TW201927864A - Polysiloxane, and doping slurry for solar energy and semiconductor - Google Patents

Polysiloxane, and doping slurry for solar energy and semiconductor Download PDF

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TW201927864A
TW201927864A TW107144911A TW107144911A TW201927864A TW 201927864 A TW201927864 A TW 201927864A TW 107144911 A TW107144911 A TW 107144911A TW 107144911 A TW107144911 A TW 107144911A TW 201927864 A TW201927864 A TW 201927864A
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polysiloxane
atom
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solar energy
semiconductor
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TW107144911A
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徐芳榮
李平
池田武史
金光男
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大陸商東麗先端材料研究開發（中國）有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
    • C08G77/398—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing boron or metal atoms
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
    • C08G77/56—Boron-containing linkages
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/04—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion materials in the liquid state

Abstract

A polysiloxane, containing at least a molecular structure fragment selected from one as shown in the following formula 1, (I), wherein, Q is an organic group containing a borate; T is an organic group containing borate, alkyl, and an organic group containing an alcoholic hydroxyl, or a hydroxyl group; X is alkyl or aryl; Y is alkyl, aryl or hydroxyl; n and m are integers, and the ratio of m to n is m : n = 0 : 100~90 : 10. A doping slurry prepared using the polysiloxane, on the basis of having good diffusivity, further has a good barrier property and a minimal diffusion in a gas. Meanwhile, since the polysiloxane itself contains a substituent group containing boron, there is no need to add other boron compounds, and since the polysiloxane is fat soluble, same can be made into a slurry of a printing type.

Description

聚矽氧烷及太陽能、半導體用摻雜漿料 Polysiloxane and doped paste for solar energy and semiconductor

本發明涉及聚矽氧烷、及用於太陽能和半導體的材料。具體而言，本發明涉及一系列取代基含有硼酸酯的聚矽氧烷的有機合成、及用於太陽能和半導體的摻雜材料。 The present invention relates to polysiloxanes and materials used in solar energy and semiconductors. In particular, the present invention relates to the organic synthesis of a series of polysiloxanes containing borate esters in substituents, and doping materials for solar energy and semiconductors.

在以往的半導體或者太陽能電池的製造中，在半導體基板中形成p型或者n型雜質擴散層的情況下，使用氣體摻雜劑或者摻雜漿料的方法均被提出過。但是，使用前述現有氣體摻雜劑或者摻雜漿料進行高溫熱擴散時，需要在非擴散面形成阻隔層。從而導致工藝過程冗長、複雜，同時成本也相應提高。如果使用離子注入方法，所需設備成本、維護成本都比較高。而且，現有漿料的性能、成本等難以達到一個有力平衡，導致其在太陽能電池產業中不具市場競爭力(參見專利文獻[1])。 In the manufacture of a conventional semiconductor or solar cell, when a p-type or an n-type impurity diffusion layer is formed in a semiconductor substrate, a method using a gas dopant or a doping paste has been proposed. However, when the conventional gas dopant or doping paste is used for high-temperature thermal diffusion, a barrier layer needs to be formed on the non-diffused surface. As a result, the process is lengthy and complicated, and the cost is correspondingly increased. If the ion implantation method is used, the equipment cost and maintenance cost are relatively high. In addition, it is difficult to achieve a strong balance between the performance and cost of the existing slurry, resulting in its lack of market competitiveness in the solar cell industry (see patent document [1]).

對於兩面都可以受光發電的雙面電池的製造工藝中，在太陽能電池所使用的半導體基板中使得p型以及n型的雜質擴散以形成雜質擴散層的工藝中，分別針對p型雜質擴散層以及n型雜質擴散層採用不同的工序。但是這樣的方法存在工序數增加的問題。如果採用具有阻隔性，即掩膜作用的旋塗型漿料來進行擴散工藝，可以達到減少工序降低成本的作用，但是旋塗型漿料在旋轉塗布過程中需要浪費>50%的漿料，無形之中增加了成本。同時雖然市面上有公司在推進 具有阻隔性，即掩膜作用的印刷型硼源漿料，但是因為使用了高成本的微粒子等原料，導致價格遠遠高於市場的需求，雖然退而求其次，將其應用在雷射等方法的局部擴散工藝中，但是仍然改變不了高成本帶來的量產困難。而且，採用兩片一組的方式塗布了硼源的一側貼合放置在石英舟的一個凹槽內，並在同一個爐管中進行硼磷共擴散的工藝後，兩片矽片由於微粒子的熔融黏在一起，從而導致不能分離矽片。 In the manufacturing process of a double-sided battery capable of receiving light from both sides, in the process of diffusing p-type and n-type impurities in a semiconductor substrate used in a solar cell to form an impurity diffusion layer, the p-type impurity diffusion layer and The n-type impurity diffusion layer uses different processes. However, such a method has a problem that the number of processes increases. If a spin-coating slurry with barrier properties, that is, a masking effect, is used to perform the diffusion process, it can reduce the process and reduce the cost, but the spin-coating slurry needs to waste more than 50% of the slurry in the spin coating process. Increasing costs invisibly. At the same time, although there are companies in the market Barrier, that is, masking printing boron source paste, but because of the use of high-cost particles and other raw materials, the price is far higher than the market demand, although the next best thing is to use it in lasers, etc. In the local diffusion process of the method, the mass production difficulty caused by high cost cannot be changed. In addition, the side coated with the boron source was placed in a groove of a quartz boat in a two-piece group, and the boron-phosphorus co-diffusion process was performed in the same furnace tube. The melts stick together, making it impossible to separate the silicon wafers.

另外作為硼源氣體摻雜劑一般為三溴化硼這樣的劇毒物質，對管路、尾氣吸收設備的要求較高，而且一旦洩露有發生大事故的可能、以及對周圍環境產生污染。 In addition, the boron source gas dopant is generally a highly toxic substance such as boron tribromide, which has high requirements on pipelines and exhaust gas absorption equipment, and once leaked, there may be a major accident, and pollution to the surrounding environment.

專利文獻[1]：中國專利申請公開文本CN 104538501A，魏青竹、陸俊宇、連維飛、倪志春，N型雙面電池及其製作方法，申請日為2015-01-15。 Patent Document [1]: Chinese Patent Application Publication CN 104538501A, Wei Qingzhu, Lu Junyu, Lian Weifei, Ni Zhichun, N-type double-sided battery and its manufacturing method, the application date is 2015-01-15.

為了解決現有半導體摻雜(包括太陽能電池p型和n型摻雜)中高成本、所使用的摻雜材料高毒性和環境污染性、摻雜的不均勻性而導致的良品率低下的缺陷，本發明提供一種聚矽氧烷、以及使用該聚矽氧烷製備的用於太陽能和半導體的摻雜漿料。 In order to solve the defects of low cost caused by the high cost, high toxicity of the doping materials used in the existing semiconductor doping (including p-type and n-type doping of solar cells, environmental pollution, and non-uniformity of doping), the present invention The invention provides a polysiloxane and a doping slurry for solar energy and semiconductors prepared using the polysiloxane.

本發明的摻雜漿料，由於原料成本較之微粒子等有了極大的降低，所以不論是製備成印刷型硼源漿料，還是製備成旋塗型硼源漿料，不論使用在整面塗布的工藝，還是局部塗布的工藝中，都具有很好的擴散均勻性以及相對於現有漿料的低成本，可以實現相關產品的市場競爭力。 Since the doped paste of the present invention has a greatly reduced raw material cost compared to particles and the like, whether it is prepared as a printed boron source paste or a spin-coated boron source paste, whether it is used for coating on the entire surface In the process, or in the process of partial coating, it has good diffusion uniformity and low cost compared to the existing slurry, which can achieve market competitiveness of related products.

本發明公開了一種聚矽氧烷，含有至少一種選自下式1所示的分子結構片段， 式1中，Q為含有硼酸酯的有機基團；T為含有硼酸酯的有機基團、烷基、含有醇羥基的有機基團或者羥基；X為烷基或者芳基；Y為烷基、芳基或者羥基；n和m為整數，並且m與n的比例為m：n=0：100~90：10。 The invention discloses a polysiloxane containing at least one molecular structure fragment selected from the following formula 1, In Formula 1, Q is an organic group containing a borate; T is an organic group containing a borate, an alkyl group, an organic group containing an alcoholic hydroxyl group, or a hydroxyl group; X is an alkyl group or an aryl group; Y is an alkane Group, aryl group or hydroxyl group; n and m are integers, and the ratio of m to n is m: n = 0: 100 ~ 90: 10.

上文所述的烷基、芳基中優選不含有硼。 The alkyl and aryl groups described above preferably do not contain boron.

出於為了易於製備、降低成本、穩定性的考慮，所述Q優選為式2所示的結構片段， 式2中，Z為碳原子數為7以下的亞烷基或者主鏈非氫原子數為7以下且含雜原子的亞烷基；R為與B原子相連的原子為碳原子的芳基、與B原子相連的原子為碳原子的烷基、與B原子相連的原子為氧原子的芳基、與B原子相連的原子為氧原子的烷基或者羥基；R1、R2、R3分別獨立為氫原子、碳原子數為3以下的有機基團或者R2與Z上的碳原子連接成環。 For consideration of ease of preparation, cost reduction, and stability, the Q is preferably a structural fragment shown in Formula 2. In Formula 2, Z is an alkylene group having 7 or less carbon atoms or an alkylene group having 7 or less non-hydrogen atoms in the main chain and a hetero atom; R is an aryl group having a carbon atom connected to the B atom, The atom connected to the B atom is an alkyl group of a carbon atom, the atom connected to the B atom is an aryl group, and the atom connected to the B atom is an oxygen or alkyl group; R1, R2, and R3 are each independently hydrogen. An atom, an organic group having 3 or less carbon atoms, or R2 is connected to a carbon atom on Z to form a ring.

