CN112811896A - Method for preparing indium tin oxide target material based on particle grading accumulation model - Google Patents

Method for preparing indium tin oxide target material based on particle grading accumulation model Download PDF

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CN112811896A
CN112811896A CN202110071125.3A CN202110071125A CN112811896A CN 112811896 A CN112811896 A CN 112811896A CN 202110071125 A CN202110071125 A CN 202110071125A CN 112811896 A CN112811896 A CN 112811896A
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刘家祥
翟晓宇
刘婷
李敏
于源
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Beijing University of Chemical Technology
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Abstract

The invention discloses a method for preparing an indium tin oxide target material based on a particle grading accumulation model. The method is characterized in that: the stacking process of the ITO particles is researched by adopting ternary and binary particle grading stacking models, and the particle size ratio of three spherical particles in the ternary particle grading stacking model satisfies the relationship
Figure DDA0002906006610000011
Figure DDA0002906006610000012
The ratio of the number of the three spherical powder particles is 1 (1-2) to 1-2; the particle size ratio of two spherical particles in the binary particle grading accumulation model satisfies the relationship
Figure DDA0002906006610000013
Or

Description

Method for preparing indium tin oxide target material based on particle grading accumulation model
Technical Field
The invention relates to a method for preparing an indium tin oxide target material with high density and low resistivity by taking three ITO spherical powder with different grain diameters as raw materials. The indium tin oxide target material prepared by the method is suitable for preparing an indium tin oxide film by a magnetron sputtering method.
Background
Indium Tin Oxide (ITO) or tin-doped Indium oxide (ITO) is a transparent conductive oxide material with excellent photoelectric properties and wide applications. The ITO thin film material has excellent electrical and optical properties, such as: low resistivity, 10-4In the order of Ω · cm; the transmittance of the light source is more than 95% in the wave band of 400-760 nm; the absorption rate of the 100-400 nm wave band is more than 85%; the reflectivity of the wave band of 760 nm-1 mm is more than 70 percent; the attenuation rate of the wave band of 0.1 mm-1 m is more than 85 percent. The ITO film is widely applied to the fields of flat panel displays, organic electroluminescent devices, vehicle windshields and the like. The main methods for preparing the ITO film include a spray pyrolysis method, a magnetron sputtering method, a magnetron reactive sputtering method of an indium tin alloy target under an oxygen atmosphere, and the like. The ITO target magnetron sputtering method is the most widely applied method, and the ITO film prepared by the method has more excellent photoelectric property and stability. The prerequisite for preparing ITO film with excellent electrical and optical properties is to prepare ITO ceramic target material with high density and low resistivity.
In the process of stacking the ITO particles, gaps exist among the particles, so that the density of the biscuit is reduced, the resistivity of the biscuit is increased, and the performance of the target is influenced. At present, ITO biscuit is prepared mainly by taking single-size particles as raw materials, and gaps inevitably exist among the particles. The invention designs ternary and binary particle grading accumulation models, prepares biscuit and target material by taking ITO spherical powder with three or two different particle sizes as raw materials, and fills small particles in gaps among large particles, thereby effectively reducing the gaps among the particles and improving the accumulation density.
Disclosure of Invention
The invention aims to take ITO spherical powder with three different grain diameters as raw materials, and small grains are filled in gaps among large grains, so that the gaps among the grains are reduced, and the accumulation is improvedAnd (4) obtaining the ITO target material with high density and low resistivity. The stacking process of the ITO particles is researched by adopting ternary and binary particle grading stacking models, and the particle diameters of three spherical particles in the ternary particle grading stacking model meet the proportional relation
Figure BDA0002906006590000021
The particle size ratio of two particles in the binary particle grading accumulation model satisfies the relationship
Figure BDA0002906006590000022
Or
Figure BDA0002906006590000023
ITO spherical powder with the particle size ranges of 275-295 nm, 108-128 nm and 54-74 nm is designed and prepared, and the average particle sizes of the three kinds of spherical powder are 285nm, 118nm and 64nm respectively. The method has the advantages of simple preparation process, simple equipment, low production cost, high density and low resistivity of the ITO target material obtained by sintering.
