KR102646917B1 - Molybdenum oxide based sintered body, metal oxide thin film using the sintered body, and thin film transistors and displa devices comprising the thin films - Google Patents
Molybdenum oxide based sintered body, metal oxide thin film using the sintered body, and thin film transistors and displa devices comprising the thin films Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 75
- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims abstract description 38
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 150000004706 metal oxides Chemical class 0.000 title claims description 57
- 229910044991 metal oxide Inorganic materials 0.000 title claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 25
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 229910052802 copper Inorganic materials 0.000 claims description 12
- 238000005477 sputtering target Methods 0.000 claims description 11
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 230000003287 optical effect Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 17
- 239000000843 powder Substances 0.000 description 21
- 239000010949 copper Substances 0.000 description 14
- 239000000758 substrate Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 238000005245 sintering Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 238000004544 sputter deposition Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 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
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 238000007780 powder milling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
본 발명은 저반사, 내화학성 및 내열성이 우수한 몰리브덴 산화물계 소결체, 상기 소결체를 이용한 박막, 상기 박막을 포함하는 박막트랜지스터 및 디스플레이 장치를 제공한다. The present invention provides a molybdenum oxide-based sintered body with excellent low reflection, chemical resistance and heat resistance, a thin film using the sintered body, a thin film transistor and a display device including the thin film.
Description
본 발명은 저반사, 내화학성 및 내열성이 우수한 몰리브덴 산화물계 소결체, 상기 소결체를 이용한 박막, 상기 박막을 포함하는 박막트랜지스터 및 디스플레이 장치에 관한 것이다. The present invention relates to a molybdenum oxide-based sintered body with excellent low reflection, chemical resistance and heat resistance, a thin film using the sintered body, a thin film transistor and a display device including the thin film.
일반적으로 평판 디스플레이(flat panel display; "FPD"), 터치 스크린 패널, 태양 전지, 발광 다이오드(light emitting diode; "LED"), 유기 발광다이오드(organic light emitting diode; "OLED")에 저반사율의 도전성 박막이 사용되고 있다.In general, low-reflectivity devices are used in flat panel displays (“FPD”), touch screen panels, solar cells, light emitting diodes (“LEDs”), and organic light emitting diodes (“OLEDs”). Conductive thin films are being used.
이에 대한 소재로서 산화인듐-산화주석(In2O3-SnO2)("ITO")이 대표적이며 ITO 조성물은 가시광선 투과도와 전기 전도율이 높은 도전성 박막을 형성하는 데 사용된다. 이러한 ITO 조성물은 우수한 저반사율 성능을 가지기는 하지만, 경제성이 떨어지기 때문에 산화인듐의 전부 또는 일부를 대체하는 소재들에 대한 연구가 계속되고 있다.A representative material for this is indium oxide-tin oxide (In 2 O 3 -SnO 2 ) (“ITO”), and the ITO composition is used to form a conductive thin film with high visible light transmittance and electrical conductivity. Although these ITO compositions have excellent low-reflectance performance, they are not economically feasible, so research is continuing on materials that replace all or part of indium oxide.
하지만 이러한 연구들에서 관심이 있는 부분은 타겟 재료를 통해 형성된 박막의 저반사율로서, 장시간 사용에 대한 박막의 신뢰도를 높일 수 있는 내화학성, 내열성의 특성에 대한 고려가 필요하다.However, the area of interest in these studies is the low reflectivity of the thin film formed from the target material, and it is necessary to consider the characteristics of chemical resistance and heat resistance, which can increase the reliability of the thin film for long-term use.
한편 본 발명자들은 기존 몰리브덴 산화물 타겟이 저반사 특성을 나타내는 반면, 내열성 및 내화학성이 상대적으로 저조하다는 것을 착안하였다.Meanwhile, the present inventors noticed that while existing molybdenum oxide targets exhibit low reflection characteristics, heat resistance and chemical resistance are relatively poor.
이에, 본 발명은 주(主)원료인 몰리브덴 산화물에 특정 금속 산화물과 금속을 소정 범위로 첨가하여 혼용함으로써 저반사 특성, 내열성 및 내화학성이 동시에 우수한 스퍼터링 타겟용 소결체, 이로부터 형성된 금속 산화물 박막, 및 상기 금속 산화물 박막이 형성된 박막트랜지스터와 디스플레이장치를 제공하는 것을 기술적 과제로 한다. Accordingly, the present invention provides a sintered body for a sputtering target that has excellent low-reflection properties, heat resistance, and chemical resistance at the same time by mixing specific metal oxides and metals in a predetermined range with molybdenum oxide, which is the main raw material; a metal oxide thin film formed therefrom; The technical task is to provide a thin film transistor and a display device formed with the metal oxide thin film.
본 발명의 다른 목적 및 이점은 하기 발명의 상세한 설명 및 청구범위에 의해 보다 명확하게 설명될 수 있다.Other objects and advantages of the present invention can be more clearly explained by the following detailed description and claims.
상기한 기술적 과제를 달성하기 위해, 본 발명은 MoO2와 MoO3을 포함하고, 상기 MoO2 및 MoO3 중 MoO2의 함량이 50~90 중량%로 구성되는 몰리브덴 산화물; Nb2O5, Ta2O5, ZrO2, TiO2, SnO2, 및 WO3으로 구성된 군에서 선택되는 1종 이상의 금속산화물(M1); 및 Mo, Ti, Cr, W, 및 Cu으로 구성된 군에서 선택되는 1종 이상의 금속(M2);을 포함하며, 당해 소결체의 총 중량 대비 적어도 70 중량% 이상의 몰리브덴 산화물을 포함하는 산화물 소결체를 제공한다. In order to achieve the above-described technical problem, the present invention includes MoO 2 and MoO 3 , and the MoO 2 content of MoO 2 and MoO 3 is 50 to 90% by weight; At least one metal oxide (M1) selected from the group consisting of Nb 2 O 5 , Ta 2 O 5 , ZrO 2 , TiO 2 , SnO 2 , and WO 3 ; And at least one metal (M2) selected from the group consisting of Mo, Ti, Cr, W, and Cu; and provides an oxide sintered body containing at least 70% by weight or more of molybdenum oxide relative to the total weight of the sintered body. .
본 발명의 일 실시예를 들면, 상기 금속(M2)은 당해 산화물 소결체 100 중량%를 기준으로 1.0 내지 5.0 중량%로 포함될 수 있다. For one embodiment of the present invention, the metal (M2) may be included in an amount of 1.0 to 5.0% by weight based on 100% by weight of the oxide sintered body.
본 발명의 일 실시예를 들면, 상기 몰리브덴 산화물과 금속산화물(M1)은 당해 산화물 소결체 100 중량%를 기준으로 95.0 내지 99.0 중량%로 포함되며, 상기 몰리브덴 산화물과 상기 금속 산화물(M1)의 함량 비율은 75 : 25 내지 90 : 10 중량비일 수 있다. For one embodiment of the present invention, the molybdenum oxide and the metal oxide (M1) are contained in an amount of 95.0 to 99.0% by weight based on 100% by weight of the oxide sintered body, and the content ratio of the molybdenum oxide and the metal oxide (M1) is The weight ratio may be 75:25 to 90:10.
본 발명의 일 실시예를 들면, 상기 산화물 소결체는 비저항이 1×10-2 Ωcm 이하이며, 상대밀도가 95% 이상일 수 있다. For one embodiment of the present invention, the oxide sintered body may have a specific resistance of 1×10 -2 Ωcm or less and a relative density of 95% or more.
