CN110256049A - A kind of preparation method of ito powder - Google Patents
A kind of preparation method of ito powder Download PDFInfo
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- CN110256049A CN110256049A CN201910717384.1A CN201910717384A CN110256049A CN 110256049 A CN110256049 A CN 110256049A CN 201910717384 A CN201910717384 A CN 201910717384A CN 110256049 A CN110256049 A CN 110256049A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
Abstract
The present invention provides a kind of preparation methods of ito powder, comprising the following steps: indium oxide, dispersing agent a) are mixed sand milling with water, obtain indium oxide slurry；B) tin oxide and dispersant are sanded, obtain tin oxide slurry；C) the indium oxide slurry, tin oxide slurry are mixed into sand milling with binder, obtains ITO slurry；D) the ITO slurry is spray-dried, obtains ito powder；The step a) and step b) is limited without sequence.Preparation method according to the invention can not only obtain ito powder, moreover it is possible to improve the mobility of ito powder, reduce its apparent density；Moreover, thinner particle can be obtained by the above method, and grain diameter is uniform, good dispersion.
Description
Technical field
The present invention relates to technical field of semiconductor, in particular to a kind of preparation method of ito powder.
Background technique
Indium tin oxide (ITO) also known as tin-doped indium oxide powder, by In2O3And SnO2It is combined, is a kind of height degeneracy
N-type semiconductor, with high visible light transmittance, infrared reflection rate, excellent electric conductivity and preferable etching performance by
To extensive concern.Therefore, the preparation of ITO powder is of great significance.
Currently, the method for preparing ITO powder mainly has: mechanical mixing, spray pyrolysis, hydro-thermal method, chemical precipitation method, molten
Glue-gel method, micro emulsion method etc..Wherein, prepared by spray pyrolysis, hydro-thermal method, chemical precipitation method, sol-gel method, micro emulsion method etc.
Process is complicated, condition is stringent；In contrast, mechanical mixing is relatively simple.Mechanical mixing be by indium oxide and tin oxide by
It after certain proportion mixing, is heat-treated, and then obtains ito powder.However, in mechanical the preparation method, the mobility of gained powder
Difference, apparent density are high, to influence sintered density when ito powder molding.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of preparation method of ito powder, preparation method energy of the invention
It enough improves the mobility of ito powder, reduce its apparent density.
The present invention provides a kind of preparation methods of ito powder, comprising the following steps:
A) indium oxide, dispersing agent are mixed into sand milling with water, obtains indium oxide slurry；
B) tin oxide and dispersant are sanded, obtain tin oxide slurry；
C) the indium oxide slurry, tin oxide slurry are mixed into sand milling with binder, obtains ITO slurry；
D) the ITO slurry is spray-dried, obtains ito powder；
The step a) and step b) is limited without sequence.
Preferably, in the step a), the specific surface area of indium oxide is 5~25m2/g；
The mass ratio of indium oxide and water is (1.5~6): 1.
Preferably, in the step b), the specific surface area of tin oxide is 5~20m2/g。
Preferably, the mass ratio of the indium oxide and binder is (20~60): 1；
The binder is the oligomeric species binder of dihydric alcohol.
Preferably, in the step a), being sanded to the average particle size of indium oxide is 1.5 μm or less；
In the step b), being sanded to the average particle size of tin oxide is 0.1~2.5 μm.
Preferably, in the step a): dispersing agent is selected from alcohols dispersing agent；The mass ratio of indium oxide and dispersing agent is (120
~250): 1.
Preferably, in the step b): dispersing agent is selected from alcohols dispersing agent；The mass ratio of tin oxide and dispersing agent is (20
~60): 1.
Preferably, the step c) includes:
C1 indium oxide slurry) is mixed into sand milling with tin oxide slurry, obtains intermediate pulp；
C2 the intermediate pulp) is mixed into sand milling with binder, obtains ITO slurry；
The step c1) in:
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 100~600min；
The step c2) in:
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 50~300min.
Preferably, in the step a):
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 100~600min；
In the step b):
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 50~300min.
Preferably, the mass ratio of the indium oxide and tin oxide is (8~99.5): 1；
The inlet temperature of the spray drying is 150~250 DEG C, and outlet temperature is 50~150 DEG C；
The binder is polyethylene glycol；
The dispersing agent is polyvinyl alcohol.
