KR20030058595A - Method for forming a film - Google Patents
Method for forming a film Download PDFInfo
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- KR20030058595A KR20030058595A KR1020010089109A KR20010089109A KR20030058595A KR 20030058595 A KR20030058595 A KR 20030058595A KR 1020010089109 A KR1020010089109 A KR 1020010089109A KR 20010089109 A KR20010089109 A KR 20010089109A KR 20030058595 A KR20030058595 A KR 20030058595A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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Abstract
Description
본 발명은 박막 형성 방법에 관한 것으로, 특히 단원자막 증착법을 사용하여 12-16족 박막을 증착하므로 소자의 수율 및 신뢰성을 향상시키는 박막 형성 방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thin film formation method, and more particularly, to a thin film formation method for improving yield and reliability of devices by depositing a group 12-16 thin film using a single-subject film deposition method.
12-16족 박막은 와이드 밴드갭(Wide bandgap) 특성으로 인해 LED(LightEmitting Diode), LD(Laser Diode) 등에 사용되고 또한 압전 소재로도 사용된다.The thin film of group 12-16 is used for LED (Light Emitting Diode), LD (Laser Diode), etc. due to its wide bandgap characteristic, and is also used as a piezoelectric material.
[화학식 1][Formula 1]
ML2+ M'L'2→ MM' + 2LL'ML 2 + M'L ' 2 → MM' + 2LL '
상기 식에서 M은 12족 원소, M'는 16족 원소, L,L'는 수소(H), 알킬(Alkyl), 아미드(Amide) 등이다.In the above formula, M is a group 12 element, M 'is a group 16 element, and L and L' are hydrogen (H), alkyl (Alkyl), amide (Amide), and the like.
상기 화학식 1과 같이 종래에는 반응성이 높은 12족, 16족 화합물을 동시에 사용하는 화학기상 증착법에 의해 박막을 형성한다.As in Chemical Formula 1, a thin film is formed by a chemical vapor deposition method using a highly reactive Group 12 and Group 16 compound at the same time.
여기서, 상기 12족과 16족 화합물은 반응온도에서 분해 특성이 서로 다르기 때문에 한가지 원소(주로 16족 화합물)를 상대적으로 과량 사용하여 박막 내에서 2개의 원소비를 1:1로 조절하기가 어렵다.Herein, the Group 12 and Group 16 compounds have different decomposition properties at the reaction temperature, so it is difficult to control two element ratios 1: 1 in the thin film by using a relatively excessive amount of one element (mainly Group 16 compound).
또한, 상기와 같이 한가지 화합물을 과량 사용하는 겅우 리간드(ligand)에서 혼입되는 불순물의 양도 증가하게 되어 좋은 물성의 막을 얻을 수 없게 된다.In addition, as described above, the amount of impurities incorporated in ligands that use excessive amounts of one compound also increases, and thus a film having good physical properties cannot be obtained.
그리고, 증착 속도와 물성을 개선하기 위하여 반응성이 높은 화합물을 사용하는 경우 기상에서 반응할 확률이 높아 파티클(Particle)이 발생되고 기판에서 반응이 진행되어도 짧은 시간에 반응이 완료되기 때문에 탄소, 수소 등의 불순물이 함유될 가능성이 크다.In the case of using a highly reactive compound to improve the deposition rate and physical properties, there is a high probability of reaction in the gas phase, so that particles are generated and the reaction is completed in a short time even when the reaction proceeds on the substrate. Is likely to contain impurities.
그러나, 종래의 박막 형성 방법은 화학기상 증착법을 사용하여 12-16족 박막을 증착하므로 다음과 같은 이유에 의해 소자의 수율 및 신뢰성이 저하되는 문제점이 있었다.However, in the conventional thin film formation method, since the Group 12-16 thin film is deposited using chemical vapor deposition, the yield and reliability of the device are deteriorated due to the following reasons.
첫째, 12족과 16족 화합물의 물성(반응온도에서 분해 특성)이 서로 다르기 때문에 박막 내에서 2개의 원소비를 1 : 1로 조절하기 어렵다.First, since the physical properties (decomposition properties at reaction temperature) of the Group 12 and Group 16 compounds are different, it is difficult to control the two element ratios to 1: 1 in the thin film.
