CN103922703A - Indium tin oxide target material and sintering preparation method thereof - Google Patents
Indium tin oxide target material and sintering preparation method thereof Download PDFInfo
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Abstract
The invention discloses an indium tin oxide target material sintering preparation method which comprises the following steps: putting a target biscuit into a sintering furnace, keeping the sintering furnace be in a normal air atmosphere, raising the temperature inside the sintering furnace in a speed of 15-100 DEG C per hour till the temperature achieves a first high temperature, keeping the temperature for 4-10 hours, converting the atmosphere inside the sintering furnace to be in a normal pressure pure oxygen atmosphere, and raising the temperature inside the sintering furnace in a speed of 20-100 DEG C per hour till the temperature achieves a second high temperature; oscillating the temperature inside the sintering furnace for 5-30 hours within an oscillation range between a third high temperature and the second high temperature, specifically, when the temperature achieves the second high temperature, raising the temperature inside the sintering furnace in a speed of 50-300 DEG C per hour till the temperature achieves the third high temperature, and when the temperature achieves the third high temperature, reducing the temperature inside the sintering furnace till the temperature achieves the second high temperature in a speed of 150-300 DEG C per hour; reducing the temperature to be the normal temperature in the speed of 20-200 DEG C per hour, so as to prepare the indium tin oxide target material. The technical scheme is low in application cost and high in product quality.
Description
Technical field
The present invention relates to tin indium oxide target material with and sintering preparation method.
Background technology
Tin indium oxide (IndiumTinOxide, be called for short ITO) be a kind of semiconductor mixtures being mixed by indium (III family) oxide compound (In2O3) and tin (IV family) oxide compound (SnO2), its mixing quality ratio is generally: 90%In2O3,10%SnO2.The main characteristic of ITO is its electricity conduction and optically transparent combination.ITO is yellow grey partially when bulk state, and when film like, is clear, colorless.Therefore target is the core material of liquid crystal panel transparency electrode, along with LCD TV, flat-panel monitor, notebook computer and mobile phone market constantly increase, the demand of ITO target is to the situation of sustainable growth.
Indium tin oxide films adopts the method deposition of electron beam evaporation, physical vapor deposition or some sputter-deposition technologies to obtain conventionally.Because the transparent conductive film that adopts magnetron sputtering method to prepare has advantages of good uniformity, long service life, it is the method for generally using at present.Yet, ITO target is in the process of magnetron sputtering, sputter area (being commonly called as " runway ") very easily produces the problem of poisoning dross, affects production efficiency and plated film quality, and in the process of magnetron sputtering, the poisoning dross of ITO target is to have the biggest problem to be solved during current ITO target is produced.
Atmosphere sintering is a kind of method that eighties of last century grows up the nineties, under can be in predetermined atmosphere, carry out sintering, obtain well behaved target, atmosphere sintering method has become the main stream approach of manufacturing high-end ITO target at present, but production unit and process regulation are required to harshness, and production cost is higher.
It is the control of density that normal pressure atmosphere sintering process is manufactured one of difficult point of ITO target, at high temperature the In in (higher than 1200 ℃) ITO sosoloid
2o
3with SnO
2decompose,
In
2O
3→In
2O+O
2(gas) （1）
2SnO
2→2SnO+O
2(gas) （2）
Due to In
2o
3, SnO
2decomposition and In
2o, SnO and O
2escape, a lot of gas channels and hole have been formed, hindered the raising of ITO target density, in order to suppress above-mentioned decomposition and volatilization process, the normal High Temperature High Pressure pure oxygen sintering that adopts, still makes in this way at present, has certain danger in production, to agglomerating plant require highly, and technique is wayward.
Summary of the invention
One of embodiment of the present invention object be to provide a kind of tin indium oxide target material with and sintering preparation method, this technical scheme can obtain the quality oxide indium tin target of the low dross rate of high-density under normal pressure atmosphere.
