CN100522800C - Process for producing microparticle and apparatus therefor - Google Patents

Process for producing microparticle and apparatus therefor Download PDF

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Publication number
CN100522800C
CN100522800C CNB200480041059XA CN200480041059A CN100522800C CN 100522800 C CN100522800 C CN 100522800C CN B200480041059X A CNB200480041059X A CN B200480041059XA CN 200480041059 A CN200480041059 A CN 200480041059A CN 100522800 C CN100522800 C CN 100522800C
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particulate
liquid
fluid
powder
production
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CN1906125A (en
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高桥诚一郎
渡边弘
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
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    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
    • C01B13/322—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state
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Abstract

A process for producing microparticles that is capable of producing microparticles, such as those of oxides, by means of simple apparatus at low cost and that is suitable to production of ITO powder; and an apparatus therefor. There is provided a process for producing microparticles, comprising feeding a raw material in the form of a liquid stream, liquid droplets or powder into a heat source; trapping any product in the form of microparticles by means of a foggy liquid fluid; and recovering the microparticles in the form of slurry through gas-liquid separation.

Description

The manufacture method of particulate and producing apparatus
Technical field
The present invention relates to manufacture method and producing apparatus such as indium oxide-tin oxide body particulate.
Background technology
Sputter is the well-known technology that is used to form film.In sputtering technology,, sputtering target forms film by being carried out sputter.Sputtering technology is used to industrial processes, because can form the film of high surface area easily, and can form high performance film with high-level efficiency.In recent years, various sputtering technologies are known, for example reactive sputtering; I.e. sputter in reactant gas, and magnetron sputtering, it has realized that by the back side that magnet is placed target the film of two-forty forms.
Among the film product that obtains by sputter, Indium sesquioxide-stannic oxide (In 2O 3-SnO 2Composite oxides, hereafter are ITO) film, owing to have high optical clarity and have high electroconductibility for visible light, therefore it has obtained using widely as nesa coating, for example be used for liquid-crystal display, be used for the hot film of life and the IR reflective film of the demist of glass.
Therefore, for high-level efficiency more with produce film more cheaply, need improve and improve sputtering condition and sputtering equipment, now still in the middle of carrying out, and the valid function of sputtering equipment be essential.Producing in the ito thin film by sputter, from new sputtering target being installed to period that initial arc (paradoxical discharge) finishes, promptly cause film and form needed period, preferably short as far as possible, but and estimate from (the accumulative total sputtering time: target lifetime) be a key issue in sputter period that the installation of target begins.
The aforementioned sputtering target that is used to form ito thin film is to make by the following method: with predetermined proportion mixed oxidization indium powder and putty powder, form under dry state or hygrometric state, then thermal sintering product (patent documentation 1).In this respect, but the Indium sesquioxide powder that has proposed high dispersing to produce high density ITO sintered compact (for example referring to patent documentation 2,3 and 4).
Another kind of currently known methods comprises that sintering passes through coprecipitation method synthetic ITO powder (for example referring to patent documentation 5) under hygrometric state.Similarly, propose the multiple wet synthetic method that is used to produce the ITO powder and be used for producing highdensity sintering ITO (for example referring to patent documentation 6-9).
Proposed to produce another method of ITO powder, indium-tin alloy is reacted with oxygen in plasma arc, the air-flow that passes through Mach number 〉=1 subsequently is with the predetermined or reaction product (referring to patent documentation 10) of rate of cooling cooling faster.Yet the use of the high velocity air of Mach number 〉=1 needs big equipment, and this can hinder the low cost and the high efficiency production of ITO powder.
Except that ITO powder production method, proposed to produce the following method of metal oxide microparticle.For example proposed several different methods, comprised metal-powder is sent into burner flame, to produce the oxide compound ultrafine particulate thus, consolidated subsequently-gas separation (for example referring to patent documentation 11-16).Method below also having proposed comprises gas injection forming metal-powder thus in molten metal; By this powder of gas delivery; And this powder sent into react as in chemical reaction or the spissated liquid, form micro mist (referring to patent documentation 17) thus.In addition, proposed to form ultramicronized method, comprised to source applying plasma arc, melted and evaporate this source thus, and spray reaction/cooling gas (referring to patent documentation 18-20) to vaporized gas such as reguline metal or metal oxide rod.
