TW201725251A - Additive for crystalline silicon acidic polishing liquid and use thereof - Google Patents
Additive for crystalline silicon acidic polishing liquid and use thereof Download PDFInfo
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本發明涉及一種結晶矽酸性拋光液的添加劑及其應用。 The invention relates to an additive for a crystalline bismuth acidic polishing liquid and an application thereof.
在結晶矽太陽能電池的製作工藝中,對矽片進行背面拋光具有以下優勢:1.光學增益,使太陽光中的紅外光反射回去,從而使電池片吸收更多的光,從而使電池片的短路電流提高;2.背場均勻,從而提高電池片的開路電壓;3.背接觸改善,能使矽片背面和鋁漿的接觸改善,達到良好的歐姆接觸;4.顯著的鈍化效果,與背面鈍化結合起來可顯著提高電池片的效率。 In the fabrication process of the crystalline germanium solar cell, the backside polishing of the tantalum sheet has the following advantages: 1. Optical gain, which reflects the infrared light in the sunlight, so that the battery sheet absorbs more light, thereby making the battery sheet The short-circuit current is improved; 2. The back field is uniform, thereby increasing the open circuit voltage of the battery; 3. The back contact is improved, the contact between the back surface of the cymbal and the aluminum paste is improved, and a good ohmic contact is achieved; 4. a significant passivation effect, The combination of back passivation can significantly increase the efficiency of the cell.
目前矽片背面拋光所用的拋光方法主要有如下三種:第一種為無機鹼拋光,雖然成本低,拋光效果也不錯,但是需要對矽片正面做氮化矽掩膜,增加了PECVD鍍膜工序,大大降低了產線的產能。第二種為四甲基氫氧化銨溶液拋光,利用這種方法拋光,可以利用正面磷矽玻璃的保護保證PN結不被破壞,而背面拋光效果比較好,但是在拋光過程中,四甲基氫氧化銨的消耗成本非常高,並且有很強的毒性,對生產操作環境不利。第三種為硝酸、氫氟酸和硫酸拋光,此方法成本較低,同時拋光效果較佳。但是,目前產線所使用的是高濃度的酸來拋光,一方面高濃度的酸霧會 在一定程度上腐蝕正面的PN結,而且有一定概率的矽片會翻邊,因此良率普遍不高;而另一方面,高濃度的酸不僅造成製造成本增加,同時使工廠的廢水處理成本增高,對環境也有一定的影響。 At present, there are mainly three polishing methods used for polishing the back side of the ruthenium. The first one is inorganic alkali polishing. Although the cost is low and the polishing effect is good, it is necessary to make a tantalum nitride mask on the front side of the ruthenium sheet, and increase the PECVD coating process. Greatly reduced the production capacity of the production line. The second is polishing with tetramethylammonium hydroxide solution. Polishing by this method can protect the PN junction from damage by the protection of the front phosphor glass, while the backside polishing effect is better, but in the polishing process, tetramethyl Ammonium hydroxide is very expensive to consume and is highly toxic, which is detrimental to the production operating environment. The third type is polishing with nitric acid, hydrofluoric acid and sulfuric acid, which is less expensive and has a better polishing effect. However, the current production line uses a high concentration of acid to polish, on the one hand, a high concentration of acid mist will Corrosion of the front PN junction to a certain extent, and the plaque with a certain probability will be cuffed, so the yield is generally not high; on the other hand, the high concentration of acid not only causes an increase in manufacturing costs, but also makes the wastewater treatment cost of the plant Increased, has a certain impact on the environment.
因此,如果能開發一種新的酸拋光添加劑,可以直接應用於現有鏈式設備上實現矽片背面拋光,既能改善矽片拋光效果,提升電池效率,又可以降低酸液濃度,減少酸液翻邊,提高電池成品率,這將為降低電池成本做出重要貢獻,這也是電池廠商一直以來期待的結果,對環境保護也有重要的意義。 Therefore, if a new acid polishing additive can be developed, it can be directly applied to the existing chain equipment to achieve the backside polishing of the cymbal, which can improve the polishing effect of the cymbal, improve the efficiency of the battery, and reduce the acid concentration and reduce the acid turnover. On the other hand, increasing the battery yield will make an important contribution to reducing the cost of the battery. This is also the result that battery manufacturers have been expecting for a long time, and it is also important for environmental protection.
