CN105353011B - A kind of metal oxide film analyzer - Google Patents
A kind of metal oxide film analyzer Download PDFInfo
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- CN105353011B CN105353011B CN201510792021.6A CN201510792021A CN105353011B CN 105353011 B CN105353011 B CN 105353011B CN 201510792021 A CN201510792021 A CN 201510792021A CN 105353011 B CN105353011 B CN 105353011B
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 11
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 59
- 229910052802 copper Inorganic materials 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 5
- 238000005261 decarburization Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 20
- 238000004458 analytical method Methods 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 6
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 4
- 239000008151 electrolyte solution Substances 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241001460678 Napo <wasp> Species 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000010407 anodic oxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910001610 cryolite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- IOXPXHVBWFDRGS-UHFFFAOYSA-N hept-6-enal Chemical compound C=CCCCCC=O IOXPXHVBWFDRGS-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007431 microscopic evaluation Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
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Abstract
本发明为解决取向硅钢板表面氧化层检测周期长，投资成本高的问题，提供了一种基于原电池反应原理，可对金属氧化层进行快速测量的分析设备，该分析设备包括电位差计、铜导杆、盖板、酸槽、水槽和恒温磁力搅拌器和多孔阻板，其中恒温磁力搅拌器控制电解质溶液温度稳定性和浓度均匀性；铜导杆为特制联结导杆，固定在多功能盖板上，可以实现传导电流、极板的定位和调节；多孔挡板能有效阻隔涡流，保证测量的稳定性；本发明提供的设备造价低、测试成本低、操作简便、测量稳定性好，可实现对金属氧化膜进行宏观、快速测量，其中附图(5)就是用本发明提供的仪器，测试取向硅钢表面氧化层的结果图示。
In order to solve the problems of long detection period and high investment cost of the oxide layer on the surface of oriented silicon steel sheet, the present invention provides an analysis device based on the principle of galvanic reaction, which can quickly measure the metal oxide layer. The analysis device includes a potentiometer, Copper guide rod, cover plate, acid tank, water tank, constant temperature magnetic stirrer and porous resistance plate, in which the constant temperature magnetic stirrer controls the temperature stability and concentration uniformity of the electrolyte solution; the copper guide rod is a special connecting guide rod, fixed on the multifunctional On the cover plate, the conduction current and the positioning and adjustment of the pole plate can be realized; the porous baffle can effectively block the eddy current and ensure the stability of the measurement; the equipment provided by the invention is low in cost, low in test cost, easy to operate, and good in measurement stability. The metal oxide film can be measured macroscopically and quickly, and the accompanying drawing (5) is a graphical representation of the result of testing the oxide layer on the surface of the oriented silicon steel with the instrument provided by the present invention.
Description
技术领域：Technical field:
本发明涉及一种物质分析设备，尤其涉及一种金属氧化膜分析仪。The invention relates to a material analysis device, in particular to a metal oxide film analyzer.
背景技术：Background technique:
取向硅钢在工业上的应用广泛，但在取向硅钢生产中可能出现表面质量缺陷等不良问题，如露晶、漏金、花斑、层间电阻低等，表面质量问题一方面会提高底层让步率，另一方面提高了铁损，同时也有损产品的形象。脱碳退火形成的氧化层质量对最终表面质量有决定性的影响，但是从脱碳退火到最终涂覆绝缘层后发现表面质量问题，再到分析问题并找到解决方案，约需数周，在这几周里会生产出大量表面质量不良的产品。因此，在脱碳退火生产线对氧化层质量进行检测，及时对表面质量作出预判，及早作出工艺调整可大大降低表面质量不良问题的发生率。Oriented silicon steel is widely used in industry, but in the production of oriented silicon steel, there may be surface quality defects and other adverse problems, such as dew crystals, gold leakage, mottle, low interlayer resistance, etc. Surface quality problems will increase the yield rate of the bottom layer on the one hand, On the other hand, the iron loss is increased, and the image of the product is also damaged. The quality of the oxide layer formed by decarburization annealing has a decisive impact on the final surface quality, but it takes about several weeks from decarburization annealing to the discovery of surface quality problems after the final coating of the insulating layer, and then to analyzing the problem and finding a solution. A large number of products with poor surface quality will be produced for several weeks. Therefore, testing the quality of the oxide layer in the decarburization annealing production line, making timely predictions on the surface quality, and making early process adjustments can greatly reduce the incidence of poor surface quality problems.
