CN105645931A - Process for sintering high-density ITO (indium-tin oxide) target under zero pressure - Google Patents
Process for sintering high-density ITO (indium-tin oxide) target under zero pressure Download PDFInfo
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- CN105645931A CN105645931A CN201610108132.5A CN201610108132A CN105645931A CN 105645931 A CN105645931 A CN 105645931A CN 201610108132 A CN201610108132 A CN 201610108132A CN 105645931 A CN105645931 A CN 105645931A
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Abstract
The invention provides a process for sintering a high-density ITO (indium-tin oxide) target under the zero pressure. The sintering time is shortened by adjusting the sintering time and temperature and strictly controlling the purity of sintering atmosphere oxygen and the purity of a load bearing board for sintering, so that the production efficiency is improved, the cost is reduced, the density of the sintered ITO target is increased, and the high-density ITO target with the relative density larger than 99.8% is prepared.
Description
Technical field
The present invention relates to ITO target and manufacture field, particularly relate to a kind of zero-pressure sintering high-density ITO target technique.
Background technology
ITO target is exactly Indium sesquioxide. and stannic oxide powder mix by a certain percentage after through a series of production technology machine-shaping, then the black gray expandable ceramic semiconductors that high-temperature atmosphere sintering (1600 degree, logical oxygen sinters) is formed. Ito thin film is to utilize ITO target as raw material, by magnetron sputtering, the gasification of ITO target is spattered and is crossed on glass substrate or flexible organic film. Ito thin film has electric conductivity and light transmission, general 30 nanometers of thickness--and 200 nanometers. At present for the preparation of ITO target, technique is very ripe, but there is long processing time in process of production unavoidably, production efficiency ITO target consistency that is low and that produce is not enough, the problem that product quality is relatively low.
The patent No. is the middle preparation method proposing a kind of ITO target of Chinese patent " preparation method of a kind of low-resistivity ITO target " of CN105130416A, it is disclosed that a kind of sintering method, its content is: the high intensity green compact that step (3) is obtained carry out the ungrease treatment of green compact for 4��6 hours 400��600 DEG C of insulations, then it is with the ramp of 5��7 DEG C/min to 1550��1650 DEG C under 100% oxygen atmosphere in volumetric concentration, it is incubated 4��6 hours, oxysome volume concentrations is reduced to 10��40% insulation 4��6 hours again, cool to room temperature with the furnace to come out of the stove, obtain the ITO target of low-resistivity. although above-mentioned sintering method can produce ITO target in shorter sintering time, but the consistency of above-mentioned target can only achieve 99.5%, it is impossible to meets high-level instructions for use.
The patent No. be CN104773998A Chinese patent " sintering method of a kind of high-compactness ITO target " in it is also proposed that the sintering method of a kind of ITO target, its content is: the THICKNESS CONTROL of load bearing board is at 5 ~ 30mm, be provided with several equidistant perforate on the surface of load bearing board, the diameter control of each perforate is at 5 ~ 20mm, ITO base substrate after drying defatted is placed on load bearing board and sends in oxygen pressure stove, when being first warming up to 500 ~ 800 �� of C with the speed of 2 ~ 5 �� of C/min, first is incubated 1 ~ 5h, it is incubated in the period described first and passes into oxygen, when oxygen presses the pressure in stove to start immediately to keep the input flow rate of oxygen when reaching 0.3 ~ 0.8MPa, second it is incubated 1 ~ 5h when being warming up to 1000 ~ 1400 �� of C with the speed of 0.5 ~ 2 �� of C/min after described first insulation, it is incubated in the period described second and the input flow rate of oxygen is adjusted to 8 ~ 30L/min, when being warming up to 1500 ~ 1650 �� of C with the speed of 0.5 ~ 2 �� of C/min again after described second insulation, the 3rd is incubated 20 ~ 60h, it is incubated in the period the described 3rd and the input flow rate of oxygen is adjusted to 5 ~ 20L/min, described 3rd insulation is cooled to 1200 �� of C with the speed of 0.5 ~ 2 �� of C/min after terminating, now close the input flow rate of oxygen and make the pressure in oxygen pressure stove press stove to implement Temperature fall oxygen again when being down to normal pressure, the ITO target of consistency >=99.8% can be obtained after Temperature fall.Above-mentioned sintering method can produce the ITO target that consistency is more than 99.5% when producing ITO target, but the time used when sintering is longer, and production efficiency is not high. Therefore, the ITO target sintering process designing a kind of sintering time ITO target consistency that is few and that produce high just seems particularly significant.
