Nanoparticle preparation device and nanoparticle preparation method
By using multi-level gradient temperature control and surfactant gas, combined with porous glass fiber spinning ball collection, the problem of irregular morphology of nanoparticles was solved, and nanoparticles with high sphericity and precise size were prepared, thus improving performance consistency.
Patent Information
- Application Number
- CN202511488023.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-17
- Publication Date
- 2025-11-18
- Estimated Expiration
- 2045-10-17
AI Technical Summary
Nanoparticles prepared by traditional methods have irregular morphologies, making it difficult to meet the requirements of applications with high performance consistency.
The process employs a temperature-controlled chamber with multi-level gradient temperature control and a step-by-step cooling treatment of the gaseous products, combined with surfactant gas and porous glass fiber spinning bundles for material collection, to control the nucleation and crystal growth process of nanoparticles.
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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Figure CN120961111A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of nanoparticle preparation technology, and in particular to nanoparticle preparation apparatus and methods. Background Technology
[0002] Nanomaterials, due to their abundant specific surface area and high activity, have wide applications in electronics, medicine, energy, and other fields. Spherical structures can significantly improve the flowability, uniformity, and filling properties of nanomaterials during application, further optimizing their performance. While traditional methods such as media milling can reduce particle size to the nanometer level, the resulting nanoparticles typically have irregular morphologies. This morphological variation can lead to unstable material properties, making it difficult to meet the requirements of some applications with high performance consistency requirements. Summary of the Invention
[0003] Therefore, it is necessary to provide a nanoparticle preparation apparatus and a nanoparticle preparation method to solve the problem of irregular morphology of nanoparticles.
[0004] One objective of this invention is to provide a nanoparticle preparation apparatus, the solution of which is as follows:
[0005] A nanoparticle preparation apparatus includes a gasification mechanism and a temperature control mechanism. The gasification mechanism is used to gasify raw materials to form gaseous products and introduce them into the temperature control mechanism. The temperature control mechanism includes a plurality of temperature control chambers connected in sequence. Each temperature control chamber has an independent 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 gaseous products.
[0006] In one embodiment, the number of temperature-controlled chambers is 3 to 5.
[0007] In one embodiment, at least one of the temperature control chambers is connected to an additional gas injection mechanism for introducing surfactant gas into the respective temperature control chamber.
[0008] In one embodiment, the nanoparticle preparation apparatus further includes a receiving mechanism located downstream of the temperature control mechanism in the direction of conveying the gas phase product, and the receiving mechanism comprises a porous glass fiber spinning ball.
[0009] In one embodiment, the porosity of the glass fiber spindle is 60%~90% and the pore size is 1nm~1500nm.
[0010] Another object of the present invention is to provide a method for preparing nanoparticles, the scheme of which is as follows:
[0011] A method for preparing nanoparticles, the method comprising the following steps:
[0012] The raw materials are gasified to form gaseous products;
[0013] Furthermore, the gaseous product is subjected to a stepwise cooling process to obtain nanoparticles.
[0014] In one embodiment, the method for preparing the nanoparticles further includes the following steps:
[0015] During the step-by-step cooling process, surfactant gas is introduced into the gaseous product.
[0016] In one embodiment, the surfactant gas includes at least one of PVP, isooctanol, octanol, heptanol, and hexanol.
[0017] In one embodiment, the method for preparing the nanoparticles further includes the following steps:
[0018] The gaseous product, after undergoing the stepwise cooling process, is passed into a porous glass fiber spinning ball to deposit and collect the nanoparticles.
[0019] In one embodiment, during the stepwise cooling process, the gaseous product sequentially passes through a first temperature zone, a second temperature zone, and a third temperature zone, with the temperature of the first temperature zone, the second temperature zone, and the third temperature zone decreasing stepwise.
[0020] In one embodiment, the boiling point or sublimation point T1 of the raw material is above 200°C and not greater 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 greater 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 greater 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 embodiment, the boiling point or sublimation point T4 of the raw material is above 3000°C, 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.