目前国内对氧化层的分析检测主要是采用扫描电镜(SEM)、X射线光电子能谱(XPS)、X射线衍射仪(XRD)及俄歇电子能谱(AES)等微观分析手段，如杂志《原子能科学技术》，2015年5月第49卷增刊刊登的文章：《包壳材料316Ti在液态铅铋中的腐蚀氧化层分析》报道采用SEM分析铅基研究实验堆候选包壳材料316Ti腐蚀后形成的双层氧化膜；杂志《特种铸造及有色金属》，2005年第25卷第3期刊登的文章：《镁合金双脉冲微弧氧化表面膜层的形成及结构分析》报道采用XRD、SEM、EDX等方法，研究了纯镁与AZ91D镁合金在六氟铝酸钠(Na3AlF6)、氢氧化钾(KOH)、六偏磷酸钠((NaPO3)6)和三乙醇胺四元组分电解液中双脉冲微弧氧化膜层的形成、膜层形貌和成分结构；杂志《中国腐蚀与防护学报》，2001年第21卷第3期刊登的文章：《铝表面高压阳极氧化膜层结构分析》报道采用XRD、SEM和XPS综合分析了铝在磷酸和钨酸钠体系中形成的高压阳极氧化膜的成分、形貌和结构。特开2004-11217号公报中公开了采用傅里叶变换红外线光谱(FT-IR)测定钢板的表面氧化底层中FeO和SiO2的含量比值。这些方法的优势在于能够对氧化层的成分、形貌、结构进行详细定性分析和定量分析，因此特别适应于科学研究，但是这些分析方法分析周期长、分析面积小、且设备投资和检测成本高，不适用于工业生产中需要长期、连续、大批量的宏观检测。At present, the analysis and detection of the oxide layer in China mainly adopt microscopic analysis methods such as scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffractometer (XRD) and Auger electron spectroscopy (AES). "Atomic Energy Science and Technology", an article published in the supplement of volume 49 in May 2015: "Analysis of the Corrosion Oxidation Layer of Cladding Material 316Ti in Liquid Lead and Bismuth" reported that SEM was used to analyze the formation of 316Ti, a candidate cladding material for lead-based research and experimental reactors after corrosion The article published in the magazine "Special Casting and Nonferrous Metals", Volume 25, Issue 3, 2005: "Formation and Structure Analysis of the Surface Film Layer of Magnesium Alloy Double Pulse Micro-arc Oxidation" reported using XRD, SEM, EDX et al. studied pure magnesium and AZ91D magnesium alloy in sodium hexafluoroaluminate (Na 3 AlF 6 ), potassium hydroxide (KOH), sodium hexametaphosphate ((NaPO 3 ) 6 ) and triethanolamine quaternary components. The formation, morphology and composition structure of the double-pulse micro-arc oxidation film in the electrolyte; the article published in the journal "Chinese Journal of Corrosion and Protection", Volume 21, Issue 3, 2001: "High-voltage anodic oxidation film on aluminum surface Structural Analysis" reported that XRD, SEM and XPS were used to comprehensively analyze the composition, morphology and structure of the high-voltage anodic oxide film formed on aluminum in phosphoric acid and sodium tungstate systems. Japanese Patent Application Laid-Open No. 2004-11217 discloses the use of Fourier transform infrared spectroscopy (FT-IR) to measure the content ratio of FeO and SiO 2 in the surface oxide bottom layer of a steel plate. The advantage of these methods is that they can carry out detailed qualitative and quantitative analysis on the composition, morphology and structure of the oxide layer, so they are especially suitable for scientific research, but these analysis methods have long analysis periods, small analysis areas, and high equipment investment and detection costs. , not suitable for long-term, continuous and large-scale macroscopic detection in industrial production.
发明内容：Invention content:
为解决上述问题，本发明利用原电池原理，提供了一种可对金属氧化膜进行宏观、快速测量的分析设备，该设备造价低、测试成本低，且操作简便、测量稳定性好。In order to solve the above problems, the present invention utilizes the principle of primary batteries to provide an analysis device capable of macroscopically and rapidly measuring metal oxide films. The device is low in cost, low in test cost, easy to operate, and has good measurement stability.
