Circuit preparation method, conductive thin film and semiconductor device

Abstract

Disclosed in the present invention are a circuit preparation method, a conductive thin film and a semiconductor device. The preparation method comprises the steps of: sequentially preparing a conductor thin-film layer and a patterned mask layer on a substrate having an adhesive metal film layer; performing first electroplating treatment to form an electroplated film layer; performing second electroplating treatment on the electroplated film layer to form a first protective film layer; removing the mask layer and performing first etching treatment; performing third electroplating treatment on an exposed part of the adhesive metal film layer and the first protective film layer to form a second protective film layer; performing roughening treatment on the second protective film layer; and performing second etching treatment on the roughened exposed part of the adhesive metal film layer.

Description

Circuit preparation method, conductive film and semiconductor device

[0001] This application claims priority to the Chinese patent application filed with the China Patent Office on December 8, 2023, with application number 2023116999274 and invention name “Circuit preparation method, conductive film and semiconductor device”, the entire contents of which are incorporated by reference into this application. Technical Field

[0002] The present application relates to the field of electronic manufacturing and electroplating technology, and in particular to a circuit preparation method, a conductive film, and a semiconductor device. Background Art

[0003] In the field of electroplating, when encountering graphic multi-layer metal thickening electroplating, it is difficult to achieve multi-layer three-dimensional coating of the surface wiring structure of the circuit pattern without separate interconnection power leads. For example, in the case of copper interconnect electroplating with low oxidation resistance, it is easy to cause reliability risks due to the lack of three-dimensional coating on the side of the graphic wiring, which ultimately leads to failure of the graphic circuit.

[0004] With the increasing demand for metal interconnects on various substrate surfaces and their relative cost decreasing, copper and nickel have become the preferred materials for substrate surface wiring in various industries due to their relatively low cost. However, due to their low oxidation resistance, copper and nickel surfaces must be coated with a protective layer to ensure long-term circuit reliability. Currently, various industries use a variety of oxidation resistance methods. Among them, to ensure high reliability and relatively low cost, traditional technology generally uses electroplating to protect the surface of copper and nickel wiring.

[0005] Traditionally, the solution for completely protecting the copper or nickel interconnect surface through electroplating is to electroplate protective copper or nickel on individual leads and then remove the leads. Although the leads are relatively thin, the lead ports are still not covered. Some patterns cannot form pattern alignment and wrapping due to the thin seams, ultimately leading to a long process and the risk of low reliability.

[0006] Summary of the Invention

[0007] Based on this, it is necessary to provide a circuit preparation method. The circuit preparation method of the present invention has fewer steps, high efficiency, can realize batch production, and has low cost.

[0008] An embodiment of the present application provides a circuit manufacturing method.

[0009] A circuit preparation method comprises the following steps:

[0010] providing a substrate having an adhered metal film layer;

[0011] preparing a conductor film layer on the adhesive metal film layer;

[0012] preparing a patterned mask layer on the conductor thin film layer;

[0013] performing a first electroplating process on the conductor thin film layer having the mask layer to form an electroplated film layer;

[0014] performing a second electroplating process on the electroplated film layer to form a first protective film layer;

[0015] removing the mask layer and performing a first etching process on the exposed conductor thin film layer;

[0016] Performing a third electroplating process on the exposed portion of the adhesive metal film layer and the first protective film layer after the first etching process to form a fully covered second protective film layer;

[0017] performing a roughening process on a portion of the second protective film layer connected to the adhesive metal film layer to remove the portion of the second protective film layer;

[0018] A second etching process is performed on the adhesion metal film layer.

[0019] In some embodiments, the substrate includes a ceramic substrate, a silicon wafer, an insulating substrate, or a semiconductor substrate.

[0020] In some embodiments, the ceramic substrate includes an aluminum oxide ceramic substrate or an aluminum nitride ceramic substrate; and / or the semiconductor substrate includes a solar cell.

[0021] In some embodiments, a substrate having an adhered metal film layer is prepared by the following steps: cleaning the substrate with a cleaning agent to remove surface contaminants, the cleaning agent comprising hydrofluoric acid, hydrochloric acid, and pure water, wherein the volumes of the hydrofluoric acid, hydrochloric acid, and pure water are (2 mL to 5 mL):(2 mL to 5 mL):100 mL;

[0022] The adhesive metal film layer is prepared on the substrate by a vacuum coating method.

[0023] In some embodiments, the circuit preparation method further satisfies at least one of the following conditions:

[0024] (1) The preparation material of the adhesive metal film layer includes one or more alloys of metals selected from the group consisting of Al, Cr, Ni, Mn, Pd, Bi, Nb, Ta, Pa, V, Ti, and W;

[0025] (2) The preparation material of the adhesion metal film layer includes metal nitrides or metal oxides of Al, Cr, Ni, Mn, Pd, Bi, Nb, Ta, Pa, V, Ti or W.

[0026] In some embodiments, the thickness of the adhesion metal film layer is 100 nm to 200 nm.

[0027] In some embodiments, the thickness of the conductor thin film layer is 20 nm to 500 nm.

[0028] In some embodiments, when preparing a patterned mask layer on the conductor thin film layer, the following steps are included:

[0029] The mask layer is prepared from materials including one or more of ink, photoresist and dry film;

[0030] And / or, when the mask layer is a non-photosensitive material, the mask layer is prepared on the conductor film layer by screen printing, spraying or spin coating; when the mask layer is a photosensitive material, the mask layer is prepared on the conductor film layer by coating, mask exposure or development technology.

[0031] In some embodiments, performing a first electroplating process on the conductor thin film layer having the mask layer to form an electroplated film layer specifically includes the following steps:

[0032] The conductor film layer is sequentially degreased and cleaned with a degreasing agent, and then activated and cleaned with an acid dip;

[0033] The conductor film layer is subjected to a first electroplating treatment.

