CN108892177A - The method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material - Google Patents

The method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material Download PDF

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Publication number
CN108892177A
CN108892177A CN201810508598.3A CN201810508598A CN108892177A CN 108892177 A CN108892177 A CN 108892177A CN 201810508598 A CN201810508598 A CN 201810508598A CN 108892177 A CN108892177 A CN 108892177A
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laser
raw material
self
product
ferrite material
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贺嘉杨
胡梦云
江梦慈
曾和平
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East China Normal University
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East China Normal University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/0018Mixed oxides or hydroxides
    • 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

Abstract

The invention discloses a kind of methods of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material, this method carries out induced with laser to material by using laser output laser, by the progress of laser regulation self-propagating reaction, laser sintered power, sintering region and sintering duration can be effectively adjusted, inductively control generates expected Ferrite Material at high temperature with this.Preparation method of the present invention is simple, can carry out adjustment in time to reaction condition and as former state to meet product requirements, raw material availability is high, no process waste, product short preparation period, and product is controllable.

Description

The method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material
Technical field
The present invention relates to a kind of generation methods of cu ferrite material, more particularly to a kind of laser-induced self-propagating reaction high temperature The method for synthesizing cu ferrite material.
Background technique
Cu ferrite belongs to the quasi-metal oxides in ferrite, has ferromagnetic specific to ferrite class compound Property.Cu ferrite is the semiconductor material of spinel structure, and structural behaviour is stablized, because of good air-sensitive property, electromagnetic property, suction The many aspects such as attached property and catalytic property characteristic and be concerned.Especially the cu ferrite of spinel-type has good Photocatalysis performance shows as the multinomial excellent characteristics such as forbidden bandwidth is narrow, light absorption wave band is wide, and ferromagnetic with being easily recycled Property, it is often studied in recent years to apply in the application field of wastewater treatment.
Since modern times, the process demand of the organic wastewater largely discharged in industrial production and life process has increasingly been compeled It cuts, in emerging high-level oxidation technology, photocatalytic oxidation is because having degradation non-selectivity, normal temperature and pressure, nontoxicity, chemical property It is stable, reusable and be concerned with the extensive prospect using solar energy.The cu ferrite of spinel structure Object is closed as a kind of typical photocatalyst material, has its small forbidden bandwidth, unglazed corrosivity, catalytic performance active etc. numerous Advantage.
The preparation method of currently used cu ferrite class compound has following several:Chemical vapour deposition, colloidal sol are solidifying Glue method, chemical coprecipitation and solid phase method.General chemical vapour deposition is suitable for experimental study, synthetic quantity is limited, at This high feature makes it be difficult to industrialized production.It is easy to form hard after the drying using ferrite powder made from sol-gal process Agglomeration shrinks when dry and greatly, easily splits, and preparation step is many and diverse.Often there is glue in precipitation process in chemical coprecipitation Shape precipitating, it is difficult to filter and wash and precipitating is uneven.Solid phase method has the characteristics that apparatus and process is simple, at low cost, yield is big, The powder granule soilless sticking of preparation, but it also has the shortcomings that energy consumption is high, difficult to control, powder is not thin enough, is easily mixed into impurity.
In conclusion preparing cu ferrite material is to hinder greatly the one of cu ferrite flow of research at present, people are urgent Need a kind of realization simple process, energy conservation, efficient, controllable, free of contamination ferrite class compound generation method.
Summary of the invention
The object of the present invention is to provide a kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material, this method Synthetic product cu ferrite rapidly and efficiently, simple process, energy conservation, efficiently, realize product it is controllable, no waste pollution object It generates.
Realizing the specific technical solution of the object of the invention is:
A kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material, feature are with copper, the oxide of copper, iron And the oxide of iron is raw material, and self-propagating reaction occurs using induced with laser, and raw material reaction is made to generate Cu2O catalyzes and synthesizes process Progress;Specifically include following steps:
Step 1:Raw material powder needed for choosing, and mixed raw material is mixed to get by raw material is full and uniform;
