TWI610392B - Method for preparing photovoltaic element - Google Patents

Method for preparing photovoltaic element Download PDF

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TWI610392B
TWI610392B TW105128601A TW105128601A TWI610392B TW I610392 B TWI610392 B TW I610392B TW 105128601 A TW105128601 A TW 105128601A TW 105128601 A TW105128601 A TW 105128601A TW I610392 B TWI610392 B TW I610392B
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carbonate
polymer layer
photovoltaic element
organic solvent
chemical formula
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TW105128601A
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TW201810494A (en
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Ling Chang
Hou Te Lu
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Daxin Mat Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
    • H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
    • H01L21/568—Temporary substrate used as encapsulation process aid

Abstract

一種光電元件的製備方法，包含：(a)於承載材上形成一層高分子層，該高分子層是以一種於光線照射下會產生降解的材料為主；(b)於高分子層上形成光電元件；(c)對該高分子層施加光線照射，以使高分子層產生降解，並使承載材與光電元件分離；及(d)利用清洗組成物清洗承載材或光電元件，清洗組成物包含由化學式1所示的鏈狀碳酸酯，及漢森溶解度參數範圍為9~15(cal/cm 3) 1/2的有機溶劑。本發明光電元件的製備方法透過使用該清洗組成物，而能使該高分子層不會殘留於該光電元件或該承載材上，也有助於回收該承載材。 A method for preparing a photovoltaic element includes: (a) forming a polymer layer on a carrier material, the polymer layer is mainly a material that will degrade under light irradiation; (b) forming on the polymer layer Photoelectric elements; (c) applying light to the polymer layer to degrade the polymer layer and separate the carrier material from the optoelectronic element; and (d) cleaning the carrier material or the optoelectronic element with a cleaning composition to clean the composition It includes a chain carbonate represented by Chemical Formula 1 and an organic solvent having a Hansen solubility parameter ranging from 9 to 15 (cal / cm 3 ) 1/2 . The method for preparing a photovoltaic element of the present invention can prevent the polymer layer from remaining on the photovoltaic element or the supporting material by using the cleaning composition, and also helps to recover the supporting material.

Description

光電元件的製備方法Preparation method of photoelectric element

本發明是有關於一種光電元件的製備方法，特別是指一種利用光線照射來分離承載材與光電元件的光電元件的製備方法。The invention relates to a method for preparing a photovoltaic element, in particular to a method for preparing a photovoltaic element that separates a carrier material from a photovoltaic element by irradiating light.

在光電、電子、半導體領域中，大多以多層薄膜基板 (也就是積體電路集成基板)進行光電或半導體裝置的製作。隨著功能性光電元件數量的增加以及光電裝置的微小化需求，多層薄膜基板也被要求具備高精密度，而於製作過程中需特別維持尺寸安定性。為了維持良好的尺寸安定性，目前最常使用的改良方式是在一個剛性承載板上進行多層薄膜基板的製作；但是，如何將承載板與多層薄膜基板進行分離，也成為後續衍生需解決的問題。In the fields of optoelectronics, electronics, and semiconductors, many multilayer film substrates (that is, integrated circuit integrated substrates) are used for the manufacture of optoelectronic or semiconductor devices. With the increase in the number of functional optoelectronic elements and the miniaturization of optoelectronic devices, multi-layer thin-film substrates are also required to have high precision, and dimensional stability must be particularly maintained during the manufacturing process. In order to maintain good dimensional stability, the most commonly used improvement method is to make a multilayer film substrate on a rigid carrier plate; however, how to separate the carrier plate from the multilayer film substrate has also become a problem to be solved in subsequent derivations. .

現有分離方法包括化學剝離、雷射剝離等。TW I485756專利公告案揭示一種薄晶圓接合及剝離的方法，包括：(1)施加一剝離層於一載材上；(2)對該載材上的剝離層進行邊緣殘餘物移除；(3)施加一黏著層至一半導體晶圓上；(4)對該載材及半導體晶圓進行接合，且該剝離層及該黏著層位於該載材與該半導體晶圓之間；(5)施予能量至該剝離層；以及(6)以一溶劑清潔半導體晶圓的一表面，以移除該黏著層之所有殘餘物。此專利公告的剝離層是透過施予紫外光或雷射光進行剝離，針對剝離層及黏著層的材料以及用以移除該黏著層之殘餘物的溶劑並沒有具體地揭露。Existing separation methods include chemical peeling, laser peeling, and the like. TW I485756 patent publication discloses a method for bonding and peeling thin wafers, including: (1) applying a peeling layer on a carrier material; (2) removing edge residues on the peeling layer on the carrier material; 3) applying an adhesive layer to a semiconductor wafer; (4) bonding the carrier material and the semiconductor wafer, and the peeling layer and the adhesive layer being located between the carrier material and the semiconductor wafer; (5) Applying energy to the release layer; and (6) cleaning a surface of the semiconductor wafer with a solvent to remove all residues of the adhesive layer. The peeling layer of this patent publication is peeled by applying ultraviolet light or laser light. The materials of the peeling layer and the adhesive layer and the solvent used to remove the residue of the adhesive layer are not specifically disclosed.

由以上說明可知，對於搭配雷射剝離製程的清潔步驟仍有待進一步被開發，以助於讓半導體晶圓等光電元件及載材上不會殘留剝離層或黏著層材料，並能有效回收載材。It can be known from the above description that the cleaning steps for the laser stripping process still need to be further developed to help prevent the release layer or adhesive layer material from remaining on the photovoltaic elements such as semiconductor wafers and the carrier material, and to effectively recover the carrier material. .

因此，本發明之目的，即在提供一種能使該高分子層不會殘留於該光電元件或該承載材上且可有效回收承載材的光電元件的製備方法。Therefore, an object of the present invention is to provide a method for preparing a photovoltaic element that can prevent the polymer layer from remaining on the photovoltaic element or the supporting material and can effectively recover the supporting material.

