A method for thin film low resistance deposition
By acid washing, initial treatment, and activation of the ceramic substrate, and using a specific ratio of nickel plating solution and activation solution, the production problem of high-precision resistors with high stability and low resistance was solved, achieving a thin film coating effect with high stability and low resistance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- YIYANG RUIJIA ELECTRONICS CO LTD
- Filing Date
- 2024-06-24
- Publication Date
- 2026-05-26
AI Technical Summary
Existing technologies are insufficient to produce high-precision resistors with high stability and low resistance values, and the simple nickel plating process cannot meet the requirements for high stability and low resistance.
The ceramic substrate undergoes pickling, pretreatment, and activation. A specific ratio of nickel plating solution and activation solution is used, including the synergistic effect of chitosan solution, sodium dodecylbenzene sulfonate solution, silane coupling agent KH560, hydroxyapatite agent, and bentonite agent. Ultrasonic activation treatment is then applied to enhance the contact effect between the activation solution and the substrate.
This improves the product's temperature coefficient of resistance (TCR), resulting in lower thermal stability, better high-temperature resistance, and corrosion resistance, thus significantly enhancing the product's performance.
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Figure BDA0004908862230000101 
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Abstract
Description
Technical Field
[0001] This invention relates to the field of coating technology, and more specifically to a method for thin-film low-resistivity coating. Background Technology
[0002] Thin-film low-resistivity (less than ohms) coating technology commonly employs chemical nickel plating, which deposits a nickel alloy film with a certain resistance value onto the surface of an alumina ceramic resistor substrate. The thickness of the film determines the resistance value and ensures it meets the resistor's performance requirements. However, simple nickel plating can only meet general low-resistance requirements and struggles to address the demand for high-stability, low-resistance, high-precision resistors. Therefore, this invention provides further improvements to the process. Summary of the Invention
[0003] In view of the deficiencies of the prior art, the purpose of this invention is to provide a thin film low-resistivity coating method to solve the problems mentioned in the background art.
[0004] The present invention solves the technical problem by adopting the following technical solution:
[0005] This invention provides a method for thin-film low-resistivity deposition, comprising the following steps:
[0006] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1-2 hours. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0007] Step 2, Preparation of nickel plating solution:
[0008] The nickel plating solution is prepared by thoroughly mixing 7-12 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0009] Step 3: Plate the activated ceramic substrate with nickel. After the process is complete, remove and dry it.
[0010] Preferably, the initial treatment and activation are carried out by thermal initial treatment at 110°C for 5-10 minutes, followed by activation treatment at 250°C at a rate of 2-4°C / min, holding the temperature for 5 minutes, then air cooling to room temperature, and finally ultrasonic activation treatment in a sufficient amount of activation solution. After activation, the product is washed with water and dried.
[0011] Preferably, the ultrasonic power of the ultrasonic activation treatment is 350-400W, and the ultrasonic time is 10-20min.
[0012] Preferably, the method for preparing the activation solution is as follows:
[0013] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 2-5% of the total amount of chitosan solution of silane coupling agent KH560 and 4-7% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0014] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 350-400W and the immersion time is 10-20min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0015] Preferably, the sodium dodecylbenzenesulfonate solution has a mass fraction of 4-7%; the chitosan solution has a mass fraction of 2-5%; and the yttrium nitrate solution has a mass fraction of 2-5%.
[0016] Preferably, the pH value of the nickel plating treatment is 9-10, and the temperature is 95°C.
[0017] Preferably, 5-10% bentonite agent of total nickel sulfate is also added to the nickel plating solution;
[0018] The preparation method of bentonite agent is as follows:
[0019] Bentonite is first heat-treated at 200-230℃ for 5-10 minutes, then cooled to 55℃ at a rate of 2-5℃ / min and held for 5 minutes. 4-7 parts of the heat-held bentonite, 1-3 parts of stearic acid, 2-5 parts of lanthanum nitrate solution and 2-4 parts of nano-silica sol are then ball-milled. After ball milling, the mixture is washed with water and dried to obtain the bentonite agent.
[0020] Preferably, the lanthanum nitrate solution has a mass fraction of 2-5%.
[0021] Preferably, the ball milling process for the blending ball milling is performed at a speed of 1000 r / min for 2 hours.