또한 본 발명은 전술한 소결체를 포함하는 스퍼터링 타겟을 제공한다.Additionally, the present invention provides a sputtering target including the above-described sintered body.
또한 본 발명은 전술한 스퍼터링 타겟으로부터 형성된 산화물 박막을 제공한다. The present invention also provides an oxide thin film formed from the above-described sputtering target.
본 발명의 일 실시예를 들면, 상기 산화물 박막은 게이트층, 소스층 및 드레인층 중 어느 하나로 포함될 수 있다. For one embodiment of the present invention, the oxide thin film may be included as one of a gate layer, a source layer, and a drain layer.
아울러 본 발명은 전술한 산화물 박막을 포함하는 디스플레이 장치를 제공한다. In addition, the present invention provides a display device including the above-described oxide thin film.
본 발명의 실시예에 따르면, 몰리브덴 산화물을 주된 성분으로 하고, 여기에 특정 금속산화물(M1)과 금속(M2)을 소정 범위로 첨가하여 혼용(混用)함으로써, 몰리브덴 산화물계 소결체의 소결성을 개선하고 고밀도를 확보할 수 있다.According to an embodiment of the present invention, molybdenum oxide is used as the main component, and a specific metal oxide (M1) and a metal (M2) are added and mixed in a predetermined range to improve the sintering properties of the molybdenum oxide-based sintered body. High density can be secured.
또한 상기 소결체로부터 형성된 박막은 저반사 특성을 가지는 동시에 내열성 및 내화학성이 우수하다. 이에 따라 이러한 박막을 포함하여 이루어지는 박막 트랜지스터 또는 디스플레이장치의 동작 신뢰성을 확보할 수 있다.In addition, the thin film formed from the sintered body has low-reflection characteristics and is excellent in heat resistance and chemical resistance. Accordingly, the operational reliability of a thin film transistor or a display device including such a thin film can be secured.
그 외 본 발명의 효과들은 이하에 기재되는 구체적인 내용을 통하여, 또는 본 발명을 실시하는 과정 중에 이 기술분야의 전문가나 연구자에게 자명하게 파악되고 이해될 것이다.Other effects of the present invention will be readily apparent and understood by experts or researchers in the technical field through the specific details described below or during the process of implementing the present invention.
도 1은 금속(M2) 포함 여부에 따른 수소열처리 후 반사율 변화를 나타낸 그래프이다. Figure 1 is a graph showing the change in reflectance after hydrogen heat treatment depending on whether metal (M2) is included.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 명세서에서 사용되는 모든 용어(기술 및 과학적 용어를 포함)는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 공통적으로 이해될 수 있는 의미로 사용될 수 있을 것이다. 또 일반적으로 사용되는 사전에 정의되어 있는 용어들은 명백하게 특별히 정의되어 있지 않은 한 이상적으로 또는 과도하게 해석되지 않는다.All terms (including technical and scientific terms) used in this specification may be used with meanings that can be commonly understood by those skilled in the art in the technical field to which the present invention pertains. Additionally, terms defined in commonly used dictionaries are not to be interpreted ideally or excessively unless clearly specifically defined.
또한 명세서 전체에서, 어떤 부분이 어떤 구성요소를 "포함" 한다고 할 때, 이는 특별히 반대되는 기재가 없는 한, 다른 구성요소를 제외하는 것이 아니라 다른 구성요소를 더 포함할 수 있는 것을 의미한다. 또한, 명세서 전체에서, "위에" 또는 "상에"라 함은 대상 부분의 위 또는 아래에 위치하는 경우 뿐만 아니라 그 중간에 또 다른 부분이 있는 경우도 포함함을 의미하는 것이며, 반드시 중력 방향을 기준으로 위쪽에 위치하는 것을 의미하는 것은 아니다. 그리고, 본원 명세서에서 "제1", "제2" 등의 용어는 임의의 순서 또는 중요도를 나타내는 것이 아니라 구성요소들을 서로 구별하고자 사용된 것이다.In addition, throughout the specification, when a part is said to "include" a certain component, this means that it may further include other components rather than excluding other components, unless specifically stated to the contrary. In addition, throughout the specification, “above” or “on” means not only the case where it is located above or below the object part, but also the case where there is another part in the middle, and it must be in the direction of gravity. It does not mean that it is located above the standard. In addition, in the present specification, terms such as “first” and “second” do not indicate any order or importance, but are used to distinguish components from each other.
<소결체 및 스퍼터링 타겟><Sintered body and sputtering target>
본 발명의 일 예는, 몰리브덴 산화물을 주(主)성분으로 하는 스퍼터링용 타겟을 제작하기 위한 금속산화물 소결체이다. An example of the present invention is a metal oxide sintered body for producing a sputtering target containing molybdenum oxide as a main component.
일 구체예를 들면, 상기 소결체는 MoO2와 MoO3을 포함하고, 상기 MoO2 및 MoO3 중 MoO2의 함량이 50~90 중량%로 구성되는 몰리브덴 산화물; Nb2O5, Ta2O5, ZrO2, TiO2, SnO2, 및 WO3으로 구성된 군에서 선택되는 1종 이상의 금속산화물(M1); 및 Mo, Ti, Cr, W, 및 Cu으로 구성된 군에서 선택되는 1종 이상의 금속(M2)을 포함하며, 당해 소결체의 총 중량 대비 적어도 70 중량% 이상의 몰리브덴 산화물을 주(主)성분으로 포함한다. For one specific example, the sintered body is a molybdenum oxide containing MoO 2 and MoO 3 , and the content of MoO 2 among the MoO 2 and MoO 3 is 50 to 90% by weight; At least one metal oxide (M1) selected from the group consisting of Nb 2 O 5 , Ta 2 O 5 , ZrO 2 , TiO 2 , SnO 2 , and WO 3 ; and at least one metal (M2) selected from the group consisting of Mo, Ti, Cr, W, and Cu, and contains at least 70% by weight or more of molybdenum oxide as a main component relative to the total weight of the sintered body. .
전술한 조성으로 이루어진 금속산화물 소결체를 타겟 재료로 사용하여 박막을 형성하는 경우, 형성된 박막은 저반사 특성을 가지는 것과 동시에 몰리브덴 산화물의 비율과 조성의 최적화를 통해 내열성 및 내화학성이 향상된다.When a thin film is formed using a metal oxide sintered body having the above-mentioned composition as a target material, the formed thin film has low-reflection characteristics and at the same time, heat resistance and chemical resistance are improved through optimization of the ratio and composition of molybdenum oxide.
이하, 각 성분에 대하여 상세하게 설명한다.Hereinafter, each component will be described in detail.
몰리브덴 산화물은 예를 들면 MoO2, MoO3, MoO4와 같이 몰리브덴에 산소가 결합된 형태를 가지는 성분이다. 본 발명에서는 몰리브덴 산화물로서 MoO2와 MoO3을 포함한다.Molybdenum oxide is a component in which oxygen is bonded to molybdenum, such as MoO 2 , MoO 3 , and MoO 4 . In the present invention, molybdenum oxide includes MoO 2 and MoO 3 .