本发明为解决上述技术问题所采用的技术方案为：The technical scheme that the present invention adopts for solving the problems of the technologies described above is:
一套金属氧化膜分析仪，包括电位差计、铜导杆、盖板、酸槽、水槽和恒温磁力搅拌器，其特征在于：酸槽上端固定盖板，两根导杆从盖板中间的槽中穿过，并固定在盖板上，两根导杆下端分别与第一极板和第二极板连接，极板浸入到酸槽的酸液中，两根导杆上端通过导线与电位差计连接，构成回路。A set of metal oxide film analyzer, including potentiometer, copper guide rod, cover plate, acid tank, water tank and constant temperature magnetic stirrer. Pass through the tank and fix it on the cover plate. The lower ends of the two guide rods are respectively connected to the first and second plates. The plates are immersed in the acid solution in the acid tank. The upper ends of the two guide rods are connected The differential meter is connected to form a loop.
按上述技术方案，所述酸槽中盛装酸和磁子，酸槽外设置保温系统，包括水槽和恒温磁力搅拌器，其中水槽置于恒温磁力搅拌器内部。According to the above technical solution, the acid tank is filled with acid and magnets, and an insulation system is set outside the acid tank, including a water tank and a constant temperature magnetic stirrer, wherein the water tank is placed inside the constant temperature magnetic stirrer.
按上述技术方案，盖板四周开有4个限位孔，酸槽上也相应开孔，通过螺栓将盖板固定在酸槽上，盖板上还开有注酸口，便于向酸槽中补充酸液。According to the above technical scheme, there are 4 limit holes around the cover plate, and corresponding holes are opened on the acid tank. Add acid.
按上述技术方案，导杆优选为铜导杆。According to the above technical solution, the guide rod is preferably a copper guide rod.
按上述技术方案，两根铜导杆从盖板中间的槽中穿过，铜导杆通过上下两个不同位置的螺栓固定在盖板上；可以通过调节铜导杆上的螺栓来调节极板的相对距离和极板的高度。According to the above technical scheme, two copper guide rods pass through the groove in the middle of the cover plate, and the copper guide rods are fixed on the cover plate by bolts at two different positions up and down; the pole plate can be adjusted by adjusting the bolts on the copper guide rods. The relative distance and the height of the plate.
按上述技术方案，两根铜导杆上部通过螺栓固定导线，下部剖开并钻孔，极板也钻孔，通过螺栓将铜导杆与极板连接，极板浸没到酸槽的酸液中。According to the above technical scheme, the upper parts of the two copper guide rods are used to fix the wires with bolts, the lower parts are cut and drilled, and the pole plates are also drilled, and the copper guide rods are connected to the pole plates through bolts, and the pole plates are immersed in the acid solution of the acid tank .
按上述技术方案，极板包括待测脱碳退火板和去掉氧化膜的基板。According to the above technical solution, the polar plate includes a decarburized annealed plate to be tested and a substrate from which the oxide film has been removed.
按上述技术方案，酸槽内设多孔阻板，可以有效阻隔涡流。According to the above technical scheme, the acid tank is provided with a porous barrier plate, which can effectively block the eddy current.
本发明基于原电池反应原理，利用金属的不同氧化物与金属基体形成的电极电位不同，完成金属含量的宏观测定。所用的铜导杆为特制联结铜导杆，可以传导电流，且可以通过调节铜导杆上的螺栓来调节极板的相对距离和极板的高度；所用的恒温磁力搅拌器能够控制电解质溶液温度稳定性和浓度均匀性；酸槽中的多孔阻板能够有效阻隔涡流，保证测量的稳定性。The invention is based on the principle of galvanic battery reaction, utilizes the different electrode potentials formed by different metal oxides and metal substrates, and completes the macroscopic measurement of metal content. The copper guide rod used is a special joint copper guide rod, which can conduct current, and the relative distance of the pole plates and the height of the pole plates can be adjusted by adjusting the bolts on the copper guide rod; the constant temperature magnetic stirrer used can control the temperature of the electrolyte solution Stability and concentration uniformity; the porous barrier in the acid tank can effectively block the eddy current and ensure the stability of the measurement.
