CN1288979A - Technology process and equiment for depositing permalloy film electrically - Google Patents
Technology process and equiment for depositing permalloy film electrically Download PDFInfo
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- 229910000889 permalloy Inorganic materials 0.000 title claims abstract description 18
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- 238000000151 deposition Methods 0.000 title claims description 15
- 238000000034 method Methods 0.000 title abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000004020 conductor Substances 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 4
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims 2
- 239000011780 sodium chloride Substances 0.000 claims 2
- 241000080590 Niso Species 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 239000005357 flat glass Substances 0.000 claims 1
- 239000012530 fluid Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000004070 electrodeposition Methods 0.000 abstract description 25
- 239000010409 thin film Substances 0.000 abstract description 12
- 238000002474 experimental method Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
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- Electroplating Methods And Accessories (AREA)
Abstract
一种电沉积坡莫合金薄膜工艺及其实施设备,属电化学的电沉积技术领域,控温水浴箱1把电沉积溶液24的温度控制在25～35℃,搅拌器3利用输运电沉积溶液24的自身动能进行溶液搅拌,电源4的正、负输出端直接跨接在液槽2的阳极23和阴极22,有节能、成品质量好和操作简便等优点,特别适于科研单位的实验室和工厂用来小批量生产高质量的坡莫合金薄膜。
An electrodeposited permalloy thin film process and its implementation equipment, belonging to the field of electrochemical electrodeposition technology, the temperature control water bath box 1 controls the temperature of the electrodeposition solution 24 at 25-35°C, and the stirrer 3 utilizes transport electrodeposition The solution 24 is stirred by its own kinetic energy, and the positive and negative output ends of the power supply 4 are directly connected to the anode 23 and cathode 22 of the liquid tank 2, which has the advantages of energy saving, good quality of finished products, and easy operation, and is especially suitable for experiments in scientific research units. The chamber and factory are used to produce high quality permalloy thin films in small batches.
Description
本发明涉及一种电沉积坡莫合金薄膜工艺及其实施设备，属电化学的电沉积技术领域。The invention relates to an electrodeposited permalloy thin film process and its implementation equipment, belonging to the technical field of electrochemical electrodeposition.
坡莫合金指组分的Fe与Ni的重量比=17～23∶83～77，尤其指组分的Fe与Ni的重量比=20∶80的铁镍合金。坡莫合金薄膜工业应用广泛：作有保护、抗腐蚀或装饰性质的结构性膜或作有电磁学性质的功能性膜。长期以来，技术人员普遍采用电沉积工艺制备坡莫合金薄膜。背景技术虽能制备质量尚可的坡莫合金薄膜，但从背景技术所要求的工作条件和所需要的实施设备看出背景技术有以下缺点。背景技术所需要的实施设备主要由控温水浴箱、液槽、搅拌器和电源组成，控温水浴箱是含水、垫块、温度传感器、水温置定器、水温指示器、电热器和开关的电热控温水浴箱，液槽是含槽盖、阳极、阴极和电沉积溶液的容器，搅拌器是含电机、电机调速器、转子和开关的转子搅拌器，电源是含正输出端、负输出端、变阻器、电流指示器和开关的直流电源，液槽内注满电沉积溶液，槽盖上安装有阳极、阴极和转子的转轴，阳极、阴极和转子浸泡在电沉积溶液内，控温水浴箱内注满水，液槽安放在垫块上浸在控温水浴箱内的水中，温度传感器紧贴液槽的外壁，电源的正输出端经变阻器、电流指示器与阳极连接，电源的负输出端与阴极连接，控温水浴箱、搅拌器和电源经各自的开关与交流市电网连接。实施电沉积工艺时，纯Ni板和被沉积物分别悬挂在阳极和阴极。背景技术采用的电沉积溶液要求的工作温度一般偏高，介于50～70℃(见电镀手册(上册)，第2版，1998年，北京：国防工业出版社出版，主编：张允诚等，PP568～570)，为使溶液恒温，控温水浴箱得经常工作，耗电多，加上溶液中水分蒸发快，溶液浓度随之改变，导致先后制备的同一批成品组分不同；搅拌器的旋转转子搅拌溶液，不论旋转转子用什么转速旋转，旋转转子总难以把溶液搅拌均匀，直接影响到成品的质量；电源经变阻器向液槽供电，调节变阻器，改变流入液槽的电流，旨使电沉积在电流密度(电流/被沉积物的表面积)为最佳值的条件下进行，在被沉积物的形状(尤其是异形)和大小经常改变时，精确的电流值不易确定，最佳电流密度不易得到，加上种种因素，如溶液搅拌不匀，溶液电阻、电源电压、电沉积电位等的波动造成实际电流密度在最佳电流密度值附近波动，导致成品组分的差异。