CN101798115B - Preparation method of ternary oxysalt compound micro-nano material - Google Patents
Preparation method of ternary oxysalt compound micro-nano material Download PDFInfo
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- CN101798115B CN101798115B CN2010101181754A CN201010118175A CN101798115B CN 101798115 B CN101798115 B CN 101798115B CN 2010101181754 A CN2010101181754 A CN 2010101181754A CN 201010118175 A CN201010118175 A CN 201010118175A CN 101798115 B CN101798115 B CN 101798115B
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Abstract
The invention discloses a preparation method of a ternary oxysalt compound micro-nano material. The method comprises the following steps: (1) ablating in an electrochemical auxiliary pulse laser liquid to prepare a precursor material; and (2) and heating the precursor material to prepare the ternary oxysalt compound micro-nano material. The obtained micro-nano material can be used for preparing microelectronic devices, lithium ion battery electrode materials or organic synthetic catalysts. The invention synthesizes the ternary compound nano material by ablating a solid target material in the electrochemical auxiliary pulse laser liquid for the first time. The method has the advantages of simple operation and low cost, does not require a strict operating environment, and can prepare the product under the conditions of normal temperature and pressure. The used liquid is de-ionized water, and thus, the synthesized material has the advantages of high purity and no other chemical impurities. Compared with the traditional electrochemical deposition, the one-dimensional micro-nano material synthesized by the invention does not need any template.
Description
Technical field
The invention belongs to ternary oxysalt compound micro little-the synthetic field of Na material, particularly a kind of utilize ablate in the electrochemistry satellite pulse laser liquid prepare ternary oxysalt compound micro little-method of Na material.
Background technology
Nano material is meant that size range is the material of 1～100nm.Particle diameter less than 100nm after, atomicity is comparable in ionic surface atom number and its body.This character has caused nano material the variation of structure that effect caused such as the small size of conventional bulk phase material, big surface and quantum tunneling and energy state to occur being different from, has produced the physics-chem characteristics such as light, electricity, magnetic, mechanics of many uniquenesses.For example nanometer iron has magnetic, original non electrically conductive material and has become conduction, strong catalytic activity etc.These properties make it have application prospects at photoelectron, microelectronics, nanometer electronic device preparation, high performance catalyst, biological field.Also just because of these potential using values, a large amount of research expenditures has all been put in the research and development of nano material, and purpose is for the new method of seeking nano materials and develops the nano material with excellent properties.
At present; Preparation method of nano material mainly comprises physical method and chemical process; Wherein physical method mainly comprises pulsed laser deposition, using vaporization condensation process; Molecular beam epitaxy (MBE), mechanical ball milling method etc., and chemical process mainly comprises chemical vapour deposition, liquid-phase precipitation method, sol-gel method, L B film method, self-assembled monolayer molecule and picture on surface method, the hot method of hydrothermal/solvent, spray pyrolysis and electrochemical process or the like.
Electrochemical process because of self characteristics as can selecting to regulate with CONTROLLED POTENTIAL or electric current, enforcement current potential or current step, add and exchange perturbation signal etc. capablely, for the nanoparticle of preparation particle diameter and controllable shapes provides a kind of effective means.In recent years, electrochemical method is causing people's very big concern aspect the preparation of nano material and the assembling research, and obtains a series of achievement in research.
Electrochemical method synthetic monodimension nanometer material generally all is to adopt the template electrochemical compound method at present; Promptly utilize the aperture to be template for nano level to micron-sized porous material, means such as combined with electrochemical deposition, electroless plating are that material atom or ion deposition form required nanostructure or nanotube on the hole wall of template.
Summary of the invention
In order to solve the weak point that exists in the above-mentioned prior art, primary and foremost purpose of the present invention is to provide a kind of ternary oxysalt compound micro micro-nano preparation methods; This method is utilized the preparation ternary oxysalt compound micro micro-nano material of ablating in the electrochemistry satellite pulse laser liquid; Be a kind of expansion and the innovation that current pulse laser ablation is prepared nano material, can prepare the little-Na material of heterogeneity through adjustment electrode materials, target.