[0024] Compared with traditional methods, the above-mentioned nanoparticle preparation apparatus and method have the following advantages:
[0025] The above-mentioned nanoparticle preparation device and method utilize multiple temperature control chambers equipped with multi-level gradient temperature control to gradually regulate the temperature of the gaseous products formed by the gasification mechanism. This enables the regulation of the diffusion, nucleation, and crystal growth processes of raw material molecules, resulting in nanoparticles with good sphericity and improving the precision of controlling the size and morphology of the nanoparticles. Attached Figure Description
[0026] Figure 1 This is a schematic diagram of a nanoparticle preparation apparatus according to an embodiment of the present invention.
[0027] Explanation of reference numerals in the attached figures:
[0028] 100. Nanoparticle preparation device; 110. Gasification mechanism; 120. Temperature control mechanism; 121. Temperature control chamber; 130. Carrier gas injection mechanism; 140. Additional gas injection mechanism; 150. Material receiving mechanism. Detailed Implementation
[0029] To make the above-mentioned objects, features, and advantages of the present invention more apparent and understandable, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. Many specific details are set forth in the following description to provide a thorough understanding of the present invention. However, the present invention can be practiced in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.
[0030] In the description of this invention, 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," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.
[0031] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.
[0032] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention 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 this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.
[0034] Please refer to Figure 1 As shown, a nanoparticle preparation apparatus 100 of one embodiment includes a vaporization mechanism 110 and a temperature control mechanism 120.
[0035] The vaporization mechanism 110 is used to vaporize the raw material to form a gaseous product and introduce it into the temperature control mechanism 120. The temperature control mechanism 120 includes a plurality of temperature control chambers 121 connected in sequence. 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 gaseous product, the temperature in the plurality of temperature control chambers 121 can be set to decrease sequentially.
[0036] The aforementioned nanoparticle preparation apparatus 100 is equipped with a temperature control mechanism 120 to progressively regulate the temperature of the gaseous products formed by vaporization through the vaporization mechanism 110. The temperature control mechanism 120 has multiple temperature control chambers 121 with multi-level gradient temperature control, which can regulate the diffusion, nucleation, and crystal growth processes of raw material molecules, obtain nanoparticles with good sphericity, and improve the accuracy of controlling the size and morphology of the nanoparticles.
[0037] Alternatively, the raw materials for preparing nanoparticles can be metals, inorganic substances, or organic substances.
[0038] The metal can be an elemental 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 Co, Cr, Fe, Mn, and Ni. Inorganic substances include, but are not limited to, at least one of Al2O3, TiO2, SiO2, ZrO2, ZnO, TiN, AlNi, Si3N4, and C. Organic substances include, but are not limited to, at least one of pentanebenzene, NPB (N,N'-di(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4,4'-diamine), and Alq3 (tris(8-hydroxyquinoline)aluminum).
[0039] In some of these examples, the gasification mechanism 110 vaporizes the raw material under vacuum conditions. -5 Pa ~ 8×10 -5 Pa, specifically, for example, 2 × 10 -5 Pa, 3×10 -5 Pa, 4×10 -5 Pa, 5×10 - 5 Pa, 6×10 -5 Pa, 7×10 -5 Pa, 8×10 -5 Pa, etc.
[0040] Optionally, the vaporization mechanism 110 may perform vaporization treatment by means of, but not limited to, magnetron sputtering, resistance wire heating, high-frequency induction heating, electron beam evaporation, and laser heating.
[0041] Optionally, the vaporization mechanism 110 may be, 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 metallic and inorganic raw materials, a suitable method is to achieve the gasification process by magnetron sputtering of metallic or inorganic targets.
[0043] For organic raw materials, a suitable method is to achieve the gasification process by using high-frequency induction heating to volatilize or elevate the organic raw materials.