Permalloy refers to the weight ratio of Fe and Ni of the components = 17-23:83-77, especially iron-nickel alloys with the weight ratio of Fe and Ni of the components = 20:80. Permalloy thin films are widely used in industry: as structural films with protective, anti-corrosion or decorative properties or as functional films with electromagnetic properties. For a long time, technicians have generally prepared permalloy thin films by electrodeposition process. Background Art Although permalloy thin films of acceptable quality can be produced, the background art has the following disadvantages from the working conditions and implementation equipment required by the background art. Background technology The required implementation equipment is mainly composed of a temperature-controlled water bath, a liquid tank, an agitator and a power supply. Electric temperature-controlled water bath box, the liquid tank is a container containing a tank cover, anode, cathode and electrodeposition solution, the stirrer is a rotor stirrer containing a motor, a motor governor, a rotor and a switch, the power supply is a positive output terminal, a negative DC power supply for output terminals, rheostats, current indicators and switches. The liquid tank is filled with electrodeposition solution. The anode, cathode and rotor shaft are installed on the tank cover. The anode, cathode and rotor are immersed in the electrodeposition solution, and the temperature is controlled. The water bath box is filled with water, the liquid tank is placed on the block and immersed in the water in the temperature-controlled water bath box, the temperature sensor is close to the outer wall of the liquid tank, the positive output end of the power supply is connected to the anode through a rheostat and a current indicator, and the power supply The negative output terminal is connected to the cathode, and the temperature-controlled water bath, the stirrer and the power supply are connected to the AC mains grid through their respective switches. When implementing the electrodeposition process, the pure Ni plate and the deposit are suspended on the anode and cathode, respectively. The working temperature required by the electrodeposition solution used in the background technology is generally high, between 50 and 70°C (see Electroplating Handbook (Volume 1), 2nd edition, 1998, Beijing: Published by National Defense Industry Press, chief editor: Zhang Yuncheng, etc., PP568 ~570), in order to keep the solution at a constant temperature, the temperature-controlled water bath has to work frequently, which consumes a lot of power. In addition, the water in the solution evaporates quickly, and the concentration of the solution changes accordingly, resulting in different components of the same batch of finished products prepared successively; the rotation of the agitator The rotor stirs the solution. No matter what speed the rotating rotor rotates, it is always difficult for the rotating rotor to stir the solution evenly, which directly affects the quality of the finished product; It is carried out under the condition that the current density (current/surface area of the deposit) is the optimum value. When the shape (especially abnormal shape) and size of the deposit are often changed, the precise current value is not easy to determine, and the optimum current density is not easy. Obtained, coupled with various factors, such as uneven stirring of the solution, fluctuations in solution resistance, power supply voltage, electrodeposition potential, etc., cause the actual current density to fluctuate around the optimal current density value, resulting in differences in the components of the finished product.
本发明的一个目的是推出一种没有背景技术缺点的电沉积坡莫合金薄膜工艺，该工艺采用的电沉积溶液要求的工作温度较低，介于25～35℃。An object of the present invention is to introduce a process for electrodepositing permalloy thin films without the disadvantages of the background technology. The electrodeposition solution used in the process requires a relatively low working temperature, between 25°C and 35°C.
本发明的另一个目的是推出一种实施上个目的所述的工艺的设备。Another object of the invention is to propose a plant for carrying out the process described in the previous object.