Another purpose of the present invention is to provide a kind of ternary oxysalt compound micro micro-nano material of method for preparing.
A purpose more of the present invention is to provide the application of above-mentioned ternary oxysalt compound micro micro-nano material.
The object of the invention is realized through following technical scheme: a kind of ternary oxysalt compound micro micro-nano preparation methods comprises following operation steps:
(1) utilize the preparation persursor material of ablating in the electrochemistry satellite pulse laser liquid:
To react target and place reaction vessel, in reaction vessel, inject liquid phase substance then, liquid phase substance submergence reaction target; Metal electrode is placed the both sides of container, and metal electrode is linked to each other with additional power source; The light path of regulating impulse laser beam makes laser beam successively through focusing on the surface in contact of reaction target and liquid phase substance behind completely reflecting mirror and the condenser lens, and surface in contact produces plasma plume; Unbalanced pulse laser and additional power source make metal electrode generation anodic oxidation and in liquid phase substance, form uniform electric field, carry out the pulsed laser ablation deposition reaction; React after 60～120 minutes, close the power supply of pulse laser and electric field, reacted liquid phase substance is taken out, drying is separated, and obtains persursor material;
(2) persursor material is added hot preparation ternary oxysalt compound micro micro-nano material:
Persursor material is placed on the high temperature material, and under air atmosphere, temperature is elevated to 550～600 ℃, and constant temperature kept 4～5 hours, was cooled to room temperature, obtained ternary oxysalt compound micro micro-nano material.
The upper surface of the said liquid phase substance of step (1) is higher than reaction target upper surface 5～20mm; The frequency of said pulse laser is 1～10Hz; The voltage of said electric field is 20～300V; Said electric field is DC electric field or alternating-electric field; Said drying is vacuum-drying, and the exsiccant temperature is 70～80 ℃.
The purity of the said reaction target of step (1) is that mass content is 99%～99.999%; Said reaction target is aluminium, vanadium, copper, iron, zinc, manganese, titanium, chromium, molybdenum, niobium, tantalum or tungsten; The target thickness of said reaction target is 3～15 millimeters; Being shaped as of said reaction target is circular or square, and the surface of reaction target polishes processing.
The said metal electrode of step (1) is magnesium, aluminium, titanium, vanadium, copper, iron, zinc, manganese, molybdenum, barium, nickel, lead, bismuth, yttrium, lutetium, lanthanum, samarium, cerium, praseodymium or neodymium; Said liquid phase substance is that deionized water or volumetric molar concentration are 10
-3Mol.L
-1～2mol.L
-1Salts solution.Said salts solution preferably sulfuric acid copper solutions or silver nitrate solution.
The said reaction vessel of step (1) is Glass Containers and plastic containers; Being shaped as of said reaction vessel is square or circular.Said Glass Containers is normal silicate Glass Containers or quartz container.
The said high temperature material of step (2) is Al
2O
3Ceramic plate.
A kind of ternary oxysalt compound micro micro-nano material according to method for preparing.
Above-mentioned ternary oxysalt compound micro micro-nano material can be applicable to prepare microelectronic device, lithium ion battery electrode material or organic catalyst compound.
Pulse laser ablation solid target also is a kind of particularly effective ways of metal and metal nanoparticle of micro-nano material that prepare in the liquid; Its cardinal principle is to utilize pulse laser and the solid target that places liquid to interact, and in liquid-solid interface, produces the plasma plume brightness.The restriction that the plasma plume brightness receives liquid produces a HTHP district, and this zone provides reaction between reaction, ablation thing and the liquid between condition such as the ablation thing etc. for some chemical reactions.
The present invention compared with prior art has following advantage and beneficial effect:
(1) the present invention receives material through ablation solid target synthesis of ternary compound in the electrochemistry satellite pulse laser liquid first; This method is simple to operate, and is with low cost, and do not have harsh operating environment requirement, can under normal temperature and pressure conditions, realize the preparation of product.