Yet above-mentioned dried synthetic method may be not suitable for producing the ITO powder.Therefore, at present, the dry method of not carrying out the ITO powder on the technical scale is synthetic.
Patent documentation 1: Japanese Patent Application Publication No.62-21751
Patent documentation 2: Japanese Patent Application Publication No.5-193939
Patent documentation 3: Japanese Patent Application Publication No.6-191846
Patent documentation 4: Japanese Patent Application Publication No.2001-261336
Patent documentation 5: Japanese Patent Application Publication No.62-21751
Patent documentation 6: Japanese Patent Application Publication No.9-221322
Patent documentation 7: Japanese Patent Application Publication No.2000-281337
Patent documentation 8: Japanese Patent Application Publication No.2001-172018
Patent documentation 9: Japanese Patent Application Publication No.2002-68744
Patent documentation 10: Japanese Patent Application Publication No.11-11946
Patent documentation 11: Japanese patent laid-open publication gazette No.1-55201
Patent documentation 12: Japanese patent laid-open publication gazette No.5-77601
Patent documentation 13: Japanese Patent No.3253338
Patent documentation 14: Japanese Patent No.3253339
Patent documentation 15: Japanese Patent No.3229353
Patent documentation 16: Japanese Patent No.3225073
Patent documentation 17: Japanese Patent Application Publication No.60-71037
Patent documentation 18: Japanese Patent Application Publication No.2002-253953
Patent documentation 19: Japanese Patent Application Publication No.2002-253954
Patent documentation 20: Japanese Patent Application Publication No.2002-263474
Summary of the invention
The problem that the present invention is to be solved
Under such situation, the purpose of this invention is to provide the method for producing particulate, this method can be by simple device with the low cost production particulate of oxide fine particle for example, and this method is suitable for producing the ITO powder.Another object of the present invention provides the equipment of producing this particulate.
The mode of dealing with problems
Be used for the first kind of pattern of the present invention that achieve the above object, the method for producing particulate is provided, it is characterized in that this method comprises that the raw material with liquid stream, drop or powder form infeeds thermal source; Capture the product of the particulate form that forms by the fluid of fog-like liquid; And separate with slurry form by solution-air and to collect particulate, wherein said thermal source is the thermal source that flame is arranged.
According to first kind of pattern, can effectively raw material be infeeded the product that thermal source obtains by the fog-like liquid fluid, and separate the particulate of effectively collecting with slurry form by solution-air with the particulate form capture.
Second kind of pattern of the present invention can be depicted as the particular of the method for first kind of pattern, wherein provides the raw material of waiting to infeed thermal source by melting material being formed liquid stream or drop.
According to second kind of pattern, the liquid stream that can will be formed by the melting material of for example metal or alloy in thermal source or the raw material of drop form are transformed into its oxide compound, and can capture oxide compound with particulate form by the fog-like liquid fluid.
The third pattern of the present invention can be depicted as the particular of the method for first kind of pattern, and the raw material of wherein waiting to infeed thermal source is the form of atomizing powder.
According to the third pattern, the raw material of the atomized powder bodily form formula that will be formed by the raw material of for example metal or alloy infeeds thermal source, forms its particulate thus.
The 4th kind of pattern of the present invention can be depicted as first particular to any one method of the third pattern, wherein carries out solution-air by cyclonic separator and separates.
According to the 4th kind of pattern, can separate by the solution-air of utilizing cyclonic separator to carry out particulate is collected as the slurry of liquid fluid.
The 5th kind of pattern of the present invention can be depicted as the particular of first to fourth kind of any one method of pattern, and wherein this thermal source is acetylene flame or DC flame passes.
According to the 5th kind of pattern, make raw material form its particulate by acetylene flame or DC flame passes.
The 6th kind of pattern of the present invention can be depicted as the particular of first to the 5th kind of any one method of pattern, and wherein this liquid fluid is a water.
