Dielectric ceramic component and method for manufacturing the same

Abstract

The present application relates to the technical field of dielectric ceramic application, in particular to a dielectric ceramic component and a preparation method thereof. The preparation method of the dielectric ceramic component comprises the following steps: providing a dielectric ceramic base body with a copper layer plated on the surface; forming a nickel-phosphorus alloy layer on the copper layer, so that the thickness of the nickel-phosphorus alloy layer is greater than or equal to 0.8 microns, and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt%-10wt%; performing surface treatment on the nickel-phosphorus alloy layer, so that the brightness of the nickel-phosphorus alloy layer is 1GU-70GU; and forming a silver layer on the surface-treated nickel-phosphorus alloy layer. The present application can solve the problem of mutual penetration and discoloration between the copper layer and the silver layer.

Description

Technical Field

[0001] This invention relates to the field of dielectric ceramics application technology, and particularly to dielectric ceramic components and their preparation methods. Background Technology

[0002] Dielectric filters are a type of dielectric ceramic component and are core devices in base stations. They are primarily made of dielectric ceramic and fabricated through processes such as metallization and tuning. The metal deposited on the dielectric ceramic has a significant impact on the filter's performance and also affects the pass rate of subsequent tuning and the company's mass production capabilities.

[0003] Currently, silver layers are typically deposited on dielectric ceramics. The main processes for depositing silver layers include: conductive silver paste coating and sintering process, vacuum PVD coating process, and traditional chemical wet process combined with electroplating process.

[0004] However, the conductive silver paste coating and sintering process suffers from significant silver loss and low utilization, resulting in high process costs. Data shows that the process of depositing a silver layer on dielectric ceramics using conductive silver paste coating and sintering accounts for over 35% of all processes in dielectric filters, and its cost accounts for over 30% of the entire process.

[0005] To reduce silver consumption, silver layers can be deposited using vacuum PVD coating, electroless plating, or electroplating. Furthermore, a thicker copper layer can be deposited on top of the dielectric ceramic before silver plating to further reduce silver consumption. However, due to the thinner silver layer, significant interpenetration and discoloration between the copper and silver layers occurs under repeated thermal shocks, resulting in severe color differences in the dielectric ceramic components. Summary of the Invention

[0006] Based on this, the present invention provides a dielectric ceramic component and its fabrication method. This solves the problem of discoloration caused by interpenetration between the copper and silver layers.

[0007] The first aspect of this invention provides a method for preparing dielectric ceramic components. The technical solution is as follows:

[0008] A method for fabricating a dielectric ceramic component includes the following steps:

[0009] Provides a dielectric ceramic substrate with a copper-plated surface;

[0010] A nickel-phosphorus alloy layer is formed on the copper layer, such that the thickness of the nickel-phosphorus alloy layer is ≥0.8μm, and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt% to 10wt%.

[0011] The nickel-phosphorus alloy layer is surface treated to achieve a gloss level of 1 GU to 70 GU.

[0012] A silver layer is formed on the surface-treated nickel-phosphorus alloy layer.

[0013] In some embodiments, the method for forming the nickel-phosphorus alloy layer on the copper layer is chemical plating, wherein the plating solution, immersion temperature and immersion time of the chemical plating are adjusted so that the thickness of the nickel-phosphorus alloy layer is ≥0.8μm and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt% to 10wt%.

[0014] In some embodiments, the plating solution, immersion temperature, and immersion time of the electroless plating are adjusted so that the thickness of the nickel-phosphorus alloy layer is 0.8 μm to 4 μm.

[0015] In some embodiments, the plating solution, immersion temperature, and immersion time of the electroless plating are adjusted so that the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 7wt% to 9wt%.

[0016] In some embodiments, after the nickel-phosphorus alloy layer is formed on the copper layer, a baking step is also included.

[0017] In some embodiments, the surface treatment is an etching process and / or a polishing process.

[0018] In some embodiments, the surface treatment is an etching process, wherein the etching solution, immersion temperature and immersion time are adjusted to make the gloss of the nickel-phosphorus alloy layer 1 GU to 70 GU.

[0019] In some embodiments, the silver layer is formed on the surface-treated nickel-phosphorus alloy layer by electroplating, wherein the electroplating solution is alkaline.

[0020] In some embodiments, the silver layer is formed on the surface-treated nickel-phosphorus alloy layer, and the process further includes a baking step.

[0021] In some embodiments, the thickness of the silver layer is ≤5μm.

[0022] A second aspect of this invention provides a dielectric ceramic component. The technical solution is as follows:

[0023] A dielectric ceramic component includes a dielectric ceramic substrate, a copper layer, a nickel-phosphorus alloy layer, and a silver layer;

[0024] The copper layer is located on the dielectric ceramic substrate;

[0025] The nickel-phosphorus alloy layer is located on top of the copper layer;

[0026] The silver layer is located on top of the nickel-phosphorus alloy layer;

[0027] The thickness of the nickel-phosphorus alloy layer is ≥0.8μm, and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt% to 10wt%, and the brightness of the nickel-phosphorus alloy layer is 1GU to 70GU.

