Nanoparticle preparation apparatus and method of nanoparticle preparation

By employing multi-level gradient temperature control and surfactant gas treatment, combined with porous glass fiber spinning spool collection, the problem of irregular nanoparticle morphology was solved, and nanoparticles with high sphericity and precise size were prepared to meet the requirements of high-performance applications.

CN120961111BActive Publication Date: 2026-03-27SHENZHEN HANKE NEW MATERIAL TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-10-17
Publication Date
2026-03-27

AI Technical Summary

Technical Problem

Nanoparticles prepared by traditional methods have irregular morphologies, making it difficult to meet the requirements of applications with high performance consistency.

Method used

The process employs a temperature-controlled chamber with multi-level gradient temperature control and a step-by-step cooling treatment of gaseous products, combined with surfactant gas and porous glass fiber spinning balls for material collection, to control the nucleation and crystal growth process of nanoparticles.

Benefits of technology

This method enables the preparation of nanoparticles with high sphericity, precise size and morphology, and improves the performance consistency of nanoparticles.

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Abstract

The present application relates to a nanoparticle preparation device and a nanoparticle preparation method. The nanoparticle preparation device comprises a gasification mechanism and a temperature control mechanism. The gasification mechanism is used to gasify raw materials to form a gas phase product and pass into the temperature control mechanism. The temperature control mechanism comprises multiple temperature control chambers that are sequentially communicated. Each temperature control chamber independently has a temperature control component, and the temperature in the multiple temperature control chambers can be set to sequentially decrease along the conveying direction of the gas phase product. The nanoparticle preparation device is provided with a temperature control mechanism to gradually regulate the temperature of the gas phase product formed by the gasification mechanism. The temperature control mechanism is provided with multiple temperature control chambers with multiple levels of gradient temperature control. The process of raw material molecular diffusion, nucleation and crystal growth can be regulated, and nanoparticles with good sphericity can be obtained. The control accuracy of the size and morphology of the nanoparticles is improved.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of nanoparticle preparation, in particular to a nanoparticle preparation device and a nanoparticle preparation method. BACKGROUND

[0002] Nanomaterials are widely used in the fields of electronics, medicine, energy, etc. due to their rich specific surface area and high activity. The spherical structure can significantly improve the flowability, uniformity and filling property of nanomaterials in the application process, further optimizing their use effect. When nanomaterials are prepared by traditional methods such as medium grinding method, although the particle size of the materials can be reduced to nanoscale, the morphology of the obtained nanoparticles is usually irregular. Such morphology difference will lead to unstable material performance, which is difficult to meet the requirements of some application scenarios with high performance consistency. SUMMARY

[0003] Therefore, it is necessary to provide a nanoparticle preparation device and a nanoparticle preparation method to solve the problem of irregular morphology of nanoparticles.

[0004] One of the purposes of the present application is to provide a nanoparticle preparation device, and the scheme is as follows:

[0005] A nanoparticle preparation device comprises a gasification mechanism and a temperature control mechanism, the gasification mechanism is used to gasify raw materials to form a gas phase product and pass into the temperature control mechanism; the temperature control mechanism comprises a plurality of temperature control chambers which are sequentially communicated, each temperature control chamber independently has a temperature control component, and along the conveying direction of the gas phase product, the temperature in the plurality of temperature control chambers can be set to sequentially decrease.

[0006] In one of the embodiments, the number of temperature control chambers is 3-5.

[0007] In one of the embodiments, at least one temperature control chamber is connected with an additional gas injection mechanism, and the additional gas injection mechanism is used to inject a surfactant gas into the corresponding temperature control chamber.

[0008] In one of the embodiments, the nanoparticle preparation device further comprises a material collecting mechanism, and the material collecting mechanism is located downstream of the temperature control mechanism in the conveying direction of the gas phase product. The material collecting mechanism comprises a glass fiber spinning cluster with a porous structure.

[0009] In one of the embodiments, the porosity of the glass fiber spinning cluster is 60%-90%, and the pore size is 1-1500 nm.

[0010] Another purpose of the present application is to provide a nanoparticle preparation method, and the scheme is as follows:

[0011] A nanoparticle preparation method comprises the following steps:

[0012] gasifying the raw material to form a gas phase product;

[0013] gradually cooling the gas phase product to obtain the nanoparticles.