A kind of tin indium oxide target material sintering preparation method that the embodiment of the present invention provides, comprising:
Target biscuit is inserted in sintering oven;
Keep atmospheric air atmosphere in described sintering oven, with 15-100 degree Celsius of temperature rise rate hourly, improve the interior temperature of described sintering oven until temperature reaches the first high temperature, under described the first high temperature, constant temperature is 4 to 10 hours;
Atmosphere in described sintering oven is converted to normal pressure pure oxygen atmosphere, with 20-100 degree Celsius of temperature rise rate hourly, improves the interior temperature of described sintering oven until temperature reaches the second high temperature;
Keep normal pressure pure oxygen atmosphere in described sintering oven, temperature in sintering oven vibrated 5 to 30 hours in the vibration interval of described the second high temperature in described third high temperature:
When temperature reaches described the second high temperature, with 50-300 degree Celsius of temperature rise rate hourly, improve temperature in described sintering oven until temperature reaches third high temperature, when temperature reaches third high temperature, with 150-300 degree Celsius of rate of temperature fall hourly, reduce the temperature in described sintering oven until temperature reaches described the second high temperature, return;
Described the first high temperature is not less than 700 degrees Celsius and is not more than 900 degrees Celsius, and described the second high temperature is not less than 1250 degrees Celsius and is not more than 1350 degrees Celsius, and described third high temperature is not less than 1500 degrees Celsius and is not more than 1650 degrees Celsius;
Atmosphere in described sintering oven is converted to atmospheric air atmosphere, with 20-200 degree Celsius of rate of temperature fall hourly, temperature in described sintering oven is down to normal temperature, obtain described tin indium oxide target material.
Alternatively, with 25 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the first high temperature, described the first high temperature equals 800 degrees Celsius, and under described the first high temperature, constant temperature is 4 hours;
With 50 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the second high temperature, described the second high temperature equals 1300 degrees Celsius;
With 50-300 degree Celsius of temperature rise rate hourly or rate of temperature fall, temperature in described sintering oven is vibrated 15 hours in the vibration interval of described the second high temperature in described third high temperature;
With 100 degrees Celsius of rate of temperature fall hourly, make temperature in described sintering oven be down to normal temperature, obtain described tin indium oxide target material.
Alternatively, with 15 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the first high temperature, described the first high temperature equals 800 degrees Celsius, and under described the first high temperature, constant temperature is 4 hours;
With 20 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the second high temperature, described the second high temperature equals 1300 degrees Celsius;
With 50 degrees Celsius of temperature rise rates hourly or rate of temperature fall, temperature in described sintering oven is vibrated 15 hours in the vibration interval of described the second high temperature in described third high temperature;
With 20 degrees Celsius of rate of temperature fall hourly, make temperature in described sintering oven be down to normal temperature, obtain described tin indium oxide target material.
Alternatively, with 40 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the first high temperature, described the first high temperature equals 800 degrees Celsius, and under described the first high temperature, constant temperature is 4 hours;
With 100 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the second high temperature, described the second high temperature equals 1300 degrees Celsius;
With 300 degrees Celsius of temperature rise rates hourly or rate of temperature fall, temperature in described sintering oven is vibrated 15 hours in the vibration interval of described the second high temperature in described third high temperature;
With 200 degrees Celsius of rate of temperature fall hourly, make temperature in described sintering oven be down to normal temperature, obtain described tin indium oxide target material.
Alternatively, described target biscuit adopts following technique to make:
Purity being not less than to 99.99% indium-tin oxide powder removes macrobead to obtain specific surface is 7-14m through grinding, sieving
2the powder of/g, obtains described target biscuit by described powder by hydraulic pressure or slurry casting moulding.
Alternatively, specifically, keep atmospheric flow air atmosphere in described sintering oven, with 15-100 degree Celsius of temperature rise rate hourly, improve the interior temperature of described sintering oven until temperature reaches the first high temperature.
Alternatively, specifically, the atmosphere in described sintering oven is converted to atmospheric flow air atmosphere, with 20-200 degree Celsius of rate of temperature fall hourly, temperature in described sintering oven is down to normal temperature.
The present embodiment provides a kind of tin indium oxide target material of being made by above-mentioned arbitrary described tin indium oxide target material sintering preparation method.