The present invention provides a kind of preparation methods of ito powder, comprising the following steps: a) by indium oxide, dispersing agent and water
Mixing is sanded, and obtains indium oxide slurry；B) tin oxide and dispersant are sanded, obtain tin oxide slurry；C) by the oxygen
Change indium slurry, tin oxide slurry mix sand milling with binder, obtain ITO slurry；D) the ITO slurry is spray-dried, is obtained
Ito powder；The step a) and step b) is limited without sequence.Initial oxidation indium, dispersing agent and water of the present invention are sanded, and are obtained
The indium oxide slurry of certain particle size；Tin oxide and dispersing agent are sanded, the tin oxide slurry of certain particle size is obtained；Again by indium oxide
Slurry, tin oxide slurry and binder are sanded, and obtain ITO slurry；The present invention is ground using specific sand milling mode, and
The specific gradually sand grinding process of setting, and the control of some parameters is combined also to occur so that process of lapping not only has physical change
Chemical change, the crystal grain of particle becomes smaller combination, formation ITO object phase, and ITO slurry system with preferable slurry state, then leads to
Spray drying is crossed, that is, forms the ito powder that apparent density is low, mobility is high.Moreover, can be obtained by the above method thinner
Particle, and grain diameter is uniform, good dispersion.In addition, the present invention simplifies without being heat-treated compared to existing machinery method
Preparation process simultaneously reduces energy consumption.
Test result shows preparation method provided by the invention, and ito powder, and the stream of gained powder is not only successfully made
Dynamic property value is in 70s/50g hereinafter, apparent density is in 1.75g/cm2Hereinafter, having high fluidity and low-apparent-density, can make
The sintered density of ito powder reaches 7.135g/cm3More than.
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
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the XRD diagram of mixed-powder；
Fig. 2 is the XRD diagram of 1 gained ito powder of embodiment；
Fig. 3 is SEM figure of the 1 gained ito powder of embodiment under 100 multiplying powers；
Fig. 4 is SEM figure of the 1 gained ito powder of embodiment under 500 multiplying powers；
Fig. 5 is SEM figure of the 2 gained ito powder of embodiment under 100 multiplying powers；
Fig. 6 is SEM figure of the 2 gained ito powder of embodiment under 500 multiplying powers；
Fig. 7 is SEM figure of the 3 gained ito powder of embodiment under 100 multiplying powers；
Fig. 8 is SEM figure of the 3 gained ito powder of embodiment under 500 multiplying powers.
Specific embodiment
The present invention provides a kind of preparation methods of ito powder, comprising the following steps:
A) indium oxide, dispersing agent are mixed into sand milling with water, obtains indium oxide slurry；
B) tin oxide and dispersant are sanded, obtain tin oxide slurry；
C) the indium oxide slurry, tin oxide slurry are mixed into sand milling with binder, obtains ITO slurry；
D) the ITO slurry is spray-dried, obtains ito powder；
The step a) and step b) is limited without sequence.
Initial oxidation indium, dispersing agent and water of the present invention are sanded, and the indium oxide slurry of certain particle size is obtained；By tin oxide with
Dispersing agent is sanded, and obtains the tin oxide slurry of certain particle size；Indium oxide slurry, tin oxide slurry and binder are sanded again, obtained
To ITO slurry；The present invention is ground using specific sand milling mode, and sets specific gradually sand grinding process, and combine
Chemical change also occur so that process of lapping not only has physical change for the control of some parameters, and the crystal grain of particle becomes smaller combination,
Formed ITO object phase, and ITO slurry system have preferable slurry state, then by spray drying, that is, formed apparent density it is low,
The high ito powder of mobility.Moreover, thinner particle can be obtained by the above method, and grain diameter is uniform, dispersed
It is good.
According to the present invention, indium oxide, dispersing agent are mixed into sand milling with water, obtain indium oxide slurry.
In the present invention, the specific surface area of the indium oxide is preferably 5~25m2/ g, using the oxidation under above-mentioned specific surface area
Indium particle advantageously forms ITO object phase in conjunction with preparation process of the invention, and improves the mobility of ito powder, reduces its pine
Fill density.Wherein, the specific surface area of the indium oxide is more preferably 8~20m2/ g prepares effect and product under the range
Above-mentioned characteristic is further promoted.The present invention is not particularly limited the source of the indium oxide, ripe according to those skilled in the art
The preparation method known obtains, and such as using indium metal, sulfuric acid and ammonium hydroxide as raw material, prepares indium hydroxide precipitating, then by forging
It burns and obtains powdered indium oxide；It wherein, is the indium oxide for obtaining above-mentioned specific surface area, the temperature of calcining is 500~1200 DEG C.