[0014] In one embodiment, the method for preparing the nanoparticles further comprises the following steps:

[0015] In the process of the gradual cooling, a surfactant gas is introduced into the gas phase product.

[0016] In one embodiment, the surfactant gas comprises at least one of PVP, isooctanol, octanol, heptanol and hexanol.

[0017] In one embodiment, the method for preparing the nanoparticles further comprises the following steps:

[0018] The gas phase product after the gradual cooling is introduced into a porous glass fiber spinning bundle to collect the nanoparticles.

[0019] In one embodiment, in the process of the gradual cooling, the gas phase product sequentially passes through a first temperature zone, a second temperature zone and a third temperature zone, and the temperatures of the first temperature zone, the second temperature zone and the third temperature zone gradually decrease.

[0020] In one embodiment, the boiling point or sublimation point T1 of the raw material is above 200°C and not more than 1000°C, the temperature of the first temperature zone is 0.5T1~0.8T1, the temperature of the second temperature zone is 0.25T1~0.5T1, and the temperature of the third temperature zone is 0.02T1~0.25T1.

[0021] In one embodiment, the boiling point or sublimation point T2 of the raw material is above 1000°C and not more than 2000°C, the temperature of the first temperature zone is 0.4T2~0.65T2, the temperature of the second temperature zone is 0.15T2~0.4T2, and the temperature of the third temperature zone is 0.01T2~0.15T2.

[0022] In one embodiment, the boiling point or sublimation point T3 of the raw material is above 2000°C and not more than 3000°C, the temperature of the first temperature zone is 0.35T3~0.55T3, the temperature of the second temperature zone is 0.08T3~0.35T3, and the temperature of the third temperature zone is 0.008T3~0.08T3.

[0023] In one of the embodiments, the raw material has a boiling point or sublimation point T4 above 3000 DEG C, the first temperature zone has a temperature of 0.3T4~0.5T4, the second temperature zone has a temperature of 0.04T4~0.3T4, and the third temperature zone has a temperature of 0.005T4~0.04T4.

[0024] Compared with the conventional scheme, the nanoparticle preparation device and the nanoparticle preparation method have the following beneficial effects:

[0025] The nanoparticle preparation device and the nanoparticle preparation method utilize the multiple temperature control chambers with multiple-stage gradient temperature control to perform step-by-step temperature regulation on the gas phase product formed by the gasification mechanism, can realize regulation of the raw material molecule diffusion, nucleation and crystal growth process, can obtain nanoparticles with better sphericity, and can improve the control accuracy of the size and morphology of the nanoparticles. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 FIG. 1 is a structure schematic diagram of a nanoparticle preparation device according to an embodiment of the present application.

[0027] REFERENCE SIGNS:

[0028] 100, nanoparticle preparation device; 110, gasification mechanism; 120, temperature control mechanism; 121, temperature control chamber; 130, carrier gas injection mechanism; 140, additional injection mechanism; 150, material collection mechanism. DETAILED DESCRIPTION

[0029] In order to make the above objectives, characteristics and advantages of the present application more apparent, specific embodiments of the present application are described in detail below with reference to the accompanying drawings. In the following description, a large number of specific details are set forth in order to provide a thorough understanding of the present application. However, the present application can be implemented in many different ways other than the embodiments described herein, and those skilled in the art can make similar improvements without departing from the scope of the present application, so the present application is not limited to the specific embodiments disclosed below.

[0030] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application.

[0031] In addition, the terms "first", "second", "third", etc. are used herein for descriptive purposes only and should not be construed as indicating or implying relative importance or an ordered sequence. Thus, features referring to "first", "second" or "third" can include, explicitly or implicitly, at least one of such features. In the description of the application, the term "a plurality" means at least two, for example, two, three, etc., unless otherwise expressly and specifically defined.

[0032] In the present application, unless otherwise expressly and specifically defined, the terms "mounting", "connecting", "connecting", "fixing" and the like should be understood in a broad sense, for example, can be fixedly connected, can be detachably connected, or can be integrated; can be mechanically connected, or can be electrically connected; can be directly connected, or can be indirectly connected through an intermediate medium; can be the internal communication of two elements or the interaction relationship between two elements, unless otherwise expressly defined. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0033] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs. The terms used in the specification of the present application herein are only for the purpose of describing specific embodiments and are not intended to limit the present application. The term "and / or" used herein includes any and all combinations of one or more related listed items.