於是，本發明光電元件的製備方法，包含： (a) 於承載材上形成一層高分子層，該高分子層是以一種於光線照射下會產生降解的材料為主； (b) 於該高分子層上形成光電元件； (c) 對該高分子層施加光線照射，以使該高分子層產生降解，並使該承載材與該光電元件分離；及 (d) 利用清洗組成物清洗該承載材或該光電元件； 其中，該清洗組成物包含由化學式1所示的鏈狀碳酸酯，以及漢森溶解度參數範圍為9~15 (cal/cm 3) 1/2的有機溶劑， [化學式1]

Figure TWI610392BD00001
， R 1及R 2為相同或不同且各自表示C 1~C 5烷基、C 2~C 5烯基或苯基。 Therefore, the method for preparing a photovoltaic element of the present invention includes: (a) forming a polymer layer on a carrier material, the polymer layer is mainly a material that will degrade under light irradiation; (b) the high A photovoltaic element is formed on the molecular layer; (c) applying light to the polymer layer to degrade the polymer layer and separate the carrier material from the photovoltaic element; and (d) cleaning the carrier with a cleaning composition Material or the photovoltaic element; wherein the cleaning composition comprises a chain carbonate represented by Chemical Formula 1 and an organic solvent having a Hansen solubility parameter ranging from 9 to 15 (cal / cm 3 ) 1/2 , [Chemical Formula 1 ]
Figure TWI610392BD00001
R 1 and R 2 are the same or different and each represents a C 1 to C 5 alkyl group, a C 2 to C 5 alkenyl group, or a phenyl group.

本發明之功效在於：本發明光電元件的製備方法是透過光線照射來分離承載材及光電元件，並利用該清洗組成物來清洗該承載材或該光電元件，進而能使該高分子層不會殘留於該光電元件或承載材上，也同時有助於回收該承載材。The effect of the present invention lies in that the method for preparing the photovoltaic element of the present invention is to separate the carrier material and the photovoltaic element through light irradiation, and use the cleaning composition to clean the carrier material or the photovoltaic element, so as to prevent the polymer layer from being damaged. Residue on the photovoltaic element or the carrier material also helps to recover the carrier material.

以下將就本發明內容進行詳細說明：The following will describe the content of the present invention in detail:

該步驟(a)的高分子層是以一種於光線照射下會產生降解的材料為主要成分。較佳地，該高分子層的材料是於雷射光照射下會產生降解。該高分子層的材料例如但不限於聚醯亞胺、聚苯并噁唑、聚酯、酚醛樹脂、丙烯酸樹脂、環氧樹脂或前述的一組合等。於本發明的一具體例中，該高分子層的材料為聚醯亞胺。該高分子層是將該材料塗佈於承載材上並於例如300°C溫度下進行加熱而形成。當該材料為聚醯亞胺時，可選擇地由例如芳香族二胺單體及芳香族四羧酸二酐單體進行反應而形成。該芳香族二胺單體例如但不限於2,2’-雙(三氟甲基)聯苯胺(TFMB)、雙(3-胺基-4-羥基苯基)異全氟丙烷、2,2’-雙(4-三胺基苯基)六氟丙烷、2,2’-雙(三氟甲基)-4,4’-二胺基苯基醚、2,2’-雙[4-(4-胺基苯氧基)苯基]六氟丙烷、2,2-雙(3-胺基-4-羥基苯基)六氟丙烷、3,4’-二胺基二苯醚、4,4’-二胺基二苯醚、1,3-雙(4-胺基苯氧基)苯、1,3-雙(3-胺基苯氧基)苯、2,2’-雙[4-(4-胺基苯氧基苯基)丙烷]等，前述的芳香族二胺可以單獨使用一種或混合使用多種。該芳香族四羧酸二酐單體例如但不限於4,4’-(六氟異丙烯)二酞酸酐、3,3’,4,4’-聯苯四羧酸二酐、4,4’-氧雙鄰苯二甲酸酐(ODPA)、3,3’,4,4’-二苯酮四羧酸二酐、雙酚A型二醚二酐等，前述的芳香族四羧酸二酐可以單獨使用一種或混合使用多種。除了芳香族四羧酸二酐外，於前述芳香族二胺單體與芳香族四羧酸二酐單體的反應中，另可加入脂肪族四羧酸二酐，例如但不限於六氟二酐(6FDA)等。The polymer layer in the step (a) is composed of a material that can be degraded under light irradiation. Preferably, the material of the polymer layer is degraded under the irradiation of laser light. The material of the polymer layer is, for example, but not limited to, polyimide, polybenzoxazole, polyester, phenol resin, acrylic resin, epoxy resin, or a combination thereof. In a specific example of the present invention, a material of the polymer layer is polyimide. The polymer layer is formed by coating the material on a carrier material and heating the material at, for example, a temperature of 300 ° C. When the material is polyimide, it may alternatively be formed by reacting, for example, an aromatic diamine monomer and an aromatic tetracarboxylic dianhydride monomer. The aromatic diamine monomer such as, but not limited to, 2,2'-bis (trifluoromethyl) benzidine (TFMB), bis (3-amino-4-hydroxyphenyl) isoperfluoropropane, 2,2 '-Bis (4-triaminophenyl) hexafluoropropane, 2,2'-bis (trifluoromethyl) -4,4'-diaminophenyl ether, 2,2'-bis [4- (4-Aminophenoxy) phenyl] hexafluoropropane, 2,2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, 3,4'-diaminodiphenyl ether, 4 , 4'-diaminodiphenyl ether, 1,3-bis (4-aminophenoxy) benzene, 1,3-bis (3-aminophenoxy) benzene, 2,2'-bis [ 4- (4-aminophenoxyphenyl) propane], etc., the aforementioned aromatic diamines may be used alone or in combination. The aromatic tetracarboxylic dianhydride monomer is, for example, but not limited to, 4,4 '-(hexafluoroisopropene) diphthalic anhydride, 3,3', 4,4'-biphenyltetracarboxylic dianhydride, 4,4 '-Oxybisphthalic anhydride (ODPA), 3,3', 4,4'-benzophenonetetracarboxylic dianhydride, bisphenol A diether dianhydride, etc., the aforementioned aromatic tetracarboxylic dianhydride The anhydride may be used singly or in combination. In addition to the aromatic tetracarboxylic dianhydride, in the reaction between the aromatic diamine monomer and the aromatic tetracarboxylic dianhydride monomer, an aliphatic tetracarboxylic dianhydride such as but not limited to hexafluorodicarboxylic Anhydride (6FDA), etc.