In the present invention, the dispersing agent is preferably modified high-molecular Ionomer, more preferably in alcohols dispersing agent
One or more；Further preferably polyvinyl alcohol.The present invention is not particularly limited the source of the dispersing agent, is general
Commercially available product is made according to preparation method well known to those skilled in the art.
In the present invention, the mass ratio of the indium oxide and dispersing agent is preferably (120~250): 1, more preferably (150~
210)∶1。
In the present invention, the mass ratio of the indium oxide and water is preferably (1.5~.6): 1.Under the material-water ratio, in conjunction with this
The preparation process of invention is conducive to improve the mobility of ito powder, reduces its apparent density.
In the present invention, in the mixing sand milling, the sand mill of use is preferably horizontal sand mill.In the present invention, the sand
The target of mill is that the average particle size of indium oxide in slurry is preferably made to reach 2.5 μm hereinafter, more preferably 1~2.5 μm, if granularity mistake
Small, particle is easy to reunite, if granularity is excessive, it will cause the apparent density of the ITO powder gone out by spraying is larger.
In the present invention, to realize above-mentioned sand milling purpose, the partial size of the zirconia ball used in the sand milling is preferably 0.1~
3.0mm.The revolving speed of the sand milling is preferably 500~1500rpm, more preferably 600~1400rpm；The time of the sand milling is excellent
It is selected as 100~600min, more preferably 150~500min.After above-mentioned sand milling, indium oxide slurry is obtained.
According to the present invention, tin oxide and dispersant are sanded, tin oxide slurry is obtained.
In the present invention, the specific surface area of the tin oxide is preferably 5~20m2/ g, using the oxidation under above-mentioned specific surface area
Tin particles advantageously form ITO object phase in conjunction with preparation process of the invention, and improve the mobility of ito powder, reduce its pine
Fill density.The present invention is not particularly limited the source of the tin oxide, for general commercially available product or according to those skilled in the art
Well known preparation method obtains.
In the present invention, the dispersing agent is preferably modified high-molecular Ionomer, more preferably in alcohols dispersing agent
One or more；Further preferably polyvinyl alcohol.The present invention is not particularly limited the source of the dispersing agent, is general
Commercially available product is made according to preparation method well known to those skilled in the art.
In the present invention, the mass ratio of the tin oxide and dispersing agent is preferably (20~60): 1, more preferably (25~50):
1。
In the present invention, in the mixing sand milling, the sand mill of use is preferably horizontal sand mill.In the present invention, the sand
The target of mill is that the average particle size of tin oxide in slurry is preferably made to reach 0.1~2.5 μm, if undersized, particle is easy to reunite,
If granularity is excessive, it will cause the apparent density of the ITO powder gone out by spraying is larger.
In the present invention, to realize above-mentioned sand milling purpose, the partial size of the zirconia ball used in the sand milling is preferably 0.1~
3.0mm.The revolving speed of the sand milling is preferably 500~1500rpm, more preferably 600~1400rpm；The time of the sand milling is excellent
It is selected as 50~300min.After above-mentioned sand milling, tin oxide slurry is obtained.
In the present invention, to sequence of the above-mentioned indium oxide slurry with acquisition tin oxide slurry is obtained, there is no limit.
According to the present invention, after obtaining indium oxide slurry and tin oxide slurry, by indium oxide slurry, tin oxide slurry and glue
It ties agent mixing to be sanded, obtains ITO slurry.
In the present invention, the mass ratio of the indium oxide and tin oxide is preferably (8~99.5): 1.
In the present invention, the binder is preferably the oligomeric species binder of dihydric alcohol；More preferably polyethylene glycol.The oxygen
The mass ratio for changing indium and binder is preferably (20~60): 1, more preferably (30~50): 1.Under the ratio, be conducive to mention
The mobility of high ito powder reduces its apparent density.