The preparation method of the ITO target material with high density and low resistivity is characterized by comprising the following steps: by solvothermal method with In (NO)3)3And SnCl4·5H2O is used as raw material, organic base triethylamine is used as precipitant, L-histidine is used as shape control agent, and dimethylformamide is used as solvent. In (NO)3)3And SnCl4·5H2The adding amount of O is calculated according to the mass ratio In of indium oxide and tin oxide In the mixed solution2O3:SnO2Adding the powder in a ratio of 9:1 to prepare ITO spherical powder with the particle size range of 275-295 nm and the average particle size of 285 nm. By coprecipitation method, using metal indium and SnCl4·5H2O as raw material, indium dissolved In nitric acid, ammonia water as precipitant, In and SnCl4·5H2The adding amount of O is calculated according to the mass ratio In of indium oxide and tin oxide In the mixed solution2O3:SnO2Adding the powder in a ratio of 9:1 to prepare ITO spherical powder with the particle size ranges of 108-128 nm and 54-74 nm and the average particle sizes of 118nm and 64 nm. Using three or two kinds of ITO powder with different grain diameters as raw material, adding dispersing agent polyvinylpyrrolidone and adhesive polyvinyl alcohol, and makingBall-milling granulation, compression molding and cold isostatic pressing to prepare a biscuit, and finally sintering the biscuit at high temperature in an oxygen atmosphere to prepare the ITO target.
Further, In (NO)3)3And SnCl4·5H2Adding a precipitator triethylamine and a shape control agent L-histidine into the mixed solution of O, so that the concentrations of the triethylamine and the L-histidine in the mixed solution are respectively 0.5-4 mol/L and 0.01-0.3 mol/L, the reaction time is 6-120 h, and the reaction temperature is 230-250 ℃.
Further, In (NO)3)3And SnCl4·5H2And (3) dropwise adding ammonia water as a precipitator into the mixed solution of O at the speed of 0.01-1 mL/s until the pH value of the solution is 9-10.
Further, a ternary and binary particle grading accumulation model is adopted to research the accumulation process of the ITO particles, and the particle size ratio of three spherical particles in the ternary particle grading accumulation model satisfies the relationship
Figure BDA0002906006590000024
The ratio of the number of the three spherical powder particles is 1 (1-2) to 1-2; the particle size ratio of two spherical particles in the binary particle grading accumulation model satisfies the relationship
Figure BDA0002906006590000025
Figure BDA0002906006590000026
Or
Figure BDA0002906006590000027
The ratio of the number of the two kinds of spherical powder particles is 1 (1-6). Ternary and binary powder grading combinations are designed, and three or two ITO spherical powders with different grain diameters are used as raw materials to prepare a biscuit and a target material.
Furthermore, the addition amount of the dispersant polyvinylpyrrolidone is 0.1-3.5% of the mass of the indium tin oxide composite powder, and the addition amount of the adhesive polyvinyl alcohol is 0.1-3.5% of the mass of the indium tin oxide composite powder.
Further, the biscuit molding process comprises the following steps: the granulation powder is molded by combining die pressing and isostatic pressing to obtain a biscuit, wherein the die pressing pressure is 3-10 MPa, and the pressure maintaining time is 3-10 min; the cold isostatic pressure is 250-350 MPa, and the pressure maintaining time is 5-15 min.
Furthermore, the sintering temperature of the target material is 1350-1600 ℃, and the sintering time of the target material is 4-16 h.