According to the 6th kind of pattern, water captures product, and collects the slurry of product-water.
The 7th kind of pattern of the present invention can be depicted as the particular of first to the 6th kind of any one method of pattern, and wherein this raw material is to be selected from least a in metal, alloy, oxide compound, nitride and the oxynitride.
According to the 7th kind of pattern, for example raw material of metal, alloy, oxide compound, nitride and oxynitride is formed its particulate.
The 8th kind of pattern of the present invention can be depicted as the particular of first to the 7th kind of any one method of pattern, and wherein this thermal source is oxidizing atmosphere or nitriding atmosphere, produces oxide fine particle, nitride particulate and oxynitride particulate thus.
According to the 8th kind of pattern, in as the oxidizing atmosphere of thermal source or nitriding atmosphere, raw material is transformed into oxide fine particle, nitride particulate or oxynitride particulate.
The 9th kind of pattern of the present invention can be depicted as the particular of first to the 7th kind of any one method of pattern, and wherein raw material is In-Sn alloy or ITO powder, by this raw material production indium oxide-tin oxide body.
According to the 9th kind of pattern, produce the slurry of ITO powder by In-Sn alloy or ITO powder.
The of the present invention ten kind of pattern can be depicted as the particular of the method for the 9th kind of pattern, and this embodiment is produced the indium oxide-tin oxide body, and the tin content of this powder is the 2.3-45 mass percent, based on SnO 2Calculate.
According to the tenth kind of pattern, ITO has kept electroconductibility by the stannic oxide of predetermined amount.
The 11 kind of pattern of the present invention can be depicted as the particular of first to the tenth kind of any one method of pattern, and wherein when capturing product by liquid fluid, product flows with 150m/s or littler maximum rate.
According to the 11 kind of pattern, can under low relatively product flow velocity, produce particulate.
In the 12 kind of pattern of the present invention, provide the equipment of producing particulate, it is characterized in that this equipment comprises:
Be used for the import with gaseous fluid and product introducing device interior, this product is to infeed thermal source by the raw material with liquid stream, drop or powder form to obtain;
Be used for spraying fog-like liquid fluidic fluid jet device to the product of introducing;
Being used for that the particulate that is captured by liquid fluid is carried out solution-air separates so that form first gas-liquid separation device of particulate slurry thus; With
An atmosphere fluidic part that is used for comprising not the particulate that is captured by liquid fluid turns back to first circulation device of fluid jet device position.
According to the 12 kind of pattern, utilize fog-like liquid to capture raw material is infeeded the product that thermal source obtains with the fluid fine particle form, carry out solution-air subsequently and separate, and at least a portion atmosphere fluid is circulated by circulation device, carry out another time solution-air subsequently and separate.Thus, can effectively collect particulate.
The 13 kind of pattern of the present invention can be depicted as the particular of the equipment of the 12 kind of pattern, this equipment further comprises second gas-liquid separation device in the first gas-liquid separation device downstream side, the atmosphere fluidic part of the particulate that is captured by liquid fluid is provided second gas-liquid separation device to be used to introduce to comprise not, be used for to atmosphere fluid jet fog-like liquid fluid, and be used to carry out the solution-air separation, obtain the slurry of particulate thus.
According to the 13 kind of pattern, the particulate that can not be collected by the effective collection of second gas-liquid separation device.
The 14 kind of pattern of the present invention can be depicted as the particular of the equipment of the 13 kind of pattern, this equipment further comprises second circulation device in the downstream side of second gas-liquid separation device, and this circulation device is used for and will comprises the inlet that a particulate atmosphere fluidic part that is not trapped by liquid fluid turns back to second gas-liquid separation device.
According to the 14 kind of pattern, separate, effectively collect particulate thus not providing the atmosphere gas of slurry further to carry out solution-air by second gas-liquid separation device.
The 15 kind of pattern of the present invention can be depicted as the particular of the 12 to the 14 kind of any one equipment of pattern, and wherein first gas-liquid separation device is a cyclonic separator.
