KR20110019466A - Method of manufaturing target for pvd - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
- 229910052738 indium Inorganic materials 0.000 claims abstract description 13
- 239000008188 pellet Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052711 selenium Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 229920002994 synthetic fiber Polymers 0.000 claims description 4
- 150000003346 selenoethers Chemical class 0.000 abstract 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 abstract 2
- 239000010949 copper Substances 0.000 abstract 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract 2
- 238000005289 physical deposition Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 8
- 239000010409 thin film Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000005240 physical vapour deposition Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000001311 chemical methods and process Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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Abstract
Description
본 발명은 물리적 증착(PVD)용 타겟 제조 방법에 관한 것으로서, 보다 구체적으로는 재료가 갖고 있는 특성상 PVD용 타겟으로 제조하기가 어려운 CIS 타겟을 간단한 제조 공정 및 낮은 제조 비용으로 제조할 수 있도록 해주는 CIS 타겟 제조 방법과 관련된 것이다.The present invention relates to a method for manufacturing a target for physical vapor deposition (PVD), and more specifically, to a CIS target, which makes it difficult to manufacture a target for PVD due to the characteristics of the material, it is possible to manufacture a CIS target with a simple manufacturing process and low manufacturing cost. It relates to a target manufacturing method.
CIS(Cu-In-Se)(Cu:In:S2=1:1:2 (몰비)) 혹은 CIGS(Cu-In-Ga-Se)(Cu:In:Ga:Se=1:1-x:x:2(0<x<1)(몰비)) 계열 태양전지는 Si 태양전지에 버금가는 높은 효율과 재료에 드는 상대적으로 적은 비용 등으로 Si 태양전지를 대체할 유력한 후보로 주목받고 있다. 한편, CIS, CIGS 계열 태양전지를 구성하는 각 층 중에 빛을 흡수하는 광 흡수층이 가장 중요한 층이라 할 수 있다.CIS (Cu-In-Se) (Cu: In: S2 = 1: 1: 2 (molar ratio)) or CIGS (Cu-In-Ga-Se) (Cu: In: Ga: Se = 1: 1-x: x: 2 (0 <x <1) (molar ratio) series solar cells are attracting attention as potential candidates to replace Si solar cells due to their high efficiency and the relatively low cost of materials. Meanwhile, the light absorbing layer that absorbs light is the most important layer among the layers constituting the CIS and CIGS series solar cells.
상기 태양전지의 흡수층을 제조하는 방법에는 여러 가지가 있는데, 현재 많이 사용하고 있는 방법은 Cu, In, Ga, Se라는 개별 타겟을 이용하는 증착시키는 것이다. 즉 각각의 타겟에 레이저 또는 전자를 충돌시켜 그 힘에 의해 타겟으로부터 미량의 물질을 분리하고, 분리된 물질을 원하는 기판에 증착하는 것이다. 그러나, 여러가지 조성의 타겟을 이용하기 때문에 박막의 조성 조절이 어렵고, 균일한 형태의 막을 제조하기가 어렵다는 문제점이 있다.There are a number of methods for manufacturing the absorber layer of the solar cell, a method currently used a lot is to deposit using a separate target, such as Cu, In, Ga, Se. In other words, a laser or electron is bombarded to each target to separate a small amount of material from the target by the force, and the separated material is deposited on a desired substrate. However, there is a problem that it is difficult to control the composition of the thin film because it uses a target of various compositions, it is difficult to produce a film of a uniform form.
이와 같이, 흡수층 제조시 개별 타겟을 이용하는 이유는 CIS, CIGS 물질이 갖고 있는 본질적인 특성에 기인한다. 구체적으로, CIS, CIGS계 물질은 3가지 이상의 원자로 이루어진 화합물인데, 이 물질의 합성을 위해서는 1000℃ 이상의 고온과 고진공이 필요하다는 문제점이 있고, 생산성에 문제가 있어, 저가의 단순 공법이 필요해 상기와 같은 방법이 채용된다.As such, the reason for using individual targets in the manufacture of absorbent layers is due to the intrinsic properties of CIS and CIGS materials. Specifically, the CIS, CIGS-based material is a compound consisting of three or more atoms, there is a problem that the high temperature and high vacuum of 1000 ℃ or more is required for the synthesis of the material, there is a problem in productivity, a low cost simple method is required The same method is employed.