[0034] In some embodiments, when performing the first electroplating process, at least one of the following conditions is met:

[0035] (1) During the degreasing process, the degreasing time is at least 40 seconds;

[0036] (2) During the acid leaching activation treatment, hydrochloric acid with a mass concentration of 5% to 15% is used for acid leaching activation for at least 40 seconds;

[0037] (3) During the cleaning process, high-purity water is used for cleaning for at least 60 seconds.

[0038] In some embodiments, during the first electroplating treatment, the substrate is placed in a copper plating solution or a nickel plating solution at a current density of 0.5 A / dm 2 ~15A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 30s to 200s, the thickness of the electroplated film layer is 2μm to 15μm, and after the electroplating is completed, it is washed with high-purity water for at least 60s and then dried.

[0039] In some embodiments, when performing a second electroplating process on the electroplated film layer to form a first protective film layer, the process specifically includes the following steps:

[0040] The electroplated film layer is sequentially degreased and cleaned with a degreasing agent, and then activated and cleaned with acid immersion;

[0041] The electroplated film layer is subjected to a second electroplating treatment.

[0042] In some embodiments, when the second electroplating process is performed, at least one of the following conditions is met:

[0043] (1) During the degreasing treatment, the degreasing time is at least 40 seconds.

[0044] (2) During the acid leaching activation treatment, hydrochloric acid with a mass concentration of 5% to 15% is used for acid leaching activation for at least 40 seconds;

[0045] (3) During the cleaning process, high-purity water is used for cleaning for at least 60 seconds.

[0046] In some embodiments, during the second electroplating process, the substrate is placed in a gold plating solution at a current density of 0.5 A / dm 2 ~1A / dm 2 Selective electroplating is performed under the condition of 0.5A / dm 2 ~10A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 3 minutes to 15 minutes, the thickness of the first protective film layer is 1 μm to 10 μm, and after the electroplating is completed, it is washed with high-purity water for at least 60 seconds and then dried.

[0047] In some embodiments, performing the first etching process on the exposed conductor film layer specifically includes the following steps:

[0048] Performing a first etching process on the exposed conductor thin film layer by wet etching or plasma dry etching;

[0049] Among them, in the wet etching, when the preparation material of the conductive thin film layer is Cu, the etching solution is a mixture of sulfuric acid, sodium persulfate and water, or a mixture of hydrogen peroxide, concentrated sulfuric acid and water, and the etching time is 20s-120s; when the preparation material of the conductive thin film layer is Ni, the etching solution is a mixture of nitric acid, sodium persulfate and water, and the etching time is 20s-100s;

[0050] In plasma dry etching, the argon gas flow rate is greater than 20 sccm, the etching process pressure is 0.01 Pa to 1 Pa, and the etching time is 10s to 1000s.

[0051] In some embodiments, the circuit preparation method further satisfies at least one of the following conditions:

[0052] (1) The mass volume ratio of sulfuric acid, sodium persulfate and water is (2 mL to 3 mL): (1 g to 5 g): (10 g to 20 g);

[0053] (2) The volume ratio of hydrogen peroxide, concentrated sulfuric acid, and water is (1 mL to 2 mL): (2 mL to 4 mL): (20 mL to 40 mL);

[0054] (3) The mass volume ratio of nitric acid, sodium persulfate and water is (2mL~3mL):(1g~5g):(10g~20g).

[0055] In some embodiments, when a third electroplating process is performed on the exposed portion of the adhesive metal film layer and the first protective film layer after the first etching process to form a fully covered second protective film layer, the method specifically includes the following steps:

[0056] Using a degreasing agent to sequentially degrease and clean the exposed portion of the adhesive metal film layer and the first protective film layer, and then perform an acid immersion activation treatment and a cleaning treatment;

[0057] A third electroplating process is performed on the exposed portion of the adhesive metal film layer and the first protective film layer to form a fully covered second protective film layer.

[0058] In some embodiments, when the third electroplating process is performed, at least one of the following conditions is met:

[0059] (1) During the degreasing process, the degreasing time is at least 40 seconds;

[0060] (2) During the acid leaching activation treatment, hydrochloric acid with a mass concentration of 5% to 15% is used for acid leaching activation for at least 40 seconds;

[0061] (3) During the cleaning process, high-purity water is used for cleaning for at least 60 seconds.

[0062] In some embodiments, during the third electroplating treatment, the substrate is placed in a gold plating solution, a silver plating solution or a tin plating solution at a current density of 0.5 A / dm 2 ~40A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 30s to 200s, the thickness of the second protective film layer is 0.5μm to 1μm, and after the electroplating is completed, it is washed with high-purity water for at least 60s and then dried.

[0063] In some embodiments, roughening the portion of the second protective film layer connected to the adhesive metal film layer specifically includes the following steps:

[0064] Performing wet sandblasting on a portion of the second protective film layer to remove a portion of the second protective film layer connected to the adhered metal film layer, wherein the diamond grain size is 100 mesh to 400 mesh, the sandblasting pressure is 0.1 MPa to 0.3 MPa, the sandblasting time is 20 seconds to 100 seconds, the water washing flow rate is 2 L / min to 10 L / min, and the water washing time is 20 seconds to 100 seconds;

[0065] After wet sandblasting, the material is dried at a temperature of 50°C to 80°C and for a time of 20s to 100s.

[0066] In some embodiments, performing the second etching process on the adhesion metal film layer specifically includes the following steps:

[0067] Performing a second etching process on the adhesion metal film layer by wet etching or plasma dry etching;

[0068] The wet etching process uses HF acid etching, with an etching time of 20s to 100s and a temperature of 25°C to 30°C.

[0069] During plasma dry etching, the etching pressure is 0.1Pa-1Pa, the etching gas is argon, the argon flow rate is greater than 20sccm, and the etching time is 10s-1000s.

[0070] Another embodiment of the present application further provides a conductive film.

[0071] A conductive film is prepared by adopting the preparation method.

[0072] Another embodiment of the present application further provides a semiconductor device.

[0073] A semiconductor device includes a conductive film.