According to the 15 kind of pattern, can carry out solution-air continuously and effectively by cyclonic separator and separate.
The 16 kind of pattern of the present invention can be depicted as the particular of the 12 to the 15 kind of any one equipment of pattern, wherein when the liquid fluid trap particles of spraying by fluid jet device, fluid flows with 150m/s or littler maximum rate.
According to the 16 kind of pattern, can produce particulate with low relatively flow velocity.
The invention effect
As indicated above, according to the present invention, the feed metal or the alloy of liquid stream, drop or powder form infeeded thermal source, and capture the product of the particulate form that forms by the fog-like liquid fluid.Thus, can effectively produce particulate in simple mode.
The accompanying drawing summary
Fig. 1: the diagrammatic layout of an embodiment of particulate production unit of the present invention.
Fig. 2: the X-ray diffractogram of the ITO powder of producing in the embodiment of the invention 1.
Fig. 3: the X-ray diffractogram of the ITO powder of producing in the embodiment of the invention 2.
Fig. 4: the X-ray diffractogram of the ITO powder of producing in the comparative example 1 of the present invention.
Fig. 5: the X-ray diffractogram of the ITO powder of producing in the comparative example 2 of the present invention.
Fig. 6: the X-ray diffractogram of the ITO powder of producing in the comparative example 3 of the present invention.
Fig. 7: the X-ray diffractogram of the ITO powder of producing in the embodiment of the invention 3.
Fig. 8: the X-ray diffractogram of the ITO powder of producing in the comparative example 4 of the present invention.
Implement best mode of the present invention
According to the method for production particulate of the present invention, the raw material of liquid stream, drop or powder form is infeeded thermal source.
This raw material can be a metal or alloy for example, and concrete example comprises the metal such as Mg, Al, Zr, Fe, Si, In and Sn, and their alloy.This raw material can be above-mentioned oxide compound, nitride and the oxynitride of any this metal or alloy.Here used " oxide compound " comprises composite oxides, and " nitride " comprises complex nitride.
Raw material fusing to be infeeded can be formed liquid stream or drop, raw material perhaps to be infeeded can be a powder.In other words, molten metal can be poured out continuously with liquid stream or drop form from container.Perhaps, raw material to be infeeded can be formed the atomizing powder.
In using the situation of In-Sn alloy, can produce the ITO powder as raw material.In addition, when using the ITO powder, can produce dissimilar ITO materials as raw material.
This thermal source can be oxidizing atmosphere or nitriding atmosphere, and concrete example comprises acetylene flame and DC flame passes.Temperature to thermal source does not have concrete restriction, if this thermal source can the deposite metal, alloy, oxide compound, nitride or oxynitride, and fully oxidation or nitrogenization raw material.What can expect is, this temperature is at least thousands of degrees centigrade in acetylene flame situation, and temperature is at least tens thousand of degrees centigrade in the DC flame passes.
When infeeding the raw material of liquid stream, drop or powder form in above-mentioned acetylene flame or the DC flame passes, produce air-flow raw material itself, corresponding oxide compound, corresponding nitride or corresponding oxynitride as product.According to the state of flame, this product can be raw material self (being metal or alloy) or corresponding oxide compound, nitride or oxynitride.In other words, when this flame is oxidizing atmosphere, form the oxide compound or the oxynitride of metal or alloy, yet when this flame is nitriding atmosphere, form the nitride or the oxynitride of metal or alloy.Perhaps, when using oxide compound, nitride or oxynitride, can form dissimilar oxide compounds, nitride or oxynitride as raw material.
According to the present invention, capture the product that forms by the fog-like liquid fluid.Particularly, with the fog-like liquid fluid, preferred spray water xi is ejected on the product that jet delivered of acetylene flame or DC flame passes generation.By the effect of fog-like liquid fluidic, product is formed particulate by chilling, and produces the slurry that comprises the particulate in the atomizing of liquids.
Treating the fog-like liquid type of fluid that infeeds does not have concrete restriction, as long as this fluid can capture and cooled product.For example, when making water, the water under the environment for use temperature (preferred pure water).Perhaps, also can use cold water.
