TW201617479A - Process to produce an electrically conductive structure and a carrier material produced by this process - Google Patents

Process to produce an electrically conductive structure and a carrier material produced by this process Download PDF

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TW201617479A
TW201617479A TW104133359A TW104133359A TW201617479A TW 201617479 A TW201617479 A TW 201617479A TW 104133359 A TW104133359 A TW 104133359A TW 104133359 A TW104133359 A TW 104133359A TW 201617479 A TW201617479 A TW 201617479A
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metal
metallization
additive
catalytically active
carrier material
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TW104133359A
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羅賓 亞烈山大 庫依格
伯恩 羅斯那
瑪爾特 凡樂
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Ｌｐｋｆ雷射暨電子股份公司
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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
    • C23C18/1603—Process or apparatus coating on selected surface areas
    • C23C18/1607—Process or apparatus coating on selected surface areas by direct patterning
    • C23C18/1608—Process or apparatus coating on selected surface areas by direct patterning from pretreatment step, i.e. selective pre-treatment
    • 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
    • C23C18/1603—Process or apparatus coating on selected surface areas
    • C23C18/1607—Process or apparatus coating on selected surface areas by direct patterning
    • C23C18/1612—Process or apparatus coating on selected surface areas by direct patterning through irradiation means
    • 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
    • C23C18/1635—Composition of the substrate
    • C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
    • C23C18/1641—Organic substrates, e.g. resin, plastic
    • 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
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
    • C23C18/2026—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by radiant energy
    • C23C18/204—Radiation, e.g. UV, laser
    • 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
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/28—Sensitising or activating
    • C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
    • H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
    • H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
    • H05K3/182—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating characterised by the patterning method
    • H05K3/185—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating characterised by the patterning method by making a catalytic pattern by photo-imaging
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/0313—Organic insulating material
    • H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
    • H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
    • H05K2201/0206—Materials
    • H05K2201/0236—Plating catalyst as filler in insulating material
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/09—Shape and layout
    • H05K2201/09009—Substrate related
    • H05K2201/09118—Moulded substrate
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/10—Using electric, magnetic and electromagnetic fields; Using laser light
    • H05K2203/107—Using laser light

Abstract

The invention relates to a method for producing an electrical conductive structure, in particular a conductor path, on a non-conductive support material which contains an additive having at least one metal compound. Said support material is at least partially exposed to electromagnetic radiation in order to activate the metal compounds contained in the additive, catalytically active germs thus forming in the activated areas with respect to an external, currentless metallization, said germs generating the electrically conductive structure on the non-conductive support material. During the method and prior to metallization, in order to efficiently and economically increase the proportion and the activity of the catalytically active germs, at least one part of the germs in the activated areas is substituted by a chemical exchange reaction by means of at least one catalytically active metal as an exchange metal. Also, the metallization takes place on the exchange metal and the optionally remaining, catalytically active germs in an external currentless metallization bath. As a result, in particular all two-step metallization processes become superfluous due to the fact that the claimed essentially increased catalytic activity allows a simple and fast metallization. The claimed method is suitable, preferably, also for plastic materials as support material which display a lower metallization suitability.

Description

製造導電構造的方法及用此方法製造的載體材料 Method for manufacturing a conductive structure and carrier material produced by the method

本發明係有關於一種在包含具至少一金屬化合物之添加劑的非導電載體材料上製造導電構造，特別是導電通路的方法，其中使得該載體材料局部承受電磁輻射，以便將該添加劑中所包含的金屬化合物活化，從而在如此活化之區域內，針對隨後的無外流的金屬化操作構成若干具催化活性的晶種，其在該非導電載體材料上產生該導電構造。 The present invention relates to a method of making a conductive structure, particularly a conductive path, on a non-conductive support material comprising an additive having at least one metal compound, wherein the support material is locally exposed to electromagnetic radiation so as to be included in the additive The metal compound is activated such that in the region of such activation, a plurality of catalytically active seed crystals are formed for subsequent subsequent outflow metallization operations which produce the electrically conductive structure on the non-conductive support material.

在實踐中，名為MID(Molded Interconnected Device)的立體模塑互聯器件已為吾人所知並被廣泛應用。MID工藝將電氣功能與機械功能集於一個構件中。舉例而言，將導電構造整合在殼體中，以此作為對傳統的印刷電路板工藝的補充，目的在於減小重量、結構空間及安裝成本。 In practice, a three-dimensional molded interconnect device called MID (Molded Interconnected Device) is known and widely used. The MID process combines electrical and mechanical functions into one component. For example, a conductive construction is integrated into the housing as a complement to conventional printed circuit board processes with the goal of reducing weight, construction space, and installation costs.

