CN115466995A - Method for improving gold plating thickness uniformity of ceramic substrate surface - Google Patents
Method for improving gold plating thickness uniformity of ceramic substrate surface Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 107
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 103
- 239000000758 substrate Substances 0.000 title claims abstract description 99
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000007747 plating Methods 0.000 title claims abstract description 80
- 239000000919 ceramic Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000009713 electroplating Methods 0.000 claims abstract description 19
- -1 gold ions Chemical class 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000011084 recovery Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000005238 degreasing Methods 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 208000005156 Dehydration Diseases 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- UUWCBFKLGFQDME-UHFFFAOYSA-N platinum titanium Chemical compound [Ti].[Pt] UUWCBFKLGFQDME-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 238000005530 etching Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000006872 improvement Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
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Abstract
Description
技术领域technical field
本发明属于电镀技术领域,进一步来说涉及陶瓷基片表面镀金技术领域,具体来说,涉及一种提高陶瓷基片表面镀金厚度均匀性的方法。The invention belongs to the technical field of electroplating, and further relates to the technical field of gold plating on the surface of ceramic substrates, in particular to a method for improving the thickness uniformity of gold plating on the surface of ceramic substrates.
背景技术Background technique
电镀就是利用电解原理在某些金属表面上镀上一薄层其它金属或合金的过程,金镀层化学性质稳定,不易氧化,接触电阻小,可满足金丝球焊或楔形焊等微组装工艺要求等诸多优点越来越受到青睐,随着微波元器件的不断发展,越来越多的产品表面需要进行镀金处理。金镀层可靠性高,但是成本相对常规的镀镍、镀锡来说高了几十至上百倍,所以如何控制金镀层的均匀性来降低生产成本是镀金需要考虑的一个重要问题。Electroplating is the process of plating a thin layer of other metals or alloys on the surface of certain metals using the principle of electrolysis. The gold coating has stable chemical properties, is not easy to oxidize, and has low contact resistance. It can meet the requirements of micro-assembly processes such as gold wire ball welding or wedge welding. And many other advantages are becoming more and more popular. With the continuous development of microwave components, more and more products need to be gold-plated on the surface. Gold plating is highly reliable, but the cost is tens to hundreds of times higher than conventional nickel plating and tin plating. Therefore, how to control the uniformity of gold plating to reduce production costs is an important issue that needs to be considered for gold plating.
微波元器件基本都是以陶瓷作为基材,陶瓷基片的尺寸为1.5英寸至4英寸。这类陶瓷基片镀金采用直流电源进行挂镀,由于电流的尖端效应,金层厚度的一致性较差,基片的边缘与中心的金层厚度差异较大,对于2英寸方形基片,基片中心达到3μm时候边缘的厚度往往都有4μm,对于贵金属电镀来说一个是造成了成本的浪费,其次厚度不均匀对于后续的刻蚀工艺也会产生影响,过程难以控制导致刻蚀均匀性差,制备成产品后微组装的一致性较差。Microwave components are basically based on ceramics, and the size of the ceramic substrate is 1.5 inches to 4 inches. This type of ceramic substrate is gold-plated with a DC power supply for rack plating. Due to the tip effect of the current, the consistency of the gold layer thickness is poor, and the thickness of the gold layer between the edge and the center of the substrate is quite different. When the center of the chip reaches 3 μm, the thickness of the edge is often 4 μm. For precious metal plating, one is a waste of cost, and secondly, the uneven thickness will also affect the subsequent etching process. The process is difficult to control and the etching uniformity is poor. The consistency of micro-assembly after preparation into products is poor.
目前业内对于提高镀金层的均匀性,有的是采用辅助阳极的方式,这种方式实现起来复杂,而且需经过不断地设计及调整,而且对于不同尺寸的陶瓷基片,需要设计不同形状的辅助阳极,这对于多品种多规格的陶瓷基片镀金生产来说是极其不方便的。有的是通过降低产品电镀时的电流密度,控制金层的沉积速率,来提高镀金层厚度的均匀性,但这种方式一方面会降低生产效率,同时对金层厚度的改善也比较有限。At present, in order to improve the uniformity of the gold-plated layer in the industry, some methods use auxiliary anodes. This method is complicated to implement and requires continuous design and adjustment. For ceramic substrates of different sizes, auxiliary anodes of different shapes need to be designed. This is extremely inconvenient for the gold-plated production of ceramic substrates with many varieties and specifications. Some methods improve the uniformity of the thickness of the gold plating layer by reducing the current density during electroplating of the product and controlling the deposition rate of the gold layer. However, this method will reduce the production efficiency on the one hand, and at the same time, the improvement of the thickness of the gold layer is relatively limited.