較佳地，該步驟(c)的光線為雷射光。更佳地，該雷射光的波長範圍為350~1500 nm。又更佳地，該雷射能量範圍為2至6瓦。Preferably, the light in step (c) is laser light. More preferably, the wavelength of the laser light is 350 ~ 1500 nm. Even more preferably, the laser energy ranges from 2 to 6 watts.

較佳地，該由化學式1所示的鏈狀碳酸酯是選自於碳酸二甲酯、碳酸二乙酯、碳酸二丙酯、碳酸二正丁酯、碳酸甲乙酯、碳酸甲丙酯、碳酸乙丙酯、烯丙基甲基碳酸酯、碳酸二烯丙酯或前述的組合。於本發明的一具體例中，該鏈狀碳酸酯為碳酸二甲酯；於本發明的另一具體例中，該鏈狀碳酸酯為碳酸甲乙酯；於本發明的另一具體例中，該鏈狀碳酸酯為碳酸二乙酯。Preferably, the chain carbonate represented by Chemical Formula 1 is selected from the group consisting of dimethyl carbonate, diethyl carbonate, dipropyl carbonate, di-n-butyl carbonate, ethyl methyl carbonate, methylpropyl carbonate, Ethyl carbonate, allyl methyl carbonate, diallyl carbonate, or a combination of the foregoing. In a specific example of the present invention, the chain carbonate is dimethyl carbonate; in another specific example of the present invention, the chain carbonate is methyl ethyl carbonate; in another specific example of the present invention The chain carbonate is diethyl carbonate.

該有機溶劑的漢森溶解度參數範圍為9~15 (cal/cm 3) 1/2；較佳地，該有機溶劑的漢森溶解度參數範圍為11~14 (cal/cm 3) 1/2。 The Hansen solubility parameter range of the organic solvent is 9 ~ 15 (cal / cm 3 ) 1/2 ; preferably, the Hansen solubility parameter range of the organic solvent is 11 ~ 14 (cal / cm 3 ) 1/2 .

較佳地，該有機溶劑於760 mmHg下的最低沸點為140°C；更佳地，該有機溶劑於760 mmHg下的最低沸點為150°C；再更佳地，該有機溶劑於760 mmHg下的沸點範圍為150~300°C。Preferably, the lowest boiling point of the organic solvent at 760 mmHg is 140 ° C; more preferably, the lowest boiling point of the organic solvent at 760 mmHg is 150 ° C; even more preferably, the organic solvent is at 760 mmHg The boiling point range is 150 ~ 300 ° C.

較佳地，該有機溶劑是選自於N-甲基吡咯烷酮(於760 mmHg下的沸點為204°C，漢森溶解度參數為11.2)、N-乙基吡咯烷酮(於760 mmHg下的沸點為204°C，漢森溶解度參數為11.1)、N-異丙基吡咯烷酮(於760 mmHg下的沸點為218°C，漢森溶解度參數為14.75)、二甲基乙醯胺(於760 mmHg下的沸點為164°C，漢森溶解度參數為11.1)、二甲基甲醯胺(於760 mmHg下的沸點為153°C，漢森溶解度參數為12.1)、二乙基甲醯胺(於760 mmHg下的沸點為176-177°C，漢森溶解度參數為10.1)、g-丁內酯(於760 mmHg下的沸點為204°C，漢森溶解度參數為12.8)、二甲基亞碸(於760 mmHg下的沸點為189°C，漢森溶解度參數為13)、丙二醇甲基醚乙酸酯(於760 mmHg下的沸點為145-146°C，漢森溶解度參數為9.6)、由化學式2所示的環狀碳酸酯、或前述的組合， [化學式2]

Figure TWI610392BD00002
， R 3、R 4、R 5及R 6為相同或不同且各自表示C 1~C 5烷基或C 2~C 5烯基。 Preferably, the organic solvent is selected from the group consisting of N-methylpyrrolidone (boiling point at 760 mmHg is 204 ° C, Hanson solubility parameter is 11.2), N-ethylpyrrolidone (boiling point at 760 mmHg is 204 ° C, Hansen solubility parameter is 11.1), N-isopropylpyrrolidone (boiling point at 760 mmHg is 218 ° C, Hanson solubility parameter is 14.75), dimethylacetamide (boiling point at 760 mmHg) 164 ° C, Hansen solubility parameter is 11.1), dimethylformamide (boiling point at 760 mmHg is 153 ° C, Hanson solubility parameter is 12.1), diethylformamide (at 760 mmHg Has a boiling point of 176-177 ° C, Hansen solubility parameter is 10.1), g-butyrolactone (boiling point at 760 mmHg is 204 ° C, Hanson solubility parameter is 12.8), dimethyl sulfene (at 760 The boiling point at mmHg is 189 ° C, the Hansen solubility parameter is 13), the propylene glycol methyl ether acetate (the boiling point at 760 mmHg is 145-146 ° C, the Hanson solubility parameter is 9.6). Cyclic carbonate, or a combination of the foregoing, [Chemical Formula 2]
Figure TWI610392BD00002
R 3 , R 4 , R 5 and R 6 are the same or different and each represents a C 1 -C 5 alkyl group or a C 2 -C 5 alkenyl group.

較佳地，該由化學式2所示的環狀碳酸酯是選自於碳酸丙烯酯(於760 mmHg下的沸點為242°C，漢森溶解度參數為13.3)或碳酸丁烯酯(於760 mmHg下的沸點為251°C，漢森溶解度參數為12.1)。Preferably, the cyclic carbonate represented by Chemical Formula 2 is selected from propylene carbonate (boiling point at 760 mmHg is 242 ° C, Hanson solubility parameter is 13.3) or butene carbonate (at 760 mmHg The boiling point is 251 ° C, and the Hansen solubility parameter is 12.1).