[0028] In some embodiments, the thickness of the nickel-phosphorus alloy layer is 0.8 μm to 4 μm.

[0029] In some embodiments, the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 7 wt% to 9 wt%.

[0030] In some embodiments, the thickness of the silver layer is ≤5 μm.

[0031] To address the issue of discoloration caused by interpenetration between the copper and silver layers in dielectric ceramic components, the inventors of this invention first attempted to add a nickel layer as a spacer between the copper and silver layers. However, during thermal shock tests to verify the reliability of the dielectric ceramic components, it was discovered that the introduction of the nickel layer frequently resulted in significant metal layer separation between the copper, nickel, and silver layers, leading to a decrease in the bonding strength between the metal layers and compromising reliability.

[0032] However, if a nickel-phosphorus alloy layer is added as a spacer between the copper and silver layers, considering the potential alkaline electroplating environment during the subsequent silver layer formation, the spacer layer needs to also possess corrosion resistance. The inventors initially attempted to use a nickel-phosphorus alloy layer with a phosphorus content below 3 wt% as the spacer (generally, a phosphorus content below 3 wt% is considered to offer better resistance to alkaline corrosion, resulting in less loss during electroplating). However, subsequent tensile and thermal shock tests revealed that even after adding a nickel-phosphorus alloy layer with a phosphorus content below 3 wt% between the copper and silver layers, the adhesion of the dielectric ceramic metal layer remained poor, reliability was not guaranteed, and the problem of discoloration between the copper and silver layers persisted. After reviewing existing literature, the inventors found that under alkaline conditions, the alkaline corrosion resistance of the nickel-phosphorus alloy layer deteriorates with increasing phosphorus content. Therefore, after attempting to increase the phosphorus content of the nickel-phosphorus alloy layer to below 3 wt%, considering the potential for silver plating in an alkaline environment, the inventors did not attempt to further increase the phosphorus content of the nickel-phosphorus alloy layer for a period of time.

[0033] However, after extensive and prolonged experimental research, the inventors of this invention discovered that adding a nickel-phosphorus alloy layer with a thickness of not less than 0.8 μm, a phosphorus mass percentage of 4wt% to 10wt%, and a brightness of 1 GU to 70 GU between the copper and silver layers of the dielectric ceramic component not only solves the problem of interpenetration and discoloration between the copper and silver layers, but also ensures good adhesion between the metal layers, guaranteeing the reliability of the dielectric ceramic component. Simultaneously, the corrosion resistance of the nickel-phosphorus alloy layer meets the application requirements. In other words, through the inventors' tireless experimentation, this invention overcomes conventional thinking and technical biases, providing a new and beneficial reference and approach for solving the surface metallization process of dielectric ceramic electronic components used at high temperatures.

[0034] Compared with traditional solutions, the present invention has the following advantages:

[0035] 1) It can reduce the consumption of silver in the silver layer, reduce costs, and avoid the problem of serious color difference in dielectric ceramic components caused by the mutual penetration and discoloration between the copper layer and the silver layer under hot and cold washing.

[0036] 2) The bonding force of each metal layer in dielectric ceramic components is good, resulting in high reliability.

[0037] 3) Subsequent silver plating can be carried out in an alkaline plating solution environment, and the corrosion resistance of the nickel-phosphorus alloy layer meets the requirements of use. Detailed Implementation

[0038] The present invention will be further described in detail below with reference to specific embodiments. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the present invention.

[0039] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0040] the term

[0041] Unless otherwise stated or in case of contradiction, the terms or phrases used herein shall have the following meanings:

[0042] In this invention, the selection range of "and / or", "or / and", and "and / or" includes any one of two or more related listed items, as well as any and all combinations of the related listed items. These arbitrary and all combinations include any two related listed items, any more related listed items, or a combination of all related listed items. It should be noted that when at least three items are connected using at least two conjunctions selected from "and / or", "or / and", and "and / or", it should be understood that the technical solution undoubtedly includes technical solutions connected by "logical AND", and also undoubtedly includes technical solutions connected by "logical OR". For example, "A and / or B" includes three parallel solutions: A, B, and A+B. For example, the technical solution of "A, and / or, B, and / or, C, and / or, D" includes any one of A, B, C, and D (that is, a technical solution that is connected by "logical OR"), as well as any and all combinations of A, B, C, and D, that is, combinations of any two or three of A, B, C, and D, and also combinations of all four of A, B, C, and D (that is, a technical solution that is connected by "logical AND").

[0043] In this invention, terms such as "multiple", "various", "multiple times", and "multi-dimensional" are used, unless otherwise specified, to refer to a quantity greater than or equal to 2. For example, "one or more" means one or more types.