本发明的工艺流程为：水槽中装水，酸槽中装酸、磁子和多孔阻板，酸槽放入水槽中，打开恒温磁力搅拌器对酸预热，将极板固定在铜导杆上，铜导杆穿过盖板中间的槽，固定在盖板上，温度稳定后，将极板浸入酸中，固定盖板，打开电位差计开始测量，当电位差计数值稳定在0mV时，测量结束。The technological process of the present invention is as follows: fill water in the water tank, install acid, magnets and porous resistance plates in the acid tank, put the acid tank in the water tank, turn on the constant temperature magnetic stirrer to preheat the acid, and fix the pole plate on the copper guide rod On the top, the copper guide rod passes through the groove in the middle of the cover plate and is fixed on the cover plate. After the temperature is stable, immerse the plate in the acid, fix the cover plate, turn on the potentiometer and start measuring. When the potential difference count value is stable at 0mV , the measurement ends.
本发明的有益效果：Beneficial effects of the present invention:
(1)设备造价低，测试成本低。(1) The equipment cost is low, and the test cost is low.
(2)操作简便，测量稳定性好。(2) Easy to operate and good measurement stability.
(3)测量周期短，可实现对金属氧化膜宏观、快速的测量；及时对表面质量作出预判，及时作出工艺调整可大大减小表面质量不良问题的发生率。(3) The measurement period is short, which can realize the macroscopic and rapid measurement of the metal oxide film; the timely prediction of the surface quality and the timely adjustment of the process can greatly reduce the incidence of poor surface quality problems.
附图说明：Description of drawings:
图1为本发明的整机结构示意图；Fig. 1 is the structural representation of complete machine of the present invention;
图2为本发明的盖板结构图；Fig. 2 is a cover plate structural diagram of the present invention;
图3为本发明的特制联结铜导杆图；Fig. 3 is the special connection copper guide rod figure of the present invention;
图4为本发明的多孔阻板结构图；Fig. 4 is the structural diagram of the porous barrier plate of the present invention;
图5为采用本发明提供的该种分析仪器，测试一种硅钢氧化膜结果图图中：1-电位差计、2-盖板、3-铜导杆、4-第一极板基板、5-第二极板脱碳退火板、6-多孔阻板、7-导线、8-恒温磁力搅拌器、9-磁子、10-酸槽、11-水槽、12-盖板槽、13-注酸孔、14-限位孔、。Fig. 5 is a diagram of the results of testing a silicon steel oxide film using the analytical instrument provided by the present invention: 1-potential difference meter, 2-cover plate, 3-copper guide rod, 4-first plate substrate, 5 -Second pole plate decarburization annealing plate, 6-porous resistance plate, 7-lead wire, 8-constant temperature magnetic stirrer, 9-magnet, 10-acid tank, 11-water tank, 12-cover plate tank, 13-injection Acid hole, 14-limit hole,.
从图5的测量曲线中可以看到FeO的峰很尖锐，说明FeO含量比较少，Fe2SiO4的峰较宽，SiO2也有一个明显的峰，但是比Fe2SiO4的峰略窄。From the measurement curve in Figure 5, it can be seen that the peak of FeO is very sharp, indicating that the content of FeO is relatively small, the peak of Fe 2 SiO 4 is wider, and SiO 2 also has an obvious peak, but it is slightly narrower than that of Fe 2 SiO 4 .
具体实施方式：Detailed ways:
实施例1Example 1
1、水槽11中注入约3000ml水，酸槽10中注入400ml，浓度为8％的硫酸，并将酸槽浸入水中；1. Pour about 3000ml of water into the water tank 11, inject 400ml of sulfuric acid with a concentration of 8% into the acid tank 10, and immerse the acid tank in the water;
2、恒温磁力搅拌器8通电，对酸预热，设定温度40℃，磁子9转速为30转/分钟；2. The constant temperature magnetic stirrer 8 is energized, the acid is preheated, the set temperature is 40°C, and the rotation speed of the magnet 9 is 30 rpm;
3、用导线7将铜导杆3与电位差计1连接，极板4和5通过螺栓固定在铜导杆3上，铜导杆3通过螺栓固定在盖板2上；3. Connect the copper guide rod 3 to the potentiometer 1 with the wire 7, the pole plates 4 and 5 are fixed on the copper guide rod 3 by bolts, and the copper guide rod 3 is fixed on the cover plate 2 by bolts;
4、盖板2盖在酸槽10上，同时极板4和5浸入酸中，用螺栓将盖板2固定在酸槽10上；4. The cover plate 2 is covered on the acid tank 10, while the pole plates 4 and 5 are immersed in the acid, and the cover plate 2 is fixed on the acid tank 10 with bolts;
5、打开电位差计1开始测量，当电位差计上显示值稳定在0mV时，反应完成，关闭电源，结束测量。5. Turn on the potentiometer 1 to start measurement. When the value displayed on the potentiometer is stable at 0mV, the reaction is completed, and the power is turned off to end the measurement.
