KR102311985B1 - Ion scavenger for solar cell, encapsulant composition for solar cell comprising same, and solar cell module - Google Patents
Ion scavenger for solar cell, encapsulant composition for solar cell comprising same, and solar cell module Download PDFInfo
- Publication number
- KR102311985B1 KR102311985B1 KR1020187029975A KR20187029975A KR102311985B1 KR 102311985 B1 KR102311985 B1 KR 102311985B1 KR 1020187029975 A KR1020187029975 A KR 1020187029975A KR 20187029975 A KR20187029975 A KR 20187029975A KR 102311985 B1 KR102311985 B1 KR 102311985B1
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- KR
- South Korea
- Prior art keywords
- ion
- substituted
- solar cell
- solar cells
- zirconium phosphate
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- 239000000203 mixture Substances 0.000 title claims description 31
- 239000008393 encapsulating agent Substances 0.000 title description 4
- 239000002516 radical scavenger Substances 0.000 title description 3
- 150000002500 ions Chemical class 0.000 claims abstract description 152
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 118
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims abstract description 97
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 23
- -1 cesium ions Chemical class 0.000 claims abstract description 22
- 229910001414 potassium ion Inorganic materials 0.000 claims abstract description 19
- 238000005342 ion exchange Methods 0.000 claims abstract description 17
- 229910001419 rubidium ion Inorganic materials 0.000 claims abstract description 17
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 16
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- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 16
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims abstract description 11
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 0.000 claims abstract description 10
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- SUXIKHBBPQWLHO-UHFFFAOYSA-N trihydroxy-(8-methylnonyl)-(8-methyl-1-phenylnonyl)-lambda5-phosphane Chemical compound CC(C)CCCCCCCP(O)(O)(O)C(CCCCCCC(C)C)C1=CC=CC=C1 SUXIKHBBPQWLHO-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
본 발명의 태양 전지용 이온 포착제는, (A) 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온 (a1)으로 치환된 α-인산지르코늄, 및 (B) 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온 (b1)으로 치환된 α-인산티타늄 중 적어도 한쪽을 함유한다.In the ion trapping agent for solar cells of the present invention, (A) at least a part of ion exchange groups are substituted with at least one ion (a1) selected from lithium ions, potassium ions, cesium ions, rubidium ions, magnesium ions and calcium ions. - at least of zirconium phosphate and (B) α-titanium phosphate in which at least a part of the ion exchange group is substituted with at least one ion (b1) selected from lithium ion, potassium ion, cesium ion, rubidium ion, magnesium ion and calcium ion. contains one
Description
본 발명은, 태양 전지의 PID(Potential Induced Degradation)의 원인이 되는 Na+ 이온을 고선택적으로 흡착하여, 내PID성이 우수한 태양 전지를 부여하는 태양 전지용 이온 포착제 및 그것을 포함하는 태양 전지용 밀봉제 조성물 그리고 태양 전지 모듈에 관한 것이다. The present invention provides an ion trapping agent for a solar cell that highly selectively adsorbs Na + ions that cause PID (Potential Induced Degradation) of a solar cell to provide a solar cell with excellent PID resistance, and a solar cell encapsulant comprising the same composition and to a solar cell module.
환경 문제에 대한 의식의 고조로부터, 클린 에너지원으로서의 태양 전지가 이용되고 있다. 일반적으로, 태양 전지는, 복수의 태양 전지 모듈을 구비하는 복합체이며, 이 태양 전지 모듈은, 표면측 투명 보호 부재와, 태양 전지 소자가 밀봉된 층과, 이면측 보호 부재(백 시트)를 구비하는 구조를 갖고 있다.BACKGROUND ART Solar cells as a clean energy source are being used from a growing awareness of environmental issues. In general, a solar cell is a composite including a plurality of solar cell modules, and the solar cell module includes a front-side transparent protective member, a layer in which the solar cell element is sealed, and a back-side protective member (back sheet). has a structure that
근년, 다수의 결정 실리콘 태양 전지 모듈을 넓은 부지에 설치하여, 전력 사업용의 태양광 발전 시스템을 구축하는 메가 솔라라고 불리는 대규모의 태양광 발전 시스템이 급증하고 있다. 이러한 대규모의 태양광 발전 시스템에 있어서는, 태양 전지 모듈 간의 배선 공사의 간소화, 배선 개수나 접속 상자의 삭감에 의한 비용 저감을 위해, 태양 전지 모듈을 다수 직렬 접속하여, 최대 시스템 전압을 600V 내지 1000V 정도로 높게 설계하는 경우가 많다. 그러나, 이와 같은 시스템 전압이 높은 결정 실리콘 태양광 발전 시스템에 있어서는, 결정 실리콘 태양 전지 모듈에 PID라고 불리는 급격한 특성 저하 현상이 발생하는 경우가 있다.In recent years, large-scale photovoltaic power generation systems called mega solar, which install a large number of crystalline silicon solar cell modules on a large site to construct a photovoltaic power generation system for electric power business, are rapidly increasing. In such a large-scale photovoltaic power generation system, in order to simplify wiring work between solar cell modules and reduce costs by reducing the number of wirings and junction boxes, a large number of solar cell modules are connected in series, and the maximum system voltage is about 600V to 1000V. They are often designed high. However, in a crystalline silicon photovoltaic power generation system having such a high system voltage, the crystalline silicon solar cell module may experience a sudden deterioration in characteristics called PID.
이러한 결정 실리콘 태양 전지 모듈의 PID 현상에 대해서는, 아직 충분히 원인이나 발생 기구가 해명되어 있지는 않다. 그러나, PID 현상은, 태양 전지 모듈에 높은 시스템 전압이 가해지고, 또한 고온 또는 고습 상태가 되었을 때 발생 및 진행되기 쉬우며, 또한 태양 전지 모듈에 역방향의 고전압을 인가함으로써 특성이 회복되는 것이 보고되어 있다.About the PID phenomenon of such a crystalline silicon solar cell module, the cause and generation|occurrence|production mechanism are not fully elucidated yet. However, the PID phenomenon tends to occur and proceed when a high system voltage is applied to the solar cell module and becomes a high temperature or high humidity state, and it has been reported that the characteristic is recovered by applying a high voltage in the reverse direction to the solar cell module. have.
이하, 일반적인 P형 웨이퍼를 사용하여 구성된 결정 실리콘 태양 전지 셀을 사용한 결정 실리콘 태양 전지 모듈에 있어서 PID 현상이 발생하는 기구에 대하여 설명한다. 결정 실리콘 태양 전지 모듈의 표면은, 통상, 소다석회 유리를 포함하는 커버 유리로 덮여 있다. 여기서, 커버 유리 표면에 수분이 있으면, 소다석회 유리로부터 금속 이온인 나트륨 이온(Na+ 이온)을 발생한다. 결정 실리콘 태양 전지 모듈의 커버 유리는, 금속 프레임으로 지지되고, 금속 프레임은 접지에 접속되어서 접지 전위가 되고 있다.Hereinafter, a mechanism in which the PID phenomenon occurs in a crystalline silicon solar cell module using a crystalline silicon solar cell configured using a general P-type wafer will be described. The surface of a crystalline silicon solar cell module is normally covered with the cover glass containing soda-lime glass. Here, when there is moisture on the surface of the cover glass, sodium ions (Na + ions), which are metal ions, are generated from the soda-lime glass. The cover glass of the crystalline silicon solar cell module is supported by a metal frame, and the metal frame is connected to the ground and has a ground potential.
이러한 상태에서 결정 실리콘 태양 전지 모듈의 내부 배선에 부(負)의 시스템 전압이 가해지면, 결정 실리콘 태양 전지 모듈의 내외에서 큰 전위차가 발생한다. 커버 유리의 표면 Na+ 이온(금속 이온)은 이 전위차에 의해 커버 유리 중이나 밀봉 충전 수지 중을 이동하여, 결정 실리콘 태양 전지 셀의 표면에 도달한다. 고온 고습의 조건에서는 커버 유리나 밀봉 수지의 체적 저항이 저하되고, 누설 전류가 증가하여, Na+ 이온(금속 이온)이 이동하기 쉬워진다.In this state, when a negative system voltage is applied to the internal wiring of the crystalline silicon solar cell module, a large potential difference occurs inside and outside the crystalline silicon solar cell module. Surface Na + ions (metal ions) of the cover glass move in the cover glass or in the sealing filling resin by this potential difference, and reach the surface of the crystalline silicon solar cell. On the conditions of high temperature, high humidity, the volume resistance of a cover glass and sealing resin falls, a leakage current increases, and Na + ion (metal ion) becomes easy to move.
통상, 결정 실리콘 태양 전지 셀의 광 입사측의 도프층(N형)의 표면은, 절연성의 패시베이션막으로 덮여 있다. 이 패시베이션막은, 대전 이온이 부착함으로써 분극한다. 이에 의해, 결정 실리콘 태양 전지 셀의 광 입사측의 도프층(N형)의 패시베이션층과의 계면 근방에 극성 역전 영역(P형)이 형성되고, 광 발생 캐리어의 이동을 방해할 수 있어, 셀 특성이 저하된다.Usually, the surface of the doped layer (N-type) on the light-incidence side of a crystalline silicon solar cell is covered with the insulating passivation film. This passivation film is polarized by the attachment of charged ions. Thereby, a polarity reversal region (P-type) is formed in the vicinity of the interface with the passivation layer of the doped layer (N-type) on the light-incident side of the crystalline silicon solar cell, and the movement of light-generated carriers can be hindered, and the cell characteristics are reduced.
이러한 PID 현상의 발생을 방지하는 방법으로서, 지금까지 몇 가지의 방법이 제안되고 있다. 예를 들어 태양광 발전 시스템에서의 대응 방법으로서는, 절연 트랜스가 딸린 인버터를 사용하고, 인버터 입력의 부극을 접지하거나 하여 태양 전지 모듈의 내부가 외부에 대해 부의 전위가 되지 않도록 하는 방법이 알려져 있다. 그러나, 근년, 인버터의 고효율화나 비용 절감을 위해 트랜스리스화가 진행되고 있어, 이러한 시스템에서의 대응은 곤란해지고 있다.As a method of preventing the occurrence of such a PID phenomenon, several methods have been proposed so far. For example, as a countermeasure method in a photovoltaic system, the method of using an inverter with an insulation transformer and grounding the negative electrode of an inverter input so that the inside of a solar cell module does not become a negative potential with respect to the outside is known. However, in recent years, trans-lease is progressing for efficiency improvement and cost reduction of inverters, and it is difficult to cope with such a system.
한편, 태양 전지 모듈에서의 대응 방법으로서, 특허문헌 1에는, EVA를 사용하여 태양 전지 셀이 밀봉된 태양 전지 모듈에 있어서, 태양 전지 모듈의 내부로의 수증기의 침입을 방지하기 위해, EVA 수지의 태양 전지 셀과 반대측에 아이오노머 수지층을 설치하는 구조가 개시되어 있다.On the other hand, as a corresponding method in a solar cell module, in patent document 1, in the solar cell module in which the solar cell was sealed using EVA, in order to prevent penetration of water vapor|steam into the inside of a solar cell module, EVA resin A structure in which an ionomer resin layer is provided on the opposite side to the solar cell is disclosed.
또한, PID 현상의 개선을 직접의 목적으로는 하고 있지 않지만, 밀봉재의 체적 저항률을 증가시키는 검토가 이루어져 있다. 특허문헌 2에는, 규소 원자에 직접 결합하는 관능기의 탄소 원자수가 4 이하인 실란 커플링제가, 에틸렌·아세트산비닐 공중합체 100중량부에 대하여 5중량부 이하의 비율로 첨가된 태양 전지 밀봉재가 개시되어 있다. 또한, 특허문헌 3에는, 에틸렌에서 유래되는 구조 단위와, 불포화 에스테르에서 유래되는 구조 단위를 갖고, 에틸렌에서 유래되는 구조 단위와 불포화 에스테르에서 유래되는 구조 단위의 총합을 100질량％로 할 때, 불포화 에스테르에서 유래되는 구조 단위의 양이 20 내지 35질량％인 에틸렌-불포화 에스테르 공중합체 100질량부에 대하여, 메타 카올린을 0.001 내지 5질량부 함유하는 수지 조성물을 사용하여 얻어진 태양 전지용 밀봉재가 개시되어 있다.Moreover, although the improvement of a PID phenomenon is not made into the objective directly, the examination which increases the volume resistivity of a sealing material is made|formed. Patent Document 2 discloses a solar cell sealing material in which a silane coupling agent having 4 or less carbon atoms in a functional group directly bonded to a silicon atom is added in a ratio of 5 parts by weight or less with respect to 100 parts by weight of the ethylene/vinyl acetate copolymer. . In Patent Document 3, it has a structural unit derived from ethylene and a structural unit derived from unsaturated ester, and when the total of the structural unit derived from ethylene and the structural unit derived from unsaturated ester is 100% by mass, unsaturated A sealing material for solar cells obtained by using a resin composition containing 0.001 to 5 parts by mass of meta kaolin with respect to 100 parts by mass of an ethylene-unsaturated ester copolymer in which the amount of the structural unit derived from the ester is 20 to 35% by mass is disclosed. .
또한, 특허문헌 4에는, 에틸렌 공중합체와, 5가 금속의 산화물, 6가 금속의 산화물, 7가 금속의 산화물, 인산 금속염으로 이루어지는 군에서 선택된 무기 이온 포집제를 함유하는 태양 전지 밀봉재용 수지 조성물이 개시되어 있다.Moreover, in patent document 4, the resin composition for solar cell sealing materials containing an ethylene copolymer and the inorganic ion scavenger selected from the group which consists of an oxide of a pentavalent metal, an oxide of a hexavalent metal, an oxide of a hexavalent metal, and a phosphate metal salt. This is disclosed.
특허문헌 4에는, 인산 금속염으로서 인산 지르코늄(무기용 이온 교환제)을 사용한 예가 기재되어 있지만, 이 이온 포착제는, Na+ 이온을 포착하지만 충분하지 않고, 또한 이온 교환으로 H+ 이온을 방출하기 때문에, 구성에 따라서는 pH가 내려가 밀봉 수지에 악영향을 미치거나, 전극 등의, 태양 전지 소자의 구성 부재의 부식을 조장하거나 하는 문제가 있다.Patent Document 4 describes an example in which zirconium phosphate (inorganic ion exchanger) is used as a metal phosphate salt, but this ion scavenger captures Na + ions, but is insufficient, and releases H + ions through ion exchange. Therefore, depending on the configuration, there is a problem that the pH is lowered and the sealing resin is adversely affected, or corrosion of the structural members of the solar cell element such as the electrode is promoted.
본 발명의 목적은, 태양 전지의 PID의 원인이 되는 Na+ 이온을 고선택적으로 흡착하는 태양 전지용 이온 포착제를 제공하는 것이다.An object of the present invention is to provide an ion trapping agent for solar cells that highly selectively adsorbs Na + ions that cause PID of solar cells.