In the present invention, when mixing sand milling, preferably carry out in the following manner:
C1 indium oxide slurry) is mixed into sand milling with tin oxide slurry, obtains intermediate pulp；
C2 the intermediate pulp) is mixed into sand milling with binder, obtains ITO slurry.
Wherein, the step c1) in, it is sanded and preferably uses horizontal sand mill.The zirconia ball used in the sand milling
Partial size is preferably 0.1~3.0mm.The revolving speed of the sand milling is preferably 500~1500rpm, more preferably 600~1400rpm；Institute
The time for stating sand milling is preferably 100~600min, more preferably 150~600min.
The step c2) in, it is sanded and preferably uses horizontal sand mill.The partial size of the zirconia ball used in the sand milling is excellent
It is selected as 0.1~3.0mm.The revolving speed of the sand milling is preferably 500~1500rpm, more preferably 600~1400rpm；The sand milling
Time be preferably 50~300min, more preferably 100~300min.After above-mentioned sanded treatment, ITO slurry is obtained.
According to the present invention, after obtaining ITO slurry, the ITO slurry is spray-dried, ito powder is obtained.
In the present invention, in the spray drying, condition is as follows: inlet temperature is preferably 150~250 DEG C, and outlet temperature is excellent
It is selected as 50~150 DEG C.After above-mentioned spray drying, ito powder is obtained.In the present invention, after the spray drying, preferably also into
Row screening.
It in preparation method provided by the invention, is ground, and is set specifically gradually using specific sand milling mode
Sand grinding process, and combine the control of some parameters that chemical change, particle also occurs so that process of lapping not only has physical change
Crystal grain become smaller combination, form ITO object phase, and ITO slurry system has preferable slurry state, then by spray drying, i.e.,
Form the ito powder that apparent density is low, mobility is high；Moreover, thinner particle, and particle can be obtained by the above method
Diameter is uniform, good dispersion.Specifically, in above-mentioned preparation process, the indium oxide raw material of suitable particle size, indium oxide and water ratio,
The sand milling granularity of the ratio and indium oxide slurry of indium oxide and binder and sand milling granularity, the two kinds of slurries of tin oxide slurry
Mixed proportion etc. for forming ITO object phase and improving that the mobility of ito powder, to reduce apparent density more crucial, pass through this
The setting of the specific preparation process of invention, and the control of above-mentioned parameter is combined, ito powder can be successfully obtained, and can mention
The mobility of high ito powder reduces its apparent density, and the sintered density of ITO powder is made to reach 7.135g/cm3More than；Moreover, energy
Thinner particle is enough obtained, and grain diameter is uniform, good dispersion.
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.In following embodiment, using 200 meshes in screening.
Embodiment 1
The preparation of 1.1ITO powder
Take indium oxide powder (specific surface area 15m2/ g) 200g, dispersing agent PVA 1g, deionized water 133g；By above-mentioned object
Material is placed in horizontal sand mill, wherein the partial size of zirconia ball is 1.2mm, and 600min is sanded under 600rpm revolving speed；Obtain oxygen
Change indium slurry, wherein indium oxide average particle size is at 1.5 μm or less.
Take stannic oxide powder (specific surface area 5m2/ g) 20g, dispersing agent PVA 1g；Above-mentioned material is placed in horizontal sand milling
In machine, wherein the partial size of zirconia ball is 1.2mm, and 300min is sanded under 500rpm revolving speed；Obtain tin oxide slurry, wherein
Tin oxide average particle size is 1.2 μm.
Above-mentioned indium oxide slurry is added in tin oxide slurry, in sand mill, 600min is sanded with 600rpm revolving speed
Afterwards, binder PEG 5g is added, continues that 300min is sanded with 600rpm revolving speed, obtains ITO slurry.
Above-mentioned ITO slurry is spray-dried, inlet temperature is 250 DEG C, outlet temperature is 150 DEG C, after screening, obtains ITO
Powder.
The characterization and test of 1.2 samples
(1) above-mentioned indium oxide powder and stannic oxide powder are obtained into mixed-powder with the mixing of mass ratio 10: 1.
X- ray powder diffraction test is carried out respectively to above-mentioned mixed-powder and gained ito powder, as a result respectively such as Fig. 1 and
Shown in Fig. 2, Fig. 1 is the XRD diagram of mixed-powder, and Fig. 2 is the XRD diagram of 1 gained ito powder of embodiment.As can be seen that being in Fig. 1
In2O3With SnO2Mixture phase；And in Fig. 2, do not find SnO in Fig. 12Characteristic peak, and mainly with In2O3Crystal structure
For phase structure, it was demonstrated that gained powder is with In2O3Crystal structure is the composite metal oxide powder of phase structure.