其中對所謂“雷射直接成型(LDS)”而言，上述工藝尤其具有意義。採用LDS方法時，在包含具特殊添加劑之塑膠顆粒的單組分注塑料中，將載體材料注塑成成型件。藉由雷射，能夠以選擇特定位置的方式在物理化學反應中將此等添加劑轉化成催化生效的晶種，其中在隨後的化學金屬化浴中，針對性地在經上述處理之部位上沈積金屬。 Among the so-called "laser direct structuring (LDS)", the above process is particularly meaningful. In the case of the LDS method, the carrier material is injection molded into a molded part in a one-component injection molding plastic containing plastic particles having a special additive. By means of laser, it is possible to convert these additives into catalytically active seed crystals in a physicochemical reaction in a manner that selects a specific position, in which a subsequent deposition in the chemical metallization bath is carried out in a targeted manner. metal.

由於透過電腦軟體對承受雷射輻射的區域進行控制，在採用 LDS方法時，能夠在最短的時間內對電路佈局進行調整或修改，而毋需對工具進行改造。以此為基礎，且基於市售的各種具LDS能力的塑膠，LDS方法最終成為MID製造領域中的領先工藝。 Due to the control of the area exposed to laser radiation through computer software, In the LDS method, the circuit layout can be adjusted or modified in the shortest time without the need to modify the tool. Based on this and based on commercially available LDS-capable plastics, the LDS method has finally become the leading technology in the MID manufacturing field.

在實踐中，應用此工藝所帶來的成本為決定性因素。其中事實證明，在LDS-MID工藝的總製造成本中，需在最後步驟中實施的金屬化操作占主要部分。在將此金屬化成本與居主要競爭地位的MID製造方法進行直接對比時，事實證明，由於表面之絕對催化活性較低，LDS-MID之金屬化操作會造成更高的成本。因此，此LDS工藝特別是針對需要較高操作靈活性的應用。特定言之，為增強此LDS方法對更大批量之生產的吸引力，需要降低金屬化成本。 In practice, the cost of applying this process is a decisive factor. It turns out that in the total manufacturing cost of the LDS-MID process, the metallization operation to be carried out in the final step is the main part. When this metallization cost is directly compared with the main competitive MID manufacturing method, it has been proved that the metallization operation of LDS-MID causes higher cost due to the lower absolute catalytic activity of the surface. Therefore, this LDS process is especially targeted at applications that require higher operational flexibility. In particular, to enhance the appeal of this LDS approach to larger batch production, there is a need to reduce metallization costs.

在實施雷射直接成型時，通常透過化學還原式銅沈積來構建整個金屬化層之主要部分。在此銅塗層後，通常對表面進行精整。例如將銅、鎳及金用作標準層系統，其中在銅塗層後，以化學還原的方式沈積鎳，以及例如在浴過程(Sudprozess)中沈積金。在此，銅之典型層厚為8μm，鎳為4μm，金為0.1μm。 In the direct laser forming process, a major portion of the entire metallization layer is typically constructed by chemical reduction copper deposition. After this copper coating, the surface is usually finished. For example, copper, nickel and gold are used as standard layer systems in which nickel is deposited in a chemically reduced manner after copper coating, and gold is deposited, for example, in a bath process (Sudprozess). Here, the typical layer thickness of copper is 8 μm, nickel is 4 μm, and gold is 0.1 μm.

根據所採用的化學組成，區分一級與二級過程。在二級過程中，針對起始金屬化操作採用銅置換浴，針對銅增強操作採用全構建銅浴(Full-Build-Kupfer-Bad)。特定言之，在將LDS方法應用於塑膠，如PC及PC/ABS共混物，以及其他因金屬化適性較低而需要專門匹配之金屬化浴的其他塑膠時，便採用上述方案。 The primary and secondary processes are differentiated according to the chemical composition employed. In the secondary process, a copper displacement bath was used for the initial metallization operation and a fully constructed copper bath (Full-Build-Kupfer-Bad) was used for the copper enhancement operation. In particular, the above approach is used when applying the LDS method to plastics, such as PC and PC/ABS blends, and other plastics that require a specially matched metallization bath due to low metallization.

經證實，以下方案適用於實踐：首先在約60℃之溫度下，在具極高化學反應能力的置換浴中，藉由金屬化產生厚度約為2-3μm的層 結構，隨後在全構建浴中繼續構建此層結構，直至達到所期望的層厚度。通常而言，僅此二級過程的成本便占MID之總製造成本的近50%，因為與更為穩定的浴相比，具較高反應能力的置換浴的壽命更短，且所採用的化學品的效率更低。因此，與全構建浴相比，藉由置換浴構建的層結構的成本大幅提昇。 It has been confirmed that the following scheme is suitable for practice: firstly, a layer having a thickness of about 2-3 μm is formed by metallization in a displacement bath having a very high chemical reactivity at a temperature of about 60 ° C. The structure is then continued to build this layer structure in the full build bath until the desired layer thickness is reached. In general, the cost of this secondary process alone accounts for nearly 50% of the total manufacturing cost of the MID because the life of the replacement bath with higher reactivity is shorter compared to the more stable bath. Chemicals are less efficient. Therefore, the cost of the layer structure constructed by the displacement bath is greatly increased compared to the full construction bath.