有鉴于此,特提出本发明。In view of this, the present invention is proposed.
发明内容Contents of the invention
本发明所要解决的技术问题是:解决现有陶瓷基片镀金层厚度均匀性差,基片与边缘厚度差异大,后续刻蚀难以控制,制备成产品后微组装一致性差的问题,从而提高陶瓷基片镀金的厚度均匀性以及节约成本。The technical problem to be solved by the present invention is to solve the problems of poor uniformity of the thickness of the gold-plated layer of the existing ceramic substrate, large difference in thickness between the substrate and the edge, difficult control of subsequent etching, and poor consistency of micro-assembly after being prepared into products, thereby improving the ceramic substrate. Thickness uniformity of sheet gold plating and cost savings.
本发明的发明构思是:镀槽带循环过滤功能,镀金溶液采用微氰中性镀金体系,阳极采用铂金钛网,对于不同尺寸的陶瓷基片制作了分别制作了专用挂具,镀金工艺流程为镀前处理(除油活化)→预镀金→主镀金→镀后处理(水洗烘干)。从以下三个方面改进镀金层膜厚的均匀性。The inventive concept of the present invention is: the plating tank has a circulation filtering function, the gold-plating solution adopts a slightly cyanide-neutral gold-plating system, the anode adopts a platinum-titanium mesh, and special hangers are made respectively for ceramic substrates of different sizes, and the gold-plating process flow is as follows: Pre-plating treatment (oil removal and activation) → pre-gold plating → main gold plating → post-plating treatment (washing and drying). The uniformity of the film thickness of the gold-plated layer is improved from the following three aspects.
(1)在主镀金槽增加超声功能,在槽子底部放置超声波振板,振板材质为锆,振动频率28KHz~40KHz,功率为1KW~2KW,在电镀金过程中开启超声波振动,目的是利用超声功能来增加镀槽内离子浓度的均匀性,进而提升镀金层膜厚均匀性。(1) Add an ultrasonic function to the main gold-plating tank, place an ultrasonic vibrating plate at the bottom of the tank, the vibrating plate is made of zirconium, the vibration frequency is 28KHz-40KHz, and the power is 1KW-2KW. The ultrasonic vibration is turned on during the electroplating process. Function to increase the uniformity of ion concentration in the plating tank, thereby improving the uniformity of the thickness of the gold-plated layer.
(2)电镀采用采用单脉冲电源,频率为1000Hz~2000Hz,占空为20%~35%,预镀金平均电流密度为0.6A/dm2±0.3A/dm2,主镀金平均电流密度为0.25A/dm2~0.45A/dm2。脉冲电源显示的一般为平均电流,它与脉冲峰值电流的关系为:I(平均电流)=I(峰值电流)×W(占空比)。通过降低占空比,增加电流的关断时间,可以有助于基片周围金离子浓度的恢复时间,从而提升镀金层膜厚均匀性。(2) Electroplating adopts a single pulse power supply, the frequency is 1000Hz-2000Hz, the duty is 20%-35%, the average current density of pre-plating gold is 0.6A/dm 2 ±0.3A/dm 2 , and the average current density of main gold-plating is 0.25 A/dm2~0.45A/dm2. The pulse power supply generally displays the average current, and its relationship with the pulse peak current is: I (average current) = I (peak current) × W (duty cycle). By reducing the duty cycle and increasing the off time of the current, it can help the recovery time of the concentration of gold ions around the substrate, thereby improving the uniformity of the thickness of the gold plating layer.