本發明的目的在於提供一種結晶矽酸性拋光液的添加劑及其應用,在對矽片進行表面拋光時,將本發明的添加劑加入到酸性溶液中,可達到優異的拋光效果,且可在低酸濃度下實現拋光。 The object of the present invention is to provide an additive for a crystalline bismuth acidic polishing liquid and an application thereof. When the enamel sheet is surface-polished, the additive of the present invention is added to an acidic solution to achieve an excellent polishing effect and can be used in a low acid. Polishing is achieved at a concentration.
為實現上述目的,本發明提供一種結晶矽酸性拋光液的添加劑,由2~5質量份的酒石酸、0.5~2.0質量份的聚乙烯醇、1~3質量份的硫酸鈉和100質量份的水組成。 In order to achieve the above object, the present invention provides an additive for a crystalline cerium acidic polishing liquid, which comprises 2 to 5 parts by mass of tartaric acid, 0.5 to 2.0 parts by mass of polyvinyl alcohol, 1 to 3 parts by mass of sodium sulfate, and 100 parts by mass of water. composition.
優選的,所述的結晶矽酸性拋光液的添加劑,由2~3質量份的酒石酸、0.5~1質量份的聚乙烯醇、1~2質量份的硫酸鈉和100質量份的水組成。 Preferably, the additive of the crystalline cerium acidic polishing liquid is composed of 2 to 3 parts by mass of tartaric acid, 0.5 to 1 part by mass of polyvinyl alcohol, 1 to 2 parts by mass of sodium sulfate, and 100 parts by mass of water.
優選的,所述水為去離子水。 Preferably, the water is deionized water.
本發明還提供一種結晶矽酸性拋光液,通過如下步驟配製:1)將酸組分溶於去離子水中,配製酸性溶液;所述酸組分包括氫氟酸、硝酸;所述酸性溶液中酸組分總的質量百分含量為22~55%;2)將上述的添加劑加入上述步驟1)中的酸性溶液中,得到 結晶矽酸性拋光液;其中,添加劑與酸性溶液的質量比為0.2~5:100。 The invention also provides a crystalline bismuth acidic polishing liquid prepared by the following steps: 1) dissolving an acid component in deionized water to prepare an acidic solution; the acid component comprises hydrofluoric acid, nitric acid; and the acid in the acidic solution The total mass percentage of the component is 22-55%; 2) adding the above additive to the acidic solution in the above step 1), A crystalline bismuth acid polishing solution; wherein the mass ratio of the additive to the acidic solution is 0.2 to 5:100.
優選的,所述酸性溶液中酸組分總的質量百分含量為27.5~45%;所述添加劑與酸性溶液的質量比為1~3:100。 Preferably, the total mass percentage of the acid component in the acidic solution is 27.5 to 45%; and the mass ratio of the additive to the acidic solution is 1 to 3:100.
優選的,所述酸組分中氫氟酸的質量百分含量為10~25%,硝酸的質量百分含量為75~90%。 Preferably, the mass fraction of hydrofluoric acid in the acid component is 10 to 25%, and the mass percentage of nitric acid is 75 to 90%.
優選的,所述酸組分還包括硫酸;所述酸組分中氫氟酸的質量百分含量為2~5%,硝酸的質量百分含量為34~66%,硫酸的質量百分含量為29~64%。 Preferably, the acid component further comprises sulfuric acid; the mass percentage of hydrofluoric acid in the acid component is 2 to 5%, the mass percentage of nitric acid is 34 to 66%, and the mass percentage of sulfuric acid is It is 29~64%.
本發明還提供一種結晶矽拋光方法,將單晶或多晶矽片浸入到上述的拋光液中進行拋光,溫度控制在攝氏6~15度,時間控制在30秒~3分鐘。 The invention also provides a crystallization enamel polishing method, wherein a single crystal or polycrystalline ruthenium sheet is immersed in the above polishing liquid for polishing, the temperature is controlled at 6 to 15 degrees Celsius, and the time is controlled in 30 seconds to 3 minutes.
本發明的優點和有益效果在於:提供一種結晶矽酸性拋光液的添加劑及其應用,在對矽片進行表面拋光時,將本發明的添加劑加入到酸性溶液中,可達到優異的拋光效果,且可在低酸濃度下實現拋光。 An advantage and a beneficial effect of the present invention is to provide an additive for a crystalline bismuth acidic polishing liquid and an application thereof, which can achieve an excellent polishing effect by adding the additive of the present invention to an acidic solution when surface-polishing the ruthenium sheet, and Polishing can be achieved at low acid concentrations.