本文中提到「有機基團」時，表示碳原子為規定範圍或規定值的有機基團，例如碳原子為規定範圍或規定值的常見取代基，例如烴類取代基，例如烷基、環烷基、烯基、炔基等。 When referring to "organic group" in this article, it means an organic group whose carbon atom is within a specified range or value. For example, common substituents whose carbon atom is within a specified range or value, such as hydrocarbon substituents, such as alkyl, ring Alkyl, alkenyl, alkynyl, etc.

在本文中使用時，「以上」、「以下」表示包括該記載之前的數值在內的範圍。並且，在本文中，記載為「某數值以上」，也表示並列地記載了「等於某數值」和「比某數值更高」的方案。類似地， 記載為「某數值以下」，也表示並列地記載了「等於某數值」和「比某數值更低」的方案。 As used herein, "above" and "below" indicate a range including the numerical values before the description. In addition, in this article, it is described as "more than a certain value", which means that the plan "equal to a certain value" and "higher than a certain value" are described in parallel. Similarly, Recorded as "below a certain value" also means that the plan "equal to a certain value" and "lower than a certain value" are recorded side by side.

出於為了使得聚矽氧烷易於熱分解、並且使得矽含量能夠使阻隔性和抑制氣中擴散的性能達到要求的考慮，所述Z優選為主鏈非氫原子數為7以下且含雜原子的亞烷基。 In order to make the polysiloxane easy to thermally decompose, and to make the silicon content meet the requirements of barrier properties and inhibition of diffusion in the gas, the Z is preferably 7 or less in the main chain and contains hetero atoms. Alkylene.

在本文中使用時，「氣中擴散」表示：在擴散過程中，摻雜漿料或者掩膜材料中的擴散劑成分向其周圍的氣體中揮發，並在氣體中擴散。 As used herein, "diffusion in gas" means that during the diffusion process, the diffusing agent component in the doping slurry or mask material volatilizes into the surrounding gas and diffuses in the gas.

出於水中溶解性、以及使得確保矽含量能夠使阻隔性、抑制氣中擴散的性能達到要求的考慮，優選所述R1、R2、R3分別獨立為氫原子、碳原子數為1的有機基團，或者R2與X上的碳原子連接成環。進一步優選所述R1、R2、R3均為氫原子。 In consideration of the solubility in water and the requirement of ensuring the silicon content to achieve the barrier properties and the ability to suppress the diffusion in the gas, it is preferred that the R1, R2, and R3 are each independently an organic group having a hydrogen atom and a carbon number of 1. , Or R2 is linked to a carbon atom on X to form a ring. More preferably, all of R1, R2, and R3 are hydrogen atoms.

出於為了增加硼含量從而提高擴散性、又或者增加矽含量從而提高阻隔性和抑制氣中擴散性的考慮，優選T為羥基、碳原子數為8以下的烷基或者含有式3所示的結構， 式3中W為碳原子數為7以下的亞烷基或者主鏈非氫原子數為7以下且含雜原子的亞烷基；R7為與B原子相連的原子為碳原子的芳基、與B原子相連的原子為碳原子的烷基、與B原子相連的原子為氧原子的芳基、與B原子相連的原子為氧原子的烷基或者羥基；R4、R5、R6分別獨立為氫原子、碳原子數為3以下的有機基團或者R5與W上的碳原子連接成環。 In order to increase the boron content to increase the diffusivity, or to increase the silicon content to improve the barrier properties and suppress the diffusivity in the gas, it is preferable that T is a hydroxyl group, an alkyl group having 8 or less carbon atoms, or a compound containing Formula 3 structure, In Formula 3, W is an alkylene group having 7 or less carbon atoms or an alkylene group having 7 or less non-hydrogen atoms in the main chain and a hetero atom; R7 is an aryl group having a carbon atom connected to the B atom, and The atom connected to the B atom is an alkyl group of a carbon atom, the atom connected to the B atom is an aryl group, and the atom connected to the B atom is an oxygen or alkyl group; R4, R5, and R6 are each independently a hydrogen atom. Or an organic group having 3 or less carbon atoms or R5 is connected to a carbon atom on W to form a ring.

出於為了使得聚矽氧烷易於熱分解、並且使得矽含量能夠使阻隔性和抑制氣中擴散的性能達到要求的考慮，所述W優選為主鏈非氫原子數為7以下且含雜原子的亞烷基。 In order to make the polysiloxane easy to thermally decompose, and to make the silicon content meet the requirements of the barrier properties and the ability to suppress the diffusion in the gas, the W is preferably 7 or less in the main chain and contains hetero atoms. Alkylene.

出於為了使得聚矽氧烷中矽含量能夠使阻隔性和抑制氣中擴散的性能達到要求的考慮，所述T優選為羥基。 In order that the silicon content in the polysiloxane can satisfy the requirements of the barrier property and the performance of suppressing the diffusion in the gas, the T is preferably a hydroxyl group.

出於為了保持阻隔性和抑制氣中擴散的性能的平衡，優選m與n的比例為m：n=0：100~50：50。 In order to maintain the balance of the barrier property and the performance of suppressing the diffusion in the gas, the ratio of m to n is preferably m: n = 0: 100 to 50:50.

出於為了可以有效調節矽的含量來調節所需的阻隔性和抑制氣中擴散的性能，優選m與n的比例為m：n=1：99~50：50。 In order to effectively adjust the content of silicon to adjust the required barrier properties and the performance of suppressing the diffusion in the gas, the ratio of m to n is preferably m: n = 1: 99 ~ 50: 50.

由於分子量過高溶解性總體降低，同時膠體化也容易發生，優選所述聚矽氧烷的重均分子量為500~50000。 Because the molecular weight is too high, the solubility is generally reduced, and colloidization is also easy to occur. The weight average molecular weight of the polysiloxane is preferably from 500 to 50,000.

出於存放使用中即使分子量增大也不會導致局部不均勻的考慮，優選所述聚矽氧烷的重均分子量為1000~13000。 Considering that even if the molecular weight is increased during storage and use, it does not cause local unevenness, the weight average molecular weight of the polysiloxane is preferably from 1,000 to 13,000.

出於延長保質期的考慮，優選所述聚矽氧烷的重均分子量為1500~6500。 In consideration of prolonging the shelf life, the weight average molecular weight of the polysiloxane is preferably 1500 to 6,500.

本發明的聚矽氧烷只要含有上述式1的分子結構片段即可，沒有特別限定。作為上述式1的分子結構片段，具體可列舉如下的例子。重複單元結構的實際排列方式並不限於下述結構例所示。 The polysiloxane of the present invention is not particularly limited as long as it contains the molecular structure fragment of Formula 1 described above. Specific examples of the molecular structure fragment of the above formula 1 include the following. The actual arrangement of the repeating unit structure is not limited to that shown in the following structural examples.

本發明還公開了一種用於太陽能和半導體的摻雜漿料(以下，也簡稱為「本發明的摻雜漿料」)，其含有作為摻雜劑的前文所述的聚矽氧烷。 The present invention also discloses a doping paste for solar energy and semiconductor (hereinafter, also simply referred to as the "doping paste of the present invention"), which contains the aforementioned polysiloxane as a dopant.

為了滿足圖案摻雜的需要，本發明的摻雜漿料中還可添加作為改善塗布性能的增黏劑，使其適用於絲網印刷。對於增黏劑沒有特別的限定，考慮到成本和性能的平衡，優選甲基纖維素、乙基纖維素、丙基纖維素、羥甲基纖維素、羥乙基纖維素、羥丙基纖維素、羧甲基纖維素、甲基羥乙基纖維素、乙基羥乙基纖維素、甲基羥丙基纖維素、醋酸纖維素、醋酸丁酸纖維素、聚丙烯醯胺、聚乙烯醇、聚乙烯吡咯烷酮、聚氧化乙烯、卡波樹脂、聚丙烯酸、聚丙烯酸酯或聚氨酯等。 In order to meet the needs of pattern doping, the doping paste of the present invention can also be added as a tackifier to improve coating performance, making it suitable for screen printing. There is no particular limitation on the thickener. Considering the balance between cost and performance, methyl cellulose, ethyl cellulose, propyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, and hydroxypropyl cellulose are preferred. , Carboxymethyl cellulose, methyl hydroxyethyl cellulose, ethyl hydroxyethyl cellulose, methyl hydroxypropyl cellulose, cellulose acetate, cellulose acetate butyrate, polyacrylamide, polyvinyl alcohol, Polyvinylpyrrolidone, polyethylene oxide, carbomer resin, polyacrylic acid, polyacrylate or polyurethane.

所述的用於太陽能和半導體的摻雜漿料，優選還含有溶 劑(以下也稱為「溶劑(A)」)。 The doped paste for solar energy and semiconductor preferably further contains a solvent Agent (hereinafter also referred to as "solvent (A)").

出於本發明所述聚矽氧烷在溶劑中的溶解性的考慮，優選所述溶劑(A)由0~10%的水以及90~100%有機溶劑組成。 In consideration of the solubility of the polysiloxane in the solvent according to the present invention, the solvent (A) is preferably composed of 0-10% water and 90-100% organic solvent.

為了進一步提升本發明所述聚矽氧烷在溶劑中的溶解性，優選所述溶劑(A)由0~5%的水以及95~100%有機溶劑組成。 In order to further improve the solubility of the polysiloxane in the solvent of the present invention, the solvent (A) is preferably composed of 0 to 5% water and 95 to 100% organic solvent.

為了更好地適用於旋轉塗布和印刷塗布，所述有機溶劑優選為沸點50~300℃的有機溶劑。 In order to be more suitable for spin coating and printing coating, the organic solvent is preferably an organic solvent having a boiling point of 50 to 300 ° C.

對於有機溶劑沒有特別的限定，優選1-甲氧基-2-丙醇、二丙酮醇、2-丙醇、正丁醇、3-甲氧基-3-甲基丁醇、二乙二醇甲***、丙二醇、二乙二醇單丁醚、二丙二醇單甲醚、α-松油醇、二乙二醇單甲醚、一縮二乙二醇、甲醇、乙醇、1,4-二氧六環、丙酮、丁酮、乳酸甲酯或乳酸乙酯等。 The organic solvent is not particularly limited, but 1-methoxy-2-propanol, diacetone alcohol, 2-propanol, n-butanol, 3-methoxy-3-methylbutanol, and diethylene glycol are preferred. Methyl ether, propylene glycol, diethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, α-terpineol, diethylene glycol monomethyl ether, diethylene glycol, methanol, ethanol, 1,4-dioxane Hexacyclic, acetone, methyl ethyl ketone, methyl lactate or ethyl lactate.