또한, 본 발명의 다른 목적은, PID에서 기인하는 출력의 저하나, 전극 등의, 태양 전지 소자의 구성 부재의 부식을 억제하는 태양 전지용 밀봉제 조성물 및 장수명의 태양 전지 모듈을 제공하는 것이다.Another object of the present invention is to provide a solar cell sealing agent composition and a long-life solar cell module that suppress a decrease in output resulting from PID and corrosion of structural members of a solar cell element, such as an electrode.
본 발명자는, 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 루비듐 이온, 세슘 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온으로 치환된 α-인산지르코늄, 및 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온으로 치환된 α-인산티타늄 중 적어도 한쪽을 함유하는 태양 전지용 이온 포착제가, PID에서 기인하는 Na+ 이온을 선택적으로 흡착하는 것을 발견하고, 본 발명을 완성하기에 이르렀다.The present inventors have found that at least a part of the ion exchange group is α-zirconium phosphate substituted with at least one ion selected from lithium ion, potassium ion, rubidium ion, cesium ion, magnesium ion and calcium ion, and at least part of the ion exchange group is lithium An ion trapping agent for solar cells containing at least one of α-titanium phosphate substituted with at least one ion selected from ions, potassium ions, cesium ions, rubidium ions, magnesium ions, and calcium ions, Na + ions resulting from PID It was discovered that it adsorb|sucked selectively, and came to complete this invention.
1. (A) 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온 (a1)으로 치환된 α-인산지르코늄, 및 (B) 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온 (b1)으로 치환된 α-인산티타늄 중 적어도 한쪽을 함유하는 것을 특징으로 하는 태양 전지용 이온 포착제.1. (A) α-zirconium phosphate in which at least a part of the ion exchanger is substituted with at least one ion (a1) selected from lithium ion, potassium ion, cesium ion, rubidium ion, magnesium ion and calcium ion, and (B) At least a part of the ion exchange group contains at least one of α-titanium phosphate substituted with at least one ion (b1) selected from lithium ion, potassium ion, cesium ion, rubidium ion, magnesium ion and calcium ion. Ion scavengers for solar cells.
2. 상기 성분 (A)는, 전체 이온 교환 용량 중, 0.1 내지 6.7meq/g가 상기 이온 (a1)으로 치환된 α-인산지르코늄인 상기 1에 기재된 태양 전지용 이온 포착제.2. The ion trapping agent for solar cells according to 1, wherein the component (A) is α-zirconium phosphate in which 0.1 to 6.7 meq/g is substituted with the ion (a1) in the total ion exchange capacity.
3. 상기 이온 (a1)으로 치환되기 전의 α-인산지르코늄이, 하기 식 (1)로 표시되는 화합물인 상기 1 또는 2에 기재된 태양 전지용 이온 포착제.3. The ion trapping agent for solar cells as described in said 1 or 2 whose (alpha)- zirconium phosphate before substitution by the said ion (a1) is a compound represented by following formula (1).
Zr1-xHfxHa(PO4)b·mH2O (1)Zr 1-x Hf x H a (PO 4 ) b mH 2 O (1)
(식 중, 0≤x≤0.2이고, 2<b≤2.1이고, a는 3b-a=4를 만족시키는 양수이고, 0≤m≤2임)(Wherein, 0≤x≤0.2, 2<b≤2.1, a is a positive number satisfying 3b-a=4, and 0≤m≤2)
4. 상기 성분 (B)는, 전체 이온 교환 용량 중, 0.1 내지 7.0meq/g가 상기 이온 (b1)으로 치환된 α-인산티타늄인 상기 1 내지 3 중 어느 한 항에 기재된 태양 전지용 이온 포착제.4. The ion trapping agent for solar cells according to any one of 1 to 3, wherein the component (B) is α-titanium phosphate in which 0.1 to 7.0 meq/g is substituted with the ion (b1) in the total ion exchange capacity. .
5. 상기 이온 (b1)으로 치환되기 전의 α-인산티타늄이, 하기 식 (2)로 표시되는 화합물인 상기 1 내지 4 중 어느 한 항에 기재된 태양 전지용 이온 포착제.5. The ion trapping agent for solar cells in any one of said 1-4 whose (alpha)-titanium phosphate before substitution by the said ion (b1) is a compound represented by following formula (2).
TiHs(PO4)t·nH2O (2)TiH s (PO 4 ) t nH 2 O (2)
(식 중, 2<t≤2.1이고, s는 3t-s=4를 만족시키는 양수이고, 0≤n≤2임)(Wherein, 2<t≤2.1, s is a positive number satisfying 3t-s=4, and 0≤n≤2)
6. 상기 1 내지 5 중 어느 한 항에 기재된 태양 전지용 이온 포착제와, 수지를 함유하는 것을 특징으로 하는 태양 전지용 밀봉제 조성물.6. Said ion trapping agent for solar cells in any one of 1-5, and resin are contained, The sealing agent composition for solar cells characterized by the above-mentioned.
7. 상기 수지가, 에틸렌·아세트산비닐 공중합 수지를 포함하는 상기 6에 기재된 태양 전지용 밀봉제 조성물.7. Said resin sealing agent composition for solar cells as described in said 6 in which contains ethylene-vinyl acetate copolymer resin.
8. 표면측 투명 보호 부재와, 이면측 보호 부재와, 태양 전지 소자와, 상기 표면측 투명 보호 부재 및 상기 이면측 보호 부재 사이에, 상기 태양 전지 소자가, 상기 6 또는 7에 기재된 태양 전지용 밀봉제 조성물을 사용하여 밀봉된 밀봉층을 구비하는 것을 특징으로 하는 태양 전지 모듈.8. The solar cell sealing member according to 6 or 7 above, wherein the solar cell element is disposed between the front side transparent protection member, the back side protection member, and the solar cell element, and between the front side transparent protection member and the back side protection member A solar cell module comprising a sealing layer sealed using a composition.
본 발명의 태양 전지용 이온 포착제는, 태양 전지의 PID의 원인이 되는 Na+ 이온을 고선택적으로 흡착하고, H+ 이온을 방출하기 어렵다. 따라서, PID에서 기인하는 출력의 저하가 억제된다. 또한, 본 발명의 태양 전지용 밀봉제 조성물은, 전극 등의, 태양 전지 소자의 구성 부재의 부식을 억제하여, 장수명의 태양 전지 모듈을 부여할 수 있다.The ion trapping agent for solar cells of this invention highly selectively adsorb|sucks Na + ion which becomes the cause of PID of a solar cell, and it is hard to release|release H + ion. Accordingly, a decrease in the output resulting from the PID is suppressed. Moreover, the sealing agent composition for solar cells of this invention can suppress corrosion of structural members of solar cell elements, such as an electrode, and can provide a long-life solar cell module.
도 1은, 본 발명의 태양 전지 모듈을 도시하는 개략 단면도이다.BRIEF DESCRIPTION OF THE DRAWINGS It is a schematic sectional drawing which shows the solar cell module of this invention.
이하, 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.
1. 태양 전지용 이온 포착제1. Ion trapping agent for solar cell
본 발명의 태양 전지용 이온 포착제는, (A) 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온 (a1)으로 치환된 α-인산지르코늄(이하, 「태양 전지용 이온 포착제 (A)」라고 함), 및 (B) 이온 교환기의 적어도 일부가 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종의 이온 (b1)으로 치환된 α-인산티타늄(이하, 「태양 전지용 이온 포착제 (B)」라고 함) 중 적어도 한쪽을 함유한다. 이온 교환기는 통상 프로톤이다.In the ion trapping agent for solar cells of the present invention, (A) at least a part of ion exchange groups are substituted with at least one ion (a1) selected from lithium ions, potassium ions, cesium ions, rubidium ions, magnesium ions and calcium ions. -zirconium phosphate (hereinafter referred to as "ion trapping agent for solar cells (A)"), and (B) at least a part of the ion exchange group is selected from lithium ions, potassium ions, cesium ions, rubidium ions, magnesium ions and calcium ions At least one of α-titanium phosphate (hereinafter referred to as “ion trapping agent for solar cells (B)”) substituted with one type of ion (b1) is contained. The ion exchanger is usually a proton.
본 발명에 있어서, 태양 전지용 이온 포착제를, 예를 들어 도 1에 도시되는 태양 전지 모듈(10)을 구성하는 태양 전지 소자(11), 이 태양 전지 소자(11)를 수지로 밀봉하는 밀봉층(13), 표면측 투명 보호 부재(15) 및 이면측 보호 부재(17) 중, 수지를 포함하는 밀봉층(13) 및 이면측 보호 부재(17)의 적어도 한쪽에 함유시킴으로써, 태양 전지의 장수명화를 도모할 수 있다. 즉, 본 발명의 태양 전지용 이온 포착제는, 프로톤(H+)을 방출하는 일이 없기 때문에, 태양 전지의 구성 부재가 분해되거나 변질되거나 하는 것이 억제되고, 출력 저하도 억제된다.In this invention, the sealing layer which seals the
상기 이온 (a1)으로 치환되기 전의 α-인산지르코늄 및 상기 이온 (b1)으로 치환되기 전의 α-인산티타늄에는, 모두 층 내에 OH기가 많이 존재하기 때문에, 미리, 리튬 이온, 칼륨 이온, 루비듐 이온, 세슘 이온, 마그네슘 이온 또는 칼슘 이온이 치환된 구조로 함으로써, H+ 이온을 방출하지 않고, Na+ 이온이 선택적으로 흡착된다고 생각된다.In both the α-zirconium phosphate before being substituted with the ion (a1) and the α-titanium phosphate before being substituted with the ion (b1), many OH groups exist in the layer, so lithium ions, potassium ions, rubidium ions, It is thought that Na + ions are selectively adsorbed without releasing H + ions by having a structure in which cesium ions, magnesium ions, or calcium ions are substituted.
본 발명의 태양 전지용 이온 포착제는, 중성이기 때문에, 전해액에 첨가한 경우에도 그의 pH를 크게 변동시키는 일은 없다. 밀봉층(13)이 알칼리성 또는 산성의 물질을 포함하는 경우, pH의 변화에 수반하여 수지가 분해되는 경우가 있다. 예를 들어, 수지가 에틸렌·아세트산비닐 공중합 수지를 포함하는 경우, 아세트산 등이 생성되기 쉬워져 태양 전지의 열화로 연결되지만, 본 발명의 태양 전지용 이온 포착제를 포함하는 밀봉층이라면, 이러한 문제가 발생하는 일은 없다.Since the ion trapping agent for solar cells of this invention is neutral, even when it adds to electrolyte solution, the pH does not fluctuate largely. When the
또한, 본 발명의 태양 전지용 이온 포착제는, 무기 화합물이기 때문에, 열 안정성이나, 용제 중에서의 안정성이 우수하다. 이로 인해, 태양 전지의 구성 부재에 함유시킨 경우, 전하가 가해진 상태에서도 안정된다.Moreover, since the ion trapping agent for solar cells of this invention is an inorganic compound, it is excellent in thermal stability and stability in a solvent. For this reason, when it contains it in the structural member of a solar cell, it is stable also in the state to which an electric charge was applied.
1-1. 태양 전지용 이온 포착제 (A)1-1. Ion trapping agent for solar cell (A)
본 발명의 태양 전지용 이온 포착제 (A)는, 상기한 바와 같이, α-인산지르코늄의 이온 (a1)에 의한 치환체이다.The ion trapping agent for solar cells (A) of this invention is a substitution product by the ion (a1) of (alpha)- zirconium phosphate as mentioned above.
상기 α-인산지르코늄은, 이하의 식 (1)로 나타나는 화합물이다.The said α- zirconium phosphate is a compound represented by the following formula (1).
Zr1-xHfxHa(PO4)b·mH2O (1)Zr 1-x Hf x H a (PO 4 ) b mH 2 O (1)
(식 중, 0≤x≤0.2이고, 2<b≤2.1이고, a는 3b-a=4를 만족시키는 수이고, 0≤m≤2임)(Wherein, 0≤x≤0.2, 2<b≤2.1, a is a number satisfying 3b-a=4, and 0≤m≤2)
상기 α-인산지르코늄의 이온 교환기는 통상 프로톤이므로, 이 프로톤의 일부 또는 전부가 이온 (a1)으로 치환되어 본 발명의 태양 전지용 이온 포착제 (A)가 형성된다. 상기 이온 (a1)은 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종인데, Na+ 이온의 양호한 포착성의 관점에서, 1가의 알칼리 금속 원소에서 유래되는 이온(리튬 이온, 칼륨 이온, 루비듐 이온 또는 세슘 이온)인 것이 바람직하다.Since the ion exchange group of the α-zirconium phosphate is usually a proton, a part or all of the proton is substituted with the ion (a1) to form the ion trapping agent for a solar cell (A) of the present invention. The ion (a1) is at least one selected from lithium ion, potassium ion, cesium ion, rubidium ion, magnesium ion, and calcium ion, from the viewpoint of good trapping property of Na + ions, ions derived from monovalent alkali metal elements ( lithium ion, potassium ion, rubidium ion or cesium ion).
본 발명의 태양 전지용 이온 포착제 (A)에 있어서, 치환되어 있는 이온 (a1)의 양은, 바람직하게는 0.1 내지 6.7meq/g, 보다 바람직하게는 1.0 내지 6.7meq/g이다. 또한, Na+ 이온 흡착능의 관점에서, 3.5 내지 6.7meq/g가 더욱 바람직하다.In the ion trapping agent for solar cells (A) of this invention, the quantity of the ion (a1) substituted becomes like this. Preferably it is 0.1-6.7 meq/g, More preferably, it is 1.0-6.7 meq/g. Further, from the viewpoint of Na + ion adsorption capacity, 3.5 to 6.7 meq/g is more preferable.
상기 식 (1)에 있어서의 x는, Na+ 이온의 포착성의 관점에서, 바람직하게는 0≤x≤0.1, 보다 바람직하게는 0≤x≤0.02이다. 또한, Hf를 포함하는 경우, 바람직하게는 0.005≤x≤0.1, 보다 바람직하게는 0.005≤x≤0.02이다. x>0.2의 경우, 이온 (a1)에 의한 이온 교환 성능은 향상되지만, 방사성의 동위체가 존재하기 때문에, 태양 전지의 구성 부품이 전자 부품을 포함하는 경우 악영향을 미치는 일이 있다. From the viewpoint of the trapping property of Na + ions, x in the formula (1) is preferably 0≤x≤0.1, more preferably 0≤x≤0.02. In addition, when Hf is included, preferably 0.005≤x≤0.1, more preferably 0.005≤x≤0.02. In the case of x>0.2, although the ion exchange performance by the ion (a1) improves, since a radioactive isotope exists, when the component of a solar cell contains an electronic component, it may exert a bad influence.
