CN109052469A - It is a kind of can electric field controls spray pyrolysis nano materials device - Google Patents

It is a kind of can electric field controls spray pyrolysis nano materials device Download PDF

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Publication number
CN109052469A
CN109052469A CN201811200198.2A CN201811200198A CN109052469A CN 109052469 A CN109052469 A CN 109052469A CN 201811200198 A CN201811200198 A CN 201811200198A CN 109052469 A CN109052469 A CN 109052469A
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CN
China
Prior art keywords
electric field
nano
burning
powder
spray pyrolysis
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CN201811200198.2A
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Chinese (zh)
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齐建全
马振伟
韩秀梅
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Northeastern University Qinhuangdao Branch
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Northeastern University Qinhuangdao Branch
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Priority to CN201811200198.2A priority Critical patent/CN109052469A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Geology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention discloses belong to nano material chemosynthesis technical field one kind can electric field controls spray pyrolysis nano materials device.The device is made of spraying device, burning and drying device, collection device and control device of electric field;The low-field electrode of control device of electric field is connect with nano-powder and nano particle collection device;The control device of electric field applies a high voltage electric field to the spray droplet containing metal ion makes it be separated into the droplet of a large amount of nanometer scales under electrostatic force, forms nanostructure with manipulation;Nanometer droplet is directly entered burning and drying device and is dried or burnt, and is finally collected by nano-powder and nano particle collection device.The present invention obtains the different nano materials of different needs by the size of control electric field and the type and intensity of heat source to manipulate the formation of nanostructure, widens the new application range of nano material.It is simple and effective be synthetically prepared nano-powder method using this device, it is low in cost.