出於對前述用於太陽能和半導體的摻雜漿料的保存穩定性以及成本控制方面的考慮，優選發明所述聚矽氧烷的總重量為漿料重量的2~35%。 In consideration of the storage stability and cost control of the aforementioned doped pastes for solar energy and semiconductors, it is preferable that the total weight of the polysiloxane in the invention is 2 to 35% of the weight of the paste.

出於控制成本，在必要的時候可以選擇不含有其它用於改善黏度的高分子化合物或微粒子。 In order to control costs, it is possible to choose not to contain other polymer compounds or fine particles for improving viscosity when necessary.

出於成本控制以及確保擴散均勻性的考慮，所述摻雜劑優選僅含有上述所述的聚矽氧烷。 In view of cost control and ensuring diffusion uniformity, the dopant preferably contains only the polysiloxane described above.

圖1為阻隔性評價實驗中矽片放置方式的示意圖。 FIG. 1 is a schematic diagram of a silicon wafer placement method in a barrier property evaluation experiment.

圖2為擴散性能以及氣中擴散評測實驗中矽片放置方式的示意圖。 FIG. 2 is a schematic diagram of a diffusion performance and a silicon wafer placement method in a gas diffusion evaluation experiment.

下面參照優選的實施方式對本發明進行說明。實施方式僅作例示之用，並不對發明加以限制，本發明的本質性內容並不必須具有實施方式中記述的所有特徵。 Hereinafter, the present invention will be described with reference to preferred embodiments. The embodiments are only for the purpose of illustration and do not limit the invention. The essential content of the invention does not necessarily have all the features described in the embodiments.

本實施方式的聚矽氧烷的重複單元結構中含有硼酸酯結構，其適用於(但不僅限於)本發明的用於太陽能和半導體的摻雜漿料。前述重複單元中含硼酸酯結構的聚矽氧烷的合成中，可使用聚矽氧烷(1)、有機溶劑(2)、酸催化劑(3)(參見後述)，反應的監控可使用凝膠滲透色譜(GPC)測試分子量來判斷反應終點。下面對本實施方式的聚矽氧烷的合成所涉及的化學品及凝膠滲透色譜(GPC)進行說明。 The repeating unit structure of the polysiloxane of this embodiment contains a borate structure, which is suitable for (but not limited to) the doping paste for solar energy and semiconductor of the present invention. In the synthesis of the polysiloxane containing a borate structure in the aforementioned repeating unit, polysiloxane (1), an organic solvent (2), and an acid catalyst (3) can be used (see below). Gel permeation chromatography (GPC) tests molecular weight to determine the end of the reaction. The chemical and gel permeation chromatography (GPC) related to the synthesis of the polysiloxane according to this embodiment will be described below.

《聚矽氧烷(1)》 "Polysiloxane (1)"

聚矽氧烷(1)可以為一種或者多種，但是其分子結構中必須含有醇羥基或者含有反應後可完全水解生成醇羥基的官能團(4)。作為官能團(4)可列舉出酯官能團、環氧乙烷、環氧丙烷官能團或易水解醚類官能團等。 Polysiloxane (1) may be one or more, but its molecular structure must contain an alcoholic hydroxyl group or a functional group (4) that can be completely hydrolyzed to form an alcoholic hydroxyl group after the reaction. Examples of the functional group (4) include an ester functional group, an ethylene oxide, a propylene oxide functional group, and an easily hydrolyzable ether functional group.

作為聚矽氧烷(1)可列舉出由3-縮水甘油基氧丙基三甲氧基矽烷、2-(3,4-環氧環己烷)乙基三甲氧基矽烷、3-縮水甘油基三甲氧基矽烷、3-(異丁烯醯氧)丙基三甲氧基矽烷、3-(甲基丙烯醯氧)丙基三甲氧基矽烷、三乙氧基(3-環氧丙基丙氧基)矽烷、二乙氧基(3-縮水甘油基氧基丙基)甲基矽烷、3-環氧丙氧丙基(二甲氧基)甲基矽烷或[8-(環氧丙基氧)-正辛基]三甲氧基矽烷等單體聚合成的聚矽氧烷。 Examples of the polysiloxane (1) include 3-glycidyloxypropyltrimethoxysilane, 2- (3,4-epoxycyclohexane) ethyltrimethoxysilane, and 3-glycidyl. Trimethoxysilane, 3- (isobutylenefluorenyl) propyltrimethoxysilane, 3- (methacryloxy) propyltrimethoxysilane, triethoxy (3-epoxypropylpropoxy) Silane, diethoxy (3-glycidyloxypropyl) methylsilane, 3-glycidoxypropyl (dimethoxy) methylsilane, or [8- (glycidyloxy)- N-octyl] trimethoxysilane polymerized monomers and other polysiloxane.

《有機溶劑(2)》 "Organic Solvents (2)"

有機溶劑(2)為在110℃以下時於強酸條件下不易水解的同時沸點高於110℃的有機溶劑。 The organic solvent (2) is an organic solvent that is not easily hydrolyzed under strong acid conditions and has a boiling point higher than 110 ° C when the temperature is below 110 ° C.

作為有機溶劑(2)可列舉出1-甲氧基-2-丙醇、二丙酮醇、2-丙醇、正丁醇、3-甲氧基-3-甲基丁醇、二乙二醇甲***、丙二醇、二乙二醇單丁醚、二丙二醇單甲醚、α-松油醇、二乙二醇單甲醚、一縮二乙二醇、二丙二醇二甲醚、二乙二醇二甲醚、二甲苯、二丙二醇二甲醚、二乙二醇二甲醚、環己酮、苯甲醚、苯***、異丁醚或乙基苯等。 Examples of the organic solvent (2) include 1-methoxy-2-propanol, diacetone alcohol, 2-propanol, n-butanol, 3-methoxy-3-methylbutanol, and diethylene glycol. Methyl ether, propylene glycol, diethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, α-terpineol, diethylene glycol monomethyl ether, diethylene glycol, dipropylene glycol dimethyl ether, diethylene glycol Dimethyl ether, xylene, dipropylene glycol dimethyl ether, diethylene glycol dimethyl ether, cyclohexanone, anisole, phenyl ether, isobutyl ether or ethylbenzene.

《酸催化劑(3)》 "Acid Catalyst (3)"

酸催化劑(3)，用作為催化聚矽氧烷(1)中醇羥基與硼酸類化合物的脫水形成硼酸酯的反應、含有前述可水解生成醇羥基基團的聚矽氧烷(1)中可水解基團的水解以及水解生成的醇羥基與硼酸類化合物的脫水形成硼酸酯的反應。 The acid catalyst (3) is used to catalyze the dehydration of alcoholic hydroxyl groups and boronic acid compounds in polysiloxane (1) to form a boric acid ester, and in the polysiloxane (1) containing the aforementioned hydrolyzable alcoholic hydroxyl group The hydrolysis of the hydrolyzable group and the reaction of the alcoholic hydroxyl group formed by the hydrolysis with the dehydration of boric acid compounds to form a borate.

作為酸催化劑(3)可列舉出鹽酸、硫酸、硝酸或超強酸等。 Examples of the acid catalyst (3) include hydrochloric acid, sulfuric acid, nitric acid, and a super acid.

《凝膠滲透色譜(GPC)》 Gel Permeation Chromatography (GPC)

凝膠滲透色譜(GPC)作為反應監控手段，使用的凝膠滲透色譜儀器為島津(shimazu)S3-4100。色譜柱：TSKgel SuperHM-H、尺寸6.0mm I.D.×15cm、部件號0018001，微粒子尺寸3&5微米。測試條件為：流動相四氫呋喃、流量0.2毫升/分、柱溫40℃、單個樣品運行時間30分。製作標準曲線所使用的標準樣品為聚苯乙烯。 As a reaction monitoring means, gel permeation chromatography (GPC) is used as a shimazu S3-4100. Chromatographic column: TSKgel SuperHM-H, size 6.0mm I.D. × 15cm, part number 0018001, particle size 3 & 5 microns. The test conditions are: mobile phase tetrahydrofuran, flow rate 0.2 ml / min, column temperature 40 ° C, and a single sample run time of 30 minutes. The standard sample used to prepare the standard curve was polystyrene.

可使用本發明的聚矽氧烷來製備本發明的用於太陽能和半導體的摻雜漿料。所述摻雜漿料除了含有聚矽氧烷之外，還可以 含有溶劑(A)。此外，所述摻雜漿料還可以含有高分子黏結劑(B)。進而，所述摻雜漿料還可以含有增黏劑。下面，對本發明的用於太陽能和半導體的摻雜漿料中除了聚矽氧烷之外還可含有的各成分進行說明。 The polysiloxane of the present invention can be used to prepare the doped paste for solar energy and semiconductor of the present invention. In addition to the doping slurry containing polysiloxane, Contains solvent (A). In addition, the doped slurry may further contain a polymer binder (B). Furthermore, the doped slurry may further include a thickener. Hereinafter, each component which can be contained in addition to polysiloxane in the doped paste for solar energy and semiconductor of this invention is demonstrated.