Therefore, application the present embodiment technical scheme, the whole sintering process of ITO target is all carried out under normal pressure, and with respect to the high-pressure sinter method of prior art, the enforcement of the present embodiment method is more easy to implement, and implementation cost is lower; And, in the present embodiment, ITO target is sintered to after the second temperature, the vibration temperature environment that adopts repeatedly gradient of temperature to change is carried out sintering to the ITO target in sintering oven, make under the comparatively high temps environment in temperature oscillation interval: the lower ITO target of the 3rd temperature (as 1650 ℃) is sosoloid, the In in ITO target
2o
3press chemical formula (1) formula and decompose, the SnO in ITO target
2press chemical formula (2) and decompose, when the lesser temps (as 1300 ℃) in temperature oscillation interval, reversed reaction is carried out in above-mentioned chemical formula (1), (2).Visible, before sintering finishes, adopt above-mentioned temperature oscillation sintering processes, can effectively suppress that decomposition due to In2O3, SnO2 causes In2O, SnO and O2 to escape affecting ITO target density and the problem of high dross rate in magnetron sputtering process.
Apply the density that the present embodiment technical scheme has improved ITO target, the target density that evidence application the present embodiment technical scheme obtains can remain on more than 99.6%, and target dross rate in magnetron sputtering process is low, and, apply this technical scheme and overcome the shortcoming that adopts High Temperature High Pressure pure oxygen sintering, sintering process safety, sintering cost is low.
Embodiment
To tie specific embodiment below and describe the present invention in detail, in this illustrative examples of the present invention and explanation, be used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and purity is at least to 99.99% ITO powder and removes macrobeads and obtain ITO target powder through grinding, cross 300 mesh sieves, and the specific surface value of ITO target powder is 7-14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding.ITO target biscuit is inserted in sintering oven.
(2) with 15-100 degree Celsius of temperature rise rate hourly, improve the interior temperature of sintering oven until temperature reaches a predetermined high temperature (being designated as the first high temperature), under the first high temperature, constant temperature is 4 to 10 hours, and this first high temperature span is 800 ± 100 degrees Celsius in the present embodiment.Can the atmosphere in sintering oven be atmospheric air atmosphere in this step, can certainly but be not limited to preferably keep the open environment of sintering oven, make it under the air atmosphere of atmospheric flow, carry out this step.
After carrying out step (1), the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 20-100 degree Celsius of temperature rise rate hourly, improve temperature in sintering oven, until temperature reaches another predetermined high temperature (being designated as the second high temperature), this first high temperature span is 1300 ± 50 degrees Celsius in the present embodiment.
(4) keep the interior normal pressure pure oxygen atmosphere of sintering oven, make temperature in sintering oven in vibration interval (the second high temperature is to third high temperature), heat up and lower the temperature and carry out temperature variation vibration.Wherein third high temperature is the highest sintering temperature of ITO target, and third high temperature span is not more than 1650 degrees Celsius for being not less than 1500 degrees Celsius.
The variation of temperature oscillation is as follows: when temperature reaches the second high temperature, with 50-300 degree Celsius of temperature rise rate hourly, improve in sintering oven temperature until temperature reaches third high temperature; When temperature reaches third high temperature, with 150-300 degree Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches the second high temperature.
The vibration of repetition said temperature, keeps temperature oscillation 5 to 30 hours.
(5) with 20-200 degree Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtains the present embodiment ITO target.When carrying out this step, can but transfer the atmosphere in current sintering oven to normal pressure air atmosphere, the open environment identical with atmosphere, also can be, but not limited to the normal pressure pure oxygen atmosphere that keeps original.
Therefore, adopting the present embodiment technical scheme, the whole sintering process of ITO target is all carried out under normal pressure, and with respect to the high-pressure sinter method of prior art, the enforcement of the present embodiment method is more easy to implement, and implementation cost is lower; And, in the present embodiment, ITO target is sintered to after the second temperature, the vibration temperature environment that adopts repeatedly gradient of temperature to change is carried out sintering to the ITO target in sintering oven, make under the comparatively high temps environment in temperature oscillation interval: the lower ITO target of the 3rd temperature (as 1650 ℃) is sosoloid, the In in ITO target
2o
3press chemical formula (1) formula and decompose, the SnO in ITO target
2press chemical formula (2) and decompose, when the lesser temps (as 1300 ℃) in temperature oscillation interval, reversed reaction is carried out in above-mentioned chemical formula (1), (2).Visible, before sintering finishes, adopt above-mentioned temperature oscillation sintering processes, can effectively suppress that decomposition due to In2O3, SnO2 causes In2O, SnO and O2 to escape affecting ITO target density and the problem of high dross rate in magnetron sputtering process.