[0074] The above-mentioned circuit preparation method can three-dimensionally wrap the circuit pattern wiring through electroplating thickening in the absence of separate interconnecting leads. Specifically, the adhesive metal film layer of the present application is composed of an alloy or a single metal. Since the adhesive metal film layer is relatively thin, its sheet resistance is between 3 ohms and 10 ohms. Therefore, when a certain power is applied, the current passing through circuits with different sheet resistances is different, resulting in the final circuit side being able to be plated, and finally forming a three-dimensional wrapping of the pattern. Since a small amount of metal layer is also electroplated on the surface of the non-graphic area, the low-adhesion surface metal on the adhesive metal film layer is removed through a relatively low-intensity roughening process such as sandblasting, and finally the adhesive metal film layer is etched. This method reduces the lead removal process, reduces the process cost, and improves efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0075] To more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present application. Those skilled in the art can also derive other drawings based on these drawings without inventive effort.

[0076] In order to more completely understand the present application and its beneficial effects, the following description will be given in conjunction with the accompanying drawings. In the following description, the same reference numerals represent the same parts.

[0077] 1-6 are schematic diagrams of a process flow of a circuit fabrication method according to an embodiment of the present invention.

[0078] Description of Reference Numerals

[0079] 100, substrate; 200, adhesive metal film layer; 300, conductor film layer; 400, mask layer; 500, electroplating film layer; 600, first protective film layer; 700, second protective film layer. DETAILED DESCRIPTION

[0080] To make the above-mentioned objects, features, and advantages of the present invention more readily apparent, specific embodiments of the present invention are described in detail below with reference to the accompanying drawings. The following description sets forth numerous specific details to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways than those described herein, and those skilled in the art may make similar modifications without departing from the scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0081] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0082] In the present invention, unless otherwise specified or limited, the terms "installed," "connected," "connect," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection; direct connection, or indirect connection through an intermediate medium; internal communication between two components, or interaction between two components, unless otherwise specified. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0083] In the present invention, unless otherwise expressly specified or limited, when a first feature is "above" or "below" a second feature, it may mean that the first and second features are in direct contact, or that the first and second features are in indirect contact through an intermediary. Furthermore, when a first feature is "above," "above," or "above" a second feature, it may mean that the first feature is directly above or diagonally above the second feature, or simply means that the first feature is at a higher level than the second feature. When a first feature is "below," "below," or "below" a second feature, it may mean that the first feature is directly below or diagonally below the second feature, or simply means that the first feature is at a lower level than the second feature.

[0084] In the description of this invention, "several" means more than one, "plurality" means more than two, "greater than," "less than," and "exceed" are understood to exclude the number itself, while "above," "below," and "within" are understood to include the number itself. The use of "first" and "second" in the description is solely for the purpose of distinguishing technical features and is not to be construed as indicating or implying relative importance, implicitly specifying the number of the indicated technical features, or implicitly specifying the order of the indicated technical features.

[0085] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this invention pertains. The terms used herein in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0086] The present invention provides a circuit fabrication method to address the risks of lengthy processes and low reliability in conventional methods that employ individual leads, undergoing interconnection electroplating with protective copper or nickel, and then removing the leads. This method involves the lead ends remaining unwrapped, and some patterns cannot be aligned due to thin seams. The circuit fabrication method is described below with reference to the accompanying figures.

[0087] The circuit fabrication method provided in the embodiment of the present application is exemplified in FIG1 , which is a schematic diagram of the process flow of the circuit fabrication method provided in the embodiment of the present application. The circuit fabrication method of the present application can be used for fabricating multi-layer electroplating circuits.

[0088] In order to more clearly illustrate the structure of the circuit preparation method, the circuit preparation method will be introduced below with reference to the accompanying drawings.

[0089] Exemplarily, a circuit preparation method includes the following steps:

[0090] Providing a substrate 100 having an adhered metal film layer 200;

[0091] A conductive film layer 300 is formed on the adhesive metal film layer 200 by a vacuum coating method;

[0092] A patterned mask layer 400 is prepared on the conductor film layer 300, as shown in FIG1 ;

[0093] Performing a first electroplating process on the exposed portion of the conductor film layer 300 having the mask layer 400 to form an electroplated film layer 500, and then performing a drying process;

[0094] A second electroplating process is performed on the electroplated film layer 500 to form a first protective film layer 600, as shown in FIG. 2 ;

[0095] The mask layer 400 is removed, as shown in FIG3 ; the exposed conductor film layer 300 is subjected to a first etching process, as shown in FIG4 ;

[0096] A third electroplating process is performed on the exposed portion of the adhesive metal film layer 200 and the first protective film layer 600 after the first etching process to form a fully covered second protective film layer 700, as shown in FIG5 ;

[0097] performing a roughening process on a portion of the second protective film layer 700 connected to the adhesive metal film layer 200 to remove the portion of the second protective film layer 700; and

[0098] The adhesion metal film layer 200 is subjected to a second etching process, as shown in Figure 6. After the second etching process, the substrate 100 is exposed.

[0099] In some embodiments, the conductive film layer 300 is made of Cu or Ni.

[0100] In some embodiments, the substrate 100 includes a ceramic substrate, a silicon wafer, an insulating substrate, or a semiconductor substrate.

[0101] In some embodiments, the ceramic substrate 100 includes an aluminum oxide ceramic substrate or an aluminum nitride ceramic substrate; and / or the semiconductor substrate includes a solar cell.

[0102] In some embodiments, the substrate 100 having the adhered metal film layer 200 is prepared by the following steps: cleaning the substrate 100 with a cleaning agent to remove surface contaminants, the cleaning agent comprising hydrofluoric acid, hydrochloric acid, and pure water, wherein the volumes of the hydrofluoric acid, hydrochloric acid, and pure water are (2-5 mL):(2-5 mL):100 mL;

[0103] The adhesive metal film layer 200 is formed on the substrate 100 by a vacuum coating method.

