CN115032029A - Experimental device for exploring growth evolution of plasma synthesized nano material - Google Patents
Experimental device for exploring growth evolution of plasma synthesized nano material Download PDFInfo
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- CN115032029A CN115032029A CN202210958935.5A CN202210958935A CN115032029A CN 115032029 A CN115032029 A CN 115032029A CN 202210958935 A CN202210958935 A CN 202210958935A CN 115032029 A CN115032029 A CN 115032029A
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Abstract
The invention provides an experimental device for researching growth evolution of a plasma synthesized nano material, which comprises a plasma generator and a reactor, wherein a sampling mechanism is used for collecting the nano material at different growth evolution stages, and the sampling mechanism comprises a plurality of sampling channels which are sequentially communicated and arranged along the direction far away from the plasma generator in the normal direction of the reactor and collecting assemblies which can extend into the reactor through the sampling channels so as to collect the nano material at different growth evolution stages. The invention utilizes the collection assembly to enter the reactor through the sampling channel in sequence to collect the nano materials at different growth stages, and places the nano materials into the transmission electron microscope for observation, and can directly perform online detection to obtain products at different growth stages in the reaction process so as to directly obtain evidence of the growth evolution process of the nano materials.
Description
Technical Field
The invention relates to the technical field of nano material synthesis equipment, in particular to a device combining a long jet plasma generator and a thermophoresis sampling platform, which is used for collecting samples at different positions of a reactor for preparing nano materials by a plasma generation method so as to obtain the growth evolution process of the nano materials.
Background
The large-scale preparation of the nano powder material is one of the important applications of the plasma. The size of the nano material (1-100 nm) is close to the coherence length of electrons and the wavelength of light, and the special effect of the super-large specific surface area of the nano material shows excellent physicochemical characteristics different from the matter in a bulk state. At present, the preparation of plasma nano-materials faces an important problem that the selectivity of nano-materials to specific chemical components or morphological structures is high, and the synthesis process is often accompanied by a large amount of byproducts. This usually requires the deep exploration of the nucleation and growth mechanism of the nanomaterial in the plasma to realize the controllable preparation of the plasma nanomaterial.
The precondition for exploring the growth evolution mechanism of the plasma synthesized nano material is to establish a set of stable and reliable nano material synthesis experiment platform with high repeatability. Because the arc plasma jet is mostly in a turbulent flow state, the large-scale structure of the arc plasma jet is influenced by arc instability (arc root fluctuation, Helmholtz resonance, arc distortion and the like) to generate radial/circumferential motion due to the flow of a high-temperature core region; in the mixed layer of the plasma and the cold air at a relatively low temperature, the fluid is easily triggered by flow instability to generate a complex turbulent flow multi-scale vortex structure. Turbulent plasma has the defects of obvious flow pulsation, strong noise, short length of a high-temperature region, large axial parameter gradient and the like, and the reliability and repeatability of sampling are difficult to realize. Meanwhile, the plasma reaction temperature is high (> 3000K), the volume is small (< 10 mm), and the gas phase reaction speed is high (< 1 ms), so that the sampling and diagnosis are difficult.
Disclosure of Invention
The invention provides an experimental device for combining a stable laminar flow thermal plasma long jet flow with a thermophoresis sampling online sampling platform, which realizes the sample collection of nano materials at different stages of growth and evolution. Meanwhile, the physical and chemical properties of the nano material at different stages can be directly detected by combining a characterization analysis technology, and the mechanism of the forming and evolution process of the nano material is understood, so that the controllable preparation of the plasma nano material synthesis is promoted.
In order to solve the technical problems, the invention adopts the following technical scheme:
an experimental apparatus for exploring the growth evolution of a plasma synthesized nano material comprises a plasma generator and a reactor arranged at the tail end of the plasma generator, and further comprises:
sampling mechanism, sampling mechanism is used for gathering the nano-material of different growth evolution stages, wherein, sampling mechanism includes that a plurality of communicates the sample passage that sets up in the reactor normal direction in proper order and can stretch into the reactor through sample passage inside in order to gather the collection subassembly of different growth evolution stage nano-material along keeping away from plasma generator direction.