於本發明的一具體例中，該有機溶劑是N-甲基吡咯烷酮；於本發明的另一具體例中，該有機溶劑是g-丁內酯；於本發明的另一具體例中，該有機溶劑是二甲基亞碸；於本發明的又另一具體例中，該有機溶劑是碳酸丙烯酯。In a specific example of the present invention, the organic solvent is N-methylpyrrolidone; in another specific example of the present invention, the organic solvent is g-butyrolactone; in another specific example of the present invention, the The organic solvent is dimethylsulfinium; in yet another specific example of the present invention, the organic solvent is propylene carbonate.

較佳地，以該清洗組成物的總重為100 wt%計算，該鏈狀碳酸酯的含量範圍為5~95 wt%，及該有機溶劑的含量範圍為5~95 wt%。Preferably, based on the total weight of the cleaning composition being 100 wt%, the content of the chain carbonate is in the range of 5 to 95 wt%, and the content of the organic solvent is in the range of 5 to 95 wt%.

在本發明被詳細描述之前，應當注意在以下的說明內容中，類似的元件是以相同的編號來表示。Before the present invention is described in detail, it should be noted that in the following description, similar elements are represented by the same numbers.

本發明將就以下實施例作進一步說明，但應瞭解的是，該實施例僅為例示說明之用，而不應被解釋為本發明實施之限制。The present invention will be further described with reference to the following examples, but it should be understood that this example is for illustrative purposes only and should not be construed as a limitation on the implementation of the present invention.

[實施例][Example]

參閱圖1，本發明光電元件的製備方法的實施例包含： (a) 於承載材1上形成一層高分子層2，該高分子層2是以一種於光線照射下會產生降解的材料為主。於本實施例中，該高分子層2是以聚醯亞胺材料為主，且該高分子層2是透過將2,2’-雙(三氟甲基)聯苯胺(TFMB)與4,4’-氧雙鄰苯二甲酸酐(ODPA)及六氟二酐(6FDA)反應而成的聚醯亞胺塗佈於玻璃承載材1上，再於300°C加熱進行脫水閉環反應後而形成。 (b) 於該高分子層2上形成光電元件3； (c) 由該玻璃承載材1表面，對該高分子層2施加一光線照射，以使該高分子層2產生降解，並使該玻璃承載材1與該光電元件3分離；及 (d) 利用一清洗組成物(圖未示)清洗表面含有該高分子層2的該光電元件3。該清洗組成物是由化學式1所示的鏈狀碳酸酯，以及漢森溶解度參數範圍為9~15 (cal/cm 3) 1/2的有機溶劑所組成。 Referring to FIG. 1, an embodiment of a method for preparing a photovoltaic element according to the present invention includes: (a) forming a polymer layer 2 on a carrier material 1, the polymer layer 2 is mainly a material that will degrade under light irradiation . In this embodiment, the polymer layer 2 is mainly made of polyimide material, and the polymer layer 2 is formed by combining 2,2'-bis (trifluoromethyl) benzidine (TFMB) with 4, Polyimide formed by the reaction of 4'-oxydiphthalic anhydride (ODPA) and hexafluorodianhydride (6FDA) is coated on glass carrier material 1, and then heated at 300 ° C for dehydration ring-closure reaction. form. (b) forming a photovoltaic element 3 on the polymer layer 2; (c) applying a light irradiation to the polymer layer 2 from the surface of the glass carrier material 1 to degrade the polymer layer 2 and make the polymer layer 2 The glass carrier 1 is separated from the photovoltaic element 3; and (d) the photovoltaic element 3 containing the polymer layer 2 on the surface is cleaned by a cleaning composition (not shown). The cleaning composition is composed of a chain carbonate represented by Chemical Formula 1 and an organic solvent having a Hansen solubility parameter ranging from 9 to 15 (cal / cm 3 ) 1/2 .

[ 測試例 1~10 及比較測試例 1~7]測試例1~10及比較測試例1~7分別進行以下測試步驟： 1. 試片製作：取總酸酐基含量為1當量的二酸酐單體[4,4’-氧雙鄰苯二甲酸酐(ODPA)及六氟二酐(6FDA)]，以及胺基含量為0.95當量的二胺單體[2,2’-雙(三氟甲基)聯苯胺(TFMB)]，依序添加於N,N-二甲基甲醯胺中，製備成固成分為20重量%之溶液；接著將此溶液於常溫下反應24小時，即可得聚醯亞胺樹脂。將聚醯亞胺樹脂塗佈於玻璃片(10 cm×10 cm)上，然後以50°C烘烤3分鐘，再以90°C烘烤20分鐘，最後以300°C烘烤30分鐘而於玻璃片上形成厚度為2.5 mm的聚醯亞胺層。將一基板層(例如聚苯并噁唑或其他圖案化金屬層)黏附於聚醯亞胺層上。利用波長355 nm的雷射光(能量為2瓦)，從玻璃片表面照射聚醯亞胺層，直至基板層及部份聚醯亞胺層與玻璃片分離，得到一試片[包含聚醯亞胺層(厚度為2.3 mm)以及基板層]。 2. 清洗能力測試：於超音波震盪下，將試片浸泡在清洗組成物中(溫度為25°C)，分別於3分鐘、5分鐘及10分鐘後量測聚醯亞胺層的厚度，再透過以下公式1計算清洗速度(nm/min)，以及透過以下公式2計算清洗能力，最後依據以下標準衡量清洗能力： [公式1] 清洗速度(nm/min)=

