CN1891662A - Method for producing sputtering target - Google Patents
Method for producing sputtering target Download PDFInfo
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- CN1891662A CN1891662A CNA2006101000945A CN200610100094A CN1891662A CN 1891662 A CN1891662 A CN 1891662A CN A2006101000945 A CNA2006101000945 A CN A2006101000945A CN 200610100094 A CN200610100094 A CN 200610100094A CN 1891662 A CN1891662 A CN 1891662A
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- burning
- sputtering target
- manufacture method
- oxide powder
- indium oxide
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 89
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 51
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 47
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002994 raw material Substances 0.000 claims description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- 239000011812 mixed powder Substances 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 7
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 235000011089 carbon dioxide Nutrition 0.000 claims description 5
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000010304 firing Methods 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract 2
- 238000007493 shaping process Methods 0.000 description 15
- 239000002002 slurry Substances 0.000 description 14
- 238000001914 filtration Methods 0.000 description 12
- 238000000465 moulding Methods 0.000 description 11
- 239000000919 ceramic Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 230000006837 decompression Effects 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000000227 grinding Methods 0.000 description 4
- 238000005238 degreasing Methods 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- AZWHFTKIBIQKCA-UHFFFAOYSA-N [Sn+2]=O.[O-2].[In+3] Chemical compound [Sn+2]=O.[O-2].[In+3] AZWHFTKIBIQKCA-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000803 paradoxical effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The method for manufacturing the sputtering target by firing a raw mixture powder containing an indium oxide powder and an stannic oxide powder comprises the steps of: calcining at least indium oxide at 1,100[deg.]C to 1,300[deg.]C; preparing the raw mixture powder by using the calcined powder; and firing the mixture powder at a temperature 150[deg.]C or higher than the calcination temperature.
Description
Technical field
The present invention relates to the manufacture method of sputtering target.
Background technology
Generally, as forming a kind of of film process, well-known have a sputtering method.As sputtering method, owing to be the method that obtains film by the sputter sputtering target, big areaization can form high performance film expeditiously easily, so obtain utilizing in industry.In addition, in recent years as the mode of sputter, in reactant gas, carry out the reactive sputtering method of sputter in addition and at the back side of target magnet is set and realizes that film forming magnetron sputtering system of high speed etc. is known.
The film that is used for such sputtering method, particularly Indium sesquioxide-stannic oxide (In
2O
3-SnO
2Composite oxides, to call " ITO " in the following text) film because the visible light permeability height, and good conductivity, so be widely used in the antisweat heating film of liquid crystal indicator, glass and the infrared reflection film etc. as nesa coating.
For this reason, for high-efficiency and low-cost more forms film, even now, carry out sputtering condition and sputter equipment etc. improvement, how to make the efficient operation of device also become important thing.In addition, in such ITO sputter, shorten from setting behind the new sputtering target initial arc (paradoxical discharge) and disappear to the time of producing product and how long can use (accumulative total sputtering time: target lifetime) become problem after once setting.
Such ITO sputtering target handlebar indium oxide powder and stannic oxide powder mix (patent documentation 1) that dry type or wet forming, sintering obtain and in certain proportion for obtaining the indium oxide powder (with reference to patent documentation 2,3,4) of the polymolecularity that highdensity ITO sintered compact proposes.
In addition, also disclose by coprecipitation method wet type synthetic ito powder has been made the scheme (referring to patent documentation 5 etc.) of ITO sintered compact, disclose the scheme (with reference to patent documentation 6～9 etc.) of a plurality of wet type synthetic methods for the ito powder that obtains highdensity sintered compact equally
But, still wishing to seek not too to be subjected to the restriction of ito powder manufacture method, highly do not control sintering condition etc. and also can become more readily available highdensity sintered compact, the result can obtain the manufacture method of the sputtering target of long target of life-span.
