WO2007114429A1 - 酸化インジウム系透明導電膜及びその製造方法 - Google Patents
酸化インジウム系透明導電膜及びその製造方法 Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- 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
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- 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
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- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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Definitions
- the present invention relates to a transparent conductive film that can be easily patterned by weak acid etching with an amorphous film, has a low resistance, has a high transmittance, and can be easily crystallized, and a method for manufacturing the same.
- ITO indium oxide-tin oxide
- liquid crystal display devices are widely used as heat-generating films for preventing condensation in glass, infrared reflective films, etc., as transparent conductive films. There is a problem that it is difficult.
- a transparent conductive film of indium oxide monozinc zinc oxide ( ⁇ ) is known as an amorphous film.
- ⁇ indium oxide monozinc zinc oxide
- Patent Document 1 JP 2005-135649 A (Claims)
- the present invention provides a transparent conductive film which can be easily patterned by weak acid etching with an amorphous film, has a low resistance, has a high transmittance, and can be further easily crystallized, and a method for producing the same It is an issue to provide.
- the present invention is an indium oxide-based transparent conductive film doped with norium, which is an amorphous film having low resistance and excellent transparency, and is easily etched by weak acid etching. Can be put together and can be crystallized more easily. As a result, the present invention has been completed.
- a first aspect of the present invention that solves the above problems is formed using a sputtering target that includes an oxide sintered body containing indium oxide and, if necessary, tin and containing barium.
- a transparent conductive film comprising indium oxide and, if necessary, tin and barium.
- the indium oxide-based transparent conductive film containing barium is excellent in transparency with low resistance, and an amorphous film can be etched with a weakly acidic etchant during film formation. It will be possible.
- a second aspect of the present invention is the transparent conductive film according to the first aspect, wherein the sputtering target is contained in an amount of 0.000001 mol or more and less than 0.10 mol with respect to 1 mol of noriumcainedium.
- the transparent conductive film is characterized by being formed by using.
- a transparent conductive film that is an amorphous film that is particularly low resistance and excellent in transparency and that can be etched with a weakly acidic etchant is obtained.
- a third aspect of the present invention is the transparent conductive film according to the first or second aspect, in which tin is contained in an amount of 0 to 0.3 mole relative to 1 mole of indium, using a sputtering target.
- the transparent conductive film is mainly composed of indium oxide and contains tin as necessary.
- the transparent conductive film of the first to third one embodiment, the resistivity is in 1. 0 X 10- 4 ⁇ 1. 0 X 10- 3 ⁇ cm A transparent conductive film is provided.
- a transparent conductive film having a predetermined resistivity is obtained.
- a fifth aspect of the present invention is the transparent conductive film according to any one of the first to fourth aspects, wherein the transparent conductive film is formed as an amorphous film.
- an amorphous film can be etched with a weak acid during film formation.
- a sixth aspect of the present invention is the transparent conductive film according to any one of the first to fifth aspects, wherein the transparent conductive film is formed as an amorphous film and then crystallized by annealing. It is in a transparent conductive film.
- a seventh aspect of the present invention is a transparent conductive film according to the sixth aspect, characterized in that crystallization by the annealing is performed at 100 to 400 ° C.
- the amorphous film is easily crystallized at 100 to 400 ° C.
- An eighth aspect of the present invention is the transparent conductive film according to the sixth or seventh aspect, wherein an average transmittance at a wavelength of 400 to 500 nm after being crystallized by the annealing is 85% or more.
- the transparent conductive film is characterized in that.
- a ninth aspect of the present invention is the transparent conductive film according to any one of the first to eighth aspects, wherein the molar ratio of tin to 1 mol of indium y force is the mol of barium to 1 mol of indium. It is equal to or greater than the value (— 2. 9 X 10 " 2 Ln (x) -6.7 X 10 _2 ) represented by the ratio X, (— 2. OX 10 _1 Ln (x) —4.6 X 10
- the optimum oxygen partial pressure which is the oxygen partial pressure at which the resistivity of the deposited amorphous film is the lowest, and the oxygen resistance at which the resistivity of the crystallized film after annealing is the lowest resistance. Since the partial pressure (or the optimum oxygen partial pressure when deposited at the annealing temperature) is different, an amorphous film is formed at an oxygen partial pressure that has a low resistance after annealing, and then annealed to reduce the resistance. A highly transparent film can be obtained. This also improves the corrosion resistance, moisture resistance, and environmental resistance in the subsequent process.