图1是本发明涉及设备的结构示意图，图中1是控温水浴箱，11是水，12是垫块，2是液槽，21是槽盖，22是阴极，23是阳极，24是电沉积溶液，3是搅拌器，31是进液管，32是出液管，33是喷嘴，4是电源。该设备由公知的装置组合而成，为简便起见，图中未示出业内人士熟悉的部件。省略的部件计有：控温水浴箱1包含的温度传感器、水温置定器、水温指示器、电热器和开关；搅拌器3包含的流量置定器、流量指示器、恒流泵和开关；电源4包含的电压置定器、电压指示器和开关。Fig. 1 is the structure schematic diagram of the equipment involved in the present invention, among the figure 1 is temperature control water bath box, 11 is water, 12 is pad, 2 is liquid tank, 21 is tank cover, 22 is cathode, 23 is anode, 24 is electric The deposition solution, 3 is a stirrer, 31 is a liquid inlet pipe, 32 is a liquid outlet pipe, 33 is a nozzle, and 4 is a power supply. The equipment is composed of known devices, and for the sake of brevity, parts familiar to those in the art are not shown in the figure. The omitted components include: the temperature sensor, water temperature setter, water temperature indicator, electric heater and switch included in the temperature control water bath box 1; the flow setter, flow indicator, constant flow pump and switch included in the agitator 3; The voltage setter, voltage indicator and switch that power supply 4 comprises.
本发明的目的是通过采用以下技术方案实现的，现结合附图说明。The purpose of the present invention is achieved by adopting the following technical solutions, which are now described in conjunction with the accompanying drawings.
一种电沉积坡莫合金薄膜工艺，在下述的设备中实施，其特征在于，步骤：A kind of electrodeposited permalloy thin film process is implemented in the following equipment, it is characterized in that, step:
第一步置定工艺条件，控温水浴箱1的水温、搅拌器3的流量和电源4的电压分别在25～35℃、5000～15000毫升/小时和1.3～1.6伏的范围内任意置定；The first step is to set the process conditions. The water temperature of the temperature-controlled water bath 1, the flow rate of the agitator 3 and the voltage of the power supply 4 are respectively set arbitrarily within the ranges of 25-35°C, 5000-15000 ml/hour and 1.3-1.6 volts. ;
第二步安装电极，把纯Ni板和被沉积物，即导电体或表面镀有导电层的绝缘体分别悬挂于阳极23和阴极22；The second step is to install the electrodes, suspending the pure Ni plate and the deposit, that is, the conductor or the insulator coated with a conductive layer on the anode 23 and the cathode 22, respectively;
第三步配制电沉积溶液24，每升电沉积溶液24含Ni2+、Fe2+、H3BO3、NaCl和糖精钠分别为10～15克、0.1～0.4克、20～30克、20～30克和0.6～0.9克，用盐酸调节该溶液的pH值至1.5～3.5，把该溶液注满液槽2；The third step is to prepare the electrodeposition solution 24. Each liter of the electrodeposition solution 24 contains 10-15 grams, 0.1-0.4 grams , 20-30 grams , 20-30 grams and 0.6-0.9 grams, adjust the pH value of the solution to 1.5-3.5 with hydrochloric acid, and fill the liquid tank 2 with the solution;
第四步实施电沉积，控温水浴箱1上电，待水11的温度升至置定水温时，搅拌器3和电源4上电，坡莫合金薄膜均匀沉积于悬挂于阴极22的被沉积物的表面，薄膜沉积速率为400～2500埃/分；The fourth step is to implement electrodeposition. The temperature-controlled water bath 1 is powered on. When the temperature of the water 11 rises to the set water temperature, the agitator 3 and the power supply 4 are powered on. The surface of the object, the film deposition rate is 400-2500 angstroms/min;
第五步成品，待上步所述薄膜的厚度满足要求时，控温水浴箱1、搅拌器3和电源4去电，从阴极22上取下被沉积物，得到成品，成品组分的Fe与Ni的重量比=17～23∶83～77。The fifth step is the finished product. When the thickness of the film described in the previous step meets the requirements, the temperature-controlled water bath 1, the agitator 3 and the power supply 4 are de-energized, and the deposited deposits are removed from the cathode 22 to obtain the finished product. The Fe content of the finished product component is The weight ratio with Ni=17～23:83～77.
根据上述的电沉积坡莫合金薄膜工艺，其特征在于，水温、流量和电压分别置定于30℃、14000毫升/小时和1.5伏；被沉积物为铜片或镀铜玻璃片；每升电沉积溶液含NiSO4·6H2O、NiCl2·6H2O、FeSO4·7H2O、H3BO3、NaCl和糖精钠分别为14.7克、35.3克、1.2克、25克、25克和0.75克，用盐酸调节该溶液的pH值至3.0，薄膜沉积速率为1800埃/分，成品组分的Fe与Ni的重量比=20∶80。According to the above-mentioned electrodeposited permalloy thin film process, it is characterized in that water temperature, flow rate and voltage are respectively set at 30 ℃, 14000 ml/hour and 1.5 volts; the deposit is copper sheet or copper-coated glass sheet; The deposition solution contains 14.7g, 35.3g , 1.2g , 25g , 25g and 0.75 grams, the pH value of this solution is adjusted to 3.0 with hydrochloric acid, film deposition rate is 1800 angstroms/minute, the weight ratio=20:80 of the Fe of finished product component and Ni.
