CN104790001A - Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt - Google Patents
Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt Download PDFInfo
- Publication number
- CN104790001A CN104790001A CN201510173706.2A CN201510173706A CN104790001A CN 104790001 A CN104790001 A CN 104790001A CN 201510173706 A CN201510173706 A CN 201510173706A CN 104790001 A CN104790001 A CN 104790001A
- Authority
- CN
- China
- Prior art keywords
- tantalum
- coating
- electroplating
- tantalum coating
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 84
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000011248 coating agent Substances 0.000 title claims abstract description 51
- 238000000576 coating method Methods 0.000 title claims abstract description 51
- 150000003839 salts Chemical class 0.000 title claims abstract description 41
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 33
- 239000010959 steel Substances 0.000 title claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 title abstract description 23
- 238000000034 method Methods 0.000 title abstract description 20
- 229910019932 CrNiMo Inorganic materials 0.000 title abstract description 8
- 238000009713 electroplating Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 230000004913 activation Effects 0.000 claims abstract description 10
- 238000007747 plating Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000004070 electrodeposition Methods 0.000 abstract description 8
- 239000000758 substrate Substances 0.000 abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000005496 eutectics Effects 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 229910002060 Fe-Cr-Al alloy Inorganic materials 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000002679 ablation Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005468 ion implantation Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013060 biological fluid Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Landscapes
- Electroplating And Plating Baths Therefor (AREA)
Abstract
本发明公开了一种中碳CrNiMo钢表面熔盐镀钽涂层及其制备方法。以含有稀土的活化液对钢镀面进行活化处理，作为阴极，以99.97%的高纯钽片为阳极，将钽源熔融于混合盐中。反应条件为：低真空条件0.02~0.1MPa，700~950°C，恒流电源的稳流模式下，在70~100mA/cm2下电镀3~5h，即可在经过活化处理的钢上获得一层金属钽涂层。本发明采用的稀土活化熔融盐电沉积镀钽方法可在低真空和大气环境下进行，对设备要求较低，成本低廉，操作简单，且反应过程中不需要有害气体，也不产生有害物质，对环境友好，用本方法制备得到的钽镀层较为致密，涂层与基体结合良好，厚度均匀。
The invention discloses a molten salt plating tantalum coating on the surface of medium-carbon CrNiMo steel and a preparation method thereof. The steel plated surface is activated with an activation solution containing rare earth, as the cathode, and 99.97% high-purity tantalum sheet as the anode, and the tantalum source is melted in the mixed salt. The reaction conditions are: low vacuum condition 0.02~0.1MPa, 700~950°C, under the constant current mode of the constant current power supply, electroplating at 70~100mA/ cm2 for 3~5h, it can be obtained on the activated steel A metallic tantalum coating. The rare earth activated molten salt electrodeposition tantalum plating method adopted in the present invention can be carried out in a low vacuum and atmospheric environment, has low requirements on equipment, low cost, simple operation, and does not require harmful gases and does not produce harmful substances during the reaction process. The method is friendly to the environment, and the tantalum coating prepared by the method is relatively dense, and the coating is well bonded to the substrate, and the thickness is uniform.
Description
技术领域 technical field
本发明涉及一种中碳CrNiMo钢表面熔盐镀钽涂层及其制备方法，在低真空条件下可在经活化处理的中碳CrNiMo钢表面利用熔融盐电镀获得钽涂层，可以提高其耐烧蚀磨损和耐腐蚀性能，延长其服役寿命。 The invention relates to a molten salt plating tantalum coating on the surface of medium-carbon CrNiMo steel and a preparation method thereof. The tantalum coating can be obtained by molten salt electroplating on the surface of medium-carbon CrNiMo steel after activation treatment under low vacuum conditions, which can improve its resistance Ablative wear and corrosion resistance, prolonging its service life.