(2) the used liquid of the present invention is deionized water, so its synthetic material purity is higher, does not have other impurity atom.
(3) with Traditional electrochemical sediment-filled phase ratio, institute's synthetic one dimension micro-nano material need not to add any template among the present invention.
Description of drawings
Fig. 1 uses the structural representation of equipment for the present invention, and wherein Fig. 1 (a) is the structural representation that step 1 is used equipment, and Fig. 1 (b) be the structural representation of step 1 use equipment; 1 is pulsed laser; 2 is total reflective mirror; 3 is condensing lens; 4 are the reaction target; 5 is D.C. regulated power supply; 6 is thin electrode; 7 is quartz cell; 8 is process furnace; 9 is ceramic plate; 10 persursor materials for the dry gained of pulse laser ablation gained product liquid in the experiment.
The two molybdic acid copper (Cu that Fig. 2 prepares for embodiment 1
3Mo
2O
9) a micro-nano rod emission electromicroscopic photograph figure.
The two molybdic acid copper (Cu that Fig. 3 prepares for embodiment 1
3Mo
2O
9) the X-ray diffraction analysis collection of illustrative plates of micro-nano rod.
The two molybdic acid copper (Cu that Fig. 4 prepares for embodiment 1
3Mo
2O
9) infrared spectrogram of micro-nano rod.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
As shown in Figure 1; Equipment of the present invention has comprised that laser apparatus 1 (adopts the Nd:YAG pulse laser; Optical maser wavelength 532nm; Pulsewidth 10ns, energy are 2.95mJ, and frequency is 5Hz), total reflective mirror 2, condenser lens 3, reaction target 4, D.C. regulated power supply 5, electrode thin slice 6, quartz cell 7, process furnace 8, ceramic plate 9 and dry separating obtained presoma material 10.At first copper electrode thin slice 6 is fixed on the both sides, two ends of quartz cell 7, reaction target 4 is placed on the centre of quartz cell 7 and injects liquid phase substance; Then electrode 6 and D.C. regulated power supply 5 usefulness leads are coupled together, regulate light path and make pulse laser just focus on reaction target 4 surfaces.When carrying out pulse laser ablation, with the VR of D.C. regulated power supply 5 to 20v.
(1) adopt aforesaid device, reaction target 4 is circular high-purity molybdenum target (purity is 99.99%), and diameter is 10mm, thick 5mm; Electrode thin slice 6 is the copper electrode thin slice; High-purity molybdenum target is put into quartz cell, in quartz cell, inject deionized water, make deionized water submergence reaction target, and the upper surface of deionized water is higher than target upper surface 5mm; Regulate laser optical path, the pulsed laser beam that makes the pulsed laser emission is through total reflective mirror with through behind the condenser lens, and the laser radiation of focusing is at the surface in contact of high-purity molybdenum target and deionized water, and surface in contact produces plasma plume; Unbalanced pulse laser and D.C. regulated power supply; Laser frequency is selected 5Hz; The VR of D.C. regulated power supply is carried in the positive and negative two ends of electrode to 20v, thereby around the reaction target, forms a gradient electric field, carry out the pulse laser ablation reaction; Reaction process continues 120 minutes, closes pulse laser and power supply.The reacted deionized water of will ablating takes out, and it is dropped on the monocrystalline silicon piece substrate, puts into vacuum-drying and under 70 ℃, carries out drying collection and obtain persursor material;
(2) persursor material is placed on the alumina ceramic plate, ceramic plate is put in the process furnace, under 600 ℃, carried out heat treated 5 hours, whole heat-processed keeps and atmosphere, is cooled to room temperature, obtains product.
Above-mentioned products obtained therefrom is carried out field emission microscope analysis, X-ray diffraction and IR spectroscopy test:
The field emission microscope photo is as shown in Figure 2, and visible by figure, the diameter of most nanometer rod is at 100～250nm, and length is at 1～5 μ.
