WO2014025017A1 - Cible de pulvérisation pour former un film d'oxyde transparent et procédé pour produire celle-ci - Google Patents

Cible de pulvérisation pour former un film d'oxyde transparent et procédé pour produire celle-ci Download PDF

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WO2014025017A1
WO2014025017A1 PCT/JP2013/071670 JP2013071670W WO2014025017A1 WO 2014025017 A1 WO2014025017 A1 WO 2014025017A1 JP 2013071670 W JP2013071670 W JP 2013071670W WO 2014025017 A1 WO2014025017 A1 WO 2014025017A1
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powder
sputtering target
oxide film
forming
transparent oxide
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PCT/JP2013/071670
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English (en)
Japanese (ja)
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齋藤　淳
張　守斌
山口　剛
佑一 近藤
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三菱マテリアル株式会社
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Priority to KR1020157001661A priority Critical patent/KR101990663B1/ko
Priority to CN201380041837.4A priority patent/CN104540976B/zh
Publication of WO2014025017A1 publication Critical patent/WO2014025017A1/fr

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Definitions

  • the present invention is a light barrier protective film suitable for an optical disc, a touch panel element, a liquid crystal display element, an electroluminescence display element, an electrophoretic display element, a gas barrier layer used for electronic paper such as a toner display element, a solar cell, etc.
  • the present invention relates to a zinc oxide-based sputtering target for forming a transparent oxide film and a method for producing the same.
  • a light transmission protective film suitable for an optical disk and further as a gas barrier layer used for electronic paper such as a touch panel element, a liquid crystal display element, an electroluminescence display element, an electrophoretic display element, a toner display element, and a solar cell.
  • a technique for producing a zinc oxide-based transparent oxide film by a sputtering method is known.
  • Patent Document 1 contains tin oxide and at least one additive element selected from the group consisting of Si, Ge, and Al.
  • the additive element is based on the total content of the additive element and Sn.
  • the composition of the crystal phase includes at least one of a metal phase of the additive element, an oxide phase of the additive element, and a composite oxide phase of the additive element and Sn.
  • the transparent oxide film obtained by this method is a transparent oxide film containing tin oxide and at least one additional element selected from the group consisting of Si, Ge, and Al. It is included at a ratio of 15 atomic% to 63 atomic% with respect to the total of the additive element and Sn, is an amorphous film, and has a refractive index of 1.90 or less at a wavelength of 633 nm.
  • Patent Document 2 describes forming a light transmission film used as a protective film for a phase change optical disk.
  • the zinc oxide-based transparent oxide film contains more SiO 2 to lower the refractive index.
  • SiO 2 when SiO 2 is added to the sputtering target, since the SiO 2 itself is insulative, high-frequency (RF) sputtering must be employed for forming the oxide film.
  • RF radio frequency
  • this high-frequency sputtering has a low film formation rate, it is expected that high-productivity direct current (DC) sputtering will be adopted when forming an oxide film. Therefore, as described in Patent Document 2, it has been proposed to reduce the resistance of the target so that DC sputtering can be employed.
  • Al 2 O 3 or Ga 2 O 3 is contained in the sputtering target, but in order to achieve transparency close to the refractive index of glass, a large amount of SiO 2 is added. Must. On the contrary, the addition of a large amount of SiO 2 makes it difficult to employ DC sputtering.
  • mixing is performed by mixing and mixing an appropriate amount of ZnO powder, SiO 2 powder, and Al 2 O 3 powder or Ga 2 O 3 powder. It is necessary to obtain a sintered body obtained by firing the powder under predetermined firing conditions. At this time, depending on the firing method, ZnO and SiO 2 react with each other in the sintered body, and large particles of a composite oxide of Zn and Si (composition formula: Zn 2 SiO 4 ) are present. It is formed.
  • An object of the present invention is to provide a zinc oxide-based sputtering target for forming a transparent oxide film that hardly causes abnormal discharge during sputtering and a method for producing the same.