Technical effects
The invention has the technical effects that: ITO spherical powder with the particle size range of 275-295 nm and the average particle size of 285nm is prepared by a solvothermal method, and ITO spherical powder with the particle size range of 108-128 nm and 54-74 nm and the average particle size of 118nm and 64nm is prepared by a coprecipitation method. And (3) powder granulation process: the addition amount of the dispersant polyvinylpyrrolidone is 0.1-3.5% of the mass of the indium tin oxide composite powder, and the addition amount of the adhesive polyvinyl alcohol is 0.1-3.5% of the mass of the indium tin oxide composite powder. Biscuit forming process: and the granulated powder is subjected to combined molding of mould pressing and isostatic pressing to obtain a biscuit. Wherein the mould pressing pressure is 3-10 MPa, and the pressure maintaining time is 3-10 min; the cold isostatic pressure is 250-350 MPa, and the pressure maintaining time is 5-15 min. The target material sintering process comprises the following steps: the sintering temperature of the target material is 1350-1600 ℃, and the sintering time of the target material is 4-16 h. The stacking process of the ITO particles is researched by adopting ternary and binary particle grading stacking models, and the particle size ratio of three spherical powder particles in the ternary particle grading stacking model satisfies the relationship
Figure BDA0002906006590000031
The ratio of the number of the three spherical powder particles is 1 (1-2) to 1-2; the particle size ratio of two spherical powder particles in the binary particle grading accumulation model satisfies the relationship
Figure BDA0002906006590000032
Or
Figure BDA0002906006590000033
Figure BDA0002906006590000034
The ratio of the number of the two kinds of spherical powder particles is 1 (1-6). Three spherical powders with the particle size ranges of 275-295 nm, 108-128 nm and 54-74 nm are preparedThe average grain diameters of the powder are 285nm, 118nm and 64nm respectively, and the high-density low-resistivity ITO target material is prepared by high-temperature sintering. The relative density of the target material was 99.67%, and the resistivity of the target material was 0.79X 10-4Ω·cm。
Drawings
FIG. 1 is a process flow chart of the method for preparing ITO target material of the invention.
FIG. 2 is a scanning electron microscope photograph of ITO target material prepared by the method of the present invention with relative density, resistivity and scanning electron microscope at different sintering temperatures. (a) Relative density and resistivity; (b)1350 ℃; (c)1400 ℃; (d)1450 ℃; (e)1500 ℃; (f)1550 ℃.
FIG. 3 is the SEM pictures of the relative density, resistivity and scanning temperature of the ITO target material prepared by the method of the present invention. (a) Relative density and resistivity; (b)6 h; (c)8 h; (d)10 h; (e)12 h; (f) and 14 h.
Detailed Description
The method comprises the following specific implementation steps:
(1) by solvothermal method with In (NO)3)3And SnCl4·5H2O is used as raw material, organic base triethylamine is used as precipitant, L-histidine is used as shape control agent, and dimethylformamide is used as solvent. In (NO)3)3And SnCl4·5H2The adding amount of O is calculated according to the mass ratio In of indium oxide and tin oxide In the mixed solution2O3:SnO2Adding the powder in a ratio of 9:1 to prepare ITO spherical powder with the particle size range of 275-295 nm and the average particle size of 285 nm. By coprecipitation method, using metal indium and SnCl4·5H2O as raw material, indium dissolved In nitric acid, ammonia water as precipitant, In and SnCl4·5H2The adding amount of O is calculated according to the mass ratio In of indium oxide and tin oxide In the mixed solution2O3:SnO2Adding the powder in a ratio of 9:1 to prepare ITO spherical powder with the particle size ranges of 108-128 nm and 54-74 nm and the average particle sizes of 118nm and 64 nm. Taking 285nm, 118nm and 64nm ITO powder as raw materials to prepare ITO biscuit and ITO target material.
(2)In(NO3)3And SnCl4·5H2In mixed solution of OAdding a precipitator triethylamine and a shape control agent L-histidine to ensure that the concentrations of the triethylamine and the L-histidine are 0.5-4 mol/L and 0.01-0.3 mol/L respectively, wherein the reaction time is 6-120 h and the reaction temperature is 230-250 ℃.
(3)In(NO3)3And SnCl4·5H2And (3) dropwise adding ammonia water as a precipitator into the mixed solution of O at the speed of 0.01-1 mL/s until the pH value of the solution is 9-10.