(3)结合通过单脉冲电源降低占空比调节基片周围金离子浓度的恢复时间,对金离子浓度有一定的要求,不能过高或过低。金离子浓度低会造成允许的电流密度小,金层外观容易出现发红等外观不良,金离子浓度高会造成金的带出多,同时浓度太高也会使降低溶液的深镀能力,所以金离子含量应控制在一个比较稳定的范围。通过理论指南与试验验证相结合的原则,把主镀金溶液的金离子含量(金离子浓度)控制在7g/L~9g/L时,在保证生产效率的同时,溶液的分散和均镀能力也是比较良好的,从而可以提升镀金层膜厚均匀性。(3) Combined with reducing the duty cycle of the single pulse power supply to adjust the recovery time of the concentration of gold ions around the substrate, there are certain requirements for the concentration of gold ions, which cannot be too high or too low. A low concentration of gold ions will result in a small allowable current density, and the appearance of the gold layer is prone to redness and other poor appearance. A high concentration of gold ions will cause more gold to be brought out. At the same time, if the concentration is too high, the deep plating ability of the solution will be reduced. The gold ion content should be controlled in a relatively stable range. Through the principle of combining theoretical guidance and experimental verification, when the gold ion content (gold ion concentration) of the main gold plating solution is controlled at 7g/L to 9g/L, while ensuring production efficiency, the dispersion and throwing ability of the solution are also improved. Relatively good, so that the thickness uniformity of the gold-plated layer can be improved.
通过这三个方面改进,在不影响生产效率的同时,提高了镀金层膜厚的均匀性,节约了生产成本,也提高了产品后续微组装的一致性。通过此技术方案进行电镀金,对于2英寸方片金层厚度可达到不均匀度<5%,金层厚度的变异系数COV<2%,对于4英寸方片不均匀度<6%,金层厚度的变异系数COV<3%。Through these three aspects of improvement, without affecting the production efficiency, the uniformity of the film thickness of the gold plating layer is improved, the production cost is saved, and the consistency of the subsequent micro-assembly of the product is also improved. Through this technical scheme for electroplating gold, the thickness of the gold layer for a 2-inch square sheet can achieve a non-uniformity <5%, and the coefficient of variation COV of the thickness of the gold layer is <2%. For a 4-inch square sheet, the unevenness of the gold layer is <6%. Coefficient of variation of thickness COV<3%.
为此,本发明提供一种提高陶瓷基片表面电镀金厚度均匀性的方法,包括如下步骤:For this reason, the invention provides a kind of method that improves the thickness uniformity of electroplated gold on ceramic substrate surface, comprises the steps:
第1步:把已溅射一层薄金的1.5英寸至4英寸的陶瓷基片装上专用挂具后,挂具为紫铜材质,整体包胶,挂钩接触部位露出;Step 1: After installing the 1.5-inch to 4-inch ceramic substrate that has been sputtered with a thin layer of gold on the special hanger, the hanger is made of red copper, the whole is covered with glue, and the contact part of the hook is exposed;
第2步进行有机溶剂除油,采用分析纯丙酮超声除油,基片需完全浸没在丙酮溶液里,超声频率为28KHz~40KHz,电流为1A~5A,浸泡时间为3分钟~6分钟;The second step is to degrease the organic solvent, use analytical pure acetone to degrease, the substrate must be completely immersed in the acetone solution, the ultrasonic frequency is 28KHz ~ 40KHz, the current is 1A ~ 5A, and the soaking time is 3 minutes ~ 6 minutes;
第3步:清洗基片,采用去离子水水洗两次,每次清洗时间为90s~180s,目的是为了去除基片表面的残留丙酮;Step 3: Clean the substrate, wash twice with deionized water, each cleaning time is 90s ~ 180s, the purpose is to remove the residual acetone on the surface of the substrate;
第4步:进行碱性化学溶剂电解除油,溶液配比为氢氧化钠18g/L~22g/L,碳酸钠22g/L~28g/L,硅酸钠4g/L,温度为55℃~65℃阴极电解除油4分钟~6分钟,电流密度为1.8A/dm2~2.2A/dm2,目的是为了进一步去除基片表面的油污,获得洁净活性的表面。Step 4: Carry out alkaline chemical solvent electrolytic degreasing, the solution ratio is sodium hydroxide 18g/L~22g/L, sodium carbonate 22g/L~28g/L, sodium silicate 4g/L, the temperature is 55℃~ Cathodic electrolytic degreasing at 65°C for 4 to 6 minutes, with a current density of 1.8A/dm 2 to 2.2A/dm 2 , the purpose is to further remove oil stains on the surface of the substrate and obtain a clean and active surface.
