WO2010058533A1 - OXYDE FRITTÉ À BASE DE ZnO-SnO2-In2O3 ET FILM CONDUCTEUR TRANSPARENT AMORPHE - Google Patents

OXYDE FRITTÉ À BASE DE ZnO-SnO2-In2O3 ET FILM CONDUCTEUR TRANSPARENT AMORPHE Download PDF

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WO2010058533A1
WO2010058533A1 PCT/JP2009/005957 JP2009005957W WO2010058533A1 WO 2010058533 A1 WO2010058533 A1 WO 2010058533A1 JP 2009005957 W JP2009005957 W JP 2009005957W WO 2010058533 A1 WO2010058533 A1 WO 2010058533A1
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sintered body
oxide
oxide sintered
tin
zinc
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PCT/JP2009/005957
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Japanese (ja)
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宇都野太
井上一吉
後藤健治
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出光興産株式会社
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Priority to CN200980146255.6A priority Critical patent/CN102216237B/zh
Priority to JP2010539126A priority patent/JPWO2010058533A1/ja
Priority to KR1020117011379A priority patent/KR101671543B1/ko
Publication of WO2010058533A1 publication Critical patent/WO2010058533A1/fr

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Definitions

  • the conventional transparent conductive film for example, in the case of an ITO film, indium which is a main component thereof is expensive, it cannot be manufactured at a low cost. Moreover, about the zinc oxide type transparent conductive film, the chemical resistance with respect to an acid, an alkali, etc. is low, and it was difficult to apply a zinc oxide type transparent conductive film to industrial products, such as a display element.
  • Patent Document 1 discloses a sputtering target composed of an In 2 O 3, ZnO and SnO 2.
  • This sputtering target discloses a transparent electrode material containing a hexagonal layered compound represented by In 2 O 3 (ZnO) m and having excellent etching characteristics.
  • Patent Document 1 proposes to precipitate an In 2 O 3 (ZnO) m phase for the purpose of reducing the bulk resistance, but the specific resistance of the In 2 O 3 (ZnO) m crystal is not so small. For this reason, the resistance of the sintered body may not decrease.
  • the manufacturing method disclosed in Patent Document 1 since the In 2 O 3 phase in which both Zn and Sn are dissolved cannot be precipitated in the target, the bulk resistance may not be sufficiently lowered.
  • the following method for producing an oxide sintered body and the like are provided. 1. (A) preparing a mixture by mixing raw material compound powders containing Zn, Sn and In; (B) forming the mixture to prepare a molded body; (C) a step of sintering the molded body at 1000 ° C. or higher and lower than 1300 ° C. for 0 hour or longer; and (d) a step of further sintering the sintered molded body at 1300 ° C. or higher and lower than 1500 ° C. for 2 hours or longer. And manufacturing method of oxide sintered body. The oxide sintered compact manufactured by the manufacturing method of 2.1. 3.
  • Relational expression (1) 0.01 ⁇ Zn / (Zn + Sn + In) ⁇ 0.15 0.80 ⁇ Sn / (Zn + Sn + In) ⁇ 0.98 0.01 ⁇ In / (Zn + Sn + In) ⁇ 0.15 6). 5.
  • the oxide sintered body according to 4, wherein the atomic ratio of zinc, tin and indium satisfies the following relational expression (2).
  • Relational expression (2) 0.01 ⁇ Zn / (Zn + Sn + In) ⁇ 0.68 0.30 ⁇ Sn / (Zn + Sn + In) ⁇ 0.50 0.01 ⁇ In / (Zn + Sn + In) ⁇ 0.50 7). 5.
  • the oxide sintered body according to 4 wherein the atomic ratio of zinc, tin and indium satisfies the following relational expression (3).
  • Relational expression (3) 0.50 ⁇ Zn / (Zn + Sn + In) ⁇ 0.80 0.10 ⁇ Sn / (Zn + Sn + In) ⁇ 0.49 0.01 ⁇ In / (Zn + Sn + In) ⁇ 0.40 8).
  • the oxide sintered body according to 3 containing a bixbite In 2 O 3 phase and a corundum In 2 O 3 phase.
  • the oxide sintered body according to 3 comprising a spinel Zn 2 SnO 4 phase and a corundum In 2 O 3 phase. 10.
  • the purity of each raw material compound powder is usually 99.9% by mass (3N) or more, preferably 99.99% by mass (4N) or more, more preferably 99.995% by mass or more, particularly preferably 99.999% by mass ( 5N) or more. If the purity of each raw material is 99.9% by mass (3N) or more, the semiconductor characteristics are not deteriorated by impurities such as Fe, Ni, Cu, and the reliability can be sufficiently maintained. In particular, when the content of Na in the raw material compound powder is less than 100 ppm, reliability can be improved when an amorphous transparent conductive film obtained from the manufactured oxide sintered body is used as a thin film transistor.
  • the average particle diameter of the raw material compound powder is preferably 0.1 ⁇ m or more and 20 ⁇ m or less from the viewpoints of powder handling and moldability.
  • the average particle diameter of the raw material oxide powder is more than 20 ⁇ m, the sinterability may be reduced, and a dense sintered body may not be obtained.
  • the average particle diameter of the raw material compound powder mixture obtained by the above mixing is preferably 0.1 to 1.0 ⁇ m. If the average particle size is less than 0.1 ⁇ m, the powder tends to aggregate, handling is poor, and a dense sintered body may not be obtained. On the other hand, if the average particle diameter exceeds 1.0 ⁇ m, a dense sintered body may not be obtained.
  • the oxide sintered body of the present invention contains zinc, tin, and indium, and includes an indium oxide phase in which zinc and tin are dissolved.
  • the oxide sintered body includes an indium oxide phase in which zinc and tin are dissolved, bulk resistance can be reduced.
  • In / (Zn + Sn + In) When In / (Zn + Sn + In) is more than 0.50, the manufacturing cost may increase. On the other hand, if In / (Zn + Sn + In) is less than 0.01, the effect of reducing the bulk resistance of the sintered body obtained by the indium oxide phase may not be exhibited. When Sn / (Zn + Sn + In) is less than 0.10, unreacted zinc oxide tends to remain in the sintered body, and thus zinc may be scattered during sintering. It is preferable that Zn / (Zn + Sn + In) is 0.80 or less because there is an effect of stabilizing the amorphous state of the obtained thin film.
