TWI793798B - 附導電性圖案之構造體的製造方法及導電性圖案構造體的製造套組 - Google Patents
附導電性圖案之構造體的製造方法及導電性圖案構造體的製造套組 Download PDFInfo
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- TWI793798B TWI793798B TW110138011A TW110138011A TWI793798B TW I793798 B TWI793798 B TW I793798B TW 110138011 A TW110138011 A TW 110138011A TW 110138011 A TW110138011 A TW 110138011A TW I793798 B TWI793798 B TW I793798B
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- Prior art keywords
- conductive pattern
- manufacturing
- plating
- copper
- pattern according
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- 238000000034 method Methods 0.000 title claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 66
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 157
- 238000007747 plating Methods 0.000 claims abstract description 148
- 239000005751 Copper oxide Substances 0.000 claims abstract description 142
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 142
- 239000006185 dispersion Substances 0.000 claims abstract description 105
- 238000000576 coating method Methods 0.000 claims abstract description 61
- 239000011248 coating agent Substances 0.000 claims abstract description 57
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- 239000000758 substrate Substances 0.000 claims abstract description 41
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000007772 electroless plating Methods 0.000 claims abstract description 25
- 238000007639 printing Methods 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims description 112
- -1 glycine compound Chemical class 0.000 claims description 97
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine group Chemical group NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 96
- 239000010949 copper Substances 0.000 claims description 81
- 239000010410 layer Substances 0.000 claims description 77
- 230000009467 reduction Effects 0.000 claims description 43
- 239000002270 dispersing agent Substances 0.000 claims description 41
- 239000003638 chemical reducing agent Substances 0.000 claims description 37
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- 239000004471 Glycine Substances 0.000 claims description 22
- 238000005238 degreasing Methods 0.000 claims description 21
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 18
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 15
- 229910001431 copper ion Inorganic materials 0.000 claims description 15
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- FSVCELGFZIQNCK-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)glycine Chemical compound OCCN(CCO)CC(O)=O FSVCELGFZIQNCK-UHFFFAOYSA-N 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000012790 adhesive layer Substances 0.000 claims description 11
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 7
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 7
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- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 claims description 6
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 4
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 abstract description 6
- 239000010408 film Substances 0.000 description 127
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 74
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 20
- 229910052698 phosphorus Inorganic materials 0.000 description 20
- 239000011574 phosphorus Substances 0.000 description 20
- 150000001875 compounds Chemical class 0.000 description 19
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- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 16
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 15
- 229940112669 cuprous oxide Drugs 0.000 description 15
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 15
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- 239000002585 base Substances 0.000 description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 10
- 239000012046 mixed solvent Substances 0.000 description 10
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000004642 Polyimide Substances 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 9
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- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 8
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- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 8
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0041—Digital printing on surfaces other than ordinary paper