본 발명은 상기한 종래 기술에서 나타나는 문제점을 해결하기 위한 것으로서, 그 목적은 새로운 장비 없이 저온에서 CIS계, CIGS계 타겟을 제조할 수 있는 방법을 제공하는 것이다.The present invention is to solve the problems appearing in the prior art, the object is to provide a method for producing a CIS-based, CIGS-based target at low temperature without new equipment.
본 발명의 다른 목적은 기존의 제조 방법과 비교하여 제조 단가를 낮출 수 있고, 새로운 상을 생성하지 않으면서 박막 증착시까지 균일한 조성을 유지할 수 있는 CIS계, CIGS계 타겟 제조 방법을 제공하는 것이다.Another object of the present invention is to provide a CIS-based or CIGS-based target manufacturing method capable of lowering the manufacturing cost compared to the existing manufacturing method and maintaining a uniform composition until thin film deposition without generating a new phase.
상기 목적을 달성하기 위하여, 본 발명에 따라서 태양전지 흡수층을 증착하는 데 사용되는 CIS계 타겟 제조 방법이 제공된다. 상기 방법은 (a) Cu, In, Se 파우더를 1:1:2의 몰비로 준비하는 단계와; (b) 상기 Cu, In, Se 파우더와 금속 볼을 용기 안에 넣고 교반하여, 이 기계적 힘에 의해 CIS 합성 물질을 제조하는 단계와; (c) 상기 합성된 CIS 물질에 Se을 추가로 첨가한 후, 볼밀을 이용하여 혼합하고 압축을 가해 타겟 형태에 대응하는 형상의 펠릿으로 제조하는 단계와; (d) 상기 제조된 펠릿에 대해 열처리를 하여 최종 CIS 타겟을 제조하는 단계를 포함하는 것을 특징으로 한다.In order to achieve the above object, according to the present invention there is provided a CIS-based target manufacturing method used for depositing a solar cell absorbing layer. The method comprises the steps of (a) preparing a Cu, In, Se powder in a molar ratio of 1: 1: 2; (b) putting Cu, In, Se powder and a metal ball into a container and stirring to prepare a CIS synthetic material by this mechanical force; (c) further adding Se to the synthesized CIS material, then mixing and compressing using a ball mill to produce pellets of a shape corresponding to the target shape; (d) heat-treating the prepared pellets to produce a final CIS target.
한 가지 실시예에 있어서, 상기 (c) 단계에서 Se은 상기 (b) 단계에서 합성한 CIS 물질에 대해 약 25~50 wt%의 비율로 추가 첨가될 수 있고, 바람직하게는 약 50 wt%의 비율로 추가 첨가될 수 있다.In one embodiment, in step (c) Se may be further added in a ratio of about 25 to 50 wt% with respect to the CIS material synthesized in step (b), preferably about 50 wt% It may be added in proportion.
한 가지 실시예에 있어서, 상기 (d) 단계에서 상기 열처리는 약 300℃의 온도 및 대기압 중에서 수행할 수 있다.In one embodiment, the heat treatment in step (d) may be performed at a temperature of about 300 ℃ and atmospheric pressure.
본 발명의 또 다른 실시예에 따라서, 태양전지 흡수층을 증착하는 데 사용되는 CIGS계 타겟 제조 방법도 제공된다. 상기 방법은 (a) Cu, In, Ga, Se 파우더를 1:1:1:2의 몰비로 준비하는 단계와; (b) 상기 Cu, In, Ga, Se 파우더와 금속 볼을 용기 안에 넣고 교반하여, 이 기계적 힘에 의해 CIGS 합성 물질을 제조하는 단계와; (c) 상기 합성된 CIGS 물질에 Se을 추가로 첨가한 후, 볼밀을 이용하여 혼합하고 압축을 가해 타겟 형태에 대응하는 형상의 펠릿으로 제조하는 단계와; (d) 상기 제조된 펠릿에 대해 열처리를 하여 최종 CIGS 타겟을 제조하는 단계를 포함하는 것을 특징으로 한다.According to another embodiment of the present invention, there is also provided a CIGS-based target manufacturing method used to deposit a solar cell absorbing layer. The method comprises the steps of: (a) preparing a Cu, In, Ga, Se powder in a molar ratio of 1: 1: 1: 2; (b) putting Cu, In, Ga, Se powder and metal balls into a container and stirring to prepare a CIGS synthetic material by this mechanical force; (c) further adding Se to the synthesized CIGS material, then mixing and compressing using a ball mill to produce pellets of a shape corresponding to the target shape; (d) heat-treating the prepared pellets to produce a final CIGS target.