採用本發明添加劑後,能使拋光反應速度加快,並可在低酸濃度下實現拋光,節約酸用量20~50%。此外,拋光後能獲得均勻平整的絨面,與背鈍化工藝結合可顯著提升電池效率。本發明添加劑應用範圍廣,既能應用於單晶矽片的拋光,亦能應用於多晶矽片的拋光,拋光後矽片的反射率可達30~40%。本發明添加劑與現有濕刻設備相容,拋光克重小,對於156*156mm的矽片,拋光克重約為0.2~0.4克(g),不至於對環境造成汙染。 By using the additive of the invention, the polishing reaction speed can be accelerated, and the polishing can be achieved at a low acid concentration, and the acid consumption is 20-50%. In addition, a uniform flat suede can be obtained after polishing, which, in combination with the back passivation process, can significantly improve cell efficiency. The additive of the invention has wide application range, can be applied to the polishing of the single crystal bismuth sheet, and can also be applied to the polishing of the polycrystalline enamel sheet, and the reflectivity of the enamel sheet after polishing can reach 30-40%. The additive of the invention is compatible with the existing wet engraving equipment, and has a small polishing weight. For a 156*156 mm bract, the polishing weight is about 0.2-0.4 g (g), so as not to pollute the environment.
圖1為本發明實施例1得到的矽片表面拋光面的顯微鏡照片;圖2為本發明實施例1得到的矽片表面拋光面的反射光譜;圖3為本發明實施例2得到的矽片表面拋光面的顯微鏡照片;圖4為本發明實施例2得到的矽片表面拋光面的反射光譜。 1 is a micrograph of a polished surface of a bract sheet obtained in Example 1 of the present invention; FIG. 2 is a reflection spectrum of a polished surface of a bract sheet obtained in Example 1 of the present invention; FIG. 3 is a batt obtained in Example 2 of the present invention; Microscopic photograph of the surface polished surface; Fig. 4 is a reflection spectrum of the polished surface of the bract sheet obtained in Example 2 of the present invention.
以下謹結合附圖和實施例,對本發明的具體實施方式作進一步描述。以下實施例僅用於更加清楚地說明本發明的技術方案,而不能以此來限制本發明的保護範圍。 The specific embodiments of the present invention are further described below in conjunction with the drawings and embodiments. The following examples are only intended to more clearly illustrate the technical solutions of the present invention, and are not intended to limit the scope of the present invention.
本發明具體實施的技術方案是: The technical solution specifically implemented by the present invention is:
實施例1 Example 1
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加劑:以100克(g)去離子水為溶劑,將2克酒石酸、0.5克聚乙烯醇和1克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將50克氫氟酸、400克硝酸等酸組分溶解於去離子水中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入10克添加劑;4)將單晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏10度,拋光時間為2分鐘。 The crystallization crucible is polished by the following steps: 1) preparing an additive for the crystalline citric acid polishing solution: dissolving 2 g of tartaric acid, 0.5 g of polyvinyl alcohol and 1 gram of sodium sulfate in deionized water in 100 g (g) of deionized water as a solvent Adding an additive; 2) preparing an acidic solution: dissolving 50 g of hydrofluoric acid, 400 g of nitric acid and the like in deionized water to obtain 1000 g of an acidic solution; 3) preparing a crystalline bismuth acidic polishing liquid: acidic at 1000 g 10 g of the additive was added to the solution; 4) The single crystal crucible was immersed in a polishing liquid for surface polishing at a polishing temperature of 10 ° C and a polishing time of 2 minutes.
圖1顯示實施例1得到的單晶矽片表面拋光面的顯微鏡照片,從圖1中可以看到矽片表面形成了均勻平滑、平整度高的拋光面結構。圖2顯示實施例1拋光後矽片表面拋光面的反射光譜,從圖2中可以看到,實施例1得到的矽片表面拋光面的反射率較高,在300-1100奈米(nm)波長範圍內的積分反射率高於35%。 Fig. 1 is a photomicrograph showing the surface-polished surface of the single crystal ruthenium sheet obtained in Example 1, and it can be seen from Fig. 1 that a uniform smooth and flat surface structure is formed on the surface of the ruthenium sheet. 2 shows the reflection spectrum of the polished surface of the ruthenium sheet after polishing in Example 1. As can be seen from FIG. 2, the surface polished surface of the ruthenium obtained in Example 1 has a high reflectance at 300-1100 nm (nm). The integrated reflectance in the wavelength range is higher than 35%.
