CN108414297B - A kind of collection device of Gaseous Detonation method nano materials - Google Patents

A kind of collection device of Gaseous Detonation method nano materials Download PDF

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CN108414297B
CN108414297B CN201810440047.8A CN201810440047A CN108414297B CN 108414297 B CN108414297 B CN 108414297B CN 201810440047 A CN201810440047 A CN 201810440047A CN 108414297 B CN108414297 B CN 108414297B
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collection device
collecting platform
detonation
nano
collection
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CN108414297A (en
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闫鸿浩
赵铁军
王小红
李晓杰
张潇飞
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Dalian University of Technology
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Dalian University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202Preparing specimens therefor

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
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Abstract

The present invention provides a kind of collection devices of Gaseous Detonation method nano materials, belong to nano material synthesis technical field.By equal length and the collecting platform shiftable haulage line with fixed device is nominally fixed with shape, obtains the fixed frame of nano material collecting device.Collecting platform is fixed on the fixed frame of collection device, the collection device of nano material is made.The device is built in Gaseous Detonation pipe, and is tested by Gaseous Detonation nano materials, particle size is had collected and is less than the sample that detonation inside pipe wall is collected into.Usefulness of the present invention has: 1) collection device stable structure, material physico-chemical property are stablized, and collect the nano material of different location.2) the nano material partial size on collection device is respectively less than detonation inside pipe wall particle size, facilitates the theory analysis for disclosing Gaseous Detonation nano materials.3) according to the sample topography feature of different location, a kind of collection specific morphology, the method for sized nanostructures material are provided.