Apply the density that the present embodiment technical scheme has improved ITO target, the target density that evidence application the present embodiment technical scheme obtains can remain on more than 99.6%, and target dross rate in magnetron sputtering process is low, and, apply this technical scheme and overcome the shortcoming that adopts High Temperature High Pressure pure oxygen sintering, sintering process safety, sintering cost is low.
Embodiment 2:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and the ITO powder that is 99.99% by purity obtains ITO target powder through grinding, cross 200 mesh sieves removal macrobeads, and the specific surface value of ITO target powder is 7m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding, ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere (for example open normal pressure atmospheric environment), with 25 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.800 degrees Celsius of lower constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 50 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1300 degrees Celsius.
(4) keep the interior normal pressure pure oxygen atmosphere of sintering oven, make temperature in sintering oven in vibration interval (1300-1600 degree Celsius), heat up and lower the temperature and carry out temperature oscillation.
The variation of temperature oscillation is as follows: when temperature reaches 1300 degrees Celsius, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1600 degrees Celsius; When temperature reaches 1600 degrees Celsius, with 100 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1300 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 15 hours.
(5) atmosphere in current sintering oven is transferred to normal pressure air atmosphere with 100 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtain the present embodiment ITO target.
embodiment 3:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and the ITO powder that is 99.99% by purity obtains ITO target powder through grinding, cross 300 mesh sieves removal macrobeads, and the specific surface value of ITO target powder is 14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding, ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 15 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 700 degrees Celsius.700 degrees Celsius of lower constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 20 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1250 degrees Celsius.
(4) keep the interior normal pressure pure oxygen atmosphere of sintering oven, make temperature in sintering oven in vibration interval (1250-1500 degree Celsius), heat up and lower the temperature and carry out temperature oscillation.
The variation of temperature oscillation is as follows: when temperature reaches 1250 degrees Celsius, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1500 degrees Celsius; When temperature reaches 1500 degrees Celsius, with 100 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1250 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 15 hours.
(5) atmosphere in current sintering oven is transferred to normal pressure air atmosphere with 20 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtain the present embodiment ITO target.
Embodiment 4:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and the ITO powder that is 99.99% by purity obtains ITO target powder through grinding, cross 300 mesh sieves removal macrobeads, and the specific surface value of ITO target powder is 14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding, ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 40 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 900 degrees Celsius.900 degrees Celsius of lower constant temperature 10 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 40 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1350 degrees Celsius.
(4) keep the interior normal pressure pure oxygen atmosphere of sintering oven, make temperature in sintering oven in vibration interval (1350-1650 degree Celsius), heat up and lower the temperature and carry out temperature oscillation.
The variation of temperature oscillation is as follows: when temperature reaches 1350 degrees Celsius, with 300 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1500 degrees Celsius; When temperature reaches 1650 degrees Celsius, with 300 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1650 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 30 hours.
(5) atmosphere in current sintering oven is transferred to normal pressure air atmosphere with 200 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtain the present embodiment ITO target.
Embodiment 5:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and the ITO powder that is 99.99% by purity obtains ITO target powder through grinding, cross 300 mesh sieves removal macrobeads, and the specific surface value of ITO target powder is 14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding, ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 15 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.800 degrees Celsius of lower constant temperature 10 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 20 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1300 degrees Celsius.
(4) keep the interior normal pressure pure oxygen atmosphere of sintering oven, make temperature in sintering oven in vibration interval (1300-1500 degree Celsius), heat up and lower the temperature and carry out temperature oscillation.
The variation of temperature oscillation is as follows: when temperature reaches 1300 degrees Celsius, with 50 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1500 degrees Celsius; When temperature reaches 1500 degrees Celsius, with 50 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1300 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 5 hours.