Figure TWI610392BD00003
(THK 10表示浸泡10分鐘後的聚醯亞胺層厚度；THK 0表示浸泡前的聚醯亞胺層厚度，即2.3 mm) [公式2] 清洗能力(%)=
Figure TWI610392BD00004
(THK f表示浸泡f分鐘後的聚醯亞胺層厚度，f為3、5或10) 所獲得數值為0~39%，表示清洗能力極差，將標註為『×』； 所獲得數值為40~74%，表示清洗能力良好，將標註為『○』； 所獲得數值為75~100%，表示清洗能力優良，將標註為『◎』。 測試例1~10及比較測試例1~7所使用的清洗組成物的成分與含量、以及清洗能力結果整理於下表1中。 [ Test Examples 1 to 10 and Comparative Test Examples 1 to 7] Test Examples 1 to 10 and Comparative Test Examples 1 to 7 respectively perform the following test steps: 1. Test piece production: Take the dianhydride monomer with a total acid anhydride group content of 1 equivalent [4,4'-oxybisphthalic anhydride (ODPA) and hexafluorodianhydride (6FDA)], and a diamine monomer with an amine content of 0.95 equivalents [2,2'-bis (trifluoromethyl) Group) benzidine (TFMB)], added sequentially to N, N-dimethylformamide, to prepare a solution with a solid content of 20% by weight; then the solution was reacted at room temperature for 24 hours to obtain Polyimide resin. Polyimide resin was coated on a glass plate (10 cm × 10 cm), and then baked at 50 ° C for 3 minutes, then at 90 ° C for 20 minutes, and finally at 300 ° C for 30 minutes. A 2.5 mm thick polyimide layer was formed on the glass sheet. A substrate layer (such as a polybenzoxazole or other patterned metal layer) is adhered to the polyimide layer. Using laser light with a wavelength of 355 nm (energy is 2 watts), the polyimide layer was irradiated from the surface of the glass sheet until the substrate layer and a part of the polyimide layer were separated from the glass sheet to obtain a test sheet [including polyimide Amine layer (2.3 mm thick) and substrate layer]. 2. Cleaning ability test: Under ultrasonic vibration, immerse the test piece in the cleaning composition (temperature: 25 ° C), and measure the thickness of the polyimide layer after 3 minutes, 5 minutes, and 10 minutes, respectively. Then calculate the cleaning speed (nm / min) through the following formula 1, and calculate the cleaning capacity through the following formula 2. Finally, measure the cleaning capacity according to the following standards: [Formula 1] Cleaning speed (nm / min) =
Figure TWI610392BD00003
(THK 10 indicates the thickness of the polyimide layer after soaking for 10 minutes; THK 0 indicates the thickness of the polyimide layer before soaking, that is, 2.3 mm) [Formula 2] Cleaning ability (%) =
Figure TWI610392BD00004
(THK f represents the thickness of the polyimide layer after f minutes of immersion, f is 3, 5, or 10) The obtained value is 0 ~ 39%, which indicates that the cleaning ability is extremely poor, and it will be marked as "×"; the obtained value is 40 ~ 74%, it means the cleaning ability is good, it will be marked as "○"; The obtained value is 75 ~ 100%, it means that the cleaning ability is good, it will be marked as "◎". The components and contents of the cleaning compositions used in Test Examples 1 to 10 and Comparative Test Examples 1 to 7, and the cleaning ability results are summarized in Table 1 below.