眾所周知，因金屬化合物之雷射活化過程中的還原，晶種包含金屬元素、金屬氧化物及其他具不同氧化態的不均一金屬化合物，其中含銅的氧化物LDS添加劑例如含有75%的銅氧化物及25%的銅元素。 It is well known that due to reduction during laser activation of a metal compound, the seed crystal contains metal elements, metal oxides and other heterogeneous metal compounds having different oxidation states, wherein the copper-containing oxide LDS additive contains, for example, 75% copper oxide. And 25% copper.

EP 2 581 469 A1係有關於進一步改進LDS方法的方案，其特別是針對由PA、PU、ABS、PC、PET、PBT、LCP或PPA構成之載體材料。此案提出，在實施金屬化操作前，藉由一溶液對先前經雷射成型之載體材料進行處理，該溶液含有能斯特電位E°≦0.35V且具較強還原能力的物質，即活潑性高於銅的物質。採用具此種能斯特電位之物質有兩個目的。一個目的在於，防止此等物質自身將銅晶種氧化，因為此等銅晶種為用於化學還原式銅沈積的、具催化活性的晶種，以及，需要防止此等銅晶種因其他物質(例如空氣中的氧)而發生氧化。另一方面，自熱力學的角度看來，此等物質具有將銅氧化物的一部分還原成具催化活性的銅晶種的潛力。亦即，EP 2 581 469 A1之目的在於，透過化學還原過程提高銅元素的量，並將其保持在較高水平，從而對無外流之銅浴中的金屬化傾向產生正面影響。 EP 2 581 469 A1 relates to a further improvement of the LDS process, in particular for carrier materials consisting of PA, PU, ABS, PC, PET, PBT, LCP or PPA. In this case, it is proposed that the previously laser-formed carrier material is treated by a solution containing a substance having a strong potential of E. ≦ 0.35 V and having a strong reducing ability, that is, lively, before the metallization operation is carried out. A substance that is higher in nature than copper. The use of a substance having such a Nernst potential has two purposes. One purpose is to prevent such substances from oxidizing the copper seed itself, since these copper seeds are catalytically active seed crystals for chemical reduction copper deposition, and it is necessary to prevent such copper crystal species from being caused by other substances. Oxidation occurs (for example, oxygen in the air). On the other hand, from a thermodynamic point of view, such materials have the potential to reduce a portion of the copper oxide to a catalytically active copper seed. That is, the purpose of EP 2 581 469 A1 is to increase the amount of copper element through a chemical reduction process and maintain it at a high level, thereby having a positive influence on the metallization tendency in the copper bath without outflow.

DE 198 33 593 A1係有關於對基板表面進行選擇性金屬化的方法，其中對表面進行預處理，使得此表面具有預設之粗糙度。在此等區 域內，局部地為基板配設晶種，透過化學金屬沈積沿晶種軌跡對此等晶種進行增強。將銅、銀、金、鎳或鈀用作成核材料，在化學金屬沈積開始前，透過交換反應將此等材料替換為具更低電化學活潑性的金屬。如此便能增強金屬之催化活性。 DE 198 33 593 A1 relates to a method for selective metallization of a substrate surface, wherein the surface is pretreated such that the surface has a predetermined roughness. In this area Within the domain, seed crystals are locally disposed on the substrate, and the seed crystals are reinforced along the seed track by chemical metal deposition. Copper, silver, gold, nickel or palladium is used as a nucleating material, and these materials are replaced by metals having a lower electrochemical activity by an exchange reaction before the start of chemical metal deposition. This enhances the catalytic activity of the metal.

EP 1 870 491 A1描述過一種經改進的，對不導電之基板表面，特別是對聚亞胺表面進行直接金屬化的方法。 EP 1 870 491 A1 describes an improved method for the direct metallization of non-conducting substrate surfaces, in particular polyimine surfaces.

DE 10 2011 000 138 A1公開過一種對主要材料為含添加劑之塑膠的基板進行選擇性金屬化的方法，其中在待金屬化的區域內，藉由燒蝕法將基板之接近表面的層移除。其中將塑膠體浸入含鈀的溶液。 DE 10 2011 000 138 A1 discloses a method for the selective metallization of a substrate whose main material is an additive-containing plastic, wherein the layer close to the surface of the substrate is removed by ablation in the region to be metallized . The plastic body is immersed in a solution containing palladium.

本發明之目的在於，以某種方式實施該方法，從而在實施金屬化操作前，高效且低成本地增大該等催化生效之晶種的比率及活性。 It is an object of the present invention to carry out the process in a manner that increases the ratio and activity of the catalytically active seed crystals efficiently and at low cost prior to performing the metallization operation.

本發明用以達成上述目的之解決方案為一種具申請專利範圍第1項之特徵的方法。本發明之其他設計方案參閱附屬項。 The solution of the present invention for achieving the above object is a method having the features of claim 1 of the patent application. Other design schemes of the present invention are referred to the dependent items.