상기 몰리브덴 산화물을 이루는 MoO2와 MoO3의 함량에 있어서, MoO2는 50 내지 90 중량%의 함량을 가지고 MoO3는 10 내지 50 중량%의 함량을 가진다. MoO2 함량이 50 중량% 미만일 경우 상대적으로 MoO3의 양이 많아져서 소결밀도가 낮게 나오고 박막으로 증착 시 화학안정성 또한 좋지 않다. 한편 MoO2의 함량이 90 중량%를 초과하는 경우, MoO2 함량이 많아짐에 따라 소결밀도는 높게 나올 수 있지만 타겟 강도가 낮아져서 타겟 내에 균열이 발생할 수 있다. 한편 이를 MoO2/MoO3 중량% 비율로 나타내면 1~16이 된다. Regarding the content of MoO 2 and MoO 3 constituting the molybdenum oxide, MoO 2 has a content of 50 to 90 wt% and MoO 3 has a content of 10 to 50 wt%. If the MoO 2 content is less than 50% by weight, the amount of MoO 3 increases relatively, resulting in low sintered density and poor chemical stability when deposited as a thin film. On the other hand, when the content of MoO 2 exceeds 90% by weight, the sintered density may be high as the MoO 2 content increases, but the target strength may be lowered and cracks may occur within the target. Meanwhile, if expressed as a MoO2/MoO3 weight% ratio, it becomes 1 to 16.
본 발명의 산화물 소결체에 포함되는 첨가성분 중 하나는 Nb2O5, Ta2O5, ZrO2, TiO2, SnO2, 및 WO3 중 적어도 하나 이상의 금속산화물(M1)이다. One of the additional components included in the oxide sintered body of the present invention is a metal oxide (M1) of at least one of Nb 2 O 5 , Ta 2 O 5 , ZrO 2 , TiO 2 , SnO 2 , and WO 3 .
이러한 금속산화물(M1)은 내화학성 및 내열성 특성을 개선하는 산화물 도펀트로서, 상기 금속산화물 첨가에 의해 몰리브덴 산화물의 내화학성 및 내열성 특성을 높일 수 있다. 이하의 설명에서는 Nb2O5, Ta2O5, ZrO2, TiO2, SnO2, 및 WO3 중 적어도 하나 이상의 성분을 기호화 하여 M1으로 표시한다.This metal oxide (M1) is an oxide dopant that improves chemical resistance and heat resistance characteristics, and the chemical resistance and heat resistance characteristics of molybdenum oxide can be improved by adding the metal oxide. In the following description, at least one of Nb 2 O 5 , Ta 2 O 5 , ZrO 2 , TiO 2 , SnO 2 , and WO 3 is symbolized and indicated as M1.
본 발명의 산화물 소결체에 포함되는 첨가성분 중 다른 하나는 Mo, Ti, Cr, W, 및 Cu으로 구성된 군에서 선택되는 1종 이상의 금속(M2)이다. Another of the additive components included in the oxide sintered body of the present invention is at least one metal (M2) selected from the group consisting of Mo, Ti, Cr, W, and Cu.
이러한 금속(M2)은 몰리브덴 산화물의 소결성을 보조하여 밀도 상승 효과를 나타내는 금속 도펀트로서, 상기 금속 첨가에 의해 몰리브덴 산화물의 내화학성 및 내열성 특성을 높일 수 있다. 이하의 설명에서는 Mo, Ti, Cr, W, 및 Cu 중 적어도 하나 이상의 성분을 기호화하여 M2로 표시한다. This metal (M2) is a metal dopant that assists in the sintering properties of molybdenum oxide and exhibits a density-increasing effect. By adding the metal, the chemical resistance and heat resistance characteristics of molybdenum oxide can be improved. In the following description, at least one component among Mo, Ti, Cr, W, and Cu is symbolized as M2.
전술한 몰리브덴 산화물, 금속산화물(M1), 및 금속(M2)을 포함하는 금속산화물 소결체는, 당해 소결체 100 중량%를 기준으로 몰리브덴 산화물과 금속산화물 95.0 내지 99.0 중량%; 및 금속(M2) 1.0 내지 5.0 중량%로 이루어진 조성을 가질 수 있다. 여기서, 몰리브덴 산화물과 금속 산화물(M1)의 함량 비율은 75 : 25 내지 90 : 10 중량비로 구성될 수 있다. 몰리브덴 산화물의 비율이 당해 금속산화물 소결체 전체에서 75 중량% 이상을 차지할 경우 박막으로 증착시 저반사 특성을 가질 수 있다.The metal oxide sintered body containing the above-described molybdenum oxide, metal oxide (M1), and metal (M2) contains 95.0 to 99.0% by weight of molybdenum oxide and metal oxide based on 100% by weight of the sintered body; and 1.0 to 5.0% by weight of metal (M2). Here, the content ratio of molybdenum oxide and metal oxide (M1) may be in a weight ratio of 75:25 to 90:10. If the proportion of molybdenum oxide accounts for more than 75% by weight of the entire metal oxide sintered body, it may have low-reflection characteristics when deposited as a thin film.
상술한 바와 같이 구성되는 본 발명에 따른 산화물 소결체는, 상대밀도가 95% 이상이며, 그 상한치는 특별히 제한되지 않는다. 또한 산화물 소결체의 비저항이 1×10-2 Ωcm 이하이며, 그 하한치는 특별히 제한되지 않는다. 그리고 산화물 소결체에 포함된 결정립의 크기는 특별히 제한되지 않으며, 일례로 1 내지 20 ㎛일 수 있으며, 구체적으로 1 내지 10 ㎛일 수 있다. The oxide sintered body according to the present invention configured as described above has a relative density of 95% or more, and its upper limit is not particularly limited. Additionally, the specific resistance of the oxide sintered body is 1×10 -2 Ωcm or less, and the lower limit is not particularly limited. And the size of the crystal grains included in the oxide sintered body is not particularly limited, and may be, for example, 1 to 20 ㎛, and specifically 1 to 10 ㎛.
또한 본 발명의 다른 일 실시예에 따른 스퍼터링 타겟은, 전술한 몰리브덴 산화물을 주(主)성분으로 하는 산화물 소결체; 및 상기 소결체의 일면에 접합되어 상기 소결체를 지지하는 백킹 플레이트를 포함한다. In addition, a sputtering target according to another embodiment of the present invention includes an oxide sintered body containing the above-described molybdenum oxide as a main component; and a backing plate bonded to one surface of the sintered body and supporting the sintered body.
여기서, 백킹 플레이트는 스퍼터링 타겟용 소결체를 지지하는 기판으로서, 당 분야에 알려진 통상적인 백킹 플레이트를 제한 없이 사용할 수 있다. 이때 백킹 플레이트를 구성하는 재료 및 이의 형상은 특별히 제한되지 않는다.Here, the backing plate is a substrate that supports the sintered body for the sputtering target, and conventional backing plates known in the art can be used without limitation. At this time, the material constituting the backing plate and its shape are not particularly limited.
<산화물 소결체 및 스퍼터링 타겟의 제조방법><Manufacturing method of oxide sintered body and sputtering target>
이하, 본 발명의 일 실시형태에 따른 산화물 소결체 및 스퍼터링 타겟의 제조방법에 대해 설명한다. 그러나 하기 제조방법에 의해서만 한정되는 것은 아니며, 필요에 따라 각 공정의 단계가 변형되거나 또는 선택적으로 혼용되어 수행될 수 있다. Hereinafter, a method for manufacturing an oxide sintered body and a sputtering target according to an embodiment of the present invention will be described. However, it is not limited to the following manufacturing method, and the steps of each process may be modified or selectively mixed as needed.