본 발명의 태양 전지용 이온 포착제 (A)를 제조하는 방법은, 특별히 한정되지 않는다. 예를 들어, 리튬 이온으로 치환된 α-인산지르코늄을 제조하는 경우, 수산화리튬(LiOH) 수용액에 α-인산지르코늄을 첨가하고, 일정 시간 교반한 후, 여과, 세정 및 건조하는 방법으로 할 수 있다. LiOH 수용액의 농도는, 특별히 한정되지 않는다. 고농도의 경우, 반응액의 염기성이 높아지고 α-인산지르코늄의 일부가 용출되는 경우가 있기 때문에, 1mol/L 이하가 바람직하고, 더욱 바람직하게는 0.1mol/L 이하이다.The method of manufacturing the ion trapping agent for solar cells (A) of this invention is not specifically limited. For example, in the case of producing α-zirconium phosphate substituted with lithium ions, α-zirconium phosphate is added to an aqueous lithium hydroxide (LiOH) solution, stirred for a certain period of time, followed by filtration, washing and drying. . The concentration of the LiOH aqueous solution is not particularly limited. In the case of a high concentration, since basicity of the reaction solution increases and a part of α-zirconium phosphate may be eluted, 1 mol/L or less is preferable, and more preferably 0.1 mol/L or less.
칼륨 이온으로 치환된 α-인산지르코늄을 제조하는 경우도, 상기와 마찬가지의 이온 교환 방법을 적용할 수 있다.Also in the case of producing α-zirconium phosphate substituted with potassium ions, the ion exchange method similar to the above can be applied.
마그네슘 이온 또는 칼슘 이온으로 치환된 α-인산지르코늄을 제조하는 경우, 마그네슘 또는 칼슘의 수산화물이 물에 용해되기 어려우므로, 일단 칼륨 등의 알칼리 금속의 이온으로 치환하고 나서, 염화마그네슘 등의 수용액을 사용하여 치환할 수 있다. 또한, 예를 들어 아세트산마그네슘 수용액에 α-인산지르코늄을 첨가하고, 동일한 조작을 행해도 된다.When producing α-zirconium phosphate substituted with magnesium ions or calcium ions, since the hydroxide of magnesium or calcium is difficult to dissolve in water, once substituted with an ion of an alkali metal such as potassium, an aqueous solution such as magnesium chloride is used can be substituted. In addition, for example, α-zirconium phosphate may be added to aqueous magnesium acetate solution, and the same operation may be performed.
1-2. 태양 전지용 이온 포착제 (B)1-2. Ion trapping agent for solar cell (B)
본 발명의 태양 전지용 이온 포착제 (B)는, 상기한 바와 같이, α-인산티타늄의 이온 (b1)에 의한 치환체이다.The ion trapping agent for solar cells (B) of this invention is a substitution product by the ion (b1) of alpha-titanium phosphate, as above-mentioned.
상기 α-인산티타늄은, 이하의 식 (2)로 나타나는 화합물이다.The said alpha-titanium phosphate is a compound represented by the following formula (2).
TiHs(PO4)t·nH2O (2)TiH s (PO 4 ) t nH 2 O (2)
(식 중, 2<t≤2.1이고, s는 3t-s=4를 만족시키는 수이고, 0≤n≤2임)(Wherein, 2<t≤2.1, s is a number that satisfies 3t-s=4, and 0≤n≤2)
α-인산티타늄의 이온 교환기는 통상 프로톤이므로, 이 프로톤의 일부 또는 전부가 이온 (b1)으로 치환되어 본 발명의 태양 전지용 이온 포착제 (B)가 형성된다. 상기 이온 (b1)은 리튬 이온, 칼륨 이온, 세슘 이온, 루비듐 이온, 마그네슘 이온 및 칼슘 이온으로부터 선택된 적어도 1종인데, Na+ 이온의 양호한 포착성의 관점에서, 1가의 알칼리 금속 원소에서 유래되는 이온(리튬 이온, 칼륨 이온, 루비듐 이온 또는 세슘 이온)인 것이 바람직하다.Since the ion exchange group of α-titanium phosphate is usually a proton, part or all of the proton is substituted with the ion (b1) to form the ion trapping agent (B) for a solar cell of the present invention. The ion (b1) is at least one selected from lithium ion, potassium ion, cesium ion, rubidium ion, magnesium ion and calcium ion, from the viewpoint of good trapping property of Na + ions, ions derived from monovalent alkali metal elements ( lithium ion, potassium ion, rubidium ion or cesium ion).
본 발명의 태양 전지용 이온 포착제 (B)에 있어서, 치환되어 있는 이온 (b1)의 양은, 바람직하게는 0.1 내지 7.0meq/g, 보다 바람직하게는 1.0 내지 7.0meq/g이다. 또한, Na+ 이온 흡착능의 관점에서, 3.5 내지 7.0meq/g가 더욱 바람직하다.In the ion trapping agent for solar cells of the present invention (B), the amount of the substituted ion (b1) is preferably 0.1 to 7.0 meq/g, more preferably 1.0 to 7.0 meq/g. Further, from the viewpoint of Na + ion adsorption capacity, 3.5 to 7.0 meq/g is more preferable.
본 발명의 태양 전지용 이온 포착제 (B)를 제조하는 방법은, 특별히 한정되지 않으며, 태양 전지용 이온 포착제 (A)의 제조 방법과 동일한 방법으로 할 수 있다.The method of manufacturing the ion trapping agent for solar cells (B) of this invention is not specifically limited, It can be set as the method similar to the manufacturing method of the ion trapping agent for solar cells (A).
본 발명의 태양 전지용 이온 포착제는, 통상, 층상 구조를 가지며, 메디안 입경의 상한은, 바람직하게는 5.0㎛, 보다 바람직하게는 3.0㎛, 더욱 바람직하게는 2.0㎛이고, 하한은, 통상 0.2㎛, 바람직하게는 0.5㎛이다. 본 발명의 태양 전지용 이온 포착제를 적용하는 구성 부재의 종류에 따라 바람직한 입경을 선택하면 된다.The ion trapping agent for solar cells of the present invention usually has a layered structure, and the upper limit of the median particle size is preferably 5.0 µm, more preferably 3.0 µm, still more preferably 2.0 µm, and the lower limit is usually 0.2 µm. , preferably 0.5 µm. What is necessary is just to select a preferable particle diameter according to the kind of structural member to which the ion trapping agent for solar cells of this invention is applied.
본 발명의 태양 전지용 이온 포착제의 수분 함유율은, 바람직하게는 10질량％ 이하, 보다 바람직하게는 5질량％ 이하이다. 수분 함유율이 10질량％ 이하임으로써, 태양 전지를 구성하는 부재로 했을 경우에, 수분이 전기 분해를 일으키는 것에서 기인하는 가스의 발생을 억제할 수 있어, 전지의 문제를 억제할 수 있다. 또한, 수분 함유율은, 칼 피셔법으로 측정할 수 있다.The water content rate of the ion trapping agent for solar cells of this invention becomes like this. Preferably it is 10 mass % or less, More preferably, it is 5 mass % or less. When the water content is 10% by mass or less, when a member constituting the solar cell is used, the generation of gas resulting from the electrolysis of water can be suppressed, and the problem of the battery can be suppressed. In addition, the water content can be measured by the Karl Fischer method.
태양 전지용 이온 포착제의 수분 함유율을 10질량％ 이하로 하는 경우에는, 특별히 한정되지 않으며, 통상 사용되는 분체의 건조 방법을 적용할 수 있다. 예를 들어, 대기압 또는 감압 하에서, 100℃ 내지 300℃에서, 6 내지 24시간 정도의 가열을 행하는 방법을 들 수 있다.When the water content rate of the ion trapping agent for solar cells shall be 10 mass % or less, it does not specifically limit, The drying method of powder normally used is applicable. For example, under atmospheric pressure or reduced pressure, the method of heating at 100 degreeC - 300 degreeC for about 6 to 24 hours is mentioned.
2. 태양 전지용 밀봉제 조성물2. Encapsulant composition for solar cells
본 발명의 태양 전지용 밀봉제 조성물은, 상기 본 발명의 태양 전지용 이온 포착제와, 수지를 함유하는 것을 특징으로 한다. 본 발명의 태양 전지용 밀봉제 조성물은, 후술되는 가교제, 가교 보조제, 접착성 개량제, 자외선 흡수제, 광 안정제, 산화 방지제 등의 다른 성분을 함유할 수 있다.The sealing agent composition for solar cells of this invention contains the said ion trapping agent for solar cells of this invention, and resin, It is characterized by the above-mentioned. The sealing agent composition for solar cells of this invention can contain other components, such as a crosslinking agent mentioned later, a crosslinking adjuvant, an adhesive improving agent, a ultraviolet absorber, a light stabilizer, and antioxidant.
본 발명의 태양 전지용 밀봉제 조성물은, 예를 들어 도 1에 도시되는 태양 전지 모듈(10)을 구성하는 표면측 투명 보호 부재(15) 및 이면측 보호 부재(17) 사이의 밀봉층(13)의 형성에 적합하다.The sealing agent composition for solar cells of this invention is the
본 발명의 태양 전지용 밀봉제 조성물에 함유되는 수지로서는, 에틸렌·아세트산비닐 공중합 수지; 폴리에틸렌, 폴리프로필렌 등의 폴리올레핀 수지; 아이오노머 수지; 에틸렌·메타크릴산 공중합체; 에틸렌·메타크릴산에스테르 공중합체; 에틸렌·아크릴산 공중합체; 에틸렌·아크릴산에스테르 공중합체; 폴리불화비닐 수지; 폴리염화비닐 수지 등을 들 수 있다. 이들 중, 투명성이 우수한 밀봉층을 형성 가능한 점에서, 에틸렌·아세트산비닐 공중합 수지가 특히 바람직하다.As resin contained in the sealing agent composition for solar cells of this invention, ethylene-vinyl acetate copolymer resin; polyolefin resins such as polyethylene and polypropylene; ionomer resin; ethylene/methacrylic acid copolymer; ethylene/methacrylic acid ester copolymer; ethylene/acrylic acid copolymer; ethylene/acrylic acid ester copolymer; polyvinyl fluoride resin; Polyvinyl chloride resin etc. are mentioned. Among these, an ethylene-vinyl acetate copolymer resin is especially preferable at the point which can form the sealing layer excellent in transparency.
상기 에틸렌·아세트산비닐 공중합 수지는, 특별히 한정되지 않지만, 태양 전지 모듈을 제조할 때, 예를 들어 진공 가열 라미네이션 공정 후, 높은 겔 분율에 의한 고가교도에 의해 100℃ 내지 150℃의 내열성이 원활하게 얻어지는 점에서, 아세트산비닐에서 유래되는 구조 단위의 함유량이 바람직하게는 20 내지 40질량％, 보다 바람직하게는 25 내지 35질량％, 더욱 바람직하게는 28 내지 33질량％인 에틸렌·아세트산비닐 공중합 수지가 바람직하다.The ethylene/vinyl acetate copolymer resin is not particularly limited, but when manufacturing a solar cell module, for example, after a vacuum heating lamination process, heat resistance at 100° C. to 150° C. smoothly due to a high degree of crosslinking due to a high gel fraction From the viewpoint of obtaining, the content of the structural unit derived from vinyl acetate is preferably 20 to 40% by mass, more preferably 25 to 35% by mass, still more preferably 28 to 33% by mass of ethylene/vinyl acetate copolymer resin desirable.
상기 에틸렌·아세트산비닐 공중합 수지의 용융 질량 유속(MFR)은, JIS K 7210에 준하는 방법(190℃)에 있어서, 바람직하게는 1g 내지 40g/10분, 보다 바람직하게는 15g 내지 40g/10분이다. 또한, 비캣 연화점은, JIS K 7206에 준하는 방법에 있어서, 바람직하게는 30℃ 내지 40℃이다.The melt mass flow rate (MFR) of the ethylene/vinyl acetate copolymer resin is preferably 1 g to 40 g/10 min, more preferably 15 g to 40 g/10 min in a method (190° C.) according to JIS K 7210. . In addition, the Vicat softening point is the method according to JIS K 7206. WHEREIN: Preferably it is 30 degreeC - 40 degreeC.
본 발명의 태양 전지용 밀봉제 조성물에 있어서, 태양 전지용 이온 포착제의 함유 비율은, 밀봉층의 투명성 및 밀봉층에 있어서의 Na+ 이온의 포착성의 관점에서, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.01 내지 1.0질량부, 보다 바람직하게는 0.05 내지 0.5질량부이다. 또한, 상기 태양 전지용 이온 포착제의 메디안 입경은, 태양 전지의 발전효율의 관점에서, 바람직하게는 0.5 내지 5.0㎛, 보다 바람직하게는 0.7 내지 2.0㎛이다.The sealing agent composition for solar cells of this invention WHEREIN: When content of the ion trapping agent for solar cells makes content of the said resin 100 mass parts from a viewpoint of transparency of a sealing layer, and the trapping property of Na + ions in a sealing layer, To, Preferably it is 0.01-1.0 mass part, More preferably, it is 0.05-0.5 mass part. Moreover, from a viewpoint of the power generation efficiency of a solar cell, the median particle diameter of the said ion trapping agent for solar cells becomes like this. Preferably it is 0.5-5.0 micrometers, More preferably, it is 0.7-2.0 micrometers.
본 발명의 태양 전지용 밀봉제 조성물은, 상기한 바와 같이 다른 성분을 함유해도 된다.The sealing agent composition for solar cells of this invention may contain another component as mentioned above.
가교제로서는, 유기 과산화물, 아조 화합물, 주석 화합물 등을 사용할 수 있다. 이들은 단독으로 사용해도 되고, 2종 이상을 조합하여 사용해도 된다.As a crosslinking agent, an organic peroxide, an azo compound, a tin compound, etc. can be used. These may be used independently and may be used in combination of 2 or more type.
유기 과산화물로서는, 디이소프로필벤젠히드로퍼옥시드, 2,5-디메틸-2,5-디(히드로퍼옥시)헥산 등의 히드로퍼옥시드류; 디-tert-부틸퍼옥시드, tert-부틸쿠밀퍼옥시드, 디쿠밀퍼옥시드, 2,5-디메틸-2,5-디(tert-부틸퍼옥시)헥산, 2,5-디메틸-2,5-디(tert-퍼옥시)헥신-3 등의 디알킬퍼옥시드류; 비스-3,5,5-트리메틸헥사노일퍼옥시드, 옥타노일퍼옥시드, 벤조일퍼옥시드, o-메틸벤조일퍼옥시드, 2,4-디클로로벤조일퍼옥시드 등의 디아실퍼옥시드류; tert-부틸퍼옥시아세테이트, tert-부틸퍼옥시-2-에틸헥사노에이트, tert-부틸퍼옥시피발레이트, tert-부틸퍼옥시옥토에이트, tert-부틸퍼옥시이소프로필카르보네이트, tert-부틸퍼옥시벤조에이트, 디-tert-부틸퍼옥시프탈레이트, 2,5-디메틸-2,5-디(벤조일퍼옥시)헥산, 2,5-디메틸-2,5-디(벤조일퍼옥시)헥신-3, tert-부틸퍼옥시-2-에틸헥실카르보네이트 등의 퍼옥시에스테르류; 메틸에틸케톤퍼옥시드, 시클로헥사논퍼옥시드 등의 케톤퍼옥시드류 등을 들 수 있다.Examples of the organic peroxide include hydroperoxides such as diisopropylbenzene hydroperoxide and 2,5-dimethyl-2,5-di(hydroperoxy)hexane; Di-tert-butylperoxide, tert-butylcumylperoxide, dicumylperoxide, 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane, 2,5-dimethyl-2,5- dialkyl peroxides such as di(tert-peroxy)hexyne-3; diacyl peroxides such as bis-3,5,5-trimethylhexanoyl peroxide, octanoyl peroxide, benzoyl peroxide, o-methylbenzoyl peroxide and 2,4-dichlorobenzoyl peroxide; tert-butylperoxyacetate, tert-butylperoxy-2-ethylhexanoate, tert-butylperoxypivalate, tert-butylperoxyoctoate, tert-butylperoxyisopropylcarbonate, tert-butyl Peroxybenzoate, di-tert-butylperoxyphthalate, 2,5-dimethyl-2,5-di(benzoylperoxy)hexane, 2,5-dimethyl-2,5-di(benzoylperoxy)hexyne- 3, peroxyesters such as tert-butylperoxy-2-ethylhexyl carbonate; Ketone peroxides, such as methyl ethyl ketone peroxide and cyclohexanone peroxide, etc. are mentioned.
