TW202122509A - 基於銀奈米粒子的油墨 - Google Patents
基於銀奈米粒子的油墨 Download PDFInfo
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- 235000011001 calcium citrates Nutrition 0.000 description 1
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 description 1
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- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 description 1
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- 239000000574 octyl gallate Substances 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 229940111695 potassium tartrate Drugs 0.000 description 1
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- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
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- 238000010008 shearing Methods 0.000 description 1
- 239000010420 shell particle Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052990 silicon hydride Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
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- 229940019931 silver phosphate Drugs 0.000 description 1
- 229910000161 silver phosphate Inorganic materials 0.000 description 1
- PGGQSYHSNJQLOQ-UHFFFAOYSA-K silver trifluoride Chemical compound F[Ag](F)F PGGQSYHSNJQLOQ-UHFFFAOYSA-K 0.000 description 1
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- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
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- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- 235000013337 tricalcium citrate Nutrition 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- QUEDXNHFTDJVIY-UHFFFAOYSA-N γ-tocopherol Chemical class OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-UHFFFAOYSA-N 0.000 description 1
- QUEDXNHFTDJVIY-DQCZWYHMSA-N γ-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-DQCZWYHMSA-N 0.000 description 1
Classifications
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H01L31/02—Details
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- H01L31/06—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by potential barriers
- H01L31/072—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by potential barriers the potential barriers being only of the PN heterojunction type
- H01L31/0745—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by potential barriers the potential barriers being only of the PN heterojunction type comprising a AIVBIV heterojunction, e.g. Si/Ge, SiGe/Si or Si/SiC solar cells
- H01L31/0747—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by potential barriers the potential barriers being only of the PN heterojunction type comprising a AIVBIV heterojunction, e.g. Si/Ge, SiGe/Si or Si/SiC solar cells comprising a heterojunction of crystalline and amorphous materials, e.g. heterojunction with intrinsic thin layer
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Abstract
本發明之目的在於基於銀奈米粒子及金屬氧化物的油墨配方。具體地,本發明係有關於基於銀奈米粒子及金屬氧化物的油墨配方,上述之油墨是穩定的,具有改善的導電性,並且可有利地形成電極及/或導電跡線,特別適用於例如矽及/或玻璃基材上的光伏電池。
Description
本發明之目的在於基於銀奈米粒子及金屬氧化物的油墨配方。具體地,本發明係有關於基於銀奈米粒子及金屬氧化物的油墨配方,上述之油墨是穩定的,具有改善的導電性,並且可有利地形成電極及/或導電跡線,特別適用於例如玻璃及/或矽基材上的光伏電池。
眾所周知,可使用導電漿料在諸如矽等基材表面上形成金屬接點。此類基材可在將太陽能轉換成電能的光伏電池(或太陽能電池)中使用。晶體矽太陽能電池可塗覆有減反射塗層,以促進光的吸收,此點在理論上提高了電池效率,但同時又因為此種減反射塗層亦為絕緣體而產生另一個問題;因此通常在施加導電漿料前將此種減反射塗層塗覆到太陽能電池上。可使用各種類型的減反射塗層,但是原則上它們皆包含氮化矽及/或氧化鈦及/或氧化矽。
因此為了形成金屬接點,將導電跡線印刷到基材上,然後將其在高溫下焙燒,但是要低於銀的熔點以及銀及矽的共晶點。若在施加導電跡線前用減反射塗層覆蓋太陽能電池,則該導電跡線應該有效地穿透減反射塗層,從而與基材形成必要的金屬接點。然而,加熱時必須防止導電跡線及/或減反射塗層中的某些成分過度地污染基材,因為此舉會使太陽能電池的性能下降。
為了能夠獲得良好的太陽能電池效率,對於所有此等關鍵問題的適當把控是至關重要的。
因此,亟需一種易於印刷的組合物,其可形成導電跡線,此等導電跡線與太陽能電池的基材形成必要的歐姆接觸,而不會降低其性能,同時在必要情況下亦考慮到了減反射層的存在。
更具體地,本發明係有關於適用於絲網印刷及/或塗層(“coating”)的基於導電奈米粒子的油墨領域。
根據本發明的基於導電奈米粒子的油墨可被印刷在所有類型的載體上。作為示例可列舉以下載體:聚合物及聚合物衍生物、複合材料、有機材料、無機材料,具體地包括下文所定義及描述的矽、玻璃及/或減反射中間層。
根據本發明的基於導電性奈米粒子的油墨具有諸多優點,其中作為非限制性示例可列舉如下:
- 退火更好(沉積物均勻性);
- 印刷過程中不產生氣泡/泡沫;