둘째, 12족과 16족 화합물의 물성(반응온도에서 분해 특성)이 서로 다르기 때문에 주로 16족의 한가지 원소를 상대적으로 과량 사용하기 때문에 불순물 함유량이 높은 막을 형성하게 된다.Second, since the physical properties (decomposition properties at the reaction temperature) of the Group 12 and Group 16 compounds are different, a film having a high impurity content is formed because a relatively large amount of one element of Group 16 is mainly used.
셋째, 막의 증착 속도와 물성을 개선하기 위하여 반응성이 높은 화합물을 사용하는 경우 기상에서 반응할 확률이 높아짐에 따라 파티클이 발생된다.Third, when a highly reactive compound is used to improve the deposition rate and physical properties of the film, particles are generated as the probability of reaction in the gas phase increases.
본 발명은 상기의 문제점을 해결하기 위해 안출한 것으로 단원자막 증착법을 사용하여 12-16족 박막을 증착하므로, 상기 단원자막 증착법은 화학기상 증착법보다 정확한 조성제어가 가능하고, 불순물 함유량이 낮은 막을 만들 수 있으며 또한 반응성이 높은 화합물을 사용하는 경우에도 파티클 발생을 억제하는 박막 형성 방법을 제공하는데 그 목적이 있다.The present invention has been made to solve the above problems, and since the thin film of the 12-16 group is deposited using the single-subject film deposition method, the single-subject film deposition method is capable of controlling the composition more precisely than the chemical vapor deposition method, and to produce a film having a lower impurity content. It is also an object of the present invention to provide a thin film formation method that suppresses particle generation even when using a highly reactive compound.
도 1a 내지 도 1c는 본 발명의 실시 예에 따른 박막 형성 방법을 도시한 단면도.1A to 1C are cross-sectional views illustrating a method of forming a thin film according to an embodiment of the present invention.
도 2는 본 발명의 박막 증착 시 화합물, 반응 기체 및 퍼지 기체 각각의 공급 순서도.2 is a supply flow chart of each of the compound, the reaction gas and the purge gas during the thin film deposition of the present invention.
< 도면의 주요 부분에 대한 부호의 설명 ><Description of Symbols for Main Parts of Drawings>
11: 반도체 기판13: ZnEt2 11: semiconductor substrate 13: ZnEt 2
15: 제 1 Ar17: H2O15: 1st Ar17: H 2 O
19: 박막19: thin film
이상의 목적을 달성하기 위한 본 발명은 기판이 안착된 반응기에 12족 화합물을 공급시키고 흡착시키는 단계, 상기 12족 화합물의 공급을 중단하고, 상기 반응기에 퍼지 기체를 공급하여 기상에 존재하는 화합물을 제거하는 단계, 상기 반응기에 16족 화합물을 공급시키는 단계, 상기 공급된 16족 화합물을 상기 12족 화합물과 반응시켜 12족과 16족 원소로 이루어진 박막을 형성하는 단계 및 상기 16족 화합물의 공급을 중단하고, 상기 반응기에 퍼지 기체를 공급하여 기상에 존재하는화합물을 제거하는 단계를 포함하는 박막 형성 방법을 제공하는 것과,The present invention for achieving the above object is the step of supplying and adsorbing the Group 12 compound to the reactor on which the substrate is seated, the supply of the Group 12 compound is stopped, the purge gas is supplied to the reactor to remove the compound present in the gas phase Supplying a Group 16 compound to the reactor, reacting the supplied Group 16 compound with the Group 12 compound to form a thin film made of Group 12 and Group 16 elements, and stopping supply of the Group 16 compound And supplying a purge gas to the reactor to remove the compound present in the gas phase.