一种实施上述的电沉积坡莫合金薄膜工艺的设备，由控温水浴箱1、液槽2、搅拌器3和电源4组成，控温水浴箱1是含水11、垫块12、温度传感器、水温置定器、水温指示器、电热器和开关的电热控温水浴箱，液槽2是含槽盖21、阴极22、阳极23和电沉积溶液24的容器，搅拌器3是含进液管31、出液管32、喷嘴33、流量置定器、流量指示器、恒流泵和开关的液体搅拌器，电源4是含正输出端、负输出端、电压置定器、电压指示器和开关的直流稳压电源，液槽2内有电沉积溶液24，槽盖21上安装有阴极22和阳极23，阴极22和阳极23浸泡在电沉积溶液24中，控温水浴箱1内有水11，液槽2安放在垫块12上和浸在水11中，温度传感器紧贴液槽2的外壁，控温水浴箱1、搅拌器3和电源4通过各自的开关与交流市电网连接，其特征在于，槽盖21上还安装有进液管31、出液管32和喷咀33，进液管31、出液管32和喷嘴33浸泡在电沉积溶液24中，电源4的正输出端和负输出端分别与阳极23和阴极22连接，控温水浴箱1的水温、搅拌器3的流量和电源4的电压的置定范围分别为25～35℃、5000～15000毫升/小时和1.3～1.6伏。A kind of equipment that implements above-mentioned electrodeposited permalloy thin film process, is made up of temperature control water bath box 1, liquid tank 2, agitator 3 and power supply 4, temperature control water bath box 1 is water-containing 11, pad 12, temperature sensor, Water temperature setter, water temperature indicator, electric heater and switch electric heating temperature control water bath box, liquid tank 2 is a container containing tank cover 21, cathode 22, anode 23 and electrodeposition solution 24, agitator 3 is a container containing liquid inlet pipe 31. Liquid outlet pipe 32, nozzle 33, flow setter, flow indicator, constant flow pump and liquid agitator of switch, power supply 4 is to contain positive output end, negative output end, voltage setter, voltage indicator and The DC stabilized power supply of the switch, the electrodeposition solution 24 is arranged in the liquid tank 2, the cathode 22 and the anode 23 are installed on the tank cover 21, the cathode 22 and the anode 23 are soaked in the electrodeposition solution 24, there is water in the temperature control water bath box 1 11. The liquid tank 2 is placed on the pad 12 and immersed in the water 11. The temperature sensor is close to the outer wall of the liquid tank 2. The temperature-controlled water bath 1, the agitator 3 and the power supply 4 are connected to the AC mains through their respective switches. It is characterized in that a liquid inlet pipe 31, a liquid outlet pipe 32 and a nozzle 33 are also installed on the tank cover 21, the liquid inlet pipe 31, the liquid outlet pipe 32 and the nozzle 33 are immersed in the electrodeposition solution 24, and the positive output of the power supply 4 terminal and negative output terminal are respectively connected with the anode 23 and the cathode 22, and the setting ranges of the water temperature of the temperature control water bath 1, the flow rate of the agitator 3 and the voltage of the power supply 4 are respectively 25～35 ℃, 5000～15000 ml/hour and 1.3 to 1.6 volts.
与背景技术相比，本发明有以下优点：Compared with background technology, the present invention has the following advantages:
1．节能。本发明采用的电沉积溶液24要求的工作温度较低，介于25～35℃。当室温高于置定水温时，控温水浴箱1内的电热器不工作，不耗电，电沉积溶液24的温度恒定于室温；当室温低于置定水温时，由于两者相差不多，所以控温水浴箱1内的电热器只需短时间工作，长时间不工作即可，耗电省。1. energy saving. The working temperature required for the electrodeposition solution 24 used in the present invention is relatively low, between 25°C and 35°C. When the room temperature was higher than the set water temperature, the electric heater in the temperature-controlled water bath 1 did not work, no power consumption, and the temperature of the electrodeposition solution 24 was constant at room temperature; when the room temperature was lower than the set water temperature, because the two were almost the same, Therefore, the electric heater in the temperature-controlling water bath box 1 only needs to work for a short time and not work for a long time, which saves power consumption.