Description

A kind of collection device of Gaseous Detonation method nano materials
Technical field
The present invention relates to a kind of collection devices of Gaseous Detonation method nano materials, more particularly, it relates to A kind of device of position-movable collection detonation reaction zone product, belongs to nano material synthesis technical field.The production being collected into Object can be used to disclose the growth mechanism of Gaseous Detonation method nano materials.
Background technique
Gaseous Detonation method is a kind of to operate the nano material system that convenient, reaction rate is fast, equipment requirement is low, product purity is high (the quick-fried temperature of Yan Honghao, Wu Linsong, Li Xiaojie, Zhao Tiejun synthesizes nano-TiO to Gaseous Detonation to Preparation Method2The influence of structure and performance [J] " Journal of Inorganic Materials " .2017,03:275-280).Gaseous Detonation method generally uses imflammable gas (such as H2, hydrocarbonization Close object etc.) and O2Or the mixed gas of the oxidizing gas such as air is ignited in closed space by electric spark as quick-fried source The gas generates the detonation of high temperature or detonation Means of Pyrolyzed Precursor prepares nano material.TiCl4Heated easily gasification, it is quick-fried frequently as gas phase Hong method prepares nano-TiO2Presoma, research finds the factors such as quick-fried source, explosion velocity, initial pressure, initial temperature, precursor concentration It can be to nano-TiO2Object phase and pattern generate different degrees of influence, or even cause change (the Ou Yangxin of its photocatalytic activity Gas deflagration and Detonation Process prepare the titanium dioxide nanoparticle research Dalian [D]: Dalian University of Technology's doctoral thesis, and 2009). Nano SnO2With Nano-meter SiO_22Respectively SnCl can be decomposed by Gaseous Detonation method4With SiCl4Preparation, and their appearance and size is same Sample is influenced (change of Yan Honghao, Wu Linsong, Li Xiaojie, Wang little Hong, Wang Shengjie the presoma with respect to the amount of substance by above-mentioned factor Change prepares Nano-meter SiO_2 to hydrogen-oxygen gas deflagration2Influence [J] " explosion and impact " .2012,06:581-584. Yan Hong of particle Great, Wang Shengjie, Li Xiaojie, Wu Linsong initial pressure prepare nano SnO to Gaseous Detonation2Influence [J] " functional material " .2013,20:3016-3019).It can get TiO by adjusting presoma type2-SnO2、TiO2-SiO2、TiO2-Fe2O3Etc. receiving Nano composite material, and the purer TiO of its photocatalytic activity2Nano particle have significantly promotion (L.S.Wu, H.H.Yan, J.L.Xiao,X.J.Li,X.H.Wang.Characterization and photocatalytic properties of SiO2-TiO2nanocomposites prepared through gaseous detonation method[J]. 《Ceramics International》.2017,43(12):9377-9381.L.S.Wu,H.H.Yan,X.J.Li, X.H.Wang.Characterization and photocatalytic properties of SnO2- TiO2nanocomposites prepared through gaseous detonation method[J].《Ceramics International".2017,43(1):1517-1521.).In addition to oxide, the carbon-clad metal of Gaseous Detonation method preparation is received Rice material, carbon nanomaterial and carbon nanotube etc. have good appearance structure and stability.Make presoma with ferrocene, it can Prepare carbon-coated iron/carbonization iron nano-particle (H.Yan, T.Zhao, X.Li, C.Hun.Hydrogen and air detonation (deflagration)synthesis of carbon-encapsulated iron nanoparticles[J], "Combustion,Explosion and Shockwaves".2015,51(4):495-501.);Make forerunner with acetylacetone copper Body can synthesize carbon copper-clad nano particle (Yan Honghao, Zhang Xiaofei, Zhao Bibo, Zhao Tiejun, Li Xiaojie gas phase/condensed explosive detonation Carbon copper-clad nanoparticle features [J] " light laser and the particle beams " .2017,08:74-78. of synthesis);Ignite benzene-oxygen gas mixture Body, can be synthesized under the conditions of negative oxygen onion-like fullerene nano material (N.Luo, H.W.Jing, Z.G.Ma, R.H.Chen.Gaseous detonation chemical synthesis of onion-like carbons[J]. "Mendeleev Communications".2017,27(2):195-197.);By adjusting imflammable gas in mixed gas Ratio, using ferrocene as catalyst can obtain carbon nano-tube material (T.J.Zhao, X.J.Li, J.H.S.Lee, H.H.Yan.The effects of hydrogen proportion on the synthesis of carbon nanomaterials with gaseous detonation(deflagration)method[J].《Materials Research Express " .2018,5 (2): 025024. Yang Rui, Li Xiaojie, Yan Honghao Gaseous Detonation method synthesis iron content multi wall Carbon nanotube [J] " Chinese Journal Of High Pressure Physics " .2017,03:209-214.).
Gaseous Detonation nano materials reaction rate is very fast, reaction process and its complexity, the life for nano particle Long mechanism mainly explains (Chen Tianwu, Luo Ning, Yan Honghao, Liu Kaixin gas phase explosion with the Kruis growth model of aerosol TiO in flow field2Numerical analysis pre-test [J] " Chinese Journal Of High Pressure Physics " .2014,06:729-735. Yan Hong of nanoparticle growth It is great, Wu Linsong, Li Xiaojie, application [J] " rare gold of the Wang Shengjie particle growth model in Gaseous Detonation nano materials Belong to material and engineering " .2015,05:1144-1148).It is calculated by numerical value, finds an important factor for influencing particle size, and pre- A possibility that surveying nano material size tunable.However, generally requiring product precipitating 10 in Gaseous Detonation nano materials Or so minute goes to collect again, so the growth phenomenon of nano particle can not be verified in an experiment.Therefore, it is necessary to a kind of special Sample collection device, nanoparticle growth machine during Gaseous Detonation is disclosed with product when obtaining Gaseous Detonation reaction System.
Summary of the invention
The purpose of the present invention is inventing a kind of collection device of Gaseous Detonation method nano materials, to obtain Gaseous Detonation Nanometer product when reaction.
Technical principle of the invention:
One, Gaseous Detonation process can generate the high temperature of nearly 3000K, and generate relatively large impact force, so, collect dress Certain heat-resisting quantity, reliable structural stability, physicochemical stability should be met by setting.
Two, collection device cannot significantly affect the propagation of detonation wave, need to have good detonation wave permeability.
Technical solution of the present invention:
A kind of collection device of Gaseous Detonation method nano materials, the collection device are placed in Gaseous Detonation experimental provision It is interior, including fixed frame and collecting platform two parts;