Summary of the invention
For above-mentioned prior art Problems existing, it is an object of the invention to provide a kind of zero-pressure sintering high-density ITO target technique, by adjusting sintering time and temperature, and the strict control of the purity to sintering atmosphere oxygen and sintering load bearing board, designs a kind of production time is few, efficiency is high and produces the ITO target consistency sintering process more than 99.8%.
The present invention provides a kind of zero-pressure sintering high-density ITO target technique, the manufacturing process steps of described ITO target is: powder process-powder process-pelletize-molding-sintering-machining-binding-inspection, wherein it is sintered to be placed in high-temperature oxygen sintering furnace plain embryo obtained for upper one molding procedure and is sintered, sintering atmosphere oxygen used in described sintering circuit, purity is 99.999%, and load bearing board used in described sintering circuit is Al2O3Load bearing board, purity is 99.99%, and time and the temperature distribution of described sintering are as follows: furnace temperature is raised to more than 1000 DEG C with 400 DEG C/hr by (one), is incubated 10 hours, oxygen flow 8L/min; (2) with 100 DEG C/hr, furnace temperature is raised to more than 1200 DEG C, is incubated 6 hours, oxygen flow 12L/min; (3) with 50 DEG C/hr, furnace temperature is raised to more than 1450 DEG C, is incubated 4 hours, oxygen flow 16L/min; (4) with 50 DEG C/hr, furnace temperature is raised to more than 1600 DEG C, is incubated 20 hours, oxygen flow 20L/min, terminates sintering.
Further improvement is that: the in-furnace temperature of the sintering electric furnace used during described sintering is 1500 DEG C ~ 1700 DEG C, and the calandria power of described sintering electric furnace is 180KW.
Further improvement is that: the interior thorax of described sintering electric furnace includes top, sidewall and siege, described top, sidewall and siege is equipped with thermal insulation board, described top and sidewall are also equipped with ceramic fibre, described siege is also equipped with refratory insulating brick.
Further improvement is that: the furnace pressure of described sintering electric furnace is zero-pressure.
The invention has the beneficial effects as follows: by adjusting sintering time and temperature, and the strict control of the purity to sintering atmosphere oxygen and sintering load bearing board, shorten sintering time thus improving production efficiency, reduce cost, and improve the ITO target density sintered out, prepare the relative density high-density ITO targe material more than 99.8%.
Detailed description of the invention
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment is only used for explaining the present invention, is not intended that limiting the scope of the present invention.
Present embodiments provide a kind of zero-pressure sintering high-density ITO target technique, the manufacturing process steps of described ITO target is: powder process-powder process-pelletize-molding-sintering-machining-binding-inspection, wherein it is sintered to be placed in high-temperature oxygen sintering furnace plain embryo obtained for upper one molding procedure and is sintered, sintering atmosphere oxygen used in described sintering circuit, purity is 99.999%, and load bearing board used in described sintering circuit is Al2O3Load bearing board, purity is 99.99%, and time and the temperature distribution of described sintering are as follows: furnace temperature is raised to 1000 DEG C with 400 DEG C/hr by (one), is incubated 10 hours, oxygen flow 8L/min;(2) with 100 DEG C/hr, furnace temperature is raised to 1200 DEG C, is incubated 6 hours, oxygen flow 12L/min; (3) with 50 DEG C/hr, furnace temperature is raised to 1450 DEG C, is incubated 4 hours, oxygen flow 16L/min; (4) with 50 DEG C/hr, furnace temperature is raised to 1600 DEG C, is incubated 20 hours, oxygen flow 20L/min, terminates sintering. The in-furnace temperature of the sintering electric furnace used during described sintering is 1600 DEG C, and the calandria power of described sintering electric furnace is 180KW. The interior thorax of described sintering electric furnace includes top, sidewall and siege, described top, sidewall and siege is equipped with thermal insulation board, described top and sidewall are also equipped with ceramic fibre, described siege is also equipped with refratory insulating brick. The furnace pressure of described sintering electric furnace is zero-pressure.