- the amorphous film is an IJ film that has a particularly high etching rate.
- An eleventh aspect of the present invention is represented by a molar ratio of tin to 1 mol of indium, y force, and a molar ratio of barium to 1 mol of indium, in the transparent conductive film according to the tenth aspect. It is a transparent conductive film characterized by being in a range equal to or less than the value of (5.9 ⁇ 10 ′′ 2 Ln (x) + 4.9 ⁇ 10 — 1 ).
- the amorphous film is an IJ film that has a high patterning etching rate.
- a twelfth aspect of the present invention is the transparent conductive film according to the eleventh aspect, wherein the molar ratio y of tin to 1 mol of indium is 0.08 or more, and The transparent conductive film is characterized in that the molar ratio X is in the range of 0.025 or less.
- the resistivity after annealing is very low, and the resistivity is 3.0 x 10 ".
- a film having a low resistance of 4 ⁇ cm or less can be obtained.
- a film is formed using a sputtering target comprising indium oxide and, if necessary, an oxide-sintered body containing tin and also containing tin,
- the present invention provides a method for producing a transparent conductive film, characterized in that an amorphous transparent conductive film containing indium oxide and, if necessary, tin and barium is obtained.
- an indium oxide-based transparent film containing barium is formed by using an oxide sintered body containing indium oxide and, if necessary, tin and containing barium.
- a conductive film With a conductive film, it is possible to obtain a film which is excellent in transparency and can be etched with a weakly acidic etchant with an amorphous film during film formation.
- the amorphous conductive film is formed into a transparent conductive film that is crystallized by annealing.
- a method for manufacturing a transparent conductive film is a fourteenth aspect of the present invention.
- the fourteenth aspect after being formed as an amorphous film, it can be relatively easily crystallized by annealing.
- the amorphous film is etched with a weakly acidic etchant and then annealed to form a crystal.
- the present invention provides a method for producing a transparent conductive film.
- the film can be formed as an amorphous film, etched with a weakly acidic etchant, annealed, and crystallized to provide weak acid resistance.
- the crystallization by the annealing is performed at 100 to 400 ° C. It exists in the manufacturing method of a transparent conductive film.
- the amorphous film can be easily crystallized at 100 to 400 ° C.
- an average wavelength of 400 to 500 nm after crystallization by the annealing is characterized in that the transmittance is 85% or more.
- the transmittance on the short wavelength side is improved, and a film having a predetermined average transmittance and excellent transparency can be obtained.
- eighteenth aspect of the present invention is the manufacturing method of the transparent conductive film of any of the aspects of the 14 to 17, the resistivity of the transparent conductive film 1. 0 X 10- 4 ⁇ 1. in 0 X 10- 3 ⁇ «method for producing a transparent conductive film, wherein the Dearuko eta.
- a transparent conductive film having a predetermined resistivity can be obtained.
- a nineteenth aspect of the present invention is the method for producing a transparent conductive film according to any one of the thirteenth to eighteenth aspects, wherein the molar ratio of tin to 1 mol of indium is y force to 1 mol of indium. It is not less than the value of (— 2. 9 X 10 " 2 Ln (x) -6. 7 X 10 _2 ) expressed by the molar ratio X of barium, (— 2. 0 X 10 _1 Ln (x) -4.
- the twentieth aspect is advantageous for a pattern in which the etching rate of the amorphous film is particularly high.
- the molar ratio of tin to 1 mol of indium y force The molar ratio of barium to 1 mol of indium X
- the twenty-first aspect is more advantageous for patterning in which the etching rate of the amorphous film is further increased.
- the molar ratio y of tin to 1 mol of indium is 0.08 or more, and 1 mol of indium And forming a film using a sputtering target having a barium molar ratio X to 0.025 or less.
- the resistivity after annealing is very low, 3.0 x 10 "
- a film having a low resistance of 4 ⁇ cm or less can be obtained.
- the relational power between the oxygen partial pressure during film formation and the resistivity after annealing is characterized in that an oxygen partial pressure that provides a low resistance is obtained and a film is formed at the oxygen partial pressure.
- a low-resistance transparent conductive film is formed by forming an amorphous film by forming an oxygen partial pressure that gives the lowest resistance after annealing, and then crystallizing the film by annealing. Obtainable.
- the invention's effect [0054]
- the amorphous film can be easily patterned by weak acid etching, and further has low resistance, high transmittance, and crystallized more easily.