[0044] It is understandable that the gaseous products can be mixed with the first carrier gas and then introduced into the temperature control mechanism 120. For example... Figure 1As shown, a carrier gas injection mechanism 130 can be installed upstream of the temperature control mechanism 120 to input a first carrier gas. The first carrier gas is, for example, an inert gas, more specifically, argon (Ar). Besides its role as a carrier gas, the collision between inert gas molecules and the gaseous products also helps to cool the gaseous products and improve particle dispersion. The flow rate of the first carrier gas is, for example, 0.01 sccm to 1000 sccm, more specifically, 0.1 sccm, 10 sccm, 100 sccm, 200 sccm, 300 sccm, 400 sccm, 500 sccm, 600 sccm, 700 sccm, 800 sccm, 900 sccm, 1000 sccm, etc.
[0045] In some examples, the volume ratio of the gaseous product to the first carrier gas is 1:(5~20). The carrier gas plays a role in cooling and transporting the gaseous product. Within this range, the gaseous product can be quickly carried away and cooled, which helps to form multiple nucleation sites and effectively controls the particle size.
[0046] In some of these examples, there are 3 to 5 temperature-controlled chambers 121.
[0047] In some examples, the temperature control mechanism 120 includes a first temperature control chamber, a second temperature control chamber, and a third temperature control chamber in sequence. The temperatures of the first, second, and third temperature control chambers decrease progressively.
[0048] In some of these examples, the boiling point or sublimation point T1 of the raw material is above 200°C and not greater than 1000°C, 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 of these 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 of these 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 of these examples, the glass fiber spinnerets are prepared by electrospinning.
[0065] Furthermore, the present invention also provides a method for preparing nanoparticles.
[0066] One embodiment of the method for preparing nanoparticles includes the following steps:
[0067] The raw materials are gasified to form gaseous products;
[0068] The gaseous product was subjected to a stepwise cooling process to obtain nanoparticles.
[0069] The above-mentioned method for preparing nanoparticles utilizes multiple temperature control chambers 121 equipped with multi-level gradient temperature control to gradually regulate the temperature of the gaseous products formed by the gasification mechanism 110. This method can control the diffusion, nucleation, and crystal growth processes of raw material molecules, obtain nanoparticles with good sphericity, and improve the accuracy of controlling the size and morphology of nanoparticles.
[0070] In some of these examples, the nanoparticles are prepared using the nanoparticle preparation apparatus 100 of any of the examples described above.
[0071] In some of these examples, the gaseous products pass sequentially through a first temperature zone, a second temperature zone, and a third temperature zone. The temperature decreases progressively in the first, second, and third temperature zones.
[0072] In some of these examples, the boiling point T1 of the raw material is above 200°C and not greater 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.
[0073] In some of these 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 of these 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 of these examples, the boiling 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.
[0076] For example, in the preparation of silver (boiling point 2212℃) nanoparticles, the temperature of the first temperature zone is 774℃~1216℃, the temperature of the second temperature zone is 177℃~774℃, and the temperature of the third temperature zone is 17.7℃~177℃.
[0077] In some of these examples, the preparation method of the nanoparticles also includes the following steps:
[0078] During the step-by-step cooling process, surfactant gas is introduced into the gaseous product.
[0079] 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.
[0080] Optionally, the surfactant gas may include, but is not limited to, at least one of polyvinylpyrrolidone (PVP), isooctyl alcohol, octanol, heptanol, and hexanol.
[0081] Simultaneously, a second carrier gas can be introduced to assist in the delivery of the surfactant gas. 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, more specifically, for example, 0.1 sccm, 10 sccm, 100 sccm, 200 sccm, 300 sccm, 400 sccm, 500 sccm, 600 sccm, 700 sccm, 800 sccm, 900 sccm, 1000 sccm, etc.
[0082] In some examples, the flow rate 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.
[0083] In some of these examples, the preparation method of the nanoparticles also includes the following steps:
[0084] The gaseous product output from the temperature control mechanism 120 is introduced into a porous glass fiber spinning ball to collect and deposit nanoparticles.