[0034] Reference is made to Figure 1 As shown, the nanoparticle preparation device 100 of an embodiment includes a gasification mechanism 110 and a temperature control mechanism 120.

[0035] The gasification mechanism 110 is used to gasify the raw material to form a gas phase product and pass into the temperature control mechanism 120. The temperature control mechanism 120 includes a plurality of temperature control chambers 121 which are sequentially communicated. Each temperature control chamber 121 independently has a temperature control component (not shown in the figure). The temperature control component is used to control the temperature of the corresponding temperature control chamber 121. Along the conveying direction of the gas phase product, the temperature in the plurality of temperature control chambers 121 can be set to decrease sequentially.

[0036] The above-mentioned nanoparticle preparation device 100 is provided with a temperature control mechanism 120 to gradually regulate the temperature of the gas phase product formed by the gasification mechanism 110. The temperature control mechanism 120 is provided with a plurality of temperature control chambers 121 with multiple gradient temperature controls, which can realize the regulation of the raw material molecular diffusion, nucleation and crystal growth process, and can obtain nanoparticles with better sphericity, and improve the control precision of the size and morphology of the nanoparticles.

[0037] Optionally, the raw material for preparing the nanoparticles can be metal, inorganic matter or organic matter.

[0038] The metal can be a single metal, such as, but not limited to, Ag, Au, Pt, Cu, Al, Zn, Fe, Pd, etc. The metal can also be an alloy, such as, but not limited to, Fe 65 Co 20 Ni 15 , Ga 68.5 In 21.5 Sn 10 , at least one of CoCrFeMnNi. The inorganic substance is, for example, but not limited to, at least one of Al2O3, TiO2, SiO2, ZrO2, ZnO, TiN, AlNi, Si3N4, C. The organic substance is, for example, but not limited to, at least one of pentacene, NPB (N,N'-di(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4,4'-diamine), Alq3 (tris(8-hydroxyquinoline) aluminum).

[0039] In some examples, the gasification mechanism 110 performs gasification treatment on the raw material under vacuum conditions. The gasification treatment is performed under a gas pressure condition of, for example, 2 x 10 -5 Pa~8 x 10 -5 Pa, specifically, for example, 2 x 10 -5 Pa, 3 x 10 -5 Pa, 4 x 10 -5 Pa, 5 x 10 - 5 Pa, 6 x 10 -5 Pa, 7 x 10 -5 Pa, 8 x 10 -5 Pa, etc.

[0040] Optionally, the gasification mechanism 110 performs gasification treatment in a manner such as, but not limited to, magnetron sputtering, resistance wire heating, high-frequency induction heating, electron beam evaporation, and laser heating, etc.

[0041] Optionally, the gasification mechanism 110 is, for example, but not limited to, a magnetron sputtering mechanism, a resistance wire heating mechanism, a high-frequency induction heating mechanism, an electron beam evaporation mechanism, and a laser heating mechanism.

[0042] For the metal and inorganic substance raw material, a more suitable manner includes realizing the gasification process by magnetron sputtering of a metal target or an inorganic substance target.

[0043] For the organic substance raw material, a more suitable manner includes realizing the gasification process by high-frequency induction heating to volatilize or sublimate the organic substance raw material.

[0044] It can be understood that the gas-phase product can be mixed with the first carrier gas and then introduced into the temperature control mechanism 120 together. For example, Figure 1As shown, a carrier gas injection mechanism 130 can be arranged upstream of the temperature control mechanism 120, for inputting a first carrier gas. The first carrier gas is for example an inert gas, and more specifically for example argon (Ar). In addition to the role of the carrier gas, the collision between the inert gas molecules and the gas-phase product can also play a role in cooling the gas-phase product and improving the dispersion effect of the particles. The flow rate of the first carrier gas is for example 0.01sccm~1000sccm, and more specifically for example 0.1sccm, 10sccm, 100sccm, 200sccm, 300sccm, 400sccm, 500sccm, 600sccm, 700sccm, 800sccm, 900sccm, 1000sccm, etc.