《溶劑(A)》 "Solvent (A)"

溶劑(A)可以是不添加水的單一有機溶劑、有機溶劑的混合溶劑，也可以是有機溶劑與水的混合溶劑。單一溶劑的情況下優選沸點高於100℃的有機溶劑，從而防止溶劑揮發過而影響塗膜的質量。在混合溶劑的情況下也可以選用沸點低於100℃的有機溶劑，如果使用了沸點低於100℃的有機溶劑，理想的是，同時其中含有相對於溶劑總質量達到40質量%以上的沸點高於100℃的有機溶劑與水的混合溶劑。為了防止在塗膜工藝中，溶劑揮發過快影響性能，即使在混合溶劑中同樣優選沸點高於100℃的溶劑。 The solvent (A) may be a single organic solvent or a mixed solvent of organic solvents without adding water, or may be a mixed solvent of an organic solvent and water. In the case of a single solvent, an organic solvent having a boiling point higher than 100 ° C. is preferred to prevent the solvent from evaporating and affect the quality of the coating film. In the case of mixed solvents, organic solvents with a boiling point of less than 100 ° C can also be used. If organic solvents with a boiling point of less than 100 ° C are used, it is desirable that they contain a high boiling point of 40% by mass or more relative to the total mass of the solvent. Mixed solvent of organic solvent and water at 100 ° C. In order to prevent the solvent from evaporating too quickly during the coating process to affect performance, solvents with a boiling point higher than 100 ° C are also preferred even in mixed solvents.

在一種優選的方案中，所述溶劑(A)由0~10%的水、以及90~100%有機溶劑組成。在又一優選的方案中，所述溶劑(A)由0~5%的水、以及95~100%有機溶劑組成。在進一步優選的方案中，所述有機溶劑為沸點50~300℃的有機溶劑。 In a preferred solution, the solvent (A) is composed of 0-10% water and 90-100% organic solvent. In another preferred solution, the solvent (A) is composed of 0 to 5% of water and 95 to 100% of an organic solvent. In a further preferred embodiment, the organic solvent is an organic solvent having a boiling point of 50 to 300 ° C.

作為溶劑(A)中所含有的有機溶劑，可列舉出1-甲氧基-2-丙醇、二丙酮醇、2-丙醇、正丁醇、3-甲氧基-3-甲基丁醇、二乙二醇甲***、丙二醇、二乙二醇單丁醚、二丙二醇單甲醚、α-松油醇、二乙二醇單甲醚、一縮二乙二醇、甲醇、乙醇、1,4-二氧六環、丙酮、丁酮、乳酸甲酯、乳酸乙酯、二甲苯、二丙二醇二甲醚、二乙二醇二甲醚、環己酮、苯甲醚、苯***、異丁醚、乙基苯等。 Examples of the organic solvent contained in the solvent (A) include 1-methoxy-2-propanol, diacetone alcohol, 2-propanol, n-butanol, and 3-methoxy-3-methylbutane. Alcohol, diethylene glycol methyl ether, propylene glycol, diethylene glycol monobutyl ether, dipropylene glycol monomethyl ether, α-terpineol, diethylene glycol monomethyl ether, diethylene glycol, methanol, ethanol, 1,4-dioxane, acetone, methyl ethyl ketone, methyl lactate, ethyl lactate, xylene, dipropylene glycol dimethyl ether, diethylene glycol dimethyl ether, cyclohexanone, anisole, phenyl ether, Isobutyl ether, ethylbenzene, etc.

《高分子黏結劑(B)》 《Polymer Adhesive (B)》

高分子黏結劑(B)具有將上述摻雜劑成分均勻分佈在摻雜漿料以及掩膜材料烘乾後所形成的固體成分裡的功能，這樣有助於對目標半導體基板的摻雜更均勻。 The polymer binder (B) has the function of uniformly distributing the above-mentioned dopant components in the solid components formed after the dopant paste and the masking material are dried, which helps the target semiconductor substrate to be more uniformly doped. .

上述高分子黏結劑(B)為聚丙烯酸系非矽高分子，或者重複單元含有醇羥基的非矽系高分子。其中優選重複單元含有醇羥基的非矽系高分子，例如聚乙烯醇、聚丙烯醇等。 The polymer binder (B) is a polyacrylic non-silicon polymer or a non-silicon polymer containing an alcoholic hydroxyl group in a repeating unit. Among these, a non-silicon polymer containing an alcoholic hydroxyl group in a repeating unit is preferable, for example, polyvinyl alcohol, polyalcohol, and the like.

《增黏劑》 "Tackifier"

增黏劑可以是單一的高分子，也可以是2種以上增黏劑的混合物。在本發明摻雜漿料中，增黏劑為溶解狀態、或者為凝膠狀態。 The tackifier may be a single polymer or a mixture of two or more tackifiers. In the doped slurry of the present invention, the tackifier is in a dissolved state or a gel state.

作為增黏劑，可以列舉出甲基纖維素、乙基纖維素、丙基纖維素、羥甲基纖維素、羥乙基纖維素、羥丙基纖維素、羧甲基纖維素、甲基羥乙基纖維素、乙基羥乙基纖維素、甲基羥丙基纖維素、醋酸纖維素、醋酸丁酸纖維素、聚丙烯醯胺、聚乙烯醇、聚乙烯吡咯烷酮、聚氧化乙烯、卡波樹脂、聚丙烯酸、聚丙烯酸酯或聚氨酯等。 Examples of the thickener include methyl cellulose, ethyl cellulose, propyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, and methyl hydroxy cellulose. Ethyl cellulose, ethyl hydroxyethyl cellulose, methyl hydroxypropyl cellulose, cellulose acetate, cellulose acetate butyrate, polypropylene amidamine, polyvinyl alcohol, polyvinyl pyrrolidone, polyethylene oxide, carbo Resin, polyacrylic, polyacrylate, or polyurethane.

《非含硼酸酯聚矽氧烷的合成(即原料的合成)》 "Synthesis of non-borate-containing polysiloxane (ie, synthesis of raw materials)"

如下所述的本合成方法為通用方法，具體實際的單體、單體比例、溶劑等根據目標化合物可以進行相應調整。 The synthesis method described below is a general method, and specific actual monomers, monomer ratios, solvents, etc. can be adjusted according to the target compound.

室溫下，在大小合適的反應器中依次加入41.21克3-縮水甘油基氧丙基三甲氧基矽烷、95.02克甲基三甲氧基矽烷和130.47克二乙二醇單甲醚。加熱升溫至40℃，然後滴加濃硫酸(0.44克)和水(78.47克)的混合溶液。滴加完成後繼續在40℃攪拌1小時。然後 升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後升高油浴溫度至120℃，攪拌。油浴升溫至120℃之後使用GPC檢測反應直至達到目標重均分子量4500±200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到用於合成本發明的硼酸酯聚矽氧烷的聚矽氧烷原料。 At room temperature, 41.21 grams of 3-glycidyloxypropyltrimethoxysilane, 95.02 grams of methyltrimethoxysilane, and 130.47 grams of diethylene glycol monomethyl ether were sequentially added to a reactor of a suitable size. The temperature was raised to 40 ° C, and then a mixed solution of concentrated sulfuric acid (0.44 g) and water (78.47 g) was added dropwise. After completion of the dropwise addition, stirring was continued at 40 ° C for 1 hour. then The temperature was raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Then raise the oil bath temperature to 120 ° C and stir. After the oil bath was heated to 120 ° C, the reaction was detected by GPC until a target weight average molecular weight of 4500 ± 200 g / mol was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. A polysiloxane raw material for synthesizing the borate polysiloxane of the present invention is obtained.

以下製備例中使用的原料019、原料038、原料045、原料089、原料127、原料130、原料163、原料235、原料244、原料271、原料274、原料278、原料279、原料286、原料287、原料352均可由本領域已知的方法(例如上文所述的方法)製得，根據具體結構，在溶劑、原料(包含原料配比)、催化劑(例如，對於環氧開環用強酸，不開環時使用弱酸，例如苯甲酸等)部分做相應調整即可。例如，原料019、原料038、原料163、原料274、原料352可按下述方法來合成。 Raw material 019, raw material 038, raw material 045, raw material 089, raw material 127, raw material 130, raw material 163, raw material 235, raw material 244, raw material 271, raw material 274, raw material 278, raw material 279, raw material 286, raw material 287 used in the following preparation examples The raw material 352 can be prepared by methods known in the art (such as the method described above). According to the specific structure, the solvent, the raw material (including the raw material ratio), and the catalyst (for example, for a strong acid for epoxy ring opening, When the ring does not open, use a weak acid (such as benzoic acid, etc.) to adjust accordingly. For example, raw material 019, raw material 038, raw material 163, raw material 274, and raw material 352 can be synthesized by the following method.

原料019製備：在大小合適的反應器中依次加入7.13克2,3-環氧丙基三甲氧基矽烷、42.55克甲基三甲氧基矽烷和49.28克3-甲氧基-3-甲基丁醇。加熱升溫至40℃，然後滴加濃硫酸(0.20克)和水(24.55克)的混合溶液。滴加完成後繼續在40℃攪拌1小時。然後升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後升高油浴溫度至120℃，攪拌。油浴升溫至120℃之後使用GPC檢測反應直至達到目標重均分子量4500±200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。 Preparation of raw material 019: 7.13 grams of 2,3-epoxypropyltrimethoxysilane, 42.55 grams of methyltrimethoxysilane, and 49.28 grams of 3-methoxy-3-methylbutane were sequentially added to a reactor of a suitable size. alcohol. The temperature was raised to 40 ° C, and then a mixed solution of concentrated sulfuric acid (0.20 g) and water (24.55 g) was added dropwise. After completion of the dropwise addition, stirring was continued at 40 ° C for 1 hour. The temperature was then raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Then raise the oil bath temperature to 120 ° C and stir. After the oil bath was heated to 120 ° C, the reaction was detected by GPC until a target weight average molecular weight of 4500 ± 200 g / mol was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C.

原料038製備：在大小合適的反應器中依次加入35.65克2,3-環氧丙基三甲氧基矽烷、23.25克二甲基二甲氧基矽烷和63.10克3-甲氧基-3-甲基丁醇。加熱升溫至40℃，然後滴加濃硫酸(0.20克) 和水(19.80克)的混合溶液。滴加完成後繼續在40℃攪拌1小時。然後升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後升高油浴溫度至120℃，攪拌。油浴升溫至120℃之後使用GPC檢測反應直至達到目標重均分子量4500±200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。 Preparation of raw material 038: 35.65 g of 2,3-epoxypropyltrimethoxysilane, 23.25 g of dimethyldimethoxysilane, and 63.10 g of 3-methoxy-3-methyl were sequentially added to a reactor of a suitable size. Butyl alcohol. Heat to 40 ° C, then add concentrated sulfuric acid (0.20 g) dropwise And water (19.80 g). After completion of the dropwise addition, stirring was continued at 40 ° C for 1 hour. The temperature was then raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Then raise the oil bath temperature to 120 ° C and stir. After the oil bath was heated to 120 ° C, the reaction was detected by GPC until a target weight average molecular weight of 4500 ± 200 g / mol was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C.