[0085] A porous glass fiber spinning ball is used instead of a traditional cooling rod for material collection. The cooled gaseous products enter the porous structure of the glass fiber spinning ball, condense, and adhere to it, thus achieving collection. The prepared nanoparticles exhibit excellent spherical morphology. After entering the porous structure of the glass fiber spinning ball, the binding force between the nanoparticles and the glass fiber material is relatively weak. Mechanical force can be used to easily remove the nanoparticles from the glass fiber spinning ball, avoiding a reduction in the sphericity of the nanoparticles.
[0086] In some of these examples, the preparation method of the nanoparticles also includes the following steps:
[0087] The nanoparticles were annealed.
[0088] Annealing can eliminate internal stress in nanoparticles and improve their crystallinity. Furthermore, annealing also helps remove any residual surfactants that may be present in the nanoparticles.
[0089] In some examples, the annealing temperature is 100℃~400℃. Further, in some examples, the annealing temperature is 200℃~350℃. In some specific examples, the annealing temperature is, for example, 100℃, 150℃, 200℃, 250℃, 300℃, 350℃, 400℃, etc.
[0090] In some examples, the annealing time is 1 hour to 3 hours. In some specific examples, the annealing time is 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, etc.
[0091] The following specific embodiments further illustrate the present invention. These specific embodiments are provided to better understand the present invention, but are not intended to limit the scope of the invention and do not constitute a limitation on its content or protection.
[0092] Example 1
[0093] This embodiment provides a nanoparticle preparation apparatus 100.
[0094] The nanoparticle preparation apparatus 100 of this embodiment includes 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 vaporization mechanism 110 includes a magnetron sputtering mechanism. The vaporization mechanism 110 vaporizes the raw material to form a gaseous product. A carrier gas injection mechanism 130 is disposed between the vaporization mechanism 110 and the temperature control mechanism 120, for introducing a first carrier gas. The gaseous product is mixed with the first carrier gas and then introduced into the temperature control mechanism 120.
[0096] The temperature control mechanism 120 includes three temperature control chambers 121 connected in sequence. Each temperature control chamber 121 has an independent temperature control component, and the temperature in the multiple temperature control chambers 121 can be set to decrease sequentially along the conveying direction of the gaseous product.
[0097] Each temperature control chamber 121 is connected to an auxiliary gas injection mechanism 140. The auxiliary gas injection mechanism 140 is used to introduce surfactant gas and a second carrier gas into the corresponding temperature control chamber 121. The auxiliary gas injection mechanism 140 includes an ultrasonic atomizer.
[0098] The receiving mechanism 150 includes a porous glass fiber spinning ball.
[0099] Example 2
[0100] This embodiment provides a method for preparing nanoparticles.
[0101] The nanoparticle preparation method of this embodiment uses the nanoparticle preparation apparatus 100 provided in Example 1.
[0102] Step 1, set the temperature of temperature control chamber 121. Along the conveying direction of the gaseous product, the three temperature control chambers 121 of the temperature control mechanism 120 are set as a high temperature zone (800℃), a medium temperature zone (350℃) and a low temperature zone (25℃) in sequence.
[0103] Step 2: The surfactant PVP gas and the carrier argon gas are introduced 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 argon gas is 800 sccm.
[0104] Step 3: Ag target material is sputtered using a magnetron sputtering mechanism to form a gaseous Ag product. This gaseous product, along with argon carrier gas, is transported to a temperature control unit 120. The flow rate of the gaseous product is 40 sccm, and the flow rate of the argon carrier gas is 800 sccm. The gaseous product and argon gas are sequentially cooled through three temperature control chambers 121. The cooled gaseous product and argon gas are then transported to a glass fiber spinning bundle for nanoparticle deposition and collection.
[0105] Step 4: Mechanically knead the glass fiber spinning spool to remove the nanoparticles from the glass fiber spinning spool.
[0106] Example 3
[0107] The steps in this embodiment are basically the same as those in Embodiment 2, except that the temperature in the medium temperature zone is 200°C and the surfactant is isooctanol.