(4) The addition amount of the dispersant polyvinylpyrrolidone is 0.1-3.5% of the mass of the indium tin oxide composite powder, and the addition amount of the adhesive polyvinyl alcohol is 0.1-3.5% of the mass of the indium tin oxide composite powder.
(5) The biscuit molding process comprises the following steps: the granulation powder is molded by combining die pressing and isostatic pressing to obtain a biscuit, wherein the die pressing pressure is 3-10 MPa, and the pressure maintaining time is 3-10 min; the cold isostatic pressure is 250-350 MPa, and the pressure maintaining time is 5-15 min.
(6) The sintering temperature of the target material is 1350-1600 ℃, and the sintering time of the target material is 4-16 h.
Example 1
37.6038 g of In (NO) were weighed out separately3)3And 4.3825 g SnCl4·5H2O was dissolved in 500mL of dimethylformamide, and heated with stirring at 70 ℃ to dissolve the indium tin salt. The above solution was subjected to a constant temperature water bath at 0 ℃ and 3.8788 g of L-histidine were added. And (3) stirring the solution uniformly, adding 50.595 g of triethylamine, continuously stirring for 15min, and pouring a proper amount of the solution into a reaction kettle with a polytetrafluoroethylene lining. And (3) placing the reaction kettle in a constant-temperature drying box at 250 ℃ for reaction for 24 hours. And respectively washing the reaction product for 5 times by using absolute ethyl alcohol and deionized water, and drying the reaction product to obtain blue ITO spherical powder with the particle size range of 275-295 nm and the average particle size of 285 nm. 5.70 g of metallic indium are dissolved in 30mL of super-pure nitric acid aqueous solution, and the solution and 1.78 g of SnCl are mixed4·5H2And adding O into 100mL of deionized water to obtain a mixed solution, dropwise adding ammonia water into the mixed solution at the normal temperature at the speed of 0.6mL/s and 0.05mL/s, continuing stirring for 15min after the pH value of the solution is 9.5, and standing and aging for 2h to obtain the ITO precursor. ITO precursor by using absolute ethyl alcohol and deionized waterAnd drying after washing for 5 times respectively. The ITO precursor is calcined for 2h at 600 ℃ to obtain yellow ITO spherical powder with the particle size ranges of 108-128 nm and 54-74 nm and the average particle sizes of 118nm and 64 nm.
The spherical powder particles are regarded as spherical to be calculated, and the ratio of the particle diameters of the three kinds of spherical powder is
Figure BDA0002906006590000051
According to the formula m-N ρ V and
Figure BDA0002906006590000052
it can be known that
Figure BDA0002906006590000053
Wherein m is the powder mass, N is the particle number of the powder, V is the particle volume, ρ is the particle density, and d is the particle diameter. The ratio of the particle number of the three spherical powder is 1:1:1 (namely N)1＝N2＝N3) Therefore, the mass ratio of the three spherical powders satisfies the relation:
Figure BDA0002906006590000054
the total mass of the ITO mixed powder was set to 10 g, and 9.2386 g, 0.6565 g, and 0.1049 g of the ITO powder with different particle sizes were weighed according to the above calculation procedure, and then 0.1 g of polyvinylpyrrolidone and 0.1 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the mill rotation speed of 500r/min to obtain the granulated powder. Weighing 5 g of granulated ITO powder, and carrying out compression molding treatment on the granulated ITO powder, wherein the mold pressing pressure is 5MPa, and the pressure maintaining time is 5 min; and then cold isostatic pressing is carried out, the pressure is 300MPa, and the pressure maintaining time is 10min, thus obtaining the biscuit. Placing the biscuit in a box furnace, setting the heating rate to be 3 ℃/min within the range from room temperature to 500 ℃, and preserving heat for 2 hours; setting the temperature rise rate to 9 ℃/min within the range of 500 ℃ to 1550 ℃, introducing oxygen into the box-type furnace at the oxygen flow rate of 120L/h, and preserving the temperature for 10h at 1550 ℃ to obtain the ITO target material with the relative density of 99.22 percent and the resistivity of 3.81 multiplied by 10-4Ω·cm。
Example 2