상기 제조방법의 바람직한 일 실시예를 들면, (i) 몰리브덴 산화물, 적어도 1종의 금속산화물(M1) 및 적어도 1종의 금속(M2)을 혼합하는 제1 단계; (ii) 혼합된 원료분말을 소결하는 제2 단계; (iii) 재료분말이 소결된 소결체를 가공하는 제3단계; 및 (iv) 소결체를 백킹플레이트에 본딩하여 타겟을 완성하는 제4 단계를 포함하여 이루어질 수 있다.A preferred embodiment of the above manufacturing method includes (i) a first step of mixing molybdenum oxide, at least one metal oxide (M1), and at least one metal (M2); (ii) a second step of sintering the mixed raw material powder; (iii) a third step of processing the sintered body in which the material powder is sintered; and (iv) a fourth step of completing the target by bonding the sintered body to the backing plate.
이하, 상기 제조방법을 각 공정 단계별로 나누어 설명하면 다음과 같다.Hereinafter, the manufacturing method will be described by dividing it into each process step as follows.
먼저 제1 단계에서는, MoO2와 MoO3로 이루어진 몰리브덴 산화물 분말; Nb2O5, Ta2O5, ZrO2, TiO2, SnO2, WO3 분말 중 적어도 1종의 금속산화물(M1); 및 Mo, Ti, Cr, W, 및 Cu 중 적어도 1종의 금속(M2)을 원하는 화학 조성에 맞게 칭량한 후 혼합한다. First, in the first step, molybdenum oxide powder consisting of MoO 2 and MoO 3 ; At least one metal oxide (M1) among Nb 2 O 5 , Ta 2 O 5 , ZrO 2 , TiO 2 , SnO 2 , and WO 3 powder; And at least one metal (M2) among Mo, Ti, Cr, W, and Cu is weighed to suit the desired chemical composition and then mixed.
구체적으로, 상기 원료분말은 몰리브덴 산화물과 금속산화물(M1) 95.0 내지 99.0 중량%; 및 금속(M2) 1.0 내지 5.0 중량%;로 포함되며, 상기 몰리브덴 산화물과 상기 금속산화물(M1)의 혼합 비율은 75 : 25 내지 90 : 10 중량비로 구성되는 조성을 가질 수 있다. 이때 몰리브덴 산화물 분말에서 MoO2의 비율은 50~90 중량% 내에서 선택할 수 있다.Specifically, the raw material powder contains 95.0 to 99.0% by weight of molybdenum oxide and metal oxide (M1); and 1.0 to 5.0% by weight of metal (M2), and the mixing ratio of the molybdenum oxide and the metal oxide (M1) may be in a weight ratio of 75:25 to 90:10. At this time, the ratio of MoO 2 in molybdenum oxide powder can be selected within 50 to 90% by weight.
상기 제1 단계의 일 구체예를 들면, 몰리브덴 산화물과 금속산화물(M1) 분말의 (MoO2+MoO3+M1)/(MoO2+MoO3) 중량% 비율이 1.03 내지 1.30%가 되도록 칭량한다. For example, in the first step, the molybdenum oxide and metal oxide (M1) powder are weighed so that the (MoO 2 +MoO 3 +M1)/(MoO 2 +MoO 3 ) weight % ratio is 1.03 to 1.30%. .
이어서 혼합된 원료분말에 금속분말(M2)을 첨가하되, 상기 금속 분말(M2)의 (MoO2+MoO3+M1+M2) / (MoO2+MoO3+M1) 중량% 비율이 1.03 내지 1.3%가 되도록 칭량한다. 여기에서 MoO2의 함량과 MoO3의 함량은 분자와 분모에서 각각 동일하다. 혼합된 분말은 지르코니아 볼을 이용하여 건식 볼밀 공정을 수행한다.Next, metal powder (M2) is added to the mixed raw material powder, and the (MoO 2 +MoO 3 +M1+M2) / (MoO 2 +MoO 3 +M1) weight % ratio of the metal powder (M2) is 1.03 to 1.3. Weigh to obtain %. Here, the content of MoO 2 and the content of MoO 3 are the same in the numerator and denominator, respectively. The mixed powder is subjected to a dry ball mill process using zirconia balls.
지르코니아 볼은 분말량의 1~3배로 칭량할 수 있고, 볼밀은 100~300 rpm의 속도로 7~9시간 동안 수행할 수 있다. 건식 볼밀을 완료한 후에 체질하여 분말 혼합을 완료할 수 있다.Zirconia balls can be weighed 1 to 3 times the amount of powder, and ball milling can be performed at a speed of 100 to 300 rpm for 7 to 9 hours. After completing the dry ball mill, powder mixing can be completed by sieving.
다음으로 제2 단계에서는, 혼합된 분말을 소결하기 위하여 카본 몰드 내부와 하부 펀치에 카본 시트를 0.1~0.5mm로 감싸고 혼합된 분말 100~300g을 장입할 수 있다. 분말을 장입한 후에 카본 시트를 덮고 상부 펀치를 설치한다.Next, in the second step, in order to sinter the mixed powder, a carbon sheet of 0.1 to 0.5 mm can be wrapped inside the carbon mold and the lower punch, and 100 to 300 g of the mixed powder can be charged. After charging the powder, cover the carbon sheet and install the upper punch.
이와 같은 과정을 통해 소결 몰드의 준비가 완료되면 핫프레스에 소결 몰드를 장입하고 소결 과정을 수행할 수 있다. 소결시 승온속도는 2~10℃/분으로 하고, 최고 열처리 온도는 700~1,100℃에서 1~3시간으로 유지할 수 있다. 승온 및 유지 온도에서의 압력은 20~50 MPa로 유지할 수 있다.Once the preparation of the sintering mold is completed through this process, the sintering mold can be charged into the hot press and the sintering process can be performed. During sintering, the temperature increase rate is 2 to 10°C/min, and the maximum heat treatment temperature can be maintained at 700 to 1,100°C for 1 to 3 hours. The pressure at elevated and maintained temperatures can be maintained at 20 to 50 MPa.
다음으로 제3 단계에서는 소결이 완료된 소결체를 취출하여 가공한다. 구체적으로는 소결체를 꺼낸 후에 타겟 상하부에 카본 시트를 제거한 다음 타겟의 표면을 연마가공한다. 카본 시트를 제거하기 위하여 상하부에 각 1mm 이상 가공할 수 있다.Next, in the third step, the sintered body that has completed sintering is taken out and processed. Specifically, after taking out the sintered body, the carbon sheets are removed from the top and bottom of the target, and then the surface of the target is polished. To remove the carbon sheet, more than 1 mm can be processed on each side.
다음으로 제4 단계에서는 가공된 소결체를 백킹플레이트에 본딩한다.Next, in the fourth step, the processed sintered body is bonded to the backing plate.
접착제로는 인듐을 사용할 수 있고, 본딩율은 95% 이상이 되도록 하는 것이 바람직하다.Indium can be used as an adhesive, and it is desirable to have a bonding rate of 95% or more.
전술한 과정을 통해 금속 산화물 타겟을 제조할 수 있다. 제조된 타겟의 타겟밀도는 95% 이상이고, 구체적으로 97.5% 이상이 되도록 하는 것이 바람직하다.A metal oxide target can be manufactured through the above-described process. The target density of the manufactured target is preferably 95% or more, and specifically, 97.5% or more.
<산화물 박막><Oxide thin film>
본 발명의 다른 일 예는, 전술한 몰리브덴 산화물계 타겟을 사용하여 증착된 금속산화물 박막이다. 이러한 금속산화물 박막은 전술한 소결체를 타겟 재료로 하여 스퍼터링을 수행함으로써 형성될 수 있다.Another example of the present invention is a metal oxide thin film deposited using the molybdenum oxide-based target described above. This metal oxide thin film can be formed by performing sputtering using the above-described sintered body as a target material.