- 停留時間更長(例如油墨不會在模版上乾化);
- 與現有油墨相比,隨時間推移的穩定性更高;
- 溶劑及奈米粒子無毒;
- 保留了奈米粒子的固有特性;特別是
- 在通常為150℃至300℃之間的退火溫度下,導電性得到改善。
本發明亦有關於一種上述之油墨的改良製備方法;最後,本發明亦有關於上述之油墨在絲網印刷及/或塗層(“coating”)領域中的用途。
根據近年來的文獻,導電膠體奈米晶體由於其新的光電、光伏及催化特性而受到了廣泛的關注。此點使得它們在奈米電子、太陽能電池、傳感器及生物醫學領域的未來應用中變得特別有意義。
導電奈米粒子的發展可訴諸於新的實現方式並且可預見到大量的新應用。奈米粒子具有非常高的表面積/體積比,並且因其表面被表面活性劑取代而具有某些特性,特別是光學特性以及可分散性。
它們的小尺寸在某些情況下可能產生量子約束效應。當粒子的至少一個尺寸小於或等於250 nm時,可使用奈米粒子此一術語。若無預先規定的形狀,奈米粒子可呈丸狀(1至250 nm))、棒狀(長度L <200至300 nm)、細線狀(幾百奈米甚至幾微米)、碟形、星形、金字塔形、四足形、塊狀或晶體的形式。
為了合成導電奈米粒子,已經開發了幾種方法。其中可非詳盡地列舉如下:
- 物理方法:
• 當基材曝露於表面發生反應或分解的揮發化學前體時,產生化學氣相沉積(亦稱“Chemical Vapor Deposition - CVD”)。該方法通常促使奈米粒子形成,其形態取決於所採用的條件;
• 熱蒸發;
• 將要構成奈米粒子的原子以氣流的形式在基材(原子被固定在此處)上受到高速轟擊時,分子束外延(亦稱“Molecular Beam Epitaxy”)
- 化學或物理方法:
• 微乳化;
• 當含有前體的溶液受到雷射束照射時,溶液中產生雷射脈衝。在溶液中沿著光束形成奈米粒子;
• 微波輻射合成;
• 表面活性劑輔助的定向合成;
• 超聲波合成;
• 電化學合成;
• 有機金屬合成;
• 在醇環境中合成。
物理合成消耗更多的原料且損耗較大。它們通常需要一定時間及高溫,使得它們在工業規模生產轉化上缺乏吸引力。此點使得它們不適用於某些基材,例如撓性基材。另外,合成係在小尺寸框架中的基材上直接完成。此等生產方法被證明是相對剛性的,並且無法在大尺寸基材上進行生產;然而,它們能夠完全適用於生產根據本發明的油墨配方中的銀奈米粒子。
化學合成具有諸多優點。首先係在溶液中進行操作,由此獲得的導電奈米粒子已經分散在溶劑中,從而有利於保存及使用。在大多數情況下,奈米粒子在合成結束時不會固定在基材上,令它們的使用具有更大的自由度。此點為使用不同尺寸及不同性質的基材開闢了道路。此等方法亦可更好地控制所涉及的原材料並限制其損耗。透過合成參數的正確調整,實現了對導電奈米粒子的合成及生長動力的良好控制。如此便能確保批次之間良好的可再現性,以及對奈米粒子最終形態的良好控制。透過化學途徑快速且大量地生產奈米粒子的能力,確保了產品具有一定的柔韌性,此種能力可實現工業規模生產。分散的導電奈米粒子的獲得為其定製化開闢了廣闊前景。因此,可根據預期應用來調節存在於奈米粒子表面上的穩定劑的性質。實際上,存在不同的濕法沉積方法。每種情況下,應該特別注意油墨的物理特性,例如表面張力或黏度。在基於奈米粒子的油墨配方中使用的助劑將有助於滿足沉積方法的要求。但是表面配體亦會影響此等參數,並且它們的選擇被證實是決定性的。因此,重要的是要對油墨有一個總體瞭解,以便將所有成分(奈米粒子、溶劑、配體及添加劑)結合在一起,並獲得與目標應用相容的產品。
油墨
本發明之目的在於,透過提供此種適用於絲網印刷及/或塗層(“coating”)領域的油墨,克服現有技術中的一種或多種缺陷,上述之油墨包含:
1、重量含量至少為30%,較佳重量含量至少為40%的銀奈米粒子,
較佳地,重量含量小於75%的銀奈米粒子,
2、重量含量至少為0.1%,較佳重量含量至少為0.2%的金屬氧化物,
較佳地,重量含量小於5%,甚至小於2%的金屬氧化物,
金屬氧化物選自粒度小於微米級的玻璃料,並且其組分中包含重量含量大於50%的氧化矽,
3、重量含量至少為10%,較佳重量含量至少為15%的沸點高於150℃的一元醇,
較佳地,重量含量小於50%,甚至小於40%的該醇,
4、重量含量至少為2%,較佳重量含量至少為4%的多元醇及/或多元醇醚,
較佳地,重量含量小於20%,甚至小於15%的多元醇及/或多元醇醚,
5、可選地,以下化合物中的一個或多個:
a. 作為流變改性劑的纖維素化合物,