背景技术 Background technique
钽具有优良的耐腐蚀性能，在室温条件下能抵御除氢氟酸以外的一切无机酸（包括王水）的侵蚀，且氢氟酸对其腐蚀也非常缓慢，常被用来制造多种高级的耐酸设备和在腐蚀介质环境下的热交换器、加热器等设备。钽在生物体内极其稳定,在常温及各种生物体液环境中均不溶解和腐蚀,也不发生化学反应，并且生物组织易于在钽植入物表面生长，因此，钽也被称为“亲生物金属”。此外，钽以高熔点著称，它的熔点高达3000°C，广泛应用于高温合金、硬质合金、化工容器等多种民用和军事领域。钽涂层良好的耐腐蚀性能与高熔点特性以及良好的机械性能，可以赋予钢材如PCrNi3Mo、25Cr3Mo3NiNb等良好的高温摩擦学性能，可应用于高温摩擦工况下的器件，如火箭发动机喷管、火炮身管、活塞环等，以提高其表面抗氧化和耐烧蚀的性能。 Tantalum has excellent corrosion resistance. It can resist the corrosion of all inorganic acids (including aqua regia) except hydrofluoric acid at room temperature, and hydrofluoric acid corrodes it very slowly. It is often used to make a variety of high-grade Advanced acid-resistant equipment and heat exchangers, heaters and other equipment in corrosive medium environments. Tantalum is extremely stable in living organisms. It does not dissolve and corrode at room temperature and in various biological fluid environments, and does not undergo chemical reactions, and biological tissues are easy to grow on the surface of tantalum implants. Therefore, tantalum is also called "biophilic". Metal". In addition, tantalum is famous for its high melting point, its melting point is as high as 3000°C, and it is widely used in various civil and military fields such as superalloys, hard alloys, and chemical containers. The good corrosion resistance, high melting point and good mechanical properties of tantalum coating can endow steel materials such as PCrNi3Mo, 25Cr3Mo3NiNb, etc. with good high-temperature tribological properties, and can be applied to devices under high-temperature friction conditions, such as rocket engine nozzles, Cannon barrels, piston rings, etc., to improve their surface oxidation resistance and ablation resistance.
目前制备钽涂层的方法主要有：磁控溅射、化学气相沉积、等离子喷涂、离子注入。磁控溅射设备昂贵、工艺复杂且钽薄层由于溅射温度较低，钽膜与基体的结合属于物理结合，结合强度不高；化学气相沉积制备的钽涂层质量不佳，而且当沉积温度较高时，对基体材料的影响较大；等离子喷涂所制的涂层不够致密，或多或少都存在一定的孔隙；离子注入所制的涂层厚度太薄，无法满足耐烧蚀磨损结构的要求。因此有必要提出一种涂层制备工艺简单、涂层厚度、结合强度满足工程应用的方法。 At present, the methods for preparing tantalum coating mainly include: magnetron sputtering, chemical vapor deposition, plasma spraying, and ion implantation. The magnetron sputtering equipment is expensive, the process is complicated, and the tantalum thin layer is due to the low sputtering temperature. The combination of the tantalum film and the substrate is a physical combination, and the bonding strength is not high; the quality of the tantalum coating prepared by chemical vapor deposition is not good, and when deposited When the temperature is high, it has a great influence on the base material; the coating made by plasma spraying is not dense enough, and there are more or less certain pores; the thickness of the coating made by ion implantation is too thin to meet the requirements of ablation and wear resistance. structural requirements. Therefore, it is necessary to propose a method with simple coating preparation process, coating thickness, and bonding strength that can meet engineering applications.
熔融盐电镀常被用来制备难熔金属，但是由于熔融盐电镀在高温下进行，在高温条件下钢的表面容易氧化，使得界面处特别容易形成较为疏松的氧化层，难以获得具有较好界面的钽涂层。 Molten salt electroplating is often used to prepare refractory metals, but because molten salt electroplating is carried out at high temperatures, the surface of steel is easily oxidized under high temperature conditions, making it easy to form a relatively loose oxide layer at the interface, and it is difficult to obtain a good interface. tantalum coating.
发明内容 Contents of the invention
本发明的目的在于提供一种经活化处理的中碳CrNiMo钢表面熔融盐电镀钽方法，获得的钽涂层结合良好、厚度均匀的，使钢的耐烧蚀磨损和耐腐蚀性能得到提高。 The object of the present invention is to provide a method for tantalum electroplating with molten salt on the surface of medium-carbon CrNiMo steel after activation treatment. The obtained tantalum coating has good bonding and uniform thickness, so that the ablation wear resistance and corrosion resistance of the steel are improved.