[0022] Compared with the prior art, the present invention has the following beneficial effects:
[0023] In this invention, the low-resistivity thin-film coating uses a ceramic substrate treated with an acid solution, followed by initial and activation treatments. The initial and activation processes involve thermal initial treatment at 110°C for 5-10 minutes, followed by activation treatment at 250°C at a rate of 2-4°C / min, holding at this temperature for 5 minutes, and then air cooling to room temperature. Finally, the substrate is placed in a sufficient amount of activation solution for ultrasonic activation treatment. The activation solution is composed of chitosan solution, sodium dodecylbenzenesulfonate solution, silane coupling agent KH560, and hydroxyapatite agent. Through the synergistic effect of the raw materials, the contact effect between the activation solution and the substrate is enhanced, improving the performance of the product. At the same time, the tungsten metal used in electroplating has the characteristics of high temperature resistance, corrosion resistance, low temperature coefficient of resistance (TCR), and good thermal stability. Furthermore, through the synergistic effect of the raw materials, the performance of the product is significantly improved. Detailed Implementation
[0024] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific examples. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0025] This embodiment of a thin-film low-resistivity coating method includes the following steps:
[0026] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1-2 hours. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0027] Step 2, Preparation of nickel plating solution:
[0028] The nickel plating solution is prepared by thoroughly mixing 7-12 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0029] Step 3: Plate the activated ceramic substrate with nickel. After the process is complete, remove and dry it.
[0030] In this embodiment, the initialization and activation are carried out by thermal initialization at 110°C for 5-10 minutes, followed by activation treatment at 250°C at a rate of 2-4°C / min, holding the temperature for 5 minutes, then air cooling to room temperature, and finally ultrasonic activation treatment in a sufficient amount of activation solution. After activation, the product is washed with water and dried.
[0031] In this embodiment, the ultrasonic power for ultrasonic activation treatment is 350-400W, and the ultrasonic time is 10-20min.
[0032] The method for preparing the activation solution in this embodiment is as follows:
[0033] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 2-5% of the total amount of chitosan solution of silane coupling agent KH560 and 4-7% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0034] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 350-400W and the immersion time is 10-20min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0035] In this embodiment, the sodium dodecylbenzenesulfonate solution has a mass fraction of 4-7%; the chitosan solution has a mass fraction of 2-5%; and the yttrium nitrate solution has a mass fraction of 2-5%.
[0036] In this embodiment, the pH value of the nickel plating treatment is 9-10, and the temperature is 95℃.
[0037] In this embodiment, bentonite agent of 5-10% of total nickel sulfate is also added to the nickel plating solution;
[0038] The preparation method of bentonite agent is as follows:
[0039] Bentonite is first heat-treated at 200-230℃ for 5-10 minutes, then cooled to 55℃ at a rate of 2-5℃ / min and held for 5 minutes. 4-7 parts of the heat-held bentonite, 1-3 parts of stearic acid, 2-5 parts of lanthanum nitrate solution and 2-4 parts of nano-silica sol are then ball-milled. After ball milling, the mixture is washed with water and dried to obtain the bentonite agent.
[0040] The lanthanum nitrate solution in this embodiment has a mass fraction of 2-5%.
[0041] In this embodiment, the ball milling process for blending and ball milling is performed at a speed of 1000 r / min for 2 hours.
[0042] Example 1.
[0043] This embodiment of a thin-film low-resistivity coating method includes the following steps:
[0044] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1 hour. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0045] Step 2, Preparation of nickel plating solution:
[0046] The nickel plating solution is prepared by thoroughly mixing 7-12 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0047] Step 3: Plate the activated ceramic substrate with nickel. After the process is complete, remove and dry it.
[0048] In this embodiment, the initialization and activation are carried out by thermal initialization at 110°C for 5-10 minutes, followed by activation treatment at 2°C / min at a rate of 2°C / min, holding the temperature for 5 minutes, then air cooling to room temperature, and finally ultrasonic activation treatment in a sufficient amount of activation solution. After activation, the product is washed with water and dried.
[0049] In this embodiment, the ultrasonic power for ultrasonic activation treatment is 350W, and the ultrasonic time is 10-20min.
[0050] The method for preparing the activation solution in this embodiment is as follows:
[0051] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 2% of the total amount of chitosan solution of silane coupling agent KH560 and 4% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0052] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 350W and the immersion time is 10min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0053] In this embodiment, the sodium dodecylbenzenesulfonate solution has a mass fraction of 4%; the chitosan solution has a mass fraction of 2%; and the yttrium nitrate solution has a mass fraction of 2%.
[0054] In this embodiment, the pH value of the nickel plating treatment is 9, and the temperature is 95°C.