[0045] In some examples, the volume ratio of the gas-phase product to the first carrier gas is 1∶(5~20). The carrier gas plays a role in cooling and transporting the gas-phase product, and within this range it can be ensured that the gas-phase product is quickly taken away and cooled, which helps to form multiple nucleation points and effectively control the particle size.

[0046] In some examples, the number of temperature control chambers 121 is 3~5.

[0047] In some examples, the temperature control mechanism 120 sequentially includes a first temperature control chamber, a second temperature control chamber, and a third temperature control chamber. The temperatures of the first temperature control chamber, the second temperature control chamber, and the third temperature control chamber decrease in stages.

[0048] In some examples, the boiling point or sublimation point T1 of the raw material is above 200℃ and not greater than 1000℃, the temperature of the first temperature control chamber is 0.5T1~0.8T1, the temperature of the second temperature control chamber is 0.25T1~0.5T1, and the temperature of the third temperature control chamber is 0.02T1~0.25T1.

[0049] In some examples, the boiling point or sublimation point T2 of the raw material is above 1000℃ and not greater than 2000℃, the temperature of the first temperature control chamber is 0.4T2~0.65T2, the temperature of the second temperature control chamber is 0.15T2~0.4T2, and the temperature of the third temperature control chamber is 0.01T2~0.15T2.

[0050] In some examples, the boiling point or sublimation point T3 of the raw material is above 2000℃ and not greater than 3000℃, the temperature of the first temperature control chamber is 0.35T3~0.55T3, the temperature of the second temperature control chamber is 0.08T3~0.35T3, and the temperature of the third temperature control chamber is 0.008T3~0.08T3.

[0051] In some of these examples, the boiling point or sublimation point T4 of the raw material is above 3000℃, the temperature of the first temperature control chamber is 0.3T4~0.5T4, the temperature of the second temperature control chamber is 0.04T4~0.3T4, and the temperature of the third temperature control chamber is 0.005T4~0.04T4.

[0052] For example, in the preparation of silver (boiling point 2212℃) nanoparticles, the temperature of the first temperature control chamber is 774℃~1216℃, the temperature of the second temperature control chamber is 177℃~774℃, and the temperature of the third temperature control chamber is 17.7℃~177℃.

[0053] like Figure 1 As shown, in some examples, the nanoparticle preparation apparatus 100 further includes an additional gas injection mechanism 140. At least one of the plurality of temperature-controlled chambers 121 is connected to the additional gas injection mechanism 140. The additional gas injection mechanism 140 is used to introduce surfactant gas and a second carrier gas into the respective temperature-controlled chamber 121.

[0054] In the above example, by introducing surfactant gas into the temperature control chamber 121, the surfactant gas can be chemically adsorbed on the surface of the nanoparticles during the condensation process, reducing the surface tension of the nanoparticles. Furthermore, due to the steric hindrance and electrostatic repulsion of the surfactant, the aggregation of nanoparticles caused by van der Waals forces can be reduced, thereby improving the dispersion effect between nanoparticles.

[0055] In some of these examples, each temperature control chamber 121 is connected to an additional gas injection mechanism 140. This allows for flexible selection of the temperature stage of the gaseous products when the surfactant gas is introduced.

[0056] In some examples, the additional gas injection mechanism 140 includes an ultrasonic atomizer and a delivery conduit. The delivery conduit connects the ultrasonic atomizer to a corresponding temperature control chamber 121. The ultrasonic atomizer is used to vaporize the surfactant to form a surfactant gas. It is understood that the additional gas injection mechanism 140 may also include a flow meter, a pressure gauge, a switching valve, etc., disposed on the delivery conduit.

[0057] Optionally, the surfactant gas may include, but is not limited to, at least one of polyvinylpyrrolidone (PVP), isooctyl alcohol, octanol, heptanol, and hexanol.

[0058] The second carrier gas is, for example, an inert gas. More specifically, the second carrier gas is, for example, argon. The flow rate of the second carrier gas is, for example, 0.1 sccm to 1000 sccm, and more specifically, for example, 0.1 sccm, 1 sccm, 10 sccm, 100 sccm, 200 sccm, 300 sccm, 400 sccm, 500 sccm, 600 sccm, 700 sccm, 800 sccm, 900 sccm, 1000 sccm, etc.