(5) atmosphere in current sintering oven is transferred to normal pressure air atmosphere with 20 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtain the present embodiment ITO target.
Embodiment 6:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and the ITO powder that is 99.99% by purity obtains ITO target powder through grinding, cross 300 mesh sieves removal macrobeads, and the specific surface value of ITO target powder is 14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding, ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 15 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.800 degrees Celsius of lower constant temperature 10 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 40 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1300 degrees Celsius.
(4) keep the interior normal pressure pure oxygen atmosphere of sintering oven, make temperature in sintering oven in vibration interval (1300-1650 degree Celsius), heat up and lower the temperature and carry out temperature oscillation.
The variation of temperature oscillation is as follows: when temperature reaches 1300 degrees Celsius, with 300 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1650 degrees Celsius; When temperature reaches 1650 degrees Celsius, with 300 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1300 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 30 hours.
(5) atmosphere in current sintering oven is transferred to normal pressure air atmosphere with 200 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtain the present embodiment ITO target.
Reference example 1:
The ITO target sintering preparation method that the present embodiment provides is mainly as follows:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and purity is not less than to 99.99% ITO powder and removes macrobeads and obtain ITO target powder through grinding, cross 300 mesh sieves, and the specific surface value of ITO target powder is 14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding, ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 25 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.800
degree Celsius lower constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 50 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1300 degrees Celsius.
(4) keep normal pressure pure oxygen atmosphere in sintering oven, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1600 degrees Celsius; 1600 degrees Celsius of lower constant temperature 15 hours.
(5) atmosphere in current sintering oven is transferred to normal pressure air atmosphere with 100 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtain the present embodiment ITO target.
Reference example 2:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and purity is at least to 99.99% ITO powder and removes macrobeads and obtain ITO target powder through grinding, cross 300 mesh sieves, and the specific surface value of ITO target powder is 7-14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding.ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 25 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.Constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 50 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1200 degrees Celsius.
(4) keep normal pressure pure oxygen atmosphere in sintering oven, make temperature in sintering oven in the vibration interval of 1200-1500, heat up and lower the temperature and carry out temperature variation vibration.
The variation of temperature oscillation is as follows: when temperature reaches 1200 degrees Celsius, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1500 degrees Celsius; When temperature reaches 1500 degrees Celsius, with 100 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1200 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 15 hours.
(5) with 100 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtains the present embodiment ITO target.
Reference example 3:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and purity is at least to 99.99% ITO powder and removes macrobeads and obtain ITO target powder through grinding, cross 300 mesh sieves, and the specific surface value of ITO target powder is 7-14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding.ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 25 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.Constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 50 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1230 degrees Celsius.
(4) keep normal pressure pure oxygen atmosphere in sintering oven, make temperature in sintering oven in the vibration interval of 1230-1500, heat up and lower the temperature and carry out temperature variation vibration.
The variation of temperature oscillation is as follows: when temperature reaches 1230 degrees Celsius, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1500 degrees Celsius; When temperature reaches 1500 degrees Celsius, with 100 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1230 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 15 hours.
(5) with 100 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtains the present embodiment ITO target.
Reference example 4:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and purity is at least to 99.99% ITO powder and removes macrobeads and obtain ITO target powder through grinding, cross 300 mesh sieves, and the specific surface value of ITO target powder is 7-14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding.ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 25 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.Constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 50 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1380 degrees Celsius.
(4) keep normal pressure pure oxygen atmosphere in sintering oven, make temperature in sintering oven in the vibration interval of 1380-1650, heat up and lower the temperature and carry out temperature variation vibration.
The variation of temperature oscillation is as follows: when temperature reaches 1380 degrees Celsius, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1650 degrees Celsius; When temperature reaches 1650 degrees Celsius, with 100 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1380 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 15 hours.
(5) with 100 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtains the present embodiment ITO target.