- B41M5/0047—Digital printing on surfaces other than ordinary paper by ink-jet printing
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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Abstract
本發明提供一種附導電性圖案之構造體的製造方法,其製造步驟簡便,且可形成層間密著性良好之附導電性圖案之構造體。本發明之一態樣係提供一種附導電性圖案之構造體的製造方法,其包含塗布膜形成步驟及鍍敷步驟,塗布膜形成步驟係將包含含有氧化銅的粒子之分散體印刷於基材而得塗布膜,鍍敷步驟係於前述塗布膜使用鍍敷液進行無電解鍍敷,前述鍍敷液係含有EDTA(乙二胺四乙酸)。
Description
本發明係關於附導電性圖案之構造體的製造方法。
電路基板係具有於基材上實施導電性配線之構造。電路基板的製造方法一般如下。首先於貼合有金屬箔之基材上塗布光阻劑。接著曝光光阻劑及顯影,而得所求電路圖案之負性狀形狀。接著將未被覆光阻劑部分之金屬箔以化學蝕刻去除,而形成圖案。藉此可製造高性能之電路基板。但是以往方法有步驟數較多較繁雜且需要光阻劑材料等缺點。
對此,以分散有金屬或金屬氧化物的粒子之分散體直接於基材上印刷所求配線圖案之直接印刷技術係備受矚目。該技術之步驟數較少且不需光阻劑材料等,可提高生產性。但是使用金屬粒子時,會因金屬粒子本身的氧化等,而有穩定性問題出現的情形。另一方面,使用金屬氧化物粒子時,為了獲得導電性而需要還原燒成步驟,故有可使用基材受限、及需要還原性氣體而提高成本的問題。
有關於上述,例如專利文獻1係記載一種導電膜的形成方法,係於基板上形成特定圖案之導電膜。該方法中,以於基板上形成與導電膜圖案幾乎相等之圖案之方式,藉由液滴吐出法形成含有金屬粒子之金屬膜,其後藉由至少1次無電解鍍敷,而以覆蓋該金屬膜表面之方式形成鍍膜,藉此獲得導電膜。
[先前技術文獻]
[專利文獻]
專利文獻1:日本特開2006-128228號公報。
專利文獻1所記載之方法係藉由組合使用金屬粒子的圖案形成及鍍敷以形成導電性及信賴性優異之導電膜,該方法中,導電膜與基材的密著性及/或導電膜內之層間密著性仍不足。
有鑑於該狀況,本發明之一態樣的目的在於提供一種附導電性圖案之構造體的製造方法,其製造步驟簡便,且可形成層間密著性良好之附導電性圖案之構造體。
本揭示包含以下態樣。
[1]一種附導電性圖案之構造體的製造方法,係包含下述步驟:
塗布膜形成步驟,將包含含有氧化銅的粒子之分散體印刷於基材而得塗布膜;
鍍敷步驟,於前述塗布膜使用鍍敷液進行無電解鍍敷;
前述鍍敷液係含有EDTA(乙二胺四乙酸)。
[2]如上述態樣1所述之附導電性圖案之構造體的製造方法,其中在前述鍍敷步驟之前進一步包含還原步驟。
[3]如上述態樣2所述之附導電性圖案之構造體的製造方法,其中前述還原步驟為濕式還原步驟。
[4]如上述態樣2或3所述之附導電性圖案之構造體的製造方法,其中前述還原步驟係包含於含有下述式所示之甘胺酸化合物之溶液中浸漬前述塗布膜,
(R1)2N-C-COOR2
(式中,R1及R2各自獨立地為氫或一價基,式中之複數個R1可互為相同或相異。)
[5]如上述態樣4所述之附導電性圖案之構造體的製造方法,其中前述甘胺酸化合物為N,N-二(2-羥基乙基)甘胺酸。
[6]如上述態樣4或5所述之附導電性圖案之構造體的製造方法,其中前述溶液為水溶液,前述甘胺酸化合物之濃度為1質量%以上50質量%以下。
[7]如上述態樣1至6中任一項所述之附導電性圖案之構造體的製造方法,其中在前述鍍敷步驟之前進一步包含脫脂步驟。
[8]如上述態樣1至7中任一項所述之附導電性圖案之構造體的製造方法,其中前述塗布膜形成步驟係藉由噴墨印刷而進行。
[9]如上述態樣1至8中任一項所述之附導電性圖案之構造體的製造方法,其中在前述塗布膜形成步驟與前述鍍敷步驟之間進一步包含乾燥前述塗布膜之乾燥步驟。
[10]如上述態樣1至9中任一項所述之附導電性圖案之構造體的製造方法,其中前述分散體係包含含有磷酸酯之分散劑。
[11]如上述態樣10所述之附導電性圖案之構造體的製造方法,其中前述分散劑之酸價(mgKOH/g)為20以上130以下。
[12]如上述態樣1至11中任一項所述之附導電性圖案之構造體的製造方法,其中前述分散體係含有還原劑,前述還原劑為肼。
[13]如上述態樣1至12中任一項所述之附導電性圖案之構造體的製造方法,其中前述分散體係含有由1-己醇、1-庚醇、及1-辛醇所成群組中選擇之1種以上的分散媒。
[14]如上述態樣1至13中任一項所述之附導電性圖案之構造體的製造方法,其中前述含有氧化銅的粒子之平均粒徑為1nm以上100nm以下。
[15]如上述態樣1至14中任一項所述之附導電性圖案之構造體的製造方法,其中前述鍍敷液係含有銅離子源及還原劑。
[16]如上述態樣15所述之附導電性圖案之構造體的製造方法,其中前述銅離子源為由CuSO4、CuCl2、CuCl、CuNO3、及Cu3(PO4)2所成群組中選擇之1種以上。
[17]如上述態樣15或16所述之附導電性圖案之構造體的製造方法,其中前述還原劑為由甲醛、四氫硼酸鉀(potassium tetrahydroborate)、二甲胺硼烷、乙醛酸、及次膦酸(phosphinic acid)所成群組中選擇之1種以上。
[18]如上述態樣1至17中任一項所述之附導電性圖案之構造體的製造方法,其中前述基材係具有密著層,
在前述塗布膜形成步驟中,將前述分散體印刷於前述密著層。
[19]一種導電性圖案構造體的製造套組,係含有由下述所成群組中選擇之至少2種:
包含含有氧化銅的粒子之分散體;
含有EDTA(乙二胺四乙酸)之鍍敷液;及
含有下述式所示之甘胺酸化合物之還原液;
(R1)2N-C-COOR2
(式中,R1及R2各自獨立地為氫或一價基,式中之複數個R1可互為相同或相異。)
根據本發明之一態樣可提供一種附導電性圖案之構造體的製造方法,其製造步驟簡便,且可形成層間密著性良好之附導電性圖案之構造體。
1:基材
2a:上清液
2b:沉殿物
2c:含氧化銅之膜
2d:氧化銅及/或銅的層
2e:鍍銅層
12:氧化銅
13:磷酸酯鹽
13a:磷
13b:酯鹽
100:氧化銅印墨
A:混合溶媒
B:乙酸銅
C:肼
D:分散劑
E:醇
圖1係表示本發明之一態樣中可使用之分散體中的氧化銅與磷酸酯鹽的關係之剖面示意圖。
圖2係表示本發明之一態樣之附導電性圖案之構造體的製造程序之剖面示意圖。
以下說明本發明之實施型態,但本發明並不限定於該等實施型態。
本發明之一態樣係提供一種附導電性圖案之構造體的製造方法。一態樣中,該方法係包含塗布膜形成步驟及鍍敷步驟,塗布膜形成步驟係將包含含有氧化銅的粒子之分散體印刷於基材而得塗布膜,鍍敷步驟係於塗布膜使用鍍敷液進行無電解鍍敷。
一態樣中,鍍敷液係含有EDTA(乙二胺四乙酸)。
根據本揭示之方法,在印刷所形成塗布膜上形成鍍敷層,藉此可在不需燒成下以所求圖案形成鍍敷層,故例如相較於使用以往光阻劑之手法係可提高生產性。又,一態樣中,可藉由鍍敷而形成空隙率較低之區域,故可降低附導電性圖案之構造體之電阻。具體方法如後述,但根據本實施型態之方法,可藉由濕式法而生成鍍敷層,故不須以往之還原性氣體及/或高溫。
以下說明各步驟之適合例。
<塗布膜形成步驟>
本步驟中係將包含含有氧化銅的粒子之分散體(本揭示中亦稱為氧化銅印墨)塗布於基材而得塗布膜。
[包含含有氧化銅的粒子之分散體]
分散體(氧化銅印墨)係包含含有氧化銅的粒子。含有氧化銅的粒子典型而言為氧化銅所構成,但可在不損及本發明效果之範圍內含有其他成分。分散體可進一步含有分散媒、分散劑、及/或還原劑。
(氧化銅)
氧化銅可舉出氧化亞銅(Cu2O)及氧化銅(II)(CuO),較佳為氧化亞銅。氧化亞銅雖為銅的價格,故相較於銀等貴金屬類較為便宜且不易發生遷移,此點較為有利,氧化銅係可使用市售品或合成品。
氧化亞銅之合成法可舉例如以下方法。
(1)於多元醇溶劑中添加水及乙醯丙酮銅錯合物,先將有機銅化合物加熱溶解,接著添加反應所需之水,進一步升溫並以有機銅之還原溫度加熱進行加熱還原之方法。
(2)將有機銅化合物(例如銅-N-亞硝基苯基羥基胺錯合物)在十六烷基胺等保護劑存在下在非活性環境中以300℃左右之高溫進行加熱之方法。
(3)將溶解於水溶液中之銅鹽以肼進行還原之方法。
其中,由於(3)之方法的操作簡便且可得平均粒徑較小之氧化亞銅,因而為佳。
氧化銅(II)之合成方法可舉出以下方法。
(1)於氯化銅(II)或硫酸銅之水溶液中添加氫氧化鈉,生成氫氧化銅後進行加熱之方法。
(2)將硝酸銅、硫酸銅、碳酸銅、氫氧化銅等在空氣中加熱至600℃左右之溫度進行熱解之方法。
其中,由於(1)之方法可得到粒徑較小之氧化銅(II),因而為佳。
合成結束後,使用離心等已知方法進行生成物溶液(作為上清液)及氧化銅(作為沉殿物)的分離。於所得氧化銅加入後述分散媒及任意後述分散劑,以均質機等已知方法攪拌分散。有時有難以藉由分散媒分散氧化銅或分散不足的情形,在如此的情況下,作為一例係可使用容易分散氧化銅之醇類(例如丁醇等)作為分散媒使分散氧化銅後,取代為所求分散媒及濃縮至所求濃度,藉此可使氧化銅良好地分散於所求分散媒。方法之一例可舉出以UF膜濃縮、以適當分散媒重複稀釋及濃縮之方法等。如此所得之氧化銅分散體係用於印刷。
一態樣中,氧化銅為微粒子狀。含有氧化銅的粒子之平均粒徑較佳為1nm以上、或3nm以上、或5nm以上,較佳為100nm以下、或50nm以下、或40nm以下。在此,平均粒徑是指分散在分散體中時之粒徑,為藉由累積法(例如使用大塚電子製FPAR-1000)測定時的值。亦即,平均粒徑不限於一次粒徑,有時為二次粒徑。平均粒徑為100nm以下時,可在低溫形成圖案,以基材通用性較大及容易在基材上形成微細圖案之傾向此點來看為較佳。又,平均粒徑為1nm以上時,分散體中的含有氧化銅的粒子之分散穩定性良好,以分散體之長期保管穩定性良好及可製作均一薄膜此點來看為較佳。一態樣中,分散體中之粒子實質上僅為含有氧化銅的粒子。此時,分散體所測定之平均粒徑值可視為含有氧化銅的粒子之平均粒徑。
一態樣中,含有氧化銅的粒子含有肼。肼可形成水合物(亦即,本揭示之肼亦有包含水合肼之概念)。肼可為製造含有氧化銅的粒子時