亦即，根據本發明之方法，在該等經活化之區域內，藉由化學交換反應，將該等無催化活性之晶種的至少一部分替換為用作交換金屬的、具催化活性的金屬，以及，在無外流之金屬化浴中，在該交換金屬上以及在視情況保留的具催化活性的晶種上進行金屬化。藉此便毋需採用二級金屬化過程，特別是毋需採用置換浴，因為本發明之大幅增強的催化活性能夠簡單且快速地實現金屬化。因此，本發明之方法較佳亦適用於用作載體材料且具較小之金屬化傾向的塑膠。 That is, according to the method of the present invention, at least a portion of the catalytically inactive seed crystals are replaced by catalytically active metals used as exchange metals by chemical exchange reactions in the activated regions. And, in a metallization bath without an outflow, metallization is carried out on the exchange metal and on the catalytically active seed crystals which are optionally retained. There is a need for a secondary metallization process, in particular a need for a displacement bath, since the greatly enhanced catalytic activity of the present invention enables metallization to be achieved simply and quickly. Accordingly, the method of the present invention is preferably also applicable to plastics which are used as carrier materials and which have a lower tendency to metallize.

其中，藉由該交換反應，可僅將該等無催化活性之晶種替換 為用作交換金屬的、具催化活性的金屬。但根據一種尤佳方案，不僅對該還原級(0)，即金屬元素進行交換，亦對氧化數(1)之晶種，特別是氧化物進行交換，從而整體上顯著增強催化活性。 Wherein, by the exchange reaction, only the non-catalytic seed crystals can be replaced It is a catalytically active metal used as an exchange metal. According to a preferred embodiment, however, not only the reduction stage (0), ie the metal element, but also the seed crystals of the oxidation number (1), in particular the oxide, are exchanged, so that the catalytic activity is significantly enhanced overall.

本發明意外發現，在以與圖1所示方程式1相似的方式，將該等銅晶種替換為具催化活性之物質(例如鈀)的情況下，與純粹的交換相比，能夠針對化學金屬化大幅增強表面之活性。方程式1及所有其他化學反應方程式皆係粗略反應方程式，其僅用於對特定事實進行闡釋，並不要求將參與該反應之所有反應物皆包含在內，亦不能用於推斷出機理。 The present inventors have unexpectedly discovered that in the case of replacing such copper seeds with catalytically active species (e.g., palladium) in a similar manner to Equation 1 of Figure 1, it is possible to target chemical metals as compared to pure exchange. It greatly enhances the activity of the surface. Equation 1 and all other chemical reaction equations are rough reaction equations that are only used to explain specific facts and do not require that all reactants involved in the reaction be included or used to infer the mechanism.

進一步的研究顯示，藉由該方法，亦能夠根據圖1所示方程式2，在包含經活化之表面的氧化(亞)銅晶種上增大晶種數目。 Further studies have shown that by this method it is also possible to increase the number of seed crystals on the oxidized (sub)copper seed crystal containing the activated surface according to Equation 2 shown in FIG.

特定言之，此意外結果對該方法特別有利，因為在空氣中的雷射成型特別是會產生諸如Cu2O的銅氧化物，其不具催化活性，故先前無法將其用作無外流之金屬沈積中的晶種。 In particular, this unexpected result is particularly advantageous for this method, since laser formation in air, in particular, produces copper oxides such as Cu 2 O, which are not catalytically active and therefore have not previously been used as metals without outflow. Seed crystals in the deposit.

該反應在室溫下發生，故本發明原則上可應用於所有塑膠。隨後在該交換金屬上透過習知之金屬化操作進行層構建，其中當然亦可多次實施交換反應，特定言之，亦可再次替換為具更高催化活性之金屬。 The reaction takes place at room temperature, so the invention is in principle applicable to all plastics. Layer formation is then carried out on the exchange metal by conventional metallization operations, wherein of course the exchange reaction can be carried out multiple times, in particular, it can be replaced again with a metal having a higher catalytic activity.

該方法之另一優點在於，在實施該金屬交換後，可選擇先前無法實現之起始金屬化操作。舉例而言，可在金屬化浴中藉由鎳實現金屬化，除其他組分外，該金屬化浴包含用作金屬源之鎳離子及用作還原劑之次磷酸鈉。無法透過銅晶種使用此類金屬化浴，需要採用具更高活性的晶種(通常為鈀)。 Another advantage of this method is that after the metal exchange is performed, an initial metallization operation that was previously unachievable can be selected. For example, metallization can be achieved by nickel in a metallization bath containing, among other components, nickel ions used as a source of metal and sodium hypophosphite used as a reducing agent. The inability to use such metallization baths through copper seeds requires the use of more active seed crystals (usually palladium).