原料163製備：在大小合適的反應器中依次加入30.04克2,3-環氧丙基三甲氧基矽烷、54.96克二甲基二甲氧基矽烷和91.46克二乙二醇單甲醚。加熱升溫至40℃，然後滴加苯甲酸(0.49克)和水(20.59克)的混合溶液。滴加完成後繼續在40℃攪拌1小時。然後升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後升高油浴溫度至120℃，攪拌。油浴升溫至120℃之後使用GPC檢測反應直至達到目標重均分子量4500±200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。 Preparation of raw material 163: 30.04 grams of 2,3-epoxypropyltrimethoxysilane, 54.96 grams of dimethyldimethoxysilane, and 91.46 grams of diethylene glycol monomethyl ether were sequentially charged into a reactor of a suitable size. The temperature was raised to 40 ° C, and then a mixed solution of benzoic acid (0.49 g) and water (20.59 g) was added dropwise. After completion of the dropwise addition, stirring was continued at 40 ° C for 1 hour. The temperature was then raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Then raise the oil bath temperature to 120 ° C and stir. After the oil bath was heated to 120 ° C, the reaction was detected by GPC until a target weight average molecular weight of 4500 ± 200 g / mol was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C.

原料274製備：在大小合適的反應器中依次加入94.54克3-縮水甘油基氧丙基三甲氧基矽烷和116.56克苯***。加熱升溫至40℃，然後滴加濃硫酸(0.20克)和水(31.68克)的混合溶液。滴加完成後繼續在40℃攪拌1小時。然後升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後升高油浴溫度至120℃，攪拌。油浴升溫至120℃之後使用GPC檢測反應直至達到目標重均分子量4500±200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。 Preparation of raw material 274: 94.54 grams of 3-glycidyloxypropyltrimethoxysilane and 116.56 grams of phenyl ether were sequentially added to a reactor of a suitable size. The temperature was raised to 40 ° C, and then a mixed solution of concentrated sulfuric acid (0.20 g) and water (31.68 g) was added dropwise. After completion of the dropwise addition, stirring was continued at 40 ° C for 1 hour. The temperature was then raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Then raise the oil bath temperature to 120 ° C and stir. After the oil bath was heated to 120 ° C, the reaction was detected by GPC until a target weight average molecular weight of 4500 ± 200 g / mol was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C.

原料352製備：在大小合適的反應器中依次加入98.55克2-(3,4-環氧環己基)乙基三甲氧基矽烷和122.58克苯***。加熱升溫至40℃，然後滴加濃硫酸(0.20克)和水(31.68克)的混合溶液。滴 加完成後繼續在40℃攪拌1小時。然後升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後升高油浴溫度至120℃，攪拌。油浴升溫至120℃之後使用GPC檢測反應直至達到目標重均分子量4500±200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。 Preparation of raw material 352: 98.55 grams of 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane and 122.58 grams of phenyl ether were sequentially added to a reactor of a suitable size. The temperature was raised to 40 ° C, and then a mixed solution of concentrated sulfuric acid (0.20 g) and water (31.68 g) was added dropwise. drop After the addition was completed, stirring was continued at 40 ° C for 1 hour. The temperature was then raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Then raise the oil bath temperature to 120 ° C and stir. After the oil bath was heated to 120 ° C, the reaction was detected by GPC until a target weight average molecular weight of 4500 ± 200 g / mol was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C.

《含硼酸酯聚矽氧烷的合成》 "Synthesis of Boron-containing Polysiloxane"

製備例1： Preparation Example 1:

室溫下，向大小合適的反應器中依次加入100克原料019(n：m=10：90)的40%的3-甲氧基-3-甲基丁醇溶液、2.92克甲基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢測反應直至達到目標重均分子量30000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A019。 At room temperature, 100 grams of a raw material 019 (n: m = 10: 90) in 40% of a 3-methoxy-3-methylbutanol solution and 2.92 grams of methylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, the reaction was detected using GPC until the target weight average molecular weight of 30,000 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A019 provided by the present invention is obtained.

製備例2： Preparation Example 2:

室溫下，向大小合適的反應器中依次加入100克原料038(n：m=50：50)的40%的3-甲氧基-3-甲基丁醇溶液、14.05克乙基硼酸。 加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應1.5小時後，使用GPC檢測反應直至達到目標重均分子量20000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A038。 At room temperature, 100 grams of a raw material 038 (n: m = 50: 50) in a 40% solution of 3-methoxy-3-methylbutanol and 14.05 grams of ethylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 1.5 hours of reaction, the reaction was monitored using GPC until the target weight average molecular weight was 20,000 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A038 provided by the present invention is obtained.

製備例3： Preparation Example 3:

室溫下，向大小合適的反應器中依次加入100克原料045(n：m=90：10)的40%的3-甲氧基-3-甲基丁醇溶液、17.13克硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應3小時後，使用GPC檢測反應直至達到目標重均分子量50000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A045。 At room temperature, 100 grams of a raw material 045 (n: m = 90: 10) in 40% of a 3-methoxy-3-methylbutanol solution and 17.13 grams of boric acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 3 hours of reaction, the reaction was detected using GPC until a target weight average molecular weight of 50,000 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A045 provided by the present invention is obtained.

製備例4： Preparation Example 4:

室溫下，向大小合適的反應器中依次加入100克原料089(n：m=80：20)的40%的二乙二醇二甲醚溶液、11.62克硼酸、24.43克3-甲氧基-3-甲基丁醇。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢 測反應直至達到目標重均分子量23000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A089。 At room temperature, 100 grams of raw material 089 (n: m = 80: 20) in 40% diethylene glycol dimethyl ether solution, 11.62 grams of boric acid, and 24.43 grams of 3-methoxy were sequentially added to a reactor of a suitable size -3-methylbutanol. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, check with GPC The reaction was measured until the target weight average molecular weight was 23,000 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A089 provided by the present invention is obtained.

製備例5： Preparation Example 5:

室溫下，向大小合適的反應器中依次加入100克原料127(n：m=70：30)的40%的二丙二醇二甲醚溶液、9.55克甲基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應1.6小時後，使用GPC檢測反應直至達到目標重均分子量17000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A127。 At room temperature, 100 g of a raw material 127 (n: m = 70: 30) of a 40% dipropylene glycol dimethyl ether solution and 9.55 g of methylboronic acid were sequentially charged into a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 1.6 hours of reaction, the reaction was monitored using GPC until the target weight-average molecular weight was 17,000 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A127 provided by the present invention is obtained.

製備例6： Preparation Example 6:

室溫下，向大小合適的反應器中依次加入100克原料130(n：m=60：40)的40%的苯甲醚溶液、17.23克苯基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2.1小時後，使用GPC檢測反應直至達到目標重均分子量21000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。 得到本發明提供的聚矽氧烷A130。 At room temperature, 100 grams of a raw material 130 (n: m = 60: 40) of a 40% anisole solution and 17.23 grams of phenylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2.1 hours of reaction, the reaction was monitored using GPC until a target weight average molecular weight of 21,000 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A130 provided by the present invention is obtained.

製備例7： Preparation Example 7:

室溫下，在大小合適的反應器中依次加入37克原料163(n：m=30：70)、60克二乙二醇單甲醚。加熱升溫至40℃，然後滴加濃硫酸(0.05克)和水(9.5克)的混合溶液。滴加完成後繼續在40℃攪拌1小時。然後升溫至70℃，並攪拌1小時20分鐘。然後升溫至100℃，並攪拌1小時。之後加入4.71克甲基硼酸，繼續維持反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢測反應直至達到目標重均分子量16000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A163。 At room temperature, 37 g of raw material 163 (n: m = 30: 70) and 60 g of diethylene glycol monomethyl ether were sequentially charged into a reactor of a suitable size. The temperature was raised to 40 ° C, and then a mixed solution of concentrated sulfuric acid (0.05 g) and water (9.5 g) was added dropwise. After completion of the dropwise addition, stirring was continued at 40 ° C for 1 hour. The temperature was then raised to 70 ° C and stirred for 1 hour and 20 minutes. The temperature was then raised to 100 ° C and stirred for 1 hour. Thereafter, 4.71 g of methylboronic acid was added, and the reaction solution was maintained at about 100 ° C. (120 ° C. in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, the reaction was monitored using GPC until a target weight average molecular weight of 16,000 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A163 provided by the present invention is obtained.

製備例8： Preparation Example 8:

室溫下，向大小合適的反應器中依次加入100克原料235的40%的苯***溶液、12.33克甲基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2.1小時後，使用GPC檢測反應直至達到目標重均分子量8000克/莫耳。 冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A235。 At room temperature, 100 grams of raw material 235 in 40% phenyl ether solution and 12.33 grams of methylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2.1 hours of reaction, the reaction was monitored using GPC until the target weight average molecular weight was 8000 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A235 provided by the present invention is obtained.

製備例9： Preparation Example 9:

室溫下，向大小合適的反應器中依次加入100克原料244的40%的苯***溶液、15.43克甲基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應3小時後，使用GPC檢測反應直至達到目標重均分子量40000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A244。 At room temperature, 100 g of a raw material 244 in 40% phenyl ether solution and 15.43 g of methylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 3 hours of reaction, the reaction was monitored using GPC until a target weight average molecular weight of 40,000 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A244 provided by the present invention is obtained.