使用作為氧化銅之還原劑之肼的殘留物,也可為在製造該粒子時另外添加者。
含有氧化銅的粒子中,氧化銅含有率較佳為10質量%以上、或30質量%以上、或50質量%以上、或70質量%以上,較佳為100質量%以下、或99質量%以下、或98質量%以下。
含有氧化銅的粒子中,肼含有率較佳為0.000000001質量%以上、或0.0000001質量%以上、或0.0000005質量%以上,較佳為10質量%以下、或5質量%以下、或1質量%以下。
含有氧化銅的粒子中,肼相對於氧化銅之質量比率較佳為0.00001以上、或0.0001以上、或0.0002以上,較佳為1以下、或0.1以下、或0.01以下。
分散體100質量%中,氧化銅之質量比率較佳為5質量%以上、或10質量%以上、或15質量%以上,較佳為60質量%以下、或55質量%以下、或50質量%以下。
(分散媒)
分散媒可分散含有氧化銅的粒子。一態樣中,分散媒可溶解分散劑。以使用氧化銅印墨形成導電性圖案的觀點來看,分散媒之揮發性會影響操作性。因此,分散媒較佳為適合於導電性圖案之形成方法,例如適合於塗布方式(尤其是印刷)。亦即,較佳為配合分散性及印刷操作性而選擇分散媒。
分散媒可使用醇類(一元醇及多元醇(例如二醇))、醇(例如二醇)之醚類、醇(例如二醇)之酯類等。分散媒之具體例可舉出丙二醇單甲基
醚乙酸酯、3-甲氧基-3-甲基-丁基乙酸酯、乙氧基丙酸乙酯、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單丙基醚、丙二醇第三丁基醚、二丙二醇單甲基醚、乙二醇丁基醚、乙二醇乙基醚、乙二醇甲基醚、乙二醇、1,2-丙二醇、1,3-丁二醇、2-戊二醇、2-甲基戊烷-2,4-二醇、2,5-己二醇、2,4-庚二醇、2-乙基己烷-1,3-二醇、二乙二醇、己二醇、辛二醇、三乙二醇、三-1,2-丙二醇、甘油、乙二醇單己基醚、二乙二醇單乙基醚、二乙二醇單丁基醚、乙二醇單丁基乙酸酯、二乙二醇單乙基醚乙酸酯、甲醇、乙醇、正丙醇、異丙醇、正丁醇、異丁醇、2-丁醇、第三丁醇、正戊醇、異戊醇、2-甲基丁醇、2-戊醇、第三戊醇、3-甲氧基丁醇、正己醇、2-甲基戊醇、1-己醇、2-己醇、2-乙基丁醇、1-庚醇、2-庚醇、3-庚醇、正辛醇、2-乙基己醇、1-辛醇、2-辛醇、正壬醇、2,6二甲基-4-庚醇、正癸醇、環己醇、甲基環己醇、3,3,5-三甲基環己醇、苄醇、二丙酮醇等。該等可單獨使用或混合複數種使用,可因應塗布方式考慮蒸發性、塗布所使用之機材、基材(亦即被塗布基材)之耐溶劑性等而選擇。以乾燥較慢、連續印刷時印墨較不易產生凝集、及噴墨之間歇穩定性良好、異常飛噴較少此點來看,分散體特佳為含有由1-己醇、1-庚醇、及1-辛醇所成群組中選擇之1種以上的分散媒。
以提高印刷連續性此點來看,分散媒之沸點以高者為佳,例如較佳為50℃以上,更佳為100℃以上,又更佳為150℃以上。另一方面,以作為分散媒之功能良好之觀點來看,上述沸點較佳為400℃以下,更佳為300℃以下,又更佳為250℃以下。
在分散體整體中,分散媒含量較佳為30質量%以上、或40質量%以上、或50質量%以上,較佳為95質量%以下、或90質量%以下。
(分散劑)
分散劑可使用可將氧化銅分散於分散媒中之化合物。分散劑之數平均分子量較佳為300以上、或350以上、或400以上,較佳為300,000以下、或200,000以下、或150,000以下。又,本揭示之數平均分子量為使用凝膠滲透層析法以標準聚苯乙烯換算所求的值。數平均分子量若為300以上,則有絕緣性優異且可增加分散體之分散穩定性之傾向,若為300,000以下則以操作性之觀點來看為較佳。分散劑之較佳係具有對氧化銅具有親和性的基。以該觀點來看,分散劑較佳為含有含磷有機物或為含磷有機物、或含有磷酸酯或為磷酸酯、或含有聚合物之磷酸酯或為聚合物之磷酸酯。聚合物之磷酸例如較佳為下述式(1)所示構造,其對於氧化銅,尤其是對於氧化亞銅之吸附性、及與基材的密著性優異。
(式中,l為1至10000之整數,m為1至10000之整數,n為1至10000之整數。)
化學式(1)中,l更佳為1至5000,又更佳為1至3000。
化學式(1)中,m更佳為1至5000,又更佳為1至3000。
化學式(1)中,n更佳為1至5000,又更佳為1至3000。
一態樣中,含磷有機物之分解溫度較佳為600℃以下,更佳為400℃以下,又更佳為200℃以下。以容易選擇分散體之分散穩定性提高效果較優異之分散劑之觀點來看,分解溫度可為50℃以上、或80℃以上、或100℃以上。一態樣中,含磷有機物之沸點較佳為300℃以下,更佳為200℃以下,又更佳為150℃以下。沸點可為30℃以上、或50℃以上、或80℃以上。本揭示中,分解溫度為以熱重示差熱分析法所測定的值。
一態樣中,以進行鍍敷時不易產生塗布膜與鍍敷層的剝離此點來看,較佳為含磷有機物。
分散劑亦可使用公知者。可舉例如長鏈聚胺基醯胺與極性酸酯的鹽、不飽和多羧酸聚胺基醯胺、聚胺基醯胺之多羧酸鹽、長鏈聚胺基醯胺與酸聚合物的鹽等具有鹼性基之聚合物。又,可舉出丙烯酸系(共)聚合物、改質聚酯酸、聚醚酯酸、聚醚系羧酸、多羧酸等聚合物之烷基銨鹽、胺鹽、醯胺胺鹽等。如此分散劑可使用市售品。
上述市售品可舉例如DISPERBYK(註冊商標)-101、DISPERBYK-102、DISPERBYK-110、DISPERBYK-111、DISPERBYK-112、DISPERBYK-118、DISPERBYK-130、DISPERBYK-140、DISPERBYK-142、DISPERBYK-145、DISPERBYK-160、DISPERBYK-161、DISPERBYK-162、DISPERBYK-163、DISPERBYK-2155、DISPERBYK-2163、DISPERBYK-2164、DISPERBYK-180、DISPERBYK-2000、DISPERBYK-2025、DISPERBYK-2163、DISPERBYK-2164、BYK-9076、BYK-9077、TERRA-204、及TERRA-U(以上為BYK公司製)、FLOREN DOPA-15B、FLOREN DOPA-15BHFS、FLOREN DOPA-22、
FLOREN DOPA-33、FLOREN DOPA-44、FLOREN DOPA-17HF、FLOREN TG-662C、及FLOREN KTG-2400(以上為共榮社化學公司製)、ED-117、ED-118、ED-212、ED-213、ED-214、ED-216、ED-350、及ED-360(以上為楠本化成社製)、PRISURF M208F、及PRISURF DBS(以上為第一工業製藥製)等。該等可單獨使用或混合複數種使用。
分散劑之酸價(mgKOH/g)較佳為20以上、或30以上,較佳為130以下、或100以下。酸價為上述範圍時,分散體之分散穩定性良好,因而為佳。尤其為平均粒徑較小之氧化銅時,上述範圍之酸價更為有效。具體而言較佳可舉出BYK公司製「DISPERBYK-102」(酸價101)、「DISPERBYK-140」(酸價73)、「DISPERBYK-142」(酸價46)、「DISPERBYK-145」(酸價76)、「DISPERBYK-118」(酸價36)、「DISPERBYK-180」(酸價94)等。
又,分散劑之胺價(mgKOH/g)與酸價的差([胺價]-[酸價])較佳為-50以上0以下。胺價係表示游離鹼及源自於游離鹼的部位的總量,酸價係表示游離脂肪酸及源自於游離脂肪酸的部位的總量。胺價及酸價分別以根據JIS K 7700或ASTM D2074之方法測定。[胺價]-[酸價]之值為-50以上0以下時,分散體之分散穩定性良好,因而為佳。[胺價]-[酸價]之值更佳為-40以上0以下,又更佳為-20以上0以下。
分散劑含量與氧化銅量成正比,並考慮所要求的分散穩定性而調整即可。分散體中,分散劑相對於氧化銅之質量比率(分散劑質量/氧化銅質量)較佳為0.0050以上、或0.050以上、或0.10以上,較佳為0.30以下、或0.25以下、或0.23以下。分散劑量會影響分散體之分散穩定性,量
若較少則氧化銅容易凝集,較多則有提高分散體之分散穩定性之傾向。但若使分散體中的分散劑含有率為35質量%以下,則可抑制鍍敷步驟後所得含銅膜中源自於分散劑之殘渣的影響,並提高導電性。一態樣中,分散體100質量%中,分散劑量較佳為0.5質量%以上、或0.8質量%以上、或1.0質量%以上,較佳為35質量%以下、或30質量%以下、或25質量%以下。
(還原劑)
一態樣中,分散體係含有還原劑。還原劑可舉出肼、鈉、硼氫化鈉、碘化鉀、亞硫酸鹽、硫代硫酸鈉、甲酸、草酸、抗壞血酸、硫化鐵(II)、氯化錫(II)、氫化二異丁基鋁、碳等,較佳為肼。肼可為水合肼之形態(亦即,本揭示之肼亦為包含水合肼之概念)。分散體含有肼,在鍍敷步驟中肼會幫助氧化銅的還原,尤其是氧化亞銅的還原,可形成電阻更低之還原銅層(作為含銅膜)。又,肼亦有利於維持分散體之分散穩定性,以鍍敷時之生產性提高之觀點來看亦為較佳。分散體中的肼可作為含有氧化銅的粒子中的成分而存在,及/或可作為與含有氧化銅的粒子不同的存在。
分散體中之還原劑含量(水合物時為去除水合水的量)與氧化銅量成正比,並考慮所要求之還原性而調整即可。一態樣中,分散體中之還原劑相對於氧化銅之質量比率(還原劑質量/氧化銅質量)較佳為0.0001以上,更佳為0.1以下、或0.05以下、或0.03以下。還原劑之質量比率為0.0001以上時,分散體之分散穩定性良好,且還原銅層之電阻較低,以此點來看為較佳,為0.1以下時,分散體之長期穩定性良好。
可併用2種類以上之還原劑。例如併用肼與肼以外之還原劑時,分散體中之肼與肼以外之還原劑的合計含量與氧化銅量成正比,並考
慮所要求還原性而調整即可。一態樣中,分散體中,相對於氧化銅之肼與肼以外之還原劑的合計質量比率(還原劑合計質量/氧化銅質量)較佳為0.0001以上,更佳為0.1以下、或0.05以下、或0.03以下。還原劑之上述合計質量比率為0.0001以上時,分散體之分散穩定性良好,且還原銅層之電阻較低,以此點來看為較佳,為0.1以下時,分散體之長期穩定性良好。