實施例2 Example 2
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加 劑:以100克去離子水為溶劑,將3克酒石酸、1克聚乙烯醇和2克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將27.5克氫氟酸、330克硝酸、192.5克硫酸等酸組分溶解於去離子水中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入50克添加劑;4)將多晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏15度,拋光時間為45秒。 The crystallization enamel is polished by the following steps: 1) Preparation of a crystalline phthalic acid polishing liquid Agent: 100 g of deionized water as solvent, 3 g of tartaric acid, 1 g of polyvinyl alcohol and 2 g of sodium sulfate dissolved in deionized water to prepare an additive; 2) formulating an acidic solution: 27.5 g of hydrofluoric acid, 330 g The acid component such as nitric acid and 192.5 g of sulfuric acid is dissolved in deionized water to obtain 1000 g of an acidic solution; 3) the crystalline cerium acidic polishing liquid is prepared: 50 g of an additive is added to 1000 g of the acidic solution; 4) the polycrystalline crucible is immersed in the polishing liquid. The surface was polished to a polishing temperature of 15 degrees Celsius and a polishing time of 45 seconds.
圖3顯示實施例2得到的多晶矽片表面拋光面的顯微鏡照片,從圖3中可以看到矽片表面形成了均勻平滑、平整度高的拋光面結構。圖4顯示實施例2拋光後矽片表面拋光面的反射光譜,從圖4中可以看到,實施例2得到的矽片表面拋光面的反射率較高,300-1100奈米(nm)波長範圍內的積分反射率高於33%。 Fig. 3 is a photomicrograph showing the surface-polished surface of the polycrystalline silicon wafer obtained in Example 2. From Fig. 3, it can be seen that the surface of the ruthenium sheet has a uniform smooth and flat surface structure. 4 shows the reflection spectrum of the polished surface of the ruthenium sheet after polishing in Example 2. As can be seen from FIG. 4, the polished surface of the ruthenium sheet obtained in Example 2 has a high reflectance of 300-1100 nm (nm) wavelength. The integral reflectance in the range is higher than 33%.
實施例3 Example 3
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加劑:以100克去離子水為溶劑,將5克酒石酸、2克聚乙烯醇和3克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將55克氫氟酸、165克硝酸等酸組分溶解於去離子水中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入30克添加劑;4)將多晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏6度,拋光時間為30秒。 The crystallization enamel is polished by the following steps: 1) preparing an additive for the crystalline phthalic acid polishing solution: 100 g of deionized water as a solvent, 5 g of tartaric acid, 2 g of polyvinyl alcohol and 3 g of sodium sulfate are dissolved in deionized water to prepare Additive; 2) Prepare acidic solution: dissolve 55 grams of hydrofluoric acid, 165 grams of nitric acid and other acid components in deionized water to obtain 1000 grams of acidic solution; 3) prepare crystalline cerium acidic polishing solution: add in 1000 grams of acidic solution 30 g of additive; 4) The polycrystalline silicon flakes were immersed in a polishing liquid for surface polishing at a polishing temperature of 6 ° C and a polishing time of 30 seconds.
實施例4 Example 4
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加劑:以100克去離子水為溶劑,將2.5克酒石酸、0.8克聚乙烯醇和1.5克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將10克氫氟酸、170克硝酸、320克硫酸等酸組分溶解於去 離子水中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入2克添加劑;4)將多晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏10度,拋光時間為3分鐘。 The crystallization enamel is polished by the following steps: 1) preparing an additive for the crystalline phthalic acid polishing solution: using 100 g of deionized water as a solvent, 2.5 g of tartaric acid, 0.8 g of polyvinyl alcohol and 1.5 g of sodium sulfate are dissolved in deionized water to prepare Additive; 2) Prepare an acidic solution: dissolve 10 grams of hydrofluoric acid, 170 grams of nitric acid, 320 grams of sulfuric acid and other acid components In ionic water, 1000 g of acidic solution is obtained; 3) preparing crystalline bismuth acidic polishing liquid: adding 2 g of additive in 1000 g of acidic solution; 4) immersing polycrystalline enamel sheet in polishing liquid for surface polishing, polishing temperature is 10 degrees Celsius, polishing The time is 3 minutes.