본 발명에 따른 CIS계, CIGS계 타겟 제조 방법에 따르면, 종래 기술과 비교하여 저온 공정으로 경질의 CIS 및 CIGS 타겟을 제조할 수 있다. 또한, 높은 압력이나 고진공도 필요하지 않으므로 비용절감을 효과를 기대할 수 있으며, 그 제조 공정도 매우 단순하다는 이점이 있다.According to the CIS-based or CIGS-based target manufacturing method according to the present invention, it is possible to produce a hard CIS and CIGS target by a low temperature process compared to the prior art. In addition, since high pressure or high vacuum is not required, cost reduction can be expected, and the manufacturing process is also very simple.
이하에서는 첨부 도면을 참조하여 본 발명의 바람직한 실시예를 설명한다. 이하의 설명에 있어서, 태양전지 등과 같이 일반적으로 널리 알려진 구성에 대한 설명은 생략한다. 이러한 설명을 생략하더라도, 당업자라면 이하의 설명을 통해 본 발명의 특징을 아무런 어려움 없이 이해할 수 있을 것이다.Hereinafter, with reference to the accompanying drawings will be described a preferred embodiment of the present invention. In the following description, a description of a generally known configuration such as a solar cell is omitted. Even if this description is omitted, those skilled in the art will be able to understand the features of the present invention without any difficulty through the following description.
본 발명자는 CIS계, CIGS계 태양전지를 제조하는 프로세스 중 태양전지의 핵심층인 광 흡수층을 CIS계, CIGS계 물질로 형성하는 방법에 대해 연구를 하였다. 종래 기술에서 설명한 바와 같이, CIS계, CIGS계 물질은 그 자체의 특성으로 인해 저온, 상압에서는 단단한 타겟으로 제조하기가 어려운데, 이를 해결하기 위해 독특한 조성을 고안하여 CIS계, CIGS계 타겟 제조에 성공하였다.The present inventors studied a method of forming a light absorbing layer, which is a core layer of a solar cell, of a CIS-based or CIGS-based solar cell, using a CIS-based or CIGS-based material. As described in the prior art, CIS-based and CIGS-based materials are difficult to be manufactured as solid targets at low temperatures and atmospheric pressures due to their characteristics. To solve this problem, CIS and CIGS-based targets have been successfully manufactured. .
먼저, mechano chemical process라고 하는 널리 알려진 방법을 이용하여 CIS 물질을 합성하였다. 즉 Cu, In, Se 물질을 미리 정해진 몰비(1:1:2)에 맞게 준비한 후, zirconia 볼과 함께 용기 안에 넣은 후, 강한 힘으로 교반하였다. 이러한 교반에 의해, 볼이 각 파우더와 충돌하게 되고, 물질에 에너지가 계속 쌓이게 되어, 기계적인 힘이 화학적인 에너지로 변환되어, CIS 물질이 합성된다. 이 과정에서, Cu, In, Se 물질이 상기 볼과의 충돌에 의해 계속 분할되면서, 표면적이 넓어지게 되어, 큰 힘을 들이지 않고도 합성이 가능하다. 이러한 mechano chemical process는 상온 및 상압에서 수행하였다.First, CIS materials were synthesized using a well-known method called mechano chemical process. That is, Cu, In, Se material was prepared in accordance with a predetermined molar ratio (1: 1: 2), and then placed in a container with zirconia balls, and stirred with a strong force. By this agitation, the balls collide with each powder, and energy continues to accumulate in the material, and mechanical forces are converted into chemical energy, thereby synthesizing the CIS material. In this process, Cu, In, Se material is continuously divided by the collision with the ball, the surface area is widened, it is possible to synthesize without a large force. This mechano chemical process was performed at room temperature and atmospheric pressure.
상기 과정에 따라 합성한 CIS 재료에 대한 XRD 패턴을 도 1에 도시하였다. 도 1에 도시한 바와 같이, CIS 단일 상이 상온, 상압 중에서 제조할 수 있다는 것 을 확인할 수 있다.XRD pattern for the CIS material synthesized according to the above process is shown in FIG. As shown in Figure 1, it can be seen that the CIS single phase can be prepared at room temperature and atmospheric pressure.