[0044] In this invention, terms such as "preferred," "better," "more suitable," and "ideal" are used only to describe implementation methods or embodiments with better effects, and should be understood not to limit the scope of protection of this invention.

[0045] In this invention, terms such as "further," "even more," and "particularly" are used for descriptive purposes to indicate differences in content, but should not be construed as limiting the scope of protection of this invention.

[0046] In this invention, the terms "optionally," "optionally," and "optional" refer to options that are optional, meaning they are selected from either "with" or "without." If multiple "optional" options appear in a technical solution, unless otherwise specified and there are no contradictions or mutual constraints, each "optional" option is independent.

[0047] In this invention, the terms "first aspect," "second aspect," "third aspect," and "fourth aspect," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or quantity, nor should they be construed as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first," "second," "third," and "fourth," etc., serve only as a non-exhaustive enumeration and should be understood not to constitute a closed limitation on quantity.

[0048] In this invention, the technical features described in an open-ended manner include both closed-ended technical solutions composed of the listed features and open-ended technical solutions that include the listed features.

[0049] In this invention, numerical intervals (i.e., numerical ranges) are involved. Unless otherwise specified, the selected numerical distributions within the aforementioned numerical intervals are considered continuous and include the two endpoints (i.e., the minimum and maximum values) of the numerical range, as well as every value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints. In this document, this is equivalent to directly listing every integer. For example, if t is an integer selected from 1 to 10, it means that t is any integer selected from the group of integers consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10. Furthermore, when multiple ranges are provided to describe features or characteristics, these ranges can be merged. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all subranges to which they are included.

[0050] Unless otherwise specified, the temperature parameters in this invention can be either constant temperature treatment or variations within a certain temperature range. It should be understood that the constant temperature treatment allows temperature fluctuations within the precision range controlled by the instrument. Fluctuations are permitted within ranges such as ±5℃, ±4℃, ±3℃, ±2℃, and ±1℃.

[0051] In this invention, % (w / w) and wt% both represent weight percentage, % (v / v) refers to volume percentage, and % (w / v) refers to mass-volume percentage.

[0052] In this invention, the luminance was tested using a "Chengqixin CQ-60G general-purpose luminance meter".

[0053] A method for fabricating a dielectric ceramic component includes the following steps:

[0054] Provides a dielectric ceramic substrate with a copper-plated surface;

[0055] A nickel-phosphorus alloy layer is formed on the copper layer, such that the thickness of the nickel-phosphorus alloy layer is ≥0.8μm, and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt% to 10wt%.

[0056] The nickel-phosphorus alloy layer is surface treated to achieve a gloss level of 1 GU to 70 GU.

[0057] A silver layer is formed on the surface-treated nickel-phosphorus alloy layer.

[0058] Optionally, in the dielectric ceramic substrate with a copper layer plated on the surface, the copper layer can be formed on the surface of the dielectric ceramic substrate by chemical plating, electroplating, or magnetron sputtering. Optionally, the material of the dielectric ceramic substrate can be selected from magnesium titanate, magnesium titanate-calcium titanate, BaMg... 1 / 3 Ti 2 / 3 O3, BaZn 1 / 3 Ti 2 / 3 O3, Ba(Co,Zn) 1 / 3 Nb 2 / 3 One or more of O3, SrTiO3-LaALO3, magnesium oxide, aluminum oxide, silicon carbide, aluminum nitride, and beryllium oxide may be added as additive phases, such as calcium carbonate / magnesium carbonate. Optionally, the thickness of the copper layer can be 8 μm to 15 μm, and the copper layer and the dielectric ceramic substrate should meet the application requirements.

[0059] In one embodiment, the dielectric ceramic substrate with a copper-plated surface is a magnesium titanate ceramic resonator, the surface of which has been plated with a qualified copper layer.

[0060] Understandably, the thickness of the copper layer can be 8 μm to 15 μm. In a dielectric ceramic substrate with a copper-plated surface, the entire surface of the dielectric ceramic substrate can be plated with a copper layer, or only a portion of the surface can be plated with a copper layer. Other layers may also be included between the dielectric ceramic substrate and the copper layer.

[0061] Optionally, before forming the nickel-phosphorus alloy layer on the copper layer, the process further includes degreasing, micro-etching, pickling, activation, and water washing. In one embodiment, before forming the nickel-phosphorus alloy layer on the copper layer, the process includes sequentially performing degreasing, water washing, micro-etching, water washing, pickling, water washing, activation, and water washing. It is understood that these steps are not mandatory. For example, if the dielectric ceramic substrate surface has just completed copper plating and is immediately ready for subsequent processes, the above steps can be omitted.

[0062] Optionally, the immersion temperature for degreasing is 30–60°C, and the immersion time is 3–10 minutes. The concentration of the degreasing agent is 3 wt%–10 wt%.