Preferably, the system further comprises a material supply system for supplying materials into the plasma generator, wherein the material supply system comprises a plasma working medium gas supply and a synthetic nanomaterial precursor material supply, and the material supply mode comprises a premixed gas intake of the synthetic nanomaterial precursor material and the plasma working medium gas or a single lateral mixed gas intake of the synthetic nanomaterial precursor material and the plasma working medium gas.
Preferably, the plasma generator includes a cathode and an anode coaxially disposed with the cathode, wherein the cathode is a rod-shaped graphite, tungsten, copper or silver electrode, and the anode is a graphite or copper electrode with a laval tube structure or a protruding structure.
Preferably, when the anode is in a laval tube structure, the anode includes a first tapered portion disposed at a terminal of the cathode, a first maintaining portion disposed at a small opening end of the first tapered portion, a second tapered portion disposed at a terminal of the first maintaining portion, a second maintaining portion disposed at a small opening end of the second tapered portion, and a sudden expansion portion disposed at a terminal of the second maintaining portion, wherein an inner diameter of the first maintaining portion is equal to an inner diameter of the sudden expansion portion.
Preferably, when the anode is a sudden expansion structure, the anode comprises a straight pipe section arranged at the tail end of the cathode and a sudden expansion section arranged at the tail end of the straight pipe section.
Preferably, the collecting assembly comprises a guide rail axially distributed along the reactor, a slide block capable of moving along the length direction of the guide rail, a moving cylinder arranged on the slide block, and a sampling probe arranged at the output end of the moving cylinder and capable of extending into the reactor for collecting the nano-materials, and the residence time of the sampling probe in the high-temperature flame of the plasma generator is less than 200ms during each sampling.
Preferably, the collection assembly further comprises a controller capable of controlling the movement of the slider and the cylinder.
Preferably, the sampling probe is an ultrathin copper mesh supporting film, a micro-grid or a high-temperature-resistant metal sheet for transmission electron microscope observation.
Preferably, the plasma generator uses Ar, He, N2, air or binary mixture of the plasmas.
Preferably, the reactor is made of high-temperature-resistant quartz glass, ceramic or metal.
According to the technical scheme, the invention has the following beneficial effects:
1. according to the invention, the nano material is formed in the plasma generator, the retention time of a product in the reactor is increased along with the increase of the distance from an anode outlet, and the nano material sequentially undergoes the processes of nucleation, surface growth, agglomeration and the like, so that the collecting assembly sequentially enters the reactor through the sampling channel to collect the nano material at different growth stages and is placed into a transmission electron microscope for observation, and thus the product at different growth stages in the reaction process can be directly obtained through online detection, and further the evidence of the growth evolution process of the nano material can be directly obtained.
2. In the invention, the influence (nucleation, surface growth and agglomeration) of different process parameters (temperature, inert gas type and flow, raw material gas type and flow and the like) on the growth evolution process of the nano material is directly proved, and an internal connection network between the process parameters and the nano material forming mechanism can be established, so that a guidance function is provided for searching the optimal process condition for preparing the nano material and the controllable preparation of the nano material.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2(a) is a cross-sectional view of a plasma generator having an anode in the form of a Laval tube;
FIG. 2(b) is a cross-sectional view of the plasma generator with a sudden expansion structure of the anode;
FIG. 3 is a cross-sectional view of a reactor;
FIG. 4 is a flow chart of the apparatus for realizing the research of the growth evolution process of the nanometer material;
FIG. 5 is a pictorial view of a long jet flame produced by the apparatus of the present invention;
FIG. 6(a) is a TEM image of graphene collected from the first sampling channel of the reactor in the apparatus of the present invention;
FIG. 6(b) is a TEM image of graphene collected from the second sampling channel of the reactor in the apparatus of the present invention;
FIG. 6(c) is a TEM image of graphene collected by the apparatus of the present invention in the third sampling channel of the reactor;
FIG. 6(d) is a TEM image of graphene collected by the apparatus of the present invention in the fourth sampling channel of the reactor;
FIG. 6(e) is a TEM image of graphene collected from the fifth sampling channel of the reactor in the apparatus of the present invention.