(2) mobility and apparent density are tested respectively to gained ito powder, the results show that the mobility of ito powder is
35.56s/50g, apparent density 1.35g/cm2。
(3) Electronic Speculum test is scanned to gained ito powder, as a result as shown in Figure 3 and Figure 4, Fig. 3 is 1 gained of embodiment
SEM figure of the ito powder under 100 multiplying powers, Fig. 4 are SEM figure of the 1 gained ito powder of embodiment under 500 multiplying powers.As can be seen that
Gained ito powder particle dispersion is preferable, and granularity is smaller, reaches 55~120 μm, and granularity is more uniform.And it can be seen by Fig. 4
Out, particle sphericity is preferable in gained powder, and surface is relatively smooth.
Embodiment 2
The preparation of 1.1ITO powder
Take indium oxide powder (specific surface area 8m2/ g) 1000g, dispersing agent PVA 5g, deionized water 500g；By above-mentioned object
Material is placed in horizontal sand mill, wherein the partial size of zirconia ball is 1.2mm, and 300min is sanded under 1000rpm revolving speed；It obtains
Indium oxide slurry, wherein indium oxide average particle size is at 1.5 μm or less.
Take stannic oxide powder (specific surface area 5m2/ g) 100g, dispersing agent PVA 5g；Above-mentioned material is placed in horizontal sand milling
In machine, wherein the partial size of zirconia ball is 1.2mm, and 200min is sanded under 1000rpm revolving speed；Tin oxide slurry is obtained,
In, tin oxide average particle size is 1.2 μm.
Above-mentioned indium oxide slurry is added in tin oxide slurry, in sand mill, 300min is sanded with 1000rpm revolving speed
Afterwards, binder PEG 28.6g is added, continues that 150min is sanded with 1000rpm revolving speed, obtains ITO slurry.
Above-mentioned ITO slurry is spray-dried, inlet temperature is 150 DEG C, outlet temperature is 100 DEG C, after screening, obtains ITO
Powder.
The characterization and test of 1.2 samples
(1) carry out x- ray powder diffraction test respectively to gained ito powder, it is as a result similar with Fig. 2, gained powder be with
In2O3Crystal structure is the composite metal oxide powder of phase structure.
(2) mobility and apparent density are tested respectively to gained ito powder, the results show that the mobility of ito powder is
55.23s/50g, apparent density 1.58g/cm2。
(3) Electronic Speculum test is scanned to gained ito powder, as a result as shown in Figure 5 and Figure 6, Fig. 5 is 2 gained of embodiment
SEM figure of the ito powder under 100 multiplying powers, Fig. 6 are SEM figure of the 2 gained ito powder of embodiment under 500 multiplying powers.As can be seen that
Gained ito powder particle dispersion is preferable, and granularity is smaller, reaches 50~120 μm, and granularity is more uniform.And it can be seen by Fig. 6
Out, particle sphericity is preferable in gained powder, and surface is relatively smooth.
Embodiment 3
The preparation of 1.1ITO powder
Take indium oxide powder (specific surface area 20m2/ g) 10Kg, dispersing agent PVA 50g, deionized water 2.857Kg；It will be upper
It states material to be placed in horizontal sand mill, wherein the partial size of zirconia ball is 1.2mm, and 100min is sanded under 1500rpm revolving speed；
Obtain indium oxide slurry, wherein indium oxide average particle size is at 1.5 μm or less.
Take stannic oxide powder (specific surface area 13m2/ g) 1Kg, dispersing agent PVA 50g；Above-mentioned material is placed in Horizontal sand
In grinding machine, wherein the partial size of zirconia ball is 1.2mm, and 50min is sanded under 1500rpm revolving speed；Tin oxide slurry is obtained,
In, tin oxide average particle size is 1.2 μm.
Above-mentioned indium oxide slurry is added in tin oxide slurry, in sand mill, 150min is sanded with 1500rpm revolving speed
Afterwards, binder PEG 250g is added, continues that 100min is sanded with 1500rpm revolving speed, obtains ITO slurry.