[0063] Optionally, the immersion time for micro-etching is 1 min to 2.5 min. The micro-etching solution formulation includes: potassium persulfate 40 g / L to 80 g / L, and sulfuric acid 1 wt% to 5 wt%.

[0064] Optionally, the pickling soaking time is 0.5 min to 3 min. The temperature is 20 to 50 °C. The pickling solution is an aqueous solution of an inorganic acid, selected from one or more of sulfuric acid, hydrochloric acid, and nitric acid. The concentration of the pickling solution is 2 wt% to 10 wt%.

[0065] Activation refers to covering a copper layer with a catalyst to enable the reduction plating of nickel and phosphorus on the copper layer. Optionally, the immersion time for activation treatment is 0.5 min to 5 min. The immersion temperature is 25 to 45℃. The formulation of the activation solution includes: palladium chloride 0.8 g / L to 0.3 g / L, hydrochloric acid 0.8 mL / L to 0.5 mL / L, and 3-methylpyridine 0.05 g / L to 0.2 g / L.

[0066] Optionally, the method for forming the nickel-phosphorus alloy layer on the copper layer is chemical plating, wherein the plating solution, immersion temperature and immersion time of the chemical plating are adjusted so that the thickness of the nickel-phosphorus alloy layer is ≥0.8μm and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt% to 10wt%.

[0067] Optionally, the electroless plating solution is selected from one or more of LA, LM, LD, HSB-97 electroless nickel-phosphorus plating agent A, HSB-97 electroless nickel-phosphorus plating agent B, DK6000A, DK6000B, DK6000C, SXEN-2002MA, and SXEN-2002MB.

[0068] Optionally, the soaking temperature is 70–90°C.

[0069] Preferably, the plating solution, immersion temperature, and immersion time of the electroless plating are adjusted to make the thickness of the nickel-phosphorus alloy layer 0.8 μm to 4 μm. More preferably, the plating solution, immersion temperature, and immersion time of the electroless plating are adjusted to make the thickness of the nickel-phosphorus alloy layer 1 μm to 3.5 μm. Even more preferably, the plating solution, immersion temperature, and immersion time of the electroless plating are adjusted to make the thickness of the nickel-phosphorus alloy layer 1 μm to 2 μm.

[0070] Preferably, the plating solution, immersion temperature, and immersion time of the electroless plating are adjusted so that the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 7wt% to 9wt%.

[0071] Optionally, after forming the nickel-phosphorus alloy layer on the copper layer, the process further includes washing and baking. Baking improves the adhesion between the nickel-phosphorus alloy layer and the copper layer.

[0072] Optionally, the baking temperature is 100–200°C. The baking time is 0.8–2 hours.

[0073] Optionally, the surface treatment may be an etching process and / or a polishing process.

[0074] Optionally, the nickel-phosphorus alloy layer is further etched, and the etching solution, immersion temperature and immersion time are adjusted to make the brightness of the nickel-phosphorus alloy layer 1 GU to 70 GU.

[0075] Optionally, the etching solution is formulated as follows: ammonium chloride 3g / L to 10g / L, aminosulfonic acid 5g / L to 20g / L, and hydrochloric acid 0.5mL / L to 3mL / L.

[0076] Optionally, the soaking temperature is 20–40°C.

[0077] Optionally, after surface treatment of the nickel-phosphorus alloy layer, the process further includes pickling and water washing steps.

[0078] Optionally, the pickling soaking time is 0.5 min to 3 min. The temperature is 20 to 50 °C. The pickling solution is an aqueous solution of an inorganic acid, selected from one or more of sulfuric acid, hydrochloric acid, and nitric acid. The concentration of the pickling solution is 2 wt% to 10 wt%.

[0079] Optionally, the method for forming a silver layer on the nickel-phosphorus alloy layer is electroplating, wherein the electroplating solution is alkaline.

[0080] Alternatively, when electroplating a silver layer, the plating solution can be a silver plating solution produced by Dongguan Metcom Precious Metals Co., Ltd. The pH value of the plating solution is 10–12, the operating temperature is 20–30℃, and the current density is 0.8–2 ASD.

[0081] Optionally, the thickness of the silver layer is ≤5μm. More optionally, the thickness of the silver layer is 0.5μm to 5μm.

[0082] Optionally, after forming a silver layer on the nickel-phosphorus alloy layer, a baking step is also included.

[0083] Optionally, the baking temperature is 100–200°C. The baking time is 1–3 hours.

[0084] In one embodiment, the method for preparing the dielectric ceramic component includes the following steps: sequentially performing degreasing, water washing, micro-etching, water washing, first acid washing, water washing, activation, water washing, nickel-phosphorus alloy plating, water washing, first baking, etching, acid washing, water washing, silver plating, and second baking on a dielectric ceramic substrate with a copper-plated surface.