[patent documentation 1] spy opens clear 62-21751 communique
[patent documentation 2] spy opens flat 5-193939 communique
[patent documentation 3] spy opens flat 6-191846 communique
[patent documentation 4] spy opens the 2001-261336 communique
[patent documentation 5] spy opens clear 62-21751 communique
[patent documentation 6] spy opens flat 9-221322 communique
[patent documentation 7] spy opens the 2000-281337 communique
[patent documentation 8] spy opens the 2001-172018 communique
[patent documentation 9] spy opens the 2002-68744 communique
Summary of the invention
The present invention is problem in view of above-mentioned these situations so that the manufacture method that can improve target lifetime and can obtain the sputtering target of highdensity sputtering target to be provided.
For solving above-mentioned problem, the manufacture method of the sputtering target of first aspect present invention, burning till when mixing the raw material contain indium oxide powder and stannic oxide powder and making sputtering target, at least at the mixed powder of 1100 ℃～1300 ℃ pre-burning indium oxide powders as raw material, this mixed powder to burn till than the high temperature more than 150 ℃ of described calcined temperature.
In the manufacture method of the sputtering target of first aspect present invention, by at least at specified temperature pre-burning indium oxide powder, the carbon content in the raw material can be obviously reduced, and, sputtering target highdensity, that target lifetime is long can be made by burning till mixed powder with the specified temperature higher than calcined temperature.
The manufacture method of the sputtering target of second aspect present invention, in first aspect present invention, the carbon content after the described indium oxide powder pre-burning is below 50ppm.
In the manufacture method of the sputtering target of second aspect present invention,, can definitely improve the target lifetime after burning till by making below the carbon content 50ppm after the indium oxide powder pre-burning.
The manufacture method of the sputtering target of third aspect present invention in the present invention first or second aspect, is carried out described indium oxide powder pre-burning, so that BET specific surface area thereafter is 0.8～4m
2/ g.
In the manufacture method of the sputtering target of third aspect present invention, carry out pre-burning within the limits prescribed by making the BET specific surface area, can improve the target density after burning till, improve target lifetime simultaneously definitely.
The manufacture method of the sputtering target of fourth aspect present invention, in the present invention first to the either side of the third aspect, the processing of avoiding raw material to contact during the mixed powder in described pre-burning and after burning till pre-burning with carbonic acid gas.
In the manufacture method of the sputtering target of fourth aspect present invention, contact with carbonic acid gas by avoiding raw material, can reduce the carbon concentration in the raw material after the pre-burning definitely.
The manufacture method of the sputtering target of fifth aspect present invention in the either side aspect the present invention first to fourth, makes density after burning till more than 99%.
In the manufacture method of the sputtering target of fifth aspect present invention, the density by making sputtering target can definitely improve target lifetime more than 99%.
The manufacture method of the sputtering target of sixth aspect present invention, in the either side aspect the present invention first to the 5th, tin content is with SnO
2Be scaled 2.3～45 quality %.
In the manufacture method of the sputtering target of sixth aspect present invention, because tin content is in the scope of regulation, so can form the film with desired electroconductibility.
In sum, in the present invention, with the temperature pre-burning raw material powder of regulation, and with the temperature range of regulation as thereafter firing temperature, can make the sputtering target that target lifetime is grown.
Embodiment
The manufacture method of sputtering target of the present invention, burning till when mixing the raw material contain indium oxide powder and stannic oxide powder and making sputtering target, at least at 1100 ℃～1300 ℃ pre-burning indium oxide powders, thereafter mixed powder to burn till than the high temperature more than 150 ℃ of described calcined temperature.
In the method for the invention, among the raw material, the pre-burning indium oxide powder is in order to reduce carbon content contained in the indium oxide powder at least.For effectively reduce carbon content must 1100 ℃～1300 ℃, preferably carry out pre-burning at 1150 ℃～1300 ℃.Even using the temperature lower to carry out pre-burning, because carbon can not reduced by the raw material powder chemisorption yet than this temperature.In addition, when using the temperature higher than this temperature to carry out pre-burning, carbon content reduces, but has problems at sintering process.That is, by to carry out sintering, can obtain the high-density sputtering target after the pre-burning, but, can make the BET specific surface area littler, might can not get highdensity target than the scope of regulation using when carrying out pre-burning than 1300 ℃ of high temperature than the high high temperature more than 150 ℃ of calcined temperature.
From this point, in the method for the invention, 1100 ℃～1300 ℃, preferably carry out pre-burning at 1150 ℃～1300 ℃.