Description

It is a kind of can electric field controls spray pyrolysis nano materials device
Technical field
The invention belongs to nano material chemosynthesis technical field, in particular to it is a kind of can the spray pyrolysis of electric field controls close At the device of nano material.
In the synthesis technology of nano-powder and nano particle it is a kind of can extra electric field new chemical reaction unit.
Background technique
With China's rapid development of economy, scientific and technical is constantly progressive, and nano material gradually causes scientific circles Greatly concern, and become worldwide research hotspot.So-called nano material generally refers to ruler at least in one-dimensional direction It is very little between 1-100nm, and there is the fairly individual property such as small-size effect, skin effect, quantum effect and Coulomb effect Matter.
Many in the chemical synthesis process of chemical field, nano material, typical nanometer pyrolysis installation includes a titration Device, burner, drying device and nano particle collection device, this device setting is simple, but bulky, and drop becomes Change and be difficult to control, pyrolysis plant cleaning is difficult, and overall cost is high;The technology of preparing for the spray pyrolysis synthesis generally studied now exists All there is very big advantage, in addition, liquid concentration and reactant ratio are continuously to become in dispersibility, purity and cost Change, that is to say, that the pattern of product is easier.However conventional spray pyrolysis equipment volume is huge, droplet variation is difficult to Control, pyrolysis plant cleaning is difficult, and overall cost is high.In order to make droplet have controllability, introducing plus high-voltage field is one Kind effective solution scheme.
Summary of the invention
The purpose of the present invention is to propose to it is a kind of can electric field controls spray pyrolysis nano materials device, feature exists In the device is made of spraying device, burning and drying device, collection device and control device of electric field;It is installed on syringe pump Syringe, syringe outlet are connect with one end of injection fluid catheter, and the injection fluid catheter other end connects spray head;It is put below spray head Burning and drying device are set, places nano-powder and nano particle collection device on spray head opposite;The high-voltage electricity of control device of electric field Pole is connect with spray head, and the low-field electrode of control device of electric field is connect with nano-powder and nano particle collection device;The electric field controls Device applies a high voltage electric field to the spray droplet containing metal ion makes it be separated into a large amount of nanometers under electrostatic force The droplet of magnitude forms nanostructure with manipulation;Nanometer droplet is directly entered burning and drying device and is dried or burnt, finally It is collected by nano-powder and nano particle collection device.
The spraying device is by syringe pump, syringe, injection fluid catheter and sprinkler composition.
The burning and drying device are simple alcolhol burner or various flame generating means;Drying device is drying box or pipe Formula furnace;The burning and drying device are one of which or both combinations.
The nano particle collection device is a simple metal mesh, metal foil or powder collection vessel.
The additional electric field of the control device of electric field output is DC electric field, low-frequency ac electric field and high-frequency electric field, electric-field strength Degree is 0~± 100000V/mm.
Beneficial effects of the present invention are exactly to introduce electric field force when drop sprays in nanometer synthesis process, by controlling electric field Size and the type and intensity of heat source obtain the different nano materials of different needs to manipulate the formation of nanostructure, open up The new application range of wide nano material.It is simple and effective be synthetically prepared nano-powder method using this device, it is low in cost.
Detailed description of the invention:
Fig. 1 is the synthesizer of the nano material under electric field controls.
Fig. 2 TiO described in embodiment 12The SEM of nanometer rods schemes
Fig. 3 TiO described in embodiment 12The XRD spectrum of nanometer rods.
Specific embodiment
The present invention propose it is a kind of can electric field controls spray pyrolysis nano materials device, below with reference to embodiment pair The invention is described further.
Fig. 1 show the synthesizer of the nano material under electric field controls, and the device is by spraying device, burning and dry dress It sets, collection device and control device of electric field composition;In Fig. 1, mounting of syringe 2, the outlet of syringe 2 and injection on syringe pump 1 One end of fluid catheter 3 connects, and the other end of injection fluid catheter 3 connects spray head 4;Burning and drying device is placed below in spray head 4 5, nano-powder is placed on 4 opposite of spray head and nano particle collection device 9, nano particle collection device 9 are supported on work by bracket 8 Make on platform table top or ground.The high-field electrode 7 of control device of electric field is connect with spray head, the low-field electrode 10 and nanometer of control device of electric field Powder and nano particle collection device 9 connect;Wherein, syringe pump 1, syringe 2, injection fluid catheter 3 and spray head 4 form spraying dress It sets.The burning and drying device are simple alcolhol burner or various flame generating means;Drying device is drying box or tube furnace; The burning and drying device are one of which or both combinations.The nano particle collection device is a simple metal Net, metal foil or powder collection vessel.
The additional electric field of the control device of electric field output is DC electric field, low-frequency ac electric field and high-frequency electric field, the electric field Controller applies a high voltage electric field to the spray droplet containing metal ion, and electric field strength is 0~± 100000V/mm.Quiet Under electric power effect, spray liquid (titanium salt solution) drop is made to be separated into the droplet of a large amount of nanometer scales, nanostructure is formed with manipulation;It receives Rice droplet is directly entered burning and drying device and is dried or burnt, and is finally received by nano-powder and nano particle collection device Collection.
Embodiment 1
By the four fourth liposoluble of 3.40g metatitanic acid in 10ml dehydrated alcohol, injection A liquid is obtained.A liquid is sucked in 10ml syringe, It is arranged on syringe pump.It is 80L/min by syringe pump setting rate of flooding.By the high-voltage electricity of syringe needle access high voltage power supply Pole, collector are stainless (steel) wire, electrode ground connection.High voltage power supply setting+4500V voltage, syringe pump bring into operation, A liquid are existed It is sprayed under high pressure by syringe, alcolhol burner is placed below ejiction opening lights ejection liquid continuous heating.Liquid is sprayed at this time to be formed Nanometer line is formed due to burning to jet out flames, collected by the collector that the solid nanoparticles object that flame is formed is grounded. After reaction, high voltage power supply and syringe pump are closed, collector is removed, directly obtains TiO2Nano particle.As shown in Figure 2 SEM photograph shows that product is the nano particle of diameter 30nm;XRD photo as shown in Figure 3 shows that product is rutile and rutile titania The multiphase structure of mine.
Embodiment 2
3.40g titanium tetrachloride is dissolved in 10ml acetone, injection A liquid is obtained.A liquid is sucked in 10ml syringe, is arranged to On syringe pump.It is 100ml/min by syringe pump setting rate of flooding.Syringe needle is accessed to the high-field electrode of high voltage power supply, Collector is stainless (steel) wire, electrode ground connection.High voltage power supply setting+5000V voltage, syringe pump brings into operation, by A liquid in high pressure Under sprayed by syringe, place tube furnace below ejiction opening, 500-700 DEG C of heating temperature, make to spray liquid continuous heating and light. Ejection liquid formation nanometer line is formed due to burning at this time jets out flames, what the solid nanoparticles object that flame is formed was grounded Collected by collector.After reaction, high voltage power supply and syringe pump are closed, collector is removed, directly obtains TiO2Nano particle. SEM photograph as shown in Figure 2 shows that product is the nano particle of diameter 30nm;XRD photo as shown in Figure 3 shows product for gold The multiphase structure of red stone and anatase.