- the transparent conductive film can be made into an effect.
- FIG. 1 is a graph showing the relationship between oxygen partial pressure and specific resistance in Examples 1 and 2 and Comparative Examples 1 and 2 of the present invention.
- FIG. 2 shows a thin film XRD pattern before and after annealing in Example 1 of the present invention.
- FIG. 3 shows a thin film XRD pattern before and after annealing in Example 2 of the present invention.
- FIG. 4 is a view showing a thin film XRD pattern before and after annealing in Comparative Example 1 of the present invention.
- FIG. 5 shows a thin film XRD pattern before and after annealing in Comparative Example 2 of the present invention.
- FIG. 6 shows transmission spectra before and after annealing in Example 1 of the present invention.
- FIG. 7 shows transmission spectra before and after annealing in Example 2 of the present invention.
- FIG. 8 shows transmission spectra before and after annealing in Comparative Example 1 of the present invention.
- FIG. 9 shows transmission spectra before and after annealing in Comparative Example 2 of the present invention.
- FIG. 10 shows the results of thin film XRD at various temperatures in the composition of Test Example A32 of the present invention.
- FIG. 11 shows the results of Test Example 5 of the present invention.
- FIG. 12 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A7 of the present invention.
- FIG. 13 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A9 of the present invention.
- FIG. 14 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A13 of the present invention.
- FIG. 15 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A20 of the present invention.
- FIG. 16 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A21 of the present invention.
- FIG. 17 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A22 of the present invention.
- FIG. 18 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A23 of the present invention.
- FIG. 19 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A31 of the present invention.
- FIG. 22 is a graph showing the relationship between oxygen partial pressure and resistivity when a film was formed at room temperature in Test Example A40 of the present invention.
- FIG. 26 is a graph showing the relationship between the oxygen partial pressure and the resistivity when the film was formed at room temperature in Test Example A59 of the present invention.
- FIG. 28 is a graph showing the relationship between the oxygen partial pressure and the resistivity when test examples A4, A6, and A35 of the present invention were formed at room temperature.
- FIG. 29 shows the results of Test Example 6 of the present invention.
- FIG. 30 shows the results of Test Example 5 and Test Example 6 of the present invention.
- FIG. 31 shows the results of Test Example 7 of the present invention.
- the sputtering target for transparent conductive film used for forming the indium oxide-based transparent conductive film of the present invention is mainly composed of indium oxide, contains tin as necessary, and contains norium. There is no particular limitation as long as it is an acid oxide sintered body and norium is present as the acid oxide, as a complex acid oxide, or as a solid solution.
- the content of norlium is in a range formed by using a sputtering target containing 0.0001 mol or more and less than 0.10 mol with respect to 1 mol of indium. If the amount is less than this, the effect of addition is not remarkable. If the amount is more than this, the resistance of the formed transparent conductive film tends to increase and the color tends to deteriorate. Note that the norlium content in the transparent conductive film formed by the above-described sputtering target is the same as the content in the used sputtering target.
- the content of tin is within a range in which a film is formed using a sputtering target containing 0 to 0.3 mol per mol of indium.
- a sputtering target containing 0.0001-0.3 moles per mole of indium.
- the carrier electron density and mobility of the sputtering target can be appropriately controlled to keep the conductivity within a good range.
- addition beyond this range is not preferable because the mobility of carrier electrons in the sputtering target is lowered and the conductivity is deteriorated.
- the content of tin in the transparent conductive film formed by the above-described sputtering target is the same content as the content in the used sputtering target.
- Such a sputtering target has a resistance value that can be sputtered by DC magnetron sputtering, it can be sputtered by a relatively inexpensive DC magnetron sputtering.
- a high-frequency magnetron sputtering apparatus is used. That's right.
- an indium oxide-based transparent conductive film having the same composition By using such a sputtering target for a transparent conductive film, an indium oxide-based transparent conductive film having the same composition can be formed.
- the composition analysis of such an indium oxide-based transparent conductive film may be conducted by ICP after dissolving the entire single film.
- the cross section of the corresponding part is cut out by FIB if necessary. It can also be specified using elemental analyzers (EDS, WDS, Auge analysis, etc.) attached to SEM, TEM, etc.
- the film formation is performed at room temperature or higher and lower than the crystallization temperature, although it varies depending on the content of norium.