In addition, be the carbon of oxidized indium powder chemistry absorption as the problem of making sputtering target, and in stannic oxide, adsorb carbon hardly, do not become problem.Thereby in the method for the invention, " at least at the mixed powder of 1100 ℃～1300 ℃ pre-burning indium oxide powders as raw material " means that the pre-burning indium oxide powder is just passable at least, not necessarily must the pre-burning stannic oxide powder.That is, when using indium oxide powder and stannic oxide, at least only the pre-burning indium oxide powder just can.Certainly, mean also and can carry out pre-burning at the state that mixes both.In addition, also can use the mixed powder that adds indium oxide-tin oxide powder (ito powder) at indium oxide powder and stannic oxide powder part, but in ito powder, because tin is solid-solubilized in the Indium sesquioxide, so absorption carbon is not problem, so not necessarily must carry out pre-burning.Certainly, it is also passable to carry out pre-burning.
In the method for the invention, the carbon content in the indium oxide powder after the pre-burning is below 50ppm, preferably below 20ppm, more preferably below 10ppm as mentioned above.As described below, the carbon that contains in the raw material powder influences target lifetime, burns to be combined with the sputtering target that carbon surpasses the raw material powder of 50ppm, and target lifetime obviously shortens.At this, when the raw material powder that uses carbon content to surpass 50ppm makes sputtering target,, and when using the following raw material powder of carbon content 50ppm, do not observe such metal because metal oxide by carbon reduction, can be confirmed metal in target.In addition, the carbon content in the indium oxide powder can use determination of carbon and sulfur device (for example, (strain) hole field makes the EMIA-2200 of manufacturing) to measure.When pre-burning contained the mixed powder of indium oxide powder, the carbon content of mensuration was considered to all be caused by Indium sesquioxide, so can calculate carbon content contained indium oxide powder from the content of indium oxide powder.
From such purpose, in the methods of the invention, the preferably processing of avoiding this raw material to contact during the burning till in pre-burning and after the pre-burning with carbonic acid gas.This is for absorbing carbon dioxide in the indium oxide powder that has prevented in pre-burning and increase the content of carbon.
In addition, in the methods of the invention, preferably carry out the pre-burning of described indium oxide powder, so that BET specific surface area thereafter is 0.8～4m
2/ g.By making the BET specific surface area within the limits prescribed, can obtain highdensity sputtering target during sintering.
In the methods of the invention, burn till the mixed powder manufacturing sputtering target that contains at the Indium sesquioxide of specified temperature pre-burning as mentioned above, at this moment, the density after burning till is preferably more than 99%.This is that target lifetime is long more because of highdensity more sputtering target.
Manufacture method to the raw material that uses in the present invention has no particular limits, as long as it is just passable to prepare to obtain the raw material of the sputtering target that target forms.In addition, raw material for example when using mixed oxidization indium powder and stannic oxide to scale, carry out before mixing and after mixing pre-burning all can, when mixing after pre-burning, the pre-burning indium oxide powder just can at least as mentioned above.
At this, the preferred tin content of the raw material of sputtering target is with SnO
2Be scaled the raw material of 2.3～45 quality %.This is because can form the cause of the film with desired electroconductibility.For example, SnO
2Solid solution capacity is the above raw materials of 2.3 quality %, and tin content is minimum also to be with SnO
2Be scaled 2.3 quality %, on the other hand, when surpassing 45 quality %, for example, because separate out SnO when forming film as sputtering target
2, hinder electroconductibility, so not preferred.
Below explanation is burnt till raw material in the methods of the invention and is obtained a example in the sputtering target operation.
The mixed powder of mixing raw material for example uses existing well-known various damp process or drying process to form, burn till.
As drying process, can enumerate (Cold Press) method of colding pressing and hot pressing (Hot Press) method etc.In cold press process, ito powder is filled into makes molding in the shaping die, under atmospheric environment or under the oxygen atmosphere, burn till, sintering.In pressure sintering, ito powder direct sintering in shaping die.