The X-ray diffraction analysis collection of illustrative plates is as shown in Figure 3, according to test result, can confirm that the nanometer rod that makes is two molybdic acid copper (Cu of rhombic system
3Mo
2O
9).
The IR spectroscopy spectrogram is as shown in Figure 4,1106cm among the figure
-1The absorption peak at place is substrate Si O
2Absorption peak, 970,941,893,810774,709,516cm
-1Be Cu
3Mo
2O
9Charateristic avsorption band (document Inorganic Chemistry, 2009,48; 2687-2692 and Journal of Solid StateChemistry, 2007,180; 119-126), thus this test result proved that further prepared that obtain is two molybdic acid copper (Cu through this method
3Mo
2O
9) material.
Through above-mentioned characterization method, but the nanometer rod that the knowledge capital invention prepares is two molybdic acid copper (Cu of rhombic system
3Mo
2O
9) the micro-nano rod, because its yardstick reaches near nanoscale, have the very high specific surface area that gets, be with a wide range of applications at aspects such as catalytic field and lithium ion battery electrode materials.
(1) adopt the used equipment of embodiment 1, reaction target 4 is circular high-purity molybdenum targets (purity is 99.999%), and diameter is 10mm, thick 5mm; Electrode thin slice 6 is the zinc electrode thin slice; High-purity molybdenum target is put into quartz cell, in quartz cell, inject time deionized water, make deionized water submergence reaction target, and the upper surface of deionized water is higher than target upper surface 8mm; Regulate laser optical path, after the pulsed laser beam that pulsed laser is launched was the condenser lens of 500mm through total reflective mirror with through focal length, the laser radiation of focusing was at the surface in contact of high-purity molybdenum target and deionized water, and surface in contact produces plasma plume; Unbalanced pulse laser and D.C. regulated power supply; Laser frequency is selected 10Hz; The VR of D.C. regulated power supply is carried in the positive and negative two ends of electrode to 50v, thereby around the reaction target, forms a gradient electric field, carry out the pulse laser ablation reaction; Reaction process continues 60 minutes, closes pulse laser and power supply.The reacted deionized water of will ablating takes out, and it is dropped on the monocrystalline silicon piece substrate, puts into vacuum drying oven and under 80 ℃, carries out drying collection and obtain persursor material;
(2) persursor material is placed on the alumina ceramic plate, the ceramic plate that is carrying persursor material is put in the process furnace, under 600 ℃, carried out heat treated 4.5 hours, whole heat-processed keeps and atmosphere, is cooled to room temperature, obtains product.
Products obtained therefrom is carried out various tests (comprising field emission microscope analysis, X-ray diffraction and IR spectroscopy), can obtain two zinc molybdates little-the Na material.
(1) adopt the used equipment of embodiment 1, reaction target 4 is circular high purity vanadium targets (purity is 99%), and diameter is 10mm, thick 15mm; Electrode thin slice 6 is the bismuth pole thin slice; The high purity vanadium target is put into the normal silicate Glass Containers, and in the normal silicate Glass Containers, injecting volumetric molar concentration is 2mol.L
-1Silver nitrate solution, make silver nitrate solution submergence reaction target, and the upper surface of silver nitrate solution is higher than target upper surface 10mm; Regulate laser optical path, after the pulsed laser beam that pulsed laser is launched was the condenser lens of 100mm through total reflective mirror with through focal length, the laser radiation of focusing was at the surface in contact of high purity vanadium target and silver nitrate solution, and surface in contact produces plasma plume; Unbalanced pulse laser and D.C. regulated power supply; Laser frequency is selected 3Hz; The VR of D.C. regulated power supply is carried in the positive and negative two ends of electrode to 300v, thereby around the reaction target, forms a gradient electric field, carry out the pulse laser ablation reaction; Reaction process continues 100 minutes, closes pulse laser and power supply.The reacted silver nitrate solution of will ablating takes out, and it is dropped on the monocrystalline silicon piece substrate, puts into vacuum drying oven and under 70 ℃, carries out drying collection and obtain persursor material;
(2) persursor material is placed on the alumina ceramic plate, the ceramic plate that is carrying persursor material is put in the process furnace, under 580 ℃, carried out heat treated 4 hours, whole heat-processed keeps and atmosphere, is cooled to room temperature, obtains product.