[表1] <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> </td><td> 鏈狀碳酸酯 </td><td> 有機溶劑 </td><td> 清洗速度(nm/min) </td><td> 清洗能力 </td><td> 最終評價 </td></tr><tr><td> 種類 </td><td> 用量(wt%) </td><td> 種類 </td><td> 用量(wt%) </td><td> 3 分鐘 </td><td> 5 分鐘 </td><td> 10 分鐘 </td></tr><tr><td> 測 試 例 </td><td> 1 </td><td> DMC </td><td> 95 </td><td> NMP </td><td> 5 </td><td> 575.3 </td><td> ◎ </td><td> ◎ </td><td> ◎ </td><td> 優良 </td></tr><tr><td> 2 </td><td> DMC </td><td> 80 </td><td> NMP </td><td> 20 </td><td> 556.7 </td><td> ◎ </td><td> ◎ </td><td> ◎ </td><td> 優良 </td></tr><tr><td> 3 </td><td> DMC </td><td> 50 </td><td> NMP </td><td> 50 </td><td> 450.1 </td><td> ○ </td><td> ◎ </td><td> ◎ </td><td> 優良 </td></tr><tr><td> 4 </td><td> DMC </td><td> 20 </td><td> NMP </td><td> 80 </td><td> 428.0 </td><td> ○ </td><td> ◎ </td><td> ◎ </td><td> 優良 </td></tr><tr><td> 5 </td><td> DMC </td><td> 5 </td><td> NMP </td><td> 95 </td><td> 481.4 </td><td> ○ </td><td> ○ </td><td> ◎ </td><td> 良好 </td></tr><tr><td> 6 </td><td> DMC </td><td> 70 </td><td> DMSO </td><td> 30 </td><td> 554.7 </td><td> ◎ </td><td> ◎ </td><td> ◎ </td><td> 優良 </td></tr><tr><td> 7 </td><td> DMC </td><td> 50 </td><td> PC </td><td> 50 </td><td> 536.7 </td><td> ◎ </td><td> ◎ </td><td> ◎ </td><td> 優良 </td></tr><tr><td> 8 </td><td> DMC </td><td> 40 </td><td> GBL </td><td> 60 </td><td> 402.7 </td><td> ○ </td><td> ○ </td><td> ◎ </td><td> 良好 </td></tr><tr><td> 9 </td><td> EMC </td><td> 70 </td><td> GBL </td><td> 30 </td><td> 475.9 </td><td> ○ </td><td> ○ </td><td> ◎ </td><td> 良好 </td></tr><tr><td> 10 </td><td> DEC </td><td> 40 </td><td> GBL </td><td> 60 </td><td> 397.8 </td><td> ○ </td><td> ○ </td><td> ◎ </td><td> 良好 </td></tr><tr><td> DMC：碳酸二甲酯；EMC：碳酸甲乙酯；DEC：碳酸二乙酯； NMP：N-甲基吡咯烷酮(於760 mmHg下的沸點為204°C，漢森溶解度參數為11.2)； DMSO：二甲基亞碸(於760 mmHg下的沸點為189°C，漢森溶解度參數為13)； PC：碳酸丙烯酯(於760 mmHg下的沸點為242°C，漢森溶解度參數為13.3)； GBL：g-丁內酯(於760 mmHg下的沸點為204°C，漢森溶解度參數為12.8)。 </td></tr></TBODY></TABLE>[Table 1]         <TABLE border = "1" borderColor = "# 000000" width = "85%"> <TBODY> <tr> <td> </ td> <td> Chain carbonates </ td> <td> Organic solvents < / td> <td> Cleaning speed (nm / min) </ td> <td> Cleaning ability </ td> <td> Final evaluation </ td> </ tr> <tr> <td> Type </ td> <td> Dosage (wt%) </ td> <td> Species </ td> <td> Dosage (wt%) </ td> <td> 3 minutes </ td> <td> 5 minutes </ td> <td> 10 minutes </ td> </ tr> <tr> <td> Test example </ td> <td> 1 </ td> <td> DMC </ td> <td> 95 </ td> < td> NMP </ td> <td> 5 </ td> <td> 575.3 </ td> <td> ◎ </ td> <td> ◎ </ td> <td> ◎ </ td> <td> Excellent </ td> </ tr> <tr> <td> 2 </ td> <td> DMC </ td> <td> 80 </ td> <td> NMP </ td> <td> 20 </ td> <td> 556.7 </ td> <td> ◎ </ td> <td> ◎ </ td> <td> ◎ </ td> <td> Excellent </ td> </ tr> <tr> < td> 3 </ td> <td> DMC </ td> <td> 50 </ td> <td> NMP </ td> <td> 50 </ td> <td> 450.1 </ td> <td> ○ </ td> <td> ◎ </ td> <td> ◎ </ td> <td> Excellent </ td> </ tr> <tr> <td> 4 </ td> <td> DMC </ td> <td> 20 </ td> <td> NMP </ td> <td> 80 </ td> <td> 428.0 </ td> <td> ○ </ td> <td> ◎ </ td> <td> ◎ </ td> <td> Excellent </ td> </ tr> <tr> <td> 5 </ td> <td> DMC </ t d> <td> 5 </ td> <td> NMP </ td> <td> 95 </ td> <td> 481.4 </ td> <td> ○ </ td> <td> ○ </ td> <td> ◎ </ td> <td> Good </ td> </ tr> <tr> <td> 6 </ td> <td> DMC </ td> <td> 70 </ td> <td> DMSO </ td> <td> 30 </ td> <td> 554.7 </ td> <td> ◎ </ td> <td> ◎ </ td> <td> ◎ </ td> <td> Excellent < / td> </ tr> <tr> <td> 7 </ td> <td> DMC </ td> <td> 50 </ td> <td> PC </ td> <td> 50 </ td> <td> 536.7 </ td> <td> ◎ </ td> <td> ◎ </ td> <td> ◎ </ td> <td> Excellent </ td> </ tr> <tr> <td> 8 </ td> <td> DMC </ td> <td> 40 </ td> <td> GBL </ td> <td> 60 </ td> <td> 402.7 </ td> <td> ○ < / td> <td> ○ </ td> <td> ◎ </ td> <td> Good </ td> </ tr> <tr> <td> 9 </ td> <td> EMC </ td> <td> 70 </ td> <td> GBL </ td> <td> 30 </ td> <td> 475.9 </ td> <td> ○ </ td> <td> ○ </ td> <td > ◎ </ td> <td> Good </ td> </ tr> <tr> <td> 10 </ td> <td> DEC </ td> <td> 40 </ td> <td> GBL < / td> <td> 60 </ td> <td> 397.8 </ td> <td> ○ </ td> <td> ○ </ td> <td> ◎ </ td> <td> Good </ td > </ tr> <tr> <td> DMC: dimethyl carbonate; EMC: ethyl methyl carbonate; DEC: diethyl carbonate; NMP: N-methylpyrrolidone (at 760 mmHg The point is 204 ° C, the Hansen solubility parameter is 11.2); DMSO: dimethylsulfinium (boiling point at 760 mmHg is 189 ° C, Hanson solubility parameter is 13); PC: propylene carbonate (at 760 mmHg The boiling point is 242 ° C, the Hansen solubility parameter is 13.3); GBL: g-butyrolactone (boiling point at 760 mmHg is 204 ° C, the Hanson solubility parameter is 12.8). </ td> </ tr> </ TBODY> </ TABLE>