As damp process, preference is as filtering formula moulding method (opening flat 11-286002 communique with reference to the spy).This filters formula moulding method, uses filtration formula shaping die, and this filtrations formula shaping die is made of the non-water soluble material that is used for making from ceramic raw material slurry decompression eliminating moisture molding.This filtration formula shaping die has: the shaping counterdie that more than one water vent is arranged; Be arranged on this shaping with the strainer that water-permeable is arranged on the counterdie; Sealing member by being used to seal this strainer from the shaping of upper face side clamping with framed.This filtration formula shaping die with decomposable mode separately above-mentioned shaping with counterdie, being shaped is fitted together with framed, sealing member and filter set, the moisture from this strainer one side side decompression eliminating slurry only.This filters the slurry that the modulation of formula moulding method is made up of powder mix, ion exchanged water and organic additive, this slurry is injected filtration formula shaping die, only the moisture of getting rid of the slurry from this strainer one side side decompression manufactures body, and the ceramic formation body that obtains is carried out burning till behind the drying defatted.
At the firing temperature of each method, for example under ITO target situation, preferred 1300～1600 ℃, more preferably 1450～1600 ℃.Carry out to the size that obtains stipulating is shaped, the mechanical workout of processing is made target thereafter.
Generally after shaping, be preferably adjustment thickness the surface is ground, and then, implement the grinding of several stages,, remove micro-cracks by implementing the surface treatment of regulation for making surface smoothing.
Embodiment
Below, based on embodiment the present invention is described, but the invention is not restricted to this.
Embodiment 1
By wet type synthetic indium oxide powder 1100 ℃ carry out indium oxide powder 90 quality % that pre-burning forms and by same wet type synthetic stannic oxide at 1050 ℃ of raw material powders that carry out stannic oxide powder quality 10% that pre-burning forms as embodiment 1.
Embodiment 2
By wet type synthetic indium oxide powder 1150 ℃ carry out indium oxide powder 90 quality % that pre-burning forms and by same wet type synthetic stannic oxide powder at 1050 ℃ of raw material powders that carry out stannic oxide powder quality 10% that pre-burning forms as embodiment 2.
Embodiment 3
By wet type synthetic indium oxide powder 1200 ℃ carry out indium oxide powder 90 quality % that pre-burning forms and by same wet type synthetic stannic oxide powder at 1050 ℃ of raw material powders that carry out stannic oxide powder quality 10% that pre-burning forms as embodiment 3.
Embodiment 4
By wet type synthetic indium oxide powder 1250 ℃ carry out indium oxide powder 90 quality % that pre-burning forms and by same wet type synthetic stannic oxide powder at 1050 ℃ of raw material powders that carry out stannic oxide powder quality 10% that pre-burning forms as embodiment 4.
Embodiment 5
By wet type synthetic indium oxide powder 1300 ℃ carry out indium oxide powder 90 quality % that pre-burning forms and by same wet type synthetic stannic oxide powder at 1050 ℃ of raw material powders that carry out stannic oxide powder quality 10% that pre-burning forms as embodiment 5.
Comparative example 1
Carrying out indium oxide powder 90 quality % that pre-burning forms and carry out stannic oxide powder quality 10% that pre-burning forms 1 raw material powder as a comparative example at 1000 ℃ at 1000 ℃ by same wet type synthetic stannic oxide powder by wet type synthetic indium oxide powder.
Test example 1
Use determination of carbon and sulfur device ((strain) hole field makes the EMIA-2200 of manufacturing), be determined at the carbon content in the indium oxide powder after each embodiment and comparative example carry out pre-burning.The results are shown in table 1.In addition, the specific surface area of the usefulness BET method of the indium oxide powder after the pre-burning is compared together shown in the table 1.
Table 1
| Specimen coding | After carbon content (ppm) pre-burning | BET specific surface area (m 2/ g) after the pre-burning |
| Embodiment 1 | 50 | 3.6 |
| Embodiment 2 | 20 | 2.5 |
| Embodiment 3 | 20 | 1.8 |
| Embodiment 4 | 20 | 1.3 |
| Embodiment 5 | 10 | 0.8 |
| Comparative example 1 | 160 | 5.7 |
Production Example 1
The raw material of embodiment 1 is mixed, grinds with dry ball mill, with the wet bulb grinding machine it is ground again and make form slurry, this slurry is injected filtration formula shaping die, and only the moisture of getting rid of the slurry from the decompression of filtering surface side is made molding, and the ceramic formation body that obtains is carried out drying defatted.The relative density of this molding after the degreasing is 67.7% of a theoretical density 7.15.