Claims (5)

1. one kind can electric field controls spray pyrolysis nano materials device, which is characterized in that the device by spraying device, Burning and drying device, collection device and control device of electric field composition;Mounting of syringe, syringe outlet and note on syringe pump One end connection of fluid catheter is penetrated, the injection fluid catheter other end connects spray head;Burning and drying device is placed below in spray head, is spraying Place nano-powder and nano particle collection device in head opposite;The high-field electrode of control device of electric field is connect with spray head, electric field controls The low-field electrode of device is connect with nano-powder and nano particle collection device;The control device of electric field gives being sprayed containing metal ion Drop applies a high voltage electric field makes it be separated into the droplet of a large amount of nanometer scales under electrostatic force, is formed and is received with manipulation Rice structure;Nanometer droplet is directly entered burning and drying device and is dried or burnt, and is finally received by nano-powder and nano particle Acquisition means are collected.
2. according to claim 1 it is a kind of can electric field controls spray pyrolysis nano materials device, which is characterized in that The spraying device is by syringe pump, syringe, injection fluid catheter and sprinkler composition.
3. according to claim 1 it is a kind of can electric field controls spray pyrolysis nano materials device, which is characterized in that The burning and drying device are simple alcolhol burner or various flame generating means;Drying device is drying box or tube furnace;Institute It states burning and drying device is one of which or both combination.
4. according to claim 1 it is a kind of can electric field controls spray pyrolysis nano materials device, which is characterized in that The nano particle collection device is a simple metal mesh, metal foil or powder collection vessel.
5. according to claim 1 it is a kind of can electric field controls spray pyrolysis nano materials device, which is characterized in that The additional electric field of control device of electric field output is DC electric field, low-frequency ac electric field and high-frequency electric field, electric field strength is 0~± 100000V/mm。
CN201811200198.2A 2018-10-16 2018-10-16 It is a kind of can electric field controls spray pyrolysis nano materials device Pending CN109052469A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1665743A (en) * 2002-07-03 2005-09-07 苏黎士联合高等工业学校 Metal oxides prepared by flame spray pyrolysis
CN104167562A (en) * 2014-07-14 2014-11-26 宁波大学 All-solid-state thin film battery based on electrostatic spray pyrolysis combined with flame spraying and preparation method
CN107236939A (en) * 2016-03-28 2017-10-10 周检 A kind of electrostatic spray pyrolysis prepares film apparatus
CN107810166A (en) * 2015-06-29 2018-03-16 赢创德固赛有限公司 The method that metal oxide powder is produced by flame spray pyrolysis

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1665743A (en) * 2002-07-03 2005-09-07 苏黎士联合高等工业学校 Metal oxides prepared by flame spray pyrolysis
CN104167562A (en) * 2014-07-14 2014-11-26 宁波大学 All-solid-state thin film battery based on electrostatic spray pyrolysis combined with flame spraying and preparation method
CN107810166A (en) * 2015-06-29 2018-03-16 赢创德固赛有限公司 The method that metal oxide powder is produced by flame spray pyrolysis
CN107236939A (en) * 2016-03-28 2017-10-10 周检 A kind of electrostatic spray pyrolysis prepares film apparatus

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HYUNCHEOL OH等: "Synthesis of ceria nanoparticles by flame electrospray pyrolysis", 《AEROSOL SCIENCE》 *

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Application publication date: 20181221