[0055] In this embodiment, bentonite agent of 5-10% of total nickel sulfate is also added to the nickel plating solution;
[0056] The preparation method of bentonite agent is as follows:
[0057] Bentonite was first heat-treated at 200℃ for 5 minutes, then cooled to 55℃ at a rate of 2℃ / min and held for 5 minutes. Four parts of the heat-held bentonite, one part of stearic acid, two parts of lanthanum nitrate solution and two parts of nano-silica sol were mixed and ball-milled. After ball milling, the mixture was washed with water and dried to obtain bentonite agent.
[0058] The lanthanum nitrate solution in this embodiment has a mass fraction of 2%.
[0059] In this embodiment, the ball milling process for blending and ball milling is performed at a speed of 1000 r / min for 2 hours.
[0060] Example 2.
[0061] This embodiment of a thin-film low-resistivity coating method includes the following steps:
[0062] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1-2 hours. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0063] Step 2, Preparation of nickel plating solution:
[0064] The nickel plating solution is prepared by thoroughly mixing 12 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0065] Step 3: Plate the activated ceramic substrate with nickel. After the process is complete, remove and dry it.
[0066] In this embodiment, the initialization and activation are carried out by thermal initialization at 110°C for 5-10 minutes, followed by activation treatment at 250°C at a rate of 4°C / min, holding the temperature for 5 minutes, then air cooling to room temperature, and finally ultrasonic activation treatment in a sufficient amount of activation solution. After activation, the product is washed with water and dried.
[0067] In this embodiment, the ultrasonic power of the ultrasonic activation treatment is 400W and the ultrasonic time is 20min.
[0068] The method for preparing the activation solution in this embodiment is as follows:
[0069] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 5% of the total amount of chitosan solution of silane coupling agent KH560 and 7% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0070] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 400W and the immersion time is 20min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0071] In this embodiment, the sodium dodecylbenzenesulfonate solution has a mass fraction of 7%; the chitosan solution has a mass fraction of 5%; and the yttrium nitrate solution has a mass fraction of 5%.
[0072] In this embodiment, the pH value of the nickel plating treatment is 10, and the temperature is 95°C.
[0073] In this embodiment, bentonite agent of 10% of the total amount of nickel sulfate is also added to the nickel plating solution;
[0074] The preparation method of bentonite agent is as follows:
[0075] Bentonite was first heat-treated at 230℃ for 10 min, then cooled to 55℃ at a rate of 5℃ / min and held for 5 min. 7 parts of the heat-held bentonite, 3 parts of stearic acid, 5 parts of lanthanum nitrate solution and 4 parts of nano-silica sol were then ball-milled. After ball milling, the mixture was washed with water and dried to obtain the bentonite agent.
[0076] The lanthanum nitrate solution in this embodiment has a mass fraction of 5%.
[0077] In this embodiment, the ball milling process for blending and ball milling is performed at a speed of 1000 r / min for 2 hours.
[0078] Example 3.
[0079] This embodiment of a thin-film low-resistivity coating method includes the following steps:
[0080] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1.5 hours. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0081] Step 2, Preparation of nickel plating solution:
[0082] The nickel plating solution is prepared by thoroughly mixing 9 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0083] Step 3: Plate the activated ceramic substrate with nickel. After the treatment is complete, remove and dry it. In this embodiment, the initial treatment and activation are carried out at 110°C for 7.5 minutes, followed by activation treatment at 250°C at a rate of 3°C / min. The activation temperature is held for 5 minutes, then air-cooled to room temperature. Finally, it is placed in a sufficient amount of activation solution for ultrasonic activation treatment. After activation, it is washed with water and dried.
[0084] In this embodiment, the ultrasonic power for ultrasonic activation treatment is 375W, and the ultrasonic time is 15min.
[0085] The method for preparing the activation solution in this embodiment is as follows:
[0086] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 3.5% of the total amount of chitosan solution of silane coupling agent KH560 and 4-7% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0087] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 375W and the immersion time is 15min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0088] In this embodiment, the sodium dodecylbenzenesulfonate solution has a mass fraction of 5.5%; the chitosan solution has a mass fraction of 3.5%; and the yttrium nitrate solution has a mass fraction of 3.5%.
[0089] In this embodiment, the pH value of the nickel plating treatment is 9.5, and the temperature is 95°C.
[0090] In this embodiment, bentonite agent comprising 7.5% of the total nickel sulfate is also added to the nickel plating solution;
[0091] The preparation method of bentonite agent is as follows:
[0092] Bentonite was first heat-treated at 215℃ for 7.5 min, then cooled to 55℃ at a rate of 3.5℃ / min and held for 5 min. 5.5 parts of the heat-held bentonite, 2 parts of stearic acid, 3.5 parts of lanthanum nitrate solution and 3 parts of nano-silica sol were then ball-milled. After ball milling, the mixture was washed with water and dried to obtain the bentonite agent.