製備例10： Preparation Example 10:

室溫下，向大小合適的反應器中依次加入100克原料271(n：m=95：5)的40%的苯***溶液、11.71克甲基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應1.5小時後，使用GPC檢測反應直至達到目標重均分子量5200克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A271。 At room temperature, 100 g of a raw material 271 (n: m = 95: 5) in a 40% phenyl ether solution and 11.71 g of methylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 1.5 hours of reaction, the reaction was detected using GPC until the target weight average molecular weight was 5200 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A271 provided by the present invention is obtained.

製備例11： Preparation Example 11:

室溫下，向大小合適的反應器中依次加入100克原料274(n：m=90：10)的40%的苯***溶液、22.60克苯基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢測反應直至達到目標重均分子量6600克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A274。 At room temperature, 100 g of a raw material 274 (n: m = 90: 10) in a 40% phenyl ether solution and 22.60 g of phenylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, the reaction was monitored using GPC until a target weight average molecular weight of 6600 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A274 provided by the present invention is obtained.

製備例12： Preparation Example 12:

室溫下，向大小合適的反應器中依次加入100克原料278(n：m=99：1)的40%的苯***溶液、12.60克硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢測反應直至達到目標重均分子量6000克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A278。 At room temperature, 100 grams of a raw material 278 (n: m = 99: 1) in 40% phenyl ether solution and 12.60 grams of boric acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, the reaction was monitored using GPC until the target weight average molecular weight was 6000 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A278 provided by the present invention is obtained.

製備例13： Preparation Example 13:

室溫下，向大小合適的反應器中依次加入100克原料279(n：m=80：20)的40%的苯***溶液、10.19克硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢測反應直至達到目標重均分子量5800克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A279。 At room temperature, 100 grams of a raw material 279 (n: m = 80: 20) in 40% phenyl ether solution and 10.19 grams of boric acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, the reaction was measured using GPC until the target weight average molecular weight was 5800 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A279 provided by the present invention is obtained.

製備例14： Preparation Example 14:

室溫下，向大小合適的反應器中依次加入100克原料286(n：m=90：10)的40%的苯***溶液、11.04克硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2.4小時後，使用GPC檢測反應直至達到目標重均分子量5800克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A286。 At room temperature, 100 grams of raw material 286 (n: m = 90: 10) in 40% phenyl ether solution and 11.04 grams of boric acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2.4 hours of reaction, the reaction was measured using GPC until the target weight average molecular weight was 5800 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A286 provided by the present invention is obtained.

製備例15： Preparation Example 15:

室溫下，向大小合適的反應器中依次加入100克原料287(n：m=90：10)的40%的苯***溶液、11.62克硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2.5小時後，使用GPC檢測反應直至達到目標重均分子量6300克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A287。 At room temperature, 100 grams of raw material 287 (n: m = 90: 10) in 40% phenyl ether solution and 11.62 grams of boric acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2.5 hours of reaction, the reaction was monitored using GPC until the target weight average molecular weight was 6300 g / mole. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A287 provided by the present invention is obtained.

製備例16： Preparation Example 16:

室溫下，向大小合適的反應器中依次加入100克原料352的40%的苯***溶液、11.72克甲基硼酸。加熱升溫至反應液100℃左右(油浴120℃)，並且通入氮氣流，除去反應中生成的水。反應2小時後，使用GPC檢測反應直至達到目標重均分子量6700克/莫耳。冷卻到40℃以下後，轉移到其它容器-20~40℃保存。得到本發明提供的聚矽氧烷A352。 At room temperature, 100 grams of a raw material 352 in 40% phenyl ether solution and 11.72 grams of methylboronic acid were sequentially added to a reactor of a suitable size. The temperature of the reaction solution was raised to about 100 ° C (120 ° C in an oil bath), and a nitrogen gas flow was passed to remove water generated during the reaction. After 2 hours of reaction, the reaction was monitored using GPC until a target weight average molecular weight of 6700 g / mole was reached. After cooling below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. The polysiloxane A352 provided by the present invention is obtained.

《用於太陽能和半導體的摻雜漿料的製備》 《Preparation of doped slurry for solar energy and semiconductor》

本發明的用於太陽能和半導體的摻雜漿料。 The doping paste for solar energy and semiconductor of the present invention.

實施例1： Example 1:

室溫下，在大小合適的反應器中加入20克製備例1所得A019，邊攪拌邊滴加由72克3-甲氧基-3-甲基丁醇與8克純淨水組成的混合溶劑。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A019 obtained in Preparation Example 1 was placed in a reactor of a suitable size, and a mixed solvent consisting of 72 grams of 3-methoxy-3-methylbutanol and 8 grams of purified water was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例2： Example 2:

室溫下，在大小合適的反應器中加入25克製備例2所得A038，邊攪拌邊滴加75克3-甲氧基-3-甲基丁醇。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 25 grams of A038 obtained in Preparation Example 2 was placed in a reactor of a suitable size, and 75 grams of 3-methoxy-3-methylbutanol was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例3： Example 3:

室溫下，在大小合適的反應器中加入20克製備例3所得A045，邊攪拌邊滴加由76克3-甲氧基-3-甲基丁醇與4克純淨水組成的混合溶劑。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A045 obtained in Preparation Example 3 was added to a reactor of a suitable size, and a mixed solvent consisting of 76 grams of 3-methoxy-3-methylbutanol and 4 grams of purified water was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例4： Example 4:

室溫下，在大小合適的反應器中加入25克製備例4所得A089，邊攪拌邊滴加75克二乙二醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於 太陽能和半導體的材料。 At room temperature, 25 grams of A089 obtained in Preparation Example 4 was added to a reactor of a suitable size, and 75 grams of diethylene glycol dimethyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a method for Solar and semiconductor materials.

實施例5： Example 5:

室溫下，在大小合適的反應器中加入25克製備例5所得A127，邊攪拌邊滴加75克二丙二醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 25 grams of A127 obtained in Preparation Example 5 was placed in a reactor of a suitable size, and 75 grams of dipropylene glycol dimethyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例6： Example 6:

室溫下，在大小合適的反應器中加入20克製備例6所得A130，邊攪拌邊滴加80克苯甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A130 obtained in Preparation Example 6 was placed in a reactor of a suitable size, and 80 grams of anisole was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例7： Example 7:

室溫下，在大小合適的反應器中加入20克製備例7所得A163，邊攪拌邊滴加72克二乙二醇單甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A163 obtained in Preparation Example 7 was charged into a reactor of a suitable size, and 72 grams of diethylene glycol monomethyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例8： Example 8:

室溫下，在大小合適的反應器中加入30克製備例8所得A235，邊攪拌邊滴加50克二乙二醇單甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於 太陽能和半導體的材料。 At room temperature, 30 grams of A235 obtained in Preparation Example 8 was charged into a reactor of a suitable size, and 50 grams of diethylene glycol monomethyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a method for Solar and semiconductor materials.

實施例9： Example 9:

室溫下，在大小合適的反應器中加入20克製備例8所得A235，邊攪拌邊滴加80克二乙二醇單甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A235 obtained in Preparation Example 8 was added to a reactor of a suitable size, and 80 grams of diethylene glycol monomethyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例10： Example 10:

室溫下，在大小合適的反應器中加入20克製備例9所得A244，邊攪拌邊滴加72克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 g of A244 obtained in Preparation Example 9 was placed in a reactor of a suitable size, and 72 g of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例11： Example 11:

室溫下，在大小合適的反應器中加入25克製備例10所得A271，邊攪拌邊滴加75克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 25 grams of A271 obtained in Preparation Example 10 was placed in a reactor of a suitable size, and 75 grams of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例12： Example 12:

室溫下，在大小合適的反應器中加入25克製備例11所得A274，邊攪拌邊滴加75克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和 半導體的材料。 At room temperature, 25 grams of A274 obtained in Preparation Example 11 was placed in a reactor of a suitable size, and 75 grams of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a method for solar energy and Semiconductor materials.

實施例13： Example 13:

室溫下，在大小合適的反應器中加入20克製備例12所得A278，邊攪拌邊滴加80克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 g of A278 obtained in Preparation Example 12 was placed in a reactor of a suitable size, and 80 g of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例14： Example 14:

室溫下，在大小合適的反應器中加入25克製備例13所得A279，邊攪拌邊滴加75克一縮二乙二醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 25 grams of A279 obtained in Preparation Example 13 was added to a reactor of a suitable size, and 75 grams of diethylene glycol dimethyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例15： Example 15:

室溫下，在大小合適的反應器中加入30克製備例14所得A286，邊攪拌邊滴加50克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 30 g of A286 obtained in Preparation Example 14 was placed in a reactor of a suitable size, and 50 g of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例16： Embodiment 16:

室溫下，在大小合適的反應器中加入25克製備例15所得A287，邊攪拌邊滴加75克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和 半導體的材料。 At room temperature, 25 grams of A287 obtained in Preparation Example 15 was placed in a reactor of a suitable size, and 75 grams of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a method for solar energy and Semiconductor materials.