According to implementationIn the calculation process in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder with three different particle sizes in example 1 are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed and treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating at a rate of 3 ℃/min within a range from room temperature to 500 ℃, and preserving heat for 2 hours; heating at a rate of 9 ℃/min within a range of 500 ℃ to 1550 ℃, introducing oxygen into the box-type furnace at a flow rate of 120L/h, and keeping the temperature at 1550 ℃ for 10h to obtain the ITO target material with a relative density of 99.67 percent and a resistivity of 0.79 multiplied by 10-4Ω·cm。
Example 3
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes were weighed, respectively, and then 0.15 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating at a rate of 3 ℃/min within a range from room temperature to 500 ℃, and preserving heat for 2 hours; heating at a rate of 9 ℃/min within a range of 500 ℃ to 1550 ℃, introducing oxygen into the box-type furnace at a flow rate of 120L/h, and keeping the temperature at 1550 ℃ for 10h to obtain the ITO target material with the relative density of 99.03% and the resistivity of 4.16 multiplied by 10-4Ω·cm。
Example 4
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. Weighing the granulated ITO powder 5The granulated particles were treated according to the molding process of example 1 to obtain an ITO green body. Placing the biscuit in a box furnace, heating at a rate of 3 ℃/min within a range from room temperature to 500 ℃, and preserving heat for 2 hours; heating at a rate of 9 ℃/min within a range of 500 ℃ to 1350 ℃, introducing oxygen into the box-type furnace at a flow rate of 120L/h, and preserving heat at 1350 ℃ for 10 h. The ITO target material has the relative density of 88.57 percent and the resistivity of 16.39 multiplied by 10-4Ω·cm。
Example 5
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating at a rate of 3 ℃/min within a range from room temperature to 500 ℃, and preserving heat for 2 hours; heating at a rate of 9 ℃/min within a range of 500-1400 ℃, introducing oxygen into the box-type furnace at a flow rate of 120L/h, and preserving heat at 1400 ℃ for 10 h. The ITO target material has a relative density of 92.33% and a resistivity of 10.03X 10-4Ω·cm。
Example 6
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and in the range of 500 ℃ to 1450 ℃, introducing oxygen into the box type furnace, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1450 ℃ for 10 h. The relative density of the prepared ITO target material is 95.62 percentResistivity of 6.31X 10-4Ω·cm。
Example 7
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1500 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1500 ℃ for 10 h. The ITO target material has a relative density of 99.45% and a resistivity of 1.86 × 10-4Ω·cm。
Example 8
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 6 h. The ITO target material has a relative density of 99.39% and a resistivity of 2.32 × 10-4Ω·cm。
Example 9
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0 g of 0.1 g of polyvinylpyrrolidone are added to the ITO mixed powder15 grams of polyvinyl alcohol. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder, wherein the ball-milling time is set. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 8 h. The ITO target material has a relative density of 99.57% and a resistivity of 1.17 × 10-4Ω·cm。
Example 10
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 12 h. The ITO target material has a relative density of 99.54% and a resistivity of 1.34 × 10-4Ω·cm。
Example 11
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:1, 9.2386 g, 0.6565 g and 0.1049 g of the ITO powder of example 1 with three different particle sizes are weighed respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol are added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating to 500 deg.C at a rate of 3 deg.C/min, and holding for 2 hr(ii) a And (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 14 h. The ITO target material has a relative density of 99.31% and a resistivity of 3.65 × 10-4Ω·cm。
Example 12
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:2:1 (i.e., N)1＝2N2＝N3) The mass of the three spherical powders satisfies the following relational expression:
Figure BDA0002906006590000091
therefore, 8.6694 g, 1.2322 g and 0.0984 g of ITO powder of three different particle sizes in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.32% and a resistivity of 2.36 × 10-4Ω·cm。
Example 13
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1:2 (i.e., N)1＝N2＝2N3) The mass of the three spherical powders satisfies the following relational expression:
Figure BDA0002906006590000092