- the film is formed in an amorphous state by performing under a temperature condition lower than 200 ° C., preferably lower than 150 ° C., and more preferably lower than 100 ° C.
- such a monolithic film has the advantage that it can be etched with a weakly acidic etchant.
- the etching is included in the patterning process and is for obtaining a predetermined pattern.
- the resistivity of the transparent conductive film obtained varies depending on the content of Roh helium, resistivity 1. a 0 X 10- 4 ⁇ 1. 0 X 10- 3 ⁇ cm.
- the crystallization temperature of the formed film varies depending on the content of barium contained, and the annealing force is increased at a temperature of 100 ° C to 400 ° C as the content increases.
- annealing refers to heating at a desired temperature for a certain period of time in air, atmosphere, or vacuum.
- the fixed time is generally a force of several minutes or several hours. In terms of industry, if the effect is the same, a short time is preferred.
- the transparent conductive film after being crystallized by annealing in this way has improved transmittance on the short wavelength side, for example, the average transmittance at a wavelength of 400 to 500 nm is 85% or more. This also eliminates the problem of a yellowish film that is a problem with IZO. In general, the higher the transmittance on the short wavelength side, the better.
- the crystallized transparent conductive film has improved etching resistance and cannot be etched with a weakly acidic etchant that can be etched with an amorphous film. This improves the corrosion resistance in the subsequent process and the environmental resistance of the device itself.
- crystallization after film formation is achieved by changing the content of norlium. Since the temperature can be set to a desired temperature, after the film formation, the amorphous state may be maintained without being subjected to a heat treatment at a temperature higher than the crystallization temperature, or after the film formation, It may be possible to change the etching resistance by heat-treating at a temperature higher than the temperature at which it is converted.
- the optimum oxygen partial pressure varies depending on the temperature depending on the composition range of the sputtering target, and the temperature at which the resistance becomes low after finishing the process. It was found that an amorphous film was formed with an oxygen partial pressure, and then annealed and crystallized to form a low-resistance transparent conductive film.
- the molar ratio of tin to 1 mol of indium is represented by X (one 2.9 X 10 " 2 Ln (x) -6. 7 X 10 _2 ) or more, and if it is less than ( -2 .
- the etching rate is particularly high when it falls within the range of 0.22 or less.For example, use an etchant in which a solution having a 50 g ZL concentration of oxalic acid is heated to 30 ° C, which will be described in detail later.
- the molar ratio of tin, y force, and the molar ratio of barium to 1 mole of indium, X (5.9 x 10 " 2 Ln (x) +4 9 X 10 _1 ) or less in the range below the etching rate, and the etching rate when using an etchant in which a solution of 50 gZL of oxalic acid was heated to 30 ° C was used.
- the etching rate is 4AZsec or higher. In such an etching rate region, a good pattern can be obtained during patterning.
- the upper limit of the etching rate is Generally, it is about 30 AZsec!
- the starting material constituting the sputtering target of the present invention is generally In.
- a method of mixing and molding these raw material powders at a desired blending ratio is not particularly limited, and conventionally known various wet methods or dry methods can be used.
- Examples of the dry method include a cold press method and a hot press method.
- the cold press method mixed powder is filled into a mold to produce a molded body and fired.
- the hot press method the mixed powder is fired and sintered in a mold.
- a filtration molding method for example, it is preferable to use a filtration molding method (see JP-A-11-286002).
- This filtration-type forming method is a filtration-type mold that also has a water-insoluble material force for obtaining a compact by draining water from a ceramic raw material slurry under reduced pressure, and has a molding base having one or more drain holes. Clamped from the upper surface side through a mold, a water-permeable filter placed on the lower mold for molding, and a sealing material for sealing the filter The molding lower mold, the molding mold, the sealing material, and the filter are each assembled so that they can be disassembled, and the water in the slurry is drained under reduced pressure only by the force on one side of the filter.
- a filter-type mold Using a filter-type mold, prepare a slurry consisting of mixed powder, ion-exchanged water and organic additives, inject this slurry into the filter-type mold, and drain the water in the slurry under reduced pressure only from one side of the filter. A molded body is manufactured, and the obtained ceramic molded body is dried and degreased and then fired.
- the firing temperature of the one formed by the cold press method or the wet method is preferably 1300 to 1650 ° C, more preferably 1500 to 1650 ° C.
- the atmosphere is an air atmosphere, an oxygen atmosphere, or a non-oxidizing atmosphere. Sex atmosphere or vacuum atmosphere.