  • the inventors of the present invention used a zinc oxide-based sputtering target containing SiO 2 , Al 2 O 3 and / or Ga 2 O 3 to dc-sputter an A1 (and / or Ga) —Zn—Si—O film. Research was conducted to form a film.
  • a sintered powder is obtained by firing a mixed powder of ZnO powder, SiO 2 powder, Al 2 O 3 powder and / or Ga 2 O 3 powder.
  • composite oxide particles of Zn 2 Si 4 of Zn 2 SiO 4 having a large particle size are formed in the substrate of the sintered body.
  • the adjustment to the formation of the composite oxide particles is difficult even if various baking conditions are devised.
  • the inventors do not obtain a sintered body by firing a mixed powder of ZnO powder, SiO 2 powder, Al 2 O 3 powder or Ga 2 O 3 powder, but first, ZnO powder and After calcining the mixed powder of SiO 2 powder to obtain a calcined body in which a composite oxide of Zn and Si of Zn 2 SiO 4 is formed, this calcined body is made into a fine pulverized powder,
  • the pulverized powder is used as a raw material powder, and the composition of the A1 (and / or Ga) -Zn-Si-O film, which is a film-forming purpose, is composed of ZnO powder and Al 2 O 3 powder or Ga 2 O 3 powder. It is easy to adjust the presence of composite oxide particles of Zn and Si in the produced sputtering target by firing the mixed powder weighed and mixed so as to obtain a fired body. This complex acid of Zn and Si Things particles was also obtained knowledge that is finely formed.
  • the obtained mixed powder was dried, granulated, and fired in the atmosphere at 1200 ° C. for 5 hours to obtain a calcined powder.
  • This calcined powder is a complex oxide of Zn and Si of Zn 2 SiO 4 .
  • the calcined powder was pulverized and granulated.
  • the calcined powder is used as a raw material powder, each raw material powder of ZnO and Al 2 O 3 is weighed so as to have a predetermined ratio, and the weighed raw material powders are mixed.
  • the obtained mixed powder was fired in a nitrogen gas atmosphere at 1400 ° C. for 3 hours to obtain a sintered body.
  • the sintered body was machined into a predetermined shape to produce a sputtering target for forming a transparent oxide film.
  • the composition component in the manufactured sputtering target was analyzed. The analysis result is shown in FIG.
  • the photograph in FIG. 1 is an element distribution image obtained by EPMA (field emission electron probe) for the manufactured sputtering target. From the four photographs in the figure, Zn, Si, A1, and O The state of composition distribution of each element can be observed individually. Note that the element distribution image by EPMA is originally a color image, but in the photograph of FIG. 1, it is converted into a black and white image. Therefore, the whiter in the photograph, the higher the concentration of the element. ing. Specifically, in the distribution image related to Al, the Al element is distributed in white spots (relatively white portions), and in the distribution image related to Zn, the Zn element exists as a whole, and among them, the concentration is high.
  • EPMA field emission electron probe
  • the white parts to be observed are distributed, and in the distribution image relating to O, it is observed that the O element is present at a certain concentration as a whole.
  • the Si element is present at a certain concentration, but is not present in the portion where the Zn element concentration is high. From these, and ZnO, composite oxides of Si and Zn and (Zn 2 SiO 4), but is presumed to exist separately.
  • the graph of FIG. 2 has shown the analysis result by X-ray diffraction (XRD) of the sputtering target for transparent oxide film formation manufactured as mentioned above.
  • XRD X-ray diffraction
  • the upper graph in FIG. 2 shows the entire peak
  • the middle graph shows the peak related to Zn 2 SiO 4
  • the lower graph shows the peak related to ZnO. .
  • ZnO and / or AZO Al-doped ZnO
  • the composite oxide of Zn and Si are separated. It can be seen that there is no SiO 2 crystal phase. If SiO 2 is present alone and crystal phase is precipitated, a corresponding peak should appear in the XRD diffraction result. In the diffraction result graph of FIG. No peak appeared and no SiO 2 crystal phase was detected.