具体的技术方案如下： The specific technical scheme is as follows:
一种中碳CrNiMo钢表面熔盐镀钽涂层的制备方法，包括如下步骤：以经过活化处理的钢试样为阴极，99.9%以上的高纯钽片为阳极，将钽源熔融于混合盐中，反应条件为低真空0.02~0.09MPa，700~950°C，恒流电源的稳流模式下，在70~100mA/cm2下电镀3~5h，即获得钽涂层，其中活化处理5min，采用的活化液组分为：10mL/LH2SO4和1-2g/LCe(NO3)3的混合液。 A method for preparing a molten-salt tantalum-plated coating on the surface of medium-carbon CrNiMo steel, comprising the following steps: taking an activated steel sample as a cathode, and a high-purity tantalum sheet with more than 99.9% as an anode, and melting a tantalum source into a mixed salt Among them, the reaction conditions are low vacuum 0.02~0.09MPa, 700~950°C, under the constant current mode of the constant current power supply, electroplating at 70~100mA/cm 2 for 3~5h, the tantalum coating is obtained, and the activation treatment is 5min , the components of the activation solution used are: a mixed solution of 10mL/LH 2 SO 4 and 1-2g/LCe(NO 3 ) 3 .
在本发明的优选方案中，钽源为K2TaF7。 In a preferred solution of the present invention, the tantalum source is K 2 TaF 7 .
在本发明的优选方案中，混合盐的组成及摩尔百分含量为46%~47%KF、10%~11%NaF和42%~44%LiF。 In the preferred solution of the present invention, the composition and mole percentage of the mixed salt are 46%~47%KF, 10%~11%NaF and 42%~44%LiF.
在本发明的更优选方案中，混合盐的组成及摩尔百分含量为：46.5%KF、11.5%NaF和42%LiF。 In a more preferred solution of the present invention, the composition and mole percentage of the mixed salt are: 46.5% KF, 11.5% NaF and 42% LiF.
在本发明的优选方案中，钽源在混合盐中的重量百分含量为10%~15%。 In a preferred solution of the present invention, the weight percentage of the tantalum source in the mixed salt is 10%-15%.
在本发明的更优选方案中，钽源在混合盐中的重量百分含量为11.5%。 In a more preferred solution of the present invention, the weight percentage of the tantalum source in the mixed salt is 11.5%.
在本发明的优选方案中，反应条件为：0.05MPa，850°C，恒流电源的稳流模式下，在80mA/cm2下电镀4h。 In the preferred version of the present invention, the reaction conditions are: 0.05MPa, 850°C, under the constant current mode of the constant current power supply, electroplating at 80mA/cm2 for 4h.
在本发明的优选方案中，钽涂层的厚度为10~25μm。 In a preferred solution of the present invention, the thickness of the tantalum coating is 10-25 μm.
本发明的原理：在中碳CrNiMo钢表面电化学沉积钽涂层涉及2个过程，即作为钽源的K2TaF7被还原成Ta、产生的Ta原子在待镀件表面沉积的过程。Ta在氟化物低熔点共晶熔盐中的电化学还原过程包括以下二个步骤： The principle of the present invention: the electrochemical deposition of tantalum coating on the surface of medium carbon CrNiMo steel involves two processes, that is, the process in which K 2 TaF 7 as a tantalum source is reduced to Ta, and the generated Ta atoms are deposited on the surface of the workpiece to be plated. The electrochemical reduction process of Ta in fluoride eutectic molten salt with low melting point comprises the following two steps:
第一步[TaF7]-2 + 3e＝TaF2(s) +5F-，(1) The first step [TaF 7 ] -2 + 3e=TaF 2 (s) +5F - , (1)
第二个反应是TaF2(s) +2e＝Ta+2F-，(2) The second reaction is TaF 2 (s) +2e=Ta+2F - , (2)
第一步是扩散控制的可逆反应，第二个步为非扩散控制的不可逆反应。在本发明中，可溶性钽阳极在电沉积过程中遭受了较为严重的腐蚀，钽阳极释放出的Ta原子使得电镀液中Ta原子的质量分数维持在一个较为稳定的水平。这也使得电镀的过程中，能够获得较为均匀的镀层。 The first step is a reversible reaction controlled by diffusion, and the second step is an irreversible reaction not controlled by diffusion. In the present invention, the soluble tantalum anode suffers severe corrosion during the electrodeposition process, and the Ta atoms released from the tantalum anode maintain the mass fraction of Ta atoms in the electroplating solution at a relatively stable level. This also enables a relatively uniform coating to be obtained during the electroplating process.