Step 2:The mixed raw material is placed in reaction vessel;
Step 3:Using laser irradiation on mixed raw material, laser is adjusted, self-propagating reaction occurs for induced with laser, raw At cu ferrite material head product;
Step 4:Later period grinding is carried out to cu ferrite material head product, obtains that particle is small, cu ferrite of good evenness Material;Wherein:
Raw material powder described in step 1 is the oxide of copper, the oxide of copper, iron and iron, is selected according to actual product demand Take the type and ratio of raw material powder;Full and uniform be mixed into obtains uniformly mixed little particle by grinding, agitating mode Powder, or tabletting is carried out to uniformly mixed small particle powder;
Induced with laser described in step 3 occur self-propagating reaction, the reaction by change heat release and transmission speed come The speed of control process, temperature, conversion ratio and product composition and structure.
The laser is continuous wave laser or pulse laser, and output laser wavelength is infrared band;It is described to swash The spectral band of light is infrared band, visible light wave range or infrared and visible light mixing wave band.
For the laser irradiation on mixed raw material, the region of irradiation, power, time pass through feedback regulation control, root Target product is generated according to demand, the real-time controllable of localization is realized to the process that preparation generates product.
The laser controlling reaction for adjusting laser and referring to laser output, is able to carry out laser focusing, to sintering zone Domain carries out spatial distribution control, including laser space lattice, laser spacescan.
It prepares environment and carries out gas control, gas N2
The present invention is radiated at raw material surface using high power laser light, and the self- propagating that control raw material carry out induced with laser is anti- It answers.Laser is exported using superpower laser, optical maser wavelength is reactant absorption bands wavelength, and it is anti-to be conducive to reactant heat absorption quickening Process is answered, realizes the self-propagating reaction of induced with laser, prepares cu ferrite material energy-efficiently;Swashed by feedback regulation control Region of the light action on reactant, power, time, generate target product according to demand, and the process for generating product to preparation is real Now localization is real-time controllable;Utilize the Cu generated in reaction process2O realizes the catalysis of reaction process, efficiently prepares product.
The present invention is suitable for various copper, the mixing of iron oxide powder controllably prepares cu ferrite material, is suitable for more Kind different material and the different preparations for requiring product.Entire production process realizes that step is simple, self- propagating process control, preparation speed Rate is high, and no waste mine generates.
Detailed description of the invention
Fig. 1 is flow chart of the present invention;
Fig. 2 is the self-propagating combustion process schematic that the present invention prepares cu ferrite material;
Fig. 3 is the XRD diagram of the cu ferrite material of preparation of the embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment and attached Figure, the present invention will be described in further detail.
The present invention synthesizes the self-propagating combustion reaction for being utilized in cu ferrite materials process and being gone out by induced with laser, is to utilize A kind of technology of self-heat generation synthetic material is chemically reacted, be otherwise known as conbustion synthesis, prepares cu ferrite class compound oneself Propagating combustion process schematic is as shown in Figure 1.This synthesis process utilizes chemical heat release, reduces outer needed for process Portion's heat source;The product of required composition and structure, synthetic impurity content are obtained by the automatic holding reaction that fast automatic wave burns It is low;It can be by the release for changing heat and transmission speed come the composition and knot of the speed of control process, temperature, conversion ratio and product Structure is realized and is adjusted controllably.
In selected reactant raw material, CuO can be decomposed into Cu on a small quantity at high temperature2O and O2, it is expressed asCu2O has the function of catalytic combustion-supporting, can promote the progress reacted under high temperature.
Preferably, described reactant raw material selection common compounds Cu, CuO, Fe2O3Deng all solid powders.
Preferably, selecting laser is continuous wave laser, exports zlasing mode power stability.
Preferably, output wavelength is used to replace common heat source by the laser of 980nm.
Preferably, using laser output spot, determining for conversion zone is realized to the selection of laser facula irradiation position Domain realizes that the material of localization generates.
Preferably, it is adjusted and is controlled using laser power, conversion zone local temperature can effectively controlled in real time, realized steady Fixed reasonable heating, annealing temperature control.
Preferably, the power of superpower laser, sintering region and sintering time comprehensively control are, it can be achieved that set effect Localized hyperthermia's control, product generating process regulate and control comprehensively.