[0104] In some embodiments, the adhesive metal film layer 200 is made of a material selected from the group consisting of Al, Cr, Ni, Mn, Pd, Bi, Nb, Ta, Pa, V, Ti, and W, or an alloy thereof.

[0105] In some embodiments, the adhesion metal film layer 200 is made of a material including a metal nitride or a metal oxide of Al, Cr, Ni, Mn, Pd, Bi, Nb, Ta, Pa, V, Ti, or W.

[0106] In some embodiments, the thickness of the adhesion metal film layer 200 is 100 nm to 200 nm.

[0107] In some embodiments, the thickness of the conductive film layer 300 is 20 nm to 500 nm.

[0108] In some embodiments, the material of the conductive film layer 300 and the material of the electroplating film layer 500 may be the same or different.

[0109] In some embodiments, the following steps are included when preparing the patterned mask layer 400 on the conductor film layer 300: the mask layer 400 is prepared using a material including one or more of ink, photoresist, and dry film.

[0110] In some embodiments, when the mask layer 400 is a non-photosensitive material, the mask layer 400 is prepared on the conductor film layer 300 by screen printing, spraying or spin coating; when the mask layer 400 is a photosensitive material, the mask layer 400 is prepared on the conductor film layer 300 by coating, mask exposure or development technology.

[0111] In some embodiments, performing a first electroplating process on the conductor film layer 300 having the mask layer 400 to form the electroplated film layer 500 specifically includes the following steps:

[0112] The conductive film layer 300 is sequentially degreased and cleaned with a degreasing agent, and then subjected to acid immersion activation and cleaning.

[0113] The conductive film layer 300 is subjected to a first electroplating process.

[0114] In some embodiments, when performing the first electroplating process, at least one of the following conditions is met:

[0115] (1) During degreasing treatment, the degreasing time should be at least 40 seconds;

[0116] (2) During acid leaching activation treatment, use hydrochloric acid with a mass concentration of 5% to 15% for at least 40 seconds;

[0117] (3) During cleaning, use high-purity water for at least 60 seconds.

[0118] In some embodiments, during the first electroplating process, the substrate 100 is placed in a copper plating solution or a nickel plating solution of the same material as the conductor film layer 300, and the current density is 0.5A / dm 2 ~15A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 5 minutes to 15 minutes, the thickness of the electroplated film layer 500 is 2 μm to 15 μm, and after the electroplating is completed, it is washed with high-purity water for at least 60 seconds and then dried.

[0119] In some embodiments, performing the second electroplating process on the electroplated film layer 500 to form the first protective film layer 600 specifically includes the following steps:

[0120] The electroplated film layer 500 is sequentially degreased and cleaned with a degreasing agent, and then activated and cleaned with acid immersion.

[0121] The electroplated film layer 500 is subjected to a second electroplating treatment.

[0122] In some embodiments, the material of the first protective film layer 600 includes but is not limited to gold, silver, and tin.

[0123] In some embodiments, when the second electroplating process is performed, at least one of the following conditions is met:

[0124] (1) During degreasing treatment, the degreasing time should be at least 40 seconds;

[0125] (2) During acid leaching activation treatment, use hydrochloric acid with a mass concentration of 5% to 15% for at least 40 seconds;

[0126] (3) During cleaning, use high-purity water for at least 60 seconds.

[0127] In some embodiments, during the second electroplating process, the substrate 100 is placed in a gold plating solution at a current density of 0.5 A / dm 2 ~1A / dm 2Selective electroplating is performed under the condition of 0.5A / dm 2 ~10A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 3 minutes to 15 minutes, the thickness of the first protective film layer 600 is 1 μm to 10 μm, and after the electroplating is completed, it is washed with high-purity water for at least 60 seconds and then dried.

[0128] In some embodiments, the first etching process performed on the exposed conductive film layer 300 specifically includes the following steps:

[0129] The exposed conductive film layer 300 is subjected to a first etching process using wet etching or plasma dry etching. In the wet etching process, when the conductive film layer 300 is made of Cu, the etching solution is a mixture of sulfuric acid, sodium persulfate, and water, or a mixture of hydrogen peroxide, concentrated sulfuric acid, and water, and the etching time is 20 seconds to 120 seconds. When the conductive film layer 300 is made of Ni, the etching solution is a mixture of nitric acid, sodium persulfate, and water, and the etching time is 20 seconds to 100 seconds. In the plasma dry etching process, the argon gas flow rate is greater than 20 seem, the etching process pressure is 0.01 Pa to 1 Pa, and the etching time is 10 seconds to 1000 seconds.

[0130] In some embodiments, the mass volume ratio of sulfuric acid, sodium persulfate and water is (2 mL to 3 mL): (1 g to 5 g): (10 g to 20 g).

[0131] In some embodiments, the volume ratio of hydrogen peroxide, concentrated sulfuric acid and water is (1 mL to 2 mL): (2 mL to 4 mL): (20 mL to 40 mL).

[0132] In some embodiments, the mass volume ratio of nitric acid, sodium persulfate and water is (2 mL to 3 mL): (1 g to 5 g): (10 g to 20 g).

[0133] In some embodiments, when a third electroplating process is performed on the exposed portion of the adhesive metal film layer 200 and the first protective film layer 600 after the first etching process to form a fully covered second protective film layer 700, the process specifically includes the following steps:

[0134] The exposed parts of the adhesive metal film layer 200 and the first protective film layer 600 are sequentially degreased and cleaned with a degreasing agent, and then acid-activated and cleaned.

[0135] A third electroplating process is performed on the exposed portions of the adhesive metal film layer 200 and the first protective film layer 600 to form a fully covered second protective film layer 700 .

[0136] In some embodiments, the second protective film layer 700 is made of materials including but not limited to inert metals such as gold, silver, and tin.

[0137] In some embodiments, when the third electroplating process is performed, at least one of the following conditions is met:

[0138] (1) During degreasing treatment, the degreasing time should be at least 40 seconds;

[0139] (2) During acid leaching activation treatment, use hydrochloric acid with a mass concentration of 5% to 15% for at least 40 seconds;

[0140] (3) During cleaning, use high-purity water for at least 60 seconds.