Above-mentioned ITO slurry is spray-dried, inlet temperature is 200 DEG C, outlet temperature is 100 DEG C, after screening, obtains ITO
Powder.
The characterization and test of 1.2 samples
(1) carry out x- ray powder diffraction test respectively to gained ito powder, it is as a result similar with Fig. 2, gained powder be with
In2O3Crystal structure is the composite metal oxide powder of phase structure.
(2) mobility and apparent density are tested respectively to gained ito powder, the results show that the mobility of ito powder is
61.31s/50g, apparent density 1.69g/cm2。
(3) Electronic Speculum test is scanned to gained ito powder, as a result as shown in Figure 7 and Figure 8, Fig. 7 is 3 gained of embodiment
SEM figure of the ito powder under 100 multiplying powers, Fig. 8 are SEM figure of the 3 gained ito powder of embodiment under 500 multiplying powers.As can be seen that
Gained ito powder particle dispersion is preferable, and granularity is smaller, and granularity is more uniform.And as seen from Figure 8, in gained powder
Particle sphericity is preferable, and surface is relatively smooth.
Embodiment 4
It is carried out according to the preparation process of embodiment 1, unlike, when preparing indium oxide slurry, adjust the addition of dispersing agent
Amount, makes the mass ratio 190: 1 of indium oxide and dispersing agent；When preparing tin oxide slurry, the additive amount of dispersing agent is adjusted, makes to aoxidize
The mass ratio of tin and dispersing agent is 40: 1.
The test of x- ray powder diffraction is carried out to gained powder, the results show that gained sample is ito powder.
According to the mobility and apparent density of the test method test gained powder of embodiment 1, the results show that its mobility
For 36.26s/50g, apparent density 1.55g/cm2。
Embodiment 5
It is carried out according to the preparation process of embodiment 1, unlike, when preparing indium oxide slurry, adjust the addition of dispersing agent
Amount, makes the mass ratio 220: 1 of indium oxide and dispersing agent；When preparing tin oxide slurry, the additive amount of dispersing agent is adjusted, makes to aoxidize
The mass ratio of tin and dispersing agent is 60: 1.
The test of x- ray powder diffraction is carried out to gained powder, the results show that gained sample is ito powder.
According to the mobility and apparent density of the test method test gained powder of embodiment 1, the results show that its mobility
For 40.56s/50g, apparent density 1.35g/cm2。
Embodiment 6
It is carried out according to the preparation process of embodiment 1, unlike, when preparing indium oxide slurry, the proportion between each component is not
Become, but dosage of each component increases simultaneously, makes the mass ratio 99: 1 of tin oxide in indium oxide and subsequent oxidation tin slurry.
The test of x- ray powder diffraction is carried out to gained powder, the results show that gained sample is ito powder.
According to the mobility and apparent density of the test method test gained powder of embodiment 1, the results show that its mobility
For 60s/50g, apparent density 1.62g/cm2。
Comparative example 1
It is carried out according to the preparation process of embodiment 4, unlike:
The additive amount of deionized water is adjusted, making indium oxide and the mass ratio of deionized water is respectively 5: 1；
It is respectively 50: 1 that the additive amount for adjusting binder, which is the mass ratio of indium oxide and binder,.
According to the test method in embodiment 1, the mobility and apparent density of 1 gained powder of test comparison example are distinguished, with
Examples 1 to 5 compares, as a result referring to table 1.
The performance test results of 1 gained powder of 1 Examples 1 to 5 of table and comparative example
It can be seen from 1 test result of table compared with comparative example 1, the mobility of Examples 1 to 5 products obtained therefrom is obviously mentioned
It rises, apparent density is substantially reduced.It proves, indium oxide: the mass ratio of water is in (1.5~6): 1, indium oxide: the mass ratio of binder
In (20~60): when 1, being able to ascend the mobility of product, reduce its apparent density.
Comparative example 2
It is carried out according to the preparation process of embodiment 2, unlike:
The specific surface area for adjusting indium oxide raw material, adjusts to 30~35m2/g；
The sand milling condition (zirconia ball partial size is 1.2mm, and 600min is sanded under 600rpm revolving speed) of tin oxide slurry is adjusted,
The average particle size of tin oxide in tin oxide slurry is sanded to 5 μm.