본 발명자는 상기 과정에 따라 만들어진 CIS 물질을 이용하여 CIS 타겟을 제작하였다. 즉 CIS 타겟은 경질의 디스크 형태인데, 상기 과정에 따라 만들어진 CIS 물질은 파우더 형태이다. 이러한 CIS 물질은 경질의 CIS 타겟 형태로 제조하기 위해서는 높은 온도와 고진공이 필요하지만, 본 발명자는 이러한 고가의 제조 프로세스가 아닌 단순화된 방법을 통해 CIS 타겟을 제조하였다.The inventor produced a CIS target using the CIS material made according to the above procedure. That is, the CIS target is in the form of a hard disk, and the CIS material made according to the above process is in the form of a powder. While such CIS materials require high temperatures and high vacuum to produce hard CIS target forms, we have prepared CIS targets through a simplified method rather than this expensive manufacturing process.
구체적으로, 본 발명자는 CIS계 물질을 구성하는 원소 중 Se 물질을 추가로 첨가하여 보았다. 구체적으로 상기 과정을 통해 제작한 CIS 물질에 과량의 Se를 (a)50 wt%, (b)33 wt%, (c)25 wt%, (d) 0 wt%씩 첨가한 뒤, 각각의 혼합물을 2시간 동안 볼밀(ball mill)을 통해 혼합한 뒤에 프레스 기를 통해 가압하여 펠릿(pellet) 형태로 제조한 후, 이 펠릿을 300℃에서 1시간 동안 질소 분위기에서 열처리를 하여 단단한 CIS 타겟을 제조할 수 있었다. 즉 Se은 217℃에서 용융될 정도로 그 융점이 매우 낮다. 이와 관련하여, 본 발명에서는 300℃ 정도로 열처리를 수행하는데, 이 온도에서 Se이 녹아 충분한 유동성을 가져 CIS 물질의 입자들 사이를 연결시켜 주기 때문에, 단단한 CIS 타겟을 제조할 수가 있다. Specifically, the present inventors further added Se material among the elements constituting the CIS-based material. Specifically, an excess of Se was added to the CIS material prepared through the above process (a) 50 wt%, (b) 33 wt%, (c) 25 wt%, and (d) 0 wt%, and then each mixture was added. After mixing through a ball mill (ball mill) for 2 hours and pressurized through a press to produce a pellet (pellet) form, the pellet is heat-treated in nitrogen atmosphere for 1 hour at 300 ℃ to produce a solid CIS target Could. That is, the melting point of Se is so low that it melts at 217 ° C. In this regard, in the present invention, the heat treatment is performed at about 300 ° C. At this temperature, Se melts and has sufficient fluidity to connect the particles of the CIS material, thereby making it possible to manufacture a rigid CIS target.
본 발명자는 상기와 같은 과정을 통해 제작한 CIS 타겟의 결정구조에 대해 XRD 분석을 수행하였으며, 그 결과를 도 2에 나타낸다. 도 2에서 보는 바와 같이, CIS의 피크(peak) 위치는 Se의 첨가에도 불구하고 변치 않았으며, 이는 첨가한 Se가 CIS 물질과 반응하지 않았다는 것을 의미하며, 또한 열처리 온도가 300℃ 정도로 낮기 때문에 새로운 상도 생성되지 않았다는 것을 알 수 있다.The present inventors performed XRD analysis on the crystal structure of the CIS target produced through the above process, and the results are shown in FIG. 2. As shown in Figure 2, the peak position of the CIS did not change despite the addition of Se, which means that the added Se did not react with the CIS material, and also because the heat treatment temperature was as low as 300 ° C It can be seen that no phase was generated.
한편, 도 3은 CIS 물질에 과량의 Se을 각각 (a) 0wt%, (b) 25 wt%, (c) 33 wt%, (d) 50 wt%씩 첨가한 후, 가압하여 타겟 형태로 만든 후 300℃에서 1시간 동안 열처리 한 다음 그 미세구조를 관찰한 사진이다. 도 3에서 볼 수 있는 바와 같이, 과량의 Se이 첨가되지 않은 경우, 기공이 많은 미세구조가 관찰되었지만, 과량의 Se이 50 wt% 첨가된 타겟의 미세구조에는 기공이 거의 없었다. 즉 Se을 약 50 wt% 과량 첨가한 경우, 가장 양호한 PVD용 CIS계 타겟을 제조할 수 있다.On the other hand, Figure 3 is added to the CIS material in excess of Se (a) 0wt%, (b) 25 wt%, (c) 33 wt%, (d) 50 wt%, respectively, and then pressurized to make a target form After the heat treatment for 1 hour at 300 ℃ is a photo observing the microstructure. As can be seen in FIG. 3, when excess Se was not added, micropores with many pores were observed, but there were almost no pores in the microstructure of the target to which 50 wt% of Se was added. That is, when Se is added in an excess of about 50 wt%, the best CIS target for PVD can be prepared.