b. 銀及/或銅及/或鎳金屬微粒,及/或
c. 分散劑,
此等可選化合物的總和占油墨重量小於30%,
上述之油墨的特徵為上述化合物的總和占油墨重量的至少90%,較佳地占油墨重量的至少95%,例如油墨重量的至少99%。
•
銀奈米粒子
根據本發明的一種實施方式,請求保護之油墨中的銀奈米粒子的粒度在1至250 nm之間,較佳地在10至250 nm之間,更較佳地在30至150 nm之間。
本發明中提及的銀奈米粒子的粒度分佈可透過任何合適的方法來測量。例如,可有利地根據以下方法進行測量:使用馬爾文公司的Nanosizer S型設備,其具有以下特徵:
DLS(動態光散射)測量方法:
- 容器類型:光學玻璃T
- 材料:銀
- 奈米粒子的折射率:0.54
- 吸光度:0.001
- 分散劑:環辛烷
- 溫度:20℃
- 黏度:2.133
- 分散劑的折射率:1.458
- 一般選項:馬克-霍溫克參數
- 分析模型:通用用途
- 平衡:120 s
- 測量次數:4
D50係指數量50%的較小銀奈米粒子的直徑。該值被視為代表粒子的平均粒度。
根據本發明的一種實施改型,銀奈米粒子為類球形及/或球形。在本發明以及下文中的請求項中,術語“類球形”係指形狀類似球形,但並非完美的圓形(“準球形”),例如橢球形。奈米粒子的形狀及粒度可有利地透過顯微鏡拍攝的照片來識別,特別是透過符合下述說明的透射電子顯微鏡(TEM)型設備。採用Thermofisher Scientific公司的透射電子顯微鏡(TEM)型設備進行測量,其具有以下特徵:
TEM-BF(Bright Field–明視野)圖像係在300 kV下拍攝,
採用了用於低倍放大的50 µm的物鏡,沒有高解析率物鏡,
使用Digital Micrograph軟體在TEM圖像上進行尺寸測量,
對代表大多數粒子的一定數量的粒子求平均值,例如20個粒子,如此便能確定奈米粒子的平均表面積、平均周長及/或平均直徑。
因此,根據本發明的此一實施改型,奈米粒子係類球形,並且透過該TEM鑑別,其特徵較佳地在於奈米粒子的平均表面積在1至20 nm2
之間,較佳地在5至15 nm2
之間,及/或在於奈米粒子的平均周長在3至20 nm之間,較佳地在5至15 nm之間,及/或奈米粒子的平均直徑在0.5至7 nm之間,較佳地在1至5 nm之間。
根據本發明一種實施改型,若無預先規定的形狀,則銀奈米粒子為丸狀、棒狀(長度L <200至300 nm)、細線狀(長度為幾百奈米甚至幾微米)、塊狀、片狀或晶體的形式。
根據本發明的一種具體實施方式,透過物理合成或化學合成預先合成了銀奈米粒子。在本發明的範圍內,可採用任何物理或化學合成。在根據本發明的一種具體實施方式中,利用有機或無機銀鹽作為銀前體,透過化學合成獲得銀奈米粒子。作為非限制性示例,可列舉乙酸銀、硝酸銀、碳酸銀、磷酸銀、三氟化銀、氯化銀、高氯酸鉀中的一種或它們的混合物。根據本發明的一種改型,前體為硝酸銀及/或乙酸銀。
根據本發明的一種具體實施方式,銀奈米粒子的合成採用化學合成,存在分散劑時利用還原劑對銀前體進行還原;此種還原可在不存在或存在溶劑的情況下進行。
因此,根據本發明使用的奈米粒子的特徵為無論採用哪種合成方式(物理或化學),其D50的值較佳地在1至250 nm之間;它們的特徵亦較佳地在於單分散(均勻)而沒有聚集體。對於球形銀奈米粒子,亦可有利地採用30至150 nm之間D50值。
本發明中提及的銀奈米粒子的含量可透過任何合適的方法來測量。例如,可有利地根據以下方法進行測量:
- 熱解重量分析
- 設備:TA Instrument公司的TGA Q50設備
- 坩堝:氧化鋁
-方法:斜面法
- 測量範圍:自環境溫度到600℃
- 升溫速度:10℃/min。
•
金屬氧化物
因此,根據本發明的油墨包含金屬氧化物,該等金屬氧化物選自尺寸小於微米級的玻璃料,並且成分中氧化矽的重量含量大於50%。
在一種實施方式中,根據本發明的導電油墨中使用的玻璃料包含重量含量大於50%的SiO2
,例如重量含量大於75%的SiO2
。
玻璃料中亦可有其他金屬氧化物,其中作為示例可列舉氧化鉍、氧化鋁、氧化鋅及氧化硼;可有利於用於本發明範圍的玻璃料組合物示例中包含SiO2
、Bi2
O3
、Al2
O3
、ZnO的混合物,該混合物在玻璃料組合物中的重量含量至少為75%,較佳重量含量至少為90%,例如重量含量為99%。
根據本發明的玻璃料組合物亦可容許包含其他組分,例如Bi2
O3
、ZnO、Al2
O3
、Ag2
O、Sb2
O3