When the product of trap particles form, this product preferably flows with about 100m/s or littler top speed with for example 150m/s or littler.
According to the present invention, the liquid fluid that comprises the particulate that traps by the atomizing of liquids fluid is carried out solution-air separate, collect particulate with the form of slurry thus.The method of collecting slurry is not had concrete restriction, and preferably use cyclonic separator.
According to method of the present invention, when using In-Sn alloy or ITO powder, can produce the powder of Indium sesquioxide-stannic oxide (ITO) as raw material.So the ITO powder that produces comprises and is dissolved in In in a large number 2O 3In SnO 2The sosoloid component.Therefore, this ITO shows high sinterability and highdensity sintering ITO is provided easily.As a result, can produce long-life sputtering target.When using the ITO powder produced by various production methods or the ITO powder by pulverizing sintering ITO generation as raw material, it is different with material powder and comprise and be dissolved in In in a large number to produce characteristic 2O 3In SnO 2The dissimilar ITO powder of sosoloid component.
Can use the material of above-mentioned ITO powder as the ITO sputtering target.The ITO sputter target material preferably has the tin content of 2.3 to 45 mass percents, based on SnO 2Calculate.
Embodiment
An embodiment of particulate production unit of the present invention is described with reference to Fig. 1 below.
This equipment has the inlet 10 that is used for introducing to device interior gaseous fluid and product 3, infeeds as thermal source and can provide in the flame 1 (acetylene flame or DC flame passes) of oxidizing atmosphere or nitriding atmosphere by the raw material 2 (for example metal and alloy) with liquid stream, drop or powder form to obtain product 3; Be used for spraying fog-like liquid fluidic fluid jet device 20 to the particulate of introducing; As the cyclonic separator 30 of gas-liquid separation device, so that being carried out solution-air, separates the particulate that is captured by liquid fluid, thus the slurry of formation particulate; With the circulation device 40 that is used for the atmosphere fluid that a part comprises not the particulate that is captured by liquid fluid is turned back to the fluid jet device position.
10 the type of entering the mouth there is not concrete restriction, as long as this inlet allows that the air-flow that comprises product infeeds device interior.This inlet can be a getter device.
In conduit 11, provide fluid jet device 20 in the downstream side of inlet 10.This fluid jet device 20 comprises, for example a plurality of injection nozzles that are used to spray water 21 feed to the pump 22 of injection nozzle 21 and the fluid container 23 of storing fluid with fluid.Fluidic injection direction by injection nozzle 21 ejections there is not concrete restriction.Yet this injection direction is preferably, and makes to spray fluid and merge by 10 air-flows of introducing that enter the mouth.To be included in by product 3 coolings in 10 gaseous fluids of introducing that enter the mouth so that form particulate by fog-like liquid fluid (for example water), and capture this particulate.In conduit 11, the Wen's pipeline section 12 that provides stream to narrow down in the downstream side of injection nozzle 21 reduces so that prevent the flow velocity of liquid-gas mixture.Providing of Wen's pipeline section 12 is not necessary.And nonessential injection nozzle 21 and the pump 22 of providing, on the contrary, can be based on the suction atomizing of liquids of gas flow generation.
Providing inlet 10 conduit 11 links to each other with inlet 31 as the cyclonic separator 30 of gas-liquid separation device.Form around cyclonic separation body 32 inwall progressive eddy current 33 by 31 solution-airmixtures that are incorporated in the cyclonic separator 30 that enter the mouth, thus that liquid ingredient is separated from the gas.Liquid ingredient promptly comprises the slurry of particulate, descends in cyclonic separator 30, and by exhaust outlet 34 gaseous fraction is discharged.
In the equipment of this embodiment, provide circulation device 40 so that link to each other with exhaust outlet 34.In other words, circulating line 41 34 links to each other with outlet, and near inlet 10 positions of circulating line 41 and conduit 11 link to each other.Gas blower 42 is among circulation tube 41.Circulation device 40 is made up of parts 41 and 42.By circulation device 40, the powder of collection at large is turned back to the upstream side of injection nozzle 21, thereby improve collection efficiency.