  • Si is present as a composite oxide of Zn and Si in the substrate of the fired body made of the Al—Zn—Si—O quaternary element, It was confirmed that no SiO 2 crystal phase was present. Therefore, when manufacturing a sputtering target for forming an A1 (and / or Ga) —Zn—Si—O transparent oxide film, a pre-fired Zn 2 SiO 4 composite oxide of Zn and Si is used.
  • the sputtering target for forming a transparent oxide film according to the present invention includes one or two of Al and Ga: 0.6 to 8.0 at%, Si: 0.0. 1 at% or more, and a total of 33.0 at% or less of Al, Ga and Si, and the balance is a fired body having a composition composed of Zn and inevitable impurities, and the fired body has a particle size of 5 ⁇ m or less.
  • the composite oxide of Zn and Si is present, the bending strength of the fired body is 90 MPa or more, the relative density of the fired body is 90% or more, The heat conductivity of the fired body is 7.5 W / m ⁇ k or more.
  • a method of manufacturing a transparent oxide film forming sputtering target of the present invention is a method for producing a transparent oxide film-forming sputtering target of (1), a ZnO powder and SiO 2 powder
  • the raw material powder blended and mixed at a molar ratio of 2: 1 is fired and then pulverized to obtain a composite oxide powder, and any one or two of the composite oxide powder, Al 2 O 3 powder and Ga 2 O 3 powder And a mixed powder obtained by mixing and mixing ZnO powder to obtain a fired body, and in the manufacturing method, the mixed powder is non-oxidized at a temperature of 1100 to 1450 ° C.
  • the manufacturing method of the sputtering target for forming the transparent oxide film includes ZnO powder having an average particle diameter of 0.1 to 3.0 ⁇ m, SiO 2 powder having an average particle diameter of 0.2 to 4.0 ⁇ m, and Al 2.
  • ZnO powder having an average particle diameter of 0.1 to 3.0 ⁇ m
  • SiO 2 powder having an average particle diameter of 0.2 to 4.0 ⁇ m
  • Al 2 aluminum 2.
  • One or two of O 3 powder and Ga 2 O 3 powder are blended and mixed, and the temperature is 1150 to 1300 ° C., the pressure is 100 to 400 kgf / cm 2 , and the non-oxidizing atmosphere is 1 to 10 hours. And is fired under pressure to obtain a fired body.
  • Si 0.1 at% or more: The content of Si in the sputtering target, with respect to the total metal component amount is less than 0.01 at%, since the effect of suppressing crystallization is small no effect of addition, whereas, if too great, SiO 2 Therefore, the Si content is preferably 0.1 at% or more and the total of Al and Ga is preferably 33 at% or less, which effectively suppresses crystallization. be able to.
  • Si + Al + Ga 33 at% or less: If the total content of Al, Ga and Si in the sputtering target exceeds 33 at%, the specific resistance of the sputtering target itself increases, abnormal discharge is likely to occur, and stable direct current sputtering becomes difficult. The total content of Al, Ga, and Si was 33 at% or less.
  • Particle size of complex oxide of Zn and Si The reason why the average particle size (D50) of the composite oxide of Zn and Si (Zn 2 SiO 4 ) present in the sputtering target is 5 ⁇ m or less is that when this particle size exceeds 5 ⁇ m, This is because abnormal discharge occurs frequently, and the occurrence of abnormal discharge was suppressed by setting the thickness to 5 ⁇ m or less.
  • the particle size of the composite oxide of Zn and Si is more preferably 4.5 ⁇ m or less, and most preferably 4.1 ⁇ m or less.
  • 5) Folding strength, relative density and thermal conductivity of the fired body The bending strength of the fired body was 90 MPa or more, the relative density of the fired body was 90% or more, and the thermal conductivity of the fired body was 7.5 W / m ⁇ k or more. The reason for this limitation is that the generation of target cracks can be suppressed.