分散體可藉由混合摻配成分並使用混合器法、超音波法、3輥法、2輥法、磨碎機、均質機、班柏立混合器、油漆搖動器、捏合機、球磨機、砂磨機、自公轉混合器等進行分散處理而製造。分散體之黏度可因應目的之塗布樣式而設計。例如網版印刷用分散體之黏度較佳為50mPa‧s以上,更佳為100mPa‧s以上,又更佳為200mPa‧s以上,較佳為50000mPa‧s以下,更佳為10000mPa‧s以下,又更佳為5000mPa‧s以下。又,分散體之黏度為使用錐板型旋轉黏度計於23℃所測定的值。
(分散體中之氧化銅與分散劑的關係)
圖1係表示本發明之一態樣可使用之分散體(氧化銅印墨)中的氧化銅與磷酸酯鹽的關係之剖面示意圖。參照圖1,本發明之一態樣中,氧化銅印墨100含有氧化銅12及磷酸酯鹽13(作為分散劑之磷酸酯之例)時,磷酸酯鹽13係以磷13a朝內側、酯鹽13b朝外側之方式分別包圍氧化銅12周圍。磷酸酯鹽13顯示電絕緣性,故磷酸酯鹽13會妨礙互相鄰接之氧化銅12間之電導通。又,磷酸酯鹽13係藉由位阻效果而抑制氧化銅印墨100之凝集。因此,氧化銅12雖為半導體(亦即具有一定程度之導電性),但被顯示電絕緣性之磷酸酯鹽13覆蓋,故氧化銅印墨100顯示電絕緣性。
另一方面,在鍍敷步驟等中,若氧化銅12還原為銅,則會形成具有優異導電性之導電性圖案區域。又,分散劑在使用含磷有機物時,導電性圖案區域中會殘留磷元素。磷元素係作為磷元素單體、磷酸化物、及含磷有機物中之至少1種而存在。但如此殘留磷元素通常會偏析存在於導電性圖案區域中,故無導電性圖案區域的電阻變大之虞。
[基材]
本實施型態所使用之基材係具有形成塗布膜之表面,可舉例如用以形成配線圖案之電路基板薄片之基板材料等。基材可以無機材料或有機材料或該等的組合構成,在一態樣中可具有密著層。
無機材料可舉例如鈉萊姆玻璃、無鹼玻璃、硼矽酸玻璃、石英玻璃等玻璃、及氧化鋁等陶瓷材料。
有機材料可舉出纖維素等紙材料、樹脂膜等高分子材料。高分子材料可舉出聚醯亞胺(PI)、聚酯(聚對苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚對苯二甲酸丁二酯(PBT)等)、聚醚碸(PES)、聚碳酸酯(PC)、聚乙烯醇(PVA)、聚乙烯縮丁醛(PVB)、聚縮醛(POM)、聚芳酯(PAR)、聚醯胺(PA)(PA6、PA66等)、聚醯胺醯亞胺(PAI)、聚醚醯亞胺(PEI)、聚苯醚(PPE)、改質聚苯醚(m-PPE)、聚苯硫醚(PPS)、聚醚酮(PEK)、聚鄰苯二甲醯胺(PPA)、聚醚腈(PENt)、聚苯并咪唑(PBI)、聚碳二亞胺、聚矽氧聚合物(聚矽氧烷)、聚甲基丙烯醯胺、腈橡膠、丙烯酸橡膠、聚四氟乙烯、環氧樹脂、酚樹脂、三聚氰胺樹脂、脲樹脂、聚甲基丙烯酸甲酯樹脂(PMMA)、聚丁烯、聚戊烯、乙烯/丙烯共聚物、乙烯/丁烯/二烯共聚物、聚丁二烯、聚異戊二烯、乙烯/丙烯/二烯共聚物、丁基橡膠、聚甲基戊烯(PMP)、聚苯乙
烯(PS)、苯乙烯/丁二烯共聚物、聚乙烯(PE)、聚氯乙烯(PVC)、聚偏二氟乙烯(PVDF)、聚醚醚酮(PEEK)、酚酚醛清漆、苯并環丁烯、聚乙烯酚、聚氯芘、聚甲醛、聚碸(PSF)、聚苯基碸樹脂(PPSU)、環烯烴聚合物(COP)、丙烯腈/丁二烯/苯乙烯樹脂(ABS)、丙烯腈/苯乙烯樹脂(AS)、聚四氟乙烯樹脂(PTFE)、聚氯三氟乙烯(PCTFE)等。尤其以可撓性、成本之觀點而言,較佳為PI、PET及PEN。
基材例如為玻璃複合基材、玻璃環氧基材等複合基材、鐵氟龍(註冊商標)基材、氧化鋁基材、低溫低濕共燒陶瓷(LTCC)、矽晶圓等。
基材之厚度較佳為1μm以上、或25μm以上,較佳為10mm以下、或250μm以下。基材之厚度為250μm以下時,可使所製作之電子裝置輕量、省空間、及可撓化,因而為佳。
[塗布膜之形成]
分散體之塗布方法可使用噴墨印刷、網版印刷、凹版直接印刷、凹版平版印刷、柔版印刷、平版印刷等。塗布可使用模具塗布、旋轉塗布、狹縫塗布、棒塗布、刀塗布、噴霧塗布、浸漬塗布等方法實施。塗布方法較佳為噴墨印刷。噴墨法不須印刷版,且配線間不會附著多餘成分,故遷移性優異。
以可形成均一導電性圖案此點來看,塗布膜乾燥後之層厚較佳為1nm以上、或10nm以上、或100nm以上,較佳為10000nm以下、或8000nm以下、或7000nm以下。
基材可具有密著層(亦稱印墨收納層),藉由將分散體印刷於該密著層上而可形成塗布膜。形成密著層之化合物(本揭示中亦稱為「塗布
用化合物」)較佳為具有-OH基、及/或具有Ar-O構造及/或M-O構造。在此,Ar表示芳香族構造,M表示金屬原子。上述密著層存在時,可在基材上密著性佳地形成包含含有氧化銅的粒子之層,又,由於熱不易傳遞至基材本體,因此亦可使用耐熱性低之樹脂,例如聚對苯二甲酸乙二酯(PET)樹脂作為基材本體,故以通用性之觀點來看較為有利。
-OH基尤其較佳為芳香族性羥基(亦即,構成-Ar-OH基之-OH基)或鍵結於金屬原子之羥基(亦即,構成-M-OH基之-OH基)。構成-Ar-OH基及-M-OH基之-OH基的活性較高,有密著層與基材本體的密著性、及/或包含含有氧化銅的粒子之層與密著層的密著性優異之傾向。
-Ar-OH基中的芳香族構造(Ar)可舉例如苯、萘、蒽、稠四苯、稠五苯、菲、芘、並、及聯伸三苯等芳香族烴;以及噻吩、噻唑、吡咯、呋喃、吡啶、吡唑、咪唑、噠嗪、嘧啶、及吡嗪等雜芳香族化合物;等源自於芳香族化合物(亦即從該等化合物去除有2個氫原子)之2價基。芳香族構造之π電子系所含電子數較佳為22以下,更佳為14以下,又更佳為10以下。π電子系所含電子數若為22以下,則結晶性不會過高,容易獲得柔軟且平滑性高之密著層。芳香族構造中,鍵結於芳香環之氫的一部分可用官能基取代。官能基可舉例如鹵基、烷基(例如甲基、異丙基、第三丁基等)、芳基(例如苯基、萘基等)、雜芳香族基(噻吩基等)、鹵芳基(例如五氟苯基、3-氟苯基、3,4,5-三氟苯基等)、烯基、炔基、醯胺基、醯基、烷氧基(例如甲氧基等)、芳氧基(例如苯氧基、萘氧基等)、鹵烷基(例如全氟烷基等)、硫氰基、及羥基等。較佳為-Ar-OH基,特佳為羥基苯基(-Ph-OH)。
-M-OH基中的金屬原子(M)可舉出矽、銀、銅、鋁、鋯、鈦、鉿、鉭、錫、鈣、鈰、鉻、鈷、鈥、鑭、鎂、錳、鉬、鎳、銻、釤、鋱、鎢、釔、鋅、及銦等。密著層需要絕緣性時,較佳為-Si-OH基或-Zr-OH基,密著層需要導電性時,較佳為-Ti-OH基或-Zn-OH基。
Ar-O構造中的芳香族構造(Ar)可為由與上述-Ar-OH基所例示芳香族化合物相同之芳香族化合物除去1個以上氫原子之構造。尤其,Ar-O構造較佳為Ph-O構造。
M-O構造中的金屬原子可使用與上述-M-OH基所例示金屬原子相同者。尤其,M-O構造較佳為Si-O構造、Ti-O構造、Zn-O構造、及Zr-O構造。
具有Si-O構造之塗布用化合物可舉例如二氧化矽系化合物(例如二氧化矽(SiO2))、及聚矽氧系化合物(例如聚矽氧烷、烷基聚矽氧烷、二甲基聚矽氧烷)等。
塗布用化合物可舉例如於聚醯亞胺、聚酯(聚對苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)等)、聚醚碸(PES)、聚碳酸酯(PC)、聚乙烯醇(PVA)、聚乙烯縮丁醛(PVB)、聚縮醛、聚芳酯(PAR)、聚醯胺(PA)、聚醯胺醯亞胺(PAI)、聚醚醯亞胺(PEI)、聚苯醚(PPE)、聚苯硫醚(PPS)、聚醚酮(PEK)、聚鄰苯二甲醯胺(PPA)、聚醚腈(PENt)、聚苯并咪唑(PBI)、聚碳二亞胺、聚矽氧聚合物(聚矽氧烷)、聚甲基丙烯醯胺、腈橡膠、丙烯酸橡膠、聚四氟乙烯、環氧樹脂、酚樹脂、三聚氰胺樹脂、脲樹脂、聚甲基丙烯酸甲酯樹脂(PMMA)、聚丁烯、聚戊烯、乙烯/丙烯共聚物、乙烯/丁烯/二烯共聚物、聚丁二烯、聚異戊二烯、聚氯丁二烯、乙烯/丙烯/二烯共聚物、
腈橡膠、氯碸化聚乙烯、丙烯酸橡膠、環氧氯丙烷橡膠、胺甲酸乙酯橡膠、丁基橡膠、氟橡膠、聚甲基戊烯(PMP)、聚苯乙烯(PS)、苯乙烯/丁二烯共聚物、聚乙烯(PE)、聚氯乙烯(PVC)、聚偏二氟乙烯(PVDF)、聚醚醚酮(PEEK)、酚酚醛清漆樹脂、苯并環丁烯、聚乙烯酚、聚氯芘、聚甲醛、聚碸(PSF)等導入上述-OH基、Ar-O構造及M-O構造中的1種以上之材料。塗布用化合物尤其較佳為酚樹脂、酚酚醛清漆樹脂、聚乙烯酚、及聚醯亞胺。
密著層之厚度上限值並無特別限定,較佳為20μm以下,更佳為5μm以下,又更佳為1μm以下,下限值較佳為0.01μm以上,更佳為0.05μm以上,又更佳為0.2μm以上。
<乾燥步驟>
本揭示之方法之一態樣可進一步在塗布膜形成步驟與鍍敷步驟之間包含乾燥塗布膜之乾燥步驟。在乾燥步驟中使塗布膜形成步驟所得塗布膜乾燥。乾燥步驟為使分散媒氣化之步驟。分散媒可在室溫氣化,也可以烘箱、真空乾燥等方法氣化。考慮基材之耐熱性,較佳為以150℃以下之溫度乾燥,更佳為以100℃以下之溫度乾燥。又,乾燥時也可導入氮或混合氫的氮(例如氫與氮的合計100體積%中含有氫3體積%左右之混合氣體)。
<還原步驟>
本揭示方法之一態樣可在鍍敷步驟之前包含還原步驟。在還原步驟中還原經過或未經過乾燥步驟之塗布膜之含氧化銅之膜,藉此獲得含銅膜。本步驟中,還原含氧化銅之膜中之含有氧化銅的粒子並生成銅,藉由銅本身之熔融及一體化而可形成含銅膜(還原銅層)。但直接鍍敷含有氧化銅的
粒子時可省略本步驟。還原方法可舉出在氮環境下以100℃以上500℃以下之溫度進行還原之方法、在混合氫的氮(例如氫與氮的合計100體積%中含有氫3體積%左右之混合氣體)中以100℃以上500℃以下之溫度進行還原之方法、於還原液中浸漬含氧化銅之膜之方法(亦即濕式還原)等。一態樣中,還原步驟為將含氧化銅之膜浸漬於還原液之步驟,亦即濕式還原步驟。
還原液含有還原劑。還原劑可為無機系或有機系。無機系還原劑可舉出硼氫化鈉、二氧化硫、亞硝酸鈉、金屬鋁、氯化鈰、硫代硫酸鈉等,有機系還原劑可舉出肼、甲醛、甲醇、檸檬酸及其鹽、草酸及其鹽、甲酸及其鹽、甘油、葡萄糖、乙二醇、下述式(2)所示甘胺酸化合物(本揭示中亦單稱為甘胺酸化合物)、L-抗壞血酸及其鹽、硫乙醇酸、鹽酸羥基胺、氫醌、亞硫酸氫鹽、異抗壞血酸、異抗壞血酸鹽、硫脲、錫系還原劑、鐵系還原劑、鋅系還原劑等。
(R1)2N-C-COOR2 (2)
(式中,R1及R2各自獨立地為氫或一價基,式中之複數個R1可互為相同或相異。)