The fixed frame further comprises shape nominal 6 and collecting platform shiftable haulage line 7, and shape nominal 6, which is located at, to be received The both ends of acquisition means form fixed frame for fixing collecting platform shiftable haulage line 7;
The collecting platform further comprises collecting platform 8 and fixed device 9, and it is solid that collecting platform 8 passes through fixed device 9 It is scheduled on collecting platform shiftable haulage line 7, and is slided on collecting platform shiftable haulage line 7.
The shape nominal 6 is the polygons, round or ellipse such as triangle, quadrangle.
The nominal 6 quantity more than two of the shape, for fixing collecting platform shiftable haulage line 7.
The composing quantity of the collecting platform shiftable haulage line is 1 or more.
The collecting platform 8 is the porous flake of the high porosity of stainless steel mesh sheet or hole greater than 0.8mm of 10 mesh Material, shape are round, ellipse or polygon.
The collection device is the corrosion-resistant, high temperature resistants, oxidation resistant material such as stainless steel, copper, titanium.
The collection nano material is TiO2、SnO2、SiO2, carbon-coated iron, carbon copper-clad, carbon packet cobalt, carbon nanotube, nanometer The nano material of the Gaseous Detonations method such as carbon synthesis.
Beneficial effects of the present invention: 1) collection device stable structure, material physico-chemical property are stablized, and collect different location Nano material.2) the nano material partial size on collection device is respectively less than detonation inside pipe wall particle size, and it is quick-fried to facilitate announcement gas phase The theory analysis of Hong nano materials.3) according to the sample topography feature of different location, a kind of collection specific morphology, ruler are provided The method of very little nano material.
Detailed description of the invention
Fig. 1 is the Detonation Tube schematic device that Gaseous Detonation experiment is used used in the present invention.
Fig. 2 is the schematic diagram of nano material collecting device.
Fig. 3 is that Gaseous Detonation prepares TiO2Transmission electron microscope (TEM) picture.
Fig. 4 is sample in the TEM picture for collecting position 1 (at Detonation Tube tail end 160mm).
Fig. 5 is sample in the TEM picture for collecting position 2 (at Detonation Tube tail end 320mm).
Fig. 6 is sample in the TEM picture for collecting position 3 (at Detonation Tube tail end 640mm).
In figure: 1 electric spark;2 vacuum pumping valves and presoma injection valve;3 vacuum meters;4 temperature control systems;5 sealing flanges;6 Shape is nominal;7 collecting platform shiftable haulage lines;8 collecting platforms;9 fixed devices.
Specific embodiment
A specific embodiment of the invention is further illustrated below in conjunction with attached drawing and technical solution.
Embodiment 1
By taking Fig. 2 is to design a model as an example.Making material diameter is 6mm, and outer diameter is that the annulus of 95mm is nominal as shape.It cuts It takes the screw thread silk steel that 3 equal length diameters are 6mm and has fixed device, as collecting platform shiftable haulage line.Finally, screw thread silk Steel both ends according to etc. angular separation fixed with annulus, complete collection device frame.The stainless steel mesh sheet of 10 mesh is cut into directly Diameter is then the disk of 95mm is fixed in the fixed frame of collection device as the collecting platform of nano material with nut On, the production of nano material collecting device can be completed.Material therefor is 304 type stainless steels.It is received with the synthesis of Gaseous Detonation method Rice TiO2It is illustrated for collection.
Gaseous Detonation pipe is cleaned up and keeps the drying of tank interior.Nano material is thoroughly cleaned with ethyl alcohol collects dress The fixed frame set simultaneously is dried, in case impurity generates pollution to sample.After being washed and dried with EtOH Sonicate ripple Collecting platform is fixed on frame according to away from Detonation Tube tail portion 160mm distance, is then placed in the nano material collecting device It in Gaseous Detonation pipe, is aligned one end with Detonation Tube tail portion, Gaseous Detonation is avoided to impact the damage to tube wall.Then blanket gas Phase Detonation Tube, vacuumizes, and after being heated to 130 DEG C, injects the TiCl of 2ml4, and be that 2:1 is filled with H according to volume ratio2With O2To 1 Atmospheric pressure.Temperature uses 20J electric spark to ignite mixed gas after keeping 5min.Gaseous Detonation pipe is opened after 5min, takes out nanometer material Expect collection device, the nano-powder on collecting platform.Finally, the sample being collected into is characterized and is analyzed.
As shown in figure 4, spherical in shape away from the sample on collecting platform at the 160mm of Detonation Tube tail portion, partial size 20mm range with It is interior.The TiO that detonation inside pipe wall is collected when no collection device2Particle (as shown in Figure 3), it is flat that partial size is significantly greater than nano material collection The TiO obtained on platform2
Embodiment 2
According to the experimental method of embodiment 1, sample collection position is adjusted to away from Gaseous Detonation pipe tail portion 320mm, remaining Step is same as Example 1.There are obvious corner angle in the sample being collected into, and partial size slightly increases, and sees the TEM of Fig. 5 sample Figure.
Embodiment 3
According to the experimental method of embodiment 1, sample collection position is adjusted to away from Gaseous Detonation pipe tail portion 640mm, remaining Step is same as Example 1.The sample being collected into has apparent corner angle, and partial size between 20-30nm, but is less than in significantly increasing The Product size that detonation inside pipe wall is collected is shown in the TEM figure of Fig. 6 sample.
In conclusion the nanometer that the present invention can obtain when Gaseous Detonation reacts by this nano material collecting device produces Object provides the experimental observation foundation of Gaseous Detonation nano materials particles collision growth, this helps to disclose Gaseous Detonation The growth mechanism and theoretical calculation of nano materials.
The parameter and scheme that the present invention is not limited to the above embodiment are not limited to Gaseous Detonation method synthesis TiO2Receipts Collection, all any modification, improvement and equivalent replacements made within spirit and principle of the invention, should be included in of the invention Within protection scope.