[0093] The lanthanum nitrate solution in this embodiment has a mass fraction of 3.5%.
[0094] In this embodiment, the ball milling process for blending and ball milling is performed at a speed of 1000 r / min for 2 hours.
[0095] Example 4.
[0096] This embodiment of a thin-film low-resistivity coating method includes the following steps:
[0097] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1 hour. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0098] Step 2, Preparation of nickel plating solution:
[0099] The nickel plating solution is prepared by thoroughly mixing 8 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0100] Step 3: Plate the activated ceramic substrate with nickel. After the process is complete, remove and dry it.
[0101] In this embodiment, the initialization and activation are carried out by thermal initialization at 110°C for 6 minutes, followed by activation treatment at 250°C at a rate of 3°C / min, holding the temperature for 5 minutes, then air cooling to room temperature, and finally ultrasonic activation treatment in a sufficient amount of activation solution. After activation, the product is washed with water and dried.
[0102] In this embodiment, the ultrasonic power of the ultrasonic activation treatment is 360W, and the ultrasonic time is 12min.
[0103] The method for preparing the activation solution in this embodiment is as follows:
[0104] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 3% of the total amount of chitosan solution of silane coupling agent KH560 and 5% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0105] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 360W and the immersion time is 12min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0106] In this embodiment, the sodium dodecylbenzenesulfonate solution has a mass fraction of 5%; the chitosan solution has a mass fraction of 3%; and the yttrium nitrate solution has a mass fraction of 4%.
[0107] In this embodiment, the pH value of the nickel plating treatment is 9.5, and the temperature is 95°C.
[0108] In this embodiment, bentonite agent comprising 8% of the total nickel sulfate is also added to the nickel plating solution;
[0109] The preparation method of bentonite agent is as follows:
[0110] Bentonite was first heat-treated at 225℃ for 8 minutes, then cooled to 55℃ at a rate of 3℃ / min and held for 5 minutes. Five parts of the heat-held bentonite, two parts of stearic acid, four parts of lanthanum nitrate solution and three parts of nano-silica sol were mixed and ball-milled. After ball milling, the mixture was washed with water and dried to obtain bentonite agent.
[0111] The lanthanum nitrate solution in this embodiment has a mass fraction of 4%.
[0112] In this embodiment, the ball milling process for blending and ball milling is performed at a speed of 1000 r / min for 2 hours.
[0113] Example 5.
[0114] This embodiment of a thin-film low-resistivity coating method includes the following steps:
[0115] Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1.2 hours. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate.
[0116] Step 2, Preparation of nickel plating solution:
[0117] The nickel plating solution is prepared by thoroughly mixing 8 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea.
[0118] Step 3: Plate the activated ceramic substrate with nickel. After the process is complete, remove and dry it.
[0119] In this embodiment, the initialization and activation are carried out by thermal initialization at 110°C for 8 minutes, followed by activation treatment at 250°C at a rate of 3°C / min, holding the temperature for 5 minutes, then air cooling to room temperature, and finally ultrasonic activation treatment in a sufficient amount of activation solution. After activation, the product is washed with water and dried.
[0120] In this embodiment, the ultrasonic power for ultrasonic activation treatment is 390W, and the ultrasonic time is 18min.
[0121] The method for preparing the activation solution in this embodiment is as follows:
[0122] Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:5. Then, 4% of the total amount of chitosan solution of silane coupling agent KH560 and 5% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution.
[0123] The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 395W and the immersion time is 18min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent.
[0124] In this embodiment, the sodium dodecylbenzenesulfonate solution has a mass fraction of 6%; the chitosan solution has a mass fraction of 4%; and the yttrium nitrate solution has a mass fraction of 3%.
[0125] In this embodiment, the pH value of the nickel plating treatment is 10, and the temperature is 95°C.
[0126] In this embodiment, bentonite agent comprising 9% of the total nickel sulfate is also added to the nickel plating solution;
[0127] The preparation method of bentonite agent is as follows:
[0128] Bentonite was first heat-treated at 210℃ for 6 minutes, then cooled to 55℃ at a rate of 3℃ / min and held for 5 minutes. Five parts of the heat-held bentonite, two parts of stearic acid, four parts of lanthanum nitrate solution and three parts of nano-silica sol were mixed and ball-milled. After ball milling, the mixture was washed with water and dried to obtain bentonite agent.
[0129] The lanthanum nitrate solution in this embodiment has a mass fraction of 4%.
[0130] In this embodiment, the ball milling process for blending and ball milling is performed at a speed of 1000 r / min for 2 hours.
[0131] Comparative Example 1.