[0059] In some examples, the volume ratio of surfactant gas to second carrier gas is 1:(250~500). Too low a surfactant content results in poor dispersion, while too high a content affects the nucleation and growth of nanoparticles, leading to the formation of irregular shapes.

[0060] like Figure 1 As shown, in some examples, the nanoparticle preparation apparatus 100 further includes a receiving mechanism 150. The receiving mechanism 150 is located downstream of the temperature control mechanism 120 in the direction of gaseous product transport. The receiving mechanism 150 is used to collect the condensed nanoparticles.

[0061] In some examples, the collecting mechanism 150 includes a porous glass fiber spindle. Traditional cooling rod collecting methods require the use of a polytetrafluoroethylene (PTFE) scraper to remove nanoparticles from the cooling rod. This process damages the nanoparticles, reducing their sphericity. In the above examples, a porous glass fiber spindle replaces the traditional cooling rod for collecting. The cooled gaseous products enter the porous structure of the glass fiber spindle, condense, and adhere to the spindle, achieving collection. The prepared nanoparticles exhibit excellent spherical morphology. After entering the porous structure of the glass fiber spindle, the binding force between the nanoparticles and the glass fiber material is weak. Mechanical force can easily remove the nanoparticles from the spindle, avoiding a reduction in sphericity. For example, the nanoparticles can be removed from the spindle by mechanical kneading, vibration, or air jetting. Air jetting, for example, can use an air gun to spray argon gas.

[0062] In some examples, the porosity of the glass fiber spinneret is 60% to 90%. This porosity range allows gaseous products to easily enter the pore structure of the glass fiber spinneret and readily deposit on the fiber. Further, in some examples, the porosity of the glass fiber spinneret is 70% to 80%. In some specific examples, the porosity of the glass fiber spinneret is, for example, 60%, 65%, 70%, 75%, 80%, 85%, 90%, etc.

[0063] In some examples, the pore size of the glass fiber spinneret is 1 nm to 1500 nm. Further, in some examples, the pore size of the glass fiber spinneret is 50 nm to 1000 nm. In some specific examples, the pore size of the glass fiber spinneret is, for example, a range between any two values ​​from 2 nm, 20 nm, 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm, 900 nm, 1000 nm, 1100 nm, 1200 nm, 1300 nm, 1400 nm, to 1500 nm.

[0064] In some examples, the glass fiber spool is prepared by an electrospinning process.

[0065] Further, the present application also provides a method for preparing the nanoparticles.

[0066] The method for preparing the nanoparticles of an embodiment comprises the following steps:

[0067] Gasifying the raw material to form a gas phase product;

[0068] Gradually reducing the temperature of the gas phase product to obtain the nanoparticles.

[0069] The method for preparing the nanoparticles described above utilizes the plurality of temperature control chambers 121 provided with the multi-stage gradient temperature control to gradually regulate the temperature of the gas phase product formed by the gasification mechanism 110, which can realize the regulation of the raw material molecular diffusion, nucleation and crystal growth process, can obtain the nanoparticles with better sphericity, and can improve the control accuracy of the size and morphology of the nanoparticles.

[0070] In some examples, the method for preparing the nanoparticles uses the nanoparticle preparation device 100 of any of the examples described above.

[0071] In some examples, the gas phase product sequentially passes through the first temperature zone, the second temperature zone and the third temperature zone. The temperatures of the first temperature zone, the second temperature zone and the third temperature zone gradually decrease.

[0072] In some examples, the boiling point T1 of the raw material is above 200℃ and not greater than 1000℃, the temperature of the first temperature zone is 0.5T1~0.8T1, the temperature of the second temperature zone is 0.25T1~0.5T1, and the temperature of the third temperature zone is 0.02T1~0.25T1.

[0073] In some examples, the boiling point T2 of the raw material is above 1000℃ and not greater than 2000℃, the temperature of the first temperature zone is 0.4T2~0.65T2, the temperature of the second temperature zone is 0.15T2~0.4T2, and the temperature of the third temperature zone is 0.01T2~0.15T2.

[0074] In some examples, the boiling point T3 of the raw material is above 2000℃ and not greater than 3000℃, the temperature of the first temperature zone is 0.35T3~0.55T3, the temperature of the second temperature zone is 0.08T3~0.35T3, and the temperature of the third temperature zone is 0.008T3~0.08T3.