By adjusting sintering time and temperature, and the strict control of the purity to sintering atmosphere oxygen and sintering load bearing board, shortening sintering time thus improving production efficiency, reducing cost, and improve the ITO target density sintered out, prepare the relative density high-density ITO targe material more than 99.8%.
Claims (4)
1. a zero-pressure sintering high-density ITO target technique, it is characterized in that: the manufacturing process steps of described ITO target is: powder process-powder process-pelletize-molding-sintering-machining-binding-inspection, wherein it is sintered to be placed in high-temperature oxygen sintering furnace plain embryo obtained for upper one molding procedure and is sintered, sintering atmosphere oxygen used in described sintering circuit, purity is 99.999%, and load bearing board used in described sintering circuit is Al2O3Load bearing board, purity is 99.99%, and time and the temperature distribution of described sintering are as follows: furnace temperature is raised to more than 1000 DEG C with 400 DEG C/hr by (one), is incubated 10 hours, oxygen flow 8L/min; (2) with 100 DEG C/hr, furnace temperature is raised to more than 1200 DEG C, is incubated 6 hours, oxygen flow 12L/min; (3) with 50 DEG C/hr, furnace temperature is raised to more than 1450 DEG C, is incubated 4 hours, oxygen flow 16L/min; (4) with 50 DEG C/hr, furnace temperature is raised to more than 1600 DEG C, is incubated 20 hours, oxygen flow 20L/min, terminates sintering.
2. a kind of zero-pressure sintering high-density ITO target technique as claimed in claim 1, it is characterised in that: the in-furnace temperature of the sintering electric furnace used during described sintering is 1500 DEG C ~ 1700 DEG C, and the calandria power of described sintering electric furnace is 180KW.
3. a kind of zero-pressure sintering high-density ITO target technique as claimed in claim 2, it is characterized in that: the interior thorax of described sintering electric furnace includes top, sidewall and siege, described top, sidewall and siege are equipped with thermal insulation board, described top and sidewall are also equipped with ceramic fibre, described siege is also equipped with refratory insulating brick.
4. a kind of zero-pressure sintering high-density ITO target technique as described in claim 1-3 any one, it is characterised in that: the furnace pressure of described sintering electric furnace is zero-pressure.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610108132.5A CN105645931A (en) | 2016-02-29 | 2016-02-29 | Process for sintering high-density ITO (indium-tin oxide) target under zero pressure |
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| CN201610108132.5A CN105645931A (en) | 2016-02-29 | 2016-02-29 | Process for sintering high-density ITO (indium-tin oxide) target under zero pressure |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167597A (en) * | 2010-12-20 | 2011-08-31 | 昆明理工大学 | Method of preparing ITO target material by oxygen atmosphere pressureless sintering process |
| CN102531636A (en) * | 2011-12-26 | 2012-07-04 | 昆明理工大学 | Preparation method of large-size ITO target material |
| CN102731067A (en) * | 2012-07-04 | 2012-10-17 | 韶关西格玛技术有限公司 | Preparation method of high-density ITO (indium tin oxide) evaporation target |
| CN103922703A (en) * | 2014-04-15 | 2014-07-16 | 广西华锡集团股份有限公司 | Indium tin oxide target material and sintering preparation method thereof |
| CN104773998A (en) * | 2015-03-31 | 2015-07-15 | 中国船舶重工集团公司第七二五研究所 | Sintering method of high-density ITO target |
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- 2016-02-29 CN CN201610108132.5A patent/CN105645931A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167597A (en) * | 2010-12-20 | 2011-08-31 | 昆明理工大学 | Method of preparing ITO target material by oxygen atmosphere pressureless sintering process |
| CN102531636A (en) * | 2011-12-26 | 2012-07-04 | 昆明理工大学 | Preparation method of large-size ITO target material |
| CN102731067A (en) * | 2012-07-04 | 2012-10-17 | 韶关西格玛技术有限公司 | Preparation method of high-density ITO (indium tin oxide) evaporation target |
| CN103922703A (en) * | 2014-04-15 | 2014-07-16 | 广西华锡集团股份有限公司 | Indium tin oxide target material and sintering preparation method thereof |
| CN104773998A (en) * | 2015-03-31 | 2015-07-15 | 中国船舶重工集团公司第七二五研究所 | Sintering method of high-density ITO target |
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Application publication date: 20160608 |