[0141] In some embodiments, the degreasing agent, model S-15S, produced by Chongqing Renfa Technology Co., Ltd., is used for degreasing.

[0142] In some embodiments, during the third electroplating process, the substrate 100 is placed in a gold plating solution, a silver plating solution or a tin plating solution at a current density of 0.5 A / dm 2 ~10A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 30s to 200s, the thickness of the second protective film layer 700 is 0.5μm to 1μm, and after the electroplating is completed, it is washed with high-purity water for at least 60s and then dried.

[0143] In some embodiments, the roughening process of the portion of the second protective film layer 700 connected to the adhesive metal film layer 200 specifically includes the following steps:

[0144] Performing wet sandblasting on a portion of the second protective film layer 700 to remove the portion of the second protective film layer 700 attached to the metal film layer 200, with the diamond grain size being 100-400 mesh, the sandblasting pressure being 0.1 MPa-0.3 MPa, the sandblasting time being 20-100 seconds, the water washing flow rate being 2 L / min-10 L / min, and the water washing time being 20-100 seconds, and finally removing the portion of the second protective film layer 700 attached to the surface of the metal film layer 200;

[0145] After wet sandblasting, the material is dried at a temperature of 50°C to 80°C and for a time of 20s to 100s.

[0146] In some embodiments, the second etching process of the adhesion metal film layer 200 specifically includes the following steps:

[0147] Performing a second etching process on the adhesion metal film layer 200 by wet etching or plasma dry etching;

[0148] During wet etching, the etching solution includes copper chloride, hydrochloric acid and pure water, wherein the volume ratio of copper chloride, hydrochloric acid and pure water is (1mL~2mL):(5mL~5mL):50mL, the etching time is 20s~100s, and the temperature is 25℃~30℃.

[0149] When wet etching cannot be used and plasma dry etching is used, the etching pressure is 0.1Pa~1Pa, the etching gas is argon, the argon flow rate is greater than 20sccm, and the etching time is 10s-1000s.

[0150] Another embodiment of the present application further provides a conductive film.

[0151] A conductive film is prepared by a preparation method.

[0152] Another embodiment of the present application further provides a semiconductor device.

[0153] A semiconductor device comprises the above-mentioned conductive film.

[0154] In some embodiments, the semiconductor device includes a discrete semiconductor, an optoelectronic semiconductor, a logic IC, an analog IC, a memory, or the like.

[0155] Another embodiment of the present application further provides a solar cell.

[0156] A solar cell comprises the above-mentioned conductive film.

[0157] Example 1

[0158] This embodiment provides a conductive film, which is prepared by the following circuit preparation method.

[0159] A circuit preparation method comprises the following steps:

[0160] (1) Select a substrate 100, which is a silicon wafer. Use a cleaning agent to clean the substrate 100 to remove surface contaminants. The cleaning agent includes hydrofluoric acid, hydrochloric acid, and pure water. The volumes of hydrofluoric acid, hydrochloric acid, and pure water are 5 mL:5 mL:100 mL.

[0161] (1) A vacuum coating method is used to form an adhesive metal film layer 200 on the surface of the substrate 100; the thickness of the adhesive metal film layer 200 is 100 nm. The adhesive metal film layer 200 is made of metal Al.

[0162] (2) A conductive film layer 300 is prepared on the adhesive metal film layer 200 by a vacuum coating method. The thickness of the conductive film layer 300 is 20 nm, and the conductive film layer 300 is made of Cu.

[0163] (3) A patterned mask layer 400 is prepared on the conductor film layer 300, as shown in FIG1 . The mask layer 400 is made of a material including photoresist. The mask layer 400 is prepared on the conductor film layer 300 using a mask exposure technique, as shown in FIG1 .

[0164] (4) The conductor film layer 300 is degreased with degreaser S-15S for 40 seconds, washed with high-purity water for 60 seconds, activated with 10% hydrochloric acid for 40 seconds, and washed with high-purity water for 60 seconds.

[0165] The exposed portion of the conductor film layer 300 is subjected to a first electroplating treatment to form an electroplated film layer 500. Referring to FIG. 2 , during the first electroplating treatment, the substrate 100 is placed in a copper plating solution at a current density of 0.5 A / dm 2 Selective electroplating was performed under the conditions of 500 nm, the electroplating time was 20 min, the thickness of the electroplated film layer was 2 μm, and after the electroplating was completed, it was washed with high-purity water for 60 s and then dried.

[0166] (5) Degreasing agent S-15S was used to degrease the electroplated film layer 500 for 40 seconds, and then it was washed with high-purity water for 60 seconds. Then, it was activated by acid immersion in 10% hydrochloric acid for 40 seconds, and then it was washed with high-purity water for 60 seconds. The electroplated film layer 500 was subjected to a second electroplating treatment. A second electroplating treatment was performed on the electroplated film layer 500 to form a first protective film layer 600, as shown in FIG2. During the second electroplating treatment, the substrate 100 was placed in a tin plating solution at a current density of 1A / dm 2 Selective electroplating was performed under the following conditions for 10 minutes. The thickness of the first protective film layer 600 was 3 μm. After the electroplating was completed, the substrate was rinsed with high-purity water for 60 seconds and then dried. See the second step in FIG. 1 .

[0167] (6) Remove the mask layer 400, as shown in FIG3 .

[0168] The first etching treatment is performed on the exposed conductor film layer 300 outside the electroplating film layer 500 by wet etching; wherein the etching solution is a mixture of sulfuric acid, sodium persulfate and water, wherein the mass volume ratio of sulfuric acid, sodium persulfate and water is 2mL:1g:10g, and the etching time is 20s, as shown in Figure 4.

[0169] (7) Degreasing agent S-15S was used to degrease the exposed part of the adhered metal film layer 200 and the first protective film layer 600 for 40 seconds, and then washed with high-purity water for 60 seconds. Then, the exposed part was activated by acid immersion in 10% hydrochloric acid for 40 seconds, and then washed with high-purity water for 60 seconds.