상기 산화물 박막은 증착 분위기에 따라 성분의 미차가 발생할 수는 있으나, 전술한 산화물 타겟을 스퍼터링하여 제조된 것이므로, 상기 타겟과 조성이 실질적으로 동일하다. 이에 따라, 상대밀도 95%를 초과하는 고밀도 특성과 1×10-2 Ωcm 이하의 우수한 비저항 특성을 갖는 산화물 박막이 형성될 수 있다. 또한 주(主)원료인 몰리브덴 산화물에 특정 금속 산화물과 금속을 소정 범위로 첨가하되, 몰리브덴 산화물 비율과 조성 최적화를 통해 내화학성, 및 내열성 특성이 향상될 수 있다.The oxide thin film may have slight differences in composition depending on the deposition atmosphere, but since it is manufactured by sputtering the oxide target described above, its composition is substantially the same as that of the target. Accordingly, an oxide thin film having high density characteristics exceeding 95% relative density and excellent resistivity characteristics of 1×10 -2 Ωcm or less can be formed. In addition, specific metal oxides and metals are added to molybdenum oxide, the main raw material, in a predetermined range, but chemical resistance and heat resistance characteristics can be improved by optimizing the molybdenum oxide ratio and composition.
일 구체예를 들면, 상기 산화물 박막은 350℃의 온도 및 30분 이상의 열처리 후 하기 식 1에 따른 광 반사율 변화율(ΔR)이 30% 이하일 수 있으며, 구체적으로 20% 이하, 보다 구체적으로 15% 이하일 수 있다. For example, the oxide thin film may have a light reflectance change rate (ΔR) of 30% or less according to Equation 1 below after heat treatment at a temperature of 350°C and for 30 minutes or more, specifically 20% or less, and more specifically 15% or less. You can.
[식 1][Equation 1]
광 반사율 변화율(ΔR, %) = (R2 - R1)/R1 ×100Light reflectance change rate (ΔR, %) = (R 2 - R 1 )/R 1 × 100
상기 식에서, In the above equation,
R1은 열처리 전 550nm 파장에 대한 박막의 광 반사율이고, R 1 is the optical reflectance of the thin film for a wavelength of 550 nm before heat treatment,
R2는 열처리 후 550nm 파장에 대한 박막의 광 반사율이다. R 2 is the light reflectance of the thin film for a wavelength of 550 nm after heat treatment.
구체적으로, 상기 산화물 박막은 열처리 전 550nm 파장에 대한 광 반사율(R1)은 10.5% 이하이며, 보다 구체적으로 10.4% 이하일 수 있다. 또한 350℃ 온도 및 30분 이상의 열처리 후 550nm 파장에 대한 광 반사율(R2)은 12.5% 이하이며, 보다 구체적으로 12% 이하일 수 있다. 이때 광 반사율(R1, R2) 및 광 반사율 변화율(ΔR)의 하한치는 특별히 제한되지 않는다.Specifically, the oxide thin film may have a light reflectance (R 1 ) of 10.5% or less at a wavelength of 550 nm before heat treatment, and more specifically, 10.4% or less. In addition, after heat treatment at a temperature of 350°C and for more than 30 minutes, the light reflectance (R 2 ) for a wavelength of 550 nm may be 12.5% or less, and more specifically, may be 12% or less. At this time, the lower limits of the light reflectance (R 1, R 2 ) and the light reflectance change rate (ΔR) are not particularly limited.
한편 전술한 광 반사율은 360~740nm의 평균 파장, 및/또는 550 nm 파장을 기준으로 측정된 것을 의미하나, 이에 특별히 제한되지 않는다. Meanwhile, the above-mentioned light reflectance means measured based on an average wavelength of 360 to 740 nm and/or a wavelength of 550 nm, but is not particularly limited thereto.
본 발명에 따른 금속산화물 박막은 당 분야에 공지된 통상의 스퍼터링법에 의해 형성(증착)될 수 있다. 이때 스퍼터링은 DC 스퍼터(Sputter)를 이용하여 수행할 수 있다.The metal oxide thin film according to the present invention can be formed (deposited) by a common sputtering method known in the art. At this time, sputtering can be performed using DC sputter.
상기 금속산화물 박막은 박막 트랜지스터(TFT)의 게이트층, 소스층 및 드레인층 중 적어도 하나로 이용될 수 있다. 또한 이러한 박막 트랜지스터는 OLED TV, 모바일폰, 태블릿 등의 디스플레이 장치에 사용될 수 있다.The metal oxide thin film can be used as at least one of the gate layer, source layer, and drain layer of a thin film transistor (TFT). Additionally, these thin film transistors can be used in display devices such as OLED TVs, mobile phones, and tablets.
구체적인 예로서, 본 발명의 실시예에 따른 금속 산화물 박막은 게이트층 하부의 저반사층으로 사용될 수 있다. 이와 같은 용도의 박막은 기판의 반사율을 낮추고 게이트 전극의 접착성을 향상시킨다.As a specific example, the metal oxide thin film according to an embodiment of the present invention can be used as a low-reflection layer under the gate layer. Thin films for this purpose lower the reflectance of the substrate and improve the adhesion of the gate electrode.
여기에서, 기판은 유리기판, 금속기판, 플라스틱 기판, 플라스틱 필름 등 통상의 디스플레이 소자 공정에서 사용 가능한 다양한 기판 중 어느 하나일 수 있다. 구체적으로 기판은 OLED TV, 모바일폰, 태블릿에 있어서 투명하게 이루어진 전면패널일 수 있다. 한편 게이트 전극은 구리, 은 등의 일반적인 전극 물질로 형성될 수 있다.Here, the substrate may be any one of various substrates that can be used in a typical display device process, such as a glass substrate, a metal substrate, a plastic substrate, or a plastic film. Specifically, the substrate may be a transparent front panel for an OLED TV, mobile phone, or tablet. Meanwhile, the gate electrode may be formed of common electrode materials such as copper and silver.
박막 증착은 DC 스퍼터의 전력밀도(Power density)를 1.0~2.0w/cm2 로 하고 아르곤 가스(Ar Gas) 분위기에서 상온에서 실시할 수 있다. 이때 금속 산화물 박막의 두께는 300 내지 500Å으로 할 수 있으나, 이에 특별히 제한되지 않는다. 또한 금속 산화물 박막 위에는 구리(Cu) 박막이 증착될 수 있다. 이때 구리 박막은 3000 내지 6000Å의 두께로 증착될 수 있다.Thin film deposition can be performed at room temperature in an argon gas (Ar Gas) atmosphere with the power density of DC sputtering being 1.0 to 2.0 w/cm 2 . At this time, the thickness of the metal oxide thin film may be 300 to 500 Å, but is not particularly limited thereto. Additionally, a copper (Cu) thin film may be deposited on the metal oxide thin film. At this time, the copper thin film may be deposited to a thickness of 3000 to 6000 Å.
한편 반사율의 측정은 당 분야에 공지된 방법에 따라 수행될 수 있다. 일례로, 금속산화물 박막이 형성된 기판 면에서 측정할 수 있고, 360~740nm의 평균 파장 및/또는 550nm 파장에 대한 광 반사율을 측정한다. 이때 광 반사율은 10.5% 이하일 수 있다.Meanwhile, measurement of reflectance can be performed according to methods known in the art. For example, it can be measured on the surface of the substrate on which the metal oxide thin film is formed, and the light reflectance is measured for an average wavelength of 360 to 740 nm and/or a wavelength of 550 nm. At this time, the light reflectance may be 10.5% or less.