  • the calcining conditions for obtaining this calcined body can be calcined in the air or in an oxygen atmosphere at a temperature of 1000 to 1500 ° C., preferably 1100 to 1200 ° C. for 2 to 9 hours. If the particle diameter of the Zn 2 SiO 4 powder is 30 ⁇ m or less, the average particle diameter (D50) of the mixed powder obtained by pulverizing and mixing this powder, the Al 2 O 3 powder, and the ZnO powder is 5 ⁇ m. It is easy to: If the particle size exceeds 30 ⁇ m, it takes too much time to ball mill and make the average particle size (D50) of the mixed powder 5 ⁇ m or less, which is not preferable.
  • the calcined powder obtained by pulverizing the calcined body that is, a fine Zn 2 SiO 4 powder is used as one raw material powder for obtaining a fired body, and ZnO powder, Al 2 O 3 powder and Ga 2 O are obtained. Any one or two raw material powders of the three powders are adjusted to a predetermined ratio so as to have a component composition of the A1 (or Ga) —Zn—Si—O quaternary oxide film for film formation. Weighing and mixing the weighed raw material powders to obtain a mixed powder.
  • this mixed powder is formed by cold isostatic pressing (CIP)
  • CIP cold isostatic pressing
  • an inert gas atmosphere such as nitrogen is applied at a temperature of 1200 to 1450 ° C., preferably at a temperature of 1350 to 1400 ° C. for 2 to 9 hours.
  • This baking may be performed by hot pressing (HP) or hot isostatic pressing (HIP).
  • HP hot pressing
  • HIP hot isostatic pressing
  • the mixed powder is heated to 1100 to 1450 ° C. in a non-oxidizing atmosphere (N 2 gas, Ar gas, vacuum), and 1 to 10
  • the fired body can be fired while maintaining time, and the fired body can be cooled at a cooling rate of 30 to 150 ° C./h.
  • the mixed powder is fired, if the firing holding time is too short and the cooling rate is too low, all of the bending strength, relative density, and thermal conductivity are lowered, and abnormal discharge occurs frequently.
  • the firing holding time is too long and the cooling rate is too high, target cracks occur, which is not preferable.
  • a ZnO powder having an average particle size of 0.1 to 3.0 ⁇ m, and an SiO 2 powder having an average particle size of 0.2 to 4.0 ⁇ m One or two of Al 2 O 3 powder and Ga 2 O 3 powder are blended and mixed, and 1 to 1 at a temperature of 1150 to 1300 ° C., a pressure of 100 to 400 kgf / cm 2 and a non-oxidizing atmosphere.
  • a fired body can be obtained by pressure firing while holding for 10 hours.
  • the manufacturing process of the calcined body is omitted. It is possible.
  • the mixed powder can be fired in a temperature of 1150 to 1300 ° C., 100 to 400 kgf / cm 2 , and a non-oxidizing atmosphere (N 2 gas, Ar gas, vacuum) for 1 to 10 hours.
  • the firing method for example, hot press or HIP can be used.
  • the average particle size of the ZnO powder and the SiO 2 powder is too small, handling during mixing becomes difficult. On the other hand, if it is too large, the particle size of the complex oxide of Zn and Si (Zn 2 SiO 4 ) during firing Is larger than 5 ⁇ m, and abnormal discharge occurs frequently.
  • the mixed powder is fired, if the firing holding time is too short and the cooling rate is too low, all of the bending strength, relative density, and thermal conductivity are lowered, and abnormal discharge occurs frequently.
  • the firing holding time is too long and the cooling rate is too high, target cracks occur, which is not preferable.
  • the manufacturing method of the sputtering target for transparent oxide film formation of this invention it is preferable to bake in the atmosphere whose oxygen content is less than air
  • the sputtering target for forming a transparent oxide film of the present invention can be used for the formation of a transparent oxide film having a low refractive index by direct current sputtering, and is suitable for a light transmission protective film, a touch panel element, and a liquid crystal display suitable for optical disks. It is suitable for use in forming a film such as a gas barrier layer used in electronic paper such as an element, an electroluminescence display element, an electrophoretic display element, and a toner display element, and a solar cell.