To discharge and be stored in the fluid container 23 by drain outlet 36 by cyclonic separator 30 liquid ingredients separated from the gas.By the upper strata clear water circulation of circulation device 40 with slurry in the container 23, the concentration that comprises the slurry of particulate thus increases gradually.
By exhaust outlet 34 major part in the vent gas of cyclonic separator 30 generations is circulated to circulating line 41.With a part of vent gas, for example the vent gas scale of construction is about 1/10, discharges by second exhaust outlet 35.
In the equipment of the present embodiment, link to each other with second exhaust outlet 35 by gas exhaust duct 43 as second cyclonic separator 50 of second gas-liquid separation device.Second cyclonic separator 50 has the structure identical with cyclonic separator 30 basically, and as gas-liquid separation device.Particularly, the solution-airmixture that is incorporated in second cyclonic separator 50 by the inlet 51 that links to each other with gas exhaust duct 43 forms around cyclonic separation body 52 inwall progressive eddy current 53, and is thus that liquid ingredient is separated from the gas.Liquid ingredient promptly comprises the slurry of particulate, descends in cyclonic separator 50, and is discharged from and is stored in the fluid container 61 by drain outlet 54.More specifically, Wen's pipeline section 44 that stream narrows down and provides water circulating pipe 62 so that keep being communicated with of Wen's pipeline section 44 and fluid container 61 in gas exhaust duct 43.When in Wen's pipeline section 44, providing high velocity air, be contained in the fluid container 61 water and can be drawn out of and spray into Wen's pipeline section 44, can capture the particulate that remains in the gas phase for water (liquid) thus.Gas exhaust duct 71 links to each other with exhaust outlet 55, and second gas blower 72 is provided in gas exhaust duct 71, so that by the help of second gas blower 72 gas is discharged by exhaust outlet 55.Can spray in the gas exhaust duct 43 by the water that the pump mentioned about cyclonic separator 30 and injection nozzle will be contained in the water receptacle 61.As mentioned above equally, can be equipped with strainers and precipitation vessel so that by neutralizing effect separating particles from liquid for fluid container 61.In addition, a part of gas circulation of discharging by exhaust outlet 55 can be arrived the upstream side of Wen's pipeline section 44 of gas exhaust duct 43, so that improve collection efficiency thus.
When cyclonic separator 30 provides enough micro particle catching efficient, needn't provide second cyclonic separator 50.In order further to improve collection efficiency, a plurality of cyclonic separators can be linked together.
The particulate production example of the equipment that uses above-mentioned embodiment will be described below.
Embodiment 1
Atomizing powder (average particle size particle size: 45 μ m) introduce the acetylene flame, thus synthetic ITO (In under dry state with In-Sn alloy (Sn:9.6wt%) 2O 3: SnO 2=90:10wt%) powder.Under dry state, collect this powder by bag filter, produce the ITO powder of embodiment 1 thus.
Embodiment 2
To be similar to the mode of embodiment 1, under dry state, synthesize the ITO powder by the acetylene flame.By under hygrometric state, collecting this powder, produce the ITO powder of embodiment 2 thus to the powder water spray.
Comparative example 1
Calcine synthetic Indium sesquioxide powder under the hygrometric state down at 1000 ℃.Similarly, calcine synthetic stannic oxide powder under the hygrometric state down at 1000 ℃.Mix incinerating Indium sesquioxide powder like this (90 quality %) and stannic oxide powder (10 quality %) by mortar, produce the oxide powder (standard product 1) of comparative example 1 thus.
Comparative example 2
Under hygrometric state,, produce the ITO powder of comparative example 2 thus by the synthetic ITO powder of co-precipitation.