儘管該交換反應毋需其他外部能量輸入，但舉例而言，亦可 根據塑膠藉由熱處理及/或藉由超音波處理來改進或加快此交換反應。研究顯示，在採用處於較寬頻率及強度範圍內的超音波時，對該交換反應之速度及均勻度特別有利。 Although the exchange reaction does not require other external energy input, for example, This exchange reaction is improved or accelerated by heat treatment according to the plastic and/or by ultrasonic treatment. Studies have shown that the speed and uniformity of the exchange reaction is particularly advantageous when using ultrasonic waves over a wide range of frequencies and intensities.

特定言之，除交換反應加快外，本發明意外發現，該方法對該雷射成型之操作窗亦具有正面影響。因此，就以傳統方式實施LDS過程時在雷射成型中無法充分活化(能量輸入過少)或嚴重受損(能量輸入過多)的表面而言，藉由該方法便能順利實現對此等表面的金屬化。此情形對該方法之可靠性極有幫助，因為錯誤實施的雷射成型不一定會導致大量的次品。因此，該方法能夠提高雷射直接成型之容錯性，故在經濟性與生態性方面比競爭對手更具優勢。 In particular, in addition to the accelerated exchange reaction, the present inventors have unexpectedly discovered that the method also has a positive impact on the operating window of the laser forming. Therefore, in the conventional implementation of the LDS process, in the case of a surface that cannot be sufficiently activated (too little energy input) or severely damaged (too much energy input) in laser forming, the surface can be smoothly realized by this method. Metalization. This situation is extremely helpful for the reliability of the method, as falsely implemented laser forming does not necessarily result in a large number of defective products. Therefore, the method can improve the fault tolerance of laser direct molding, so it is more advantageous than the competition in terms of economy and ecology.

研究中發現的另一優點在於，就各種塑膠之金屬化傾向而言，該方法具有平均化作用。與採用諸如聚醯胺之塑膠的情形相比，在採用諸如聚碳酸酯之塑膠時，雷射活化中預計產生的晶種更少，且此等晶種之金屬-金屬氧化物比例更差。而該方法則能提昇各種塑膠上產生的催化晶種密度的相似度，從而將金屬化操作進一步簡化，因為用於不同塑膠之金屬浴的差異減小，毋需使此等浴具備不同之活性，且金屬化持續時間變得均衡，進而特別是實現金屬化過程的協調性。 Another advantage found in the study is that the method has an averaging effect in terms of the metallization tendency of various plastics. In the case of plastics such as polycarbonate, it is expected that less seed crystals are produced in laser activation than in the case of plastics such as polyamine, and the metal-metal oxide ratios of such crystals are even worse. The method can improve the similarity of the density of the catalytic seed crystals produced on various plastics, thereby further simplifying the metallization operation, because the difference in the metal bath for different plastics is reduced, and it is not necessary to make the baths have different activities. And the metallization duration becomes equalized, and in particular the coordination of the metallization process is achieved.

此外，事實證明，該方法適於在不對金屬化能力構成明顯限制的情況下，減少塑膠中所需的添加劑的量。此點一方面對該過程之總成本有正面影響，因為所需使用的添加劑減少，另一方面，雷射直接成型所需之添加劑對物理特性(例如塑膠之耐衝擊性及彈性)的影響亦有所減小。 Furthermore, it has proven to be suitable for reducing the amount of additives required in plastics without significantly limiting the metallization capacity. On the one hand, this has a positive impact on the total cost of the process, because the additives used are reduced, and on the other hand, the effects of the additives required for laser direct structuring on physical properties such as impact resistance and elasticity of plastics are also Decreased.

根據本發明意外發現的尤佳方案，就因塑膠中含有之添加劑 無法透過雷射照射轉換或充分轉換成催化金屬晶種，故本身在活性極高之置換浴中不發生明顯金屬沈積的表面而言，亦可使用該方法使得此等經雷射活化之表面具備催化活性。特定言之，此情形見於高活潑性的金屬化合物，因為熱力學動力會嚴重削弱金屬還原，且通常僅發生金屬還原的中間級。 A particularly preferred solution according to the present invention, due to the additives contained in the plastic It is not possible to convert or fully convert into a catalytic metal seed crystal by laser irradiation. Therefore, in the case of a surface where no significant metal deposition occurs in the highly active replacement bath, this method can also be used to make these laser-activated surfaces Catalytic activity. In particular, this situation is seen in highly active metal compounds because thermodynamic forces can severely impair metal reduction, and typically only intermediate stages of metal reduction occur.

此外，亦可根據塑膠藉由熱處理及/或藉由超音波處理，來改進或加快該金屬化浴中的金屬化。 In addition, metallization in the metallization bath can be improved or accelerated by heat treatment according to the plastic and/or by ultrasonic treatment.

