner bracket, and the 4 pressure reducing valves are respectively connected to the 4 gas cylinders carrying carrier gas. Among them, the pressure reducing valve is a manual switch.

[0016] According to the above technical solution,

[0017] Another embodiment, a method for preparing adjustable-size clusters, the steps of which include:

[0018] After starting the power supply, set the constant current parameter; the range of the set constant current parameter is 100ma - 1000ma;

[0019] The control device controls the first stepping motor and the second stepping motor to move, thereby driving the first electrode and the second electrode to touch each other;

[0020] When it is observed through the window flange that the first electrode and the second electrode touch each other, set the moving distance of the first electrode and the second electrode in the control device;

[0021] After setting the gas flow parameter in the control device, the control device transmits the gas flow parameter signal to the gas flow meter to control the gas flow meter to control the gas flow of the carrier gas in the 4 gas cylinders carrying carrier gas;

[0022] After setting the distances between the copper mesh carbon film for depositing the required atomic clusters and the first electrode and the second electrode respectively, apply a pulsed voltage to cause the first electrode and the second electrode to generate spark ablation, and use the carrier gas to blow out for condensation growth for 30 minutes to obtain nano-cluster particles.

[0023] According to the above technical solution, the moving range of the first electrode and the second electrode is 0.5 mm - 1.5 mm.

[0024] According to the above technical solution, the range of the copper mesh carbon film from the first electrode and the second electrode is 10 cm - 50 cm. A pipeline can be connected to the outlet of the reaction chamber, and the copper mesh carbon film is placed in this pipeline.

[0025] Among them, the increase in the collection distance of the copper mesh carbon film is equivalent to increasing the flight time of the particles in space. A longer flight time allows for more collisions between the cluster particles and the gas atoms in the air, resulting in an increase in the average particle size.

[0026] According to the above technical solution, the nano-cluster particles include elemental metals, metal oxides, alloys, and semiconductor materials with particle sizes ranging from atomic level to 20 nanometers.

[0027] Compared with the prior art, the beneficial effects achieved by the present invention are as follows: The present invention generates elemental metals, metal oxides, alloys, and semiconductor materials with particle sizes ranging from atomic level to 20 nanometers through pulsed voltage to cause spark ablation of the electrodes under room temperature and standard atmospheric pressure conditions. It breaks through the limitations of traditional production methods, eliminates the need for chemical precursors or organic ligands, directly generates nanoparticles in the gas phase under normal temperature and pressure, and has a simple and fast operation method. Only a simple adjustment of the collection distance of the sample can adjust the size of the clusters. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The drawings are used to provide a further understanding of the present invention and constitute a part of the specification. They are used together with the embodiments of the present invention to explain the present invention and do not constitute a limitation to the present invention. In the drawings:

[0029] Figure 1 is a schematic structural diagram of a cluster preparation device with adjustable size according to the present invention;

[0030] Figure 2 is a schematic diagram of the partial structure of the reaction chamber;

[0031] Figure 3 is the STEM characterization diagram of tungsten cluster samples 1, 2, 3, and 4 in the examples;

[0032] Figure 4 is the STEM characterization diagram of different elements under the same parameters in the examples;

[0033] In the figures: 1, control device; 2, gas cylinder fixing rack; 3, internal support; 4, power supply; 5, reaction chamber; 6, first stepping motor; 7, second stepping motor; 8, first electrode; 9, second electrode; 10, window flange; 11, pressure reducing valve; 12, gas flow meter. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0034] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0035] Embodiment 1

[0036] A size-adjustable cluster preparation device includes:

[0037] A control device 1, belonging to the general control center, is used to monitor and control the operating state of the cluster preparation device;

[0038] A gas cylinder fixing rack 2 is used to fix and carry the gas cylinder of the carrier gas. The gas cylinder fixing rack 2 is arranged on one side of the internal support 3; the gas cylinder fixing rack 2 fixes 4 gas cylinders carrying the carrier gas. There are 4 gas flow meters 12 arranged above the internal support 3, and the 4 gas flow meters 12 are respectively connected to the 4 gas cylinders carrying the carrier gas; there are 4 pressure reducing valves 11 arranged on one side of the internal support 3, and the 4 pressure reducing valves 11 are respectively connected to the 4 gas cylinders carrying the carrier gas. The gas flow meter 12 transmits the monitored gas flow data to the control device 1, and the control device 1 controls the gas flow meter 12 to control the gas flow according to the received gas flow data, and the control device 1 controls the opening and closing of the pressure reducing valve 11.