According to the test method in embodiment 1, the object phase of 2 gained powder of comparative example, and the mobility of test powders are detected
And apparent density, it is compared with embodiment 2, as a result referring to table 2.
The performance test results of 2 comparative example of table, 2 gained powder
It can be seen from 2 test result of table compared with comparative example 2, the mobility of 2 products obtained therefrom of embodiment is obviously improved,
Apparent density is substantially reduced.It proves, indium oxide specific surface area is controlled in 5~25m2/ g, and control the sand milling of tin oxide slurry
When partial size to tin oxide average particle size is 0.1~2.5 μm, it is able to ascend the mobility of product, and keep low-apparent-density.
Comparative example 3
Feeding is carried out according to embodiment 3, unlike, preparation method is ground using direct mixing；It is specific as follows: will to own
Material is placed in horizontal sand mill, is turned that 600min is sanded with 1500rpm, is obtained ITO slurry.Above-mentioned ITO slurry is spray-dried,
Inlet temperature is 200 DEG C, outlet temperature is 80 DEG C, after screening, obtains powder.
Mobility and apparent density test are carried out to gained powder, it is found that apparent density and mobility value increase, respectively
For 2.56g/cm2And 102.23s/50g.It proves, prepared by the specific mode that is gradually sanded according to the invention, could be acquired of fine quality
Good ito powder.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.To these embodiments
A variety of modifications will be readily apparent to those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to widest model consistent with the principles and novel features disclosed in this article
It encloses.
Claims (10)
1. a kind of preparation method of ito powder, which comprises the following steps:
A) indium oxide, dispersing agent are mixed into sand milling with water, obtains indium oxide slurry；
B) tin oxide and dispersant are sanded, obtain tin oxide slurry；
C) the indium oxide slurry, tin oxide slurry are mixed into sand milling with binder, obtains ITO slurry；
D) the ITO slurry is spray-dried, obtains ito powder；
The step a) and step b) is limited without sequence.
2. preparation method according to claim 1, which is characterized in that in the step a), the specific surface area of indium oxide is 5
~25m2/g；
The mass ratio of indium oxide and water is (1.5~6): 1.
3. preparation method according to claim 1, which is characterized in that in the step b), the specific surface area of tin oxide is 5
~20m2/g。
4. preparation method according to claim 1, which is characterized in that the mass ratio of the indium oxide and binder is (20
~60): 1；
The binder is the oligomeric species binder of dihydric alcohol.
5. preparation method according to claim 1, which is characterized in that in the step a), being averaged to indium oxide is sanded
Granularity is 2.5 μm or less；
In the step b), being sanded to the average particle size of tin oxide is 0.1~2.5 μm.
6. preparation method according to claim 1 or 5, which is characterized in that in the step a):
Dispersing agent is selected from alcohols dispersing agent；
The mass ratio of indium oxide and dispersing agent is (120~250): 1.
7. preparation method according to claim 1 or 5, which is characterized in that in the step b):
Dispersing agent is selected from alcohols dispersing agent；
The mass ratio of tin oxide and dispersing agent is (20~60): 1.
8. preparation method according to claim 1 or 4, which is characterized in that the step c) includes:
C1 indium oxide slurry) is mixed into sand milling with tin oxide slurry, obtains intermediate pulp；
C2 the intermediate pulp) is mixed into sand milling with binder, obtains ITO slurry；
The step c1) in:
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 100~600min；
The step c2) in:
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 50~300min.
9. preparation method according to claim 1 or 5, which is characterized in that in the step a):
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 100~600min；
In the step b):
The zirconia ball partial size used in sand milling is 0.1~3.0mm；
The revolving speed of sand milling is 500~1500rpm, and the time is 50~300min.
10. preparation method according to claim 1, which is characterized in that the mass ratio of the indium oxide and tin oxide is (8
~99.5): 1；
The inlet temperature of the spray drying is 150~250 DEG C, and outlet temperature is 50~150 DEG C；
The binder is polyethylene glycol；
The dispersing agent is polyvinyl alcohol.
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| CN116216770A (en) * | 2022-12-15 | 2023-06-06 | 先导薄膜材料（广东）有限公司 | Blue IZO powder and preparation method thereof |
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| CN116216770A (en) * | 2022-12-15 | 2023-06-06 | 先导薄膜材料（广东）有限公司 | Blue IZO powder and preparation method thereof |
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Application publication date: 20190920 |