In the figure: 10. a plasma generator; 110. a cathode; 120. an anode; 121. a first tapering portion; 122. a first maintaining part; 123. a second tapered portion; 124. a second maintaining part; 125. a sudden expansion part; 121', a straight pipe section; 122', a sudden expansion section; 20. a reactor; 30. a sampling mechanism; 310. a sampling channel; 320. a collection assembly; 321. a guide rail; 322. a slider; 323. a cylinder; 324. a sampling probe; 325. and a controller.
Detailed Description
A preferred embodiment of the present invention will be described in detail below with reference to the accompanying drawings.
Referring to fig. 1, 3, 4, 5, an experimental apparatus for exploring growth evolution of a plasma synthesized nanomaterial comprises a plasma generator 10, a reactor 20 disposed at the end of the plasma generator, the reactor being in communication with the plasma generator, and a sampling mechanism 30 for collecting nanomaterials at different growth evolution stages, wherein the sampling mechanism comprises a plurality of sampling channels 310 sequentially disposed on the sidewall of the reactor in the direction away from the plasma generator, and a collecting assembly 320 capable of extending into the reactor through the sampling channels to collect nanomaterials at different growth evolution stages, it should be noted that the reactor direction in the present invention is perpendicular to the axial direction of the reactor, it can be understood that the sampling channels 310 are disposed perpendicular to the sidewall of the reactor, the method for generating stable laminar flow thermal long jet of the present invention is that an inert gas is ignited between a cathode and an anode to form an arc, the anode can promote to form stable long jet flow, the form and flow field distribution of the jet flow can be changed by adjusting the flow of inert gas, and after the jet flow is stable, hydrocarbon raw materials are introduced into the plasma generator, then long jet flow shaped flame is formed in the plasma generator, nano materials are formed in the plasma generator, along with the increase of the distance from an anode outlet, the retention time of products in the reactor is prolonged, the nano materials sequentially generate the processes of nucleation, surface growth, agglomeration and the like, in this way, the collecting assembly is utilized to sequentially collect the nano materials in different growth stages through the sampling channel, and the nano materials are placed into a transmission electron microscope for observation, so that products in different growth stages in the reaction process can be directly obtained through online detection, and further evidence of the growth evolution process of the nano materials is directly obtained.
In addition, it should be noted that, the sampling channel 310 is plugged by a high temperature-resistant rubber plug in the process of not sampling so as to plug the channel inlet, thereby reducing the interference of the external environment on the flame flow field inside the reactor.
As a preferable technical proposal, the invention also comprises a material supply system for supplying materials into the plasma generator, the material supply system comprises a plasma working medium gas supply and a synthetic nano material precursor material supply, the material supply mode comprises the premixed gas intake of the synthetic nano material precursor material and the plasma working medium gas or the single lateral mixed gas intake of the synthetic nano material precursor material and the plasma working medium gas, namely, the precursor material for synthesizing the nano material and the working medium gas of the plasma are mixed and then enter the gas, or the synthetic nano material precursor material and the plasma working medium gas are independently mixed and fed from the side of the plasma generator, and it needs to be noted that the proportion of carbon atoms in the reactor does not exceed 0.06 percent of the total amount, so that the long jet flow form is prevented from being changed due to coking.
As a preferred technical solution of the present invention, a plurality of the sampling channels 310 are distributed along the same straight line on the sidewall of the reactor 20, that is, the plurality of sampling channels are located on the same straight line, and since the time for the nanomaterial to grow in the reactor is longer the farther away from the anode outlet, when the samples are collected along the plurality of sampling channels, the nanomaterials in different growth evolution stages can be collected, it should be noted that the sampling channels in this embodiment are not limited to be distributed along the straight line of the reactor method, but can be distributed irregularly along the sidewall of the reactor, only the plurality of sampling channels need to be sequentially distributed along the direction away from the plasma generator, preferably, the sampling channels adopt the arrangement of this embodiment, and for this embodiment, the number of the sampling channels is 8.