Carrying out the co-precipitation wet method by following program synthesizes.At first, at ambient temperature In (4N) (20g) is dissolved in nitric acid (special grade chemical, concentration: 60-61%) in (133cc), produce solution (pH=-1.5) thus.Similarly, at ambient temperature Sn (4N) (2.12g) is dissolved in hydrochloric acid (special grade chemical, concentration: 35-36%) in (100cc), produce solution (pH=-1.9) thus.Two kinds of solution are mixed, thereby obtain mixed acid solution.Do not observe precipitation in the mixing process, and find that the pH of mixing solutions is-1.5.Subsequently, the ammoniacal liquor (special grade chemical) of adding 25% neutralizes in this acidic solution, thus with pH regulator to 6.5, and separates out white mass.After several hours, remove supernatant liquid, and with pure water washing and precipitating thing (2L * 3), subsequently 80 ℃ dry down, 600 ℃ of bakings three hours down, and dehydration, thus by the synthetic generation of wet method ITO powder.
Comparative example 3
Under 1550 ℃ or higher temperature, mixture (the stannic oxide content: 10wt%) of synthetic Indium sesquioxide powder and stannic oxide powder under the sintering hygrometric state.ITO grinds with sintering, produces the ITO powder of comparative example 3 thus.
Test implementation example 1
Analyze embodiment 1 and 2 and the SnO of each ITO powder of comparative example 1-3 2Sosoloid content.Trace routine is as follows.Before the test, in air with embodiment 1 and 2 and the ITO powder of comparative example 2 and 3 1000 ℃ down calcining three hours so that make the SnO that separates out 2The SnO that particle growth becomes to be easy to detect 2Macrobead,
1. respond to coupling high frequency plasma spectrum analysis (ICP spectrum analysis).In order to calculate, suppose that each ITO powder just is made up of In, Sn and oxygen (O), and can have a certain amount of hypoxgia.According to the ratio of analytical value calculating In and Sn, and calculating is transformed into In respectively at all In and Sn element 2O 3And SnO 2In under the condition 2O 3With SnO 2Weight ratio.
To embodiment 1 and 2 and the ITO powder of comparative example 1-3 carry out powder x-ray diffraction analysis (XRD: utilize MXP 18II, the product of Mac Science), measure the SnO that separates out of each powder thus 2Content.In each situation, check composite oxides (In from the diffractogram of correspondence 4Sn 3O 12) existence.When not detecting these composite oxides, according to In 2O 3(222) integration diffracted intensity and SnO 2The ratio of integration diffracted intensity (110) with respect to the standard product 1 of comparative example 1, is determined the SnO that separates out of ITO powder 2Content (mass percent).Particularly, separate out SnO 2Content (mass percent) is according to SnO 2The SnO that obtains of X-ray diffraction integrated intensity 2Content is supposed not to be dissolved in In 2O 3In and the SnO by about 1000 ℃ calcining growth 2Component can show SnO 2(110) X-ray diffraction peak.Fig. 2 to Fig. 6 has shown the result of X-ray diffraction analysis.
3. based on the result of " 1 " and " 2 ", by detecting but not by icp analysis by X-ray diffraction as SnO 2(110) detected SnO 2Amount obtains the SnO of each ITO powder 2Sosoloid content (In 2O 3In).
The result is as shown in table 1.
Find that the ITO powder of embodiment 1 and 2 has the SnO of 2.35wt% and 2.42wt% 2Sosoloid content, this is higher than the SnO by the ITO powder of the synthetic gained comparative example 2 of wet method 2Sosoloid content 2.26wt%.Find ITO powder formation composite oxides by the comparative example 3 of pulverizing the sintered product generation.Therefore, can not measure the SnO of the ITO powder of comparative example 3 2Sosoloid content.
Table 1
Figure C200480041059D00161
Embodiment 3
Atomizing powder (average particle size particle size: 45 μ m) introduce the DC flame passes, with In-Sn alloy (Sn:9.6wt%) so that under dry state, synthesize ITO (In thus 2O 3: SnO 2=90:10wt%) powder.By under hygrometric state, collecting this powder, produce the ITO powder of embodiment 3 thus to powder jetting water.