[0170] The substrate 100 is placed in a tin plating solution at a current density of 2A / dm 2A third electroplating process is performed for 200 seconds to form a second protective film layer 700 connected to the adhesive metal film layer 200 and the first protective film layer 600. The thickness of the second protective film layer 700 is 1 μm. After the electroplating, the surface is rinsed with high-purity water for 60 seconds and then dried. See FIG5 .

[0171] (8) The portion of the second protective film layer 700 on the adhered metal film layer 200 is wet-sandblasted to remove the portion of the second protective film layer 700. The diamond grain size is 100 mesh, the sandblasting pressure is 0.1 MPa, the sandblasting time is 100 s, the water washing flow rate is 2 L / min, and the water washing time is 20 s. After the wet-sandblasting, the portion is dried at a drying temperature of 50°C and a drying time of 100 s.

[0172] (9) The adhesion metal film layer 200 is subjected to a second etching process by wet etching to expose a portion of the substrate 100. The wet etching is performed using a KOH solution with a mass concentration of 5%, an etching time of 30 seconds, and a temperature of 30°C. See FIG6 .

[0173] Example 2

[0174] This embodiment provides a conductive film, which is prepared by the following circuit preparation method.

[0175] A circuit preparation method comprises the following steps:

[0176] (1) Select a substrate 100, which is an alumina ceramic substrate 100. Use a cleaning agent to clean the substrate 100 to remove surface contaminants. The cleaning agent includes hydrofluoric acid, hydrochloric acid, and pure water, wherein the volumes of hydrofluoric acid, hydrochloric acid, and pure water are 2 mL:2 mL:100 mL.

[0177] (1) A vacuum coating method is used to form an adhesive metal film layer 200 on the surface of the substrate 100; the thickness of the adhesive metal film layer 200 is 200 nm. The preparation material of the adhesive metal film layer 200 includes metal Ni and Cr alloy.

[0178] (2) A conductive film layer 300 is prepared on the adhesive metal film layer 200 by vacuum coating. The thickness of the conductive film layer 300 is 500 nm. The conductive film layer 300 is made of Ni.

[0179] (3) A patterned mask layer 400 is prepared on the conductor film layer 300 using ink by screen printing, as shown in FIG1 .

[0180] (4) Degreasing agent S-15S was used to degrease the exposed portion of the conductor film layer 300 for 40 seconds, and then the exposed portion was washed with high-purity water for 60 seconds. The exposed portion was then activated by acid immersion in 10% hydrochloric acid for 40 seconds, and then washed with high-purity water for 60 seconds.

[0181] The exposed portion of the conductor film layer 300 is subjected to a first electroplating treatment to form an electroplated film layer 500. Referring to FIG. 2 , during the first electroplating treatment, the substrate 100 is placed in a nickel plating solution at a current density of 5 A / dm 2 Selective electroplating was performed under the conditions of 500 nm, the electroplating time was 30 min, the thickness of the electroplated film layer was 8 μm, and after the electroplating was completed, it was washed with high-purity water for 60 s and then dried.

[0182] (5) The conductor film layer 300 is degreased with degreaser S-15S for 40 seconds, washed with high-purity water for 60 seconds, then activated with 10% hydrochloric acid for 40 seconds, and washed with high-purity water for 60 seconds.

[0183] The electroplating film layer 500 is subjected to a second electroplating treatment, and a second electroplating treatment is performed on the electroplating film layer 500 to form a first protective film layer 600, as shown in FIG2. During the second electroplating treatment, the substrate 100 is placed in a gold plating solution at a current density of 0.5 A / dm 2 Selective electroplating is performed under the following conditions, the electroplating time is 30 minutes, the thickness of the first protective film layer 600 is 3 μm, and after the electroplating is completed, it is washed with high-purity water for 60 seconds and then dried.

[0184] (6) Remove the mask layer 400, as shown in FIG3 .

[0185] The exposed conductor film layer 300 is first etched by wet etching, wherein the etching solution is a mixture of nitric acid, sodium persulfate and water, the mass volume ratio of nitric acid, sodium persulfate and water is 2mL:1g:10g, and the etching time is 100s, as shown in FIG4 .

[0186] (7) Degreasing agent S-15S was used to degrease the exposed part of the adhered metal film layer 200 and the exposed part of the electroplated film layer 500 for 40 seconds, and then washed with high-purity water for 60 seconds. Then, the exposed part was activated by acid immersion in 10% hydrochloric acid for 40 seconds, and then washed with high-purity water for 60 seconds.

[0187] The substrate 100 is placed in a gold plating solution at a current density of 31 A / dm 2 A third electroplating process is performed for 1 minute to form a second protective film layer 700 connected to the adhesive metal film layer 200 and the protective film layer 600. The thickness of the second protective film layer 700 is 1 μm. After the electroplating is completed, the surface is rinsed with high-purity water for 60 seconds and then dried. See FIG5 .

[0188] (8) The portion of the second protective film layer 700 on the adhered metal film layer 200 is wet-sandblasted to remove the portion of the second protective film layer 700. The diamond grain size is 400 mesh, the sandblasting pressure is 0.2 MPa, the sandblasting time is 20 s, the water washing flow rate is 10 L / min, and the water washing time is 20 s. After the wet-sandblasting, the second protective film layer 700 is dried at a drying temperature of 80°C for 20 s.

[0189] (9) Plasma dry etching is used to perform a second etching process on the adhesion metal film layer 200 to remove a portion of the adhesion metal film layer 200, exposing a portion of the substrate 100. The etching pressure is 1 Pa, the etching gas is argon, the argon flow rate is greater than 20 sccm, and the etching time is 100 s. See FIG6 .

[0190] The performance of the conductive films prepared in Example 1 and Example 2 was tested. The test results are shown in Table 1.