본 발명의 실시예에 따른 금속 산화물 박막은 내열성, 내화학성 특성이 우수하다. 내열성, 내화학성 평가는 아래와 같이 수행할 수 있으나, 이에 특별히 제한되지 않는다.The metal oxide thin film according to an embodiment of the present invention has excellent heat resistance and chemical resistance properties. Heat resistance and chemical resistance evaluation can be performed as follows, but is not particularly limited thereto.
내열성을 평가하기 위해, 상술한 바와 같이 증착된 박막을 200~400℃의 분위기에서 30분 이상의 열처리를 하는 방법을 사용할 수 있다. 열처리는 일반적인 진공 열처리로 및/또는 수소 열처리로에서 수행할 수 있다. 열처리 후 박막의 특성 변화를 관찰함으로써 내열성을 평가할 수 있다. 내열성 지표의 예를 들면, 열처리 후 반사율(R2)과 열처리 전 반사율(R1)과의 차이(R2-R1)는 대략 1.5% 이하이며, 구체적으로 1.2% 이하일 수 있다. 또한 전술한 식 1에 따라 산출된 반사율 변화율(ΔR)을 통해 평가할 수도 있다. In order to evaluate heat resistance, a method of heat treating the deposited thin film as described above in an atmosphere of 200 to 400° C. for 30 minutes or more can be used. Heat treatment can be performed in a general vacuum heat treatment furnace and/or a hydrogen heat treatment furnace. Heat resistance can be evaluated by observing changes in the properties of the thin film after heat treatment. For example, as an example of a heat resistance index, the difference (R 2 -R 1 ) between the reflectance after heat treatment (R 2 ) and the reflectance before heat treatment (R 1 ) may be approximately 1.5% or less, and specifically, 1.2% or less. It can also be evaluated through the reflectance change rate (ΔR) calculated according to Equation 1 described above.
또한 내화학성을 평가하기 위해, 형성된 박막에 리소그라피 방법을 이용하여 미세 패턴을 형성하고 형성된 미세 패턴의 단면을 관찰하는 방법을 사용할 수 있다. 구체적으로 위와 같이 본 발명의 금속 산화물과 구리의 2개 층으로 형성된 박막에 1~2 ㎛ 두께의 포토레지스트(Positive PR Strip)를 도포한 후 60~80℃에서 대략 0.5~2 시간 정도 베이킹(Backing)하여 포토레지스터를 고형화한다. 이어서 마스크(PRMask)를 정렬한 후 노광을 하여 일정 선폭의 패턴을 만든다. 이렇게 만든 패턴을 에칭(etching)하여 금속 산화물과 구리로 구성된 2층의 미세 패턴을 형성할 수 있다. 이와 같이 미세 패턴이 형성된 기판에서 포토레지스트를 제거한 후 미세 패턴에서 금속 산화물의 단면을 FIB-SEM으로 관찰할 수 있다. 이러한 본 발명의 박막은 에칭 이후에도 잔사가 발생되지 않게 되며, 이를 통해 내화학성을 평가할 수 있다. Additionally, in order to evaluate chemical resistance, a method of forming a fine pattern on the formed thin film using a lithography method and observing the cross section of the formed fine pattern can be used. Specifically, as described above, a 1-2 ㎛ thick photoresist (Positive PR Strip) is applied to the thin film formed of two layers of the metal oxide and copper of the present invention, and then baked at 60-80°C for approximately 0.5-2 hours. ) to solidify the photoresist. Next, the mask (PRMask) is aligned and exposed to create a pattern with a certain line width. By etching the pattern created in this way, a two-layer fine pattern composed of metal oxide and copper can be formed. After removing the photoresist from the substrate on which the fine pattern is formed, the cross section of the metal oxide in the fine pattern can be observed using FIB-SEM. The thin film of the present invention does not generate residue even after etching, and through this, chemical resistance can be evaluated.
이하, 본 발명을 실시예를 통하여 상세히 설명하면 다음과 같다. 단, 하기 실시예는 본 발명을 예시하는 것일 뿐, 본 발명이 하기 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail through examples. However, the following examples are merely illustrative of the present invention, and the present invention is not limited by the following examples.
[실시예 1] [Example 1]
MoO2/MoO3 중량% 비율이 6.8이고, (MoO2+MoO3+Nb2O5+Mo) / (MoO2+MoO3+Nb2O5)의 중량% 비율이 1.05가 되도록 분말을 계량하였다. 계량된 분말을 1L 플라스틱 통에 넣고, 알루미나 볼을 상기 분말량의 3배수로 투입하였다. 알루미나 볼은 3~10mm 볼을 사용하였다. 계량된 분말과 볼의 투입이 완료되면, 볼밀 기계에서 170~230 rpm의 속도로 8시간 동안 건식 혼합을 실시하였다. 수득한 건식 분말을 핫프레스(Hot Press)로 가압 소결을 하였다. 이때 핫프레스의 내부 진공 조건은 10-1 torr에서 실시하며, 승온속도는 3~7℃, 최고 온도는 1,000~1,100℃, 유지시간은 1~3시간 정도로 유지하여 소결을 진행한 후 노냉을 수행하였다. Weigh the powder so that the weight% ratio of MoO 2 /MoO 3 is 6.8 and the weight% ratio of (MoO 2 +MoO 3 +Nb 2 O 5 +Mo) / (MoO 2 +MoO 3 +Nb 2 O 5 ) is 1.05. did. The measured powder was placed in a 1L plastic container, and alumina balls were added in an amount three times the amount of the powder. Alumina balls of 3 to 10 mm were used. Once the weighed powder and balls were completely added, dry mixing was performed in a ball mill machine at a speed of 170 to 230 rpm for 8 hours. The obtained dry powder was pressurized and sintered using a hot press. At this time, the internal vacuum conditions of the hot press are performed at 10 -1 torr, the temperature increase rate is 3~7℃, the maximum temperature is 1,000~1,100℃, and the holding time is maintained at about 1~3 hours to proceed with sintering, followed by furnace cooling. did.
상기와 같이 얻어진 실시예 1의 금속산화물 소결체는 소결 밀도가 97.6%이고, 비저항은 1.15×10-3 Ωcm로 측정되었다. The metal oxide sintered body of Example 1 obtained as described above had a sintered density of 97.6%, and a specific resistance was measured at 1.15×10 -3 Ωcm.
[실시예 2] [Example 2]
MoO2/MoO3 중량% 비율이 6.6이고, (MoO2+MoO3+Nb2O5+Mo) / (MoO2+MoO3+Nb2O5)의 wt% 비율이 1.05 대신 1.08이 되도록 계량된 분말을 사용한 것을 제외하고는, 상기 실시예 1과 동일하게 실시하여 실시예 2의 소결체를 제조하였다. Weighing so that the MoO 2 /MoO 3 wt% ratio is 6.6, and the wt% ratio of (MoO 2 +MoO 3 +Nb 2 O 5 +Mo) / (MoO 2 +MoO 3 +Nb 2 O 5 ) is 1.08 instead of 1.05. The sintered body of Example 2 was manufactured in the same manner as Example 1, except that the powder was used.
상기와 같이 제조된 실시예 2의 소결체는 소결 밀도가 97.8%이고, 비저항은 1.2×10-3 Ωcm로 측정되었다. The sintered body of Example 2 prepared as above had a sintered density of 97.8% and a specific resistance was measured at 1.2×10 -3 Ωcm.