2．溶液搅拌均匀，成品质量好。本发明采用本发明人发明的专利号为ZL002162.8的液体搅拌装置作为搅拌器3，恒流泵把液槽2内的部分电沉积溶液24从进液管31吸入，经恒流泵、出液管32，从喷嘴33排出，喷嘴33的直径比进液管31的直径小得多，因此液体排出流速比吸入流速大得多，排出流速大的液体能量高，足以激起整个液槽2内的电沉积溶液24循环流动，使电沉积溶液24搅拌充分和均质完善，确保电沉积工艺在被沉物的表面沉积厚薄均匀的优质坡莫合金薄膜。2. The solution is evenly stirred, and the finished product is of good quality. The present invention adopts the liquid stirring device with the patent No. ZL002162.8 invented by the inventor as the stirrer 3, and the constant-current pump sucks the part of the electrodeposition solution 24 in the liquid tank 2 from the liquid inlet pipe 31, and passes through the constant-current pump and the outlet The liquid pipe 32 is discharged from the nozzle 33. The diameter of the nozzle 33 is much smaller than that of the liquid inlet pipe 31, so the liquid discharge flow rate is much higher than the suction flow rate, and the liquid with a large discharge flow rate has high energy, which is enough to stir up the entire liquid tank 2 The electrodeposition solution 24 inside circulates and flows, so that the electrodeposition solution 24 is fully stirred and homogeneous, and ensures that the electrodeposition process deposits a high-quality permalloy thin film with a uniform thickness on the surface of the object to be deposited.
3．稳压供电，操作简便。本发明采用直流稳压电源向液槽2供电，电源的输出电压可置定，置定时不需估算被沉积物的表面积，操作简便。3. Regulated power supply, easy to operate. The present invention uses a DC stabilized power supply to supply power to the liquid tank 2, the output voltage of the power supply can be set, and the timing does not need to estimate the surface area of the deposited deposits, and the operation is simple and convenient.
本发明特别适于科研单位的实验室和工厂用来小批量生产高质量和重复性好的各种形状(尤其是异形)和大小的坡莫合金薄膜。The invention is especially suitable for laboratories and factories of scientific research units to produce high-quality and repeatable permalloy thin films of various shapes (especially irregular shapes) and sizes in small batches.
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| CN 00125288 CN1117178C (en) | 2000-09-20 | 2000-09-20 | Technology process and equiment for depositing permalloy film electrically |
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| CN 00125288 CN1117178C (en) | 2000-09-20 | 2000-09-20 | Technology process and equiment for depositing permalloy film electrically |
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| CN1288979A true CN1288979A (en) | 2001-03-28 |
| CN1117178C CN1117178C (en) | 2003-08-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 00125288 Expired - Fee Related CN1117178C (en) | 2000-09-20 | 2000-09-20 | Technology process and equiment for depositing permalloy film electrically |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1894442B (en) * | 2003-10-22 | 2012-01-04 | 内克斯系统公司 | Method and apparatus for fluid processing a workpiece |
| CN103243356A (en) * | 2012-10-11 | 2013-08-14 | 湖南理工学院 | Preparation method of iron-nickel-cobalt-molybdenum alloy foil by electrodeposition |
| CN111155167A (en) * | 2020-01-13 | 2020-05-15 | 中国原子能科学研究院 | Electroplating device |
| CN112323131A (en) * | 2020-11-03 | 2021-02-05 | 重庆圣盈达科技开发有限公司 | Method for removing bubbles on surface of electroplated workpiece |
-
2000
- 2000-09-20 CN CN 00125288 patent/CN1117178C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1894442B (en) * | 2003-10-22 | 2012-01-04 | 内克斯系统公司 | Method and apparatus for fluid processing a workpiece |
| CN103243356A (en) * | 2012-10-11 | 2013-08-14 | 湖南理工学院 | Preparation method of iron-nickel-cobalt-molybdenum alloy foil by electrodeposition |
| CN111155167A (en) * | 2020-01-13 | 2020-05-15 | 中国原子能科学研究院 | Electroplating device |
| CN112323131A (en) * | 2020-11-03 | 2021-02-05 | 重庆圣盈达科技开发有限公司 | Method for removing bubbles on surface of electroplated workpiece |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1117178C (en) | 2003-08-06 |
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