CN107098378B - A kind of polymolecularity ITO raw powder's production technology - Google Patents
A kind of polymolecularity ITO raw powder's production technology Download PDFInfo
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- CN107098378B CN107098378B CN201710262344.3A CN201710262344A CN107098378B CN 107098378 B CN107098378 B CN 107098378B CN 201710262344 A CN201710262344 A CN 201710262344A CN 107098378 B CN107098378 B CN 107098378B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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Abstract
The present invention discloses a kind of polymolecularity ITO raw powder's production technology, belongs to indium tin oxide composite powder preparation technical field, comprising the following steps: weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, weighs SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；Take NH4AC buffer solution, is added composite dispersing agent in buffer solution；Ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, generate indium tin hydroxide presoma；It after fully reacting, is aged, filters, obtained indium tin hydroxide presoma is used into water and organic solvent washing respectively；Indium tin hydroxide presoma after washing is placed at room temperature, naturally dry；4h is calcined at high temperature, obtains yellow ito powder.Using ITO powder hard aggregation is few made of preparation method of the present invention, good fluidity, is easy to compression moulding.
Description
Technical field
The present invention relates to indium tin oxide composite powder preparation technical fields, in particular to a kind of to prepare ITO with coprecipitation
The method of powder.
Background technique
Ito thin film can be prepared by ITO target through magnetron sputtering method, in the industrial production, mostly use magnetron sputtering greatly
ITO target is sputtered into very thin layer of transparent conductive film (thickness 100nm or so) on glass, is performed etching to film by method,
To prepare the electrode material of flat-panel monitor.Ito powder is the raw material for preparing ITO sputtering coating target, high-quality to be obtained,
Highdensity ITO sputtering target material then needs to form the ito powder of uniform ultrapure ultra-fine high agglutinating property.
In general, be to ito powder specific requirement: particle size is less than 100nm, and specific surface area is greater than 15m2/ g, and
And granule-morphology, in spherical, particle size distribution range is narrow, and hard aggregation is few.The preparation for the ITO powder reported in various countries' document at present
Method mainly has to be prepared ito powder method and has at present: homogeneous co-precipitation process, aqueous solution coprecipitation, electrolysis method, sol-gel
Method, spray burning method, spray heating decomposition etc..Chemical coprecipitation have simple process be easily achieved work metaplasia produce, product it is pure
Basic step: the advantages that degree is high, component is uniform, favorable dispersibility is pressed ingredient metering and is prepared containing soluble metal salt solution；With
Precipitating reagent is added dropwise in mixing salt solution metal salt is homogeneously crystallized, Precipitation；It is dissolved by thermal dehydration and high-temperature calcination
Equal processing prepare fine powder.
But particle dispersion made from existing method is not highly desirable, partial size is answered in 100nm or more with this tin indium oxide
The density for closing the target of powder preparation cannot generally reach 99% or more, it is difficult to meet the requirement of high performance thin film plated film.
Summary of the invention
The present invention provides a kind of polymolecularity ITO raw powder's production technology, solves ITO powder made from existing preparation method
The problem that body dispersibility is undesirable, reunion is more, sintering activity is low.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of polymolecularity ITO raw powder's production technology, comprising the following steps:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, is weighed
SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 6~8 NH4AC buffer solution, is added composite dispersing agent in buffer solution；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, generate indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 5~8 hours, is then filtered by vacuum, the indium tin hydroxide that will be obtained
Presoma uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, obtains yellow ito powder.
Wherein it is preferred to which the additional amount of the composite dispersing agent is the 2~5% of ITO powder total amount.
Wherein it is preferred to the composite dispersing agent be the dodecyl sodium sulfate of mass ratio 1:2:1, pregelatinized starch and
Polyvinylpyrrolidone.
Wherein it is preferred to adjust the rate of addition of ammonium hydroxide during dropwise addition in the step (3), make the pH value of solution
It is basically unchanged.
Wherein it is preferred to which the calcination temperature of the step (6) is 700~1000 DEG C.