實施例5 Example 5
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加劑:以100克去離子水為溶劑,將4克酒石酸、1.5克聚乙烯醇和2.5克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將30克氫氟酸、270克硝酸等酸組分溶解於去離子水中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入20克添加劑;4)將單晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏13度,拋光時間為1分鐘。 The crystallization enamel is polished by the following steps: 1) preparing an additive for the crystalline phthalic acid polishing liquid: 4 g of tartaric acid, 1.5 g of polyvinyl alcohol and 2.5 g of sodium sulfate are dissolved in deionized water using 100 g of deionized water as a solvent. Additive; 2) Prepare acidic solution: dissolve 30 grams of hydrofluoric acid, 270 grams of nitric acid and other acid components in deionized water to obtain 1000 grams of acidic solution; 3) prepare crystalline cerium acidic polishing solution: add in 1000 grams of acidic solution 20 g of additive; 4) The single crystal crucible was immersed in a polishing liquid for surface polishing at a polishing temperature of 13 ° C and a polishing time of 1 minute.
實施例6 Example 6
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加劑:以100克去離子水為溶劑,將3克酒石酸、1克聚乙烯醇和2克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將10克氫氟酸、165克硝酸、75克硫酸等酸組分溶解於去離子水中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入40克添加劑;4)將多晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏15度,拋光時間為45秒。 The crystallization enamel is polished by the following steps: 1) preparing an additive for the crystalline phthalic acid polishing solution: 3 g of tartaric acid, 1 gram of polyvinyl alcohol and 2 g of sodium sulfate are dissolved in deionized water using 100 g of deionized water as a solvent. Additive; 2) Prepare acidic solution: dissolve 10 grams of hydrofluoric acid, 165 grams of nitric acid, 75 grams of sulfuric acid and other acid components in deionized water to obtain 1000 grams of acidic solution; 3) prepare crystalline cerium acidic polishing solution: at 1000 grams 40 g of the additive was added to the acidic solution; 4) the polycrystalline crucible was immersed in a polishing solution for surface polishing at a polishing temperature of 15 ° C and a polishing time of 45 seconds.
實施例7 Example 7
通過如下步驟對結晶矽拋光:1)配製結晶矽酸拋光液的添加劑:以100克去離子水為溶劑,將3克酒石酸、1克聚乙烯醇和2克硫酸鈉溶解於去離子水中,製得添加劑;2)配製酸性溶液:將11克氫氟酸、145.2克硝酸、63.8克硫酸等酸組分溶解於去離子水 中,得到1000克酸性溶液;3)配製結晶矽酸性拋光液:在1000克酸性溶液中加入8克添加劑;4)將單晶矽片浸入拋光液中進行表面拋光,拋光溫度為攝氏10度,拋光時間為1分鐘。 The crystallization enamel is polished by the following steps: 1) preparing an additive for the crystalline phthalic acid polishing solution: 3 g of tartaric acid, 1 gram of polyvinyl alcohol and 2 g of sodium sulfate are dissolved in deionized water using 100 g of deionized water as a solvent. Additive; 2) Prepare acidic solution: dissolve 11 grams of hydrofluoric acid, 145.2 grams of nitric acid, 63.8 grams of sulfuric acid and other acid components in deionized water In the process, 1000 g of acidic solution is obtained; 3) preparing a crystalline bismuth acidic polishing liquid: adding 8 g of an additive to 1000 g of an acidic solution; 4) immersing the single crystal slab into a polishing liquid for surface polishing at a polishing temperature of 10 degrees Celsius. The polishing time is 1 minute.
惟以上所述之具體實施例,僅係用於例釋本發明之特點及功效,而非用於限定本發明之可實施範疇,於未脫離本發明上揭之精神與技術範疇下,任何運用本發明所揭示內容而完成之等效改變及修飾,均仍應為下述之申請專利範圍所涵蓋。 However, the specific embodiments described above are merely used to exemplify the features and functions of the present invention, and are not intended to limit the scope of the present invention, and may be applied without departing from the spirit and scope of the present invention. Equivalent changes and modifications made to the disclosure of the present invention are still covered by the scope of the following claims.
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