마지막으로, 본 발명자는 Se이 첨가된 타겟 중 가장 밀도가 좋았던 타겟, 즉 50 wt%의 Se이 과량 첨가된 타겟을 이용하여 PVD 공정을 통해 CIS 박막을 증착하였다. 그 증착된 박막에 대해 XRD 분석을 수행하였으며, 그 결과를 도 4에 나타내었다. 도 4에서 볼 수 있는 바와 같이, 타겟의 XRD 패턴에서는 Se이 검출되었으나(도 2 참조), 박막을 증착시킨 후에는 Se이 관찰되지 않았다. 즉 Se은 그 융점이나 기화 온도가 낮아 PVD를 이용하여 증착하는 동안 충분히 기화되어, 박막에 Se이 포함되지 않은 것으로 추측된다. 따라서, 상기한 본 발명에 따라 제작한 CIS계 타겟을 이용하여 박막을 증착할 경우, CIS 단일 상을 얻을 수 있다.Finally, the inventors deposited the CIS thin film through the PVD process using the most dense target among Se-added targets, that is, a target added with 50 wt% Se. XRD analysis was performed on the deposited thin film, and the results are shown in FIG. 4. As can be seen in FIG. 4, Se was detected in the XRD pattern of the target (see FIG. 2), but Se was not observed after the thin film was deposited. That is, Se has a low melting point or vaporization temperature and is sufficiently vaporized during deposition using PVD, and it is presumed that Se is not included in the thin film. Therefore, when the thin film is deposited using the CIS-based target prepared according to the present invention described above, a CIS single phase can be obtained.
상기 실시예는 CIS 타겟을 제조하는 것과 관련된 것이다. 그러나, 본 발명은 CIGS계 타겟을 제조하는 데에도 적용될 수 있으며, 이때에도 CIS 타겟 제조와 동일한 프로세스를 통해, CIGS계 타겟을 제조할 수 있으며, 이 역시 본 발명의 범위 내에 속하는 것이다. 즉 본 발명은 상기 실시예에 제한되는 것이 아니라, 특허청구범위 내에서 다양하게 변형 및 수정할 수 있으며, 이들 역시 본 발명의 범위에 속하는 것이다. 따라서, 본 발명은 특허청구범위 및 그 균등물에 의해서만 제한된다.This embodiment relates to manufacturing a CIS target. However, the present invention can be applied to manufacturing a CIGS-based target, and in this case, it is possible to produce a CIGS-based target through the same process as manufacturing a CIS target, which is also within the scope of the present invention. That is, the present invention is not limited to the above embodiments, but may be variously modified and modified within the scope of the claims, and these are also within the scope of the present invention. Accordingly, the invention is limited only by the claims and the equivalents thereof.
도 1은 Mechano chemical process를 통해 제조한 CIS 물질의 XRD 패턴을 보여준다.Figure 1 shows the XRD pattern of the CIS material prepared through the Mechano chemical process.
도 2는 도 1의 CIS 물질에 과량의 Se를 혼합한 물질을 약 300℃에서 1시간 동안 열처리한 후의 XRD 패턴을 보여주는 도면이다.FIG. 2 is a view showing an XRD pattern after heat-treating a material in which an excess of Se is mixed with the CIS material of FIG. 1 at about 300 ° C. for 1 hour.
도 3은 도2의 혼합 물질의 미세구조를 보여주는 현미경 사진이다.3 is a micrograph showing the microstructure of the mixed material of FIG.
도 4는 50 wt%의 과량 Se이 첨가된 타겟을 이용하여 박막을 증착한 후 박막의 XRD 패턴을 보여주는 도면이다.4 is a diagram showing an XRD pattern of a thin film after depositing a thin film using a target to which an excess of Se of 50 wt% is added.
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