第5步:清洗基片表面残留的碱性除油液,采用两次去离子水水洗,每次清洗时间为90s~180s;Step 5: Clean the residual alkaline degreasing liquid on the surface of the substrate, and wash with deionized water twice, each cleaning time is 90s ~ 180s;
第6步:用浓度为30g/L~60g/L柠檬酸进行活化3分钟~5分钟,目的是为了去除基片金属表面的氧化膜,对金属表面进行活化,使待镀基片表面露出活性表面;Step 6: Activate with citric acid with a concentration of 30g/L~60g/L for 3 minutes to 5 minutes, the purpose is to remove the oxide film on the metal surface of the substrate, activate the metal surface, and expose the active surface of the substrate to be plated. surface;
第7步:清洗基片表面残留的活化液,采用三次去离子水洗,每次清洗时间为90s~180s;Step 7: Clean the residual activation solution on the surface of the substrate by washing with deionized water three times, each cleaning time is 90s ~ 180s;
第8步:预镀金,采用单脉冲电源,频率为1000Hz~2000Hz,占空为20%~35%,电流密度为0.3A/dm2~0.9A/dm2,时间为30S,预镀金的作用主要是提高镀层结合力和防止污染主镀金槽;Step 8: Pre-plating gold, using a single pulse power supply, the frequency is 1000Hz ~ 2000Hz, the duty is 20% ~ 35%, the current density is 0.3A/dm2 ~ 0.9A/dm2, the time is 30S, the role of pre-plating gold is mainly Improve the bonding force of the coating and prevent pollution of the main gold plating tank;
第9步:开启主镀金槽的超声,振动频率为28KHz~40KHz,超声电流为1A~5A;Step 9: Turn on the ultrasonic of the main gold-plating tank, the vibration frequency is 28KHz-40KHz, and the ultrasonic current is 1A-5A;
第10步:主镀金,采用单脉冲电源,频率为1000Hz~2000Hz,占空为20%~35%,电流密度为0.25A/dm2~0.45A/dm2,电镀时间为5min~30min。Step 10: Main gold plating, using a single pulse power supply, the frequency is 1000Hz-2000Hz, the duty is 20%-35%, the current density is 0.25A/dm2-0.45A/dm2, and the plating time is 5min-30min.
第11步:清洗基片,去除基片表面残留的镀金溶液,采用两次去离子水洗,每次清洗时间为90s~180s;Step 11: Clean the substrate, remove the residual gold plating solution on the surface of the substrate, and wash with deionized water twice, each cleaning time is 90s~180s;
第12步:进一步清洗基片表面,用超声去离子热水洗,温度为58℃~62℃,超声频率为28KHz~40KHz,超声电流为1A~5A,清洗时间为90s~180s;Step 12: Further clean the surface of the substrate, wash with ultrasonic deionized hot water, the temperature is 58°C-62°C, the ultrasonic frequency is 28KHz-40KHz, the ultrasonic current is 1A-5A, and the cleaning time is 90s-180s;
第13步:采用分析纯无水乙醇进行脱水处理,时间为10s~30s,脱水后把基片放置于烘干夹具上;Step 13: Use analytical pure ethanol for dehydration treatment for 10s to 30s, and place the substrate on the drying jig after dehydration;
第14步:对基片进行烘干处理,温度为65℃~75℃,烘干时间为10min~30min,烘干后装袋;Step 14: Dry the substrate at a temperature of 65°C to 75°C and a drying time of 10min to 30min, and pack it into bags after drying;
第15步:测量金层厚度,对于电镀金后的每片厚度采用Fisher X射线膜厚仪器进行测量,采用9点法测量,如图1所示。Step 15: Measure the thickness of the gold layer. The thickness of each piece after electroplating gold is measured with a Fisher X-ray film thickness instrument, and the 9-point method is used for measurement, as shown in Figure 1.
不均匀度=[(T最大值-T最小值)/(2×T平均值)]×100%Unevenness = [(T maximum value - T minimum value )/(2×T average value )]×100%
式中T平均值为测量金层的平均厚度,T最大值、T最小值为金层厚度的最大值与最小值,n为测量点数,COV为金层厚度的变异系数。不均匀度和COV值越小说明电镀金层的厚度均匀性越好。In the formula, the average value of T is the average thickness of the measured gold layer, the maximum value of T and the minimum value of T are the maximum and minimum values of the thickness of the gold layer, n is the number of measurement points, and COV is the coefficient of variation of the thickness of the gold layer. The smaller the unevenness and the COV value, the better the thickness uniformity of the electroplated gold layer.