本发明的有益效果： Beneficial effects of the present invention:
（1）本发明采用熔融盐电沉积的方法，不需要大型设备和贵重材料，成本低廉，操作简单。 (1) The present invention adopts the method of molten salt electrodeposition, which does not require large-scale equipment and expensive materials, and has low cost and simple operation.
（2）反应过程中不需要有害气体，也不产生有害物质，所以本方法对环境友好。 (2) No harmful gas is required and no harmful substances are produced during the reaction process, so the method is environmentally friendly.
（3）稀土活化液的活化使得钽涂层与基体结合更良好。 (3) The activation of the rare earth activation solution makes the tantalum coating better bond with the substrate.
（4）钽涂层沉积的过程也是扩散的过程，涂层结合性能良好。 (4) The deposition process of tantalum coating is also a diffusion process, and the coating has good bonding performance.
（5）钽涂层在瞬时脉冲高温以及机械磨损作用下能较好的保护钢基体。 (5) The tantalum coating can better protect the steel substrate under the action of instantaneous pulse high temperature and mechanical wear.
附图说明 Description of drawings
图1为本发明实施例1钽涂层的熔融盐电镀方法制备得到的钽涂层的SEM图（其中1为钽，2为中碳CrNiMo钢基板）； Fig. 1 is the SEM image of the tantalum coating prepared by the molten salt electroplating method of the tantalum coating in Example 1 of the present invention (wherein 1 is tantalum, and 2 is a medium-carbon CrNiMo steel substrate);
图2为本发明实施例1钽涂层的熔融盐电镀方法制备的钽涂层的线扫描EDS成分分析。 Fig. 2 is a line scan EDS component analysis of the tantalum coating prepared by the molten salt electroplating method of the tantalum coating in Example 1 of the present invention.
具体实施方式 Detailed ways
以下通过实施例和附图对本发明做进一步阐述。 The present invention will be further elaborated below through the embodiments and the accompanying drawings.
实施例1 Example 1
本实施例钽涂层的熔融盐电镀方法如下： The molten salt electroplating method of the tantalum coating in this embodiment is as follows:
采用线切割将中碳PCrNi3Mo钢板材线切割成片状试样，规格为φ30×4mm，并经研磨、清洗及干燥处理。将Fe-Cr-Al丝点焊至试样的一端作为电极引线，电沉积采用二电极体系，即以中碳PCrNi3Mo钢试样为阴极，可溶性钽电极为阳极，K2TaF7作为钽源，以三元共晶（混合盐）40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF为钽源K2TaF7的溶剂，K2TaF7在溶剂中的含量为11.5wt%。将上述配好的混合盐及钽源放入氧化铝坩埚中，先抽真空至0.05MPa，然后升温到850°C。中碳PCrNi3Mo钢经活化液10mL/L的H2SO4，1.5g/L Ce(NO3) 3活化5min，采用恒流电源进行电沉积，电流密度为80mA/cm2沉积4h，即在中碳PCrNi3Mo钢上沉积一层厚度约为16μm的钽镀层。 The medium-carbon PCrNi3Mo steel plate was wire-cut into sheet samples with a specification of φ30×4mm by wire cutting, and was ground, cleaned and dried. The Fe-Cr-Al wire was spot-welded to one end of the sample as the electrode lead, and the electrodeposition adopts a two-electrode system, that is, the medium-carbon PCrNi3Mo steel sample is used as the cathode, the soluble tantalum electrode is used as the anode, and K 2 TaF 7 is used as the tantalum source. The ternary eutectic (mixed salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF is used as the solvent of the tantalum source K 2 TaF 7 , and the content of K 2 TaF 7 in the solvent is 11.5wt%. Put the above prepared mixed salt and tantalum source into an alumina crucible, first evacuate to 0.05MPa, and then heat up to 850°C. Medium-carbon PCrNi3Mo steel was activated with 10mL/L H 2 SO 4 , 1.5g/L Ce(NO 3 ) 3 for 5 minutes, and then electrodeposited with a constant current power supply at a current density of 80mA/cm 2 for 4 hours. A layer of tantalum coating with a thickness of about 16 μm was deposited on carbon PCrNi3Mo steel.