實施例17： Example 17:

室溫下，在大小合適的反應器中加入25克製備例16所得A352，邊攪拌邊滴加75克苯***。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 25 grams of A352 obtained in Preparation Example 16 was placed in a reactor of a suitable size, and 75 grams of phenyl ether was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例18： Embodiment 18:

室溫下，在大小合適的反應器中加入76克二乙二醇單甲醚，邊攪拌邊加入4克聚乙二醇(聚環氧乙烷)，室溫下攪拌待完全溶解後，邊攪拌邊滴加20克製備例8所得A235。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, put 76 g of diethylene glycol monomethyl ether in a reactor of appropriate size, add 4 g of polyethylene glycol (polyethylene oxide) while stirring, and stir at room temperature until it is completely dissolved. 20 g of A235 obtained in Preparation Example 8 was added dropwise with stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例19： Example 19:

室溫下，在大小合適的反應器中加入77克苯***，邊攪拌邊加入3克乙基纖維素，室溫下攪拌待完全溶解後，邊攪拌邊滴加20克製備例10所得A271。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 77 g of phenyl ether was added to a reactor of a suitable size. 3 g of ethyl cellulose was added while stirring. After stirring at room temperature to completely dissolve, 20 g of A271 obtained in Preparation Example 10 was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例20： Example 20:

室溫下，在大小合適的反應器中加入75克苯***，邊攪拌邊加入 5克聚氨酯，室溫下攪拌待完全溶解後，邊攪拌邊滴加20克製備例12所得A278。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, add 75 grams of phenyl ether to a properly sized reactor and add while stirring 5 grams of polyurethane was stirred at room temperature to be completely dissolved, and 20 grams of A278 obtained in Preparation Example 12 was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例21： Example 21:

室溫下，在大小合適的反應器中加入76克苯***，邊攪拌邊加入4克聚乙二醇(聚環氧乙烷)，室溫下攪拌待完全溶解後，邊攪拌邊滴加20克製備例13所得A279。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, put 76 grams of phenyl ether into a reactor of appropriate size, and add 4 grams of polyethylene glycol (polyethylene oxide) while stirring. After stirring at room temperature until completely dissolved, add 20 drops while stirring. G of A279 obtained in Preparation Example 13. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例22： Example 22:

室溫下，在大小合適的反應器中加入77克苯***，邊攪拌邊加入3克聚乙二醇(聚環氧乙烷)，室溫下攪拌待完全溶解後，邊攪拌邊滴加20克製備例13所得A279。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, add 77 grams of phenyl ether to a reactor of appropriate size, and add 3 grams of polyethylene glycol (polyethylene oxide) while stirring. After stirring at room temperature to completely dissolve, add 20 drops while stirring. G of A279 obtained in Preparation Example 13. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例23： Example 23:

室溫下，在大小合適的反應器中加入80克二乙二醇二甲醚，邊攪拌邊滴加20克製備例17所得A397。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 80 grams of diethylene glycol dimethyl ether was added to a reactor of a suitable size, and 20 grams of A397 obtained in Preparation Example 17 was added dropwise while stirring. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例24： Example 24:

室溫下，在大小合適的反應器中加入80克二乙二醇二甲醚，邊攪拌邊滴加20克其中A403重量含量為40%(其中m：n=15：85)的二乙二醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, add 80 grams of diethylene glycol dimethyl ether to a reactor of the appropriate size, and add 20 grams of diethylene glycol with 40% A403 by weight (where m: n = 15: 85) while stirring Glyme. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例25： Example 25:

室溫下，在大小合適的反應器中加入80克二乙二醇二甲醚，邊攪拌邊滴加20克其中A404重量含量為39%(其中m：n=10：90)的二乙二醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, add 80 grams of diethylene glycol dimethyl ether to a reactor of the appropriate size, and add 20 grams of diethylene glycol with 39% by weight of A404 (where m: n = 10: 90) while stirring. Glyme. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例26： Example 26:

室溫下，在大小合適的反應器中加入80克二乙二醇二甲醚，邊攪拌邊滴加20克其中A405重量含量為39%(其中m：n=10：90)的二乙二醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, add 80 grams of diethylene glycol dimethyl ether to a reactor of the appropriate size, and add 20 grams of diethylene glycol with 39% by weight of A405 (where m: n = 10: 90) while stirring. Glyme. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例27： Example 27:

室溫下，在大小合適的反應器中加入80克二乙二醇二甲醚，邊攪拌邊滴加20克其中A404重量含量為41%(其中m：n=5：95)的二乙二 醇二甲醚。滴加完成後繼續室溫攪拌1小時後，轉移到其它容器並在-20~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, add 80 grams of diethylene glycol dimethyl ether to a reactor of the appropriate size, and add 20 grams of diethylene glycol with 41% by weight of A404 (where m: n = 5: 95) while stirring. Glyme. After completion of the dropwise addition, stirring was continued at room temperature for 1 hour, and then transferred to another container and stored at -20 to 40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例28： Example 28:

室溫下，在大小合適的反應器中加入20克製備例6所得A130，邊攪拌邊滴加80克苯甲醚。然後分批加入10克聚環氧丙烷。然後40~50℃攪拌2小時，自然冷卻至室溫後，轉移到其它容器並在0~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A130 obtained in Preparation Example 6 was placed in a reactor of a suitable size, and 80 grams of anisole was added dropwise while stirring. Then 10 g of polypropylene oxide was added in portions. Then stir at 40 ~ 50 ℃ for 2 hours. After cooling to room temperature, transfer to another container and store at 0 ~ 40 ℃. The invention provides a material for solar energy and semiconductor provided by the present invention.

實施例29： Example 29:

室溫下，在大小合適的反應器中加入20克製備例6所得A284，邊攪拌邊滴加80克苯甲醚。然後分批加入8克聚乙烯吡咯烷酮。然後50~60℃攪拌2小時，自然冷卻至室溫後，轉移到其它容器並在0~40℃保存。得到本發明提供的一種用於太陽能和半導體的材料。 At room temperature, 20 grams of A284 obtained in Preparation Example 6 was placed in a reactor of a suitable size, and 80 grams of anisole was added dropwise while stirring. 8 grams of polyvinylpyrrolidone were then added in portions. Then stir at 50-60 ° C for 2 hours. After cooling to room temperature, transfer to another container and store at 0-40 ° C. The invention provides a material for solar energy and semiconductor provided by the present invention.

對比例1： Comparative Example 1:

室溫下，在大小合適的反應器中依次加入58.55克3-甲氧基-3-甲基丁醇和4.22克聚乙烯醇。加熱升溫至80℃，然後滴加36.00克水。滴加完成後繼續在80℃攪拌直至聚乙烯醇完全溶解。然後添加0.73克三氧化二硼，並在80℃繼續攪拌1小時。冷卻至40℃以下，轉移到其它容器並在-20~40℃保存。得到摻雜漿料。 At room temperature, 58.55 grams of 3-methoxy-3-methylbutanol and 4.22 grams of polyvinyl alcohol were added to a suitably sized reactor in this order. The temperature was raised to 80 ° C, and then 36.00 g of water was added dropwise. After the dropwise addition was completed, stirring was continued at 80 ° C until the polyvinyl alcohol was completely dissolved. Then 0.73 g of boron trioxide was added and stirring was continued at 80 ° C for 1 hour. Cool to below 40 ° C, transfer to another container and store at -20 ~ 40 ° C. A doped slurry was obtained.

對比例2： Comparative Example 2:

室溫下，在大小合適的反應器中依次加入58.55克3-甲氧基-3-甲 基丁醇和4.22克聚乙烯醇。加熱升溫至80℃，然後滴加36.00克水。滴加完成後繼續在80℃攪拌直至聚乙烯醇完全溶解。然後添加0.73克三氧化二硼，並在80℃繼續攪拌1小時。然後滴加重均分子量4400克/莫耳的聚二甲基矽氧烷40質量%二乙二醇單甲醚溶液16.67克。持續攪拌1小時。冷卻至40℃以下，有油狀物析出。得到摻雜漿料均勻性不足，無法用於後續測試。 At room temperature, 58.55 grams of 3-methoxy-3-formaldehyde were sequentially added to a reactor of the appropriate size. Butanol and 4.22 grams of polyvinyl alcohol. The temperature was raised to 80 ° C, and then 36.00 g of water was added dropwise. After the dropwise addition was completed, stirring was continued at 80 ° C until the polyvinyl alcohol was completely dissolved. Then 0.73 g of boron trioxide was added and stirring was continued at 80 ° C for 1 hour. Then, 16.67 g of a 40 mass% diethylene glycol monomethyl ether solution having a weight average molecular weight of 4400 g / mol was added dropwise. Stirring was continued for 1 hour. After cooling to 40 ° C or less, an oily substance precipitated. The obtained doped slurry has insufficient uniformity and cannot be used for subsequent testing.

《摻雜漿料以及掩膜材料的性能評測》 "Performance Evaluation of Doped Slurry and Masking Materials"

根據實施例1~29以及對比例1所製備的摻雜漿料及掩膜材料，分別使用旋轉塗布條件塗布在6英寸N型單晶矽片上，然後進行熱擴散來評測相關性能。漿料塗布條件分別為：A)低黏度漿料採用旋轉塗布法轉速2000rpm持續10秒；B)高黏度漿料採用絲網印刷法。矽片A：半導體用單面拋光，CZ直拉法摻磷N型單晶矽片，晶向100，電阻率0.5-6Ω.cm，厚度625微米。矽片B：太陽能電池用雙面製絨，CZ直拉法摻磷N型單晶矽片，晶向100，電阻率1-7Ω.cm，厚度180微米。阻隔性評價時矽片放置方式如說明書附圖1，氣中擴散性評價時矽片放置方式如說明書附圖2。電阻測試儀：日本NAPSON四探針電阻率測試儀，手動版RT-70V/RG-7。性能測評結果如下： The doping pastes and masking materials prepared according to Examples 1 to 29 and Comparative Example 1 were respectively coated on a 6-inch N-type single crystal silicon wafer using spin coating conditions, and then thermal diffusion was performed to evaluate related performance. The slurry coating conditions are: A) the low-viscosity slurry uses a spin coating method at a speed of 2000 rpm for 10 seconds; B) the high-viscosity slurry uses a screen printing method. Wafer A: Single-sided polishing for semiconductors, CZ Czochralski-doped N-type single crystal silicon wafer, crystal orientation 100, resistivity 0.5-6Ω.cm, thickness 625 microns. Wafer B: Double-sided texturing for solar cells, CZ direct-pulling phosphorus-doped N-type single crystal silicon wafer, crystal orientation 100, resistivity 1-7Ω.cm, thickness 180 microns. The method for placing silicon wafers in the evaluation of barrier properties is as shown in FIG. 1 of the specification, and the method for placing the silicon wafers in the evaluation of gas diffusion is as shown in FIG. 2 of the description. Resistance tester: Japan NAPSON four-probe resistivity tester, manual version RT-70V / RG-7. The performance evaluation results are as follows:

從上述表1和表2中的測評結果可以發現，與對比例1的性能相比，添加了本發明所提供的聚矽氧烷的摻雜漿料在保持同等程度的擴散性的基礎上，阻隔性和對氣中擴散的抑制均得到了大幅度 的提高。 From the evaluation results in the above Tables 1 and 2, it can be found that compared with the performance of Comparative Example 1, the doped slurry added with the polysiloxane provided by the present invention maintains the same degree of diffusibility, Both the barrier properties and the suppression of gas diffusion have been greatly improved Of improvement.