As a preferred technical solution of the present invention, the plasma generator 10 includes a cathode 110 and an anode 120 coaxially disposed with the cathode, wherein a distance between a tip of the cathode and an outlet of the anode is 65 mm, the cathode is a graphite, tungsten, copper, or silver electrode in a rod shape, the anode is a graphite or copper electrode in a laval tube structure or a sudden expansion structure, the cathode needs to have a slow ablation rate, the stability of the jet flow can be maintained, and the anode needs to be made of a material that avoids other impurities introduced by the evaporation of the anode.
Further, when the anode is a laval tube structure, fig. 2(a) shows a cross-sectional view of the plasma generator anode 120, where the cross-section of the gas inlet is gradually reduced to form a first tapered portion 121, then the first retaining annular structure forms a first retaining portion 122, then the second tapered portion 123 is designed in the middle section, and the first retaining annular structure with the smallest cross-section area forms a second retaining portion 124, and finally the second retaining annular structure with the largest cross-section area forms a second protruding portion 125, where the first tapered portion, the first retaining portion, the second tapered portion, the second retaining portion and the second protruding portion form a through channel structure, so that the inert gas is combusted between the cathode and the anode to form a stable long jet flow.
Of course, the anode structure of the present invention can also be configured as a sudden expansion structure, specifically referring to fig. 2(b), the sudden expansion structure includes a straight pipe section 121 'disposed at the end of the cathode 110 and a sudden expansion section 122' disposed at the end of the straight pipe section, the diameter of the straight pipe section is d1, the length is l1, the diameter of the sudden expansion section is d2, the length is l2, and (d 2-d 1)/l 2 < 5 is satisfied, no matter which structure the anode adopts, it is used to generate a stable long plasma jet, and the temperature and speed parameter fluctuation of the generated plasma jet is less than 5%, the length is greater than 200mm, and it remains stable for a long time (> 10 min).
Furthermore, in order to avoid the overhigh temperature of the plasma generator during the reaction, the plasma generator is protected, circulating cooling water systems are arranged on the cathode and the anode to cool the plasma generator, and similarly, the flanges connected with the two ends of the reactor are also connected with circulating cooling water, so that the cracking caused by overhigh temperature of the reactor is avoided.
As a preferred technical solution of the present invention, the collecting assembly 320 includes a guide rail 321 axially distributed along the reactor 20, a slider 322 capable of moving along a length direction of the guide rail, a moving cylinder 323 disposed on the slider, and a sampling probe 324 disposed at an output end of the moving cylinder, the guide rail of this embodiment may employ a linear motor or other components capable of moving linearly, which may drive the slider to move along an axial direction of the reactor, that is, to move to a position corresponding to different sampling channels, and then may drive the sampling probe to enter the reactor through the moving cylinder, so as to collect the nanomaterial sample in the reactor by using the sampling probe, the moving cylinder in the present invention may employ an electric cylinder or an air cylinder, it should be noted that a center of the sampling probe is aligned to a center of a channel of the reactor, and each time of sampling, a staying time of the sampling probe in a high temperature flame of the plasma generator is less than 200ms, so as to ensure the smooth sampling process and avoid danger.
Further, the collecting assembly 320 further includes a controller 325, and the controller is configured to control the movement of the slider 322 and the actuating cylinder 323 to drive the sampling probe to enter the sampling channels at different positions, so as to collect the nanomaterial products at different growth evolution stages.
Further, the reactor 20 in this embodiment is made of high temperature resistant quartz glass, ceramic or metal, and the quartz glass is not only resistant to high temperature, but also provides the internal view of the reactor, so as to facilitate finding the working condition capable of generating stable jet flame, that is, the flame shape can be photographed by setting a CCD high-speed camera, and the flame shape generated in the whole plasma generator can be detected.