The ceramic formation body that obtains is burnt till at 1600 ℃, obtain sputtering target as sintered compact.Its relative density is 99.9%.
Production Example 2
The raw material of embodiment 4 is mixed, grinds with dry ball mill, with the wet bulb grinding machine it is ground again and make form slurry, this slurry is injected filtration formula shaping die, and only the moisture of getting rid of the slurry from the decompression of filtering surface side is made molding, and the ceramic formation body that obtains is carried out drying defatted.The relative density of this molding after the degreasing is 68.0% of a theoretical density 7.15.
The ceramic formation body that obtains is burnt till at 1600 ℃, obtain sputtering target as sintered compact.Its relative density is 99.0%.
Compare Production Example 1
The raw material of comparative example 1 is mixed, grinds with dry ball mill, with the wet bulb grinding machine it is ground again and make form slurry, this slurry is injected filtration formula shaping die, and only the moisture of getting rid of the slurry from the decompression of filtering surface side is made molding, and the ceramic formation body that obtains is carried out drying defatted.The relative density of this molding after the degreasing is 60.0% of a theoretical density 7.15.
The ceramic formation body that obtains is burnt till at 1600 ℃, obtain sputtering target as sintered compact.Its relative density is 99.0%.
Test example 2
Use the sputtering target of Production Example 1,2 and comparison Production Example 1 to measure breakdown characteristics.That is, carry out continuous sputter with the DC magnetron sputtering, measure the life-span of 50Counts in following condition.At this, in the so-called 50Counts life-span, be meant and remove from bringing into use each target to dropping into electric weight 10Wh/cm
2Initial stage punctures number of times, and accumulation punctures number of times and reaches 50 times input electric weight (Wh/cm
2).In addition, the electric arc detecting device made from bright moral electric arc technology company (MAM Genesis) detects and punctures.The result is as shown in table 2 below.
From this result as can be seen, use by the present invention and compare in the comparison Production Example of the sputtering target of the pre-burning indium oxide powder of the specified temperature indium oxide powder low with using calcined temperature, breakdown characteristics is good, and target lifetime is long.
(sputtering condition)
Target size: 6 inches of diameters, thickness 6mm
Sputter mode: DC magnetron sputtering
Gas barrier: wheel-rotating pump+cryopump
Arrive vacuum tightness: 3.0 * 10
-7[Torr]
Ar pressure: 3.0 * 10
-3[Torr]
Oxygen partial pressure: 3.0 * 10
-5[Torr]
Sputter electric power: 300W (power density 1.6W/cm
2)
Table 2
| 50Counts life-span (Watt.hour/cm 2) | |
| Production Example 1 | 75 |
| Production Example 2 | 84 |
| Compare Production Example 1 | 29 |
Claims (9)
1. the manufacture method of sputtering target, it is characterized in that, burning till when mixing the raw material contain indium oxide powder and stannic oxide powder and making sputtering target, at least at the mixed powder of 1100 ℃～1300 ℃ pre-burning indium oxide powders as raw material, this mixed powder to burn till than the high temperature more than 150 ℃ of described calcined temperature.
2. the manufacture method of sputtering target as claimed in claim 1 is characterized in that, the carbon content after the described indium oxide powder pre-burning is below 50ppm.
3. the manufacture method of sputtering target as claimed in claim 1 or 2 is characterized in that, carries out described indium oxide powder pre-burning, so that BET specific surface area thereafter is 0.8～4m
2/ g.
4. the manufacture method of sputtering target as claimed in claim 1 is characterized in that, in described pre-burning and up to the mixed powder after the pre-burning burn till during avoid raw material to contact with carbonic acid gas processing.
5. the manufacture method of sputtering target as claimed in claim 2 is characterized in that, in described pre-burning and up to the mixed powder after the pre-burning burn till during avoid raw material to contact with carbonic acid gas processing.
6. the manufacture method of sputtering target as claimed in claim 1 is characterized in that, makes density after burning till more than 99%.