아조 화합물로서는, 아조비스이소부티로니트릴, 아조비스(2,4-디메틸발레로니트릴) 등을 들 수 있다.Examples of the azo compound include azobisisobutyronitrile and azobis(2,4-dimethylvaleronitrile).
또한, 주석 화합물로서는, 디부틸주석디아세테이트, 디부틸주석디라우레이트, 디부틸주석디옥테이트, 디옥틸주석디라우레이트 등을 들 수 있다.Examples of the tin compound include dibutyltin diacetate, dibutyltin dilaurate, dibutyltin dioctate, and dioctyltin dilaurate.
본 발명의 태양 전지용 밀봉제 조성물이 가교제를 함유하는 경우, 그 함유 비율은, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.01 내지 2.0질량부, 보다 바람직하게는 0.05 내지 1.5질량부이다.When the sealing agent composition for solar cells of this invention contains a crosslinking agent, when the content rate makes content of the said resin 100 mass parts, Preferably it is 0.01-2.0 mass parts, More preferably, it is 0.05-1.5 mass parts. am.
가교 보조제는, 가교제에 의한 가교 반응을 촉진시키는 것이며, 바람직하게는 탄소 원자-탄소 원자 이중 결합 및 에폭시기의 적어도 한쪽을 갖는 다관능 단량체, 보다 바람직하게는, 알릴기, 메타크릴로일기, 아크릴로일기, 비닐기 등을 갖는 다관능 단량체이고, 구체예로서는, 폴리알릴 화합물, 폴리(메트)아크릴옥시 화합물, 에폭시 화합물 등을 들 수 있다. 이들은 단독으로 사용해도 되고, 2종 이상을 조합하여 사용해도 된다.The crosslinking aid accelerates the crosslinking reaction by the crosslinking agent, and is preferably a polyfunctional monomer having at least one of a carbon atom-carbon atom double bond and an epoxy group, more preferably an allyl group, a methacryloyl group, or an acryloyl group. It is a polyfunctional monomer which has a diyl, a vinyl group, etc., and a polyallyl compound, a poly(meth)acryloxy compound, an epoxy compound etc. are mentioned as a specific example. These may be used independently and may be used in combination of 2 or more type.
폴리알릴 화합물로서는, 트리알릴이소시아누레이트, 트리알릴시아누레이트, 디알릴프탈레이트, 디알릴푸마레이트, 디알릴말레이트 등을 들 수 있다.Examples of the polyallyl compound include triallyl isocyanurate, triallyl cyanurate, diallyl phthalate, diallyl fumarate, and diallyl malate.
폴리(메트)아크릴옥시 화합물로서는, 트리메틸올프로판트리메타크릴레이트, 트리메틸올프로판트리아크릴레이트, 에틸렌글리콜디아크릴레이트, 에틸렌글리콜디메타크릴레이트, 1,4-부탄디올디아크릴레이트, 1,6-헥산디올디아크릴레이트, 1,9-노난디올디아크릴레이트 등을 들 수 있다.Examples of the poly(meth)acryloxy compound include trimethylolpropane trimethacrylate, trimethylolpropane triacrylate, ethylene glycol diacrylate, ethylene glycol dimethacrylate, 1,4-butanediol diacrylate, and 1,6- Hexanediol diacrylate, 1,9- nonanediol diacrylate, etc. are mentioned.
또한, 에폭시 화합물로서는, 글리시딜아크릴레이트, 글리시딜메타크릴레이트, 4-히드록시부틸아크릴레이트글리시딜에테르, 1,6-헥산디올디글리시딜에테르, 1,4-부탄디올디글리시딜에테르, 시클로헥산디메탄올디글리시딜에테르, 트리메틸올프로판폴리글리시딜에테르 등을 들 수 있다.Examples of the epoxy compound include glycidyl acrylate, glycidyl methacrylate, 4-hydroxybutyl acrylate glycidyl ether, 1,6-hexanediol diglycidyl ether, and 1,4-butanediol diglycidyl ether. Cydyl ether, cyclohexane dimethanol diglycidyl ether, trimethylol propane polyglycidyl ether, etc. are mentioned.
본 발명의 태양 전지용 밀봉제 조성물이 가교 보조제를 함유하는 경우, 그 함유 비율은, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.01 내지 3.0질량부, 보다 바람직하게는 0.05 내지 2.0질량부이다.When the sealing agent composition for solar cells of this invention contains a crosslinking adjuvant, when the content rate makes content of the said resin 100 mass parts, Preferably it is 0.01-3.0 mass parts, More preferably, it is 0.05-2.0 mass is wealth
접착성 개량제는, 바람직하게는 메타크릴로일기, 아크릴로일기, 비닐기 등의 중합성 불포화 결합을 갖는 기, 또는 알콕시기 등의 가수분해성기를 갖는 실란 화합물이며, 종래 공지된 실란 커플링제를 사용할 수 있다.The adhesion improving agent is preferably a silane compound having a group having a polymerizable unsaturated bond such as a methacryloyl group, an acryloyl group, a vinyl group, or a hydrolysable group such as an alkoxy group, and a conventionally known silane coupling agent is used. can
상기 실란 커플링제로서는, 비닐트리클로로실란, 비닐트리스(β-메톡시에톡시)실란, 비닐트리에톡시실란, 비닐트리메톡시실란, γ-메타크릴옥시프로필트리메톡시실란, β-(3,4-에폭시시클로헥실)에틸트리메톡시실란, γ-글리시독시프로필메틸디에톡시실란, N-β(아미노에틸)γ-아미노프로필트리메톡시실란, N-β(아미노에틸)γ-아미노프로필메틸디메톡시실란, γ-아미노프로필트리에톡시실란, N-페닐-γ-아미노프로필트리메톡시실란, γ-머캅토프로필트리메톡시실란, γ-클로로프로필트리메톡시실란 등을 들 수 있다.Examples of the silane coupling agent include vinyltrichlorosilane, vinyltris(β-methoxyethoxy)silane, vinyltriethoxysilane, vinyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, β-(3 ,4-epoxycyclohexyl)ethyltrimethoxysilane, γ-glycidoxypropylmethyldiethoxysilane, N-β(aminoethyl)γ-aminopropyltrimethoxysilane, N-β(aminoethyl)γ-amino and propylmethyldimethoxysilane, γ-aminopropyltriethoxysilane, N-phenyl-γ-aminopropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, and γ-chloropropyltrimethoxysilane. have.
본 발명의 태양 전지용 밀봉제 조성물이 접착성 개량제를 함유하는 경우, 그 함유 비율은, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.01 내지 3.0질량부이다.When the sealing agent composition for solar cells of this invention contains an adhesive improving agent, when the content rate makes content of the said resin 100 mass parts, Preferably it is 0.01-3.0 mass parts.
자외선 흡수제로서는, 벤조페논계 화합물, 벤조트리아졸계 화합물, 트리아진계 화합물, 살리실산에스테르계 화합물 등을 들 수 있다. 이들은, 단독으로 사용해도 되고, 2종 이상을 조합하여 사용해도 된다.Examples of the ultraviolet absorber include a benzophenone-based compound, a benzotriazole-based compound, a triazine-based compound, and a salicylic acid ester-based compound. These may be used independently and may be used in combination of 2 or more type.
상기 자외선 흡수제로서는, 2-히드록시-4-메톡시벤조페논, 2-히드록시-4-메톡시-2'-카르복시벤조페논, 2-히드록시-4-옥톡시벤조페논, 2-히드록시-4-n-도데실옥시벤조페논, 2-히드록시-4-n-옥타데실옥시벤조페논, 2-히드록시-4-벤질옥시벤조페논, 2-히드록시-4-메톡시-5-술포벤조페논, 2-히드록시-5-클로로벤조페논, 2,4-디히드록시벤조페논, 2,2'-디히드록시-4-메톡시벤조페논, 2,2'-디히드록시-4,4'-디메톡시벤조페논, 2,2',4,4'-테트라히드록시벤조페논, 2-(2-히드록시-5-메틸페닐)벤조트리아졸, 2-(2-히드록시-5-tert-부틸페닐)벤조트리아졸, 2-(2-히드록시-3,5-디메틸페닐)벤조트리아졸, 2-(2-메틸-4-히드록시페닐)벤조트리아졸, 2-(2-히드록시-3-메틸-5-tert-부틸페닐)벤조트리아졸, 2-(2-히드록시-3,5-디-tert-부틸페닐)벤조트리아졸, 2-(2-히드록시-3,5-디메틸페닐)-5-메톡시벤조트리아졸, 2-(2-히드록시-3-tert-부틸-5-메틸페닐)-5-클로로벤조트리아졸, 2-(2-히드록시-5-tert-부틸페닐)-5-클로로벤조트리아졸, 2-[4,6-비스(2,4-디메틸페닐)-1,3,5-트리아진-2-일]-5-(옥틸옥시)페놀, 2-(4,6-디페닐-1,3,5-트리아진-2-일)-5-(헥실옥시)페놀, 페닐살리실레이트, p-옥틸페닐살리실레이트 등을 들 수 있다.Examples of the ultraviolet absorber include 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-2'-carboxybenzophenone, 2-hydroxy-4-octoxybenzophenone, and 2-hydroxy -4-n-dodecyloxybenzophenone, 2-hydroxy-4-n-octadecyloxybenzophenone, 2-hydroxy-4-benzyloxybenzophenone, 2-hydroxy-4-methoxy-5- Sulfobenzophenone, 2-hydroxy-5-chlorobenzophenone, 2,4-dihydroxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy- 4,4'-dimethoxybenzophenone, 2,2',4,4'-tetrahydroxybenzophenone, 2-(2-hydroxy-5-methylphenyl)benzotriazole, 2-(2-hydroxy- 5-tert-butylphenyl)benzotriazole, 2-(2-hydroxy-3,5-dimethylphenyl)benzotriazole, 2-(2-methyl-4-hydroxyphenyl)benzotriazole, 2-( 2-hydroxy-3-methyl-5-tert-butylphenyl)benzotriazole, 2-(2-hydroxy-3,5-di-tert-butylphenyl)benzotriazole, 2-(2-hydroxy -3,5-dimethylphenyl)-5-methoxybenzotriazole, 2-(2-hydroxy-3-tert-butyl-5-methylphenyl)-5-chlorobenzotriazole, 2-(2-hydroxyl -5-tert-Butylphenyl)-5-chlorobenzotriazole, 2-[4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-5-( Octyloxy)phenol, 2-(4,6-diphenyl-1,3,5-triazin-2-yl)-5-(hexyloxy)phenol, phenylsalicylate, p-octylphenylsalicylate and the like.
본 발명의 태양 전지용 밀봉제 조성물이 자외선 흡수제를 함유하는 경우, 그 함유 비율은, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.01 내지 3.0질량부이다.When the sealing agent composition for solar cells of this invention contains a ultraviolet absorber, when the content rate makes content of the said resin 100 mass parts, Preferably it is 0.01-3.0 mass parts.
광 안정제는, 광 열화에서 발생하는 라디칼을 포착하는 것이라면, 특별히 한정되지 않으며, 힌더드 아민계 화합물, 티올계 화합물, 티오에테르계 화합물 등을 사용할 수 있다. 이들은 단독으로 사용해도 되고, 2종 이상을 조합하여 사용해도 된다.The light stabilizer is not particularly limited as long as it traps radicals generated from light degradation, and hindered amine-based compounds, thiol-based compounds, thioether-based compounds, and the like can be used. These may be used independently and may be used in combination of 2 or more type.
상기 광 안정제로서는, 힌더드 아민계 화합물이 바람직하고, 그 구체예로서는, 숙신산디메틸-1-(2-히드록시에틸)-4-히드록시-2,2,6,6-테트라메틸피페리딘 중축합물, 폴리[{6-(1,1,3,3-테트라메틸부틸)아미노-1,3,5-트리아진-2,4-디일}{(2,2,6,6-테트라메틸-4-피페리딜)이미노}헥사메틸렌{{2,2,6,6-테트라메틸-4-피페리딜)이미노}], N,N'-비스(3-아미노프로필)에틸렌디아민-2,4-비스[N-부틸-N-(1,2,2,6,6-펜타메틸-4-피페리딜)아미노]-6-클로로-1,3,5-트리아진 축합물, 비스(2,2,6,6-테트라메틸-4-피페리딜)세바케이트, 2-(3,5-디-tert-4-히드록시벤질)-2-n-부틸말론산비스(1,2,2,6,6-펜타메틸-4-피페리딜) 등을 들 수 있다.As the light stabilizer, a hindered amine compound is preferable, and a specific example thereof is dimethyl succinate-1-(2-hydroxyethyl)-4-hydroxy-2,2,6,6-tetramethylpiperidine polycondensate. compound, poly[{6-(1,1,3,3-tetramethylbutyl)amino-1,3,5-triazine-2,4-diyl}{(2,2,6,6-tetramethyl- 4-piperidyl)imino}hexamethylene {{2,2,6,6-tetramethyl-4-piperidyl)imino}], N,N'-bis(3-aminopropyl)ethylenediamine- 2,4-bis[N-butyl-N-(1,2,2,6,6-pentamethyl-4-piperidyl)amino]-6-chloro-1,3,5-triazine condensate; Bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate, 2-(3,5-di-tert-4-hydroxybenzyl)-2-n-butylmalonic acid bis(1 , 2,2,6,6-pentamethyl-4-piperidyl) and the like.
본 발명의 태양 전지용 밀봉제 조성물이 광 안정제를 함유하는 경우, 그 함유 비율은, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.01 내지 3.0질량부이다.When the sealing agent composition for solar cells of this invention contains an optical stabilizer, when the content rate makes content of the said resin 100 mass parts, Preferably it is 0.01-3.0 mass parts.
산화 방지제는, 태양광의 열 에너지에 대한 열 안정성을 부여하는 것이라면, 특별히 한정되지 않으며, 모노페놀계 화합물, 비스페놀계 화합물, 고분자형 페놀계 화합물, 황계 화합물, 인산계 화합물 등을 사용할 수 있다. 이들은 단독으로 사용해도 되고, 2종 이상을 조합하여 사용해도 된다.The antioxidant is not particularly limited as long as it imparts thermal stability to the thermal energy of sunlight, and monophenol-based compounds, bisphenol-based compounds, high-molecular-type phenolic compounds, sulfur-based compounds, phosphoric acid-based compounds, and the like can be used. These may be used independently and may be used in combination of 2 or more type.