技术效果:Technical effect:
1.通过超声波的空化效应,加强溶液的搅拌作用,提升镀金溶液离子浓度的均匀性;1. Through the cavitation effect of ultrasonic waves, the stirring effect of the solution is strengthened, and the uniformity of the ion concentration of the gold plating solution is improved;
2.通过采用单脉冲电源的方式,使电镀时候的电流是间断通电的,使得基片周围的金离子浓度有恢复的时间,通过调节占空比和频率,因为镀金溶液中金离子浓度本身不高,使基片周围的金离子浓度一直保持在稳定的范围。2. By adopting a single pulse power supply, the current during electroplating is intermittently energized, so that the concentration of gold ions around the substrate has time to recover. By adjusting the duty cycle and frequency, the concentration of gold ions in the gold-plating solution itself does not change. High, so that the concentration of gold ions around the substrate has been kept in a stable range.
3.通过控制镀金溶液的金离子浓度为7g/L~9g/L,使镀金溶液具有良好分散性和均镀能力,提升镀金层膜厚的均匀性,提高产品质量一致性和生产效率。因为金离子浓度低会造成允许的电流密度小,金层外观容易出现发红等外观不良,金离子浓度高会造成金的带出多,同时浓度太高也会使降低溶液的深镀能力,所以金离子含量应控制在7g/L~9g/L,是比较稳定的范围。3. By controlling the gold ion concentration of the gold-plating solution to 7g/L-9g/L, the gold-plating solution has good dispersibility and throwing ability, improves the uniformity of the gold-plated film thickness, and improves product quality consistency and production efficiency. Because the low gold ion concentration will cause the allowable current density to be small, the appearance of the gold layer is prone to redness and other poor appearance, and the high gold ion concentration will cause more gold to be brought out. At the same time, if the concentration is too high, the deep plating ability of the solution will be reduced. Therefore, the gold ion content should be controlled at 7g/L-9g/L, which is a relatively stable range.
本发明广泛应用于陶瓷基片的表面镀金,用于提升镀金层的均匀性,达到节约成本以及提升后续微组装一致性的目的。The invention is widely applied to the surface gold plating of ceramic substrates, and is used for improving the uniformity of the gold plating layer, achieving the purpose of saving costs and improving the consistency of subsequent micro-assembly.
附图说明Description of drawings
图1为测试点分布示意图。Figure 1 is a schematic diagram of the test point distribution.
具体实施方式detailed description
所述一种提高陶瓷基片表面镀金厚度均匀性的方法,具体实施方式如下:Described a kind of method that improves the thickness uniformity of gold plating on the ceramic substrate surface, the specific implementation method is as follows:
实施案列1:Implementation case 1:
2英寸方形99%氧化铝陶瓷基片(50.8mm×50.8mm×0.5mm)电镀金,种子层为TiW/Ni/Au,单挂片数为8片,金层厚度要求为3μm~4μm。2-inch square 99% alumina ceramic substrate (50.8mm×50.8mm×0.5mm) is electroplated with gold, the seed layer is TiW/Ni/Au, the number of single hanging pieces is 8 pieces, and the thickness of the gold layer is required to be 3 μm to 4 μm.