實際應用包含但並不僅限於：上述實施例所述的聚合物結構、分子量，摻雜漿料的組成成分、含量，適用的半導體基材，塗布的條件，擴散條件等。 Practical applications include, but are not limited to, the polymer structure, molecular weight, composition and content of doped slurry, applicable semiconductor substrate, coating conditions, diffusion conditions, etc. described in the above embodiments.

《工業上的可利用性》 `` Industrial availability ''

本發明所提供的聚矽氧烷可以用於摻雜漿料、半導體(包含太陽能電池)中。 The polysiloxane provided by the present invention can be used in doped pastes and semiconductors (including solar cells).

本申請要求以中國專利申請號CN 201711313794.7作為優先權申請的所有權益，該優先權申請的全部記載內容均通過參照併入本文，與將該優先權申請文件的所有記載直接記載於本申請文件中的情況一樣。 This application claims all the rights and interests of the Chinese patent application number CN 201711313794.7 as the priority application. The entire content of the priority application is incorporated herein by reference, and all the records of the priority application file are directly recorded in the application file. The situation is the same.

Claims (21)

一種聚矽氧烷，其特徵在於：含有至少一種選自下式1所示的分子結構片段， 式1中，Q為含有硼酸酯的有機基團；T為含有硼酸酯的有機基團、烷基、含有醇羥基的有機基團或者羥基；X為烷基或者芳基；Y為烷基、芳基或者羥基；n和m為整數，並且m與n的比例為m：n=0：100~90：10。 A polysiloxane, characterized in that it contains at least one molecular structure fragment selected from the following formula 1, In Formula 1, Q is an organic group containing a borate; T is an organic group containing a borate, an alkyl group, an organic group containing an alcoholic hydroxyl group, or a hydroxyl group; X is an alkyl group or an aryl group; Y is an alkane Group, aryl group or hydroxyl group; n and m are integers, and the ratio of m to n is m: n = 0: 100 ~ 90: 10. 如請求項1之聚矽氧烷，其中，所述Q為式2所示的結構片段， 式2中，Z為碳原子數為7以下的亞烷基或者主鏈非氫原子數為7以下且含雜原子的亞烷基；R為與B原子相連的原子為碳原子的芳基、與B原子相連的原子為碳原子的烷基、與B原子相連的原子為氧原子的芳基、與B原子相連的原子為氧原子的烷基或者羥基；R1、R2、R3分別獨立為氫原子、碳原子數為3以下的有機基團，或者R2與Z上的碳原子連接成環。 The polysiloxane of claim 1, wherein Q is a structural fragment represented by Formula 2, In Formula 2, Z is an alkylene group having 7 or less carbon atoms or an alkylene group having 7 or less non-hydrogen atoms in the main chain and a hetero atom; R is an aryl group having a carbon atom connected to the B atom, The atom connected to the B atom is an alkyl group of a carbon atom, the atom connected to the B atom is an aryl group, and the atom connected to the B atom is an oxygen or alkyl group; R1, R2, and R3 are each independently hydrogen. Atoms, organic groups having 3 or less carbon atoms, or R2 and carbon atoms on Z are connected to form a ring. 如請求項2之聚矽氧烷，其中，所述Z為主鏈非氫原子數為7以下且含雜原子的亞烷基。 The polysiloxane according to claim 2, wherein Z is an alkylene group having 7 or less non-hydrogen atoms in the main chain and containing a hetero atom. 如請求項2之聚矽氧烷，其中，所述R1、R2、R3分別獨立為氫原子、碳原子數為1的有機基團，或者R2與Z上的碳原子連接成環。 For example, the polysiloxane of claim 2, wherein R1, R2, and R3 are each independently a hydrogen atom and an organic group having 1 carbon atom, or R2 and a carbon atom on Z are connected to form a ring. 如請求項1之聚矽氧烷，其中，T為羥基、碳原子數為8以下的 烷基，或者T含有式3所示的結構， 式3中W為碳原子數為7以下的亞烷基或者主鏈非氫原子數為7以下且含雜原子的亞烷基；R7為與B原子相連的原子為碳原子的芳基、與B原子相連的原子為碳原子的烷基、與B原子相連的原子為氧原子的芳基、與B原子相連的原子為氧原子的烷基或者羥基；R4、R5、R6分別獨立為氫原子、碳原子數為3以下的有機基團或者R5與W上的碳原子連接成環。 For example, the polysiloxane of claim 1, wherein T is a hydroxyl group, an alkyl group having 8 or less carbon atoms, or T contains a structure represented by Formula 3, In Formula 3, W is an alkylene group having 7 or less carbon atoms or an alkylene group having 7 or less non-hydrogen atoms in the main chain and a hetero atom; R7 is an aryl group having a carbon atom connected to the B atom, and The atom connected to the B atom is an alkyl group of a carbon atom, the atom connected to the B atom is an aryl group, and the atom connected to the B atom is an oxygen or alkyl group; R4, R5, and R6 are each independently a hydrogen atom. Or an organic group having 3 or less carbon atoms or R5 is connected to a carbon atom on W to form a ring. 如請求項5之聚矽氧烷，其中，所述W為主鏈非氫原子數為7以下且含雜原子的亞烷基。 The polysiloxane according to claim 5, wherein the W has a main chain non-hydrogen atom number of 7 or less and a hetero atom-containing alkylene group. 如請求項5之聚矽氧烷，其中，所述T為羥基。 The polysiloxane according to claim 5, wherein T is a hydroxyl group. 如請求項1之聚矽氧烷，其中，m與n的比例為m：n=0：100~50：50。 For example, the polysiloxane of claim 1, wherein the ratio of m to n is m: n = 0: 100 ~ 50: 50. 如請求項8之聚矽氧烷，其中，m與n的比例為m：n=1：99~50：50。 For example, the polysiloxane of claim 8, wherein the ratio of m to n is m: n = 1: 99 ~ 50: 50. 如請求項1之聚矽氧烷，其中，所述聚矽氧烷的重均分子量為500~50000。 The polysiloxane according to claim 1, wherein the polysiloxane has a weight average molecular weight of 500 to 50,000. 如請求項10之聚矽氧烷，其中，所述聚矽氧烷的重均分子量為1000~13000。 The polysiloxane of claim 10, wherein the polysiloxane has a weight average molecular weight of 1,000 to 13,000. 如請求項11之聚矽氧烷，其中，所述聚矽氧烷的重均分子量為1500~6500。 The polysiloxane according to claim 11, wherein the polysiloxane has a weight average molecular weight of 1500 to 6,500. 一種用於太陽能和半導體的摻雜漿料，其特徵在於：含有作為摻 雜劑的請求項1至12中任一項之聚矽氧烷。 A doping paste for solar energy and semiconductor, characterized in that The polysiloxane of any one of Claims 1 to 12 of the hybrid agent. 如請求項13之用於太陽能和半導體的摻雜漿料，其中，還含有增黏劑。 The doping paste for solar energy and semiconductor as claimed in claim 13, further comprising a tackifier. 如請求項13之用於太陽能和半導體的摻雜漿料，其中，還含有溶劑。 The doping paste for solar energy and semiconductor as claimed in claim 13, further comprising a solvent. 如請求項15之用於太陽能和半導體的摻雜漿料，其中，所述溶劑由0~10%的水、以及90~100%有機溶劑組成。 The doping paste for solar energy and semiconductor as claimed in claim 15, wherein the solvent is composed of 0-10% water and 90-100% organic solvent. 如請求項16之用於太陽能和半導體的摻雜漿料，其中，所述溶劑由0~5%的水、以及95~100%有機溶劑組成。 The doping paste for solar energy and semiconductor according to claim 16, wherein the solvent is composed of 0 to 5% water and 95 to 100% organic solvent. 如請求項17之用於太陽能和半導體的摻雜漿料，其中，所述有機溶劑為沸點50~300℃的有機溶劑。 The doping slurry for solar energy and semiconductor according to claim 17, wherein the organic solvent is an organic solvent having a boiling point of 50 to 300 ° C. 如請求項18之用於太陽能和半導體的摻雜漿料，其中，所述聚矽氧烷的總重量為漿料重量的2~35%。 For example, the doped slurry for solar energy and semiconductor of claim 18, wherein the total weight of the polysiloxane is 2 to 35% of the weight of the slurry. 如請求項14之用於太陽能和半導體的摻雜漿料，其中，所述增黏劑為選自甲基纖維素、乙基纖維素、丙基纖維素、羥甲基纖維素、羥乙基纖維素、羥丙基纖維素、羧甲基纖維素、甲基羥乙基纖維素、乙基羥乙基纖維素、甲基羥丙基纖維素、醋酸纖維素、醋酸丁酸纖維素、聚丙烯醯胺、聚乙烯醇、聚乙烯吡咯烷酮、聚氧化乙烯、卡波樹脂、聚丙烯酸、聚丙烯酸酯或聚氨酯中的一種或多種。 The doping paste for solar energy and semiconductor according to claim 14, wherein the thickener is selected from the group consisting of methyl cellulose, ethyl cellulose, propyl cellulose, hydroxymethyl cellulose, and hydroxyethyl Cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, methyl hydroxyethyl cellulose, ethyl hydroxyethyl cellulose, methyl hydroxypropyl cellulose, cellulose acetate, cellulose acetate butyrate, poly One or more of acrylamide, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide, carbomer resin, polyacrylic acid, polyacrylate, or polyurethane. 如請求項14至20中任一項之用於太陽能和半導體的摻雜漿料，其中，所述摻雜劑僅含有請求項1至12中任一項之聚矽氧烷。 The doping paste for solar energy and semiconductor according to any one of claims 14 to 20, wherein the dopant contains only the polysiloxane of any one of claims 1 to 12.
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