상기 12족 화합물로 ML2를 사용하고 M은 Zn, Cd 및 Hg 중 선택된 하나 또는 그 이상으로 사용하고, L은 H, C1-C10알킬(alkyl), C2-C10alkenyl, C1-C8alkoxy, C6-C12aryl, β-diketonates, cyclopentadienyl, C1-C8alkylcyclopentadienyl 및 상기의 물질에 할로겐이 첨가된 유도체들 중 선택된 하나 또는 그 이상으로 사용하는 것과,ML 2 is used as the Group 12 compound, M is one or more selected from Zn, Cd, and Hg, and L is H, C 1 -C 10 alkyl, C 2 -C 10 alkenyl, C 1 Using at least one selected from -C 8 alkoxy, C 6 -C 12 aryl, β-diketonates, cyclopentadienyl, C 1 -C 8 alkylcyclopentadienyl and derivatives in which halogen is added to the above materials,
상기 12족 화합물을 100 ∼ 900℃ 온도의 기판 표면에 흡착시키는 것과,Adsorb | sucking the said Group 12 compound to the board | substrate surface of 100-900 degreeC temperature,
상기 16족 화합물로 M'L'2를 사용하고 M'은 O, S, Se 및 Te 중 선택된 하나 또는 그 이상으로 사용하고 L'은 H, C1-C10알킬(alkyl), C2-C10alkenyl, C1-C8alkoxy, C6-C12aryl, β-diketonates, cyclopentadienyl, C1-C8alkylcyclopentadienyl 및 상기의 물질에 할로겐이 첨가된 유도체들 중 선택된 하나 또는 그 이상으로 사용하는 것과,M'L ' 2 is used as the Group 16 compound, M' is used as one or more selected from O, S, Se, and Te, and L 'is H, C 1 -C 10 alkyl, C 2- One or more selected from among C 10 alkenyl, C 1 -C 8 alkoxy, C 6 -C 12 aryl, β-diketonates, cyclopentadienyl, C 1 -C 8 alkylcyclopentadienyl and halogenated derivatives And
상기 퍼지 기체로 Ar, Ne, N2및 He 중 선택된 하나 또는 그 이상으로 사용하는 것과,Using at least one selected from Ar, Ne, N 2 and He as the purge gas,
상기 12족 화합물, 16족 화합물 및 퍼지 기체 각각의 공급시간을 0.1 ∼ 5초로 하는 것을 특징으로 한다.The supply time of each of the Group 12 compound, the Group 16 compound and the purge gas is 0.1 to 5 seconds.
[화학식 2][Formula 2]
ZnR2+ H2O→ ZnO + 2HRZnR 2 + H 2 O → ZnO + 2HR
상기 식에서 R은 H, Alkyl, Amide 등이다.Wherein R is H, Alkyl, Amide and the like.
[화학식 3][Formula 3]
Zn(NR2)2+ H2O→ ZnO + 2HNR2 Zn (NR 2 ) 2 + H 2 O → ZnO + 2HNR 2
상기 식에서 M(NR2)2는 아미드 화합물이고, HNR2는 반응생성물이다.Wherein M (NR 2 ) 2 is an amide compound and HNR 2 is a reaction product.
본 발명의 원리는 원자층 증착법을 이용하여 12족과 16족 원소로 이루어진 박막을 증착하는 방법으로, 상기 Zn 화합물로 ZnR2를 사용한 화학식 2 또는 Zn 화합물로 Zn(NR2)2를 사용한 화학식 3과 같이 반응하여 ZnO막을 형성한다.The principle of the present invention is a method of depositing a thin film composed of Group 12 and Group 16 elements using atomic layer deposition, using Chemical Formula 2 using ZnR 2 as the Zn compound or Chemical Formula 3 using Zn (NR 2 ) 2 as the Zn compound. Reaction is performed to form a ZnO film.
이하, 첨부된 도면을 참조하여 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
도 1a 내지 도 1c는 본 발명의 실시 예에 따른 박막 형성 방법을 도시한 단면도이고, 도 2는 본 발명의 박막 증착 시 화합물, 반응 기체 및 퍼지 기체 각각의 공급 순서도이다.1A to 1C are cross-sectional views illustrating a method of forming a thin film according to an exemplary embodiment of the present invention, and FIG. 2 is a flow chart of supplying a compound, a reaction gas, and a purge gas, respectively, when the thin film is deposited.