所述钽涂层的截面SEM图及钽涂层的线扫描EDS成分分析参见图1和图2。 See Figure 1 and Figure 2 for the cross-sectional SEM image of the tantalum coating and the line-scan EDS component analysis of the tantalum coating.
由图1、图2可知，本发明钽涂层的熔融盐电镀方法在中碳PCrNi3Mo钢上获得的钽涂层与基体结合良好、厚度较为均匀。 It can be seen from Fig. 1 and Fig. 2 that the tantalum coating obtained by the molten salt electroplating method of the tantalum coating of the present invention on medium carbon PCrNi 3 Mo steel is well bonded to the substrate and has a relatively uniform thickness.
实施例2 Example 2
采用线切割将中碳PCrNi3Mo钢板材线切割成片状试样，规格为φ30×4mm，并经研磨、清洗及干燥处理。将Fe-Cr-Al丝点焊至试样的一端作为电极引线，电沉积采用二电极体系，即以以中碳PCrNi3Mo钢试样为阴极，可溶性钽电极为阳极，K2TaF7作为钽源，以三元共晶（混合盐）40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF为钽源K2TaF7的溶剂，K2TaF7在溶剂中的含量为10wt%。将上述配好的混合盐及钽源放入氧化铝坩埚中，先抽真空至0.09MPa，然后升温到700°C。中碳PCrNi3Mo钢经活化液10mL/L的H2SO4，1g/L Ce(NO3) 3活化5min，采用恒流电源进行电沉积，电流密度为70mA/cm2沉积3h，即在中碳PCrNi3Mo钢上沉积一层厚度约为10μm的钽镀层。 The medium-carbon PCrNi3Mo steel plate was wire-cut into sheet samples with a specification of φ30×4mm by wire cutting, and was ground, cleaned and dried. The Fe-Cr-Al wire was spot-welded to one end of the sample as the electrode lead, and the electrodeposition used a two-electrode system, that is, the medium-carbon PCrNi3Mo steel sample was used as the cathode, the soluble tantalum electrode was used as the anode, and K 2 TaF 7 was used as the tantalum source. , using ternary eutectic (mixed salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF as the solvent of tantalum source K 2 TaF 7 , and the content of K 2 TaF 7 in the solvent is 10wt%. Put the mixed salt and tantalum source prepared above into an alumina crucible, firstly evacuate to 0.09MPa, and then heat up to 700°C. Medium-carbon PCrNi3Mo steel is activated by 10mL/L H 2 SO 4 , 1g/L Ce(NO 3 ) 3 for 5 minutes, and then electrodeposited with a constant current power supply at a current density of 70mA/cm 2 for 3 hours. A layer of tantalum coating with a thickness of about 10 μm is deposited on PCrNi3Mo steel.
所述钽镀层的截面扫描图和EDS线扫描与实施例1类似。 The cross-sectional scan diagram and EDS line scan of the tantalum coating are similar to those in Example 1.
实施例3 Example 3
采用线切割将中碳32Cr2Mo1VA钢板材线切割成片状试样，规格为φ30×4mm，并经研磨、清洗及干燥处理。将Fe-Cr-Al丝点焊至试样的一端作为电极引线，电沉积采用二电极体系，即以中碳32Cr2Mo1VA钢试样为阴极，可溶性钽电极为阳极，K2TaF7作为钽源，以三元共晶（混合盐）40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF为钽源K2TaF7的溶剂，K2TaF7在溶剂中的含量为15wt%。将上述配好的混合盐及钽源放入氧化铝坩埚中，先抽真空至0.02MPa，然后升温到950°C。中碳32Cr2Mo1VA钢经活化液10mL/L的H2SO4，2g/L Ce(NO3) 3活化5min，采用恒流电源进行电沉积，电流密度为100mA/cm2沉积5h，即在中碳32Cr2Mo1VA钢上沉积一层厚度约为25μm的钽镀层。 The medium carbon 32Cr2Mo1VA steel sheet was wire-cut into sheet samples with a specification of φ30×4mm by wire cutting, and was ground, cleaned and dried. The Fe-Cr-Al wire was spot-welded to one end of the sample as the electrode lead, and the electrodeposition used a two-electrode system, that is, the medium-carbon 32Cr2Mo1VA steel sample was used as the cathode, the soluble tantalum electrode was used as the anode, and K 2 TaF 7 was used as the tantalum source. The ternary eutectic (mixed salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF is used as the solvent of the tantalum source K 2 TaF 7 , and the content of K 2 TaF 7 in the solvent is 15wt%. Put the above prepared mixed salt and tantalum source into an alumina crucible, first evacuate to 0.02MPa, and then heat up to 950°C. Medium-carbon 32Cr2Mo1VA steel was activated with 10mL/L H 2 SO 4 , 2g/L Ce(NO 3 ) 3 for 5 minutes, and then electrodeposited with a constant current power supply at a current density of 100mA/cm 2 for 5 hours. A layer of tantalum coating with a thickness of about 25 μm is deposited on 32Cr2Mo1VA steel.