  • Group 3 elements excluding actinides include Sc, Y and lanthanoids (La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu). From the viewpoint of relatively low cost and high chemical resistance, Y, La, Ce, Yb and Gd are preferred.
  • the oxide sintered body of the present invention can be used as a sputtering target by performing processing such as polishing.
  • the sintered body is ground by, for example, a surface grinder so that the surface roughness Ra is 5 ⁇ m or less.
  • the sputter surface of the target may be mirror-finished so that the average surface roughness Ra is 1000 angstroms or less.
  • a known polishing technique such as mechanical polishing, chemical polishing, mechanochemical polishing (a combination of mechanical polishing and chemical polishing) can be used.
  • the atomic ratio of Zn, Sn, and In preferably satisfies the following formula. 0.26 ⁇ Zn / (Zn + Sn + In) ⁇ 0.70 0.05 ⁇ Sn / (Zn + Sn + In) ⁇ 0.49 0.01 ⁇ In / (Zn + Sn + In) ⁇ 0.25 In particular, it is preferable to satisfy the following formula. 0.30 ⁇ Zn / (Zn + Sn + In) ⁇ 0.49 0.20 ⁇ Sn / (Zn + Sn + In) ⁇ 0.49 0.10 ⁇ In / (Zn + Sn + In) ⁇ 0.25
  • the amorphous transparent conductive film of the present invention can be formed by sputtering a sputtering target comprising the oxide sintered body of the present invention. Since the oxide sintered body of the present invention has high conductivity, a DC sputtering method having a high film formation rate can be applied when a sputtering target is used. In addition to the DC sputtering method described above, any sputtering method such as a magnetron sputtering method, an RF sputtering method, an AC sputtering method, a pulsed DC sputtering method, or an opposed sputtering method can be applied to the sputtering target comprising the oxide sintered body of the present invention. Sputtering without abnormal discharge is possible.
  • the concentration of the oxidizing gas may be appropriately adjusted depending on the desired film conductivity, light transmittance, and the like. This adjustment can be performed by, for example, the substrate temperature, the sputtering pressure, or the like.
  • the O 2 concentration is preferably 0.2 to 50% by volume.
  • the resulting film may be colored yellow and the resistance of the film may be increased.
  • the O 2 concentration is more than 50% by volume, the deposition cost of the thin film at the time of sputtering becomes slow, which may increase the production cost.
  • the O 2 concentration is 10% by volume or more and the obtained film has a carrier concentration of 10 15 to 10 18 cm ⁇ 3 by heat treatment, it can be used as a semiconductor.
  • the pressure in the sputtering apparatus (the pressure in the chamber) is preferably 10 ⁇ 6 to 10 ⁇ 3 Pa.
  • the pressure in the chamber exceeds 10 ⁇ 3 Pa, it is affected by residual moisture remaining in the vacuum, so that resistance control may be difficult.
  • the pressure in the chamber is less than 10 ⁇ 6 Pa, it takes time for evacuation, which may deteriorate productivity.
  • Examples of the substrate on which the amorphous transparent conductive film of the present invention is formed include glass, ceramics, plastics, and metals.
  • the substrate temperature during film formation is not particularly limited, but is preferably 300 ° C. or less from the viewpoint of easily obtaining an amorphous film.
  • the substrate temperature may be about room temperature when no intentional heating is performed. Also,
  • oxygen introduced during sputtering is not fixed in the film, and thus the substrate is preferably post-heated (heat treatment).
  • This heat treatment is preferably carried out at 150 to 350 ° C., preferably 200 to 300 ° C. in the air, nitrogen or vacuum.
  • heat treatment is less than 150 ° C., oxygen in the thin film is gradually discharged and the conductive film may be deteriorated.
  • the heat treatment exceeds 350 ° C., the resistance of the conductive film may increase.
  • the geometric film thickness (hereinafter simply referred to as film thickness) of the amorphous transparent conductive film of the present invention is preferably 2 nm to 5 ⁇ m, more preferably 2 nm to 300 nm.
  • film thickness of the amorphous transparent conductive film is more than 5 ⁇ m, the film formation time becomes long and the cost may increase.
  • the film thickness of the amorphous transparent conductive film is less than 2 nm, the specific resistance of the amorphous transparent conductive film may be increased.
  • composition of the amorphous transparent conductive film of the present invention generally matches the composition of the sputtering target used.
  • the amorphous transparent conductive film of the present invention obtained using the sputtering target comprising the oxide sintered body of the present invention has a specific resistance of 5000 ⁇ cm or less and a visible light region transmittance of 78% or more. it can.
  • the specific resistance of the amorphous transparent conductive film can be controlled by the In 2 O 3 content.
  • PVA polyvinyl alcohol
  • the prepared compact is desolvated at 400 ° C., and air is introduced at a flow rate of 500 ml / min, and the first stage sintering is performed at a sintering temperature of 1100 ° C., atmospheric pressure, holding time of 2 hours, and then further increased.
  • the second stage of sintering was performed at a sintering temperature of 1300 ° C., atmospheric pressure, and holding time of 10 hours to produce a sintered body.
  • the bulk resistance of the obtained sintered body was evaluated. The results are shown in Table 1.
  • the bulk resistance was measured by a 4-terminal method by cutting a 3 ⁇ 3 ⁇ 30 mm prism sample.
  • XRD X-ray diffraction measurement
  • the obtained thin film was subjected to X-ray diffraction measurement as in the case of the sintered body, the obtained X-ray diffraction pattern was flat, and it was confirmed that the obtained thin film was amorphous.