상기 산화 방지제로서는, 2,6-디-tert-부틸-p-크레졸, 부틸화히드록시아니솔, 2,6-디-tert-부틸-4-에틸페놀, 2,2'-메틸렌-비스-(4-메틸-6-tert-부틸페놀), 2,2'-메틸렌-비스-(4-에틸-6-tert-부틸페놀), 4,4'-티오비스-(3-메틸-6-tert-부틸페놀), 4,4'-부틸리덴-비스-(3-메틸-6-tert-부틸페놀), 3,9-비스〔{1,1-디메틸-2-{β-(3-tert-부틸-4-히드록시-5-메틸페닐)프로피오닐옥시}에틸}2,4,8,10-테트라옥사스피로〕5,5-운데칸, 1,1,3-트리스-(2-메틸-4-히드록시-5-tert-부틸페닐)부탄, 1,3,5-트리메틸-2,4,6-트리스(3,5-디-tert-부틸-4-히드록시벤질)벤젠, 테트라키스-{메틸렌-3-(3',5'-디-tert-부틸-4'-히드로키스페닐)프로피오네이트}메탄, 비스{(3,3'-비스-4'-히드록시-3'-tert-부틸페닐)부티릭애시드}글루콜에스테르, 디라우릴티오디프로피오네이트, 디미리스틸티오디프로피오네이트, 디스테아릴티오프로피오네이트, 트리페닐포스파이트, 디페닐이소데실포스파이트, 페닐디이소데실포스파이트, 4,4'-부틸리덴-비스-(3-메틸-6-tert-부틸페닐-디-트리데실)포스파이트, 사이클릭네오펜탄테트라일비스(옥타데실포스파이트), 트리스디페닐포스파이트, 디이소데실펜타에리트리톨디포스파이트, 9,10-디히드로-9-옥사-10-포스파페난트렌-10-옥시드, 10-(3,5-디-tert-부틸-4-히드록시벤질)-9,10-디히드로-9-옥사-10-포스파페난트렌-10-옥시드, 10-데실옥시-9,10-디히드로-9-옥사-10-포스파페난트렌, 사이클릭네오펜탄테트라일비스(2,4-디-tert-부틸페닐)포스파이트, 사이클릭네오펜탄테트라일비스(2,6-디-tert-메틸페닐)포스파이트, 2,2-메틸렌비스(4,6-tert-부틸페닐)옥틸포스파이트 등을 들 수 있다.Examples of the antioxidant include 2,6-di-tert-butyl-p-cresol, butylated hydroxyanisole, 2,6-di-tert-butyl-4-ethylphenol, 2,2'-methylene-bis- (4-methyl-6-tert-butylphenol), 2,2'-methylene-bis-(4-ethyl-6-tert-butylphenol), 4,4'-thiobis-(3-methyl-6- tert-butylphenol), 4,4'-butylidene-bis-(3-methyl-6-tert-butylphenol), 3,9-bis[{1,1-dimethyl-2-{β-(3) -tert-Butyl-4-hydroxy-5-methylphenyl)propionyloxy}ethyl}2,4,8,10-tetraoxaspiro]5,5-undecane, 1,1,3-tris-(2- methyl-4-hydroxy-5-tert-butylphenyl)butane, 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene, tetrakis-{methylene-3-(3',5'-di-tert-butyl-4'-hydrokisphenyl)propionate}methane, bis{(3,3'-bis-4'-hydroxy- 3'-tert-butylphenyl)butyric acid}glucol ester, dilaurylthiodipropionate, dimyristylthiodipropionate, distearylthiopropionate, triphenylphosphite, diphenylisodecyl Phosphite, phenyldiisodecylphosphite, 4,4'-butylidene-bis-(3-methyl-6-tert-butylphenyl-di-tridecyl)phosphite, cyclic neopentanetetraylbis(octa decylphosphite), trisdiphenylphosphite, diisodecylpentaerythritol diphosphite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 10-(3,5- di-tert-butyl-4-hydroxybenzyl)-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 10-decyloxy-9,10-dihydro-9 -oxa-10-phosphaphenanthrene, cyclic neopentanetetraylbis(2,4-di-tert-butylphenyl)phosphite, cyclic neopentanetetraylbis(2,6-di-tert-methylphenyl) phosphite, 2,2-methylenebis(4,6-tert-butylphenyl)octylphosphite, etc. are mentioned.
본 발명의 태양 전지용 밀봉제 조성물이 산화 방지제를 함유하는 경우, 그 함유 비율은, 상기 수지의 함유량을 100질량부로 했을 경우에, 바람직하게는 0.05 내지 3.0질량부이다.When the sealing agent composition for solar cells of this invention contains antioxidant, when the content rate makes content of the said resin 100 mass parts, Preferably it is 0.05-3.0 mass parts.
본 발명의 태양 전지용 밀봉제 조성물은, 원료 성분을 혼합함으로써 제조할 수 있지만, 태양 전지용 이온 포착제, 다른 성분 등이, 수지를 모상으로 하여, 이 모상 중에서 분산되는 형태인 것이 바람직하다. 특히, 가교제 등, 수지와 가교 구조를 형성하는 성분이 배합된 경우에는, 수지가 미가교 또는 반가교인 채로 포함되는 것이 바람직하다.Although the solar cell sealing agent composition of this invention can be manufactured by mixing raw material components, It is preferable that it is the form in which the ion trapping agent for solar cells, another component, etc. use resin as a mother phase, and are disperse|distributed in this mother phase. In particular, when a component that forms a crosslinked structure with a resin, such as a crosslinking agent, is blended, it is preferable that the resin is contained in an uncrosslinked or semi-crosslinked state.
따라서, 도 1에 있어서의 밀봉층(13)을 형성하는 경우에는, 예를 들어 본 발명의 태양 전지용 밀봉제 조성물을 혼련한 후, 압출기에 투입하고, T 다이 성형 또는 캘린더 성형에 의해 박육 형상으로 하고, 소정의 사이즈로 가공하여 얻어진 미가교 또는 반가교의 태양 전지 모듈용 밀봉재 시트를 사용하는 것이 바람직하다.Therefore, when forming the
3. 태양 전지 모듈3. Solar module
본 발명의 태양 전지 모듈은, 예를 들어 도 1에 도시되는 것처럼, 태양 전지 소자(11)와, 표면측 투명 보호 부재(15)와, 이면측 보호 부재(17)와, 상기 표면측 투명 보호 부재(15) 및 상기 이면측 보호 부재(17) 사이에, 태양 전지 소자(11)가, 상기 본 발명의 태양 전지용 밀봉제 조성물을 사용하여 밀봉(포매)된 밀봉층(13)을 구비한다. 태양 전지 소자(11)끼리는, 인터커넥터(19)에 의해 접속되어 있다. 또한, 도 1에서는 집전 전극 등을 생략하고 있다.The solar cell module of the present invention includes, for example, as shown in FIG. 1 , a
태양 전지 소자(11)는, 광전 효과에 의해 수광면에 입사된 광을 전기로 변환하는 기능을 갖는 것이며, 실리콘, 화합물 반도체 등을 포함하는 것이 바람직하다.The
밀봉층(13)은, 바람직하게는, 가교제를 함유하는 태양 전지용 밀봉제 조성물을 사용하여 형성된, 가교 수지 조성물을 포함하는 층이고, 태양 전지 소자(11) 및 인터커넥터(19)가 소정의 위치에 고정되도록 포매되어 있다.The
표면측 투명 보호 부재(15)는, 통상, 내후성, 내풍압성, 내우박성 등이 우수한 재료를 포함하며, 폴리에스테르 수지, 폴리카르보네이트 수지 등의 수지 또는 유리를 포함하는 것으로 할 수 있지만, 통상, 소다석회 유리 등의 유리를 포함한다.The surface-side transparent
이면측 보호 부재(17)는, 통상, 내가수분해 폴리에틸렌테레프탈레이트 수지, 폴리불화비닐 수지 등의, 내후성이 우수한 재료를 포함한다. 이면측 보호 부재(17)는, 밀봉층(13)을 투과한 광을 반사하는 작용을 가져도 된다.The backside
본 발명의 태양 전지 모듈 제조 방법은 특별히 제한되지 않으며, 종래 공지된 방법을 적용할 수 있다. 예를 들어, 이면측 보호 부재와, 가교제를 함유하는 태양 전지용 밀봉제 조성물을 사용하여 얻어진, 미가교 또는 반가교의 태양 전지 모듈용 밀봉재 시트와, 태양 전지 소자와, 가교제를 함유하는 태양 전지용 밀봉제 조성물을 사용하여 얻어진, 미가교 또는 반가교의 태양 전지 모듈용 밀봉재 시트와, 표면측 투명 보호 부재를, 이 순서대로 적층하여 적층물로 한 후, 이 적층물을 진공 상태에서 가열 압착하는 진공 가열 라미네이션에 제공하는 방법으로 할 수 있다. 이 진공 가열 라미네이션에 의해, 2장의 태양 전지 모듈용 밀봉재 시트 사이에 태양 전지 소자를 매몰시켜, 가교 수지 조성물을 형성함과 함께, 이것을 포함하는 밀봉층 및 이면측 보호 부재, 그리고 표면측 투명 보호 부재 및 밀봉층을, 각각 접착 일체화하여, 본 발명의 태양 전지 모듈을 제조할 수 있다.The solar cell module manufacturing method of the present invention is not particularly limited, and a conventionally known method may be applied. For example, an uncrosslinked or semi-crosslinked solar cell module sealing material sheet obtained using a back surface side protective member and a solar cell sealing agent composition containing a crosslinking agent, a solar cell element, and a solar cell sealing agent containing a crosslinking agent Vacuum heating lamination in which an uncrosslinked or semi-crosslinked sealing material sheet for a solar cell module obtained using the composition and a transparent protective member on the surface side are laminated in this order to form a laminate, and then the laminate is heat-compressed in a vacuum state. This can be done by providing By this vacuum heating lamination, a solar cell element is buried between two solar cell module sealing material sheets, and while forming a crosslinked resin composition, a sealing layer containing this, a back surface side protective member, and a surface side transparent protection member And the sealing layer can be each adhesively integrated, and the solar cell module of this invention can be manufactured.
본 발명의 태양 전지 모듈에 있어서, 밀봉층(13)이 특수한 이온 포착제를 함유하기 때문에, 태양 전지의 사용 중에 밀봉층(13) 중에 침입한 수분이나, 가수분해에서 발생한 산을 포획할뿐만 아니라, 태양 전지 소자(11)의 열화를 방지할 수 있고, 또한 표면측 투명 보호 부재가 유리를 포함하는 경우에 있어서, 유리로부터 밀봉층(13)에 대하여, PID(Potential-induced degradation; 태양 전지 모듈에 고전압이 가해져 출력이 대폭으로 저하되는 현상)의 주원인이 되는 나트륨 이온(Na+ 이온)이 침투해도 그 확산을 방지할 수 있어, 태양 전지 모듈(10)의 출력 저하를 억제할 수 있다.In the solar cell module of the present invention, since the
실시예Example
이하, 본 발명을 실시예에 의해 구체적으로 설명한다. 단, 본 발명은 하기의 실시예에 한정되는 것은 아니다.Hereinafter, the present invention will be specifically described by way of Examples. However, the present invention is not limited to the following examples.
1. 평가 방법1. Evaluation method
(1) pH 측정(1) pH measurement
하기 (2)에서 이온 포착제를 첨가한 후의 수용액, 또는 하기 (3)에서 얻어진 추출수의 pH를, 호리바 세이사꾸쇼사제 유리 전극식 수소 이온 농도 지시계 「D-51」(형식명)에 의해 측정하였다. 측정은, JIS Z 8802 「pH 측정 방법」에 준거하고, 측정 온도는 25℃이다.The pH of the aqueous solution after adding the ion trapping agent in (2) or the extracted water obtained in (3) below is measured by a glass electrode type hydrogen ion concentration indicator "D-51" (model name) manufactured by Horiba Seisakusho Co., Ltd. measured. The measurement is based on JIS Z 8802 "pH measuring method", and the measurement temperature is 25 degreeC.
(2) NaCl 수용액 중에 있어서의 태양 전지용 이온 포착제의 Na+ 이온 흡착능 (2) Na + ion adsorption capacity of the ion trapping agent for solar cells in NaCl aqueous solution
태양 전지용 이온 포착제의 Na+ 이온 흡착능을, ICP 발광 분광 분석법에 의해 평가하였다. 구체적인 평가 방법은 다음과 같다. The Na + ion adsorption capacity of the ion trapping agent for solar cells was evaluated by ICP emission spectroscopy. The specific evaluation method is as follows.
먼저, 물 1L에 0.254g NaCl을 용해하고, Na+ 이온이 100ppm인 수용액을 제조하였다. 그 수용액에 대하여 이온 포착제가 1.0질량％의 농도가 되도록 첨가하고, 충분히 혼합한 후, 정치하였다. 그리고, 이온 포착제를 첨가하여 8시간 후의 Na+ 이온 농도를 서모 피셔 사이언티픽사제 ICP 발광 분광 장치 「iCAP7600 DUO」(형식명)로 측정하였다. 그리고, Na+ 이온 포착률을 하기 식에 의해 구하였다.First, 0.254 g of NaCl was dissolved in 1 L of water, and an aqueous solution having Na + ions of 100 ppm was prepared. After adding and fully mixing an ion trapping agent so that it might become a density|concentration of 1.0 mass % with respect to the aqueous solution, it left still. Then, the Na + ion concentration 8 hours after adding the ion trapping agent was measured with an ICP emission spectrometer "iCAP7600 DUO" (model name) manufactured by Thermo Fisher Scientific. And the Na + ion capture rate was calculated|required by the following formula.