Preferably, gas control, environmental gas N can be carried out to environment is prepared2Guarantee reaction synthesis process without environment gas Body influences.
The preparation of the laser-induced self-propagating reaction high―temperature nuclei cu ferrite material:
Raw material powder is chosen, type and the ratio etc. of reactant can be changed according to actual product demand.
Ready raw material powder is pre-processed, obtains uniformly mixed little particle by modes such as grinding stirrings Powder.Tabletting can also be carried out to powder according to demand.
Self- propagating process is induced by way of laser irradiation, copper ferrite material needed for high―temperature nuclei.The Gao Gong used The laser power of rate laser can carry out feedback adjustment according to the actual situation;The laser facula overlay area of laser output can It is adjusted according to demand, covering part powder area, the growth of generating process self- propagating may be selected;According to the demand purity of product And ingredient, laser power can be adjusted in real time, changed sintering time, controlled self-propagating reaction rate;Laser control reaction is strong Degree, reaction are controllable in real time.This process can synthesize target initial stage product.
The head product that induced with laser generates is processed.Initial stage product can be ground, obtain evengranular production Object powder.Initial stage product can be screened according to product requirements.
Obtain the cu ferrite product that the properties such as granular size, the uniformity meet demand.
Prepare the self-propagating combustion process of cu ferrite class compound as shown in Figure 2.
Embodiment 1
According to molar ratio copper oxide:Di-iron trioxide is 1:1 weighs totally 3 grams of two kinds of compound powders, wherein copper oxide For 1.000g, di-iron trioxide 2.000g.Weighed powder is placed in mortar, mix and is fully ground using alms bowl pestle, So that each compound powder is uniformly mixed.
The tiling of obtained mixed-powder is placed in high-temperature resistant container.It the use of laser is continuous optical semiconductor laser, Wavelength is 980nm, and output power is adjusted to 61W, and output laser irradiation is on powder surface, wherein spot size and tiling powder plane It is in the same size.After continuing 60s, laser is closed, forms the hardened block identical with laser facula size of black at this time.
The product tentatively generated is taken out with tweezers, and tentatively judges that generating product can be attracted using magnet, is iron Magnetisable material.Head product is placed in mortar, is adequately ground with alms bowl pestle, product, which is easily smashed to pieces, is ground into little particle. The product powder i.e. cu ferrite material of even particle size exquisiteness is obtained after sufficient grinding.
Embodiment 2
According to molar ratio copper oxide:Di-iron trioxide is 2:1 weighs totally 3 grams of two kinds of compound powders, wherein copper oxide For 1.500g, di-iron trioxide 1.500g.Weighed powder is placed in mortar, mix and is fully ground using alms bowl pestle, So that each compound powder is uniformly mixed.
Product preparation condition step forms with embodiment 1 and has magnetic hardened bulk identical with laser facula size Object, and product powder i.e. cu ferrite material is obtained after being fully ground.
Embodiment 3
According to molar ratio copper oxide:Di-iron trioxide is 5:2 weigh totally 3 grams of two kinds of compound powders, wherein copper oxide For 1.667g, di-iron trioxide 1.333g.Weighed powder is placed in mortar, mix and is fully ground using alms bowl pestle, So that each compound powder is uniformly mixed.
Product preparation condition step forms with embodiment 1 and has magnetic hardened bulk identical with laser facula size Object, and product powder i.e. cu ferrite material is obtained after being fully ground.
Embodiment 4
According to molar ratio copper oxide:Di-iron trioxide is 4:1 weighs totally 3 grams of two kinds of compound powders, wherein copper oxide For 2.0000g, di-iron trioxide 1.0000g.Weighed powder is placed in mortar, mix and is sufficiently ground using alms bowl pestle Mill, so that each compound powder is uniformly mixed.
Product preparation condition step forms with embodiment 1 and has magnetic hardened bulk identical with laser facula size Object, and product powder i.e. cu ferrite material is obtained after being fully ground.
Embodiment 5
According to molar ratio copper:Copper oxide:Di-iron trioxide is 1:1:1 weighs totally 3.8 grams of three kinds of compound powders, wherein Copper is 0.8000g, copper oxide 1.0000g, di-iron trioxide 2.0000g.Weighed powder is placed in mortar, is mixed And be fully ground using alms bowl pestle, so that each compound powder is uniformly mixed.
Product preparation condition step forms with embodiment 1 and has magnetic hardened bulk identical with laser facula size Object, and product powder i.e. cu ferrite material is obtained after being fully ground.
Each embodiment prepares the XRD diagram of cu ferrite class compound as shown in Figure 3.
Particular embodiments described above, the technical issues of to solution of the invention, technical scheme and beneficial effects carry out It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to The present invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this Within the protection scope of invention.