[0191] Table 1

[0192] In summary, the above-mentioned circuit preparation method can perform three-dimensional wrapping of the circuit pattern wiring by electroplating thickening in the absence of separate interconnecting leads. Specifically, the adhesive metal film layer 200 of the present application is composed of an alloy or a single metal. Since the adhesive metal film layer 200 is relatively thin and its square resistance is between 3 ohms and 10 ohms, when a certain power is applied, the current passing through the circuits with different square resistances is different, resulting in the final circuit side being able to be plated, and finally forming a three-dimensional wrapping of the pattern. Since a small amount of metal layer is also electroplated on the surface of the non-patterned area, the low-adhesion surface metal on the adhesive metal film layer 200 is removed through a relatively low-intensity roughening process such as sandblasting, and finally the adhesive metal film layer 200 is etched. This method reduces the lead removal process, reduces the process cost, and improves efficiency.

[0193] In the above embodiments, the description of each embodiment has its own focus. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0194] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0195] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be determined by the appended claims.

Claims

1. A circuit preparation method, characterized in that: The steps include: Providing a substrate (100) having an adherent metal film layer (200); Preparing a conductor thin film layer (300) on the adhesive metal film layer (200); Preparing a patterned mask layer (400) on the conductor thin film layer (300); Performing a first electroplating treatment on the conductor thin film layer (300) having the mask layer (400) to form an electroplated film layer (500); Performing a second electroplating process on the electroplated film layer (500) to form a first protective film layer (600); removing the mask layer (400) and performing a first etching process on the exposed conductor thin film layer (300); Performing a third electroplating process on the exposed portion of the adhesive metal film layer (200) and the first protective film layer (600) after the first etching process to form a fully covered second protective film layer (700); Performing a roughening treatment on a portion of the second protective film layer (700) connected to the adhesive metal film layer (200) to remove the portion of the second protective film layer (700); as well as The adhesion metal film layer (200) is subjected to a second etching process.

2. The circuit preparation method according to claim 1, characterized in that: The substrate (100) comprises a ceramic substrate, a silicon wafer, an insulating substrate or a semiconductor substrate.

3. The circuit preparation method according to claim 2, characterized in that: The ceramic substrate includes an aluminum oxide ceramic substrate and an aluminum nitride ceramic substrate.

4. The circuit preparation method according to claim 2, characterized in that: The semiconductor substrate includes a solar cell.

5. The circuit preparation method according to claim 1, characterized in that: The substrate (100) with an adhered metal film layer (200) is prepared by the following steps: using a cleaning agent to clean the substrate (100) to remove surface contaminants, the cleaning agent comprising hydrofluoric acid, hydrochloric acid and pure water, wherein the volumes of the hydrofluoric acid, hydrochloric acid and pure water are (2mL-5mL):(2mL-5mL):100mL; The adhesive metal film layer (200) is prepared on the substrate (100) by a vacuum coating method.

6. The circuit preparation method according to any one of claims 1 to 5, characterized in that: The preparation material of the adhesion metal film layer (200) includes one or more alloys of metals selected from the group consisting of Al, Cr, Ni, Mn, Pd, Bi, Nb, Ta, Pa, V, Ti and W.

7. The circuit preparation method according to any one of claims 1 to 6, characterized in that: The preparation material of the adhesion metal film layer (200) includes metal nitrides or metal oxides of Al, Cr, Ni, Mn, Pd, Bi, Nb, Ta, Pa, V, Ti or W.

8. The circuit preparation method according to any one of claims 1 to 7, characterized in that: The thickness of the adhesive metal film layer (200) is 100nm-200nm.

9. The circuit preparation method according to any one of claims 1 to 8, characterized in that: The thickness of the conductor thin film layer (300) is 20nm-500nm.

10. The circuit preparation method according to any one of claims 1 to 9, characterized in that: When preparing a patterned mask layer (400) on the conductor thin film layer (300), the following steps are included: The mask layer (400) is prepared from materials including one or more of ink, photoresist and dry film.

11. The circuit preparation method according to any one of claims 1 to 10, characterized in that: When the mask layer (400) is a non-photosensitive material, the mask layer (400) is prepared on the conductor film layer (300) by screen printing, spraying or spin coating; when the mask layer (400) is a photosensitive material, the mask layer (400) is prepared on the conductor film layer (300) by coating, mask exposure or development technology.

12. The circuit preparation method according to any one of claims 1 to 11, characterized in that: When the conductor thin film layer (300) having the mask layer (400) is subjected to a first electroplating treatment to form an electroplated film layer (500), the steps specifically include: The conductor film layer (300) is subjected to degreasing treatment and cleaning treatment in sequence by using a degreasing agent, and then subjected to acid immersion activation treatment and cleaning treatment; The conductor film layer (300) is subjected to a first electroplating treatment.

13. The circuit preparation method according to claim 12, characterized in that: When the first electroplating treatment is performed, the degreasing time during the degreasing treatment is at least 40 seconds.

14. The circuit preparation method according to any one of claims 12 to 13, characterized in that: In the first electroplating treatment, during the acid immersion activation treatment, hydrochloric acid with a mass concentration of 5% to 15% is used for acid immersion activation for at least 40 seconds.

15. The circuit preparation method according to any one of claims 12 to 14, characterized in that: During the first electroplating treatment, during the cleaning treatment, high-purity water is used for cleaning for at least 60 seconds.

16. The circuit preparation method according to any one of claims 1 to 15, characterized in that: During the first electroplating treatment, the substrate (100) is placed in a copper plating solution or a nickel plating solution at a current density of 0.5 A / dm 2 ~15A / dm 2 The selective electroplating is carried out under the condition of 30s to 200s, the thickness of the electroplated film layer (500) is 2μm to 15μm, and after the electroplating is completed, it is washed with high-purity water for at least 60s and then dried.