[0075] In some examples, the raw material has a boiling point T4 of 3000℃ or higher, the first temperature zone has a temperature of 0.3T4~0.5T4, the second temperature zone has a temperature of 0.04T4~0.3T4, and the third temperature zone has a temperature of 0.005T4~0.04T4.

[0076] For example, for the preparation of silver nanoparticles (boiling point 2212℃), the first temperature zone has a temperature of 774℃~1216℃, the second temperature zone has a temperature of 177℃~774℃, and the third temperature zone has a temperature of 17.7℃~177℃.

[0077] In some examples, the method for preparing nanoparticles further comprises the following steps:

[0078] During the gradual cooling process, a surfactant gas is introduced into the gas phase product.

[0079] In the above examples, by introducing a surfactant gas into the temperature control chamber 121, the surfactant gas can be chemisorbed on the surface of the nanoparticles during condensation, reducing the surface tension of the nanoparticles, and due to the steric hindrance and electrostatic repulsion of the surfactant, the agglomeration of nanoparticles due to van der Waals forces can be reduced, improving the dispersion effect between nanoparticles.

[0080] Optionally, the surfactant gas includes, but is not limited to, at least one of polyvinylpyrrolidone (PVP), isooctanol, octanol, heptanol, and hexanol.

[0081] At the same time, a second carrier gas that assists in the delivery of the surfactant gas can be introduced. The second carrier gas is, for example, an inert gas. More specifically, the second carrier gas is, for example, argon. The flow rate of the second carrier gas is, for example, 0.1sccm~1000sccm, and more specifically, for example, 0.1sccm, 10sccm, 100sccm, 200sccm, 300sccm, 400sccm, 500sccm, 600sccm, 700sccm, 800sccm, 900sccm, 1000sccm, etc.

[0082] In some examples, the flow rate ratio of the surfactant gas to the second carrier gas is 1∶(250~500). If the content of the surfactant is too low, the dispersion effect is poor, and if the content is too high, it will affect the nucleation and growth of the nanoparticles, leading to the formation of irregular shapes.

[0083] In some examples, the method for preparing nanoparticles further comprises the following steps:

[0084] The gas phase product output from the temperature control mechanism 120 is introduced into the porous structure of the glass fiber spinning cluster for deposition and collection of nanoparticles.

[0085] The porous glass fiber bundle is used to replace the traditional cooling rod to collect the material. The cooled gas phase product enters the pore structure of the glass fiber bundle, and is condensed and attached to the glass fiber bundle to realize collection. The prepared nanoparticles have excellent spherical morphology. After entering the pore structure of the glass fiber bundle, the binding force between the nanoparticles and the glass fiber material is weak, and the nanoparticles can be easily taken out from the glass fiber bundle by mechanical force, thereby avoiding reducing the sphericity of the nanoparticles.

[0086] In some examples, the method for preparing the nanoparticles further comprises the following steps:

[0087] The nanoparticles are subjected to annealing treatment.

[0088] The annealing treatment can eliminate the internal stress of the nanoparticles and improve the crystallinity of the nanoparticles. In addition, the annealing treatment is also beneficial to removing the surfactant that may be left in the nanoparticles.

[0089] In some examples, the temperature of the annealing treatment is 100-400°C. Further, in some examples, the temperature of the annealing treatment is 200-350°C. In some specific examples, the temperature of the annealing treatment is, for example, 100°C, 150°C, 200°C, 250°C, 300°C, 350°C, 400°C, etc.

[0090] In some examples, the time of the annealing treatment is 1-3h. In some specific examples, the time of the annealing treatment is 1h, 1.5h, 2h, 2.5h, 3h, etc.

[0091] The following specific examples are provided to further illustrate the present application. The present application provides the following specific examples for better further understanding of the present application, and is not limited to the following specific examples, which do not constitute a limitation on the content and protection scope of the present application.

[0092] Example 1

[0093] The present embodiment provides a nanoparticle preparation device 100.

[0094] The nanoparticle preparation device 100 of the present embodiment comprises a gasification mechanism 110, a temperature control mechanism 120, a carrier gas injection mechanism 130, an additional gas injection mechanism 140, and a material collection mechanism 150.