第1步:把已溅射一层薄金的2英寸陶瓷基片装上专用挂具后,挂具为紫铜材质,整体包胶,挂钩接触部位露出;Step 1: After installing the 2-inch ceramic substrate that has been sputtered with a thin layer of gold on the special hanger, the hanger is made of red copper, the whole is covered with glue, and the contact part of the hook is exposed;
第2步进行有机溶剂除油,采用分析纯丙酮超声除油,基片需完全浸没在丙酮溶液里,超声频率为40KHz,电流为2.5A,浸泡时间为5分钟;The second step is to carry out organic solvent degreasing, using analytical pure acetone for ultrasonic degreasing, the substrate must be completely immersed in the acetone solution, the ultrasonic frequency is 40KHz, the current is 2.5A, and the soaking time is 5 minutes;
第3步:清洗基片,采用去离子水水洗两次,每次清洗时间为2分钟,目的是为了去除基片表面的残留丙酮;Step 3: Clean the substrate, wash twice with deionized water, each cleaning time is 2 minutes, the purpose is to remove residual acetone on the surface of the substrate;
第4步:进行碱性化学溶剂电解除油,溶液配比为氢氧化钠18g/L~22g/L,碳酸钠22g/L~28g/L,硅酸钠4g/L,温度为55℃~65℃阴极电解除油4分钟~6分钟,电流密度为1.8A/dm2~2.2A/dm2,目的是为了进一步去除基片表面的油污,获得洁净活性的表面;Step 4: Carry out alkaline chemical solvent electrolytic degreasing, the solution ratio is sodium hydroxide 18g/L~22g/L, sodium carbonate 22g/L~28g/L, sodium silicate 4g/L, the temperature is 55℃~ Cathodic electrolytic degreasing at 65°C for 4 to 6 minutes, with a current density of 1.8A/dm2 to 2.2A/dm2, the purpose is to further remove the oil on the surface of the substrate and obtain a clean and active surface;
第5步:清洗基片表面残留的碱性除油液,采用两次去离子水水洗,每次清洗时间为2分钟;Step 5: Clean the residual alkaline degreasing liquid on the surface of the substrate, and wash with deionized water twice, each cleaning time is 2 minutes;
第6步:用浓度为30g/L~60g/L柠檬酸,活化3分钟~5分钟,目的是为了去除基片金属表面的氧化膜,对金属表面进行活化,使待镀基片表面露出活性表面;Step 6: Use citric acid with a concentration of 30g/L~60g/L to activate for 3 minutes to 5 minutes. The purpose is to remove the oxide film on the metal surface of the substrate, activate the metal surface, and expose the active surface of the substrate to be plated. surface;
第7步:清洗基片表面残留的活化液,采用三次去离子水洗,每次清洗时间为2分钟;Step 7: Clean the residual activation solution on the surface of the substrate by washing with deionized water three times, each time for 2 minutes;
第8步:预镀金,采用单脉冲电源,频率为1500Hz,占空比为30%,电流密度为0.6A/dm2,时间为30S,预镀金的作用主要是提高镀层结合力和防止污染主镀金槽;Step 8: Pre-plating gold, using a single pulse power supply, the frequency is 1500Hz, the duty cycle is 30%, the current density is 0.6A/dm 2 , and the time is 30S. The role of pre-plating gold is mainly to improve the bonding force of the coating and prevent pollution. gold-plated tank;
第9步:开启主镀金槽的超声,振动频率为40KHz,超声电流为1.8A;Step 9: Turn on the ultrasonic of the main gold-plating tank, the vibration frequency is 40KHz, and the ultrasonic current is 1.8A;
第10步:主镀金,采用单脉冲电源,频率为1500Hz,占空比未30%,电流密度为0.35A/dm2,电镀时间为15分钟;Step 10: For main gold plating, use a single pulse power supply with a frequency of 1500Hz, a duty cycle of 30%, a current density of 0.35A/dm 2 , and an electroplating time of 15 minutes;
第11步:清洗基片,去除基片表面残留的镀金溶液,采用两次去离子水洗,每次清洗时间为2分钟;Step 11: Clean the substrate, remove the residual gold plating solution on the surface of the substrate, and wash with deionized water twice, each cleaning time is 2 minutes;
第12步:进一步清洗基片表面,用超声去离子热水洗,温度为58℃~62℃,超声频率为40KHz,超声电流为3A,清洗时间为2分钟;Step 12: further clean the surface of the substrate, wash with ultrasonic deionized hot water, the temperature is 58 ℃ ~ 62 ℃, the ultrasonic frequency is 40KHz, the ultrasonic current is 3A, and the cleaning time is 2 minutes;
第13步:采用分析纯无水乙醇进行脱水处理,时间为10s~30s,脱水后把基片放置于烘干夹具上;Step 13: Use analytical pure ethanol for dehydration treatment for 10s to 30s, and place the substrate on the drying jig after dehydration;
第14步:对基片进行烘干处理,温度为65℃~75℃,烘干时间为20分钟,烘干后装袋;Step 14: Dry the substrate at a temperature of 65°C to 75°C for 20 minutes, and bag it after drying;
第15步:测量金层厚度,对于电镀金后的每片厚度采用Fisher X射线膜厚仪器进行测量,采用如图书所示的9点法测量,测量数据见表1。Step 15: Measure the thickness of the gold layer. For the thickness of each piece after electroplating, use a Fisher X-ray film thickness instrument to measure, and use the 9-point method as shown in the book. The measurement data is shown in Table 1.