[0108] Example 4
[0109] The steps in this embodiment are basically the same as those in Embodiment 2, except that the sputtering target is Cu and the temperature in the high-temperature zone is 900℃.
[0110] Example 5
[0111] The steps in this embodiment are basically the same as those in Embodiment 2, except that the sputtering target is Al.
[0112] Example 6
[0113] The steps in this embodiment are basically the same as those in Embodiment 2, except that the sputtering target is CoCrFeMnNi, the high temperature zone temperature is 1000℃, and the medium temperature zone temperature is 350℃.
[0114] Example 7
[0115] The steps in this embodiment are basically the same as those in Embodiment 2, except that the sputtering target is Al2O3 and the temperature in the high-temperature zone is 1100℃.
[0116] Example 8
[0117] The steps in this embodiment are basically the same as those in Embodiment 2, except that the sputtering target is TiO2 and the temperature in the high-temperature zone is 1000℃.
[0118] Example 9
[0119] The steps in this embodiment are basically the same as those in Embodiment 2, except that the raw material is N,N'-bis(1-naphthyl)-N,N'-diphenyl-1,1'-biphenyl-4,4'-diamine (NPB), and the gasification mechanism uses high-frequency induction heating with a high-temperature zone temperature of 200°C and a medium-temperature zone temperature of 100°C.
[0120] Comparative Example 1
[0121] The steps in this comparative example are basically the same as those in Example 2, except that the temperature of all three temperature control chambers 121 is set to room temperature, and no surfactant PVP gas or carrier argon gas is introduced into the medium temperature zone.
[0122] Comparative Example 2
[0123] The steps in this comparative example are basically the same as those in Example 2, except that the temperature of all three temperature-controlled chambers 121 is set to room temperature.
[0124] The nanoparticles prepared in the above embodiments and comparative examples are shown in Table 1.
[0125] Table 1
[0126]
[0127] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0128] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.
Claims
1. A nanoparticle preparation apparatus, characterized in that, It includes a gasification mechanism and a temperature control mechanism. The gasification mechanism is used to gasify the raw material to form a gaseous product and introduce it into the temperature control mechanism. The temperature control mechanism includes a plurality of temperature control chambers connected in sequence. Each temperature control chamber has an independent 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 gaseous product.
2. The nanoparticle preparation apparatus as described in claim 1, characterized in that, The number of temperature-controlled chambers is 3 to 5.
3. The nanoparticle preparation apparatus as described in claim 1, characterized in that, At least one of the temperature control chambers is connected to an additional gas injection mechanism for introducing surfactant gas into the respective temperature control chamber.
4. The nanoparticle preparation apparatus according to any one of claims 1 to 3, characterized in that, The nanoparticle preparation apparatus further includes a receiving mechanism, which is located downstream of the temperature control mechanism in the direction of conveying the gas phase product. The receiving mechanism includes a porous glass fiber spinning ball.
5. The nanoparticle preparation apparatus as described in claim 4, characterized in that, The porosity of the glass fiber spinneret is 60%~90%, and the pore size is 1nm~1500nm.
6. A method for preparing nanoparticles, characterized in that, Includes the following steps: The raw materials are gasified to form gaseous products; Furthermore, the gaseous product is subjected to a stepwise cooling process to obtain nanoparticles.
7. The method for preparing nanoparticles as described in claim 6, characterized in that, The method for preparing the nanoparticles further includes the following steps: During the step-by-step cooling process, surfactant gas is introduced into the gaseous product.
8. The method for preparing nanoparticles as described in claim 7, characterized in that, The surfactant gas includes 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 method for preparing the nanoparticles further includes the following steps: The gaseous product, after undergoing the stepwise cooling process, is passed into a porous glass fiber spinning ball to deposit and collect the nanoparticles.
10. The method for preparing nanoparticles according to any one of claims 6 to 8, characterized in that, During the stepwise cooling process, the gaseous products sequentially pass through the first temperature zone, the second temperature zone, and the third temperature zone. 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 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 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; Alternatively, 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 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.
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