therefore, 9.1427 g, 0.6497 g and 0.2076 g of ITO powder of three different particle sizes in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed and prepared by the molding method of example 1And treating the granules to obtain an ITO biscuit. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.12% and a resistivity of 1.31 × 10-4Ω·cm。
Example 14
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:2:2 (i.e., N)1＝2N2＝2N3) The mass of the three spherical powders satisfies the following relational expression:
Figure BDA0002906006590000093
therefore, 8.5849 g, 1.2202 g and 0.1949 g of ITO powder of three different particle sizes in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 98.75% and a resistivity of 6.11 × 10-4Ω·cm。
Example 15
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000101
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1 (i.e., N)1＝N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000102
accordingly, 9.8878 g and 0.1122 g of the compound prepared in example 1 were weighed out separately285nm and 64nm ITO powder, and then 0.1 g polyvinylpyrrolidone and 0.15 g polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours at the rotating speed of 500r/min to obtain the granulated powder. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has the relative density of 99.07 percent and the resistivity of 4.62 multiplied by 10-4Ω·cm。
Example 16
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000103
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:3 (i.e., N)1＝3N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000104
therefore, 9.6707 g and 0.3293 g of the 285nm and 64nm ITO powders prepared in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.19% and a resistivity of 2.31 × 10-4Ω·cm。
Example 17
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000111
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:5 (i.e., N)1＝5N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000112
therefore, 9.4629 g and 0.5371 g of the 285nm and 64nm ITO powders prepared in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.59% and a resistivity of 0.91 × 10-4Ω·cm。
Example 18
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000113
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:6 (i.e., N)1＝6N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000114
therefore, 9.3623 g and 0.6377 g of the 285nm and 64nm ITO powders prepared in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace at room temperature to 500 ℃ at a heating rate of3 ℃/min, and keeping the temperature for 2 hours; oxygen is introduced into the box furnace in the interval of 500 ℃ to 1550 ℃, the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has the relative density of 99.43 percent and the resistivity of 1.37 multiplied by 10-4Ω·cm。
Example 19
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000115
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:1 (i.e., N)1＝N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000116
therefore, 9.3365 g and 0.6635 g of the 285nm and 118nm ITO powders prepared in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.09% and a resistivity of 4.56 × 10-4Ω·cm。
Example 20
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000121
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:3 (i.e., N)1＝3N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000122
thus, 8.2426 g and 1.7574 g of nut were weighed out separatelyThe 285nm and 118nm ITO powders prepared in example 1 were mixed, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.21% and a resistivity of 2.25 × 10-4Ω·cm。
Example 21
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000123
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:5 (i.e., N)1＝5N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000124
therefore, 7.3782 g and 2.6218 g of the 285nm and 118nm ITO powders prepared in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.63% and a resistivity of 0.86 × 10-4Ω·cm。
Example 22
The ratio of the particle diameters of the two spherical powders is
Figure BDA0002906006590000131
According to the calculation procedure in example 1, when the ratio of the number of particles is 1:6 (i.e., N)1＝6N2) The mass of the two kinds of spherical powder satisfies the following relational expression:
Figure BDA0002906006590000132