  • the composition of the thin film was measured by ICP emission analysis, it was confirmed that it was the same as the composition of the target used. Further, the specific resistance and transmittance (wavelength 550 nm) of the obtained thin film were evaluated. The results are shown in Table 2.
  • Examples 2 to 20 and Comparative Examples 1 to 5 The raw material oxide powder shown in Table 1 was used, and the production conditions of the sintered body (sintering temperature and holding time of the first stage sintering and the second stage sintering) were performed under the conditions shown in Table 1. A sintered body was produced and evaluated in the same manner as in Example 1, and a thin film was formed and evaluated. The evaluation results of the sintered body are shown in Table 1, and the evaluation results of the thin film are shown in Table 2. In addition, although film formation was attempted using the targets of Comparative Examples 1 to 5, a thin film could not be formed because DC sputtering discharge could not be performed or discharge could not be maintained.
  • PVA polyvinyl alcohol
  • the bulk resistance was measured by a four-terminal method by cutting a 3 ⁇ 3 ⁇ 30 mm prism sample. The bulk resistance was 26.3 m ⁇ cm.
  • the composition of the sintered body was calculated from the weighed value of each raw material powder.
  • the average particle size of the dry powder was measured with a Microtrac particle size measuring device (manufactured by Nikkiso Co., Ltd.).
  • the obtained sintered body for a sputtering target was analyzed by X-ray diffraction.
  • Experimental example 1 The amorphous transparent conductive films formed in Examples 1 and 4 were each immersed in a 10% nitric acid solution for 5 minutes, and then the electrical characteristics (specific resistance) were evaluated again with Loresta (manufactured by Mitsubishi Yuka). There was no change in the electrical characteristics of the immersed amorphous transparent conductive films of Examples 1 and 4.
  • Experimental example 2 The amorphous transparent conductive films formed in Examples 7 and 10 were each immersed in a PAN nitric acid solution (aluminum etching solution, manufactured by Kanto Chemical Co., Inc.) for 5 minutes, and the film thickness and electrical characteristics (resistivity) were again measured. evaluated. There was no change in the film thickness and electrical characteristics of the amorphous transparent conductive films of Examples 7 and 10 immersed.
  • the amorphous transparent conductive films formed in Examples 7 and 10 were each immersed in an oxalic acid aqueous solution for 1.5 minutes, and then the film thickness was evaluated. There was no change in the film thickness of the amorphous transparent conductive films of Examples 7 and 10 immersed.
  • Experimental example 3 An oxide semiconductor thin film having a thickness of 50 nm was formed on the thermal oxide film of a hard-doped Si substrate with a 300 nm-thick thermal oxide film using the oxide sintered body produced in Example 16, and a gold electrode was formed. A semiconductor element having a channel length of 200 ⁇ m and a channel width of 500 ⁇ m was manufactured. The manufactured semiconductor element was evaluated for TFT characteristics using a semiconductor characteristic evaluation apparatus 4200-SCS (manufactured by Keithley Instruments Co., Ltd.). As a result, it was confirmed that the manufactured semiconductor element had good TFT characteristics.
  • Experimental Example 4 A semiconductor element was produced and evaluated in the same manner as in Experimental Example 3 except that the oxide sintered body produced in Example 17 was used instead of the oxide sintered body produced in Example 16. As a result, it was confirmed that the manufactured semiconductor element had good TFT characteristics.
  • Example 5 A semiconductor element was produced using the sputtering target made of the oxide sintered body produced in Example 21. On the thermal oxide film of a hard-doped Si substrate with a 100 nm thick thermal oxide film, an oxide semiconductor thin film having a thickness of 50 nm is formed using the target prepared in Example 21, and the channel length having a gold electrode: A semiconductor element having a thickness of 200 ⁇ m and a channel width of 500 ⁇ m was produced. About the produced semiconductor element, when the TFT characteristic was evaluated using the semiconductor characteristic evaluation apparatus, it confirmed that it had a favorable TFT characteristic.
  • Example 6 The sputtering target made of the oxide sintered body produced in Example 21 was used. A thin film transistor was manufactured. After forming a transparent conductive film made of 100 nm of Mo on a glass substrate, a gate electrode was formed by photolithography. A gate insulating film was formed by laminating 200 nm of SiO 2 by PECVD. An oxide film was formed over the gate insulating film using the sputtering target of Example 21, a semiconductor layer with a thickness of 25 nm was formed by photolithography, and heat treatment was performed at 250 ° C. for 1 hour. After forming the SiO 2 protective film as an etching stopper layer, Ti / Al / Ti source / drain electrodes were formed. Heat treatment was performed at 300 ° C.
  • the amorphous transparent conductive film of the present invention is amorphous, it has no surface irregularities and is smooth, and can be suitably used as a transparent electrode for touch panels and flat panel displays.
  • the amorphous transparent conductive film of the present invention can provide a transparent film without heating the substrate, it is suitable for an antistatic film having a protective film function such as a plastic film or a touch panel produced on plastic. It can be suitably used as a transparent electrode film.
  • the substrate with an amorphous transparent conductive film of the present invention can be suitably used as a display element, a transparent surface heater, or an antistatic article.