7. the manufacture method of sputtering target as claimed in claim 2 is characterized in that, makes density after burning till more than 99%.
8. the manufacture method of sputtering target as claimed in claim 1 is characterized in that, tin content is with SnO
2Be scaled 2.3～45 quality %.
9. the manufacture method of sputtering target as claimed in claim 2 is characterized in that, tin content is with SnO
2Be scaled 2.3～45 quality %.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005190805A JP2007009268A (en) | 2005-06-29 | 2005-06-29 | Method for manufacturing sputtering target |
| JP2005190805 | 2005-06-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1891662A true CN1891662A (en) | 2007-01-10 |
| CN100513354C CN100513354C (en) | 2009-07-15 |
Family
ID=37596896
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101000945A Active CN100513354C (en) | 2005-06-29 | 2006-06-29 | Method for producing sputtering target |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP2007009268A (en) |
| KR (1) | KR100814320B1 (en) |
| CN (1) | CN100513354C (en) |
| TW (1) | TWI306124B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102471871A (en) * | 2009-08-07 | 2012-05-23 | 住友金属矿山株式会社 | Tablet for vapor deposition and process for producing same |
| CN102959122A (en) * | 2010-08-05 | 2013-03-06 | 三菱综合材料株式会社 | Method for producing sputtering target, and sputtering target |
| CN116332637A (en) * | 2023-02-14 | 2023-06-27 | 芜湖映日科技股份有限公司 | Method for preparing ITO rotary target in solar cell industry |
| CN116496081A (en) * | 2023-04-17 | 2023-07-28 | 湘潭大学 | Indium tin oxide ternary compound target material and preparation method and application thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6359901B2 (en) * | 2014-07-16 | 2018-07-18 | 三菱マテリアル株式会社 | Sputtering target |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2979648B2 (en) * | 1990-12-20 | 1999-11-15 | 住友金属鉱山株式会社 | ITO sintered body |
| DE19822570C1 (en) * | 1998-05-20 | 1999-07-15 | Heraeus Gmbh W C | High density hot isostatically pressed indium-tin oxide sputter target |
| KR100474846B1 (en) * | 2002-03-22 | 2005-03-09 | 삼성코닝 주식회사 | Indium oxide powder, manufacturing method thereof, and manufacturing method of high density indium tin oxide target using the same |
| KR100577743B1 (en) * | 2004-07-01 | 2006-05-10 | 전자부품연구원 | Stack filter for use in signal transmitting and receiving part of mobile phone |
-
2005
- 2005-06-29 JP JP2005190805A patent/JP2007009268A/en not_active Withdrawn
-
2006
- 2006-06-19 TW TW095121840A patent/TWI306124B/en active
- 2006-06-28 KR KR1020060058442A patent/KR100814320B1/en not_active IP Right Cessation
- 2006-06-29 CN CNB2006101000945A patent/CN100513354C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102471871A (en) * | 2009-08-07 | 2012-05-23 | 住友金属矿山株式会社 | Tablet for vapor deposition and process for producing same |
| CN102471871B (en) * | 2009-08-07 | 2014-02-26 | 住友金属矿山株式会社 | Tablet for vapor deposition and process for producing same |
| TWI491580B (en) * | 2009-08-07 | 2015-07-11 | Sumitomo Metal Mining Co | Tablet for vapor depositing and method for producing the same |
| CN102959122A (en) * | 2010-08-05 | 2013-03-06 | 三菱综合材料株式会社 | Method for producing sputtering target, and sputtering target |
| CN116332637A (en) * | 2023-02-14 | 2023-06-27 | 芜湖映日科技股份有限公司 | Method for preparing ITO rotary target in solar cell industry |
| CN116496081A (en) * | 2023-04-17 | 2023-07-28 | 湘潭大学 | Indium tin oxide ternary compound target material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| TWI306124B (en) | 2009-02-11 |
| CN100513354C (en) | 2009-07-15 |
| KR100814320B1 (en) | 2008-03-18 |
| KR20070001811A (en) | 2007-01-04 |
| JP2007009268A (en) | 2007-01-18 |
| TW200710245A (en) | 2007-03-16 |
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