  • the sputtering target for forming a transparent oxide film of the present invention since a fine composite oxide of Zn and Si having a particle size (D50) of 5 ⁇ m or less is present in the fired body, direct current sputtering is used.
  • D50 particle size
  • the transparent oxide film-forming sputtering target advance to create a composite oxide of a previously tentatively calcined Zn 2 SiO 4 and Zn and Si as raw material powder, and the raw material powder, and ZnO powder , Al 2 O 3 powder and / or Ga 2 O 3 powder, mixed powder weighed to have a component composition of A1 (and / or Ga) —Zn—Si—O film for film formation
  • the procedure of firing it becomes easy to refine the composite oxide of Zn and Si of Zn 2 SiO 4 existing in the sputtering target, and the amount thereof can be easily adjusted. be able to.
  • a calcined body made of a composite oxide of Zn and Si obtained by firing a raw material powder of zinc oxide powder and silicon oxide powder.
  • the calcined body was prepared and pulverized to obtain a composite oxide powder of Zn and Si.
  • the obtained composite oxide powder of Zn and Si, zinc oxide powder, and mixed powder of one or two of aluminum oxide powder and gallium oxide powder are fired after molding to obtain a fired body. This was machined to produce a sputtering target. This production will be described in detail below.
  • the obtained mixed powder is dried, granulated, and fired in the atmosphere at 1200 ° C. for 5 hours to obtain a calcined body (complex oxide of Zn and Si: Zn 2 SiO 4 ).
  • This calcined body and a zirconia ball of 5 times the weight (weight ratio) are put in a plastic container and wet pulverized in a ball mill apparatus for 24 hours.
  • alcohol is used for the solvent in this case, for example.
  • Each of the weighed raw material powders and zirconia balls of 5 times the weight (weight ratio) are put in a plastic container and wet-mixed for 24 hours in a ball mill apparatus.
  • alcohol is used for the solvent in this case, for example.
  • the obtained mixed powder was dried, granulated, molded by cold isostatic pressing (CIP), and then fired in a nitrogen gas atmosphere at 1400 ° C. for 3 hours to obtain a fired body.
  • this baking can also be performed by hot pressing (HP) under a load of 200 kgf ⁇ cm ⁇ 2 at 1200 ° C. for 3 hours in a vacuum or an inert atmosphere.
  • the fired body was machined to obtain a sputtering target having a diameter of 125 mm and a thickness of 5 mm.
  • the sputtering targets of Examples 1 to 8 and Comparative Examples 1 to 4 shown in Table 1 were manufactured.
  • the calcined body in the case of the comparative example 4 was baked at the temperature of 950 degreeC.
  • a composite oxide powder of Zn and Si is used as a raw material powder, and a mixed powder containing this powder and other raw material powders is fired to obtain a fired body.
  • a composite oxide powder of Zn and Si is not obtained as a raw material powder by calcination of zinc oxide (ZnO) and silicon oxide (SiO 2 ).
  • the raw material powder of zinc oxide (ZnO) and silicon oxide (SiO 2 ) was mixed so as to have a predetermined ratio, and fired under the same conditions as described above to prepare a fired body.
  • Table 2 shows the metal compositions of the sputtering targets of Examples 1 to 13 and Comparative Examples 1 to 8.
  • XRD analysis> The XRD analysis was performed by the same method as the XRD analysis shown in FIG. The presence or absence of an XRD peak was confirmed by XRD analysis on the sputtering target. This XRD analysis was performed under the following conditions. Preparation of sample: The sample was wet-polished with SiC-Paper (grit 180) and dried, and then used as a measurement sample. Equipment: Rigaku Electric Co., Ltd.
  • EBSD analysis> The size of the composite oxide (Zn 2 SiO 4 ) particles of Zn and Si in the structure of the sputtering target was confirmed from the IQ map obtained by EBSD.
  • the IQ map measured the particle size quantitatively by observing a cross-sectional area of 95 ⁇ m ⁇ 33 ⁇ m.