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Abstract

L'invention concerne un procédé de production d'un oxyde fritté qui comprend les étapes (a) à (d) suivantes : (a) mélanger des poudres composites de matières premières qui contiennent respectivement Zn, Sn et In, de manière à préparer un mélange, (b) mouler le mélange de manière à préparer un produit moulé, (c) fritter le produit moulé à une température égale ou supérieure à 1 000°C et inférieure à 1 300°C pendant 0 heure ou plus longtemps et (d) poursuivre le frittage du produit moulé fritté à une température égale ou supérieure à 1 300°C et inférieure à 1 500°C pendant 2 heures ou plus longtemps.
PCT/JP2009/005957 2008-11-20 2009-11-09 OXYDE FRITTÉ À BASE DE ZnO-SnO2-In2O3 ET FILM CONDUCTEUR TRANSPARENT AMORPHE WO2010058533A1 (fr)

Priority Applications (3)

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CN200980146255.6A CN102216237B (zh) 2008-11-20 2009-11-09 ZnO-SnO2-In2O3类氧化物烧结体及非晶质透明导电膜
JP2010539126A JPWO2010058533A1 (ja) 2008-11-20 2009-11-09 ＺｎＯ−ＳｎＯ２−Ｉｎ２Ｏ３系酸化物焼結体及び非晶質透明導電膜
KR1020117011379A KR101671543B1 (ko) 2008-11-20 2009-11-09 ＺｎＯ-ＳｎＯ₂-Ｉｎ₂Ｏ₃계 산화물 소결체 및 비정질 투명 도전막

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WO2012108504A1 (fr) * 2011-02-10 2012-08-16 株式会社コベルコ科研 Corps fritté d'oxyde, et cible de pulvérisation cathodique
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WO2012153507A1 (fr) * 2011-05-10 2012-11-15 出光興産株式会社 CIBLE DE PULVÉRISATION CATHODIQUE D'In2O3-SnO2-ZnO
WO2012153522A1 (fr) * 2011-05-10 2012-11-15 出光興産株式会社 Cible de pulvérisation à in2o3-zno
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JP2015038027A (ja) 2015-02-26
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