本發明能夠提昇LDS-MID之金屬化中的活性，具體方式為，對包含活潑性低於銅之金屬鹽的銅晶種進行針對性的氧化，從而針對無外流之金屬化操作增強該等晶種之品質，即活性。將該等銅晶種替換為貴金屬晶種(例如鈀)的其他優點在於，將因空氣中的氧造成的金屬晶種之氧化減小至最小程度，甚或完全避免，從而對位於該雷射活化與該金屬化操作之間的、在對活化表面進行氧化去活化前出現的時間跨度產生積極作用。此外，交換操作後對催化活性的“凍結”不僅用於將數星期的貯存時間拓展為原則上無限且無活性損失的貯存能力，亦相應增強生產之靈活性，因為雷射成型與金屬化操作毋需在時間方面相互匹配。 The present invention can enhance the activity in the metallization of LDS-MID by specifically oxidizing a copper seed containing a metal salt having a lower activity than copper to enhance the crystal for metallization operation without outflow. The quality of the species, that is, the activity. Other advantages of replacing such copper seeds with noble metal seeds (e.g., palladium) are that the oxidation of the metal seed crystals due to oxygen in the air is minimized, or even completely avoided, so that the laser is activated. A positive effect occurs between the metallization operation and the time span that occurs prior to oxidative deactivation of the activated surface. In addition, the “freezing” of catalytic activity after the exchange operation is not only used to extend the storage time of several weeks into a storage capacity that is in principle unlimited and inactive, and also enhances the flexibility of production because of laser forming and metallization operations. There is no need to match each other in terms of time.

實例1： Example 1:

在兩個由聚碳酸酯/丙烯腈-丁二烯-苯乙烯(XANTAR® LDS 3710，Mitsubishi Engineering Plastics)構成之具LDS能力的注塑式塑膠體上，使用 市售的波長為1064奈米的雷射器(MicroLine3D，LPKF Laser & Electronics AG)，透過15mJ/mm2的單脈衝能量密度分別對尺寸為10×10mm之區域進行成型。將此等板件中的一個浸入由硝酸銀(200mg/L)構成之水性溶液6分鐘，並施加頻率為35kHz的超音波。隨後用水對該樣本進行充分的沖洗，以將多餘的硝酸銀移除，並將該樣本與未經處理之板件一起浸入調溫至47℃的化學金屬化浴(ENPLATE LDS CU-400，Enthone)。在該浴中停留5分鐘後，將該等樣本取出，用清水沖洗該等樣本，並用壓縮空氣對其進行乾燥。在該經硝酸銀處理之樣本上，憑肉眼便能識別出銅層。而在未經處理之樣本上則明顯尚無銅沈積。 On two LDS-capable injection molded plastic bodies consisting of polycarbonate/acrylonitrile butadiene styrene (XANTAR® LDS 3710, Mitsubishi Engineering Plastics), commercially available mines with a wavelength of 1064 nm were used. The emitter (MicroLine 3D, LPKF Laser & Electronics AG) was molded into a region having a size of 10 × 10 mm through a single pulse energy density of 15 mJ/mm 2 . One of the plates was immersed in an aqueous solution composed of silver nitrate (200 mg/L) for 6 minutes, and an ultrasonic wave having a frequency of 35 kHz was applied. The sample was then thoroughly rinsed with water to remove excess silver nitrate and the sample was immersed in a chemical metallization bath (ENPLATE LDS CU-400, Enthone) tempered to 47 °C with untreated plates. . After standing in the bath for 5 minutes, the samples were taken out, the samples were rinsed with water, and dried with compressed air. On the silver nitrate treated sample, the copper layer was recognized by the naked eye. There was clearly no copper deposit on the untreated samples.

實例2： Example 2:

在兩個由聚碳酸酯(XANTAR® LDS 3730，Mitsubishi Engineering Plastics)構成之具LDS能力的注塑式塑膠體上，使用市售的波長為1064奈米的雷射器(MicroLine3D，LPKF Laser & Electronics AG)對若干尺寸為10×10mm之區域進行成型。其中，使得針對各區域的成型參數各不相同，從而在每個塑膠體上透過3至500mJ/mm2的能量密度對若干區域進行成型。將此等板件中的一個浸入由氯化鈀(500mg/L)及氯化鈉(20g/L)構成之水性溶液5分鐘，並施加頻率為35kHz的超音波。隨後用水對該樣本進行充分的沖洗，並將該樣本與未經處理之板件一起浸入調溫至46℃的化學金屬化浴(ENPLATE LDS CU-400，Enthone)。在30分鐘後終止該金屬化操作，並藉由X射線螢光(XRF)對各區域上實現的銅層厚度進行測定。 On two LDS-capable injection molded plastic bodies made of polycarbonate (XANTAR® LDS 3730, Mitsubishi Engineering Plastics), a commercially available laser with a wavelength of 1064 nm (MicroLine3D, LPKF Laser & Electronics AG) ) A number of areas of size 10 x 10 mm were formed. Among them, the molding parameters for each region are made different, so that a plurality of regions are formed by perforating an energy density of 3 to 500 mJ/mm 2 per plastic body. One of the plates was immersed in an aqueous solution consisting of palladium chloride (500 mg/L) and sodium chloride (20 g/L) for 5 minutes, and an ultrasonic wave having a frequency of 35 kHz was applied. The sample was then thoroughly rinsed with water and the sample was immersed with an untreated plate in a chemical metallization bath (ENPLATE LDS CU-400, Enthone) tempered to 46 °C. The metallization operation was terminated after 30 minutes, and the thickness of the copper layer achieved on each region was measured by X-ray fluorescence (XRF).