- a mechanical force for forming “calorie” is applied to predetermined dimensions to obtain a target.
- a total amount of 200 g was prepared at a ratio of 4 wt%, mixed in a dry state by a ball mill, and calcined at 1100 ° C for 3 hours in the air to obtain Bain O powder.
- BET 15m 2 Zg In O powder 84.7wt%
- a target was prepared in the same manner as in Production Example 1 except that Sn was equivalent to about 0.15 mol), and a film was formed in the same manner.
- the density of this target 6.
- a 74GZcm 3, Balta resistivity 2. was 92 X 10- 3 ⁇ cm.
- a target was prepared in the same manner as in Production Example 1 except that Sn was equivalent to about 0.10 mol), and a film was formed in the same manner.
- the density of this target was 6. 81gZcm 3, bulk resistivity was 5. 62 X 10- 4 ⁇ cm.
- the sputtering target of each manufacturing example was mounted on a 4-inch DC magnetron sputtering system, and the substrate temperature was 100 ° C and the oxygen partial pressure was changed from 0 to 2. Osccm in increments of 0.5 sccm (0 to 6 . corresponds to 46 X 10- 5 Torr), depositing a barium-containing indium oxide film (ITO-BaO) and IZO film, to obtain a transparent conductive film of example 2 and Comparative example 1, 2.
- ITO-BaO indium oxide film
- IZO film a transparent conductive film of example 2 and Comparative example 1, 2.
- the sputtering conditions were as follows, and a film with a thickness of 1200 A was obtained.
- T 6mm Sputtering method: DC magnetron sputtering
- Sputtering power 130W (Power density 1.6 WZcm 2 )
- Example 2 and Comparative Examples 1 and 2 transparent conductive films produced at the optimum oxygen partial pressure in film formation at 100 ° C were cut into 13 mm square sizes, and these samples were 300 in the atmosphere. Annealed at ° C for 1 hour.
- Figures 2 to 5 show the thin film XRD patterns before and after annealing.
- Example 2 the transparent conductive film produced at the optimum oxygen partial pressure in film formation at 100 ° C. was cut out to a size of 13 mm square, and the transmission spectrum was measured. The transmission spectrum of the film after annealing in Test Example 1 was measured in the same manner. These results are shown in Figs. Table 1 shows the average transmittance of each sample.
- Example 2 and Comparative Examples 1 and 2 the transparent conductive films produced at the optimum oxygen partial pressure in film formation at 100 ° C. were cut out to a size of 10 ⁇ 50 mm, and ITO-05N (oxalic acid) was used as the etching solution.
- ITO-05N oxalic acid
- System manufactured by Kanto Chemical Co., Ltd. (oxalic acid concentration: 50 gZL), it was confirmed whether or not etching was possible at a temperature of 30 ° C.
- the sample after the annealing in Test Example 1 was confirmed in the same manner.
- Examples 1 and 2 were amorphous, they were crystallized after force annealing, which can be etched with a weakly acidic etchant, and it was found that etching cannot be performed. Further, in the case of Comparative Example 1 and Comparative Example 2 of IZO, it was confirmed that both can be etched because they are amorphous films before and after annealing.
- a total amount of 200 g was prepared at a ratio of 4 wt%, mixed in a dry state by a ball mill, and calcined at 1100 ° C for 3 hours in the air to obtain Bain O powder.
- SnO powder corresponds to the moles of Ba and Sn in Table 2 and Table 3 below with respect to Inl mole.
- a total amount of about 1. Okg was prepared in such a ratio and mixed with a ball mill. Thereafter, an aqueous PVA solution was added as a binder, mixed, dried, and cold pressed to obtain a molded body.
- This molded body was degreased at 600 ° C. in the atmosphere for 10 hours and at a temperature of 60 ° C. Zh, and then fired at 1600 ° C. for 8 hours in an oxygen atmosphere to obtain a sintered body.
- the firing conditions are specifically from room temperature to 800. C up to 100. Heated up with CZh, 800. C force is also 1600. C up to 400. The temperature is raised at CZh, held for 8 hours, and then cooled from 1600 ° C to room temperature at 100 ° CZh.
- this sintered body was processed to obtain a target. Density and Balta resistivity at this time, the composition of the A32 For example, each 6. 88gZcm 3, a 2. 81 X 10 _4 Q cm, a Ito ⁇ configuration of A22, respectively 6. 96gZcm 3, 2. 87 X 10 _4 Q cm.