、GeO2
、In2
O3
、P2
O5
、V2
O5
、Nb2
O5
、Ta2
O5
;及/或鹼金屬氧化物及/或鹼土金屬氧化物,例如分別是Na2
O、Li2
O 及/或K2
O及BaO、CaO、MgO及/或SrO。
根據本發明的一個具體實施方式在於,玻璃料組合物不包含有意添加的鉛或硼;在此種實施方式中,術語“不含有意添加的鉛及/或硼”係指鉛含量小於約1000 ppm及/或硼含量小於約1000 ppm的玻璃料。
本發明中提及的玻璃料的含量可透過任何合適的方法來測量。例如,與銀奈米粒子採用相同的方法。根據一種實施方式,油墨中玻璃料的總含量為油墨重量的0.1%至5%之間,較佳地為油墨重量的0.2%至2%之間。
本發明中提及的玻璃料及金屬氧化物的粒度可透過任何合適的方法來測量。例如,與銀奈米粒子採用相同的方法。根據本發明的一種具體實施方式,玻璃料以及金屬氧化物的粒度將有利地在5至250 nm之間。對於類球形銀奈米粒子,可有利地採用5至50 nm之間D50值。作為示例可列舉採用比表面積在150至250 m2
/g(BET)之間的二氧化矽。玻璃料的平均表面積(根據上述TEM測量)在1至20 nm2
之間,較佳地在5至15 nm2
之間,及/或平均周長在3至20 nm之間,較佳地在5至15 nm之間,及/或平均直徑在0.5至7 nm之間,較佳地在1至5 nm之間,因此有利地能夠在本發明的範圍內使用。
•
沸點高於150℃
的一元醇
因此,根據本發明的油墨包含沸點高於150℃的一元醇;例如2,6-二甲基-4-庚醇及/或萜烯醇。根據本發明的油墨較佳地包含萜烯醇,選自薄荷醇、神經醇、桉樹腦、熏衣草醇、肉豆蔻醇、萜品醇(α-、β-、γ-萜品醇及/或4-萜品醇;較佳地α-萜品醇)、異冰片醇、香茅醇、芳樟醇、冰片醇、香葉醇及/或兩種或更多種上述之醇的混合物。
•
多元醇及/或多元醇醚
因此,根據本發明的油墨包含多元醇及/或多元醇醚。多元醇及/或多元醇醚的特徵較佳地在於沸點低於260℃。可列舉二醇(例如乙二醇、丙二醇、二甘醇、三亞甲基二醇、1,3-丁二醇、1,2-丁二醇、2,3-丁二醇、五亞甲基二醇、己烯乙二醇等),及/或乙二醇醚(例如乙二醇單醚或乙二醇二醚,作為示例可列舉乙二醇單丙醚、乙二醇單丁醚、乙二醇單苯醚、丙烯乙二醇單苯醚、二乙二醇甲醚、二乙二醇乙醚、二乙二醇丙醚、二乙二醇丁醚(丁基卡必醇)、丙二醇單甲醚、丙二醇單丁醚、丙二醇單丙醚、乙二醇二甲醚、乙二醇二乙醚、乙二醇二丁醚、甘醇、二乙二醇二乙醚、二丁二醇二乙醚、二甘醇、二甘醇二乙醚、二甘醇二丁醚)及/或二醇醚乙酸酯(例如2-丁氧基乙酸酯、乙二醇乙醚乙酸酯、乙二醇丁醚乙酸酯、丙二醇甲醚乙酸酯)及/或兩種或多種上述之化合物的混合物。
•
作為流變改性劑的可選纖維素化合物
因此,根據本發明的油墨可選地包含流變改性劑,有利地選自纖維素化合物。作為示例可列舉烷基纖維素、羥烷基纖維素及羧烷基纖維素,較佳地乙基纖維素。
根據本發明的一種實施方式,請求保護之油墨包含纖維素化合物,其重量含量高於0.5%,例如重量含量高於1%;然而應該較佳地將其在油墨中的重量含量維持在5%以下,甚至2%以下。
•
銀、銅及/或鎳金屬微粒
因此,根據本發明的油墨可選地包含銀、銅及/或鎳金屬微粒。此等微粒可呈球形、絮片狀及/或細絲狀,並且較佳地粒度小於15 μm,例如小於10 μm,較佳地小於5 μm。微粒的平均表面積(根據上述TEM測量)在1至25 µm2
之間,較佳地在5至15 µm2
之間,及/或平均周長在3至20 µm之間,較佳地在5至15 µm之間,及/或平均直徑在1至7 µm之間,較佳地在1至5μm之間,因此有利地能夠在本發明的範圍內使用。
作為示例,金屬微粒可由銀、或銅-銀混合物或鎳-銀混合物構成。具體地,此等微粒可具有銅芯及銀殼,或者鎳芯及銀殼。若為芯/殼粒子,則構成芯體的金屬應占微粒總構成重量的85-95%。
根據本發明的一種實施方式,請求保護之油墨中的此等微粒的重量含量高於5%,例如重量含量高於10%;然而應該較佳地將其在油墨中的含量維持在25%以下,甚至20%以下。
•
分散劑
因此,根據本發明的油墨可選地包含銀分散劑,例如有機分散劑,其較佳地包含至少一個碳原子。此等有機分散劑亦可包含一種或多種非金屬雜原子,例如鹵素化合物、氮、氧、硫、矽。作為示例可列舉硫醇及其衍生物,胺及其衍生物(例如氨基醇及氨基醇醚),羧酸及其羧酸酯衍生物及/或它們的混合物。