如圖2所示，與未經處理之板件相比，該經氯化鈀處理之樣本在較小能量密度下便開始金屬化，且整體言之，該樣本在所有能量密度下皆能更 快地構建銅，以及，金屬沈積停止時該樣本所處於的功率更高。 As shown in Figure 2, the palladium chloride treated sample begins to metallize at a lower energy density than the untreated plate, and overall, the sample can be more energy at all energy densities. The copper is built quickly, and the sample is at a higher power when the metal deposition stops.

實例3： Example 3:

在兩個由聚碳酸酯/丙烯腈-丁二烯-苯乙烯(XANTAR® LDS 3710，Mitsubishi Engineering Plastics)構成之具LDS能力的注塑式塑膠體上，使用市售的波長為1064奈米的雷射器(MicroLine3D,LPKF Laser & Electronics AG)，透過15mJ/mm2的單脈衝能量密度分別對尺寸為10×10mm之區域進行成型。將此等板件中的一個浸入由氯化鈀(500mg/L)及30%鹽酸(50ml/L)構成之水性溶液5分鐘，並施加頻率為130kHz的超音波。隨後用水對該樣本進行充分的沖洗，並將該樣本與未經處理之板件一起浸入調溫至47℃的化學金屬化浴(ENPLATE LDS CU-400，Enthone)。在該浴中停留5分鐘後，將該等樣本取出，用清水沖洗該等樣本，並用壓縮空氣對其進行乾燥。在該經鈀處理之樣本上，憑肉眼便能識別出銅層。而在未經處理之樣本上則明顯尚無銅沈積。 On two LDS-capable injection molded plastic bodies consisting of polycarbonate/acrylonitrile butadiene styrene (XANTAR® LDS 3710, Mitsubishi Engineering Plastics), commercially available mines with a wavelength of 1064 nm were used. The emitter (MicroLine 3D, LPKF Laser & Electronics AG) was molded into a region having a size of 10 × 10 mm through a single pulse energy density of 15 mJ/mm 2 . One of the plates was immersed in an aqueous solution consisting of palladium chloride (500 mg/L) and 30% hydrochloric acid (50 ml/L) for 5 minutes, and an ultrasonic wave having a frequency of 130 kHz was applied. The sample was then thoroughly rinsed with water and the sample was immersed in an chemical metallization bath (ENPLATE LDS CU-400, Enthone) tempered to 47 °C along with the untreated panels. After standing in the bath for 5 minutes, the samples were taken out, the samples were rinsed with water, and dried with compressed air. On the palladium treated sample, the copper layer was recognized by the naked eye. There was clearly no copper deposit on the untreated samples.

圖3及4示出將CuCr2O4及CuO用作塑膠中之LDS添加劑時的作用機理，以作為補充。 Figures 3 and 4 show the mechanism of action when CuCr 2 O 4 and CuO are used as LDS additives in plastics.

Claims (17)