Claims (8)

1. a kind of collection device of Gaseous Detonation method nano materials, which is characterized in that the collection device is placed in Gaseous Detonation In experimental provision, including fixed frame and collection part two parts;
The fixed frame further comprises shape nominal (6) and collecting platform shiftable haulage line (7), and shape nominal (6) is located at The both ends of collection device form fixed frame for fixing collecting platform shiftable haulage line (7);
The collection part further comprises collecting platform (8) and fixes device (9), and collecting platform (8) passes through fixed device (9) it is removably fixed on collecting platform shiftable haulage line (7), and is slided on collecting platform shiftable haulage line (7).
2. collection device according to claim 1, which is characterized in that the collection device is corrosion-resistant, high temperature resistant, resistance to Oxidation material is made.
3. collection device according to claim 1 or 2, which is characterized in that the shape nominal (6) is polygon, circle Shape or ellipse, quantity more than two.
4. collection device according to claim 1 or 2, which is characterized in that the group of the collecting platform shiftable haulage line (7) It is 1 or more at quantity.
5. collection device according to claim 3, which is characterized in that the composition of the collecting platform shiftable haulage line (7) Quantity is 1 or more.
6. according to claim 1, collection device described in 2 or 5, which is characterized in that the collecting platform (8) be 10 purposes not The porous sheet material of the high porosity of rust steel mesh piece or hole greater than 0.8mm, shape are round, ellipse or polygon.
7. collection device according to claim 3, which is characterized in that the collecting platform (8) is the stainless steel of 10 mesh The porous sheet material of the high porosity of mesh sheet or hole greater than 0.8mm, shape are round, ellipse or polygon.
8. collection device according to claim 4, which is characterized in that the collecting platform (8) is the stainless steel of 10 mesh The porous sheet material of the high porosity of mesh sheet or hole greater than 0.8mm, shape are round, ellipse or polygon.
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JP6110116B2 (en) * 2012-11-28 2017-04-05 日本写真印刷株式会社 Gas component adsorption tube, gas component collection device, and gas component collection method.
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CN105836729B (en) * 2016-04-11 2017-12-05 大连理工大学 The method that Gaseous Detonation method synthesizes iron content CNT
CN107305168B (en) * 2016-04-22 2020-05-22 中国石油化工股份有限公司 Gaseous mercury catches mercury device
CN206161388U (en) * 2016-11-03 2017-05-10 内蒙古包钢钢联股份有限公司 Raw coke oven gas composition detects sample and takes integrated equipment
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CN206740458U (en) * 2017-05-10 2017-12-12 广西壮族自治区环境保护科学研究院 A kind of eight grades of abiotic stepwise sampler rain insensitive devices
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