[0039] A cluster generating device is used to prepare clusters. The cluster generating device includes: a power supply 4, a generating cavity 5, a first stepping motor 6, a second stepping motor 7, a first electrode 8, and a second electrode 9;

[0040] The power supply 4 is arranged below the internal support 3. The first stepping motor 6 and the second stepping motor 7 are respectively arranged on both sides of the generating cavity 5. The output end of the first stepping motor 6 is connected to the first electrode 8, and the output end of the second stepping motor 7 is connected to the second electrode 9; openings matching the first electrode 8 and the second electrode 9 are respectively opened on both sides of the generating cavity 5, and a viewing window flange 10 is arranged above the generating cavity 5.

[0041] Embodiment 2 uses the size-adjustable cluster preparation device of Embodiment 1 to prepare tungsten clusters, and the steps include:

[0042] After starting the power supply 4, set the constant current parameter to 100 ma;

[0043] The control device 1 controls the first stepping motor 6 and the second stepping motor 7 to move, thereby driving the first electrode 8 and the second electrode 9 to touch each other; at this time, the distance between the first electrode 8 and the second electrode 9 is 0 cm; the first electrode 8 and the second electrode 9 are tungsten electrodes;

[0044] When it is observed through the window flange 10 that the first electrode 8 and the second electrode 9 are in contact, set the moving distance of the first electrode 8 and the second electrode 9 to 0.75 cm in the control device 1, and complete the setting of the distance between the two electrodes to 1.5 cm;

[0045] Set the gas flow parameter to 1 slm in the control device 1. The control device 1 transmits the gas flow parameter signal to the gas flowmeter 12 to control the gas flowmeter 12 to control the gas flow of the carrier gas in the gas cylinder carrying the carrier gas;

[0046] After setting the position of the copper mesh carbon film of the required tungsten clusters to be 5 cm away from the first electrode 8 and the second electrode 9, apply a pulsed voltage to cause the first electrode 8 and the second electrode 9 to generate spark ablation, and use the carrier gas to blow out for condensation growth for 30 min, then stop the operation of the device and take out the tungsten cluster sample 1.

[0047] Under the condition that the constant current is 100 ma, the electrode spacing is set to 1.5 cm, and the gas flow parameter is 1 slm and remains unchanged, set the distance between the copper mesh carbon film of the required tungsten clusters and the first electrode 8 and the second electrode 9 to 10 cm, and apply a pulsed voltage to cause the first electrode 8 and the second electrode 9 to generate spark ablation, and use the carrier gas to blow out for condensation growth for 30 min, then stop the operation of the device and take out the tungsten cluster sample 2.

[0048] Under the condition that the constant current is 100 ma, the electrode spacing is set to 1.5 cm, and the gas flow parameter is 3 slm and remains unchanged, use the above method for preparing tungsten clusters to prepare tungsten cluster samples 3 and 4 at positions where the copper mesh carbon film of the tungsten clusters is set to be 5 cm and 10 cm away from the first electrode 8 and the second electrode 9 respectively.

[0049] Perform STEM characterization on the tungsten cluster sample 1 and the tungsten cluster sample 2 to obtain the STEM characterization of the tungsten cluster samples 1, 2, 3, and 4 Figure 3 , Figure 3 In the figure, (a) represents the STEM characterization diagram of the tungsten cluster sample 1, (b) in the figure represents the STEM characterization diagram of the tungsten cluster sample 2, (c) in the figure represents the STEM characterization diagram of the tungsten cluster sample 3, and (d) in the figure represents the STEM characterization diagram of the tungsten cluster sample 4;

[0050] It can be clearly seen from the figure that when other parameters are the same, by increasing the collection distance, the size of the clusters can be increased. The increase in the collection distance is equivalent to increasing the flight time of the particles in space. A longer flight time can cause more collisions between the cluster particles and the gas atoms in the air, resulting in an increase in the average particle size of the particles.

[0051] Preparation steps of different element clusters in Example 3:

[0052] After starting the power supply 4, set the constant current parameter to 100 ma;

[0053] The control device 1 controls the movement of the first stepping motor 6 and the second stepping motor 7, thereby driving the first electrode 8 and the second electrode 9 to touch each other; at this time, the distance between the first electrode 8 and the second electrode 9 is 0 cm;

[0054] When it is observed through the window flange 10 that the first electrode 8 and the second electrode 9 touch each other, set the moving distance of the first electrode 8 and the second electrode 9 to 0.75 cm in the control device 1, and complete the setting of the distance between the two electrodes to 1.5 cm;

[0055] Set the gas flow parameter in the control device 1 to 1 slm. The control device 1 transmits the gas flow parameter signal to the gas flowmeter 12 to control the gas flowmeter 12 to control the gas flow of the carrier gas in the gas cylinder carrying the carrier gas

[0056] Set the copper mesh carbon film of the required copper clusters at a position 5 cm away from the first electrode 8 and the second electrode 9. Apply a pulsed voltage to cause the first electrode 8 and the second electrode 9 to generate spark ablation, and use the carrier gas to blow out for condensation growth. After 30 minutes, stop the operation of the device and take out the copper clusters. Under the same conditions, iron clusters, nickel clusters, and titanium clusters are prepared by the above cluster preparation method. Among them, the types of the first electrode 8 and the second electrode 9 for the prepared copper clusters, iron clusters, nickel clusters, and titanium clusters are copper electrodes, iron electrodes, nickel electrodes, and titanium electrodes, respectively.