Comparative example 4
Be similar to comparative example 1, calcine synthetic Indium sesquioxide powder under the hygrometric state down at 1000 ℃.Similarly, calcine synthetic stannic oxide powder under the hygrometric state down at 1000 ℃.By mortar incinerating Indium sesquioxide powder like this (90 mass percent) and stannic oxide powder (10 mass percent) are mixed, produce the oxide powder (standard product 2) of comparative example 4 thus
Test implementation example 2
Be similar to test implementation example 1, analyze the SnO of each ITO powder of embodiment 3 and comparative example 4 2Sosoloid content.Pass through X ' PertPRO MPD (product of Spectris company limited) and carry out powder x-ray diffraction analysis (XRD).The result is as shown in table 2.Fig. 7 and Fig. 8 have shown the result of X-ray diffraction analysis.
Find the SnO of the ITO powder of embodiment 3 2Sosoloid content is 3.00wt%, and this is significantly higher than by the acetylene flame but not the SnO of the ITO powder of the embodiment 2 that the DC flame passes obtains 2Sosoloid content.
Table 2

Claims (16)

1. produce the method for particulate, it is characterized in that this method comprises that the raw material with liquid stream, drop or powder form infeeds thermal source; Capture the product of the particulate form that forms by the fog-like liquid fluid; And separate with slurry form by solution-air and to collect particulate, wherein said thermal source is the thermal source that flame is arranged.
2. according to the method for the production particulate of claim 1, wherein provide the raw material of waiting to infeed thermal source by melting material being formed liquid stream or drop.
3. according to the method for the production particulate of claim 1, the raw material of wherein waiting to infeed thermal source is the form of atomizing powder.
4. according to the method for the production particulate of claim 1, wherein carry out this solution-air and separate by cyclonic separator.
5. according to the method for the production particulate of claim 1, wherein this thermal source is acetylene flame or DC flame passes.
6. according to the method for the production particulate of claim 1, wherein this liquid fluid is a water.
7. according to the method for the production particulate of claim 1, wherein this raw material is to be selected from least a in metal, alloy, oxide compound, nitride and the oxynitride.
8. according to the method for the production particulate of claim 1, wherein this thermal source is oxidizing atmosphere or nitriding atmosphere, produces oxide fine particle, nitride particulate or oxynitride particulate thus.
9. according to the method for the production particulate of claim 1, wherein raw material is In-Sn alloy or ITO powder, by this raw material production indium oxide-tin oxide body.
10. according to the method for the production particulate of claim 9, this method produces tin content and presses SnO 2Be calculated as the indium oxide-tin oxide body of 2.3-45 mass percent.
11. according to the method for any one production particulate of claim 1 to 10, wherein when capturing product by liquid fluid, this product flows with 150m/s or littler maximum rate.
12. produce the equipment of particulate, it is characterized in that this equipment comprises:
Be used for the import with gaseous fluid and product introducing device interior, this product is to infeed thermal source by the raw material with liquid stream, drop or powder form to obtain;
Be used for spraying fog-like liquid fluidic fluid jet device to the product of introducing;
Being used for that the particulate that is captured by liquid fluid is carried out solution-air separates so that form first gas-liquid separation device of particulate slurry thus; With
An atmosphere fluidic part that is used for comprising not the particulate that is captured by liquid fluid turns back to first circulation device of fluid jet device position.
13. equipment according to the production particulate of claim 12, this equipment comprises second gas-liquid separation device in addition in the first gas-liquid separation device downstream side, the atmosphere fluidic part of the particulate that is captured by liquid fluid is provided second gas-liquid separation device to be used to introduce to comprise not, be used for to atmosphere fluid jet fog-like liquid fluid, and be used to carry out the solution-air separation, obtain the slurry of particulate thus.
14. equipment according to the production particulate of claim 13, this equipment comprises second circulation device in addition in the downstream side of second gas-liquid separation device, and the atmosphere fluidic part that this second circulation device is used for comprising not the particulate that is captured by liquid fluid turns back to the inlet of second gas-liquid separation device.
15. according to the equipment of the production particulate of claim 12, wherein first gas-liquid separation device is a cyclonic separator.
16. according to the equipment of any one production particulate of claim 12 to 15, wherein when the liquid fluid trap particles of spraying by fluid jet device, fluid flows with 150m/s or littler maximum rate.
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