根據本發明的一種實施方式,請求保護之油墨包含的此等分散劑的重量含量高於0.1%,例如重量含量高於0.5%;然而應該較佳地將其在油墨中的重量含量維持在3%以下,甚至2%以下。
•
其他化合物
儘管此舉並非根據本發明的較佳實施方式,但是請求保護之油墨亦允許在其配方中存在其他化合物。但是,較佳地,將其在油墨中的重量含量限制在10%以下,例如在油墨中的重量含量小於5%,在油墨中的重量含量小於1%。作為示例可列舉水、一元醇及/或抗氧化劑。一元醇較佳地選自具有直鏈或支鏈脂族基團的醇,例如具有1至10個碳原子的醇。作為示例可列舉甲醇、乙醇、丁醇、庚醇、二甲基庚醇、2,6-二甲基-4-庚醇及/或兩種或更多種上述之醇的混合物。作為抗氧化劑的示例,可列舉:
- 抗壞血酸或維生素C(E300)、抗壞血酸鈉(E301)、抗壞血酸鈣(E302)、5-6-1-二乙醯抗壞血酸(E303)、6-1-棕櫚基抗壞血酸(E304);
- 枸櫞酸(E330)、枸櫞酸鈉(E331)、枸櫞酸鉀(E332)、枸櫞酸鈣(E333);
- 酒石酸(E334)、酒石酸鈉(E335)、酒石酸鉀(E336)、酒石酸鈉鉀(E337);
- 丁基羥基茴香醚(E320)及丁基羥基甲苯(E321);
- 辛基(E311)沒食子酸酯或十二烷基(E312)沒食子酸酯;
- 乳酸鈉(E325)、乳酸鉀(E326)或乳酸鈣(E327);
- 卵磷脂(E322);
- 天然生育酚(E306)、合成α-生育酚(E307)、合成γ-生育酚(E308)、合成δ-生育酚(E309),所有構成維生素E的生育酚;
- 丁香酚、百里酚及/或肉桂醛,
- 以及兩種或更多種上述之抗氧化劑的混合物。
根據本發明,20℃時,在40 s-1
的剪切速率下測得的油墨黏度通常在1000至100000 mPa.s之間,較佳地在5000至50000 mPa.s之間,例如在10000至40000 mPa.s之間。
黏度可透過任何合適的方法來測量。例如,可有利地根據以下方法進行測量:
-設備:TA Instrument公司的AR-G2流量計
- 處理時間:100 s-1
下預剪切3分鐘/平衡1分鐘
- 試驗類型:剪切等級
- 等級:40 s-1
、100 s-1
、1000 s-1
- 每級持續時間:5分鐘
- 模式:線性
- 測量:每10秒鐘
- 溫度:20℃
- 曲線處理方法:牛頓法
- 處理區域:整個曲線
根據本發明的一種實施方式,該油墨亦可在其組合物中添加其他化合物,其中可列舉添加劑(例如矽烷類添加劑),其目的在於改善對各類機械應力的抵抗力,例如對於諸多基材的附著性。
基材
根據本發明的基於導電奈米粒子的油墨可被印刷在所有類型的載體上。作為示例可列舉以下載體:聚合物及聚合物衍生物、複合材料、有機材料、無機材料,具體地是下文所定義及描述的矽、玻璃、ITO玻璃、AZO玻璃、SiN玻璃及/或減反射中間層。
基材可有利地用於太陽能電池或光伏電池中,當日光中的光子從價帶到導帶激發半導體上的電子時,太陽能電池或光伏電池將太陽能轉換為電能。流向導帶的電子被金屬接點收集。
舉例來說,光伏電池由具有不同功能的層堆疊組成:由電子供體及受體材料組成的有源層、正負電極以及附加層(減反射、更高摻雜等),它們可提高電池的性能。在此種傳統的光伏電池中,有源層由單晶或多晶矽組成,其上面沉積有基於氮化矽SiN或氫化氮化矽SiNx:H的減反射層。至於電極,它們通常由背面的鋁及正面的銀構成。
此類電池的製造步驟如下:透過化學蝕刻使矽層紋理化,然後形成供體/受體結(磷擴散,然後進行等離子蝕刻以打開該結並消除短路)。然後,透過PECVD沉積使減反射層的沉積到位。最後,電池的金屬化在於,透過絲網印刷在背面的鋁實心層及正面的銀柵格上形成沉積。接點退火通常係透過烤箱,特別是透過在700-800℃的極高溫下進行的“焙燒”步驟來完成。
近年來,出現了一種新型的混合電池:異質結太陽能電池。此等電池在許多方面與上述傳統電池不同。首先,有源層由多層帶有各種摻雜體的晶體矽及非晶矽層組成。另外,正面及背面都有兩層ITO。金屬化亦有所不同,此點因為金屬化在於透過絲網印刷在正面及背面的銀柵格上形成沉積。最後,就製造方法而言,有必要說明的是,此等電池未經過上一段中描述的焙燒步驟(“firing”),而是經過了不超過250℃的熱處理,因而本案所請求保護之油墨是完美的。
根據本發明的一種實施改型,根據本發明的基於奈米粒子的油墨的製備,特徵為以下步驟:
S1=在機械攪拌及加熱條件下,使乙基纖維素分散到萜品醇中;
S2=在機械攪拌及室溫條件下,使奈米級玻璃料分散到S1中;