  • EBSD collected the pattern using OIM Data Collection of TSL Solutions, Inc., and calculated the particle size using OIM Analysis 5.31 manufactured by the company.
  • the specific resistance of the sputtering target was measured using a resistance measuring instrument Loresta GP manufactured by Mitsubishi Chemical Corporation.
  • the number of abnormal discharges was measured by a film formation test according to the above film formation conditions. Based on the measurement results, the possibility of direct current (DC) sputtering of the sputtering targets of Examples 1 to 13 and Comparative Examples 1 to 8 was evaluated. The results of the measurement / evaluation are shown in Table 3.
  • a calcined body made of a complex oxide of Zn and Si (Zn 2 SiO 4 ), pulverized and fired after firing the powder, and the calcined body is ground to a composite oxide of Zn and Si (Zn 2 SiO 4 ) powder is obtained.
  • the obtained mixed powder of Zn 2 SiO 4 powder, ZnO powder, and one or two of aluminum oxide (Al 2 O 3 ) powder and gallium oxide (Ga 2 O 3 ) powder is fired after molding. By doing this, a fired body was obtained and machined to produce a sputtering target.
  • the method for producing the sputtering target for forming a transparent oxide film firing holding that affects the bending strength, thermal conductivity, and relative density of the fired body obtained by firing the above-mentioned mixed powder compact.
  • the time and the cooling rate after firing were adjusted as shown in Table 4, and the transparent oxide film forming sputtering targets of Examples 101 to 127 were produced.
  • Examples 101 to 109 when a mixed powder of Zn 2 SiO 4 powder: 50.0 mol%, Al 2 O 3 powder: 3.0 mol%, and ZnO powder: remainder is used, Examples 110 to 118 are used.
  • Examples 119 to 127 are Zn 2 SiO 4 powder: 22.0 mol%, Al 2 O 3 powder: 0.6 mol%, and a mixed powder of ZnO powder: remainder are shown representatively.
  • a plate having dimensions of width: 4 mm, length: 40 mm, thickness: 3 mm was cut out from the fired body obtained above to produce a bending test piece. Using this test piece, a three-point bending test was performed by the method specified in JIS R-1601 to determine the bending strength (MPa).
  • the sample obtained from the fired body obtained above was measured for thermal conductivity (W / m ⁇ k) by a laser flash method.
  • Analytical apparatus NETZSCH-Geratebau GmbH, Xe flash analyzer, sample size: 10 mm ⁇ 10 mm, thickness: 2 mm, measurement temperature: 25 ° C., standard comparison sample: SUS310, pulse width: 0.2 ms, charge level: 270 V Measurements were made. This measurement was performed three times on the same sample, and the average value of the measured values was obtained.
  • the relative density ratio (%) was calculated by machining the fired body to a predetermined size, measuring the weight, obtaining the bulk density, and dividing by the theoretical density ⁇ fn .
  • the theoretical density ⁇ fn was determined by the following formula based on the weight of the raw material. Since this formula shows a case where both Al 2 O 3 powder and Ga 2 O 3 powder are mixed, in the second embodiment, only Al 2 O 3 powder is mixed, so C4: Ga 2 It is determined that there is no term relating to O 3 .
  • XRD analysis, analysis by EPMA, and specific resistance measurement were performed on the sputtering targets of Examples 101 to 127 shown in Table 4.
  • XRD analysis, analysis by EPMA, and specific resistance measurement were performed under the same conditions as those for the sputtering target of the first example. The results are shown in Table 5.
  • a film formation test was performed under the same film formation conditions as in the first example. The number of abnormal discharges was measured by a film formation test according to the above film formation conditions. Based on the measurement results, the possibility of direct current (DC) sputtering of the sputtering targets of Examples 101 to 127 was evaluated. The results of the measurement / evaluation are shown in Table 5.
  • any of the sputtering targets of Examples 101 to 127 ZnO and Zn 2 SiO 4 were formed in the target structure in the XRD analysis and EPMA analysis described above. It can be confirmed that the Zn 2 SiO 4 particle size is 5 ⁇ m or less. Further, as a result of performing direct current sputtering using the sputtering targets of Examples 101 to 127, in all cases, the number of occurrences of abnormal discharge was small, and it was proved that direct current sputtering can be performed in any of the Examples. The generation of particles could not be confirmed.