[0085] The first and second pickling processes follow the pickling steps described above. The first and second baking processes follow the baking steps described above.

[0086] The purpose of water washing is to remove residual liquid from the surface of the intermediate product. Deionized water is used in all of the above water washing steps.

[0087] A dielectric ceramic component includes a dielectric ceramic substrate, a copper layer, a nickel-phosphorus alloy layer, and a silver layer;

[0088] The copper layer is located on the dielectric ceramic substrate;

[0089] The nickel-phosphorus alloy layer is located on top of the copper layer;

[0090] The silver layer is located on top of the nickel-phosphorus alloy layer.

[0091] Alternatively, the dielectric ceramic matrix material may be selected from magnesium titanate, magnesium titanate-calcium titanate, or BaMg. 1 / 3 Ti 2 / 3 O3, BaZn 1 / 3 Ti 2 / 3 O3, Ba(Co,Zn) 1 / 3 Nb 2 / 3 One or more of O3, SrTiO3-LaALO3, magnesium oxide, aluminum oxide, silicon carbide, aluminum nitride, and beryllium oxide may be added as additive phases, such as calcium carbonate / magnesium carbonate.

[0092] Optionally, the thickness of the copper layer is 8 μm to 15 μm. It is understood that the copper layer may be located on part or all of the surface of the dielectric ceramic substrate. Other layers may also be included between the dielectric ceramic substrate and the copper layer.

[0093] In this invention, the thickness of the nickel-phosphorus alloy layer is ≥0.8 μm. Furthermore, the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4 wt% to 10 wt%, and the gloss level of the nickel-phosphorus alloy layer is 1 GU to 70 GU.

[0094] Understandably, the thickness of the nickel-phosphorus alloy layer includes, but is not limited to, 0.8 μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, and 4 μm. Preferably, the thickness of the nickel-phosphorus alloy layer is 0.8 μm to 4 μm; more preferably, the thickness of the nickel-phosphorus alloy layer is 1 μm to 3.5 μm; even more preferably, the thickness of the nickel-phosphorus alloy layer is 1 μm to 2 μm. Furthermore, the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4 wt% to 10 wt%.

[0095] Understandably, the mass percentage of phosphorus in the nickel-phosphorus alloy layer includes, but is not limited to, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, and 10 wt%. Preferably, the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 7 wt% to 9 wt%.

[0096] Optionally, the thickness of the silver layer is ≤5μm. More preferably, the thickness of the silver layer is 0.5μm to 5μm.

[0097] In one embodiment, the dielectric ceramic component of the present invention is a high-frequency dielectric filter.

[0098] The following description, in conjunction with specific embodiments and comparative examples, will provide further details. Unless otherwise specified, all raw materials and instruments used in the following specific embodiments are commercially available. Unless otherwise specified, all processes involved are conventionally selected by those skilled in the art.

[0099] Example 1

[0100] This embodiment provides a dielectric ceramic component and its fabrication method, the steps of which are as follows:

[0101] Step 1: Obtain a dielectric ceramic substrate with copper plating on its surface.

[0102] Step 2: Immerse the intermediate product from Step 1 in a degreasing agent at 50°C for 5 minutes, with auxiliary stirring. The degreasing agent is Degreasing Agent 6169 (provided by Guangdong Dongshuo Technology Co., Ltd.), with a concentration of 3 wt%.

[0103] Step 3: Wash the intermediate product obtained in step 2 twice with deionized water.

[0104] Step 4: Immerse the intermediate product obtained in Step 3 in a micro-etching solution for 1.5 minutes. The micro-etching solution consists of 60 g / L potassium persulfate and 2 wt% sulfuric acid.

[0105] Step 5: Wash the intermediate product obtained in step 4 twice with deionized water.

[0106] Step 6: Immerse the intermediate product obtained in Step 5 in sulfuric acid for pickling. The immersion time is 2 minutes, the temperature is 50°C, and the concentration of sulfuric acid is 5 wt%.

[0107] Step 7: Wash the intermediate product obtained in step 6 twice with deionized water.

[0108] Step 8: Immerse the intermediate product obtained in Step 7 in the activation solution for activation treatment. The immersion time is 1 minute and the immersion temperature is 35℃. The formula of the activation solution includes: palladium chloride 0.2 g / L, hydrochloric acid 0.3 mL / L, and 3-methylpyridine 0.8 g / L.

[0109] Step 9: Wash the intermediate product obtained in step 8 twice with deionized water.

[0110] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 0.8μm. The chemical plating solution formula is: LA 50mL / L, LM 150mL / L, and LD 2mL / L. LA, LM, and LD are L-series nickel-phosphorus plating solutions from Guangdong Dongshuo Technology Co., Ltd. The resulting nickel-phosphorus alloy layer contains 8.5wt% phosphorus.