表1 2寸方片膜厚数据Table 1 2-inch square film thickness data
通过公式计算可以得出:T平均值=3.55μm,T最大值=3.62μm,T最小值=3.36μm,不均匀度=3.66%,COV=1.4%。Calculated by the formula, it can be obtained that the average value of T=3.55 μm, the maximum value of T=3.62 μm, the minimum value of T=3.36 μm, the unevenness=3.66%, and the COV=1.4%.
可以看出2寸方片通过此方案电镀出来的金层膜厚均匀性较好,不均匀度为3.66%,COV为1.4%。It can be seen that the thickness uniformity of the gold layer electroplated on the 2-inch square piece by this scheme is relatively good, the unevenness is 3.66%, and the COV is 1.4%.
实施案列2:Implementation case 2:
4英寸方形99%氧化铝陶瓷基片(101.6mm×101.6mm×0.5mm)电镀金,种子层为TaN/TiW/Au,金层厚度要求为4μm~5μm。A 4-inch square 99% alumina ceramic substrate (101.6mm×101.6mm×0.5mm) is electroplated with gold, the seed layer is TaN/TiW/Au, and the thickness of the gold layer is required to be 4 μm to 5 μm.
第1步:把已溅射一层薄金的4英寸陶瓷基片装上专用挂具后,挂具为紫铜材质,整体包胶,挂钩接触部位露出;Step 1: After installing the 4-inch ceramic substrate that has been sputtered with a thin layer of gold on the special hanger, the hanger is made of red copper, the whole is covered with glue, and the contact part of the hook is exposed;
第2步进行有机溶剂除油,采用分析纯丙酮超声除油,基片需完全浸没在丙酮溶液里,超声频率为40KHz,电流为2.5A,浸泡时间为5分钟;The second step is to carry out organic solvent degreasing, using analytical pure acetone for ultrasonic degreasing, the substrate must be completely immersed in the acetone solution, the ultrasonic frequency is 40KHz, the current is 2.5A, and the soaking time is 5 minutes;
第3步:清洗基片,采用去离子水水洗两次,每次清洗时间为2分钟,目的是为了去除基片表面的残留丙酮;Step 3: Clean the substrate, wash twice with deionized water, each cleaning time is 2 minutes, the purpose is to remove residual acetone on the surface of the substrate;
第4步:进行碱性化学溶剂电解除油,溶液配比为氢氧化钠18g/L~22g/L,碳酸钠22g/L~28g/L,硅酸钠4g/L,温度为55℃~65℃阴极电解除油4分钟~6分钟,电流密度为1.8A/dm2~2.2A/dm2,目的是为了进一步去除基片表面的油污,获得洁净活性的表面。Step 4: Carry out alkaline chemical solvent electrolytic degreasing, the solution ratio is sodium hydroxide 18g/L~22g/L, sodium carbonate 22g/L~28g/L, sodium silicate 4g/L, the temperature is 55℃~ Cathodic electrolytic degreasing at 65°C for 4 to 6 minutes, with a current density of 1.8A/dm2 to 2.2A/dm2. The purpose is to further remove the oil on the surface of the substrate and obtain a clean and active surface.