도 1a 및 도 2를 참조하면, 아르곤(Ar)을 운반 기체로 사용하여 기화된 12족 화합물인 ZnEt2(13)를 반도체 기판(11)이 안착된 반응기로 공급시킨다. 이때, 상기 12족 화합물로 ML2를 사용하고 M은 Zn, Cd 및 Hg 중 선택된 하나 또는 그 이상으로 사용하고, L은 H, C1-C10알킬(alkyl), C2-C10alkenyl, C1-C8alkoxy, C6-C12aryl, β-diketonates, cyclopentadienyl, C1-C8alkylcyclopentadienyl 및 상기의 물질에 할로겐이 첨가된 유도체들 중 선택된 하나 또는 그 이상으로 사용한다.1A and 2, argon (Ar) is used as a carrier gas to supply ZnEt 2 (13), a vaporized Group 12 compound, to a reactor on which the semiconductor substrate 11 is seated. In this case, ML 2 is used as the Group 12 compound, M is one or more selected from Zn, Cd, and Hg, and L is H, C 1 -C 10 alkyl, C 2 -C 10 alkenyl, C 1 -C 8 alkoxy, C 6 -C 12 aryl, β-diketonates, cyclopentadienyl, C 1 -C 8 alkylcyclopentadienyl and halogen-added derivatives of the above materials are used as one or more.
도 1b 및 도 2를 참조하면, 100 ∼ 900℃ 온도의 상기 반도체 기판(11) 표면에 상기 ZnEt2(13)를 흡착시킨다.1B and 2, the ZnEt 2 13 is adsorbed onto the surface of the semiconductor substrate 11 at a temperature of 100 to 900 ° C.
그리고, 상기 ZnEt2(13)의 공급을 중단하고 퍼지 기체인 제 1 Ar(15)을 상기 반응기에 공급하여 상기 반도체 기판(11) 표면에 흡착된 ZnEt2(13)를 제외한 기상에 존재하는 화합물을 진공으로 제거한다.Then, the supply of the ZnEt 2 (13) is stopped and the first Ar (15), which is a purge gas, is supplied to the reactor to exist in the gas phase except for ZnEt 2 (13) adsorbed on the surface of the semiconductor substrate 11 Is removed by vacuum.
이어, 반응 기체로 16족 화합물인 H2O(17)를 상기 반응기에 공급시킨다. 이때, 상기 16족 화합물로 M'L'2를 사용하고 M'은 O, S, Se 및 Te 중 선택된 하나 또는 그 이상으로 사용하고 L'은 H, C1-C10알킬(alkyl), C2-C10alkenyl, C1-C8alkoxy, C6-C12aryl, β-diketonates, cyclopentadienyl, C1-C8alkylcyclopentadienyl 및 상기의 물질에 할로겐이 첨가된 유도체들 중 선택된 하나 또는 그 이상으로 사용한다.Subsequently, H 2 O (17), a Group 16 compound, is supplied to the reactor as a reaction gas. In this case, M'L ' 2 is used as the Group 16 compound, M' is used as one or more selected from O, S, Se, and Te, and L 'is H, C 1 -C 10 alkyl, C One or more of 2 -C 10 alkenyl, C 1 -C 8 alkoxy, C 6 -C 12 aryl, β-diketonates, cyclopentadienyl, C 1 -C 8 alkylcyclopentadienyl and derivatives in which halogen is added to the above materials use.
도 1c 및 도 2를 참조하면, 상기 공급된 H2O(17)를 상기 ZnEt2(13)와 반응시켜 12족과 16족 원소로 이루어진 박막(19)을 형성한다.1C and 2, the supplied H 2 O 17 is reacted with the ZnEt 2 13 to form a thin film 19 made of group 12 and group 16 elements.
그리고, 상기 H2O(17)의 공급을 중단하고, 퍼지 기체인 제 2 Ar(21)을 상기 반응기에 공급하여 반응 생성물 및 반응하지 않은 상기 H2O(17)를 제거한다.Then, the supply of the H 2 O (17) is stopped, and a second Ar (21), which is a purge gas, is supplied to the reactor to remove the reaction product and the unreacted H 2 O (17).