[실시예 3] [Example 3]
MoO2/MoO3 중량% 비율이 6.5이고, (MoO2+MoO3+Nb2O5+Mo) / (MoO2+MoO3+Nb2O5)의 wt% 비율이 1.05 대신 1.18이 되도록 계량된 분말을 사용한 것을 제외하고는, 상기 실시예 1과 동일하게 실시하여 실시예 3의 소결체를 제조하였다. Powder weighed so that the MoO2/MoO3 wt% ratio is 6.5 and the wt% ratio of (MoO 2 +MoO 3 +Nb 2 O 5 +Mo) / (MoO 2 +MoO 3 +Nb 2 O 5 ) is 1.18 instead of 1.05. The sintered body of Example 3 was manufactured in the same manner as Example 1, except that .
상기와 같이 제조된 실시예 3의 소결체는 소결 밀도가 99.9%이고, 비저항은 1.07×10-3 Ωcm로 측정되었다.The sintered body of Example 3 prepared as above had a sintered density of 99.9% and a specific resistance was measured at 1.07×10 -3 Ωcm.
[비교예 1] [Comparative Example 1]
Mo 금속을 사용하지 않고, (MoO2+MoO3+Nb2O5)/(MoO2+MoO3+Nb2O5)의 wt% 비율을 1 이 되도록 계량된 분말을 사용한 것을 제외하고는, 상기 실시예 1과 동일하게 실시하여 비교예 1의 소결체를 제조하였다. Except that Mo metal was not used and powder weighed so that the wt% ratio of (MoO 2 +MoO 3 +Nb 2 O 5 )/(MoO 2 +MoO 3 +Nb 2 O 5 ) was 1 was used. The sintered body of Comparative Example 1 was manufactured in the same manner as Example 1.
상기와 같이 제조된 비교예 1의 소결체는 소결 밀도가 96.1%이고, 비저항은 1.27×10-3 Ωcm로 측정되었다.The sintered body of Comparative Example 1 prepared as described above had a sintered density of 96.1% and a specific resistance of 1.27×10 -3 Ωcm.
[실험예 1: 소결체의 물성 평가][Experimental Example 1: Evaluation of physical properties of sintered body]
실시예 1 내지 3 및 비교예 1에서 제조된 소결체의 물성의 결과를 하기 표 1에 정리하였다.The results of the physical properties of the sintered bodies prepared in Examples 1 to 3 and Comparative Example 1 are summarized in Table 1 below.
(M2)metal
(M2)
MoO3 MoO 2 /
MoO 3
(MoO2+MoO3+M1)(MoO 2 +MoO 3 +M1+M2)/
(MoO 2 +MoO 3 +M1)
(%)Sintered Density
(%)
(Ωcm)resistivity
(Ωcm)
상기 표 1에 나타난 바와 같이, 실시예와 비교예 모두에서 기준치에 해당하는 비저항 1×10-2 Ωcm 이하, 타겟 밀도는 95% 이상을 만족하였다. 다만, 타켓 밀도의 측면에서 실시예 1 내지 실시예 3가 비교예 1에 비해 보다 우수하고, 비저항도 더 낮다는 것을 확인하였다. 이에 따라 타겟 밀도가 높고 비저항이 낮은 실시예 1 내지 실시예 3의 경우 박막 증착 시 더 안정적으로 플라즈마 형성이 가능하다는 것을 알 수 있었다.As shown in Table 1, in both examples and comparative examples, the specific resistance of 1×10 -2 Ωcm or less and the target density of 95% or more were satisfied, which corresponds to the standard values. However, it was confirmed that Examples 1 to 3 were superior to Comparative Example 1 in terms of target density and had lower specific resistance. Accordingly, it was found that in the case of Examples 1 to 3, where the target density was high and the specific resistance was low, more stable plasma formation was possible when depositing a thin film.
[실험예 2: 박막의 물성 평가][Experimental Example 2: Evaluation of physical properties of thin film]
실시예 1 내지 3 및 비교예 1에서 제조된 소결체를 타겟 재료로 하여 박막을 형성한 후, 박막의 내열성을 하기와 같이 평가하였다.After forming a thin film using the sintered body manufactured in Examples 1 to 3 and Comparative Example 1 as a target material, the heat resistance of the thin film was evaluated as follows.
구체적으로, 각 소결체를 이용하여 게이트층 하부의 저반사층으로 하는 박막을 제작하였다. 이러한 박막은 기판(유리) 상에 저반사 및 게이트 전극의 접착성을 향상시키기 위한 것이다.Specifically, a thin film serving as a low-reflection layer below the gate layer was produced using each sintered body. This thin film is intended to improve low reflection and adhesion of the gate electrode on the substrate (glass).
저반사 박막은 실시예 1~3 및 비교예 1의 소결체를 포함하는 타겟을 DC스퍼터를 이용하여 전력밀도(Power density)는 0.5~3.6w/cm2로 하고 아르곤 가스 분위기 하에서 투명한 글래스 기판 위에 증착하여 박막을 형성하였으며, 박막 두께는 350Å로 증착하였다.The low-reflection thin film was deposited on a transparent glass substrate under an argon gas atmosphere using a target containing the sintered body of Examples 1 to 3 and Comparative Example 1 with a power density of 0.5 to 3.6 w/cm 2 using DC sputtering. A thin film was formed, and the thin film was deposited to a thickness of 350Å.
추가로 전술한 박막 위에 전극을 형성하였다. 전극은 구리 타겟을 DC스퍼터를 이용하여 전력밀도(Power density)는 0.5~3.6w/cm2로 하고 아르곤 가스분위기에서 형성하였으며, 박막두께는 6000Å으로 하였다.Additionally, electrodes were formed on the aforementioned thin film. The electrode was formed in an argon gas atmosphere using a copper target with a power density of 0.5~3.6w/cm 2 using DC sputtering, and the thin film thickness was 6000Å.
이러한 상태에서 글래스 기판 면에서 박막의 최초 반사율을 측정한 후 진공열처리로에서 350℃의 온도로 30분 이상 열처리한 후 반사율을 다시 측정하고 양 반사율을 비교하였다. 이때 반사율은 360~740 nm의 평균 파장 및/또는 550 nm 파장에서의 반사율 수치를 사용하였으며, 이들의 결과를 하기 표 2에 기재하였다.In this state, the initial reflectance of the thin film was measured on the surface of the glass substrate, and then heat treated in a vacuum heat treatment furnace at a temperature of 350°C for more than 30 minutes, and then the reflectance was measured again and both reflectances were compared. At this time, the reflectance values at an average wavelength of 360 to 740 nm and/or a wavelength of 550 nm were used, and the results are listed in Table 2 below.
반사율 (열처리전)
360~740nm 평균 기준
(550 nm)Low reflection/Cu thin film
Reflectance (before heat treatment)
Based on average of 360~740nm
(550 nm)
반사율(열처리후)
360~740nm 평균 기준
(550 nm)Low reflection/Cu thin film
Reflectance (after heat treatment)
Based on average of 360~740nm
(550 nm)
변화율
(%)reflectivity
rate of change
(%)
상기 표 2에 나타난 바와 같이, 비교예 1의 최초 반사율은 양호하였으나, 열처리 후의 반사율은 크게 증가하였음을 알 수 있었다. As shown in Table 2, the initial reflectance of Comparative Example 1 was good, but it was found that the reflectance after heat treatment increased significantly.