[表2] <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> </td><td> 鏈狀碳酸酯 </td><td> 有機溶劑 </td><td> 清洗速度(nm/min) </td><td> 清洗能力 </td><td> 最終評價 </td></tr><tr><td> 種類 </td><td> 用量(wt%) </td><td> 種類 </td><td> 用量(wt%) </td><td> 3 分鐘 </td><td> 5 分鐘 </td><td> 10 分鐘 </td></tr><tr><td> 比較測試例 </td><td> 1 </td><td> - </td><td> 0 </td><td> NMP </td><td> 100 </td><td> 306.5 </td><td> × </td><td> ○ </td><td> ○ </td><td> 稍差 </td></tr><tr><td> 2 </td><td> - </td><td> 0 </td><td> GBL </td><td> 100 </td><td> 156.5 </td><td> × </td><td> × </td><td> × </td><td> 極差 </td></tr><tr><td> 3 </td><td> - </td><td> 0 </td><td> DMSO </td><td> 100 </td><td> 29.87 </td><td> × </td><td> × </td><td> × </td><td> 極差 </td></tr><tr><td> 4 </td><td> - </td><td> 0 </td><td> PC </td><td> 100 </td><td> 45.5 </td><td> × </td><td> × </td><td> × </td><td> 極差 </td></tr><tr><td> 5 </td><td> - </td><td> 0 </td><td> BC </td><td> 100 </td><td> 33.4 </td><td> × </td><td> × </td><td> × </td><td> 極差 </td></tr><tr><td> 6 </td><td> DMC </td><td> 20 </td><td> MEA </td><td> 80 </td><td> 5.6 </td><td> × </td><td> × </td><td> × </td><td> 極差 </td></tr><tr><td> 7 </td><td> DMC </td><td> 20 </td><td> 正己烷 </td><td> 80 </td><td> 13.5 </td><td> × </td><td> × </td><td> × </td><td> 極差 </td></tr><tr><td> BC：2-丁氧基乙醇(於760 mmHg下的沸點為169-173°C，漢森溶解度參數為10.2)； MEA：單乙醇胺(於760 mmHg下的沸點為170°C，漢森溶解度參數為15.4) 正己烷 (於760 mmHg下的沸點為69°C，漢森溶解度參數為7.3) </td></tr></TBODY></TABLE>[Table 2]         <TABLE border = "1" borderColor = "# 000000" width = "85%"> <TBODY> <tr> <td> </ td> <td> Chain carbonates </ td> <td> Organic solvents < / td> <td> Cleaning speed (nm / min) </ td> <td> Cleaning ability </ td> <td> Final evaluation </ td> </ tr> <tr> <td> Type </ td> <td> Dosage (wt%) </ td> <td> Species </ td> <td> Dosage (wt%) </ td> <td> 3 minutes </ td> <td> 5 minutes </ td> <td> 10 minutes </ td> </ tr> <tr> <td> Comparative test case </ td> <td> 1 </ td> <td>-</ td> <td> 0 </ td> <td> NMP </ td> <td> 100 </ td> <td> 306.5 </ td> <td> × </ td> <td> ○ </ td> <td> ○ </ td> <td > Slightly worse </ td> </ tr> <tr> <td> 2 </ td> <td>-</ td> <td> 0 </ td> <td> GBL </ td> <td> 100 </ td> <td> 156.5 </ td> <td> × </ td> <td> × </ td> <td> × </ td> <td> Extremely bad </ td> </ tr> < tr> <td> 3 </ td> <td>-</ td> <td> 0 </ td> <td> DMSO </ td> <td> 100 </ td> <td> 29.87 </ td> <td> × </ td> <td> × </ td> <td> × </ td> <td> Extremely bad </ td> </ tr> <tr> <td> 4 </ td> <td >-</ td> <td> 0 </ td> <td> PC </ td> <td> 100 </ td> <td> 45.5 </ td> <td> × </ td> <td> × </ td> <td> × </ td> <td> Extremely bad </ td> </ tr> <tr> <td> 5 </ td> <td>-</ td> <td> 0 </ td> <t d> BC </ td> <td> 100 </ td> <td> 33.4 </ td> <td> × </ td> <td> × </ td> <td> × </ td> <td> Extremely bad </ td> </ tr> <tr> <td> 6 </ td> <td> DMC </ td> <td> 20 </ td> <td> MEA </ td> <td> 80 < / td> <td> 5.6 </ td> <td> × </ td> <td> × </ td> <td> × </ td> <td> Extremely bad </ td> </ tr> <tr > <td> 7 </ td> <td> DMC </ td> <td> 20 </ td> <td> n-hexane </ td> <td> 80 </ td> <td> 13.5 </ td> <td> × </ td> <td> × </ td> <td> × </ td> <td> Extremely bad </ td> </ tr> <tr> <td> BC: 2-butoxy Ethanol (boiling point at 760 mmHg is 169-173 ° C, Hansen solubility parameter is 10.2); MEA: monoethanolamine (boiling point at 760 mmHg is 170 ° C, Hanson solubility parameter is 15.4) n-hexane (in The boiling point at 760 mmHg is 69 ° C, and the Hansen solubility parameter is 7.3) </ td> </ tr> </ TBODY> </ TABLE>

由表1及表2結果可以得知，使用鏈狀碳酸酯及特定有機溶劑所組成的清洗組成物，確實能有效去除殘留的聚醯亞胺層，並展現優異的清洗能力及清洗速度(高於370 nm/min)。From the results in Tables 1 and 2, it can be known that the cleaning composition composed of a chain carbonate and a specific organic solvent can effectively remove the remaining polyimide layer and exhibit excellent cleaning ability and cleaning speed (high At 370 nm / min).

反觀比較測試例1~5的結果，當僅單純使用一種有機溶劑作為清洗組成物時，除了NMP可以去除部份聚醯亞胺層外，其餘有機溶劑無法有效去除聚醯亞胺層，而無法展現符合業界使用的清洗能力及清洗速度(低於350 nm/min)。In contrast, when comparing the results of Test Examples 1 to 5, when only one organic solvent is used as the cleaning composition, except for NMP, which can partially remove the polyimide layer, the remaining organic solvents cannot effectively remove the polyimide layer, and cannot Demonstrates cleaning capabilities and cleaning speeds (less than 350 nm / min) consistent with industry usage.

由比較測試例6及7結果來看，當使用胺類或正己烷作為有機溶劑，即使與鏈狀碳酸酯混合使用作為清洗組成物，仍無法有效去除聚醯亞胺層。From the results of Comparative Test Examples 6 and 7, when an amine or n-hexane was used as the organic solvent, the polyimide layer could not be effectively removed even if it was mixed with a chain carbonate as a cleaning composition.

綜上所述，本發明光電元件的製備方法是透過光線照射來分離承載材及光電元件，並利用該清洗組成物來清洗該承載材或該光電元件，進而能使該高分子層不會殘留於該光電元件或承載材上，也同時有助於回收該承載材。In summary, the method for preparing a photovoltaic element of the present invention is to separate the carrier material and the photovoltaic element through light irradiation, and use the cleaning composition to clean the carrier material or the photovoltaic element, so that the polymer layer does not remain. On the photovoltaic element or the carrier material, it also helps to recover the carrier material.

惟以上所述者，僅為本發明之實施例而已，當不能以此限定本發明實施之範圍，凡是依本發明申請專利範圍及專利說明書內容所作之簡單的等效變化與修飾，皆仍屬本發明專利涵蓋之範圍內。However, the above are only examples of the present invention. When the scope of implementation of the present invention cannot be limited in this way, any simple equivalent changes and modifications made in accordance with the scope of the patent application and the content of the patent specification of the present invention are still Within the scope of the invention patent.

1‧‧‧承載材
2‧‧‧高分子層
3‧‧‧光電元件1‧‧‧ bearing material
2‧‧‧ polymer layer
3‧‧‧Photoelectric element

本發明之其他的特徵及功效，將於參照圖式的實施方式中清楚地呈現，其中： ［圖1］是本發明方法的實施例的流程示意圖。Other features and effects of the present invention will be clearly presented in the embodiment with reference to the drawings, wherein: [FIG. 1] is a schematic flowchart of an embodiment of the method of the present invention.