[0095] The gasification mechanism 110 comprises a magnetron sputtering mechanism. The gasification mechanism 110 gasifies the raw material to form a gas phase product. The carrier gas injection mechanism 130 is arranged between the gasification mechanism 110 and the temperature control mechanism 120, and is used to introduce a first carrier gas. The gas phase product is mixed with the first carrier gas and introduced into the temperature control mechanism 120.

[0096] The temperature control mechanism 120 comprises three temperature control chambers 121 connected in sequence. Each temperature control chamber 121 independently has a temperature control component, and the temperature in the plurality of temperature control chambers 121 can be set to decrease sequentially along the conveying direction of the gas-phase product.

[0097] Each temperature control chamber 121 is connected with an additional gas injection mechanism 140. The additional gas injection mechanism 140 is used to inject a surfactant gas and a second carrier gas into the corresponding temperature control chamber 121. The additional gas injection mechanism 140 comprises an ultrasonic atomizer.

[0098] The material collecting mechanism 150 comprises a porous glass fiber spinning bundle.

[0099] Embodiment 2

[0100] The embodiment provides a preparation method of nanoparticles.

[0101] The preparation method of the nanoparticles of the embodiment uses the nanoparticle preparation device 100 provided in Embodiment 1.

[0102] Step 1, setting the temperature of the temperature control chamber 121. Along the conveying direction of the gas-phase product, the three temperature control chambers 121 of the temperature control mechanism 120 are sequentially set to a high-temperature zone (800°C), a medium-temperature zone (350°C), and a low-temperature zone (25°C).

[0103] Step 2, injecting a surfactant PVP gas and a carrier gas argon into the medium-temperature zone through the additional gas injection mechanism 140. The flow rate of the PVP gas is 0.5 sccm, and the flow rate of the carrier gas argon is 800 sccm.

[0104] Step 3, sputtering an Ag target material through the magnetron sputtering mechanism to form an Ag gas-phase product, and conveying the gas-phase product to the temperature control mechanism 120 along with the carrier gas argon. The flow rate of the gas-phase product is 40 sccm, and the flow rate of the carrier gas argon is 800 sccm. The gas-phase product and the argon sequentially pass through the three temperature control chambers 121 for step-by-step cooling. The cooled gas-phase product and the argon are conveyed to the glass fiber spinning bundle for deposition and collection of the nanoparticles.

[0105] Step 4, mechanically rubbing the glass fiber spinning bundle to make the nanoparticles come out of the glass fiber spinning bundle.

[0106] Embodiment 3

[0107] The embodiment is basically the same as the steps of Embodiment 2, and the only difference is that the medium-temperature zone temperature is 200°C, and the surfactant is isooctanol.

[0108] Embodiment 4

[0109] The embodiment is basically the same as the steps of Embodiment 2, and the only difference is that the sputtering target material is Cu, and the high-temperature zone temperature is 900°C.

[0110] Example 5

[0111] The procedure of this example is basically the same as that of Example 2, except that the sputtering target is Al.

[0112] Example 6

[0113] The procedure of this example is basically the same as that of Example 2, except that the sputtering target is CoCrFeMnNi, the temperature of the high-temperature zone is 1000°C, and the temperature of the medium-temperature zone is 350°C.

[0114] Example 7

[0115] The procedure of this example is basically the same as that of Example 2, except that the sputtering target is AI2O3, and the temperature of the high-temperature zone is 1100°C.

[0116] Example 8

[0117] The procedure of this example is basically the same as that of Example 2, except that the sputtering target is TiO2, and the temperature of the high-temperature zone is 1000°C.

[0118] Example 9

[0119] The procedure of this example is basically the same as that of Example 2, except that the raw material is N,N'-di(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4,4'-diamine (NPB), the gasification mechanism uses high-frequency induction heating, the temperature of the high-temperature zone is 200°C, and the temperature of the medium-temperature zone is 100°C.

[0120] Comparative Example 1

[0121] The procedure of this comparative example is basically the same as that of Example 2, except that the temperature of the three temperature-controlled chambers 121 is set to room temperature, and no surfactant PVP gas and carrier gas argon are input into the medium-temperature zone.

[0122] Comparative Example 2

[0123] The procedure of this comparative example is basically the same as that of Example 2, except that the temperature of the three temperature-controlled chambers 121 is set to room temperature.