17. The circuit preparation method according to any one of claims 1 to 16, characterized in that: When a second electroplating process is performed on the electroplated film layer (500) to form a first protective film layer (600), the process specifically comprises the following steps: The electroplated film layer (500) is sequentially subjected to degreasing treatment and cleaning treatment using a degreasing agent, and then subjected to acid immersion activation treatment and cleaning treatment; The electroplated film layer (500) is subjected to a second electroplating treatment.

18. The circuit preparation method according to claim 17, characterized in that: During the second electroplating treatment, the degreasing time is at least 40 seconds during the degreasing treatment.

19. The circuit preparation method according to any one of claims 17 to 18, characterized in that: In the second electroplating treatment, during the acid immersion activation treatment, hydrochloric acid with a mass concentration of 5% to 15% is used for acid immersion activation for at least 40 seconds.

20. The circuit preparation method according to any one of claims 17 to 19, characterized in that: During the second electroplating treatment, during the cleaning treatment, high-purity water is used for cleaning for at least 60 seconds.

21. The circuit preparation method according to any one of claims 1 to 20, characterized in that: During the second electroplating treatment, the substrate (100) is placed in a gold plating solution at a current density of 0.5 A / dm 2 ~1A / dm 2 or placing the substrate (100) in a tin plating solution at a current density of 0.5 A / dm 2 ~10A / dm 2 Selective electroplating is performed under the conditions of 3 minutes to 15 minutes, the thickness of the first protective film layer (600) is 1 μm to 10 μm, and after the electroplating is completed, it is washed with high-purity water for at least 60 seconds and then dried.

22. The circuit preparation method according to any one of claims 1 to 21, characterized in that: When the exposed conductor film layer (300) is subjected to a first etching process, the process specifically comprises the following steps: Performing a first etching process on the exposed conductor film layer (300) by wet etching or plasma dry etching; In the wet etching, when the preparation material of the conductor thin film layer (300) is Cu, the etching solution is a mixture of sulfuric acid, sodium persulfate and water, or a mixture of hydrogen peroxide, concentrated sulfuric acid and water, and the etching time is 20s-120s; when the preparation material of the conductor thin film layer (300) is Ni, the etching solution is a mixture of nitric acid, sodium persulfate and water, and the etching time is 20s-100s; In plasma dry etching, the argon gas flow rate is greater than 20 sccm, the etching process pressure is 0.01 Pa to 1 Pa, and the etching time is 10s to 1000s.

23. The circuit preparation method according to claim 22, characterized in that: In the wet etching, the mass volume ratio of sulfuric acid, sodium persulfate and water is (2mL-3mL):(1g-5g):(10g-20g).

24. The circuit preparation method according to claim 22, characterized in that: In the wet etching, the volume ratio of hydrogen peroxide, concentrated sulfuric acid and water is (1 mL to 2 mL): (2 mL to 4 mL): (20 mL to 40 mL).

25. The circuit preparation method according to claim 22, characterized in that: In the wet etching, the mass volume ratio of nitric acid, sodium persulfate and water is (2 mL to 3 mL): (1 g to 5 g): (10 g to 20 g).

26. The circuit preparation method according to any one of claims 1 to 25, characterized in that: When a third electroplating process is performed on the exposed part of the adhesive metal film layer (200) and the first protective film layer (600) after the first etching process to form a fully covered second protective film layer (700), the process specifically comprises the following steps: Using a degreasing agent to sequentially perform degreasing treatment and cleaning treatment on the exposed part of the adhesive metal film layer (200) and the first protective film layer (600), and then perform acid immersion activation treatment and cleaning treatment; The exposed parts of the adhesive metal film layer (200) and the first protective film layer (600) are subjected to a third electroplating treatment to form a fully covered second protective film layer (700).

27. The circuit preparation method according to claim 26, characterized in that: During the third electroplating treatment, the degreasing time is at least 40 seconds.

28. The circuit preparation method according to any one of claims 26 to 27, characterized in that: In the third electroplating treatment, during the acid immersion activation treatment, hydrochloric acid with a mass concentration of 5% to 15% is used for acid immersion activation for at least 40 seconds.

29. The circuit preparation method according to any one of claims 26 to 28, characterized in that: During the third electroplating treatment, the cleaning process is performed using high-purity water for at least 60 seconds.

30. The circuit preparation method according to any one of claims 1 to 29, characterized in that: During the third electroplating treatment, the substrate (100) is placed in a gold plating solution, a silver plating solution or a tin plating solution at a current density of 0.5 A / dm 2 ~40A / dm 2 Selective electroplating is performed under the condition of 30s to 200s, the thickness of the second protective film layer (700) is 0.5μm to 1μm, and after the electroplating is completed, it is washed with high-purity water for at least 60s and then dried.

31. The circuit preparation method according to any one of claims 1 to 30, characterized in that: When the part of the second protective film layer (700) connected to the adhesive metal film layer (200) is subjected to a roughening treatment, the following steps are specifically included: Performing wet sandblasting on part of the second protective film layer (700) to remove part of the second protective film layer (700) connected to the adhered metal film layer (200), wherein the diamond grain size is 100-400 mesh, the sandblasting pressure is 0.1Mpa-0.3Mpa, the sandblasting time is 20s-100s, the water washing flow rate is 2L / min-10L / min, and the water washing time is 20s-100s; The wet sandblasting is followed by drying, the drying temperature is 50°C to 80°C, and the drying time is 20s to 100s.

32. The circuit preparation method according to any one of claims 1 to 31, characterized in that: When the adhesion metal film layer (200) is subjected to a second etching process, the following steps are specifically included: Performing a second etching process on the adhesion metal film layer (200) by wet etching or plasma dry etching; In the wet etching, HF acid is used for etching, the etching time is 20s to 100s, and the temperature is 25°C to 30°C; During plasma dry etching, the etching pressure is 0.1Pa~1Pa, the etching gas is argon, and the argon flow rate is Greater than 20sccm, etching time is 10s-1000s.

33. A conductive film, characterized in that: The preparation method is described in any one of claims 1 to 32.

34. A semiconductor device, characterized in that: Comprising the conductive film as described in claim 33.

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