Na+ 이온 포착률=((초기 농도(100ppm)-시험 후(8시간 후)의 Na+ 이온 농도)/초기 농도(100ppm))×100Na+ ion capture rate = ((initial concentration (100 ppm) - Na + ion concentration after test (8 hours)) / initial concentration (100 ppm)) x 100
(3) 태양 전지용 밀봉제 조성물을 사용하여 형성된 가교 수지 시험편의 Na+ 이온 흡착능 (3) Na + ion adsorption capacity of the crosslinked resin test piece formed using the solar cell encapsulant composition
태양 전지용 이온 포착제 1.0질량부와, 미츠이 듀퐁 폴리케미컬사제 에틸렌·아세트산비닐 공중합 수지 「EV150R」(상품명) 100질량부와, 아르케마 요시토미사제 tert-부틸퍼옥시-2-에틸헥실카르보네이트 「루페록스 TBEC」(상품명, 가교제) 0.5질량부와, 아르케마 요시토미사제 2,5-디메틸-2,5-디(tert-부틸퍼옥시)헥산 「루페록스 101」(상품명, 가교제) 0.5질량부와, Sartomer사제 트리메틸올프로판트리메타크릴레이트 「SR350」(상품명, 가교 보조제) 1.0질량부와, Sartomer사제 트리알릴이소시아누레이트 「SR533」(상품명, 가교 보조제) 1.0질량부와, 기시다 가가꾸사제 염화나트륨 0.025질량부를 혼합하여 태양 전지용 밀봉제 조성물을 얻은 후, 메이끼 세이사쿠쇼사제 사출 성형기 「M-50A(II)-DM」(형식명)을 사용하고, 성형 온도를 150도 하여, 가교된 수지 시험편(110mm×110mm×2mm)을 얻었다. 또한, 상기 염화나트륨은, 실시예 및 비교예 간의, Na+ 이온 농도의 측정값의 차이를 현저하게 하기 위해 에틸렌·아세트산비닐 공중합 수지에 대한 나트륨량이 약 100ppm이 되도록 한 것이다.1.0 mass part of ion trapping agent for solar cells, 100 mass parts of ethylene/vinyl acetate copolymer resin "EV150R" (trade name) manufactured by Mitsui DuPont Polychemical Co., Ltd. (trade name), tert-butylperoxy-2-ethylhexyl carbonate manufactured by Arkema Yoshitomi Corporation 0.5 parts by mass of "Luperox TBEC" (trade name, crosslinking agent), and 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane "Luperox 101" (trade name, crosslinking agent) manufactured by Arkema Yoshitomi 0.5 1 part by mass, 1.0 parts by mass of trimethylolpropane trimethacrylate "SR350" (trade name, crosslinking aid) manufactured by Sartomer, 1.0 parts by mass of triallyl isocyanurate "SR533" (trade name, crosslinking aid) manufactured by Sartomer, group; After mixing 0.025 parts by mass of sodium chloride manufactured by Shida Chemical to obtain a solar cell sealing agent composition, an injection molding machine manufactured by Meiki Seisakusho Co., Ltd. "M-50A(II)-DM" (model name) was used, and the molding temperature was set to 150 degrees. Thus, a crosslinked resin test piece (110 mm × 110 mm × 2 mm) was obtained. In addition, the sodium chloride is such that the amount of sodium with respect to the ethylene/vinyl acetate copolymer resin is about 100 ppm in order to make the difference in the measured values of Na + ion concentration between the Examples and Comparative Examples remarkable.
이어서, 이 가교 수지 시험편 10g을 절삭 가공하여, 소편(5mm×5mm×2mm 정도)으로 하고, 순수 50mL와 함께 100mL의 폴리 용기에 넣어, 마개를 막았다. 그리고, 이 폴리 용기를 95℃에서 20시간 정치하였다. 그리고, 가교 수지 시험편으로부터 순수 중에 용출된 성분을 포함하는 추출수의 분석 및 pH 측정을 행하였다. Na+ 이온 농도를 ICP 발광 분광 분석으로 측정하였다. 또한, 아세트산 농도를 이온 크로마토그래피로 측정하였다.Next, 10 g of this crosslinked resin test piece was cut into small pieces (about 5 mm x 5 mm x 2 mm), put into a 100 mL poly container together with 50 mL of pure water, and capped. And this poly container was left still at 95 degreeC for 20 hours. Then, from the cross-linked resin test piece, the extraction water containing the component eluted in pure water was analyzed and the pH was measured. Na + ion concentrations were determined by ICP emission spectroscopy. In addition, the acetic acid concentration was measured by ion chromatography.
2. 이온 포착제의 제조 및 평가2. Preparation and evaluation of ion scavengers
실시예 1Example 1
순수 850mL에, 옥시염화지르코늄 8수화물 0.272몰을 용해한 후, 옥살산 2수화물 0.788몰을 첨가하고, 이것을 용해시켰다. 이 수용액을 교반하면서, 인산 0.57몰을 첨가하였다. 이것을 교반하면서, 103℃에서 8시간 환류하였다. 냉각 후, 얻어진 침전물을 물로 잘 세정한 후, 150℃에서 건조함으로써, 인산지르코늄을 포함하는 인편상 분말을 얻었다. 이 인산지르코늄에 대하여 분석한 결과, α-인산지르코늄(H형)(이하, 「α-인산지르코늄(Z1)」이라고 함)인 것을 확인하였다.After dissolving 0.272 mol of zirconium oxychloride octahydrate in 850 mL of pure water, 0.788 mol of oxalic acid dihydrate was added and this was dissolved. While stirring this aqueous solution, 0.57 mol of phosphoric acid was added. While stirring this, it refluxed at 103 degreeC for 8 hours. After cooling, the obtained deposit was washed well with water, and then dried at 150°C to obtain a flaky powder containing zirconium phosphate. As a result of analyzing this zirconium phosphate, it was confirmed that it was alpha-zirconium phosphate (H type) (henceforth "alpha-zirconium phosphate (Z1)").
상기 α-인산지르코늄(Z1)을, 불산을 첨가한 질산 중에서 자비 용해한 후, ICP 발광 분광 분석에 제공함으로써, 다음 조성식을 얻었다.The α-zirconium phosphate (Z1) was boiled and dissolved in nitric acid to which hydrofluoric acid was added, and then subjected to ICP emission spectroscopy to obtain the following compositional formula.
ZrH2.03(PO4)2.01·0.05H2OZrH 2.03 (PO 4 ) 2.01 0.05H 2 O
또한, α-인산지르코늄(Z1)의 메디안 직경을, 호리바 세이사꾸쇼제 레이저 회절식 입도 분포계 「LA-700」(형식명)에 의해 측정한 결과, 0.9㎛였다.Moreover, it was 0.9 micrometer as a result of measuring the median diameter of (alpha)- zirconium phosphate (Z1) by the Horiba Corporation laser diffraction type particle size distribution analyzer "LA-700" (model name).
이어서, α-인산지르코늄(Z1) 25g을, 0.1N-LiOH 수용액 1000mL를 교반하면서, 첨가하고, 이것을 8시간 교반하였다. 그 후, 침전물을 수세하고, 150℃에서 20시간 진공 건조하여, ZrLi1.03H1.00(PO4)2.01·0.05H2O를 포함하는 리튬 이온 치환형 α-인산지르코늄을 제조하였다. 칼 피셔법에 의한 수분 함유율은 0.5％였다. 이 리튬 이온 치환형 α인산지르코늄은, 모든 양이온 교환 용량 중, 4meq/g가 리튬 이온으로 치환된 것이다. 이하, 「4meq-Li 치환형 α-인산지르코늄 A1-1」로 하였다.Next, 25 g of α-zirconium phosphate (Z1) was added while stirring 1000 mL of a 0.1N-LiOH aqueous solution, followed by stirring for 8 hours. Thereafter, the precipitate was washed with water and vacuum dried at 150° C. for 20 hours to prepare a lithium ion-substituted α-zirconium phosphate containing ZrLi 1.03 H 1.00 (PO 4 ) 2.01 ·0.05H 2 O. The water content by the Karl Fischer method was 0.5%. In this lithium ion-substituted α zirconium phosphate, 4 meq/g of all cation exchange capacities were substituted with lithium ions. Hereinafter, it was set as "4meq-Li-substituted α-zirconium phosphate A1-1".
이어서, 이 4meq-Li 치환형 α-인산지르코늄 A1-1을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this 4meq-Li substitution type alpha-zirconium phosphate A1-1, said various evaluation was performed, and the result is shown in Table 1.
실시예 2Example 2
0.1N-LiOH 수용액의 사용량을 2500mL로 한 것 이외에는, 실시예 1과 동일한 조작을 행하여, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 리튬 이온으로 치환된, ZrLi2.03(PO4)2.01·0.05H2O를 포함하는 리튬 이온 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.3％였다. 이하, 「전체 Li 치환형 α-인산지르코늄 A1-2」로 하였다. ZrLi 2.03 (PO 4 ) 2.01 in which all cation exchangers (cation exchange capacity: 6.7 meq/g) were substituted with lithium ions, the same operation as in Example 1 was performed except that the amount of 0.1N-LiOH aqueous solution was 2500 mL. A lithium ion-substituted α-zirconium phosphate containing 0.05H 2 O was prepared. The water content was 0.3%. Hereinafter, it was set as "all Li-substituted type alpha-zirconium phosphate A1-2".
이어서, 이 전체 Li 치환형 α-인산지르코늄 A1-2를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, said various evaluation was performed using the ion trapping agent for solar cells containing this all Li-substituted alpha-zirconium phosphate A1-2, and the result is shown in Table 1.
실시예 3Example 3
0.1N-LiOH 수용액 대신에, 0.1N-KOH 수용액을 사용한 것 이외에는, 실시예 1과 동일한 조작을 행하여, ZrK1.03H1.00(PO4)2.01·0.03H2O를 포함하는 칼륨 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.5％였다. 이 칼륨 치환형 α-인산지르코늄은, 모든 양이온 교환 용량 중, 4meq/g가 리튬 이온으로 치환된 것이다. 이하, 「4meq-K 치환형 α-인산지르코늄 A1-3」으로 하였다.Potassium-substituted α-phosphate containing ZrK 1.03 H 1.00 (PO 4 ) 2.01 0.03H 2 O was carried out in the same manner as in Example 1 except that 0.1N-KOH aqueous solution was used instead of 0.1N-LiOH aqueous solution. Zirconium was prepared. The water content was 0.5%. In this potassium-substituted α-zirconium phosphate, 4 meq/g of all cation exchange capacities were substituted with lithium ions. Hereinafter, it was set as "4meq-K-substituted α-zirconium phosphate A1-3".
이어서, 이 4meq-K 치환형 α-인산지르코늄 A1-3을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this 4meq-K substitution type alpha-zirconium phosphate A1-3, said various evaluation was performed, and the result is shown in Table 1.
실시예 4Example 4
0.1N-KOH 수용액의 사용량을 2500mL로 한 것 이외에는, 실시예 3과 동일한 조작을 행하여, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 칼륨 이온으로 치환된, ZrK2.03(PO4)2.01을 포함하는 칼륨 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「전체 K 치환형 α-인산지르코늄 A1-4」로 하였다. ZrK 2.03 (PO 4 ) 2.01 in which all cation exchangers (cation exchange capacity: 6.7 meq/g) were substituted with potassium ions, the same operation as in Example 3 was performed except that the amount of 0.1N-KOH aqueous solution was 2500 mL. Potassium-substituted α-zirconium phosphate containing a was prepared. The water content was 0.4%. Hereinafter, it was set as "all K-substituted α-zirconium phosphate A1-4".
이어서, 이 전체 K 치환형 α-인산지르코늄 A1-4를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all-K-substituted alpha-zirconium phosphate A1-4, said various evaluation was performed, and the result is shown in Table 1.
실시예 5Example 5
탈이온수 850mL에, Hf의 함유량이 0.18％인 옥시염화지르코늄 8수화물 0.272몰을 용해한 후, 옥살산 2수화물 0.788몰을 첨가하고, 이것을 용해시켰다. 이 수용액을 교반하면서, 인산 0.57몰을 첨가하였다. 이것을 교반하면서, 98℃에서 8시간 환류하였다. 냉각 후, 얻어진 침전물을 물로 잘 세정한 후, 150℃에서 건조함으로써, 인산지르코늄을 포함하는 인편상 분말을 얻었다. 이 인산지르코늄에 대하여 분석한 결과, α-인산지르코늄(H형)(이하, 「α-인산지르코늄 (Z2)」라고 함)인 것을 확인하였다.In 850 mL of deionized water, 0.272 mol of zirconium oxychloride octahydrate having an Hf content of 0.18% was dissolved, and then 0.788 mol of oxalic acid dihydrate was added and this was dissolved. While stirring this aqueous solution, 0.57 mol of phosphoric acid was added. While stirring this, it refluxed at 98 degreeC for 8 hours. After cooling, the obtained deposit was washed well with water, and then dried at 150°C to obtain a flaky powder containing zirconium phosphate. As a result of analyzing this zirconium phosphate, it was confirmed that it was alpha-zirconium phosphate (H type) (henceforth "alpha-zirconium phosphate (Z2)").
상기 α-인산지르코늄 (Z2)를, 불산을 첨가한 질산 중에서 자비 용해한 후, ICP 발광 분광 분석에 제공함으로써, 다음 조성식을 얻었다.The α-zirconium phosphate (Z2) was boiled and dissolved in nitric acid to which hydrofluoric acid was added, and then subjected to ICP emission spectroscopy to obtain the following compositional formula.
Zr0.99Hf0.01H2.03(PO4)2.01·0.05H2OZr 0.99 Hf 0.01 H 2.03 (PO 4 ) 2.01 0.05H 2 O
또한, α-인산지르코늄 (Z2)의 메디안 직경은 0.8㎛였다.In addition, the median diameter of alpha-zirconium phosphate (Z2) was 0.8 micrometer.
이어서, α-인산지르코늄 (Z2) 25g을, 0.1N-LiOH 수용액 1000mL를 교반하면서 첨가하고, 이것을 8시간 교반하였다. 그 후, 침전물을 수세하고, 150℃에서 20시간 진공 건조하여, Zr0.99Hf0.01Li1.03H1.00(PO4)2.01·0.2H2O를 포함하는 리튬 이온 치환형 α-인산지르코늄을 제조하였다. 칼 피셔법에 의한 수분 함유율은 0.4％였다. 이 리튬 이온 치환형 α인산지르코늄은, 모든 양이온 교환 용량 중, 4meq/g가 리튬 이온으로 치환된 것이다. 이하, 「4meq-Li 치환형 α-인산지르코늄 A2-1」로 하였다.Next, 25 g of α-zirconium phosphate (Z2) was added while stirring 1000 mL of a 0.1N-LiOH aqueous solution, followed by stirring for 8 hours. Thereafter, the precipitate was washed with water and vacuum dried at 150° C. for 20 hours to prepare a lithium ion-substituted α-zirconium phosphate containing Zr 0.99 Hf 0.01 Li 1.03 H 1.00 (PO 4 ) 2.01 ·0.2H 2 O. The water content by the Karl Fischer method was 0.4%. In this lithium ion-substituted α zirconium phosphate, 4 meq/g of all cation exchange capacities were substituted with lithium ions. Hereinafter, it was referred to as "4meq-Li-substituted α-zirconium phosphate A2-1."
이어서, 이 4meq-Li 치환형 α-인산지르코늄 A2-1을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this 4meq-Li substitution type alpha-zirconium phosphate A2-1, said various evaluation was performed, and the result is shown in Table 1.
실시예 6Example 6
0.1N-LiOH 수용액의 사용량을 2500mL로 한 것 이외에는, 실시예 5와 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 리튬 이온으로 치환된, Zr0.99Hf0.01Li2.03(PO4)2.01·0.1H2O를 포함하는 리튬 이온 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.3％였다. 이하, 「전체 Li 치환형 α-인산지르코늄 A2-2」로 하였다. Zr 0.99 Hf 0.01 Li 2.03 (Zr 0.99 Hf 0.01 Li 2.03) in which all cation exchangers (cation exchange capacity: 6.7 meq/g) were substituted with lithium ions PO 4 ) A lithium ion-substituted α-zirconium phosphate containing 2.01 ·0.1H 2 O was prepared. The water content was 0.3%. Hereinafter, it was set as "all Li-substituted α-zirconium phosphate A2-2".