Reference example 5:
(1) previously prepared good ITO target biscuit is inserted in sintering oven;
The ITO target of the present embodiment adopts following methods to make, and purity is at least to 99.99% ITO powder and removes macrobeads and obtain ITO target powder through grinding, cross 300 mesh sieves, and the specific surface value of ITO target powder is 7-14m
2/ g's, then powder is obtained to ITO target biscuit by hydraulic pressure or slurry casting moulding.ITO target biscuit is inserted in sintering oven.
(2) keeping the atmosphere in sintering oven is atmospheric flow air atmosphere, with 25 degrees Celsius of temperature rise rates hourly, improves the interior temperature of sintering oven until temperature reaches 800 degrees Celsius.Constant temperature 4 hours.Then the atmosphere in sintering oven is converted to normal pressure pure oxygen atmosphere.。
(3) keep normal pressure pure oxygen atmosphere in sintering oven, with 50 degrees Celsius of temperature rise rates hourly, improve temperature in sintering oven, until temperature reaches 1400 degrees Celsius.
(4) keep normal pressure pure oxygen atmosphere in sintering oven, make temperature in sintering oven in the vibration interval of 1400-1650, heat up and lower the temperature and carry out temperature variation vibration.
The variation of temperature oscillation is as follows: when temperature reaches 1400 degrees Celsius, with 100 degrees Celsius of temperature rise rates hourly, improve in sintering ovens temperature until temperature reaches 1650 degrees Celsius; When temperature reaches 1650 degrees Celsius, with 100 degrees Celsius of rate of temperature fall hourly, reduce temperature in sintering oven until temperature reaches 1400 degrees Celsius.
The vibration of repetition said temperature, keeps temperature oscillation 15 hours.
(5) with 100 degrees Celsius of rate of temperature fall hourly, temperature in sintering oven is down to normal temperature, obtains the present embodiment ITO target.
The ITO target respectively above-described embodiment 2-6 and comparative example 1-5 method being obtained adopts Archimedes's drainage, measure the density of target, and respectively each target is made respectively to magnetron sputtering plating according to identical magnetron sputtering membrane process target is carried out to magnetron sputtering film test, when the sputter of target accumulative total reaches 160wh/cm2, measure the surface cord fraction of coverage of target.
DCO result data is in detail shown in ginseng one.
Table one
| Sample number into spectrum | Target density | Plated film rear surface dross fraction of coverage |
| Embodiment 2 | 99.8% | 10% |
| Embodiment 3 | 99.1% | 40% |
| Embodiment 4 | 99.4% | 30% |
| Embodiment 5 | 99.6% | 20% |
| Embodiment 6 | 99.7% | 25% |
| Reference example 1 | 98.50% | 100% |
| Reference example 2 | 98.92% | 40% |
| Reference example 3 | 98.85% | 45% |
| Reference example 4 | 98.95% | 43% |
| Reference example 5 | 98.90% | 50% |
Wherein the dross rate in table one is specially and on magnetic sputter runway, exists tumor (target corrodes the oxide compound tumor that runway can generate black gradually) region with respect to the ratio of the area in sputter runway region.、
In addition, it should be noted that, in ITO target field, the qualified density of the ITO target of sintering is generally 99%, surpasses 99% and is considered to as qualified target, otherwise be defective unavailable target.
From table one, adopt embodiment of the present invention technical scheme can obtain beyond thought effect.
Above-described embodiment, does not form the restriction to this technical scheme protection domain.The modification of doing within any spirit at above-mentioned embodiment and principle, be equal to and replace and improvement etc., within all should being included in the protection domain of this technical scheme.