Claims (5)

1. a kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material, which is characterized in that with the oxidation of copper, copper The oxide of object, iron and iron is raw material, and self-propagating reaction occurs using induced with laser, and raw material reaction is made to generate Cu2O is catalyzed and synthesized The progress of process;Specifically include following steps:
Step 1:Raw material powder needed for choosing, and mixed raw material is mixed to get by raw material is full and uniform;
Step 2:The mixed raw material is placed in reaction vessel;
Step 3:Using laser irradiation on mixed raw material, laser is adjusted, self-propagating reaction occurs for induced with laser, generates copper Ferrite Material head product;
Step 4:Later period grinding is carried out to cu ferrite material head product, obtains that particle is small, cu ferrite material of good evenness; Wherein:
Raw material powder described in step 1 is the oxide of copper, the oxide of copper, iron and iron, is chosen according to actual product demand former The type and ratio at feed powder end;Full and uniform be mixed into obtains uniformly mixed small particle powder by grinding, agitating mode, Or tabletting is carried out to uniformly mixed small particle powder;
Self-propagating reaction occurs for induced with laser described in step 3, which is controlled by changing release and the transmission speed of heat The speed of process, temperature, conversion ratio and product composition and structure.
2. a kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material according to claim 1, feature It is:Laser described in step 3 is continuous wave laser or pulse laser, and output laser wavelength is infrared band;It is described to swash The spectral band of light is infrared band, visible light wave range or infrared and visible light mixing wave band.
3. a kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material according to claim 1, feature It is:For laser irradiation described in step 3 on mixed raw material, the region of irradiation, power, time pass through feedback regulation control System, generates target product according to demand, realizes the real-time controllable of localization to the process that preparation generates product.
4. a kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material according to claim 1, feature It is:It is described adjust laser refer to laser output laser controlling reaction, be able to carry out laser focusing, to sintering region into The control of row spatial distribution, including laser space lattice, laser spacescan.
5. a kind of method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material according to claim 1, feature It is:It prepares environment and carries out gas control, gas N2
CN201810508598.3A 2018-05-24 2018-05-24 The method of laser-induced self-propagating reaction high―temperature nuclei cu ferrite material Pending CN108892177A (en)

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CN109704396A (en) * 2019-01-28 2019-05-03 广东朗研科技有限公司 A kind of preparation method of CaCu 3 Ti 4 O
CN112898005A (en) * 2021-03-24 2021-06-04 云南华谱量子材料有限公司 Preparation method of normal-temperature high-radiance infrared radiation ceramic material
CN112897528A (en) * 2021-03-24 2021-06-04 云南华谱量子材料有限公司 Method for synthesizing boron carbide/carbon powder material by laser sintering
CN115401212A (en) * 2022-08-05 2022-11-29 西安交通大学 P type Cu 2 Additive manufacturing method of Se-based thermoelectric material

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109704396A (en) * 2019-01-28 2019-05-03 广东朗研科技有限公司 A kind of preparation method of CaCu 3 Ti 4 O
CN109704396B (en) * 2019-01-28 2021-06-01 广东朗研科技有限公司 Preparation method of calcium copper titanate
CN112898005A (en) * 2021-03-24 2021-06-04 云南华谱量子材料有限公司 Preparation method of normal-temperature high-radiance infrared radiation ceramic material
CN112897528A (en) * 2021-03-24 2021-06-04 云南华谱量子材料有限公司 Method for synthesizing boron carbide/carbon powder material by laser sintering
CN115401212A (en) * 2022-08-05 2022-11-29 西安交通大学 P type Cu 2 Additive manufacturing method of Se-based thermoelectric material

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