S3=在機械攪拌及室溫條件下,使可選微粒(銀及/或銅及/或鎳粉)分散到S2中;
S4=在機械攪拌及室溫條件下,向S2或S3中添加存在於丁基卡必醇中的銀奈米粒子。
由此獲得的油墨可直接使用或經充分稀釋以得到所需的特性。
根據一種或多種實施方式,該導電油墨透過絲網印刷或塗層(“coating”)被印刷到基材表面上或減反射中間層(其自身黏附至基材)上。有利地,將組件加熱到低於250℃的溫度以形成導電跡線。在一種實施方式中,如本申請中前面所討論的,熱處理使得玻璃料熔化並穿透減反射中間層,從而與基材形成接觸。在一種或多種實施方式中,導電物質在導體與基材的界面處形成微晶形,從而改善導體與半導體基材之間的電接觸或歐姆接觸。
因此,本發明亦有關於請求保護之油墨用於絲網印刷及/或塗層(“coating”)以便在製造異質結太陽能電池過程中形成導電跡線的用途;油墨的此種用途,其特徵亦有利地在於,導電跡線的形成包括在低於250℃的溫度下進行熱處理。
因此,對於本領域技術人員而言顯而易見的是,在不脫離請求保護之本發明的應用範圍的情況下,本發明允許採用許多其他特定形式的實施方式。因此,所示實施方式應該被視作示例,但是可在所附申請專利範圍的範圍所限定的領域內對本實施例進行修改。
現在將透過下面列出的配方來說明本發明及其優點。根據說明書上文中描述的較佳實施方式製備油墨配方。
根據本發明製備了油墨配方,該油墨配方包含:
- 重量含量為55%的銀奈米粒子,其D50值為130 nm,
- 重量含量為20%的絮片狀銀微粒,其D50值為2.3 µm,
- 重量含量為5%的丁基卡必醇,
- 重量含量為17.6%的萜品醇,
- 重量含量為1.4%的乙基纖維素,
- 重量含量為1%的SiO2
,其初級D50值為12 nm。
此種配方在40 s-1
的剪切速率下測得的黏度為30 000 mPa.s。在150℃下加熱10min,然後在200℃下加熱30min,透過塗層(濕厚度為24μm)使此種油墨沉積在塗覆ITO的矽板上,可獲得6 mOhm/sq的方電阻及出色的附著性(根據ASTM D3359為5B)。
現在將透過下面列出的配方來說明本發明及其優點。根據說明書上文中描述的較佳實施方式製備油墨配方。
根據本發明製備了油墨配方,該油墨配方包含:
- 重量含量為55%的銀奈米粒子,其D50值為130 nm,
- 重量含量為20%的絮片狀銀微粒,其D50值為2.3 µm,
- 重量含量為5%的丁基卡必醇,
- 重量含量為17.6%的萜品醇,
- 重量含量為1.4%的乙基纖維素,
- 重量含量為1%的SiO2
,其初級D50值為12 nm。
此種配方在40 s-1
的剪切速率下測得的黏度為30 000 mPa.s。在150℃下加熱10min,然後在200℃下加熱30min,透過塗層(濕厚度為24μm)使此種油墨沉積在塗覆ITO的矽板上,可獲得6 mOhm/sq的方電阻及出色的附著性(根據ASTM D3359為5B)。
Claims (13)
- 一種油墨,其中該油墨包含總和占該油墨的重量至少90%的以下多個化合物: (1)銀奈米粒子,其重量含量至少為30%; (2)金屬氧化物,其重量含量至少為0.1%,該金屬氧化物選自粒度小於微米級的玻璃料,並且該玻璃料的組分中包含重量含量大於50%的氧化矽; (3)沸點高於150℃的一元醇,其重量含量至少為10%; (4)多元醇及/或多元醇醚,其重量含量至少為2%;及 (5)可選的化合物,為以下化合物中的一個或多個: (a)作為流變改性劑的纖維素化合物; (b)銀及/或銅及/或鎳金屬微粒;及/或 (c)分散劑, 其中該等可選的化合物的總和占該油墨重量的30%以下。
- 如請求項1之油墨,其中該油墨包含: (1)該銀奈米粒子的重量含量至少為40%; (2)該金屬氧化物的重量含量至少為0.2%; (3)該沸點高於150℃的一元醇的重量含量至少為15%;及 (4)該多元醇及/或多元醇醚的重量含量至少為4%。
- 如前述請求項任一項之油墨,其中該油墨包含: (1)該銀奈米粒子的重量含量小於75%; (2)該金屬氧化物的重量含量小於5%; (3)該沸點高於150℃的一元醇的重量含量小於50%;及 (4)該多元醇及/或多元醇醚的重量含量小於20%。
- 如請求項3之油墨,其中該油墨包含: (2)該金屬氧化物的重量含量小於2%; (3)該沸點高於150℃的一元醇的重量含量小於40%;及 (4)該多元醇及/或多元醇醚的重量含量小於15%。