[0111] Step 11: Wash the intermediate product obtained in step 10 twice with deionized water and bake it at 150°C for 1 hour.

[0112] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 22s. The brightness of the nickel-phosphorus alloy layer is measured to be 70 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0113] Step 13: Place the intermediate product obtained in step 12 into an oven and bake at 150°C for 2 hours. Remove and cool to room temperature.

[0114] Step 14: Immerse the intermediate product obtained in Step 13 in sulfuric acid for pickling treatment. The immersion time is 2 minutes, the temperature is 50°C, and the concentration of sulfuric acid is 5 wt%.

[0115] Step 15: Wash the intermediate product obtained in step 14 twice with deionized water.

[0116] Step 16: Immerse the intermediate product obtained in Step 15 into a silver plating bath for silver plating treatment. The plating solution is provided by Dongguan Metcom Precious Metals Co., Ltd., model BRIGHT-100 series, with a pH value of 11, an operating temperature of 30℃, a current density of 2ASD, and a silver layer thickness of 0.5μm.

[0117] Step 17: Place the intermediate product obtained in Step 16 into an oven and bake at 150°C for 2 hours. Remove and cool to room temperature. Dielectric ceramic components are obtained.

[0118] Example 2

[0119] This embodiment provides a dielectric ceramic component and its preparation method, which is basically the same as that in Embodiment 1, except that step 10 is different, as follows:

[0120] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer electroless plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 4μm. The formulation of the chemical plating solution is: 50mL / L of chemical nickel-phosphorus alloy plating solution LA, 150mL / L of chemical nickel-phosphorus alloy plating solution LM, and 2mL / L of chemical nickel-phosphorus alloy plating solution LD. The resulting nickel-phosphorus alloy layer contains 8.5wt% phosphorus.

[0121] Example 3

[0122] This embodiment provides a dielectric ceramic component and its preparation method, which is basically the same as that in Embodiment 1, except that steps 10, 12, and 16 are different, as detailed below:

[0123] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 1.6μm. The chemical plating solution formula is: 100mL / L of HSB-97 nickel-phosphorus plating agent A and 100mL / L of HSB-97 nickel-phosphorus plating agent B, with a pH of 4.9. HSB-97 nickel-phosphorus plating agent A and HSB-97 nickel-phosphorus plating agent B are provided by Guangdong Dongshuo Technology Co., Ltd. The resulting nickel-phosphorus alloy layer contains 6.5wt% phosphorus.

[0124] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 124s. The brightness of the nickel-phosphorus alloy layer is measured to be 1 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0125] Step 16: Immerse the intermediate product obtained in Step 15 into a silver plating bath for silver plating treatment. The plating solution is provided by Dongguan Metcom Precious Metals Co., Ltd., model BRIGHT-100 series, with a pH value of 11, an operating temperature of 30℃, a current density of 2ASD, and a silver layer thickness of 5μm.

[0126] Example 4

[0127] This embodiment provides a dielectric ceramic component and its preparation method, which is basically the same as that in Embodiment 1, except that steps 10, 12, and 16 are different, as detailed below:

[0128] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 2.5μm. The formulation of the chemical plating solution is: chemical nickel-phosphorus plating solution DK6000A 30mL / L, chemical nickel-phosphorus plating solution DK6000B 35mL / L, and chemical nickel-phosphorus plating solution DK6000C 40mL / L. DK6000A, DK6000B, and DK6000C are from the DK6000 series of nickel-phosphorus plating solutions developed by Guangdong Dongshuo Technology Co., Ltd. The resulting nickel-phosphorus alloy layer contains 5.2wt% phosphorus.

[0129] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 83s. The brightness of the nickel-phosphorus alloy layer is measured to be 38.5 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0130] Step 16: Immerse the intermediate product obtained in Step 15 into a silver plating bath for silver plating treatment. The plating solution is provided by Dongguan Metcom Precious Metals Co., Ltd., model BRIGHT-100 series, with a pH value of 11, an operating temperature of 30℃, a current density of 2ASD, and a silver layer thickness of 2μm.

[0131] Example 5

[0132] This embodiment provides a dielectric ceramic component and its preparation method, which is basically the same as that in Embodiment 1, except that steps 10, 12, and 16 are different, as detailed below:

[0133] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer electroless plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 3.6μm. The formulation of the chemical plating solution is: 30mL / L of chemical nickel-phosphorus alloy plating solution LA, 100mL / L of chemical nickel-phosphorus alloy plating solution LM, and 2mL / L of chemical nickel-phosphorus alloy plating solution LD. The phosphorus content in the resulting nickel-phosphorus alloy layer is 10wt%.