- Sputtering targets A1 to A60 of each production example were mounted on a 4-inch DC magnetron sputtering system, and the substrate temperature was changed to room temperature (about 20 ° C) and the oxygen partial pressure was changed between 0 and 3. Osccm ( 0 to: equivalent to L 1 X 10 _2 Pa), and transparent conductive films of Test Examples A1 to A60 were obtained.
- the sputtering conditions were as follows, and a film with a thickness of 1200 A was obtained.
- Substrate temperature room temperature
- Sputtering power 130W (Power density 1.6 WZcm 2 )
- the resistivity during film formation refers to the resistivity of the film at the optimum oxygen partial pressure during film formation at room temperature (see Test Example 5).
- Etching rate refers to the etching rate of an amorphous film deposited at room temperature when it is etched at an ITO-05N (oxalic acid concentration of 50 gZL) solution temperature of 30 ° C (see Test Example 6).
- the post-anneal resistivity refers to the resistivity of the film when the film is annealed at 250 ° C and then annealed at the lowest oxygen partial pressure after annealing at 250 ° C (see Test Example 5).
- the average transmittance after annealing is the average of the film wavelength of 400 to 500 nm when 250 ° C annealing is performed at 250 ° C annealing and film formation is performed at the lowest oxygen partial pressure.
- the transmittance is shown.
- the crystallization temperatures shown in Table 2 and Table 3 were determined as follows. A film deposited at room temperature with an oxygen partial pressure that gives the lowest resistance after annealing at 250 ° C, from 100 ° C to 300 ° C (450 ° C if necessary) in 50 ° C increments in air for 1 hour Annealing was performed and the membrane was analyzed by thin HXRD. At the halo peak indicating an amorphous film formed at room temperature, the diffraction temperature is detected by the annealing temperature increasing. The first temperature was determined as the crystallization temperature. As an example, Fig. 10 shows the results of thin film XRD at various temperatures in the composition of A32. Figure 10 shows that the lower force is also 100. C, 150. C, 200. C, 250. C, 300. This represents the thin HXRD of C. In this case, the crystallization temperature is 200 ° C. As another method for determining the crystallization temperature, the high temperature thin HXRD method can also be used.
- the optimum oxygen partial pressure is obtained by determining the relationship between the oxygen partial pressure at room temperature (about 20 ° C) and the resistivity of the film formed at that partial pressure. Both In addition, the relationship between the resistivity after annealing the film deposited at each oxygen partial pressure at 250 ° C. and the partial pressure of the deposited oxygen shows that the oxygen partial pressure at which the resistivity after annealing is the lowest is 250. The optimum oxygen partial pressure for film formation at ° C was determined, and it was determined whether or not the optimum oxygen partial pressure was different between the two. .
- the oxygen partial pressure at which the film has low resistance is different from the oxygen partial pressure at which the film after annealing has low resistance, or the optimal oxygen partial pressure at 250 ° C is different from the optimal oxygen partial pressure at room temperature.
- the crystallized film after annealing was deposited at an oxygen partial pressure at which the resistance becomes the lowest, not at the optimum oxygen partial pressure obtained from the resistivity immediately after film formation. This is more preferable because the resistivity of the film after annealing becomes lower.
- FIGS. 12 to 27 show graphs showing the relationship between oxygen partial pressure and resistivity during film formation at room temperature.
- ⁇ indicates the resistivity of the film immediately after deposition
- ⁇ indicates the resistivity after annealing at 250 ° C. It can be seen that for most samples it is preferable to deposit at a low oxygen partial pressure where the oxygen partial pressure at which the film after annealing at 250 ° C is low resistance is lower than that at room temperature. ⁇ A60! / After the annealing at 250 ° C, the film has a low resistance, and the oxygen partial pressure is higher than that at room temperature. It can be seen that a film is obtained and preferable.
- the crystallization temperature for example In the case of annealing at 400 ° C., it goes without saying that the film is preferably formed at an oxygen partial pressure at which the resistivity after annealing is lowest. Considering this case, the molar ratio X of norium is preferably less than 0.05.
- the molar ratio of tin to 1 mole of indium y force is represented by the molar ratio of barium to 1 mole of indium X (— 2. 9 X 10 " 2 Ln (x) -6 7 AX 10 _2 ) or more and 0.2 AZ or less, it is 3 AZsec or more, and in particular, (5.9 X 10 " 2 Ln (x) +4.9 X 10" 1 ) In the range below the value, it was obvious that it would be 4 AZsec or more.