第5步:清洗基片表面残留的碱性除油液,采用两次去离子水水洗,每次清洗时间为2分钟;Step 5: Clean the residual alkaline degreasing liquid on the surface of the substrate, and wash with deionized water twice, each cleaning time is 2 minutes;
第6步:用浓度为30g/L~60g/L柠檬酸,活化3分钟~5分钟,目的是为了去除基片金属表面的氧化膜,对金属表面进行活化,使待镀基片表面露出活性表面;Step 6: Use citric acid with a concentration of 30g/L~60g/L to activate for 3 minutes to 5 minutes. The purpose is to remove the oxide film on the metal surface of the substrate, activate the metal surface, and expose the active surface of the substrate to be plated. surface;
第7步:清洗基片表面残留的活化液,采用三次去离子水洗,每次清洗时间为2分钟;Step 7: Clean the residual activation solution on the surface of the substrate by washing with deionized water three times, each time for 2 minutes;
第8步:预镀金,采用单脉冲电源,频率为1200Hz,占空比为25%,电流密度为0.6A/dm2,时间为30S,预镀金的作用主要是提高镀层结合力和防止污染主镀金槽;Step 8: Pre-plating gold, using single pulse power supply, frequency 1200Hz, duty cycle 25%, current density 0.6A/dm 2 , time 30S, the function of pre-plating gold is mainly to improve the bonding force of the coating and prevent pollution. gold-plated tank;
第9步:开启主镀金槽的超声,振动频率为40KHz,超声电流为2A;Step 9: Turn on the ultrasonic of the main gold-plating tank, the vibration frequency is 40KHz, and the ultrasonic current is 2A;
第10步:主镀金,采用单脉冲电源,频率为1200Hz,占空比未25%,电流密度为0.32A/dm2电镀时间为15分钟。Step 10: For main gold plating, use a single pulse power supply with a frequency of 1200Hz, a duty cycle of 25%, a current density of 0.32A/dm 2 and a plating time of 15 minutes.
第11步:清洗基片,去除基片表面残留的镀金溶液,采用两次去离子水洗,每次清洗时间为2分钟;Step 11: Clean the substrate, remove the remaining gold plating solution on the surface of the substrate, and wash with deionized water twice, each cleaning time is 2 minutes;
第12步:进一步清洗基片表面,用超声去离子热水洗,温度为58℃~62℃,超声频率为40KHz,超声电流为3A,清洗时间为2分钟;Step 12: further clean the surface of the substrate, wash with ultrasonic deionized hot water, the temperature is 58 ℃ ~ 62 ℃, the ultrasonic frequency is 40KHz, the ultrasonic current is 3A, and the cleaning time is 2 minutes;
第13步:采用分析纯无水乙醇进行脱水处理,时间为10s~30s,脱水后把基片放置于烘干夹具上;Step 13: Use analytical pure ethanol for dehydration treatment for 10s to 30s, and place the substrate on the drying jig after dehydration;
第14步:对基片进行烘干处理,温度为65℃~75℃,烘干时间为20分钟,烘干后装袋;Step 14: Dry the substrate at a temperature of 65°C to 75°C for 20 minutes, and bag it after drying;
第15步:测量金层厚度,对于电镀金后的每片厚度采用Fisher X射线膜厚仪器进行测量,采用如图1所示的9点法测量,测量数据见表2。Step 15: Measure the thickness of the gold layer. The thickness of each piece after electroplating is measured with a Fisher X-ray film thickness instrument. The 9-point method shown in Figure 1 is used for measurement, and the measurement data are shown in Table 2.
表2 4寸方片膜厚测试数据Table 2 4-inch square film thickness test data
通过公式计算可以得出:T平均值=4.57μm,T最大值=4.81μm,T最小值=4.32μm,不均匀度=5.36%,COV=2.97%。Calculated by the formula, it can be obtained that the average value of T=4.57 μm, the maximum value of T=4.81 μm, the minimum value of T=4.32 μm, the unevenness=5.36%, and the COV=2.97%.
可以看出4寸方片通过此方案电镀出来的金层膜厚均匀性较好,不均匀度为5.36%,COV为2.97%。It can be seen that the thickness uniformity of the gold layer electroplated by this scheme on the 4-inch square sheet is relatively good, with an unevenness of 5.36% and a COV of 2.97%.
最后应说明的是:上述实施例仅仅是为清楚地说明所作的举例,本发明包括但不限于以上实施例,这里无需也无法对所有的实施方式予以穷举。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。凡符合本发明要求的实施方案均属于本发明的保护范围。Finally, it should be noted that the above-mentioned embodiments are only examples for clear description, and the present invention includes but is not limited to the above-mentioned embodiments, and it is not necessary and impossible to exhaustively describe all implementation modes here. For those of ordinary skill in the art, on the basis of the above description, other changes or changes in different forms can also be made. All implementations that meet the requirements of the present invention belong to the protection scope of the present invention.
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