一種在包含至少一添加劑的非導電載體材料上製造導電構造，特別是導電通路的方法，該至少一添加劑具有至少一金屬化合物，其中使得該載體材料在待產生導電通路構造之區域內局部承受電磁輻射，以及，在此等區域內實施金屬化，從而在該非導電載體材料上產生該導電構造，其特徵在於，在該等施加有電磁輻射之區域內，藉由化學反應，將含有的無催化活性之添加劑的至少一部分及/或其因該電磁輻射而產生的無催化活性之片段，替換為至少一用作交換金屬的、具催化活性的金屬，以及，最後在該交換金屬上實施金屬化。 A method of making a conductive structure, particularly a conductive path, on a non-conductive support material comprising at least one additive, the at least one additive having at least one metal compound, wherein the support material is locally exposed to electromagnetic energy in a region where the conductive path structure is to be produced Radiation, and, in such regions, metallization to produce the electrically conductive structure on the non-conductive support material, characterized in that, in the region where the electromagnetic radiation is applied, the chemical reaction comprises a non-catalytic At least a portion of the active additive and/or its catalytically inactive fragments resulting from the electromagnetic radiation are replaced with at least one catalytically active metal used as the exchange metal, and finally metallization is carried out on the exchange metal . 如申請專利範圍第1項之方法，其特徵在於，針對該交換反應，將該非導電載體材料浸入一水性溶液。 The method of claim 1, wherein the non-conductive support material is immersed in an aqueous solution for the exchange reaction. 如申請專利範圍第2項之方法，其特徵在於，該水性溶液不包含在該交換反應中以還原的方式起作用的組分。 The method of claim 2, wherein the aqueous solution does not comprise a component that acts in a reducing manner in the exchange reaction. 如申請專利範圍第2或3項之方法，其特徵在於，該水性溶液包含溶解的金屬鹽。 The method of claim 2, wherein the aqueous solution comprises a dissolved metal salt. 如前述申請專利範圍中至少一項之方法，其特徵在於，透過超音波處理來協助該交換反應。 A method according to at least one of the preceding claims, characterized in that the exchange reaction is assisted by ultrasonic processing. 如前述申請專利範圍中至少一項之方法，其特徵在於，在將該非導電載體材料浸入期間，至少暫時地對該水性溶液施加處於高於10kHz之頻率範圍內的聲場。 A method according to at least one of the preceding claims, characterized in that during the immersion of the non-conductive carrier material, a sound field in the frequency range above 10 kHz is applied at least temporarily to the aqueous solution. 如前述申請專利範圍中至少一項之方法，其特徵在於，透過該交換反應將鈀、銀、鉑或金施覆至該等施加有電磁輻射的區域。 A method according to at least one of the preceding claims, characterized in that palladium, silver, platinum or gold is applied to the regions to which electromagnetic radiation is applied through the exchange reaction. 如前述申請專利範圍中至少一項之方法，其特徵在於，以某種方式對該電磁輻射的作用進行控制，以及，以某種方式選擇該至少一添加劑，使得在未發生交換反應或其他化學反應的情況下，不會因該非導電載體材料之電磁輻射而在無外流之金屬化浴中產生具催化活性的晶種。 A method according to at least one of the preceding claims, characterized in that the effect of the electromagnetic radiation is controlled in a manner and the at least one additive is selected in such a way that no exchange reaction or other chemistry occurs In the case of the reaction, no catalytically active seed crystals are produced in the metallization bath without the outflow due to the electromagnetic radiation of the non-conductive support material. 如前述申請專利範圍中至少一項之方法，其特徵在於，該無催化活性之添加劑中所含有的金屬化合物包含金屬氧化物。 A method according to at least one of the preceding claims, characterized in that the metal compound contained in the catalytically inactive additive comprises a metal oxide. 如前述申請專利範圍中至少一項之方法，其特徵在於，透過該雷射活化對該添加劑中之金屬的氧化態進行還原。 A method according to at least one of the preceding claims, characterized in that the oxidation state of the metal in the additive is reduced by the laser activation. 如前述申請專利範圍中至少一項之方法，其特徵在於，在該載體材料及/或在該添加劑中設有吸收劑，其有助於該電磁輻射之能量的轉換，以便將該金屬化合物活化。 A method according to at least one of the preceding claims, characterized in that an absorbent is provided in the carrier material and/or in the additive, which facilitates the conversion of the energy of the electromagnetic radiation in order to activate the metal compound . 如前述申請專利範圍中至少一項之方法，其特徵在於，透過該化學交換反應，僅將該添加劑之無催化活性的部分替換為該至少一用作交換金屬的、具催化活性的金屬。 The method according to at least one of the preceding claims, characterized in that, by the chemical exchange reaction, only the catalytically inactive portion of the additive is replaced by the at least one catalytically active metal used as the exchange metal. 如前述申請專利範圍中至少一項之方法，其特徵在於，透過該化學交換反應，既將該添加劑之無催化活性的部分，亦將該添加劑之具催化活性的部分替換為該至少一用作交換金屬的、具催化活性的金屬。 A method according to at least one of the preceding claims, characterized in that, through the chemical exchange reaction, both the catalytically inactive portion of the additive and the catalytically active portion of the additive are replaced by the at least one Exchange of metal, catalytically active metals. 一種包含添加劑之載體材料，在該載體材料上藉由該如前述申請專利範圍中至少一項之方法製造導電構造，特別是導電通路，其特徵在於，該載體材料所含有之主要材料成分為聚合物、陶瓷、木材及/或玻璃。 A support material comprising an additive, on which a conductive structure, in particular a conductive path, is produced by the method according to at least one of the preceding claims, characterized in that the main material component of the carrier material is polymerized Material, ceramic, wood and / or glass. 如申請專利範圍第14項之載體材料，其特徵在於，該載體材料特別是為藉由注塑法制成的模製體。 The carrier material of claim 14 is characterized in that the carrier material is in particular a molded body produced by injection molding. 如申請專利範圍第14項之載體材料，其特徵在於，該載體材料特別是為藉由增材製造方法，例如熔融沈積成型、選擇性雷射燒結、立體光微影及其他方法製成的模製體。 The carrier material according to claim 14 is characterized in that the carrier material is in particular a mold made by an additive manufacturing method such as fused deposition molding, selective laser sintering, stereo photolithography and the like. Body. 如申請專利範圍第14項之載體材料，其特徵在於，藉由施覆法或塗佈法，例如噴射過程或浸入過程，將該載體材料施覆至位於下方之模製體。 The carrier material of claim 14 is characterized in that the carrier material is applied to the molded body located below by an application method or a coating method such as a spraying process or an immersion process.
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