上述式(2)所示甘胺酸化合物為甘胺酸或其衍生物。甘胺酸衍生物可舉例如N-[N-(苄基氧羰基)胺乙醯基]-L-脯胺酸、N-苄氧羰基甘胺酸-4-硝基苯基、L-(2-氯苯基)甘胺酸氯化物、BOC-NA-甲基-L-苯基甘胺酸、乙醯胺基(氰基)乙酸乙酯、茬酚橙、D-(-)-2-(2,5-二氫苯基)甘胺酸、Cbz-環己基-L-甘胺酸、(R)-α-[(3-乙氧基-1-甲基-3-側氧基-1-丙烯基)胺基]苯乙酸鉀、N-(二苯基亞甲基)甘胺酸第三丁酯、D-炔丙基甘胺酸、(S)-α-胺基-4-氟苯乙酸、N-(第三丁氧基羰基)-L-2-環己基甘胺酸、甘胺酸甲酯鹽酸鹽、D-
2-烯丙基甘胺酸鹽酸鹽、(S)-2-環己基-2-胺基乙酸、(2S)-N-[[(羧甲基)胺基羰基]甲基]-2-胺基-4-甲基戊醯胺、(R)-2-胺基-4-炔丙乙酸、(R)-N-BOC-炔丙基甘胺酸、N-苄基甘胺酸、(S)-N-BOC-A-烯丙基甘胺酸二環己胺、BOC-D-環丙基甘胺酸、N-(第三丁氧基羰基)-D-2-苯基甘胺酸、(R)-(-)-N-(3,5-二硝基苯甲醯基)-α-苯基甘胺酸、L-2-氯苯基甘胺酸、4-氟-D-苯基甘胺酸、BOC-L-環丙基甘胺酸、甘胺酸苄基對甲苯磺酸酯、(S)-N-BOC-烯丙基甘胺酸、(R)-N-BOC-烯丙基甘胺酸、(R)-4-羥基-α-[(3-甲氧基-1-甲基-3-側氧基-1-丙烯基)胺基]苯乙酸鉀、N-[(9H-茀-9-基甲氧基)羰基]-D-2-苯基甘胺酸、DL-白胺醯基胺乙醯基甘胺酸、胺乙醯基胺乙醯基甘胺酸、N-(第三丁氧基羰基)-L-炔丙基甘胺酸、2-胺基-2-[3-(三氟甲基)苯基]乙酸、(S)-N-BOC-3-羥基金剛烷基甘胺酸、N-[三(羥基甲基)甲基]甘胺酸、2-炔丙基-L-甘胺酸、N-(三苯基甲基)甘胺酸、N-苄基甘胺酸乙酯、2-(2-側氧基-2-羥基乙胺基)安息香酸、FMOC-D-烯丙基甘胺酸、L-2-(4-氯苯基)甘胺酸、D-2-環己基甘胺酸、N,N-二(2-羥基乙基)甘胺酸、N-(苄基氧羰基)-D-苯基甘胺酸、N-[(9H-茀-9-基甲氧基)羰基]-L-2-苯基甘胺酸、苄基氧羰基胺基(二甲氧基膦基)乙酸甲酯、N-(第三丁氧基羰基)甘胺酸甲酯、4-(三氟甲基)苯基甘胺酸、胺乙醯基-DL-白胺酸、N-甲苯磺醯基甘胺酸、N-(第三丁氧基羰基)-D-2-環己基甘胺酸、N-甲醯基甘胺酸、N-T-丁基甘胺酸HCL、(R)-2-烯丙基甘胺酸、H-甘胺酸苄酯鹽酸鹽、N-苄氧羰基-L-2-苯基甘胺酸、(二苯基亞甲胺基)乙酸乙酯(二苯基亞甲胺基)乙酸乙酯、羥苯甘胺酸(oxfenicine)、L-甲硫胺醯基甘胺酸、(4-羥基苯基)(胺基)乙酸、(R)-α-胺基苯乙酸甲酯鹽酸鹽、L-A-環丙基甘胺酸、N-苄基甘胺酸鹽酸鹽、D-環丙基甘胺酸、α-胺基-4-氟
苯乙酸、甘胺酸第三丁酯鹽酸鹽、N-(第三丁氧基羰基)-2-膦醯基甘胺酸三甲酯、N-[(9H-茀-9-基甲氧基)羰基]甘胺酸、N-(4-羥基苯基)甘胺酸、DL-2-(4-氯苯基)甘胺酸、L-A-環己基甘胺酸、甘胺酸乙酯鹽酸鹽、N-[(甲氧基羰基)甲基]胺基甲酸苄酯、DL-2-(2-氯苯基)甘胺酸、L-環戊基甘胺酸、N-BOC-2-(4’-氯苯基)-D-甘胺酸、BOC-L-環戊基甘胺酸、D-(2-氯苯基)甘胺酸氯化物、N-鄰苯二甲醯基甘胺酸、N-甲醯基甘胺酸乙酯、N-(第三丁氧基羰基)-L-2-苯基甘胺酸、N-(第三丁氧基羰基)甘胺酸、N-(2-胺基乙基)甘胺酸、N-苯基甘胺酸、N,N-二甲基甘胺酸鹽酸鹽、(S)-N-FMOC-烯丙基甘胺酸、D-(-)-2-(4-羥基苯基)甘胺酸、L(+)-2-苯基甘胺酸甲酯鹽酸鹽、乙二胺四乙酸三鈉、N-(第三丁氧基羰基)胺乙醯基甘胺酸、(2R)-2-胺基-2-苯乙酸乙酯鹽酸鹽、N-乙醯基甘胺酸乙酯、L-白胺醯基甘胺酸水合物、L-2-烯丙基甘胺酸鹽酸鹽等。
上述式(2)中,R1較佳為具有1個以上羥基之碳數1至4之一價基。
上述式(2)中,R2較佳為氫、或碳數1至3之烴基。
又,甘胺酸衍生物較佳為具備分子中具有2個以上羥基之構造之化合物。使用具有2個以上羥基之甘胺酸衍生物可提高後步驟之鍍敷步驟之速度,且在步驟中不易產生膜的剝離,以此點來看較有利。具備分子中具有2個以上羥基之構造之化合物之適合例有N,N-二(2-羥基乙基)甘胺酸、N-[三(羥基甲基)甲基]甘胺酸等。
還原步驟為濕式還原步驟時,以還原速度良好且可安定還原之觀點來看,還原液中之還原劑濃度例如可為1.0g/L以上、或3.0g/L以
上、或5.0g/L以上、或10.0g/L以上,例如可為600g/L以下、或570g/L以下、或550g/L以下、或520g/L以下、或500g/L以下。
以還原速度良好且可安定還原之觀點來看,還原液中之還原劑濃度例如可為0.1質量%以上、或0.3質量%以上、或0.5質量%以上、或1.0質量%以上,例如可為60質量%以下、或57質量%以下、或55質量%以下、或52質量%以下、或50質量%以下。
一態樣中,還原液含有上述式(2)所示甘胺酸化合物。還原液中之該甘胺酸化合物之濃度較佳為1質量%以上、或8質量%以上、或16質量%以上,較佳為50質量%以下、或32質量%以下。
典型態樣中,還原液含有溶媒。溶媒系可為水系或有機溶媒系。溶媒可舉例如水、乙醇、1-丁醇、2-丙醇、甲苯、己烷、苯、氯仿、二氯甲烷、乙酸、乙酸乙酯、四氫呋喃、丙酮、乙腈、N,N-二甲基甲醯胺、二甲基亞碸等。尤其以再利用之觀點來看較佳為水、乙醇、1-丁醇、及2-丙醇。
還原液中之溶媒特佳為水,尤其甘胺酸化合物與水的組合以成本及生產性之觀點來看為較佳。還原液之特佳係甘胺酸化合物之濃度為1質量%以上50質量%之水溶液。
一態樣中,以生產性之觀點,亦即還原進行較快的觀點來看,還原液較佳為含有N,N-二(2-羥基乙基)甘胺酸及/或檸檬酸。尤其使用N,N-二(2-羥基乙基)甘胺酸時,在還原液中銅會形成2價離子並與甘胺酸形成錯合物,藉此可促進氧化銅還原為銅,以此點來看為較佳。
還原中較佳係以還原液中之還原劑濃度為固定之方式一邊攪拌一邊浸漬塗布膜。
還原液較佳為含有特定以上之銅離子及/或氧化銅。藉此可抑制濕式還原時塗布膜的脫落。還原液中之銅離子濃度或氧化銅濃度、或銅離子與氧化銅的合計濃度較佳為1質量%以上、或5質量%以上,較佳為99質量%以下、或90質量%以下。一態樣中,藉由於溶媒中添加由乙酸銅、氯化銅、氧化銅、金屬銅、及本揭示之包含含有氧化銅的粒子之分散體所成群組中選擇之1種以上而調製還原液,可於還原液中含有銅離子及/或氧化銅。一態樣中,藉由使氧化銅從塗布膜擴散至溶媒中,可使還原液含有氧化銅。
以生產性、還原進行較快之觀點來看,濕式還原步驟之溫度較佳為20℃以上,更佳為30℃以上,又更佳為40℃以上。又,以獲得均一含銅膜之觀點來看較佳為100℃以下,更佳為90℃以下。
亦可同時進行濕式還原步驟及鍍敷步驟中的無電解鍍敷。以生產性提高之觀點來看,較佳為同時進行濕式還原步驟及鍍敷步驟。具體而言,使後述鍍敷液含有還原劑,藉此可同時進行濕式還原步驟及鍍敷步驟。又,此時,鍍敷液中,還原劑濃度及鍍敷物質濃度(一態樣中為銅濃度)較佳為以成為本揭示之還原液及鍍敷液所例示範圍內之方式調整溶媒量。
<洗淨步驟>
進行濕式還原時,可在該濕式還原後使用適當洗淨液去除未還原部及還原液。藉此可在基材上殘留乾淨的還原區域。另一方面也可不進行洗淨步驟。不論任一情形都可獲得藉由導電性圖案之還原區域而賦予導電性之
基材(以下稱為導電性基材)。但直接鍍敷含氧化銅之膜時,有時可省略本步驟。
進行洗淨時之洗淨液可使用分散或溶解氧化銅之液。具體例可舉出水、丙二醇單甲基醚乙酸酯、3-甲氧基-3-甲基-丁基乙酸酯、乙氧基丙酸乙酯、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單丙基醚、丙二醇第三丁基醚、二丙二醇單甲基醚、乙二醇丁基醚、乙二醇乙基醚、乙二醇甲基醚、乙二醇、1,2-丙二醇、1,3-丁二醇、2-戊二醇、2-甲基戊烷-2,4-二醇、2,5-己二醇、2,4-庚二醇、2-乙基己烷-1,3-二醇、二乙二醇、己二醇、辛二醇、三乙二醇、三-1,2-丙二醇、甘油、乙二醇單己基醚、二乙二醇單乙基醚、二乙二醇單丁基醚、乙二醇單丁基乙酸酯、二乙二醇單乙基醚乙酸酯、甲醇、乙醇、正丙醇、異丙醇、正丁醇、異丁醇、2-丁醇、第三丁醇、正戊醇、異戊醇、2-甲基丁醇、2-戊醇、第三戊醇、3-甲氧基丁醇、正己醇、2-甲基戊醇、1-己醇、2-己醇、2-乙基丁醇、1-庚醇、2-庚醇、3-庚醇、正辛醇、2-乙基己醇、2-辛醇、正壬醇、2、6二甲基-4-庚醇、正癸醇、環己醇、甲基環己醇、3,3,5-三甲基環己醇、苄醇、二丙酮醇、丙酮等溶媒。尤其在塗布膜含有分散劑時,上述溶媒可良好地洗掉氧化銅而佳。溶媒特佳為水、乙醇、丁醇、異丙醇、及丙酮。又,上述洗淨液除了溶媒以外也可含有分散劑。分散劑可使用前述者,但更佳為含磷有機物。
<脫脂步驟>
本揭示之方法之一態樣可在鍍敷步驟之前具有包含氧化銅之膜或含銅膜進行脫脂之步驟。一態樣中,氧化銅不會還原而直接脫脂,藉此可提高生產性。又,另一態樣中可在還原氧化銅(例如於前述還原步驟)後脫脂。脫
脂方法可舉出UV法、濕式脫脂法等。藉由脫脂步驟可使其後之鍍敷成長速度加快並提高生產性。又,本步驟可降低鍍敷後之導電性層(亦即鍍敷層,在含氧化銅之膜中之氧化銅還原態樣中進一步為還原銅層)的空隙率,亦即可降低最終導電性層的空隙率。又,無電解鍍敷及脫脂可一起進行,此時可省略脫脂步驟。
以附導電性圖案之構造體之層間密著性之觀點來看,脫脂步驟較佳為藉由將含氧化銅之膜或含銅膜浸漬於包含含胺基之化合物之脫脂液而進行。含胺基之化合物可舉出丙胺酸、精胺酸、天冬醯胺、半胱胺酸、麩醯胺酸、甘胺酸、組胺酸、異白胺酸、白胺酸、離胺酸、甲硫胺酸、苯基丙胺酸、脯胺酸、絲胺酸、蘇胺酸、色胺酸、酪胺酸、纈胺酸等胺基酸類、甲胺、二甲胺、乙胺、三甲胺、二乙胺、三乙胺、丙胺、異丙胺、二異丙胺等烷基胺類、2-胺基乙醇、二乙醇胺、三乙醇胺、N-甲基乙醇胺、N,N-二甲基乙醇胺等烷醇胺類、乙二胺、二乙三胺、四乙五胺、三(羥基甲基)胺基甲烷、間二甲苯二胺、對二甲苯二胺、1,3-雙(胺基甲基)環己烷等多胺類、牛磺酸等胺基磺酸、2-胺基乙烷硫醇等胺基硫醇類、3-甲基吡啶基胺、3-吡啶甲醇等含氮雜環式化合物類。以有助於鍍敷成長速度之觀點來看,特佳為2-胺基乙醇。
脫脂液為可為市售品,具體而言係列舉可自上村工業股份有限公司取得之ALC-009(包含作為具有胺基之化合物之2-胺基乙醇)、Atotech Japan股份有限公司之Cleaner Securigant 902(包含作為具有胺基之化合物之2-胺基乙醇)等。