[0132] Unlike Example 3, no activation solution treatment was used.
[0133] Comparative Example 2.
[0134] Unlike Example 3, no hydroxyapatite agent was added to the activation solution.
[0135] Comparative Example 3.
[0136] Unlike Example 3, hydroxyapatite is used instead of hydroxyapatite.
[0137] Comparative Example 4.
[0138] Unlike Example 3, no bentonite agent was added.
[0139] Comparative Example 5.
[0140] Unlike Example 3, the bentonite agent is directly replaced by bentonite raw material.
[0141] The products of Examples 1-3 and Comparative Examples 1-5 of this invention were placed under 2% hydrochloric acid for 24 hours to test their acid resistance stability. The performance test results are as follows.
[0142]
[0143]
[0144] As can be seen from Examples 1-5 and Comparative Examples 1-5, the products of Examples 1-3 of the present invention have excellent low resistance and significant acid corrosion resistance. The performance of the products deteriorates when the product is not treated with an activation solution, the activation solution is not filled with hydroxyapatite, the hydroxyapatite is replaced with hydroxyapatite, the bentonite is not added, or the bentonite is directly replaced with bentonite raw material. Only when the raw material of the product is obtained by the method of the present invention is the product performance most significant.
[0145] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.
[0146] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A method for depositing a low-resistivity thin film, characterized in that, Includes the following steps: Step 1: First, the ceramic substrate is pickled with 2% hydrochloric acid for 1-2 hours. After pickling, it is then subjected to initial treatment and activation treatment to obtain an activated ceramic substrate. Step 2, Preparation of nickel plating solution: The nickel plating solution is prepared by thoroughly mixing 7-12 g / L nickel sulfate, 15 g / L sodium tungstate, 31.5 g / L sodium hypophosphite, 35 g / L sodium citrate, 2 ml / L ammonia, and 5 g / L thiourea. Step 3: Plate the activated ceramic substrate with nickel. After the treatment is complete, remove and dry it. The initial treatment and activation are carried out by thermal initial treatment at 110℃ for 5-10 minutes, and then the temperature is increased to 250℃ at a rate of 2-4℃ / min for activation treatment. The activation is held at this temperature for 5 minutes, then air-cooled to room temperature. Finally, it is placed in a sufficient amount of activation solution for ultrasonic activation treatment. After activation, it is washed with water and dried. The method for preparing the activation solution is as follows: Chitosan solution was added to sodium dodecylbenzenesulfonate solution at a weight ratio of 2:
5. Then, 2-5% of the total amount of chitosan solution of silane coupling agent KH560 and 4-7% of the total amount of chitosan solution of hydroxyapatite agent were added and stirred thoroughly to obtain an activated solution. The preparation method of hydroxyapatite agent is as follows: hydroxyapatite is immersed in a sufficient amount of yttrium nitrate solution for immersion treatment. The immersion power is 350-400W and the immersion time is 10-20min. After immersion, the solution is filtered and dried to obtain hydroxyapatite agent. The nickel plating solution also contains 5-10% bentonite as a total amount of nickel sulfate; The preparation method of bentonite agent is as follows: Bentonite is first heat-treated at 200-230℃ for 5-10 minutes, then cooled to 55℃ at a rate of 2-5℃ / min and held for 5 minutes. 4-7 parts of the heat-held bentonite, 1-3 parts of stearic acid, 2-5 parts of lanthanum nitrate solution and 2-4 parts of nano-silica sol are then ball-milled. After ball milling, the mixture is washed with water and dried to obtain the bentonite agent.
2. The thin film low-resistivity deposition method according to claim 1, characterized in that, The ultrasonic activation treatment has an ultrasonic power of 350-400W and an ultrasonic time of 10-20min.
3. The thin-film low-resistivity deposition method according to claim 2, characterized in that, The ultrasonic power is 35W and the ultrasonic time is 15min.
4. The thin-film low-resistivity deposition method according to claim 3, characterized in that, The sodium dodecylbenzenesulfonate solution has a mass fraction of 4-7%; the chitosan solution has a mass fraction of 2-5%; and the yttrium nitrate solution has a mass fraction of 2-5%.
5. The thin-film low-resistivity coating method according to claim 1, characterized in that, The nickel plating treatment has a pH value of 9-10 and a temperature of 95℃.
6. The thin-film low-resistivity deposition method according to claim 1, characterized in that, The lanthanum nitrate solution has a mass fraction of 2-5%.
7. The thin-film low-resistivity deposition method according to claim 1, characterized in that, The ball milling process for the blending was carried out at a speed of 1000 r / min for 2 hours.