이에 비해, 실시예 1~3의 경우 최초 반사율이 모두 양호하였으며, 열처리 후의 반사율 변화도 크지 않음을 확인하였다. 특히 실시예들의 경우 수소열처리로에서 350℃에서 30분 이상 열처리한 후 반사율이 최초 반사율로부터 10% 이내의 변화를 보임으로써, 비교예에 비해 내열성이 더 우수한 박막 특성을 갖는다는 것을 알 수 있었다.In contrast, in the case of Examples 1 to 3, the initial reflectance was all good, and it was confirmed that the change in reflectance after heat treatment was not significant. In particular, in the case of the examples, the reflectance showed a change of less than 10% from the initial reflectance after heat treatment at 350 ° C. for more than 30 minutes in a hydrogen heat treatment furnace, showing that the thin film had better heat resistance and better heat resistance characteristics than the comparative example.
Claims (10)
Nb2O5, Ta2O5, ZrO2, TiO2, SnO2, 및 WO3으로 구성된 군에서 선택되는 1종 이상의 금속산화물(M1); 및
Mo, Ti, Cr, W, 및 Cu으로 구성된 군에서 선택되는 1종 이상의 금속(M2);을 포함하며,
당해 소결체의 총 중량 대비 적어도 70 중량% 이상의 몰리브덴 산화물을 포함하는 산화물 소결체.Molybdenum oxide containing MoO 2 and MoO 3 and having a content of MoO 2 of 50 to 90% by weight among the MoO 2 and MoO 3 ;
At least one metal oxide (M1) selected from the group consisting of Nb 2 O 5 , Ta 2 O 5 , ZrO 2 , TiO 2 , SnO 2 , and WO 3 ; and
Contains at least one metal (M2) selected from the group consisting of Mo, Ti, Cr, W, and Cu,
An oxide sintered body containing at least 70% by weight or more of molybdenum oxide relative to the total weight of the sintered body.
상기 금속(M2)은 당해 산화물 소결체 100 중량%를 기준으로 1.0 내지 5.0 중량%로 포함되는, 산화물 소결체. According to paragraph 1,
The metal (M2) is contained in an amount of 1.0 to 5.0% by weight based on 100% by weight of the oxide sintered body.
상기 몰리브덴 산화물과 금속산화물(M1)은 당해 산화물 소결체 100 중량%를 기준으로 95.0 내지 99.0 중량%로 포함되며,
상기 몰리브덴 산화물과 상기 금속 산화물(M1)의 함량 비율은 75 : 25 내지 90 : 10 중량비인, 산화물 소결체.According to paragraph 1,
The molybdenum oxide and metal oxide (M1) are contained in an amount of 95.0 to 99.0% by weight based on 100% by weight of the oxide sintered body,
The content ratio of the molybdenum oxide and the metal oxide (M1) is 75:25 to 90:10 by weight.
비저항이 1×10-2 Ωcm 이하이며,
상대밀도가 95% 이상인, 산화물 소결체.According to paragraph 1,
The specific resistance is less than 1×10 -2 Ωcm,
Oxide sintered body with a relative density of 95% or more.
350℃의 온도 및 30분 이상의 열처리 후 하기 식 1에 따른 광 반사율 변화율(ΔR)이 30% 이하인, 산화물 박막:
[식 1]
광 반사율 변화율(ΔR, %) = (R2 - R1)/R1 ×100
상기 식에서,
R1은 열처리 전 550nm 파장에 대한 박막의 광 반사율이고,
R2는 열처리 후 550nm 파장에 대한 박막의 광 반사율이다. According to clause 6,
An oxide thin film having a light reflectance change rate (ΔR) of 30% or less according to Equation 1 below after heat treatment at a temperature of 350°C and for more than 30 minutes:
[Equation 1]
Light reflectance change rate (ΔR, %) = (R 2 - R 1 )/R 1 × 100
In the above equation,
R 1 is the optical reflectance of the thin film for a wavelength of 550 nm before heat treatment,
R 2 is the light reflectance of the thin film for a wavelength of 550 nm after heat treatment.
열처리 전 550nm 파장에 대한 광 반사율(R1)은 10.5% 이하이며,
350℃ 온도 및 30분 이상의 열처리 후 550nm 파장에 대한 광 반사율(R2)은 12.5% 이하인, 산화물 박막. According to clause 6,
The optical reflectance (R 1 ) for the 550 nm wavelength before heat treatment is 10.5% or less,
An oxide thin film having a light reflectance (R 2 ) of 12.5% or less for a wavelength of 550 nm after heat treatment at a temperature of 350° C. and for more than 30 minutes.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
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| KR1020210124217A KR102646917B1 (en) | 2021-09-16 | 2021-09-16 | Molybdenum oxide based sintered body, metal oxide thin film using the sintered body, and thin film transistors and displa devices comprising the thin films |
| TW111134818A TW202313520A (en) | 2021-09-16 | 2022-09-15 | Molybdenum oxide based sintered body, sputtering target, oxide thin film using the sintered body, and thin film transistors and display devices including the thin films |
| CN202211128996.5A CN115819083B (en) | 2021-09-16 | 2022-09-16 | Molybdenum oxide-based sintered body, thin film using the sintered body, thin film transistor including the thin film, and display device |
| KR1020240032499A KR20240038936A (en) | 2021-09-16 | 2024-03-07 | Molybdenum oxide based sintered body, metal oxide thin film using the sintered body, and thin film transistors and displa devices comprising the thin films |
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| KR1020240032499A KR20240038936A (en) | 2021-09-16 | 2024-03-07 | Molybdenum oxide based sintered body, metal oxide thin film using the sintered body, and thin film transistors and displa devices comprising the thin films |
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| JP2005256175A (en) | 2005-04-27 | 2005-09-22 | Asahi Glass Ceramics Co Ltd | Target and method of producing high refractive index film by the target |
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| CN1918672B (en) * | 2004-03-09 | 2012-10-03 | 出光兴产株式会社 | Thin film transistor, thin film transistor substrate, liquid crystal display device, sputtering target, transparent conductive film, transparent electrode, and method for producing same |
| US20070071985A1 (en) | 2005-09-29 | 2007-03-29 | Prabhat Kumar | Sputtering target, low resistivity, transparent conductive film, method for producing such film and composition for use therein |
| KR101255707B1 (en) * | 2006-08-29 | 2013-04-17 | 엘지디스플레이 주식회사 | Thin Film Transistor device and method for fabricating thereof |
| JP5214194B2 (en) * | 2007-08-10 | 2013-06-19 | 住友化学株式会社 | Organic electroluminescence device including metal-doped molybdenum oxide layer and manufacturing method |
| KR20140023491A (en) * | 2012-08-16 | 2014-02-27 | 삼성코닝정밀소재 주식회사 | Sputtering target and organic light emitting diode display device including black matrix deposited by the same |
| CN104649664A (en) * | 2013-11-21 | 2015-05-27 | 青岛润鑫伟业科贸有限公司 | Molybdenum dioxide conductive ceramic material |
| EP3467140A1 (en) * | 2017-10-06 | 2019-04-10 | Plansee SE | Target material for deposition of molybdenum oxide layers |
| WO2019176552A1 (en) * | 2018-03-13 | 2019-09-19 | Ｊｘ金属株式会社 | Oxide thin film, and oxide sintered body for sputtering target for producing oxide thin film |
| KR20200020855A (en) * | 2018-08-09 | 2020-02-26 | 제이엑스금속주식회사 | Oxide thin film formed using the oxide sputtering target, its manufacturing method, and this oxide sputtering target |
| EP3715496A1 (en) * | 2019-03-29 | 2020-09-30 | Plansee SE | Sputtering target for producing layers containing molybdenum oxide |
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| TW202313520A (en) | 2023-04-01 |
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| KR20240038936A (en) | 2024-03-26 |
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