以去除鍍敷反應之阻礙物質之觀點來看,脫脂液中之含胺基之化合物之濃度較佳為5mmol/L以上,更佳為10mmol/L以上,又更佳為20mmol/L以上。又,以促進鍍敷反應之觀點來看,較佳為100mmol/L以下,更佳為90mmol/L以下,又更佳為80mmol/L以下。
以有助於鍍敷成長速度之觀點來看,含氧化銅之膜或含銅膜於脫脂液之浸漬時間較佳為1分鐘以上,更佳為2分鐘以上。又,以降低對基材的損傷之觀點來看,較佳為15分鐘以內,更佳為10分鐘以內。以均一脫脂之觀點來看,較佳為在攪拌下浸漬。
為了提高鍍敷之成長速度促進效果,浸漬溫度較佳為15℃以上,更佳為30℃以上,又更佳為40℃以上。又,以降低對基材的損傷之觀點來看,較佳為70℃以下,更佳為60℃以下。
<鍍敷步驟>
本發明之一態樣中,係對於經過或未經過乾燥步驟、還原步驟及/或脫脂步驟之塗布膜(一態樣中為乾燥步驟後之經過或未經過濕式還原步驟及/或脫脂步驟之塗布膜)之含氧化銅之膜或含銅膜進行無電解鍍敷。一態樣中,在含氧化銅之膜未還原下直接進行鍍敷,藉此可提高生產性。無電解鍍敷可還原含氧化銅之膜中之氧化銅的一部分或全部,或可不還原該氧化銅。又,另一態樣中,將還原(例如濕式還原)含氧化銅之膜所得的含銅膜進行無電解鍍敷,藉此可提高導電性。藉由無電解鍍敷而可形成導電性圖案,該導電性圖案係由含有氧化銅及/或其還原物之銅的層及鍍敷層所構成。藉此可製造附導電性圖案之構造體。以圖案應用性範圍之觀點來看,無電解
鍍敷較為有利。鍍敷方法可應用一般的無電解鍍敷法。例如可與脫脂步驟或洗淨步驟一起進行無電解鍍敷。
無電解鍍敷中使用鍍敷液。含氧化銅之膜或含銅膜(尤其是乾燥步驟後作為塗布膜之含氧化銅之膜或含銅膜)容易因外部應力產生剝離,故使鍍敷析出產生不均,若應力集中於一部分,則鍍敷步驟時,有時會產生該含氧化銅之膜或含銅膜的剝離。一態樣中,鍍敷液含有EDTA(乙二胺四乙酸)。EDTA係發揮作為錯合劑功能,而與銅離子形成穩定性高之錯合物,故可抑制鍍敷浴中的副反應,並使浴安定化,可均一進行鍍敷析出,藉此有助於防止含氧化銅之膜或含銅膜的剝離。因此,使用含有EDTA之鍍敷液有助於製造層間密著性優異之附導電性圖案之構造體。又,EDTA在高溫液中亦安定,故在加溫下(例如30℃以上)使用含有EDTA之鍍敷液時,有助於加快鍍敷速度。又,若在進行濕式還原後以含有EDTA(乙二胺四乙酸)之鍍敷液進行鍍敷,則可促進銅鍍敷成長,藉此可提高生產性,故為特佳。以可良好地獲得EDTA的優點之觀點來看,鍍敷液中之EDTA量較佳為7g/L以上、或10g/L以上、或15g/L以上,以降低鍍敷析出物中之雜質並降低電阻之觀點來看,較佳為50g/L以下、或45g/L以下、或40g/L以下。
典型態樣中,鍍敷液係含有銅離子源及還原劑。銅離子源在液中可作為離子存在。例如可一邊進行空氣起泡一邊將含氧化銅之膜或含銅膜浸漬於鍍敷液。鍍敷液中之銅離子係藉由無電解鍍敷而還原,於含氧化銅之膜或含銅膜的表面析出銅,而形成鍍銅層。無電解鍍敷中,含氧化
銅之膜中之氧化銅之一部分或全部可藉由鍍敷液而還原,也可不還原,因此於氧化銅及/或含銅的層上形成鍍銅層。
以提高鍍敷速度之觀點來看,鍍敷液之銅濃度較佳為1.5g/L以上、或1.8g/L以上、或2.0g/L以上,以鍍敷被膜之均一性之觀點來看,較佳為5.0g/L以下、或4.0g/L以下、或3.5g/L以下、或3.0g/L以下。尤其組合濕式還原與鍍敷時,鍍敷液之銅濃度較佳為1.8g/L以上3.5g/L以下。
鍍敷液所含有之銅離子源可舉例如CuSO4、CuCl2、CuCl、CuNO3、Cu3(PO4)2等,以形成密著性優異之鍍敷之觀點來看,較佳為CuCl2及CuSO4。
鍍敷液可含有由甲醛(CH2O)、四氫硼酸鉀、二甲胺硼烷、乙醛酸、及次膦酸所成群組中選擇之1種以上作為還原劑。鍍敷液中之還原劑量較佳為0.1g/L以上、或0.5g/L以上、或1.0g/L以上,較佳為15.0g/L以下、或12.0g/L以下、或9.0g/L以下。
鍍敷液除了EDTA(乙二胺四乙酸)以外可進一步含有額外的錯合劑。額外的錯合劑可舉例如酒石酸鉀鈉、三乙醇胺、硫酸銨、檸檬酸、甘胺酸等。鍍敷液中之額外的錯合劑量較佳為5g/L以上、或7g/L以上、或10g/L以上,較佳為50g/L以下、或45g/L以下、或40g/L以下。
鍍敷液可因應所求而進一步含有界面活性劑。
鍍敷液可為市售品。市售品可使用取自上村工業股份有限公司之SULCUP ELC-SP,取自Meltex股份有限公司之Melplate CU-390、Melplate CU-5100P、取自奧野製藥工業股份有限公司之OPC COPPER
NCA、取自Rohm and Haas股份有限公司之C4500、取自Atotech股份有限公司之PrintganthUPlus、取自日本MacDermid股份有限公司之Cu-510等。
以要求更高速之鍍敷成長來看,鍍敷液所進行無電解鍍敷浴之溫度較佳為25℃以上、或30℃以上、或35℃以上,較佳為80℃以下、或70℃以下、或65℃以下。鍍敷時間較佳為5分鐘以上、或10分鐘以上,較佳為60分鐘以下、或50分鐘以下、或40分鐘以下。
以可流通附導電性圖案之構造體所需的電流之點來看,鍍敷(一態樣中為鍍銅層)之層厚較佳為300nm以上、或500nm以上、或1μm以上、或2μm以上,較佳為100μm以下、或50μm以下、或30μm以下。
一態樣中可在無電解鍍敷後實施電解鍍敷。電解鍍敷可利用一般的電鍍法。例如於含有銅離子之溶液(鍍敷浴)中加入電極及實施鍍敷之對象之導電性基材。接著,由外部直流電源將直流電流施加於電極與導電性基材之間。一態樣中,可於導電性基材上之還原銅層連接冶具(例如夾子)藉此可對還原銅層施加電流,該冶具係與外部直流電源之電極對中的一者連接。其結果可於導電性基材上之還原銅層表面因銅離子的還原而析出銅,並形成鍍銅層。
電解鍍敷浴可使用例如硫酸銅浴、硼氟化銅浴、氰化銅浴、及焦磷酸銅浴。以安全性及生產性之觀點來看,較佳為硫酸銅浴及焦磷酸銅浴。
硫酸銅鍍敷浴適合使用例如含有硫酸銅五水合物、硫酸及氯之硫酸性硫酸銅鍍敷浴。硫酸銅鍍敷浴中之硫酸銅五水合物濃度較佳為
50g/L以上、或100g/L以上,較佳為300g/L以下、或200g/L以下。硫酸濃度較佳為40g/L以上、或80g/L以上,較佳為160g/L以下、或120g/L以下。鍍敷浴之溶媒通常為水。鍍敷浴之溫度較佳為20℃以上、或30℃以上,較佳為60℃以下、或50℃以下。電解處理時之電流密度較佳為1A/dm2以上、或2A/dm2以上,較佳為15A/dm2以下、或10A/dm2以下。
焦磷酸銅鍍敷浴較佳為例如含有焦磷酸銅及焦磷酸鉀之鍍敷浴。焦磷酸銅鍍敷浴中之焦磷酸銅濃度較佳為60g/L以上、或70g/L以上,較佳為110g/L以下、或90g/L以下。焦磷酸鉀濃度較佳為240g/L以上、或300g/L以上,較佳為470g/L以下、或400g/L以下。鍍敷浴之溶媒通常為水。鍍敷浴之pH較佳為8.0以上、或8.2以上,較佳為9.0以下、或8.8以下。為了調整pH值可添加氨水等。鍍敷浴之溫度較佳為20℃以上、或30℃以上,較佳為60℃以下、或50℃以下。電解處理時之電流密度較佳為0.5A/dm2以上、或1A/dm2以上,較佳為10A/dm2以下、或7A/dm2以下。
電解鍍敷用鍍敷浴可進一步含有界面活性劑。
<附導電性圖案之構造體的製造方法之適合例>
以下參照圖2說明附導電性圖案之構造體的製造方法之更具體適合例。
首先於水與丙二醇(PG)的混合溶媒A中溶解乙酸銅B,加入肼C並攪拌(圖2(a))。
接著藉由離心(圖2(b))而將生成物溶液(上清液2a)及氧化亞銅(沉殿物2b)固液分離(圖2(c))。
接著於沉殿物2b加入分散劑D及醇E使沉殿物分散,而得含有氧化銅之分散體(圖2(d))。
接著將含有氧化銅之分散體以噴墨法或凹版印刷法等印刷於基材上(圖2(e))而形成塗布膜,接著乾燥。其結果可於基材1上形成含有氧化銅及分散劑之含氧化銅之膜(氧化銅層)2c(圖2(f))。
接著進行於包含含有胺基之化合物之脫脂液浸漬含氧化銅之膜之脫脂步驟,接著進行鍍敷步驟(圖2(g))。又,可省略脫脂步驟。鍍敷步驟中,氧化銅層中之氧化銅之一部分或全部可被還原。其結果可於基材1上形成氧化銅及/或銅(亦即氧化銅之還原物)的層2d及鍍銅層2e(圖2(h))。
用以上程序而可製造附導電性圖案之構造體。
如上述,根據本揭示之方法可用極低成本且低能量製作導電性層,故可更簡便地製造附導電性圖案之構造體。
<追加層之形成>
本揭示之附導電性圖案之構造體除了前述之基材及導電性層可具有追加層。追加層可舉例如樹脂層及焊料層。
[樹脂層]
一態樣中,較佳為以樹脂層覆蓋部分導電性層。藉由以樹脂層覆蓋部分導電性層,即可防止導電性圖案氧化並提高信賴性。又,導電性層存在未以樹脂層覆蓋之部分,藉此可將零件電性接合。
樹脂層一例為密封材層。樹脂層例如可藉由轉移成型、壓縮成型等而形成。所使用之樹脂可舉例如聚乙烯(PE)、聚丙烯(PP)、聚醯亞胺
(PI)、聚酯(聚對苯二甲酸乙二酯(PET)、聚萘二甲酸乙二酯(PEN)、聚對苯二甲酸丁二酯(PBT)等)、聚醚碸(PES)、聚碳酸酯(PC)、聚乙烯醇(PVA)、聚乙烯縮丁醛(PVB)、聚縮醛(POM)、聚芳酯(PAR)、聚醯胺(PA)(PA6、PA66等)、聚醯胺醯亞胺(PAI)、聚醚醯亞胺(PEI)、聚苯醚(PPE)、改質聚苯醚(m-PPE)、聚苯硫醚(PPS)、聚醚酮(PEK)、聚醚醚酮(PEEK)、聚鄰苯二甲醯胺(PPA)、聚醚腈(PENt)、聚苯并咪唑(PBI)、聚碳二亞胺、聚矽氧聚合物(聚矽氧烷)、聚甲基丙烯醯胺、腈橡膠、丙烯酸橡膠、聚四氟乙烯、環氧樹脂、酚樹脂、三聚氰胺樹脂、脲樹脂、聚甲基丙烯酸甲酯樹脂(PMMA)、聚丁烯、聚戊烯、乙烯/丙烯共聚物、乙烯/丁烯/二烯共聚物、聚丁二烯、聚異戊二烯、乙烯/丙烯/二烯共聚物、丁基橡膠、聚甲基戊烯(PMP)、聚苯乙烯(PS)、苯乙烯/丁二烯共聚物、聚氯乙烯(PVC)、聚偏二氟乙烯(PVDF)、酚酚醛清漆、苯并環丁烯、聚乙烯酚、聚氯芘、聚甲醛、聚碸(PSF)、聚苯基碸樹脂(PPSU)、環烯烴聚合物(COP)、丙烯腈/丁二烯/苯乙烯樹脂(ABS)、丙烯腈/苯乙烯樹脂(AS)、聚四氟乙烯(PTFE)、聚氯三氟乙烯(PCTFE)等。又,樹脂層之厚度較佳為0.1μm以上、或0.5μm以上,較佳為1mm以下、或800μm以下。
在製造後之完成品(附導電性圖案之構造體其本身及含有其之製品)中,密封材層可由外部壓力保護導電性圖案,可提高附導電性圖案之構造體之長期穩定性。