이어서, 이 전체 Li 치환형 α-인산지르코늄 A2-2를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Li-substituted alpha-zirconium phosphate A2-2, said various evaluation was performed, and the result is shown in Table 1.
실시예 7Example 7
0.1N-LiOH 수용액 대신에, 0.1N-KOH 수용액을 사용한 것 이외에는, 실시예 5와 동일한 조작을 행하고, Zr0.99Hf0.01K1.03H1.00(PO4)2.01·0.03H2O를 포함하는 칼륨 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.5％였다. 이 칼륨 치환형 α-인산지르코늄은, 모든 양이온 교환 용량 중, 4meq/g가 리튬 이온으로 치환된 것이다. 이하, 「4meq-K 치환형 α-인산지르코늄 A2-3」으로 하였다.Potassium substitution containing Zr 0.99 Hf 0.01 K 1.03 H 1.00 (PO 4 ) 2.01 0.03H 2 O was carried out in the same manner as in Example 5 except that a 0.1N-KOH aqueous solution was used instead of the 0.1N-LiOH aqueous solution. Form α-zirconium phosphate was prepared. The water content was 0.5%. In this potassium-substituted α-zirconium phosphate, 4 meq/g of all cation exchange capacities were substituted with lithium ions. Hereinafter, it was set as "4meq-K-substituted α-zirconium phosphate A2-3".
이어서, 이 4meq-K 치환형 α-인산지르코늄 A2-3을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this 4meq-K substitution type alpha-zirconium phosphate A2-3, said various evaluation was performed, and the result is shown in Table 1.
실시예 8Example 8
0.1N-KOH 수용액의 사용량을 2500mL로 한 것 이외에는, 실시예 7과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 칼륨 이온으로 치환된, Zr0.99Hf0.01K2.03(PO4)2.01을 포함하는 칼륨 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「전체 K 치환형 α-인산지르코늄 A2-4」로 하였다.Zr 0.99 Hf 0.01 K 2.03 (Zr 0.99 Hf 0.01 K 2.03 ( PO 4 ) Potassium-substituted α-zirconium phosphate containing 2.01 was prepared. The water content was 0.4%. Hereinafter, it was set as "all K-substituted α-zirconium phosphate A2-4".
이어서, 이 전체 K 치환형 α-인산지르코늄 A2-4를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, said various evaluation was performed using the ion trapping agent for solar cells containing this all K-substituted alpha-zirconium phosphate A2-4, and the result is shown in Table 1.
실시예 9Example 9
0.1N-LiOH 수용액 대신에, 0.1N-Rb2CO3 수용액 2500mL를 사용한 것 이외에는, 실시예 5와 동일한 조작을 행하여, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 루비듐 이온으로 치환된 루비듐 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 Rb 치환형 α-인산지르코늄 A2-5」로 하였다. In the same manner as in Example 5, except that 2500 mL of 0.1N-Rb 2 CO 3 aqueous solution was used instead of 0.1N-LiOH aqueous solution, all cation exchangers (cation exchange capacity: 6.7 meq/g) were replaced with rubidium ions. Rubidium-substituted α-zirconium phosphate was prepared. The water content was 0.5%. Hereinafter, it was set as "all Rb-substituted α-zirconium phosphate A2-5".
이어서, 이 전체 Rb 치환형 α-인산지르코늄 A2-5를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, said various evaluation was performed using the ion trapping agent for solar cells containing this all Rb substitution type alpha-zirconium phosphate A2-5, and the result is shown in Table 1.
실시예 10Example 10
0.1N-LiOH 수용액 대신에, 0.1N-Cs2CO3 수용액 2500mL를 사용한 것 이외에는, 실시예 5와 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 세슘 이온으로 치환된 세슘 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「전체 Cs 치환형 α-인산지르코늄 A2-6」으로 하였다. The same operation as in Example 5 was performed except that 2500 mL of 0.1N-Cs 2 CO 3 aqueous solution was used instead of 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 6.7 meq/g) were replaced with cesium ions. A cesium-substituted α-zirconium phosphate was prepared. The water content was 0.4%. Hereinafter, it was set as "all Cs-substituted α-zirconium phosphate A2-6".
이어서, 이 전체 Cs 치환형 α-인산지르코늄 A2-6을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Cs-substituted alpha-zirconium phosphate A2-6, said various evaluation was performed, and the result is shown in Table 1.
실시예 11Example 11
0.1N-LiOH 수용액 대신에, 0.1N-(CH3COO)2Mg 수용액 2500mL를 사용한 것 이외에는, 실시예 5와 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 마그네슘 이온으로 치환된 마그네슘 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 Mg 치환형 α-인산지르코늄 A2-7」로 하였다. The same operation as in Example 5 was performed except that 2500 mL of a 0.1N-(CH 3 COO) 2 Mg aqueous solution was used instead of the 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 6.7 meq/g) were converted to magnesium ions. Magnesium-substituted α-zirconium phosphate substituted with was prepared. The water content was 0.5%. Hereinafter, it was set as "all Mg substitution type alpha-zirconium phosphate A2-7".
이어서, 이 전체 Mg 치환형 α-인산지르코늄 A2-7을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Mg substitution type alpha-zirconium phosphate A2-7, said various evaluation was performed, and the result is shown in Table 1.
실시예 12Example 12
0.1N-LiOH 수용액 대신에, 0.1N-(CH3COO)2Ca 수용액 2500mL를 사용한 것 이외에는, 실시예 5와 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 칼슘 이온으로 치환된 칼슘 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.6％였다. 이하, 「전체 Ca 치환형 α-인산지르코늄 A2-8」로 하였다. The same operation as in Example 5 was performed except that 2500 mL of 0.1N-(CH 3 COO) 2 Ca aqueous solution was used instead of 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 6.7 meq/g) were converted to calcium ions Calcium-substituted α-zirconium phosphate substituted with was prepared. The water content was 0.6%. Hereinafter, it was referred to as "all Ca-substituted α-zirconium phosphate A2-8."
이어서, 이 전체 Ca 치환형 α-인산지르코늄 A2-8을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, said various evaluation was performed using the ion trapping agent for solar cells containing this all Ca substitution type alpha-zirconium phosphate A2-8, and the result is shown in Table 1.
실시예 13Example 13
탈이온수 400mL에, 75％ 인산 405g을 추가하고, 이 수용액을 교반하면서, 황산티타닐(TiO2 환산 함유량: 33％) 137g을 첨가하였다. 이것을 교반하면서 100℃에서 48시간 환류하였다. 냉각 후, 얻어진 침전물을 물로 잘 세정하고, 150℃에서 건조함으로써, 인산티타늄을 포함하는 인편상 분말을 얻었다. 이 인산티타늄에 대하여 분석한 결과, α-인산티타늄(H형)인 것을 확인하였다.To 400 mL of deionized water, 405 g of 75% phosphoric acid was added, and while the aqueous solution was stirred, 137 g of titanyl sulfate (TiO 2 converted content: 33%) was added. This was refluxed at 100°C for 48 hours while stirring. After cooling, the obtained precipitate was washed well with water and dried at 150°C to obtain a flaky powder containing titanium phosphate. As a result of analyzing this titanium phosphate, it was confirmed that it was α-titanium phosphate (type H).
상기 α-인산티타늄을, 불산을 첨가한 질산 중에서 자비 용해한 후, ICP 발광 분광 분석에 제공함으로써, 다음 조성식을 얻었다.The α-titanium phosphate was boiled in nitric acid to which hydrofluoric acid was added, and then subjected to ICP emission spectroscopy to obtain the following compositional formula.
TiH2.03(PO4)2.01·0.1H2OTiH 2.03 (PO 4 ) 2.01 0.1H 2 O
또한, α-인산티타늄의 메디안 직경을 측정한 결과, 0.7㎛였다.Moreover, as a result of measuring the median diameter of (alpha)- titanium phosphate, it was 0.7 micrometer.
이어서, α-인산티타늄 25g을 0.1N-LiOH 수용액 1000mL에 교반하면서, 첨가하고, 이것을 8시간 교반하였다. 그 후, 침전물을 수세하고, 150℃에서 20시간 진공 건조하여, TiLi1.03H1.00(PO4)2.01·0.2H2O를 포함하는 리튬 이온 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.5％였다. 이 리튬 이온 치환형 α-인산티타늄은, 모든 양이온 교환 용량 중, 4meq/g가 리튬 이온으로 치환된 것이다. 이하, 「4meq-Li 치환형 α-인산티타늄 B-1」로 하였다.Then, 25 g of α-titanium phosphate was added to 1000 mL of 0.1N-LiOH aqueous solution while stirring, and this was stirred for 8 hours. Thereafter, the precipitate was washed with water and vacuum dried at 150° C. for 20 hours to prepare a lithium ion-substituted α-titanium phosphate containing TiLi 1.03 H 1.00 (PO 4 ) 2.01 ·0.2H 2 O. The water content was 0.5%. In this lithium ion-substituted α-titanium phosphate, 4 meq/g of all cation exchange capacities are substituted with lithium ions. Hereinafter, it was referred to as "4meq-Li-substituted α-titanium phosphate B-1."
이어서, 이 4meq-Li 치환형α-인산티타늄 B-1을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this 4meq-Li substitution type alpha-titanium phosphate B-1, said various evaluation was performed, and the result is shown in Table 1.
실시예 14Example 14
0.1N-LiOH 수용액의 사용량을 2500mL로 한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 리튬 이온으로 치환된, TiLi2.03(PO4)2.01·0.1H2O를 포함하는 리튬 이온 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「전체 Li 치환형 α-인산티타늄 B-2」로 하였다. TiLi 2.03 (PO 4 ) 2.01 in which all cation exchangers (cation exchange capacity: 7.0 meq/g) were substituted with lithium ions, the same operation as in Example 13 was carried out except that the amount of 0.1N-LiOH aqueous solution was 2500 mL. A lithium ion-substituted α-titanium phosphate containing 0.1H 2 O was prepared. The water content was 0.4%. Hereinafter, it was set as "all Li-substituted type alpha-titanium phosphate B-2".
이어서, 이 전체 Li 치환형 α-인산티타늄 B-2를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Li-substituted alpha-titanium phosphate B-2, said various evaluation was performed, and the result is shown in Table 1.
실시예 15Example 15
0.1N-LiOH 수용액 대신에, 0.1N-KOH 수용액을 사용한 것 이외에는, 실시예 13과 동일한 조작을 행하고, TiK1.03H1.00(PO4)2.01·0.05H2O를 포함하는 칼륨 이온 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「4meq-K 치환형 α-인산티타늄 B-3」으로 하였다.Potassium ion substitution type α- containing TiK 1.03 H 1.00 (PO 4 ) 2.01 ·0.05H 2 O was carried out in the same manner as in Example 13 except that 0.1N-KOH aqueous solution was used instead of 0.1N-LiOH aqueous solution. Titanium phosphate was prepared. The water content was 0.4%. Hereinafter, it was referred to as "4meq-K-substituted α-titanium phosphate B-3".
이어서, 이 4meq-K 치환형 α-인산티타늄 B-3을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this 4meq-K substitution type alpha-titanium phosphate B-3, said various evaluation was performed, and the result is shown in Table 1.
실시예 16Example 16
0.1N-KOH 수용액의 사용량을 2500mL로 한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 칼륨 이온으로 치환된, TiK2.03(PO4)2.00을 포함하는 칼륨 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 K 치환형 α-인산티타늄 B-4」로 하였다. TiK 2.03 (PO 4 ) 2.00 in which all cation exchangers (cation exchange capacity: 7.0 meq/g) were substituted with potassium ions, the same operation as in Example 13 was performed except that the amount of 0.1N-KOH aqueous solution was 2500 mL. A potassium-substituted α-titanium phosphate containing a was prepared. The water content was 0.5%. Hereinafter, it was referred to as "all K-substituted α-titanium phosphate B-4".
이어서, 이 전체 K 치환형 α-인산티타늄 B-4를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all-K-substituted alpha-titanium phosphate B-4, said various evaluation was performed, and the result is shown in Table 1.
실시예 17Example 17
0.1N-LiOH 수용액 대신에, 0.1N-Rb2CO3 수용액 2500mL를 사용한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 루비듐 이온으로 치환된 루비듐 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「전체 Rb 치환형 α-인산티타늄 B-5」로 하였다. The same operation as in Example 13 was performed except that 2500 mL of a 0.1N-Rb 2 CO 3 aqueous solution was used instead of the 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 7.0 meq/g) were replaced with rubidium ions. Rubidium-substituted α-titanium phosphate was prepared. The water content was 0.4%. Hereinafter, it was referred to as "all Rb-substituted α-titanium phosphate B-5".
이어서, 이 전체 Rb 치환형 α-인산티타늄 B-5를 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Rb-substituted alpha-titanium phosphate B-5, said various evaluation was performed, and the result is shown in Table 1.
실시예 18Example 18
0.1N-LiOH 수용액 대신에, 0.1N-Cs2CO3 수용액 2500mL를 사용한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 세슘 이온으로 치환된 세슘 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 Cs 치환형 α-인산티타늄 B-6」으로 하였다. The same operation as in Example 13 was performed except that 2500 mL of 0.1N-Cs 2 CO 3 aqueous solution was used instead of 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 7.0 meq/g) were replaced with cesium ions. A cesium-substituted α-titanium phosphate was prepared. The water content was 0.5%. Hereinafter, it was referred to as "all Cs-substituted α-titanium phosphate B-6".
이어서, 이 전체 Cs 치환형 α-인산티타늄 B-6을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Cs-substituted alpha-titanium phosphate B-6, said various evaluation was performed, and the result is shown in Table 1.
실시예 19Example 19
0.1N-LiOH 수용액 대신에, 0.1N-(CH3COO)2Mg 수용액 2500mL를 사용한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 마그네슘 이온으로 치환된 마그네슘 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 Mg 치환형 α-인산티타늄 B-7」로 하였다. The same operation as in Example 13 was performed except that 2500 mL of a 0.1N-(CH 3 COO) 2 Mg aqueous solution was used instead of the 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 7.0 meq/g) were converted to magnesium ions. A magnesium-substituted α-titanium phosphate substituted with was prepared. The water content was 0.5%. Hereinafter, it was set as "all Mg substitution type alpha-titanium phosphate B-7".
이어서, 이 전체 Mg 치환형 α-인산티타늄 B-7을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Mg-substituted alpha-titanium phosphate B-7, said various evaluation was performed, and the result is shown in Table 1.
실시예 20Example 20
0.1N-LiOH 수용액 대신에, 0.1N-(CH3COO)2Ca 수용액 2500mL를 사용한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 칼슘 이온으로 치환된 칼슘 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.4％였다. 이하, 「전체 Ca 치환형 α-인산티타늄 B-8」로 하였다. The same operation as in Example 13 was performed except that 2500 mL of a 0.1N-(CH 3 COO) 2 Ca aqueous solution was used instead of the 0.1N-LiOH aqueous solution, and all cation exchangers (cation exchange capacity: 7.0 meq/g) were converted to calcium ions Calcium-substituted α-titanium phosphate substituted with was prepared. The water content was 0.4%. Hereinafter, it was set as "all Ca-substituted α-titanium phosphate B-8".