1‧‧‧承載材 1‧‧‧ bearing material

2‧‧‧高分子層 2‧‧‧ polymer layer

3‧‧‧光電元件 3‧‧‧Photoelectric element

Claims (9)

一種光電元件的製備方法，包含： (a) 於承載材上形成一層高分子層，該高分子層是以一種於光線照射下會產生降解的材料為主； (b) 於該高分子層上形成光電元件； (c) 對該高分子層施加光線照射，以使該高分子層產生降解，並使該承載材與該光電元件分離；及 (d) 利用清洗組成物清洗該承載材或該光電元件； 其中，該清洗組成物包含由化學式1所示的鏈狀碳酸酯，以及漢森溶解度參數範圍為9~15 (cal/cm 3) 1/2的有機溶劑， [化學式1]
Figure TWI610392BC00001
， R 1及R 2為相同或不同且各自表示C 1~C 5烷基、C 2~C 5烯基或苯基。 A method for preparing a photovoltaic element includes: (a) forming a polymer layer on a carrier material, the polymer layer is mainly a material that will degrade under light irradiation; (b) on the polymer layer Forming a photovoltaic element; (c) applying light irradiation to the polymer layer to cause degradation of the polymer layer and separating the carrier material from the photovoltaic element; and (d) cleaning the carrier material or the component with a cleaning composition Photoelectric element; wherein, the cleaning composition includes a chain carbonate represented by Chemical Formula 1, and an organic solvent having a Hansen solubility parameter ranging from 9 to 15 (cal / cm 3 ) 1/2 , [Chemical Formula 1]
Figure TWI610392BC00001
R 1 and R 2 are the same or different and each represents a C 1 to C 5 alkyl group, a C 2 to C 5 alkenyl group, or a phenyl group. 如請求項1所述的光電元件的製備方法，其中，該高分子層的材料是選自於聚醯亞胺、聚苯并噁唑、聚酯、酚醛樹脂、丙烯酸樹脂、環氧樹脂或前述的組合。The method for manufacturing a photovoltaic device according to claim 1, wherein the material of the polymer layer is selected from the group consisting of polyimide, polybenzoxazole, polyester, phenol resin, acrylic resin, epoxy resin, or the foregoing The combination. 如請求項1所述的光電元件的製備方法，其中，該由化學式1所示的鏈狀碳酸酯是選自於碳酸二甲酯、碳酸二乙酯、碳酸二丙酯、碳酸二正丁酯、碳酸甲乙酯、碳酸甲丙酯、碳酸乙丙酯、烯丙基甲基碳酸酯、碳酸二烯丙酯或前述的組合。The method for producing a photovoltaic element according to claim 1, wherein the chain carbonate represented by Chemical Formula 1 is selected from the group consisting of dimethyl carbonate, diethyl carbonate, dipropyl carbonate, and di-n-butyl carbonate. , Methyl ethyl carbonate, methyl propyl carbonate, ethyl propyl carbonate, allyl methyl carbonate, diallyl carbonate, or a combination thereof. 如請求項1所述的光電元件的製備方法，其中，該有機溶劑於760 mmHg下的最低沸點為140°C。The method for preparing a photovoltaic element according to claim 1, wherein the lowest boiling point of the organic solvent at 760 mmHg is 140 ° C. 如請求項1所述的光電元件的製備方法，其中，該有機溶劑是選自於N-甲基吡咯烷酮、N-乙基吡咯烷酮、N-異丙基吡咯烷酮、二甲基乙醯胺、二甲基甲醯胺、二乙基甲醯胺、g-丁內酯、二甲基亞碸、丙二醇甲基醚乙酸酯、由化學式2所示的環狀碳酸酯、或前述的組合， [化學式2]
Figure TWI610392BC00002
， R 3、R 4、R 5及R 6為相同或不同且各自表示C 1~C 5烷基或C 2~C 5烯基。 The method for producing a photovoltaic device according to claim 1, wherein the organic solvent is selected from the group consisting of N-methylpyrrolidone, N-ethylpyrrolidone, N-isopropylpyrrolidone, dimethylacetamide, and dimethyl Methylformamide, diethylformamide, g-butyrolactone, dimethylmethane, propylene glycol methyl ether acetate, a cyclic carbonate represented by Chemical Formula 2, or a combination thereof, [Chemical formula 2]
Figure TWI610392BC00002
R 3 , R 4 , R 5 and R 6 are the same or different and each represents a C 1 -C 5 alkyl group or a C 2 -C 5 alkenyl group. 如請求項5所述的光電元件的製備方法，其中，該由化學式2所示的環狀碳酸酯是選自於碳酸丙烯酯或碳酸丁烯酯。The method for producing a photovoltaic element according to claim 5, wherein the cyclic carbonate represented by Chemical Formula 2 is selected from propylene carbonate or butene carbonate. 如請求項5所述的光電元件的製備方法，其中，該有機溶劑是選自於N-甲基吡咯烷酮、g-丁內酯、二甲基亞碸或碳酸丙烯酯。The method for producing a photovoltaic element according to claim 5, wherein the organic solvent is selected from the group consisting of N-methylpyrrolidone, g-butyrolactone, dimethylsulfinium, and propylene carbonate. 如請求項1所述的光電元件的製備方法，其中，以該清洗組成物的總重為100 wt%計算，該鏈狀碳酸酯的含量範圍為5~95 wt%，及該有機溶劑的含量範圍為5~95 wt%。The method for preparing a photovoltaic device according to claim 1, wherein the content of the chain carbonate is in a range of 5 to 95 wt%, and the content of the organic solvent is calculated based on a total weight of the cleaning composition of 100 wt%. The range is 5 ~ 95 wt%. 如請求項1所述的光電元件的製備方法，其中，該步驟(c)的光線是雷射光。The method for manufacturing a photovoltaic element according to claim 1, wherein the light in step (c) is laser light.
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