以確保良好的長期穩定性之觀點來看,樹脂層一例之密封材層之透濕度較佳為1.0g/m2/day以下,更佳為0.8g/m2/day以下,又更佳為
0.6g/m2/day以下。藉由降低透濕度而可防止水分從密封材層之外部混入,可抑制導電性圖案氧化。透濕度越低越好。上述透濕度為以杯法測定之值。
即使在製造時有時會使用到的氧阻隔層剝離後,密封材層也可作為對附導電性圖案之構造體賦予氧阻隔功能之功能層。作為其他功能而可具有附導電性圖案之構造體處理時之耐傷性、保護附導電性圖案之構造體不受外界污染之防污性、使用強韌樹脂時提升對附導電性圖案之構造體之剛性等功能。
[焊料層]
一態樣中,較佳為於導電性層之基材側之相反側之一部分形成焊料層。藉由焊料層而可連接導電性層與其他構件。焊料層例如可藉由迴焊法而形成。焊料層可為Sn-Pb系、Pb-Sn-Sb系、Sn-Sb系、Sn-Pb-Bi系、Bi-Sn系、Sn-Cu系、Sn-Pb-Cu系、Sn-In系、Sn-Ag系、Sn-Pb-Ag系、Pb-Ag系等焊料層。焊料層之厚度較佳為0.1μm以上、或0.5μm以上,較佳為2mm以下、或1mm以下。
<導電性圖案構造體的製造套組>
本揭示之一態樣提供一種導電性圖案構造體的製造套組,係含有本揭示之分散體、本揭示之鍍敷液、及本揭示之還原液中的至少2種。該套組有利於簡便地製造層間密著性良好之附導電性圖案之構造體。更具體而言,本揭示之一態樣提供一種導電性圖案構造體的製造套組,係含有由下述所成群組中選擇之至少2種:
包含含有氧化銅的粒子之分散體;
含有EDTA(乙二胺四乙酸)之鍍敷液;及
含有下述式所示甘胺酸化合物之還原液;
(R1)2N-C-COOR2
(式中,R1及R2各自獨立地為氫或一價基,式中之複數個R1可互為相同或相異。)
本揭示之導電性圖案構造體的製造套組可含有之分散體、鍍敷液及還原液個別之較佳構成例係如前述,在此省略說明。導電性圖案構造體的製造套組較佳為含有本揭示之分散體及本揭示之鍍敷液,或含有本揭示之分散液、本揭示之鍍敷液、及本揭示之還原液。
(實施例)
以下藉由實施例及比較例具體地說明本發明,但本發明並不限定於該等實施例。
<評價方法>
[肼定量方法]
藉由標準添加法進行肼之定量。
於樣品(分散體)50μL加入肼33μg、替代性物質(肼15N2H4)33μg、苯甲醛1質量%之乙腈溶液1ml。最後加入磷酸20μL,4小時後進行GC/MS(氣相層析儀/質譜分析)測定。
同樣地於樣品(分散體)50μL加入肼66μg、替代性物質(肼15N2H4)33μg、苯甲醛1質量%之乙腈溶液1ml。最後加入磷酸20μL,4小時後進行GC/MS測定。
同樣地於樣品(分散體)50μL加入肼133μg、替代性物質(肼15N2H4)33μg、苯甲醛1質量%之乙腈溶液1ml。最後加入磷酸20μL,4小時後進行GC/MS測定。
最後於樣品(分散體)50μL中在不加入肼下加入替代性物質(肼15N2H4)33μg、苯甲醛1質量%之乙腈溶液1ml,最後加入磷酸20μL,4小時後進行GC/MS測定。
由上述4個GC/MS測定以m/z=207之層析圖獲得肼之波峰面積值。接著藉由m/z=209之質量層析獲得替代性之波峰面積值。x軸為所添加之肼質量/所添加之替代性物質質量,y軸為肼之波峰面積值/替代性物質之波峰面積值,藉由標準添加法而得校準曲線。
將由校準曲線所得Y截距值除以所添加之肼質量/所添加之替代性物質質量,而得肼之質量。
[測定平均粒徑]
分散體之平均粒徑是使用大塚電子製FPAR-1000藉由累積法而測定。
[測定厚度]
使用觸診式膜厚測定機測定。
裝置:Bruker公司製DektakXT。
Stylus Force:3mg。
Speed:200μm/s。
<實施例1>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有
限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及1-庚醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為36nm。肼量為3000質量ppm。
將所得分散體藉由噴墨印刷於聚醯亞胺(PI)膜(TORAY杜邦公司製Kapton 500H,厚度125μm)印刷。
裝置:DIMATIX Materials Printer DMP-2831。
噴頭:DMC-11610。
電壓:25V。
印刷後,於25℃之大氣下將塗布膜內之溶媒揮發24小時,而得含氧化銅之膜之試料1。所得試料1之膜厚為400nm。
接著將含有EDTA(乙二胺四乙酸)之無電解鍍敷液之奧野製藥工業股份有限公司製OPC COPPER NCA(水溶液、鍍敷浴中的EDTA量約為2.6質量%)加溫至60℃,將試料1浸漬30分鐘。處理後取出試料水洗。水洗後以四端點法測定本試料之電阻值為80μΩ‧cm。處理後之試料厚度為1000nm,鍍敷層之厚度為600nm。可確認銅之鍍敷生長。
<實施例2>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及1-庚醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為36nm。肼量為3000質量ppm。
於PET膜(東洋紡股份有限公司製COSMOSHINE A4100,厚度100μm)滴入Colcoat PX(Colcoat股份有限公司製)1mL,以1500rpm旋轉塗布50秒。其後以100℃之烘箱乾燥30分鐘,而得附塗布層(厚度50nm之密著層)之PET膜。
將上述分散體藉由噴墨印刷於上述附塗布層之PET膜印刷。
裝置:DIMATIX Materials Printer DMP-2831。
噴頭:DMC-11610。
電壓:25V。
印刷後,於25℃之大氣下將塗布膜內之溶媒揮發24小時,而得含氧化銅之膜之試料2。所得試料2之膜厚為400nm。
接著將無電解鍍敷液之奧野製藥工業股份有限公司製OPC COPPER NCA加溫至60℃,將試料2浸漬30分鐘。處理後取出試料水洗。水洗後以四端點法測定本試料之電阻值為93μΩ‧cm。處理後之試料厚度為800nm,鍍敷層之厚度為400nm。可確認銅之鍍敷生長。
<實施例3>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及1-庚醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為36nm。肼量為3000質量ppm。
將所得分散體藉由噴墨印刷於聚醯亞胺膜(TORAY杜邦公司製Kapton 500H,厚度125μm)印刷。
裝置:DIMATIX Materials Printer DMP-2831。
噴頭:DMC-11610。
電壓:25V。
印刷後,於25℃之大氣下乾燥24小時揮發塗布膜內之溶媒,而得含氧化銅之膜之試料3。所得試料3之膜厚為200nm。
將N,N-二(2-羥基乙基)甘胺酸溶解於水而調製32質量%之溶液。將其使用作為還原液,於加熱至80℃之狀態之該還原液浸漬上述含氧化銅之膜5分鐘。其後以乙醇洗淨而得銅膜。
接著將無電解鍍敷液之奧野製藥工業股份有限公司製OPC COPPER NCA加溫至60℃,將試料浸漬30分鐘。處理後取出試料水洗。水洗後以四端點法測定本試料之電阻值為12μΩ‧cm。處理後之試料厚度為1500nm,鍍敷層之厚度為1300nm。可確認銅鍍敷生長。
<實施例4>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及1-庚醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為30nm。肼量為3000質量ppm。
將所得分散體以旋轉塗布法塗布於聚醯亞胺膜(TORAY杜邦公司製Kapton 500H,厚度125μm),於25℃之大氣下乾燥24小時揮發塗布膜內之溶媒,而得含氧化銅之膜之試料4。所得試料4之膜厚為1200nm。
將N,N-二(2-羥基乙基)甘胺酸溶解於水而調製16質量%之溶液。將其使用作為還原液,於加熱至73℃之狀態之該還原液浸漬上述含氧化銅之膜10分鐘。其後以水洗淨而得銅膜。
將鍍敷之前處理液之上村工業股份有限公司製ACL-009以成為50mL/L之方式溶解於水,而得處理液。於加溫至50℃之該處理液將試料4浸漬5分鐘。處理後取出試料水洗。接著將無電解鍍敷液之奧野製藥工業股份有限公司製OPC COPPER NCA加溫至60℃,將試料浸漬30分鐘。處理後取出試料水洗。水洗後以四端點法測定本試料之電阻值為36μΩ‧cm。處理後之試料厚度相較於鍍敷處理前成長7200nm。可確認銅之鍍敷並生長。
<實施例5>
N,N-二(2-羥基乙基)甘胺酸水溶液之溫度為60℃,除此之外以與實施例4相同方式而得試料5。以四端點法測定本試料之電阻值為19μΩ‧cm。處理後之試料厚度相較於鍍敷處理前生長8200nm。可確認銅之鍍敷並生長。
<實施例6>
於N,N-二(2-羥基乙基)甘胺酸水溶液浸漬含氧化銅之膜之時間為5分鐘,除此之外以與實施例5相同方式而得試料6。以四端點法測定本試料
之電阻值為21μΩ‧cm。處理後之試料厚度相較於鍍敷處理前生長8200nm。可確認銅之鍍敷生長。
<實施例7>
N,N-二(2-羥基乙基)甘胺酸水溶液之濃度為8質量%、N,N-二(2-羥基乙基)甘胺酸水溶液之溫度為73℃,除此之外以與實施例6相同方式而得試料7。以四端點法測定本試料之電阻值為13μΩ‧cm。處理後之試料厚度相較於鍍敷處理前生長9600nm。可確認銅之鍍敷生長。
<實施例8>
於N,N-二(2-羥基乙基)甘胺酸水溶液浸漬含氧化銅之膜之時間為10分鐘,除此之外以與實施例7相同方式而得試料8。以四端點法測定本試料之電阻值為10μΩ‧cm。處理後之試料厚度相較於鍍敷處理前生長9600nm。可確認銅之鍍敷+生長。
<實施例9>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及1-庚醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為28nm。肼量為3000質量ppm。