이어서, 이 전체 Ca 치환형 α-인산티타늄 B-8을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.Next, using the ion trapping agent for solar cells containing this all Ca-substituted alpha-titanium phosphate B-8, said various evaluation was performed, and the result is shown in Table 1.
실시예 21Example 21
전체 Li 치환형 α-인산지르코늄 A1-2 및 전체 K 치환형 α-인산지르코늄 A1-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.All Li-substituted α-zirconium phosphate A1-2 and all K-substituted α-zirconium phosphate A1-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 1.
실시예 22Example 22
전체 Li 치환형 α-인산지르코늄 A1-2 및 전체 Li 치환형 α-인산지르코늄 A2-2를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.All Li-substituted α-zirconium phosphate A1-2 and all Li-substituted α-zirconium phosphate A2-2 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 1.
실시예 23Example 23
전체 Li 치환형 α-인산지르코늄 A1-2 및 전체 K 치환형 α-인산지르코늄 A2-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.All Li-substituted α-zirconium phosphate A1-2 and all K-substituted α-zirconium phosphate A2-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 1.
실시예 24Example 24
전체 Li 치환형 α-인산지르코늄 A1-2 및 전체 Li 치환형 α-인산티타늄 B-2를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 1에 나타내었다.All Li-substituted α-zirconium phosphate A1-2 and all Li-substituted α-titanium phosphate B-2 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 1.
실시예 25Example 25
전체 Li 치환형 α-인산지르코늄 A1-2 및 전체 K 치환형 α-인산티타늄 B-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All Li-substituted α-zirconium phosphate A1-2 and all K-substituted α-titanium phosphate B-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 26Example 26
전체 K 치환형 α-인산지르코늄 A1-4 및 전체 Li 치환형 α-인산지르코늄 A2-2를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All K-substituted α-zirconium phosphate A1-4 and all Li-substituted α-zirconium phosphate A2-2 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 27Example 27
전체 K 치환형 α-인산지르코늄 A1-4 및 전체 K 치환형 α-인산지르코늄 A2-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All K-substituted α-zirconium phosphate A1-4 and all K-substituted α-zirconium phosphate A2-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 28Example 28
전체 K 치환형 α-인산지르코늄 A1-4 및 전체 Li 치환형 α-인산티타늄 B-2를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All K-substituted α-zirconium phosphate A1-4 and all Li-substituted α-titanium phosphate B-2 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 29Example 29
전체 K 치환형 α-인산지르코늄 A1-4 및 전체 K 치환형 α-인산티타늄 B-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All K-substituted α-zirconium phosphate A1-4 and all K-substituted α-titanium phosphate B-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 30Example 30
전체 Li 치환형 α-인산지르코늄 A2-2 및 전체 K 치환형 α-인산지르코늄 A2-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All Li-substituted α-zirconium phosphate A2-2 and all K-substituted α-zirconium phosphate A2-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 31Example 31
전체 Li 치환형 α-인산지르코늄 A2-2 및 전체 Li 치환형 α-인산티타늄 B-2를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All Li-substituted α-zirconium phosphate A2-2 and all Li-substituted α-titanium phosphate B-2 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 32Example 32
전체 Li 치환형 α-인산지르코늄 A2-2 및 전체 K 치환형 α-인산티타늄 B-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All Li-substituted α-zirconium phosphate A2-2 and all K-substituted α-titanium phosphate B-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 33Example 33
전체 K 치환형 α-인산지르코늄 A2-4 및 전체 Li 치환형 α-인산티타늄 B-2를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All K-substituted α-zirconium phosphate A2-4 and all Li-substituted α-titanium phosphate B-2 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 34Example 34
전체 K 치환형 α-인산지르코늄 A2-4 및 전체 K 치환형 α-인산티타늄 B-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All K-substituted α-zirconium phosphate A2-4 and all K-substituted α-titanium phosphate B-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
실시예 35Example 35
전체 Li 치환형 α-인산티타늄 B-2 및 전체 K 치환형 α-인산티타늄 B-4를, 질량비 1:1로 혼합하여 태양 전지용 이온 포착제를 얻었다. 그리고, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.All Li-substituted α-titanium phosphate B-2 and all K-substituted α-titanium phosphate B-4 were mixed at a mass ratio of 1:1 to obtain an ion trapping agent for solar cells. And said various evaluation was performed, and the result is shown in Table 2.
비교예 1Comparative Example 1
양이온으로 치환되어 있지 않은 α-인산지르코늄(H형)인, 도아 고세사제 무기 이온 교환체 「IXE100」(상품명)을 그대로 사용하고, 각종 평가를 행하였다. 결과를 표 2에 나타내었다.Various evaluations were performed using the inorganic ion exchanger "IXE100" (trade name) manufactured by Toagosei Corporation, which is α-zirconium phosphate (type H) not substituted with a cation as it is. The results are shown in Table 2.
비교예 2Comparative Example 2
0.1N-LiOH 수용액 대신에, 0.1N-NaOH 수용액 2500mL를 사용한 것 이외에는, 실시예 5와 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 6.7meq/g)가 나트륨 이온으로 치환된, Zr0.99Hf0.01Na2.03(PO4)2.01·0.05H2O를 포함하는 나트륨 치환형 α-인산지르코늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 Na 치환형 α-인산지르코늄」으로 하였다. Zr 0.99 , in which all cation exchangers (cation exchange capacity: 6.7 meq/g) were substituted with sodium ions, the same operation as in Example 5 was performed except that 2500 mL of 0.1N-NaOH aqueous solution was used instead of 0.1N-LiOH aqueous solution Sodium-substituted α-zirconium phosphate containing Hf 0.01 Na 2.03 (PO 4 ) 2.01 ·0.05H 2 O was prepared. The water content was 0.5%. Hereinafter, it was set as "all Na-substituted α-zirconium phosphate."
이어서, 이 전체 Na 치환형 α-인산지르코늄을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.Next, said various evaluation was performed using the ion trapping agent for solar cells containing this Na-substituted type alpha-zirconium phosphate, and the result is shown in Table 2.
비교예 3Comparative Example 3
실시예 13에서 제조된 α-인산티타늄(H형)을 그대로 사용하고, 각종 평가를 행하였다. 결과를 표 2에 나타내었다.The α-titanium phosphate (type H) prepared in Example 13 was used as it was, and various evaluations were performed. The results are shown in Table 2.
비교예 4Comparative Example 4
0.1N-LiOH 수용액 대신에, 0.1N-NaOH 수용액 2500mL를 사용한 것 이외에는, 실시예 13과 동일한 조작을 행하고, 모든 양이온 교환기(양이온 교환 용량: 7.0meq/g)가 나트륨 이온으로 치환된, TiNa2.03(PO4)2.00·0.05H2O를 포함하는 나트륨 치환형 α-인산티타늄을 제조하였다. 수분 함유율은 0.5％였다. 이하, 「전체 Na 치환형 α-인산티타늄」으로 하였다.Instead of 0.1N-LiOH aqueous solution, 0.1N-NaOH aqueous solution was used to 2500mL, performed in the same manner as in Example 13, all the cation-exchange (cation exchange capacity: 7.0meq / g) substituted by a sodium ion, TiNa 2.03 (PO 4 ) Sodium-substituted α-titanium phosphate containing 2.00 ·0.05H 2 O was prepared. The water content was 0.5%. Hereinafter, it was set as "all Na-substituted alpha-titanium phosphate".
이어서, 이 전체 Na 치환형 α-인산티타늄을 포함하는 태양 전지용 이온 포착제를 사용하여, 상기의 각종 평가를 행하고, 그 결과를 표 2에 나타내었다.Next, using the ion trapping agent for solar cells containing this total Na-substituted alpha-titanium phosphate, said various evaluation was performed, and the result is shown in Table 2.
비교예 5Comparative Example 5
미즈사와 가가꾸사제 Y형 제올라이트 「미즈카시브스 Y-520」(상품명)을 150℃에서 20시간 건조한 후, 각종 평가를 행하였다. 결과를 표 2에 나타내었다.After drying the Y-type zeolite "Mizuka Sieves Y-520" (trade name) manufactured by Mizusawa Chemical Co., Ltd. at 150°C for 20 hours, various evaluations were performed. The results are shown in Table 2.
표 1 및 표 2로부터, 실시예 1 내지 35의 태양 전지용 이온 포착제는, NaCl 수용액 중에 있어서의 Na+ 이온의 포착률이 높고, 또한 pH의 변동이 1 이내인 것을 알 수 있었다. 또한, 가교 수지 시험편을 순수에 침지한 후의 추출수 중에 있어서도, 실시예 1 내지 35의 태양 전지용 이온 포착제는, Na+ 이온의 높은 용출 억제 성능을 나타내었다. 이들의 결과로부터, 본 발명의 이온 포착제는, 태양 전지의 PID의 원인으로 여겨지고 있는 Na+ 이온을 흡착하는 한편, pH의 변동이 없기 때문에, 밀봉 수지의 열화를 촉진하지 않고, 태양 전지의 PID를 억제할 수 있다.From Table 1 and Table 2, it turned out that the ion trapping agent for solar cells of Examples 1-35 has a high Na + ion capture rate in NaCl aqueous solution, and the fluctuation|variation of pH is less than 1. Moreover, also in the extraction water after immersing a crosslinked resin test piece in pure water, the ion trapping agents for solar cells of Examples 1-35 showed the high elution suppression performance of Na + ion. From these results, while the ion trapping agent of this invention adsorb|sucks Na + ion which is considered to be the cause of PID of a solar cell, since there is no fluctuation|variation in pH, it does not accelerate|stimulate deterioration of sealing resin, but PID of a solar cell. can suppress.
본 발명의 태양 전지용 이온 포착제는, 태양 전지의 PID의 원인이 되는 Na+ 이온을 고선택적으로 흡착하고, H+ 이온을 방출하기 어려우므로, 태양 전지 모듈을 구성하는 밀봉층, 이면측 보호 부재 등을 형성하는 부재에 함유시킬 수 있다. 이에 의해, 내구성이 우수한 태양 전지를 형성할 수 있다. 또한, 은 전극의 페이스트 등에도 첨가하여 사용하는 것이 가능하다.Since the ion trapping agent for solar cells of the present invention highly selectively adsorbs Na + ions that cause PID of the solar cell and hardly releases H + ions, the sealing layer constituting the solar cell module and the backside protective member It can be contained in the member which forms a etc. Thereby, a solar cell excellent in durability can be formed. Moreover, it is possible to add and use it also to the paste etc. of a silver electrode.
10: 태양 전지 모듈, 11: 태양 전지 소자, 13: 밀봉층, 15: 표면측 투명 보호 부재, 17: 이면측 보호 부재, 19: 인터커넥터10 solar cell module, 11: solar cell element, 13 sealing layer, 15 front side transparent protection member, 17 back side protection member, 19 interconnector
Claims (8)
Zr1-xHfxHa(PO4)b·mH2O (1)
(식 중, 0≤x≤0.2이고, 2<b≤2.1이고, a는 3b-a=4를 만족시키는 수이고, 0≤m≤2임)The ion trapping agent for solar cells according to claim 1 or 2, wherein the α-zirconium phosphate before being substituted with the ion (a1) is a compound represented by the following formula (1).
Zr 1-x Hf x H a (PO 4 ) b mH 2 O (1)
(Wherein, 0≤x≤0.2, 2<b≤2.1, a is a number that satisfies 3b-a=4, and 0≤m≤2)
TiHs(PO4)t·nH2O (2)
(식 중, 2<t≤2.1이고, s는 3t-s=4를 만족시키는 수이고, 0≤n≤2임)The ion trapping agent for solar cells according to claim 1 or 2, wherein the α-titanium phosphate before being substituted with the ion (b1) is a compound represented by the following formula (2).
TiH s (PO 4 ) t nH 2 O (2)
(Wherein, 2<t≤2.1, s is a number that satisfies 3t-s=4, and 0≤n≤2)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| PCT/JP2017/008215 WO2017175524A1 (en) | 2016-04-05 | 2017-03-02 | Ion scavenger for solar cell, solar cell sealant composition containing same, and solar cell module |
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| KR102612759B1 (en) * | 2017-12-15 | 2023-12-13 | 도아고세이가부시키가이샤 | Ion trapper, separator for lithium ion battery and lithium ion secondary battery |
| EP3820938B1 (en) * | 2018-07-12 | 2022-06-01 | SABIC Global Technologies B.V. | Photovoltaic element and polymer composition for front sheet thereof |
| CN110229623A (en) * | 2019-06-28 | 2019-09-13 | 北京知淘科技有限责任公司 | A kind of solar photovoltaic assembly packaging EVA adhesive film and preparation method thereof |
| EP4328263A1 (en) * | 2021-11-10 | 2024-02-28 | LG Chem, Ltd. | Crosslinking aid composition for olefin-based copolymer, crosslinking agent composition, and additive for optical device encapsulant composition |
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| JP2015032804A (en) | 2013-08-07 | 2015-02-16 | 東レ株式会社 | Encapsulant for solar cell, and solar cell module using the same |
| JP2015138805A (en) * | 2014-01-20 | 2015-07-30 | 東洋インキＳｃホールディングス株式会社 | Resin composition for solar cell sealing material, and solar cell sealing material |
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| US4180551A (en) * | 1971-04-08 | 1979-12-25 | Texas A&M University System | Modified zirconium phosphates |
| JPH10192697A (en) * | 1997-01-09 | 1998-07-28 | Toagosei Co Ltd | Adsorbent for cobalt or manganese ions |
| JP2011077172A (en) | 2009-09-29 | 2011-04-14 | Toppan Printing Co Ltd | Sealing material sheet and solar battery module |
| US9460829B2 (en) | 2011-09-01 | 2016-10-04 | Sumitomo Chemical Company, Limited | Resin composition, resin pellet, method for producing resin pellet, and solar cell encapsulant |
| KR20140072934A (en) * | 2012-12-03 | 2014-06-16 | 도레이첨단소재 주식회사 | Encapsulation composition for a solarcell and preparing process fo the sheet using the same |
| JP2015159189A (en) * | 2014-02-24 | 2015-09-03 | 旭化成株式会社 | Solar battery resin seal sheet |
| CN104530994B (en) * | 2014-12-30 | 2016-09-14 | 苏州度辰新材料有限公司 | A kind of anti-PID packaging adhesive film for photovoltaic cell |
| US20180166749A1 (en) * | 2015-06-04 | 2018-06-14 | Toagosei Co., Ltd. | Ion-trapping agent, electrolyte solution, and separator for lithium-ion rechargeable battery, and lithium-ion rechargeable battery |
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| JP2015138805A (en) * | 2014-01-20 | 2015-07-30 | 東洋インキＳｃホールディングス株式会社 | Resin composition for solar cell sealing material, and solar cell sealing material |
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| TW201808796A (en) | 2018-03-16 |
| KR20180132709A (en) | 2018-12-12 |
| CN108778991B (en) | 2021-11-16 |
| JPWO2017175524A1 (en) | 2019-02-07 |
| TWI731941B (en) | 2021-07-01 |
| CN108778991A (en) | 2018-11-09 |
| JP6658871B2 (en) | 2020-03-04 |
| WO2017175524A1 (en) | 2017-10-12 |
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