Beneficial effects of the present invention:
Composite dispersing agent dodecyl sodium sulfate, pregelatinized starch and polyvinyl pyrrole is added in the present invention in buffer solution
Alkanone, dodecyl sodium sulfate are anionic surfactant, can form electric double layer between powder granule, between particle
Van der Waals force can be generated, double electrical layers can be reinforced, reaches electrostatic repulsion, meanwhile, dodecyl sodium sulfate has length
Carbochain forms steric hindrance effect；And pregelatinized starch can be dissolved in cold water, belongs to polymer electrolyte with polyvinylpyrrolidone
Surfactant has Long carbon chain, mainly plays peptizaiton by steric hindrance.Dodecyl sodium sulfate of the present invention, pre- glue
Changing starch, identical synergistic effect as composite dispersing agent can effectively reduce the reunion of coprecipitation reaction with polyvinylpyrrolidone
Property.The ITO powder dispersity of preparation is good, and particle size distribution is relatively uniform, and by XPS analysis, In, Sn in ITO powder are first
Element is more than single oxide form, some exists in the form of composite oxides.Using made of preparation method of the present invention
ITO powder hard aggregation is few, good fluidity, is easy to compression moulding.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is the typical microstructure figure of polymolecularity ITO powder in the embodiment of the present invention 1.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of polymolecularity ITO raw powder's production technologies, comprising the following steps:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, is weighed
SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 7 NH4AC buffer solution, is added composite dispersing agent in buffer solution；The composite dispersing agent
Additional amount be ITO powder total amount 4%；Composite dispersing agent is dodecyl sodium sulfate, the pregelatinized starch of mass ratio 1:2:1
And polyvinylpyrrolidone；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, during dropwise addition, adjust the dropwise addition of ammonium hydroxide
Speed is basically unchanged the pH value of solution, generates indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 7 hours, is then filtered by vacuum, the indium tin hydroxide forerunner that will be obtained
Body uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, calcination temperature is 850 DEG C, obtains yellow ito powder.
ITO powder dispersity manufactured in the present embodiment is good, particle size distribution is relatively uniform, hard aggregation is few, good fluidity,
It is easy to compression moulding, the typical micro-structure of powder is shown in Fig. 1.
Embodiment 2
The present embodiment provides a kind of polymolecularity ITO raw powder's production technologies, comprising the following steps:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, is weighed
SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 6 NH4AC buffer solution, is added composite dispersing agent in buffer solution；The composite dispersing agent
Additional amount be ITO powder total amount 2%；Composite dispersing agent is dodecyl sodium sulfate, the pregelatinized starch of mass ratio 1:2:1
And polyvinylpyrrolidone；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, during dropwise addition, adjust the dropwise addition of ammonium hydroxide
Speed is basically unchanged the pH value of solution, generates indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 8 hours, is then filtered by vacuum, the indium tin hydroxide forerunner that will be obtained
Body uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, calcination temperature is 950 DEG C, obtains yellow ito powder.
ITO powder dispersity manufactured in the present embodiment is good, particle size distribution is relatively uniform, hard aggregation is few, good fluidity,
It is easy to compression moulding.
Embodiment 3
The present embodiment provides a kind of polymolecularity ITO raw powder's production technologies, comprising the following steps:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, is weighed
SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 7 NH4AC buffer solution, is added composite dispersing agent in buffer solution；The composite dispersing agent
Additional amount be ITO powder total amount 5%；Composite dispersing agent is dodecyl sodium sulfate, the pregelatinized starch of mass ratio 1:2:1
And polyvinylpyrrolidone；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, during dropwise addition, adjust the dropwise addition of ammonium hydroxide
Speed is basically unchanged the pH value of solution, generates indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 5 hours, is then filtered by vacuum, the indium tin hydroxide forerunner that will be obtained
Body uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, calcination temperature is 700 DEG C, obtains yellow ito powder.
ITO powder dispersity manufactured in the present embodiment is good, particle size distribution is relatively uniform, hard aggregation is few, good fluidity,
It is easy to compression moulding.
Embodiment 4
The present embodiment provides a kind of polymolecularity ITO raw powder's production technologies, comprising the following steps:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, is weighed
SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 8 NH4AC buffer solution, is added composite dispersing agent in buffer solution；The composite dispersing agent
Additional amount be ITO powder total amount 3%；Composite dispersing agent is dodecyl sodium sulfate, the pregelatinized starch of mass ratio 1:2:1
And polyvinylpyrrolidone；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, during dropwise addition, adjust the dropwise addition of ammonium hydroxide
Speed is basically unchanged the pH value of solution, generates indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 6 hours, is then filtered by vacuum, the indium tin hydroxide forerunner that will be obtained
Body uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, calcination temperature is 900 DEG C, obtains yellow ito powder.
ITO powder dispersity manufactured in the present embodiment is good, particle size distribution is relatively uniform, hard aggregation is few, good fluidity,
It is easy to compression moulding.
Embodiment 5
The present embodiment provides a kind of polymolecularity ITO raw powder's production technologies, comprising the following steps:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, is weighed
SnCl4·5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 7 NH4AC buffer solution, is added composite dispersing agent in buffer solution；The composite dispersing agent
Additional amount be ITO powder total amount 4%；Composite dispersing agent is dodecyl sodium sulfate, the pregelatinized starch of mass ratio 1:2:1
And polyvinylpyrrolidone；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, during dropwise addition, adjust the dropwise addition of ammonium hydroxide
Speed is basically unchanged the pH value of solution, generates indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 7 hours, is then filtered by vacuum, the indium tin hydroxide forerunner that will be obtained
Body uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, calcination temperature is 1000 DEG C, obtains yellow ito powder.
ITO powder dispersity manufactured in the present embodiment is good, particle size distribution is relatively uniform, hard aggregation is few, good fluidity,
It is easy to compression moulding.