[0134] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 58s. The brightness of the nickel-phosphorus alloy layer is measured to be 53.5 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0135] Step 16: Immerse the intermediate product obtained in Step 15 into a silver plating bath for silver plating treatment. The plating solution is provided by Dongguan Metcom Precious Metals Co., Ltd. The pH value of the plating solution is 11, the operating temperature is 30℃, the current density is 2ASD, and the silver layer thickness is 3.5μm.

[0136] Example 6

[0137] This embodiment provides a dielectric ceramic component and its preparation method, which is basically the same as that in Embodiment 1, except that steps 10, 12, and 16 are different, as detailed below:

[0138] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 0.8μm. The formulation of the chemical plating solution is: chemical nickel-phosphorus plating solution DK6000A 35mL / L, chemical nickel-phosphorus plating solution DK6000B 28mL / L, and chemical nickel-phosphorus plating solution DK6000C 35mL / L. The phosphorus content in the resulting nickel-phosphorus alloy layer is 4wt%.

[0139] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 103s. The brightness of the nickel-phosphorus alloy layer is measured to be 18 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0140] Step 16: Immerse the intermediate product obtained in Step 15 into a silver plating bath for silver plating treatment. The plating solution is provided by Dongguan Metcom Precious Metals Co., Ltd. The pH value of the plating solution is 11, the operating temperature is 30℃, the current density is 2ASD, and the silver layer thickness is 1.7μm.

[0141] Comparative Example 1

[0142] This comparative example provides a dielectric ceramic component and its preparation method, which is basically the same as that in Example 2, except that steps 10 and 12 are different, as detailed below:

[0143] Step 10: Immerse the intermediate product obtained in Step 9 in a nickel plating bath for nickel plating. The plating solution consists of 75 g / L nickel sulfamate and 20 g / L nickel chloride. The pH of the plating solution is 4.2. The nickel sulfamate was provided by Guangdong Guanghua Technology Co., Ltd. The operating temperature is 50℃, the current density is 3 ASD, and the nickel layer thickness is 4 μm.

[0144] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 30s. The brightness of the nickel-phosphorus alloy layer is measured to be 60 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0145] Comparative Example 2

[0146] This comparative example provides a dielectric ceramic component and its preparation method, which is basically the same as that in Example 2, except that steps 10 and 12 are different, as detailed below:

[0147] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 4μm. The chemical plating solution consists of: 100mL / L of SXEN-2002MA and 200mL / L of SXEN-2002MB, with a pH of 7.3. SXEN-2002MA and SXEN-2002MB were provided by Hangzhou Mercury Surface Technology Co., Ltd. The resulting nickel-phosphorus alloy layer contains 2.3wt% phosphorus.

[0148] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 30s. The brightness of the nickel-phosphorus alloy layer is measured to be 65.5 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0149] Comparative Example 3

[0150] This comparative example provides a dielectric ceramic component and its preparation method, which is basically the same as that in Example 2, except that steps 10 and 12 are different, as detailed below:

[0151] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 4μm. The chemical plating solution consists of 100mL / L of SXEN-2002MA and 100mL / L of SXEN-2002MB chemical plating solutions, with a pH of 4.6. The resulting nickel-phosphorus alloy layer contains 13.7wt% phosphorus.

[0152] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 42s. The brightness of the nickel-phosphorus alloy layer is measured to be 70 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0153] Comparative Example 4

[0154] This comparative example provides a dielectric ceramic component and its preparation method, which is basically the same as Example 2, except that step 10 is different, as follows:

[0155] Step 10: Immerse the intermediate product obtained in Step 9 in a chemical plating solution to perform a nickel-phosphorus alloy layer plating treatment. The immersion temperature is 80℃, and the immersion is continued until the thickness of the nickel-phosphorus alloy layer is 0.72μm. The chemical plating solution consists of: LA 50mL / L, LM 150mL / L, and LD 2mL / L. The resulting nickel-phosphorus alloy layer contains 8.5wt% phosphorus.

[0156] Comparative Example 5

[0157] This comparative example provides a dielectric ceramic component and its preparation method, which is basically the same as that in Example 2, except that step 12 is different, as detailed below:

[0158] Step 12: Immerse the intermediate product obtained in Step 11 in an etching solution for nickel etching. The immersion temperature is 25℃ and the immersion time is 10s. The brightness of the nickel-phosphorus alloy layer is measured to be 82.5 GU. The etching solution formula is: ammonium chloride 5g / L, aminosulfonic acid 8g / L, and hydrochloric acid 2mL / L.

[0159] Performance testing

[0160] The dielectric ceramic components prepared in the above embodiments and comparative examples were subjected to performance tests, specifically as follows:

[0161] 1. The adhesion strength between each metal layer is tested using a tensile test method (GB / T 5270-2005 Test Method for Adhesion Strength of Electrodeposited and Chemically Deposited Metallic Coatings on Metallic Substrates). The adhesion strength is the tensile force required to break one or more metal layers under tensile force. Industrially, the adhesion strength between each metal layer must be greater than 20 N / mm². 2 To meet application requirements.