所述钽镀层的截面扫描图和EDS线扫描与实施例1类似。 The cross-sectional scan diagram and EDS line scan of the tantalum coating are similar to those in Example 1.
实施例4 Example 4
采用线切割将中碳25Cr3Mo3NiNb钢板材线切割成片状试样，规格为φ30×4mm，并经研磨、清洗及干燥处理。将Fe-Cr-Al丝点焊至试样的一端作为电极引线，电沉积采用二电极体系，即以中碳25Cr3Mo3NiNb钢试样为阴极，可溶性钽电极为阳极，K2TaF7作为钽源，以三元共晶（混合盐）40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF为钽源K2TaF7的溶剂，K2TaF7在溶剂中的含量为12.5wt%。将上述配好的混合盐及钽源放入氧化铝坩埚中，先抽真空至0.07MPa，然后升温到900°C。中碳25Cr3Mo3NiNb钢经活化液10mL/L的H2SO4，1.7g/L Ce(NO3) 3活化5min，采用恒流电源进行电沉积，电流密度为90mA/cm2沉积4.5h，即在中碳25Cr3Mo3NiNb钢上沉积一层厚度约为18μm的钽镀层。 The medium-carbon 25Cr3Mo3NiNb steel plate was wire-cut into sheet samples with a size of φ30×4mm by wire cutting, and was ground, cleaned and dried. The Fe-Cr-Al wire was spot-welded to one end of the sample as the electrode lead, and the electrodeposition used a two-electrode system, that is, the medium-carbon 25Cr3Mo3NiNb steel sample was used as the cathode, the soluble tantalum electrode was used as the anode, and K 2 TaF 7 was used as the tantalum source. The ternary eutectic (mixed salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF is used as the solvent of the tantalum source K 2 TaF 7 , and the content of K 2 TaF 7 in the solvent is 12.5wt%. Put the above prepared mixed salt and tantalum source into the alumina crucible, firstly evacuate to 0.07MPa, and then raise the temperature to 900°C. Medium-carbon 25Cr3Mo3NiNb steel was activated with 10mL/L H 2 SO 4 , 1.7g/L Ce(NO 3 ) 3 for 5 minutes, and then electrodeposited with a constant current power supply at a current density of 90mA/cm 2 for 4.5 hours. A layer of tantalum coating with a thickness of about 18 μm is deposited on medium carbon 25Cr3Mo3NiNb steel.