[0124] The nanoparticles obtained in the above examples and comparative examples are shown in Table 1.

[0125] Table 1

[0126]

[0127] Any combination of the technical features in the above-described embodiments can be made, and for the sake of brevity, not all possible combinations are described, however, as long as the combination of the technical features does not exist in contradiction, it shall be considered within the scope of the present disclosure.

[0128] The above-described embodiments only express several implementation manners of the present application, and the description is relatively specific and detailed, but it shall not be understood as a limitation on the patent scope of the present application. It shall be pointed out that, for ordinary skilled persons in the art, several modifications and improvements can be made without departing from the concept of the present application, and these shall be within the protection scope of the present application. Therefore, the protection scope of the present application patent shall be subject to the appended claims.

Claims

1. A nanoparticle production apparatus, characterized by, The device comprises a gasification mechanism for gasifying raw materials to form a gas phase product and feeding the gas phase product into a temperature control mechanism; the temperature control mechanism comprises a plurality of temperature control chambers connected in sequence, each of the temperature control chambers independently has a temperature control component, and the temperature in the plurality of temperature control chambers can be set to decrease sequentially along the conveying direction of the gas phase product; In the process of gradually reducing the temperature, the gas phase product sequentially passes through a first temperature zone, a second temperature zone and a third temperature zone; The boiling point or sublimation point T1 of the raw material is above 200℃ and not more than 1000℃, the temperature of the first temperature zone is 0.5T1-0.8T1, the temperature of the second temperature zone is 0.25T1-0.5T1, and the temperature of the third temperature zone is 0.02T1-0.25T1; Alternatively, the boiling point or sublimation point T2 of the raw material is above 1000℃ and not more than 2000℃, the temperature of the first temperature zone is 0.4T2-0.65T2, the temperature of the second temperature zone is 0.15T2-0.4T2, and the temperature of the third temperature zone is 0.01T2-0.15T2; Alternatively, the boiling point or sublimation point T3 of the raw material is above 2000℃ and not more than 3000℃, the temperature of the first temperature zone is 0.35T3-0.55T3, the temperature of the second temperature zone is 0.08T3-0.35T3, and the temperature of the third temperature zone is 0.008T3-0.08T3; Alternatively, the boiling point or sublimation point T4 of the raw material is above 3000℃, the temperature of the first temperature zone is 0.3T4-0.5T4, the temperature of the second temperature zone is 0.04T4-0.3T4, and the temperature of the third temperature zone is 0.005T4-0.04T4.

2. The nanoparticle preparation apparatus of claim 1, wherein The number of the temperature control chambers is 3-5.

3. The nanoparticle production apparatus of claim 1, wherein At least one of the temperature control chambers is connected with an additional gas injection mechanism for feeding a surfactant gas into the corresponding temperature control chamber.

4. The nanoparticle preparation apparatus of any one of claims 1 to 3, wherein The nanoparticle preparation device further comprises a material collecting mechanism, which is located downstream of the temperature control mechanism along the conveying direction of the gas phase product, and comprises a glass fiber spinning bundle with a porous structure.

5. The nanoparticle production apparatus of claim 4, wherein The porosity of the glass fiber spinning bundle is 60%-90%, and the pore size is 1nm-1500nm.

6. A method of preparing nanoparticles, characterized by, The nanoparticle preparation device of any one of claims 1-5, the preparation method comprises the following steps: gasifying raw materials to form a gas phase product; and gradually reducing the temperature of the gas phase product to obtain nanoparticles.

7. The method of claim 6, wherein the nanoparticles are prepared by a method comprising: The nanoparticle preparation method further comprises the following steps: In the process of gradually reducing the temperature, a surfactant gas is fed into the gas phase product.

8. The method of claim 7, wherein the nanoparticles are prepared by a method comprising: The surfactant gas comprises at least one of PVP, isooctanol, octanol, heptanol and hexanol.

9. The method for preparing nanoparticles according to any one of claims 6 to 8, characterized in that, The nanoparticle preparation method further comprises the following steps: The gas phase product after the gradual temperature reduction is fed into a glass fiber spinning bundle with a porous structure for deposition and collection of the nanoparticles.

Citation Information

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