여기서, 상술한 본 발명의 공정 단계 즉 12족 화합물→퍼지 기체→16족 화합물→퍼지 기체 또는 12족 화합물→퍼지 기체→반응촉매기체→퍼지 기체→16족 화합물→퍼지 기체를 하나의 사이클(Cycle)로 각각의 공급시간을 0.1 ∼ 5초로 하여 반복하여 실행하므로 소정 두께의 박막을 증착시킬 수 있다. 그리고 상기 퍼지 기체로 Ar, Ne, N2및 He 중 선택된 하나 또는 그 이상으로 사용한다.Here, the above-described process steps of the present invention, that is, the group 12 compound → purge gas → group 16 compound → purge gas or group 12 compound → purge gas → reaction catalyst gas → purge gas → group 16 compound → purge gas in one cycle (Cycle) Each supply time is repeated from 0.1 to 5 seconds so that a thin film of a predetermined thickness can be deposited. And used as one or more selected from Ar, Ne, N 2, and He as the purge gas.
또한, 상기 반응촉매기체로 H2, NH3, NH2R, NHR2, NR3, hydrazine, C1-C10alkylhydrazine, C1-C10dialkylhydrazine 또는 이들의 혼합기체를 사용하고 R은 H, C1-C10alkyl, C2-C10alkenyl, C1-C8alkoxy, C6-C12aryl 및 상기의 물질에 할로겐이 첨가된 유도체들 중 선택된 하나 또는 그 이상이다.In addition, H 2, the catalyst in the reaction gas NH 3, NH 2 R, NHR 2, NR 3, hydrazine, C 1 -C 10 alkylhydrazine, C 1 -C 10 dialkylhydrazine or using a mixed gas, and R is H, One or more selected from among C 1 -C 10 alkyl, C 2 -C 10 alkenyl, C 1 -C 8 alkoxy, C 6 -C 12 aryl, and derivatives in which halogen is added to the above materials.
본 발명의 박막 형성 방법은 단원자막 증착법을 사용하여 12-16족 박막을 증착하므로 다음과 같은 이유에 의해 소자의 수율 및 신뢰성을 향상시키는 특징이 있다.Since the thin film forming method of the present invention deposits a group 12-16 thin film using the single-subject film deposition method, there is a feature to improve the yield and reliability of the device for the following reasons.
첫째, 단원자막 증착법은 화학기상 증착법보다 정확한 조성제어가 가능하기 때문에 12족과 16족 원소비를 1 : 1로 조절하기 용이하다.First, since the single-subject film deposition method enables more accurate composition control than the chemical vapor deposition method, it is easy to adjust the element ratio of group 12 and group 16 to 1: 1.
둘쩨, 한가지 원소를 과량 사용하지 않아도 되기 때문에 불순물 함유량이 낮은 막을 형성한다.Secondly, since one element does not have to be used in excess, a film with low impurity content is formed.
셋째, 각각의 화합물을 각각 넣어주기 때문에 반응성이 높은 화합물을 사용하는 경우에도 파티클 발생을 억제한다.Third, since each compound is added to each other, even when using highly reactive compounds, particle generation is suppressed.
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US4058430A (en) * | 1974-11-29 | 1977-11-15 | Tuomo Suntola | Method for producing compound thin films |
US4389973A (en) * | 1980-03-18 | 1983-06-28 | Oy Lohja Ab | Apparatus for performing growth of compound thin films |
KR100273473B1 (en) * | 1999-04-06 | 2000-11-15 | 이경수 | Method for forming a thin film |
KR20010098618A (en) * | 2000-04-14 | 2001-11-08 | 추후제출 | Method of growing a thin film onto a substrate |
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US4058430A (en) * | 1974-11-29 | 1977-11-15 | Tuomo Suntola | Method for producing compound thin films |
US4389973A (en) * | 1980-03-18 | 1983-06-28 | Oy Lohja Ab | Apparatus for performing growth of compound thin films |
KR100273473B1 (en) * | 1999-04-06 | 2000-11-15 | 이경수 | Method for forming a thin film |
KR20010098618A (en) * | 2000-04-14 | 2001-11-08 | 추후제출 | Method of growing a thin film onto a substrate |
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Publication number | Priority date | Publication date | Assignee | Title |
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US7371429B2 (en) | 2005-02-14 | 2008-05-13 | Samsung Electronics Co., Ltd. | Precursor, thin layer prepared including the precursor, method of preparing the thin layer and phase-change memory device |
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