將所得分散體以旋轉塗布法塗布於聚醯亞胺膜(TORAY杜邦公司製Kapton 500H,厚度125μm),於25℃之大氣下乾燥24小時揮發塗布膜內之溶媒,而得含氧化銅之膜之試料9。所得試料9之膜厚為500nm。
將檸檬酸溶解於水並調製24質量%之溶液。將其使用作為還原液,於加熱至60℃之狀態之該還原液將上述含氧化銅之膜浸漬5分鐘。其後以水洗淨而得銅膜。
將鍍敷之前處理液之上村工業股份有限公司製ACL-009以成為50mL/L之方式溶解於水,而得處理液。於加溫至50℃之該處理液將試料9浸漬5分鐘。處理後取出試料水洗。接著將無電解鍍敷液之奧野製藥工業股份有限公司製OPC COPPER NCA加溫至60℃,將試料浸漬30分鐘。處理後取出試料水洗。水洗後,處理後之試料厚度相較於鍍敷處理前生長1300nm。以四端點法測定本試料之電阻值為13μΩ‧cm。可確認銅之鍍敷生長。
<實施例10至13>
(噴墨適性之評價)
將分散體之溶媒變更為丁醇(實施例10)、己醇(實施例11)、庚醇(實施例12)、或辛醇(實施例13),除此之外以與實施例1相同程序調製分散體(印墨)。對所得印墨評價噴墨之間歇穩定性。測量進行間歇吐出時到噴嘴產生堵塞為止的時間,以1小時以上為A、30分鐘以上且未滿1小時為B、未滿30分鐘為C的方式評價。間歇穩定性之評價條件如下。
裝置:DIMATIX Materials Printer DMP-2831。
噴頭:DMC-11610。
電壓:25V。
吐出噴嘴數:7(No.5至11)。
有無吐出之判斷:以DropWatcher目視。
丁醇溶媒之印墨為評價C,己醇溶媒之印墨為評價B,庚醇溶媒之印墨及辛醇溶媒之印墨為評價A。由該等結果可知以庚醇或辛醇為溶媒之印墨的噴墨適性良好。
<比較例1>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫使成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及乙醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為21nm。肼量為3000質量ppm。
將所得分散體以旋轉塗布法塗布於聚醯亞胺膜(TORAY杜邦公司製Kapton 500H,厚度125μm),在大氣下100℃之烘箱加熱1小時
並揮發塗布膜內之溶媒,而得含氧化銅之膜之試料10。所得試料10之膜厚為1100nm。
接著,作為鍍敷之前處理液而混合月桂基硫酸鈉(4.9質量%)、2-胺基乙醇(4.9質量%)、甘胺酸(4.9質量%)、二乙三胺(2.4質量%)、及水(82.9質量%),其後以水稀釋為20倍體積,而得處理液。於加溫至50℃之該處理液將試料10浸漬5分鐘。處理後取出試料水洗。接著,無電解鍍敷液含有硫酸銅(Cu為2.5g/L)、酒石酸鉀鈉(16g/L)、福馬林(HCHO為10g/L)、2,2-聯吡啶(10mg/L)、聚乙二醇(PEG)(100mg/L)、及氫氧化鈉水溶液(添加至pH成為12為止),將該液加溫至60℃,將試料浸漬30分鐘。處理後取出試料水洗。觀察試料,所形成之含氧化銅之膜皆剝離,無法確認到銅之鍍敷生長。
<比較例2>
於鍍敷液加入硫酸鎳0.5g/L,除此之外以與比較例1相同方式而得試料11。觀察試料,所形成之含氧化銅之膜皆剝離,無法確認到銅之鍍敷生長。
<比較例3>
作為鍍敷之前處理而混合硫酸(36質量%)、乙二醇(4.3質量%)、聚氧伸乙基月桂基醚(1.7質量%)、水(58質量%),將該混合液體以水稀釋為10倍體積並加溫至40℃,將試料浸漬5分鐘,除此之外以與比較例1相同方式而得試料12。觀察試料,所形成之含氧化銅之膜皆剝離,無法確認到銅之鍍敷生長。
<比較例4>
於蒸餾水(共榮製藥股份有限公司製)7560g、1,2-丙二醇(關東化學股份有限公司製)3494g之混合溶媒中溶解乙酸銅(II)一水合物(關東化學股份有限公司製)806g,以外部溫度控制器使液溫成為-5℃。花費20分鐘加入肼一水合物(東京化成工業股份有限公司製)235g,在氮環境下攪拌30分鐘後,以外部溫度控制器使液溫成為25℃,在氮環境下攪拌90分鐘。攪拌後以離心分離上清液及沉殿物。於所得沉殿物390g加入DISPERBYK-145(BYK-Chemie製)(酸價:76mgKOH/g、胺價:71mgKOH/g之含磷有機物)13.7g(分散劑含量4g)、及1-庚醇(關東化學股份有限公司製)907g,在氮環境下使用均質機分散,而得含有氧化亞銅之分散體1365g。
分散體良好地分散,平均粒徑為30nm。肼量為3000質量ppm。
將所得分散體以噴霧法塗布於聚醯亞胺膜(TORAY杜邦公司製Kapton 500H,厚度125μm),於25℃之大氣下乾燥24小時揮發塗布膜內之溶媒,而得含氧化銅之膜之試料13。所得試料之膜厚為200nm。
將N,N-二(2-羥基乙基)甘胺酸溶解於水而調製16質量%之溶液。將其使用作為還原液,於加熱至73℃之狀態之該還原液將上述含氧化銅之膜浸漬30分鐘。其後以水洗淨而得銅膜。
接著,作為鍍敷之前處理液而混合月桂基硫酸鈉(4.9質量%)、2-胺基乙醇(4.9質量%)、甘胺酸(4.9質量%)、二乙三胺(2.4質量%)、及水(82.9質量%),其後以水稀釋為20倍體積,而得處理液。於加溫至50℃之該處理液將試料13浸漬5分鐘。處理後取出試料水洗。接著,無電解鍍敷液含有硫酸銅(Cu為2.5g/L)、酒石酸鉀鈉(16g/L)、福馬林(HCHO為
10g/L)、2,2-聯吡啶(10mg/L)、聚乙二醇(PEG)(100mg/L)、及氫氧化鈉水溶液(添加至pH成為12為止),將該液加溫至60℃,將試料浸漬30分鐘。處理後取出試料水洗。觀察試料,所形成之含氧化銅之膜皆剝離,無法確認到銅之鍍敷生長。
<綜合評價>
以導電性能之觀點來看,電阻值係以低者為佳。又,以生產性之觀點來看,鍍敷之生長速度係以快者為佳。電阻值以未滿15μΩ‧cm為3分、15μΩ‧cm以上且未滿50μΩ‧cm為2分、50μΩ‧cm以上為1分的方式評價。又,鍍敷生長膜厚以未滿1000nm為1分、1000nm以上且未滿5000nm為2分、5000nm以上為3分的方式評價。此外將電阻值之評價分數及鍍敷生長膜厚之評價分數的總和作為總評價分數。結果呈示於表1。
又,本發明並不限定於上述實施型態或實施例。根據所屬技術領域中之一般知識者可將上述實施型態或實施例施行設計變更等,又,可任意組合上述實施型態或實施例,但施行該等變更等之態樣亦包含於本發明之範圍。
(產業上之可利用性)
本發明之一態樣可適合用於製造印刷配線板、電子裝置、電磁波屏蔽、抗靜電膜等。
1:基材
2a:上清液
2b:沉殿物
2c:含氧化銅之膜
2d:氧化銅及/或銅的層
2e:鍍銅層
A:混合溶媒
B:乙酸銅
C:肼
D:分散劑
E:醇
Claims (19)
- 一種附導電性圖案之構造體的製造方法,係包含下述步驟:塗布膜形成步驟,將包含含有氧化銅的粒子之分散體印刷於基材而得塗布膜;鍍敷步驟,於前述塗布膜使用鍍敷液進行無電解鍍敷;前述鍍敷液係含有EDTA(乙二胺四乙酸)。
- 如請求項1所述之附導電性圖案之構造體的製造方法,其中在前述鍍敷步驟之前進一步包含還原步驟。
- 如請求項2所述之附導電性圖案之構造體的製造方法,其中前述還原步驟為濕式還原步驟。
- 如請求項2或3所述之附導電性圖案之構造體的製造方法,其中前述還原步驟係包含於含有下述式所示之甘胺酸化合物之溶液中浸漬前述塗布膜者,(R1)2N-C-COOR2(式中,R1及R2各自獨立地為氫或一價基,式中之複數個R1可互為相同或相異。)
- 如請求項4所述之附導電性圖案之構造體的製造方法,其中前述甘胺酸化合物為N,N-二(2-羥基乙基)甘胺酸。
- 如請求項4所述之附導電性圖案之構造體的製造方法,其中前述溶液為水溶液,前述甘胺酸化合物之濃度為1質量%以上50質量%以下。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中在前述鍍敷步驟之前進一步包含脫脂步驟。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述塗布膜形成步驟係藉由噴墨印刷而進行。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中在前述塗布膜形成步驟與前述鍍敷步驟之間進一步包含乾燥前述塗布膜之乾燥步驟。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述分散體係包含含有磷酸酯之分散劑。
- 如請求項10所述之附導電性圖案之構造體的製造方法,其中前述分散劑之酸價(mgKOH/g)為20以上130以下。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述分散體係含有還原劑,前述還原劑為肼。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述分散體係含有由1-己醇、1-庚醇、及1-辛醇所成群組中選擇之1種以上的分散媒。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述含有氧化銅的粒子之平均粒徑為1nm以上100nm以下。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述鍍敷液係含有銅離子源及還原劑。
- 如請求項15所述之附導電性圖案之構造體的製造方法,其中前述銅離子源為由CuSO4、CuCl2、CuCl、CuNO3、及Cu3(PO4)2所成群組中選擇之1種以上。
- 如請求項15所述之附導電性圖案之構造體的製造方法,其中前述還原劑為由甲醛、四氫硼酸鉀、二甲胺硼烷、乙醛酸、及次膦酸所成群組中選擇之1種以上。
- 如請求項1至3中任一項所述之附導電性圖案之構造體的製造方法,其中前述基材係具有密著層,在前述塗布膜形成步驟中,將前述分散體印刷於前述密著層。
- 一種導電性圖案構造體的製造套組,係含有由下述所成群組中選擇之至少2種:包含含有氧化銅的粒子之分散體;含有EDTA(乙二胺四乙酸)之鍍敷液;及含有下述式所示甘胺酸化合物之還原液;(R1)2N-C-COOR2(式中,R1及R2各自獨立地為氫或一價基,式中之複數個R1可互為相同或相異。)
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