- 如前述請求項任一項之油墨,其中該油墨中的該等銀及/或銅及/或鎳金屬微粒的含量大於該油墨重量的5%且小於該油墨重量的25%,例如大於該油墨重量的10%且小於該油墨重量的20%。
- 如前述請求項任一項之油墨,其中該油墨中的該纖維素化合物的含量大於該油墨重量的0.5%且小於該油墨重量的5%,例如大於該油墨重量的1%且小於該油墨重量的2%。
- 如前述請求項任一項之油墨,其中該油墨中的該分散劑的含量大於該油墨重量的0.1%且小於該油墨重量的3%,例如大於該油墨重量的0.5%且小於該油墨重量的2%。
- 如前述請求項任一項之油墨,其中該油墨中的該沸點高於150℃的一元醇為2,6-二甲基-4-庚醇及/或萜烯醇。
- 如請求項8之油墨,其中該油墨中的該萜烯醇為萜品醇。
- 如前述請求項任一項之油墨,其中該油墨中的該多個化合物的總和至少為該油墨重量的95%,例如至少為該油墨重量的99%。
- 如前述請求項任一項之油墨,其中該油墨在20℃時,在40 s-1 的剪切速率下測得的油墨黏度在1000至100000 mPa.s之間,較佳地在5000至50000 mPa.s之間,例如在10000至40000 mPa.s之間。
- 一種將如前述請求項任一項之油墨用於絲網印刷及/或塗層以在製造異質結太陽能電池過程中形成導電跡線的用途。
- 如前一請求項之油墨的用途,其中該導電跡線的形成包括在低於250℃的溫度下進行熱處理。
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DE112007001507T5 (de) * | 2006-06-30 | 2009-07-30 | Mitsubishi Materials Corp. | Zusammensetzung für die Herstellung einer Elektrode einer Solarzelle, Verfahren zur Herstellung der Elektrode und Solarzelle, welche die durch dieses Verfahren erhältliche Elektrode umfasst |
ES2438745T3 (es) * | 2009-09-04 | 2014-01-20 | Basf Se | Composición para la impresión de circuitos impresos así como un procedimiento para la fabricación de células solares |
WO2011026852A1 (de) * | 2009-09-04 | 2011-03-10 | Basf Se | Zusammensetzung zum drucken von elektroden |
KR101795112B1 (ko) * | 2010-10-28 | 2017-11-07 | 헤레우스 프레셔스 메탈즈 노스 아메리카 콘쇼호켄 엘엘씨 | 금속 첨가제를 함유하는 태양 전지 금속화 |
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KR20140098922A (ko) * | 2013-01-31 | 2014-08-11 | 엘에스전선 주식회사 | 전도성 잉크 조성물 및 이로부터 전극을 형성하는 방법 |
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WO2021115750A1 (fr) | 2021-06-17 |
KR20230009353A (ko) | 2023-01-17 |
US20220389257A1 (en) | 2022-12-08 |
CN114846093A (zh) | 2022-08-02 |
EP4073182A1 (fr) | 2022-10-19 |
IL293709A (en) | 2022-08-01 |
FR3104600B1 (fr) | 2022-04-22 |
FR3104600A1 (fr) | 2021-06-18 |
JP2023505495A (ja) | 2023-02-09 |
CA3160175A1 (fr) | 2021-06-17 |
BR112022011173A2 (pt) | 2022-08-23 |
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