Furthermore, the time for sampling the nano-materials at different growth and evolution stages through the sampling channel is determined by the program control of the controller and the pressure of the air cylinder, so that proper sampling time needs to be ensured in order to ensure that enough actual samples are obtained, the sampling time is not too long or too short, and therefore, the program setting of the controller needs to be unchanged and the pressure of the air cylinder is kept consistent during each sampling. Specifically, the actual time is directly observed and recorded by a CCD high-speed camera, and repeated experiments and verifications of the CCD camera are needed, so that on one hand, enough samples are deposited on the sampling probe for analysis, and on the other hand, the burning loss of the sampling probe caused by overlong retention time in the center of the reactor is avoided.
As a preferred technical solution of the present invention, the sampling probe 324 is an ultra-thin copper mesh supporting film, a micro-grid or a high temperature resistant metal sheet for transmission electron microscope observation, wherein the thickness of the sampling probe is about 30 μm, and the interference to the flame flow field is small.
In a preferred embodiment of the present invention, the plasma used in the plasma generator 10 is Ar, He, N2, air, or a binary mixture of the above plasmas.
An embodiment of the present invention is given below, and specifically, the plasma gas phase synthesis of nano graphene sheet is taken as an example for explanation, and graphene is sp 2 The unique two-dimensional structure of the new material of the two-dimensional honeycomb lattice structure formed by hybridized carbon atoms endows the new material with excellent physical, chemical, electromagnetic, optical and other properties, so that the new material has wide application prospect in the fields of electronic devices, materials, energy sources, environment, biology, machinery and the like.
The main structure size of the device is as follows:
the diameter of the cathode is 8mm, the anode adopts a Laval tube structure, the length of the anode is 100mm, the distance between the gas inlet tapered section and the gas inlet tapered section is 25mm, the inner diameter of the large opening end is 30mm, the inner diameter of the small opening end is 14mm, the inner diameter of the minimum section, namely the inner diameter of the maintaining part II is 8mm, the length is 10mm, the inner diameter of the sudden expansion part is 14mm, and the length is 35 mm;
the total length of the reactor is 500mm, the inner diameter of each sampling channel is 18mm, and the center distance between the two sampling channels is 40 mm;
the pressure of the air compressor is 4 Mpa;
plasma gas: ar, flow rate 8 slm;
hydrocarbon raw material gas: c 2 H 4 The flow rate is 0.2 slm;
the arc current is: 100A;
the arc power is: 2.6 kW.
The whole process is as follows:
step 1: opening a gas supply system, introducing argon into the plasma generator, starting arc by using current of 60A, and running for 10-20 minutes to preheat the device;
and 2, step: introducing ethylene gas, adjusting current parameters and establishing stable long plasma jet;
and step 3: sampling different positions of the jet flow on line by adopting a sampling mechanism;
and 4, step 4: characterizing the physical and chemical properties of the sampling product in the step 3, such as the morphology structure and the like;
and 5: adjusting synthesis process parameters, repeating the steps 1-4, analyzing the obtained research results, and constructing an internal network relation between the process conditions for preparing the graphene and the formation mechanism;
fig. 6(a), 6(b), 6(c), 6(d), and 6(e) are transmission electron microscope images of samples taken from the first sampling channel closest to the anode nozzle to the fifth sampling channel, respectively.
As shown in fig. 6(a), 6(b), 6(c), 6(d), and 6(e), the product observed in the first sampling channel is a small graphene aggregate, and the whole is transparent with less shaded area. The aggregate is formed by stacking three graphene sheets, the size of a single graphene sheet is 50-150 nm, and the nucleation process of graphene can be closer to a nozzle. In the sample at the second sampling channel, an aggregate with a relatively large projected area appeared, while the size of the single graphene sheet was slightly increased, indicating that graphene surface growth occurred during this growth from the first sampling channel to the second sampling channel. The graphene aggregates in the third sampling channel and the fourth sampling channel are further increased, and meanwhile, the edge curl of the graphene is increased, the transparency is lowered, and the number of graphene layers is relatively thickened, so that two processes, surface growth and stacking agglomeration, of the graphene can occur in the process. At this stage, the surface growth process of graphene may be stopped, the stacking agglomeration of graphene and the curling increase, which may be caused by too long retention time of graphene in high temperature.