[0057] Perform STEM characterization on the prepared copper clusters, iron clusters, nickel clusters, and titanium clusters to obtain STEM characterizations of different elements under the same parameters Figure 4 , Figure 4 In (a) represents the STEM characterization diagram of copper clusters, (b) represents the STEM characterization diagram of iron clusters, (c) represents the STEM characterization diagram of nickel clusters, and (b) represents the STEM characterization diagram of titanium clusters. It can be seen from the figure that the prepared samples are basically single atoms and are much darker compared to the tungsten samples. The brightness and darkness of the dark field image of the spherical aberration electron microscope are mainly determined by the atomic weight, that is, the heavier the element, the brighter it appears.

[0058] It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "including", "comprising" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes other elements not expressly listed, or also includes elements inherent to such process, method, article or device.

[0059] Finally, it should be noted that the above are only preferred embodiments of the present invention and are not used to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions recorded in the foregoing embodiments or perform equivalent replacements on some of the technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A size-adjustable cluster preparation device, characterized in that: include: A control device (1), belonging to the general control center, is used to monitor and control the operation status of the cluster preparation equipment; A gas cylinder fixing frame (2) for fixing a gas cylinder carrying a carrier gas, wherein the gas cylinder fixing frame (2) is arranged on one side of the internal support (3); A cluster generating device for preparing clusters, the cluster generating device comprising: a power source (4), a generating chamber (5), a first stepping motor (6), a second stepping motor (7), a first electrode (8) and a second electrode (9); The power source (4) is arranged below the internal support (3); a first stepper motor (6) and a second stepper motor (7) are respectively arranged on both sides of the generating cavity (5); the output end of the first stepper motor (6) is connected to the first electrode (8), and the output end of the second stepper motor (7) is connected to the second electrode (9); openings matching the first electrode (8) and the second electrode (9) are respectively opened on both sides of the generating cavity (5).

2. The size-adjustable cluster preparation device according to claim 1, characterized in that: A window flange (10) is provided above the generating cavity (5).

3. The size-adjustable cluster preparation device according to claim 1, characterized in that: The gas cylinder fixing frame (2) fixes four gas cylinders carrying carrier gas, and four gas flow meters (12) are arranged above the internal bracket (3), and the four gas flow meters (12) are respectively connected to the four gas cylinders carrying carrier gas; The gas flow meter (12) transmits the monitored gas flow data to the control device (1), and the control device (1) controls the gas flow meter (12) to control the gas flow according to the received gas flow data.

4. The size-adjustable cluster preparation device according to claim 1, characterized in that: Four pressure reducing valves (11) are provided on one side of the internal support (3), and the four pressure reducing valves (11) are respectively connected to four gas cylinders carrying carrier gas.

5. The method for preparing size-adjustable clusters according to claim 1, characterized in that: The types of the first electrode (8) and the second electrode (9) are consistent with the types of clusters to be prepared.

6. A method for preparing size-adjustable clusters, characterized in that: The steps include: After starting the power supply (4), set the constant current parameter; the constant current setting parameter range is 100ma-1000ma; The control device (1) controls the first stepper motor (6) and the second stepper motor (7) to move and thereby drive the first electrode (8) and the second electrode (9) to touch each other; When the first electrode (8) and the second electrode (9) are observed to touch each other through the window flange (10), the moving distance of the first electrode (8) and the second electrode (9) is set in the control device (1); After the gas flow rate parameters are set in the control device (1), the control device (1) transmits the gas flow rate parameter signal to the gas flow meter (12) to control the gas flow meter (12) to control the gas flow rate of the carrier gas in the four gas cylinders carrying the carrier gas; After setting the distance between the copper mesh carbon film on which the atomic clusters are to be deposited and the first electrode (8) and the second electrode (9), a pulse voltage is applied to cause spark ablation of the first electrode (8) and the second electrode (9), and a carrier gas is used to blow them out for condensation to obtain the desired nano cluster particles.

7. The method for preparing size-adjustable clusters according to claim 1, characterized in that: The movement range of the first electrode (8) and the second electrode (9) is 0.5 mm-1.5 mm.

8. The method for preparing size-adjustable clusters according to claim 1, characterized in that: The copper mesh carbon film is within a range of 10 cm to 50 cm from the first electrode (8) and the second electrode (9).

9. The method for preparing size-adjustable clusters according to claim 1, characterized in that: The nanocluster particles include single metals, metal oxides, alloys and semiconductor materials with particle sizes ranging from atomic level to 20 nanometers.

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