Claims (8)
1. a tin indium oxide target material sintering preparation method, is characterized in that, comprising:
Target biscuit is inserted in sintering oven;
Keep atmospheric air atmosphere in described sintering oven, with 15-100 degree Celsius of temperature rise rate hourly, improve the interior temperature of described sintering oven until temperature reaches the first high temperature, under described the first high temperature, constant temperature is 4 to 10 hours;
Atmosphere in described sintering oven is converted to normal pressure pure oxygen atmosphere, with 20-100 degree Celsius of temperature rise rate hourly, improves the interior temperature of described sintering oven until temperature reaches the second high temperature;
Keep normal pressure pure oxygen atmosphere in described sintering oven, temperature in sintering oven vibrated 5 to 30 hours in the vibration interval of described the second high temperature in described third high temperature:
When temperature reaches described the second high temperature, with 50-300 degree Celsius of temperature rise rate hourly, improve temperature in described sintering oven until temperature reaches third high temperature, when temperature reaches third high temperature, with 150-300 degree Celsius of rate of temperature fall hourly, reduce the temperature in described sintering oven until temperature reaches described the second high temperature, return;
Described the first high temperature is not less than 700 degrees Celsius and is not more than 900 degrees Celsius, and described the second high temperature is not less than 1250 degrees Celsius and is not more than 1350 degrees Celsius, and described third high temperature is not less than 1500 degrees Celsius and is not more than 1650 degrees Celsius;
Atmosphere in described sintering oven is converted to atmospheric air atmosphere, with 20-200 degree Celsius of rate of temperature fall hourly, temperature in described sintering oven is down to normal temperature, obtain described tin indium oxide target material.
2. tin indium oxide target material sintering preparation method according to claim 1, is characterized in that,
With 25 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the first high temperature, described the first high temperature equals 800 degrees Celsius, and under described the first high temperature, constant temperature is 4 hours;
With 50 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the second high temperature, described the second high temperature equals 1300 degrees Celsius;
With 50-300 degree Celsius of temperature rise rate hourly or rate of temperature fall, temperature in described sintering oven is vibrated 15 hours in the vibration interval of described the second high temperature in described third high temperature;
With 100 degrees Celsius of rate of temperature fall hourly, make temperature in described sintering oven be down to normal temperature, obtain described tin indium oxide target material.
3. tin indium oxide target material sintering preparation method according to claim 1, is characterized in that,
With 15 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the first high temperature, described the first high temperature equals 800 degrees Celsius, and under described the first high temperature, constant temperature is 4 hours;
With 20 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the second high temperature, described the second high temperature equals 1300 degrees Celsius;
With 50 degrees Celsius of temperature rise rates hourly or rate of temperature fall, temperature in described sintering oven is vibrated 15 hours in the vibration interval of described the second high temperature in described third high temperature;
With 20 degrees Celsius of rate of temperature fall hourly, make temperature in described sintering oven be down to normal temperature, obtain described tin indium oxide target material.
4. tin indium oxide target material sintering preparation method according to claim 1, is characterized in that,
With 40 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the first high temperature, described the first high temperature equals 800 degrees Celsius, and under described the first high temperature, constant temperature is 4 hours;
With 100 degrees Celsius of temperature rise rates hourly, temperature in described sintering oven is increased to described the second high temperature, described the second high temperature equals 1300 degrees Celsius;
With 300 degrees Celsius of temperature rise rates hourly or rate of temperature fall, temperature in described sintering oven is vibrated 15 hours in the vibration interval of described the second high temperature in described third high temperature;
With 200 degrees Celsius of rate of temperature fall hourly, make temperature in described sintering oven be down to normal temperature, obtain described tin indium oxide target material.
5. according to arbitrary described tin indium oxide target material sintering preparation method of claim 1 to 4, it is characterized in that,
Described target biscuit adopts following technique to make:
Purity being not less than to 99.99% indium-tin oxide powder removes macrobead to obtain specific surface is 7-14m through grinding, sieving
2the powder of/g, obtains described target biscuit by described powder by hydraulic pressure or slurry casting moulding.
6. according to arbitrary described tin indium oxide target material sintering preparation method of claim 1 to 4, it is characterized in that,
Specifically, keep atmospheric flow air atmosphere in described sintering oven, with 15-100 degree Celsius of temperature rise rate hourly, improve the interior temperature of described sintering oven until temperature reaches the first high temperature.
7. according to arbitrary described tin indium oxide target material sintering preparation method of claim 1 to 4, it is characterized in that,
Specifically, the atmosphere in described sintering oven is converted to atmospheric flow air atmosphere, with 20-200 degree Celsius of rate of temperature fall hourly, temperature in described sintering oven is down to normal temperature.
8. a tin indium oxide target material of being made by the arbitrary described tin indium oxide target material sintering preparation method of claim 1 to 7.
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