therefore, 7.0106 g and 2.9894 g of the 285nm and 118nm ITO powders prepared in example 1 were weighed, respectively, and then 0.1 g of polyvinylpyrrolidone and 0.15 g of polyvinyl alcohol were added to the ITO mixed powder. And (3) ball-milling the mixed powder in an agate ball-milling tank for 3 hours to obtain granulated powder, wherein the rotating speed is 500 r/min. 5 g of granulated ITO powder was weighed, and the granulated particles were treated according to the molding process in example 1 to obtain an ITO green compact. Placing the biscuit in a box furnace, heating the biscuit within the range from room temperature to 500 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 2 hours; and (3) introducing oxygen into the box-type furnace within the range of 500-1550 ℃, wherein the flow rate of the oxygen is 120L/h, the heating rate is 9 ℃/min, and the temperature is kept at 1550 ℃ for 10 h. The ITO target material has a relative density of 99.44% and a resistivity of 1.31 × 10-4Ω·cm。

Claims (5)

1. A method for preparing an indium tin oxide target material based on a particle grading accumulation model is characterized by comprising the following steps: preparing a mixed solution by using indium and tin metal or indium and tin metal soluble salt as raw materials, preparing ITO composite powder with different particle sizes by a solvothermal method or a coprecipitation method, and preparing an indium tin oxide target material by granulating, molding and sintering the composite powder; the method is characterized in that: preparing ITO (indium tin oxide) biscuit from ITO composite powder with different particle sizes by adopting a ternary particle or binary particle grading accumulation model, wherein the particle size ratio of three particles in the ternary particle grading accumulation model satisfies the relationship
Figure FDA0002906006580000011
The ratio of the number of the three powder particles is 1 (1-2) to 1-2; the particle size ratio of two particles in the binary particle grading accumulation model satisfies the relationship
Figure FDA0002906006580000012
Or
Figure FDA0002906006580000013
The ratio of the particle numbers of the two kinds of powders is 1 (1 to 6).
2. The method of claim 1, wherein: the solvothermal method is with In (NO)3)3And SnCl4·5H2O as a raw material, In (NO)3)3And SnCl4·5H2The adding amount of O is calculated according to the mass ratio In of indium oxide and tin oxide In the mixed solution2O3:SnO2Adding 9:1 dimethylformamide as a solvent, L-histidine as a shape control agent, wherein the addition amount is 0.01-0.3 mol/L calculated as the final concentration in the mixed solution, organic base triethylamine as a precipitator, the addition amount is 0.5-4 mol/L calculated as the final concentration in the mixed solution, the reaction temperature is 230-250 ℃, the reaction time is 6-120 h, and the ITO spherical powder with the particle size range of 275-295 nm and the average particle size of 285nm is prepared; the coprecipitation method is to use metallic indium and SnCl4·5H2O as raw material, indium dissolved in nitric acid, indium and SnCl4·5H2The adding amount of O is calculated according to the mass ratio In of indium oxide and tin oxide In the mixed solution2O3:SnO2Adding ammonia water as a precipitator at a dropping speed of 0.01-1 mL/s, dropping until the pH value of the solution is 9-10, drying the precipitate, and calcining to prepare ITO spherical powder with the particle size range of 108-128 nm, the average particle size of 118nm, the particle size range of 54-74 nm and the average particle size of 64 nm.
3. The method of claim 1, wherein: weighing three or two ITO spherical powder with the average particle sizes of 285nm, 118nm and 64nm, and mixing the three or two ITO spherical powder together to ensure that the ratio of the particle numbers of the three powder is 1 (1-2) to 1-2; the ratio of the particle numbers of the two kinds of powder is 1 (1 to 6); adding dispersant polyvinylpyrrolidone with the addition amount of 0.1-3.5% of the mass of the mixed ITO spherical powder, and adding adhesive polyvinyl alcohol with the addition amount of 0.1-3.5% of the mixed ITO spherical powder; and mixing the mixed powder in a planet ball mill to obtain the granulated powder.
4. The method of claim 1, wherein: compression molding the granulated powder, and then carrying out cold isostatic pressing to obtain a biscuit; wherein the mould pressing pressure is 3-10 MPa, and the pressure maintaining time is 3-10 min; the cold isostatic pressure is 250-350 MPa, and the pressure maintaining time is 5-15 min.
5. The method of claim 1, wherein: and sintering the biscuit in an oxygen atmosphere to obtain the ITO target, wherein the sintering temperature is 1350-1600 ℃, and the sintering time is 4-16 h.
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