  • a composite oxide of Zn and Si was calcined and ZnO powder and SiO 2 powder (Zn 2 SiO 4) as a raw material powder, Table Although the mixed powder having the raw material composition shown in FIG. 1 was fired, in the third example, the manufacturing process of the calcined body was omitted, and instead of using the Zn 2 SiO 4 powder, a considerable amount of ZnO powder and SiO 2 were used. Two powders were used as raw powders.
  • ZnO powder and SiO 2 powder having a particle diameter shown in Table 6. Further, the firing temperature and firing retention time affecting the bending strength, thermal conductivity and relative density of the fired body were adjusted as shown in Table 6, and the transparent oxides of Examples 201 to 227 were used. A sputtering target for film formation was produced. Examples 201 to 209 use a mixed powder of SiO 2 powder: 25.4 mol%, Al 2 O 3 powder: 1.6 mol%, and ZnO powder: the balance.
  • Examples 210 to 218 When using a mixed powder of SiO 2 powder: 30.6 mol%, Al 2 O 3 powder: 0.4 mol%, and ZnO powder: balance, Examples 219 to 227 are SiO 2 powder: 15 The case where a mixed powder of .3 mol%, Al 2 O 3 powder: 0.4 mol%, and ZnO powder: remainder is used is representatively shown.
  • any of the sputtering targets of Examples 201 to 227 ZnO and Zn 2 SiO 4 were formed in the target structure in the XRD analysis and EPMA analysis described above. It can be confirmed that the Zn 2 SiO 4 particle size is 5 ⁇ m or less. Furthermore, as a result of performing direct current sputtering using the sputtering targets of Examples 201 to 227, the number of occurrences of abnormal discharge was small in any case, and it was proved that direct current sputtering can be performed in any of the Examples. The generation of particles could not be confirmed.
  • a mixed powder of ZnO powder and SiO 2 powder is temporarily fired to obtain Zn and Si having a composition of Zn 2 SiO 4 .
  • a calcined body is obtained by forming a composite oxide, and the calcined body is made into a fine pulverized powder.
  • the pulverized powder is used as a raw material powder, ZnO powder, Al 2 O 3 powder, and Ga. Since a fired body is obtained by firing a mixed powder obtained by mixing one or two kinds of 2 O 3 powder, a fine complex oxide of Zn and Si (Zn 2) is contained in the fired body.
  • the sputtering target was able to reduce the specific resistance and enable direct current (DC) sputtering. Furthermore, since a sputtering target having appropriate bending strength, thermal conductivity and relative density can be obtained, occurrence of abnormal discharge can be reduced and target cracking can be suppressed.

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Abstract

La présente invention concerne une cible de pulvérisation pour former un film d'oxyde transparent à base d'oxyde de zinc, qui est capable de former un film d'oxyde transparent par pulvérisation en courant continu, tout en étant exempte de l'occurrence de décharge anormale. Cette cible de pulvérisation pour former un film d'oxyde transparent est caractérisée en ce qu'elle un corps cuit d'une composition qui contient 0,6 à 8,0 % atomique de Al et/ou Ga et 0,1 % atomique ou plus de Si de sorte que le total de Al, Ga et Si est 33,0 % atomique ou moins par rapport à la quantité totale de tous les éléments métalliques, le complément étant constitué de Zn et d'impuretés inévitables. Cette cible de pulvérisation pour former un film d'oxyde transparent est également caractérisée en ce que des particules d'oxyde complexe de Zn et Si, qui ont des diamètres de particule de 5 μm ou moins, sont présentes dans le corps cuit.
PCT/JP2013/071670 2012-08-10 2013-08-09 Cible de pulvérisation pour former un film d'oxyde transparent et procédé pour produire celle-ci WO2014025017A1 (fr)

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