所述钽镀层的截面扫描图和EDS线扫描与实施例1类似。 The cross-sectional scan diagram and EDS line scan of the tantalum coating are similar to those in Example 1.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510173706.2A CN104790001A (en) | 2015-04-13 | 2015-04-13 | Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510173706.2A CN104790001A (en) | 2015-04-13 | 2015-04-13 | Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104790001A true CN104790001A (en) | 2015-07-22 |
Family
ID=53555183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510173706.2A Pending CN104790001A (en) | 2015-04-13 | 2015-04-13 | Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104790001A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814673A (en) * | 1969-07-02 | 1974-06-04 | Gen Electric | Process for tantalliding and niobiding base metal compositions |
| JP2001279486A (en) * | 2000-03-30 | 2001-10-10 | Japan Science & Technology Corp | Method for plating tantalum |
| CN101638804A (en) * | 2008-07-30 | 2010-02-03 | 宝山钢铁股份有限公司 | Chromium-free passivation solution for tin plate and method for using same |
| CN102330095A (en) * | 2011-08-29 | 2012-01-25 | 中国科学院合肥物质科学研究院 | A kind of Al2O3 coating preparation method on the surface of steel base material |
| CN103060863A (en) * | 2013-01-18 | 2013-04-24 | 沈阳瑞康达科技有限公司 | Method for preparing Ni-Ti surface tantalum plating layer with halide fused salt electro-deposition |
-
2015
- 2015-04-13 CN CN201510173706.2A patent/CN104790001A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814673A (en) * | 1969-07-02 | 1974-06-04 | Gen Electric | Process for tantalliding and niobiding base metal compositions |
| JP2001279486A (en) * | 2000-03-30 | 2001-10-10 | Japan Science & Technology Corp | Method for plating tantalum |
| CN101638804A (en) * | 2008-07-30 | 2010-02-03 | 宝山钢铁股份有限公司 | Chromium-free passivation solution for tin plate and method for using same |
| CN102330095A (en) * | 2011-08-29 | 2012-01-25 | 中国科学院合肥物质科学研究院 | A kind of Al2O3 coating preparation method on the surface of steel base material |
| CN103060863A (en) * | 2013-01-18 | 2013-04-24 | 沈阳瑞康达科技有限公司 | Method for preparing Ni-Ti surface tantalum plating layer with halide fused salt electro-deposition |
Non-Patent Citations (1)
| Title |
|---|
| 王升 等: "熔盐电镀钽及其耐磨损烧蚀性能", 《中国表面工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103014793B (en) | Method for preparing titanium carbide coating through pulse electrodeposition | |
| CN104562128B (en) | A kind of method for preparing thermal protection ceramic layer on metal or metallic composite surface | |
| CN104637551A (en) | Application of Ti3SiC2-Based Ceramic Materials as Molten Fluoride Salt Corrosion Resistant Materials | |
| JPS589151B2 (en) | Method of forming a corrosion-resistant coating on a metal substrate | |
| CN103805995B (en) | The restorative procedure of carbon/carbon compound material anti-oxidant rhenium/iridium coating layer surface imperfection | |
| RU2660448C2 (en) | Electrode of aluminum electrolytic cell (options) | |
| CN101974770A (en) | Aqueous solution for electrodepositing iridium layer and method for preparing iridium layer in aqueous solution by way of electrodeposition | |
| CN104372394A (en) | Preparation method for oxide ceramic layer | |
| CN103806044B (en) | The method of electrolytic preparation iridium coating layer in chloro-iridic acid caesium-Chlorides molten salts | |
| CN103060862A (en) | Titanium coating and preparation method thereof | |
| CN105385989B (en) | A kind of salt melting system, compound cocatalyst and the application of the binary permeation of molybdenum or molybdenum alloy | |
| Wang et al. | Stability investigation of electrodeposited zirconium diboride ceramic coatings in molten zinc | |
| CN105385988B (en) | A kind of preparation method of molybdenum or molybdenum alloy surface rare earth metal boron binary co-penetration layer | |
| CN104790001A (en) | Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt | |
| CN106544627B (en) | A kind of high temperature thermal corrosion resistant composite coating and preparation method thereof | |
| CN102002743A (en) | Preparation method for electroplating thick tungsten coating on pure copper or copper alloy substrate with molten salt | |
| CN113279030A (en) | Molten salt electrodeposition method of niobium coating | |
| Frazer et al. | Electrodeposition of zirconium diboride from oxides dissolved in molten cryolite | |
| RU2543659C1 (en) | Method for production of composite metal-ceramic coating at valve metals and their alloys | |
| CN105970151B (en) | Surface treatment method, metal carbide coating, alloy workpiece | |
| CN104746114A (en) | Fe-Mo composite material and preparation method thereof | |
| CN105063692B (en) | A kind of Fe V functionally gradient material (FGM)s and preparation method thereof | |
| RU2402633C1 (en) | Procedure for application of combined heat resistant coating | |
| US20220396883A1 (en) | Methods and systems for electroless plating a first metal onto a second metal in a molten salt bath, and surface pretreatments therefore | |
| CN108588789A (en) | A kind of preparation method for the processing solution and boron titanium compound preparing boron titanium compound film layer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150722 |