[0162] 2. The dielectric ceramic components were subjected to thermal shock testing (-55℃ to +125℃) using a DeLta GS-TS225 series thermal cycling test chamber. After every 50 shock cycles, the components were removed, the plating appearance was observed, and the reliability of the components was analyzed. Industrially, dielectric ceramic components must withstand more than 1000 thermal shock cycles without discoloration to meet application requirements.

[0163] The specific test results are shown in Table 1.

[0164] Table 1

[0165]

[0166] Results analysis:

[0167] The test results show that when a nickel-phosphorus alloy layer with a thickness of at least 0.8 μm, a phosphorus content of 4 wt% to 10 wt%, and a brightness of 1 GU to 70 GU is added between the copper and silver layers of the dielectric ceramic component, the bonding strength between the metal layers meets the requirements of industrial applications. Regarding reliability, only slight discoloration was observed in Examples 1 and 6, but the reliability of Examples 1 and 6 still meets the requirements of industrial applications. Furthermore, the reliability test results indicate that the corrosion resistance of the nickel-phosphorus alloy layer meets the usage requirements.

[0168] In Comparative Example 1, even with a pure nickel layer thickness of 4 μm, it still failed to prevent the interpenetration of copper and silver under repeated hot and cold washing. Furthermore, when the phosphorus content, brightness, and thickness were outside the aforementioned ranges, the bonding strength between the layers significantly deteriorated, and the dielectric ceramic components exhibited discoloration due to interpenetration between the copper and silver layers after repeated hot and cold shocks, thus compromising their reliability.

[0169] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above 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.

[0170] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A method for preparing a dielectric ceramic component, characterized in that, Includes the following steps: Provides a dielectric ceramic substrate with a copper-plated surface; A nickel-phosphorus alloy layer is formed on the copper layer, wherein the thickness of the nickel-phosphorus alloy layer is 0.8 μm to 4 μm, and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4 wt% to 10 wt%. The nickel-phosphorus alloy layer is surface treated to achieve a gloss level of 1 GU to 70 GU. A silver layer is formed on the surface-treated nickel-phosphorus alloy layer.

2. The method for preparing dielectric ceramic components according to claim 1, characterized in that, The method for forming the nickel-phosphorus alloy layer on the copper layer is chemical plating. The plating solution, immersion temperature and immersion time of the chemical plating are adjusted so that the thickness of the nickel-phosphorus alloy layer is 0.8μm~4μm and the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt%~10wt%.

3. The method for preparing dielectric ceramic components according to claim 2, characterized in that, Adjust the plating solution, immersion temperature, and immersion time of the electroless plating to achieve a nickel-phosphorus alloy layer thickness of 1 μm to 3.5 μm; and / or, The plating solution, immersion temperature, and immersion time of the electroless plating are adjusted so that the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 7wt%~9wt%.

4. The method for preparing dielectric ceramic components according to claim 1, characterized in that, The surface treatment is etching and / or polishing.

5. The method for preparing dielectric ceramic components according to claim 4, characterized in that, The surface treatment is an etching process. The etching solution, immersion temperature and immersion time of the etching process are adjusted so that the brightness of the nickel-phosphorus alloy layer is 1 GU~70 GU.

6. The method for preparing dielectric ceramic components according to claim 1, characterized in that, The method for forming the silver layer on the surface-treated nickel-phosphorus alloy layer is electroplating, wherein the electroplating solution is alkaline.

7. The method for preparing the dielectric ceramic component according to any one of claims 1 to 6, characterized in that, After forming the nickel-phosphorus alloy layer on the copper layer, the process further includes a baking step; and / or, After the silver layer is formed on the surface-treated nickel-phosphorus alloy layer, a baking step is also included.

8. The method for preparing the dielectric ceramic component according to any one of claims 1 to 6, characterized in that, The thickness of the silver layer is ≤5μm.

9. A dielectric ceramic component, characterized in that, It includes a dielectric ceramic substrate, a copper layer, a nickel-phosphorus alloy layer, and a silver layer: The copper layer is located on the dielectric ceramic substrate; The nickel-phosphorus alloy layer is located on top of the copper layer; The silver layer is located on top of the nickel-phosphorus alloy layer; The thickness of the nickel-phosphorus alloy layer is 0.8μm to 4μm, the mass percentage of phosphorus in the nickel-phosphorus alloy layer is 4wt% to 10wt%, and the brightness of the nickel-phosphorus alloy layer is 1GU to 70GU.

10. The dielectric ceramic component according to claim 9, characterized in that, The thickness of the nickel-phosphorus alloy layer is 1 μm to 3.5 μm; and / or, The mass percentage of phosphorus in the nickel-phosphorus alloy layer is 7wt%~9wt%; and / or, The thickness of the silver layer is ≤5μm.

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