Products obtained therefrom is carried out various tests (comprising the field emission microscope analysis, X-ray diffraction and IR spectroscopy), can obtain pucherite little-the Na material.
(1) adopt the used equipment of embodiment 1, reaction target 4 is the high-purity tungsten target of quadrate (purity is 99.99%), and diameter is 10mm, thick 10mm; Electrode thin slice 6 is the zinc electrode thin slice; High-purity tungsten target is put into quartz cell, and in quartz cell, injecting volumetric molar concentration is 10
-3Mol.L
-1Copper-bath, make copper-bath submergence reaction target, and the upper surface of copper-bath is higher than target upper surface 20mm; Regulate laser optical path, after the pulsed laser beam that pulsed laser is launched was the condenser lens of 100mm through total reflective mirror with through focal length, the laser radiation of focusing was at the surface in contact of high-purity tungsten target and copper-bath, and surface in contact produces plasma plume; Unbalanced pulse laser and D.C. regulated power supply; Laser frequency is selected 1Hz; The VR of D.C. regulated power supply is carried in the positive and negative two ends of electrode to 200v, thereby around the reaction target, forms a gradient electric field, carry out the pulse laser ablation reaction; Reaction process continues 80 minutes, closes pulse laser and power supply.The reacted copper-bath of will ablating takes out, and it is dropped on the monocrystalline silicon piece substrate, puts into vacuum drying oven and under 75 ℃, carries out drying collection and obtain persursor material;
(2) persursor material is placed on the alumina ceramic plate, the ceramic plate that is carrying persursor material is put in the process furnace, under 550 ℃, carried out heat treated 5 hours, whole heat-processed keeps and atmosphere, is cooled to room temperature, obtains product.
Products obtained therefrom is carried out various tests (comprising the field emission microscope analysis, X-ray diffraction and IR spectroscopy), just can obtain zinc tungstate little-the Na particle.
(1) adopt the used equipment of embodiment 1, reaction target 4 is quadrate high purity titanium target (purity is 99.99%), and diameter is 10mm, thick 15mm; Electrode thin slice 6 is a barium electrode thin slice; The high purity titanium target is put into quartz cell, in quartz cell, inject time deionized water, make deionized water submergence reaction target, and the upper surface of deionized water is higher than target upper surface 20mm; Regulate laser optical path, after the pulsed laser beam that pulsed laser is launched was the condenser lens of 100mm through total reflective mirror with through focal length, the laser radiation of focusing was at the surface in contact of high-purity tungsten target and deionized water, and surface in contact produces plasma plume; Unbalanced pulse laser and D.C. regulated power supply; Laser frequency is selected 3Hz; The VR of D.C. regulated power supply is carried in the positive and negative two ends of electrode to 120v, thereby around the reaction target, forms a gradient electric field, carry out the pulse laser ablation reaction; Reaction process continues 120 minutes, closes pulse laser and power supply.The reacted deionized water of will ablating takes out, and it is dropped on the monocrystalline silicon piece substrate, puts into vacuum drying oven and under 78 ℃, carries out drying collection and obtain persursor material;
(2) persursor material is placed on the alumina ceramic plate, the ceramic plate that is carrying persursor material is put in the process furnace, under 600 ℃, carried out heat treated 5 hours, whole heat-processed keeps and atmosphere, is cooled to room temperature, obtains product.