In the embodiment, a thermophoresis sampling mechanism is adopted for online sampling to obtain a solid product, a transmission electron microscope is combined for graphene morphology structure representation, the properties of the product at different growth stages in the reaction process are obtained, further evidence of the graphene growth evolution process is directly obtained, and the internal network relation between the process conditions for preparing the graphene and the formation mechanism can be constructed.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. An experimental device for researching growth evolution of plasma synthesized nano material comprises a plasma generator (10) and a reactor (20) arranged at the tail end of the plasma generator, and is characterized by further comprising:
sampling mechanism (30), sampling mechanism is used for gathering the nano-material of different growth evolution stages, wherein, sampling mechanism includes that a plurality of is along keeping away from plasma generator direction in proper order the intercommunication set up in reactor (20) normal direction sampling channel (310) and can stretch into reactor inside in order to gather the collection subassembly (320) of different growth evolution stage nano-material through sampling channel.
2. The experimental apparatus for exploring the growth evolution of plasma synthesized nano materials according to claim 1, further comprising a material supply system for supplying materials into the plasma generator, wherein the material supply system comprises a plasma working medium gas supply and a synthetic nano material precursor material supply, and the material supply mode comprises a premixed gas intake of the synthetic nano material precursor material and the plasma working medium gas or a single lateral mixed gas intake of the synthetic nano material precursor material and the plasma working medium gas.
3. The experimental apparatus for exploring the growth and evolution of plasma synthesized nano materials according to claim 1, wherein the plasma generator (10) comprises a cathode (110) and an anode (120) coaxially disposed with the cathode, wherein the cathode is a graphite, tungsten, copper or silver electrode in a rod shape, and the anode is a graphite or copper electrode in a Laval tube structure or a sudden expansion structure.
4. The experimental apparatus for exploring the growth and evolution of plasma synthesized nano-materials as claimed in claim 3, wherein when the anode is of a Laval tube structure, the anode comprises a first tapered portion (121) disposed at the end of the cathode (110), a first sustaining portion (122) disposed at the small end of the first tapered portion, a second tapered portion (123) disposed at the end of the first sustaining portion, a second sustaining portion (124) disposed at the small end of the second tapered portion, and a second sudden expansion portion (125) disposed at the end of the second sustaining portion, wherein the inner diameter of the first sustaining portion is equal to the inner diameter of the sudden expansion portion.
5. The experimental apparatus for exploring the growth evolution of plasma synthesized nanomaterials as claimed in claim 3, which comprises a straight tube section (121 ') disposed at the end of the cathode (110) and a sudden-expansion section (122') disposed at the end of the straight tube section when the anode is in a sudden-expansion structure.
6. The experimental apparatus for exploring the growth and evolution of plasma synthesized nano materials according to claim 4 or 5, wherein the collecting assembly (320) comprises a guide rail (321) axially distributed along the reactor (20), a slide block (322) capable of displacing along the length direction of the guide rail, a moving cylinder (323) arranged on the slide block, and a sampling probe (324) arranged at the output end of the moving cylinder and capable of extending into the reactor for collecting nano materials, and the residence time of the sampling probe in the high-temperature flame of the plasma generator is less than 200ms during each sampling.
7. The experimental apparatus for exploring the growth evolution of plasma synthesized nanomaterials according to claim 6, wherein the collection assembly (320) further includes a controller (325) capable of controlling the actions of the slide (322) and the actuating cylinder (323).
8. The experimental apparatus for exploring the growth evolution of plasma synthesized nano materials according to claim 6, wherein the sampling probe (324) is an ultra-thin copper mesh supporting film, a micro-grid or a high temperature resistant metal sheet for transmission electron microscope observation.
9. The experimental apparatus for exploring the growth evolution of plasma synthesized nanomaterials according to claim 1, wherein the plasma generator (10) uses plasma of Ar, He, N2, air or binary mixture of the aforementioned plasmas.
10. The experimental apparatus for exploring the growth evolution of plasma synthesized nanomaterials of claim 1, wherein the reactor (20) is made of high temperature resistant quartz glass, ceramic or metal.
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