For mobility, the porosity etc. for characterizing powder, angle of repose, plate angle, apparent density and vibration density are generallyd use
Degree is to be characterized.
Angle of repose is also referred to as angle of repose, refers to that the Free Surface of powder stack layer under static balance state, is formed with horizontal plane
Maximum angle angle of repose.It is to make to fall under powder nature by ad hoc fashion to be formed on particular platform.Angle of repose pair
The mobility of powder influences maximum, and angle of repose is smaller, and the mobility of powder is better.
Plate angle refers to vertically lifts the plate being embedded in powder upwards, Free Planar (inclined-plane) of the powder on plate
Angle between plate is known as plate angle with the average value of angle after being shaken.Plate angle is smaller, the mobility of powder
It is stronger.
Tap density refers to that powder filling after special container, vibrates container, so that the gap in powder is destroyed,
Make powder for the density after tightly packed state.Mobility and the porosity etc. for being known that powder by measuring tap density
Data.
Apparent density refers to density of the powder in special container after nature full state.
Angle of repose, the plate of the resulting indium tin oxide composite powder of above-described embodiment are tested with powder tester for overall characteristic
Angle, apparent density and tap density (specific value is seen attached list)
| Angle of repose (°) | Plate angle (°) | Apparent density (g/cm3) | Tap density (g/cm3) | |
| Embodiment 1 | 28.72 | 37.18 | 1.58 | 1.84 |
| Embodiment 2 | 31.73 | 41.76 | 1.64 | 1.92 |
| Embodiment 3 | 27.22 | 46.78 | 1.52 | 1.79 |
| Embodiment 4 | 30.86 | 42.33 | 1.58 | 1.80 |
| Embodiment 5 | 29.67 | 39.79 | 1.64 | 1.94 |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of polymolecularity ITO raw powder's production technology, it is characterised in that the following steps are included:
(1) it weighs metal In and is added to HNO3It is completely dissolved in solution, according to In2O3/SnO2Mass ratio is 9:1, weighs SnCl4·
5H2O white crystal is added in indium salts solution, is stirred evenly and is prepared mixing salt solution；
(2) taking pH value is 6~8 NH4AC buffer solution, is added composite dispersing agent in buffer solution；The composite dispersing agent is
Dodecyl sodium sulfate, pregelatinized starch and the polyvinylpyrrolidone of mass ratio 1:2:1；The additional amount of the composite dispersing agent
It is the 2~5% of ITO powder total amount；
(3) ammonium hydroxide and mixing salt solution are added dropwise in buffer solution simultaneously, generate indium tin hydroxide presoma；
(4) after fully reacting, precipitating is aged 5~8 hours, is then filtered by vacuum, the indium tin hydroxide forerunner that will be obtained
Body uses water and organic solvent washing into filtrate without Cl respectively-Ion exists；
(5) the indium tin hydroxide presoma after washing is placed at room temperature, naturally dry obtains white powder；
(6) white powder is calcined into 4h at high temperature, obtains yellow ito powder.
2. a kind of polymolecularity ITO raw powder's production technology according to claim 1, it is characterised in that: the step (3)
During dropwise addition, adjust the rate of addition of ammonium hydroxide, be basically unchanged the pH value of solution.
3. a kind of polymolecularity ITO raw powder's production technology according to claim 1, it is characterised in that: the step (6)
Calcination temperature be 700~1000 DEG C.
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| CN113353971B (en) * | 2021-06-25 | 2023-01-31 | 河北恒博新材料科技股份有限公司 | Preparation method of spherical nanoscale high-dispersion ITO powder |
| CN114772632A (en) * | 2022-04-20 | 2022-07-22 | 柳州华锡有色设计研究院有限责任公司 | Method for accurately controlling pH value to promote ITO powder consistency |
| CN116621575A (en) * | 2023-06-09 | 2023-08-22 | 河北惟新科技有限公司 | Preparation method of heavily doped ITO powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994894A (en) * | 2006-12-29 | 2007-07-11 | 昆明理工大学 | Liquid phase coprecipitation method for producing superfine tin indium oxide powder |
| CN105036181A (en) * | 2015-07-23 | 2015-11-11 | 柳州华锡铟锡材料有限公司 | Preparation method for mixed particle morphology ITO powder |
| CN105731527A (en) * | 2016-01-29 | 2016-07-06 | 北京化工大学 | Coprecipitation preparation method of nanoscale indium tin oxide powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994894A (en) * | 2006-12-29 | 2007-07-11 | 昆明理工大学 | Liquid phase coprecipitation method for producing superfine tin indium oxide powder |
| CN105036181A (en) * | 2015-07-23 | 2015-11-11 | 柳州华锡铟锡材料有限公司 | Preparation method for mixed particle morphology ITO powder |
| CN105731527A (en) * | 2016-01-29 | 2016-07-06 | 北京化工大学 | Coprecipitation preparation method of nanoscale indium tin oxide powder |
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