Products obtained therefrom is carried out various tests (comprising the field emission microscope analysis, X-ray diffraction and IR spectroscopy), just can obtain barium titanate little-the Na particle.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. ternary oxysalt compound micro micro-nano preparation methods is characterized in that comprising following operation steps:
(1) utilize the preparation persursor material of ablating in the electrochemistry satellite pulse laser liquid:
To react target and place reaction vessel, in reaction vessel, inject liquid phase substance then, liquid phase substance submergence reaction target; Metal electrode is placed the both sides of container, and metal electrode is linked to each other with additional power source; The light path of regulating impulse laser beam makes laser beam successively through focusing on the surface in contact of reaction target and liquid phase substance behind completely reflecting mirror and the condenser lens, and surface in contact produces plasma plume; Unbalanced pulse laser and additional power source make metal electrode generation anodic oxidation and in liquid phase substance, form uniform electric field, carry out the pulsed laser ablation deposition reaction; React after 60～120 minutes, close the power supply of pulse laser and electric field, reacted liquid phase substance is taken out, drying is separated, and obtains persursor material;
The purity of said reaction target is that mass content is 99%～99.999%; Said reaction target is aluminium, vanadium, copper, iron, zinc, manganese, titanium, chromium, molybdenum, niobium, tantalum or tungsten; Said metal electrode is magnesium, aluminium, titanium, vanadium, copper, iron, zinc, manganese, molybdenum, barium, nickel, lead, bismuth, yttrium, lutetium, lanthanum, samarium, cerium, praseodymium or neodymium;
(2) persursor material is added hot preparation ternary oxysalt compound micro micro-nano material:
Persursor material is placed on the high temperature material, and under air atmosphere, temperature is elevated to 550～600 ℃, and constant temperature kept 4～5 hours, was cooled to room temperature, obtained ternary oxysalt compound micro micro-nano material.
2. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 1 is characterized in that: the upper surface of the said liquid phase substance of step (1) is higher than reaction target upper surface 5～20mm; The frequency of said pulse laser is 1～10Hz; The voltage of said electric field is 20～300V; Said electric field is DC electric field or alternating-electric field; Said drying is vacuum-drying, and the exsiccant temperature is 70～80 ℃.
3. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 1 is characterized in that: the target thickness of the said reaction target of step (1) is 3～15 millimeters; Being shaped as of said reaction target is circular or square, and the surface of reaction target polishes processing.
4. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 1 is characterized in that: the said liquid phase substance of step (1) is that deionized water or volumetric molar concentration are 10
-3Mol
.L
-1～2mol
.L
-1Salts solution.
5. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 4, it is characterized in that: said salts solution is copper-bath or silver nitrate solution.
6. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 1 is characterized in that: the said reaction vessel of step (1) is Glass Containers and plastic containers; Being shaped as of said reaction vessel is square or circular.
7. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 6, it is characterized in that: said Glass Containers is normal silicate Glass Containers or quartz container.
8. a kind of ternary oxysalt compound micro micro-nano preparation methods according to claim 1 is characterized in that: the said high temperature material of step (2) is Al
2O
3Ceramic plate.
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| CN102189271B (en) * | 2011-06-18 | 2013-04-17 | 中国科学院合肥物质科学研究院 | Method for preparing Ag/TiO2 nano composite material |
| CN102649162B (en) * | 2012-04-26 | 2014-09-17 | 中山大学 | Method for preparing noble metal nano material or transitional metal oxide nano material |
| CN104528807A (en) * | 2015-01-05 | 2015-04-22 | 南京航空航天大学 | Preparation method for multibasic oxide nanometer material |
| CN105268996B (en) * | 2015-12-02 | 2018-05-15 | 中国科学院物理研究所 | Prepare device and its operating method and the application of the controllable nano particle of size |
| CN105366954B (en) * | 2015-12-04 | 2017-12-12 | 南京理工大学 | A kind of preparation method of nanometer tungsten oxide electrochomeric films |
| CN107978740A (en) * | 2017-11-16 | 2018-05-01 | 格林美（无锡）能源材料有限公司 | A kind of laser burn preparation method of nickel-cobalt-manganternary ternary anode material |
| CN112439422A (en) * | 2020-12-07 | 2021-03-05 | 岭南师范学院 | Cu3Mo2O9/BiVO4Nano heterostructure composite material and preparation method and application thereof |
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