- the result combined with the result of Test Example 5 is shown in FIG.
- the optimum partial pressure of oxygen at room temperature and the annealing temperature of 250 ° C is different, and the etching rate is 3 A / sec or more.
- the etching rate was over 4 A / sec.
- the resistivity of the film formed at room temperature at an annealing temperature for example, an optimum oxygen partial pressure of 250 ° C, and then annealed and crystallized is 3.0X. It is clear that it is less than 10 _4 ⁇ « ⁇ .
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Abstract
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US11/886,071 US7754110B2 (en) | 2006-03-31 | 2007-04-02 | Indium-oxide-based transparent conductive film and method for producing the film |
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KR20090127357A (ko) * | 2007-03-30 | 2009-12-10 | 미츠이 긴조쿠 고교 가부시키가이샤 | 산화인듐계 투명 도전막의 제조 방법 |
WO2009044897A1 (ja) * | 2007-10-03 | 2009-04-09 | Mitsui Mining & Smelting Co., Ltd. | 酸化インジウム系透明導電膜及びその製造方法 |
JPWO2009044898A1 (ja) * | 2007-10-03 | 2011-02-17 | 三井金属鉱業株式会社 | 酸化インジウム系透明導電膜及びその製造方法 |
WO2010116980A1 (ja) * | 2009-04-08 | 2010-10-14 | 三井金属鉱業株式会社 | 配線基板及び接続構造 |
EP2428500B1 (en) | 2009-10-06 | 2018-02-28 | JX Nippon Mining & Metals Corporation | Indium oxide sintered body, indium oxide transparent conductive film, and method for manufacturing the transparent conductive film |
JP5562000B2 (ja) * | 2009-10-28 | 2014-07-30 | Jx日鉱日石金属株式会社 | 酸化物焼結体及びその製造方法 |
CN104871258B (zh) * | 2012-12-19 | 2017-05-17 | 株式会社钟化 | 带透明电极的基板及其制造方法 |
JP6288347B2 (ja) * | 2016-04-22 | 2018-03-07 | 旭硝子株式会社 | ディスプレイ用ガラス基板 |
WO2018047977A1 (ja) * | 2016-09-12 | 2018-03-15 | 株式会社アルバック | 透明導電膜付き基板の製造方法、透明導電膜付き基板の製造装置、及び透明導電膜付き基板 |
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JPH06290641A (ja) * | 1993-03-30 | 1994-10-18 | Asahi Glass Co Ltd | 非晶質透明導電膜 |
JPH08188465A (ja) * | 1995-01-10 | 1996-07-23 | Tosoh Corp | 導電性セラミックス及びその製造方法 |
JP2004149883A (ja) * | 2002-10-31 | 2004-05-27 | Mitsui Mining & Smelting Co Ltd | 高抵抗透明導電膜用スパッタリングターゲット及び高抵抗透明導電膜の製造方法 |
JP2005135649A (ja) * | 2003-10-28 | 2005-05-26 | Mitsui Mining & Smelting Co Ltd | 酸化インジウム系透明導電膜及びその製造方法 |
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WO2006001469A2 (en) * | 2004-06-23 | 2006-01-05 | Sharp Kabushiki Kaisha | Organic electroluminescence device, image display apparatus and lighting apparatus including the same charge transport material |
JPWO2009044898A1 (ja) * | 2007-10-03 | 2011-02-17 | 三井金属鉱業株式会社 | 酸化インジウム系透明導電膜及びその製造方法 |
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Publication number | Priority date | Publication date | Assignee | Title |
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JPH06290641A (ja) * | 1993-03-30 | 1994-10-18 | Asahi Glass Co Ltd | 非晶質透明導電膜 |
JPH08188465A (ja) * | 1995-01-10 | 1996-07-23 | Tosoh Corp | 導電性セラミックス及びその製造方法 |
JP2004149883A (ja) * | 2002-10-31 | 2004-05-27 | Mitsui Mining & Smelting Co Ltd | 高抵抗透明導電膜用スパッタリングターゲット及び高抵抗透明導電膜の製造方法 |
JP2005135649A (ja) * | 2003-10-28 | 2005-05-26 | Mitsui Mining & Smelting Co Ltd | 酸化インジウム系透明導電膜及びその製造方法 |
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