实施例2Example 2
1、水槽11中注入约4000ml水，酸槽10中注入500ml，浓度为10％的硫酸，并将酸槽10浸入水中；1, inject about 4000ml water in the water tank 11, inject 500ml in the acid tank 10, the concentration is 10% sulfuric acid, and the acid tank 10 is immersed in water;
2、恒温磁力搅拌器8通电，对酸预热，设定温度40℃，磁子9转速为40转/分钟；2. The constant temperature magnetic stirrer 8 is energized, the acid is preheated, the set temperature is 40°C, and the rotation speed of the magnet 9 is 40 rpm;
3、用导线7将铜导杆3与电位差计1连接，极板4和5通过螺栓固定在铜导杆3上，铜导杆3通过螺栓固定在盖板2上；3. Connect the copper guide rod 3 to the potentiometer 1 with the wire 7, the pole plates 4 and 5 are fixed on the copper guide rod 3 by bolts, and the copper guide rod 3 is fixed on the cover plate 2 by bolts;
4、盖板2盖在酸槽10上，同时极板4和5浸入酸中，用螺栓将盖板2固定在酸槽10上；4. The cover plate 2 is covered on the acid tank 10, while the pole plates 4 and 5 are immersed in the acid, and the cover plate 2 is fixed on the acid tank 10 with bolts;
5、打开电位差计1开始测量，当电位差计上显示值稳定在0mV时，反应完成，关闭电源，结束测量。5. Turn on the potentiometer 1 to start measurement. When the value displayed on the potentiometer is stable at 0mV, the reaction is completed, and the power is turned off to end the measurement.
实施例3Example 3
1、水槽11中注入约4000ml水，酸槽10中注入600ml，浓度为12％的硫酸，并将酸槽10浸入水中；1, inject about 4000ml water in the water tank 11, inject 600ml in the acid tank 10, the concentration is 12% sulfuric acid, and the acid tank 10 is immersed in water;
2、恒温磁力搅拌器8通电，对酸预热，设定温度40℃，磁子9转速为40转/分钟；2. The constant temperature magnetic stirrer 8 is energized, the acid is preheated, the set temperature is 40°C, and the rotation speed of the magnet 9 is 40 rpm;
3、用导线7将铜导杆3与电位差计1连接，极板4和5通过螺栓固定在铜导杆3上，铜导杆3通过螺栓固定在盖板2上；3. Connect the copper guide rod 3 to the potentiometer 1 with the wire 7, the pole plates 4 and 5 are fixed on the copper guide rod 3 by bolts, and the copper guide rod 3 is fixed on the cover plate 2 by bolts;
4、盖板2盖在酸槽10上，同时极板4和5浸入酸中，用螺栓将盖板2固定在酸槽10上；4. The cover plate 2 is covered on the acid tank 10, while the pole plates 4 and 5 are immersed in the acid, and the cover plate 2 is fixed on the acid tank 10 with bolts;
5、打开电位差计1开始测量，当电位差计上显示值稳定在0mV时，反应完成，关闭电源，结束测量。5. Turn on the potentiometer 1 to start measurement. When the value displayed on the potentiometer is stable at 0mV, the reaction is completed, and the power is turned off to end the measurement.
实施例4Example 4
1、水槽11中注入约4000ml水，酸槽10中注入600ml，浓度为12％的硫酸，并将酸槽10浸入水中；1, inject about 4000ml water in the water tank 11, inject 600ml in the acid tank 10, the concentration is 12% sulfuric acid, and the acid tank 10 is immersed in water;
2、恒温磁力搅拌器8通电，对酸预热，设定温度50℃，磁子9转速为50转/分钟；2. The constant temperature magnetic stirrer 8 is energized, the acid is preheated, the set temperature is 50°C, and the rotation speed of the magnet 9 is 50 rpm;
3、用导线7将铜导杆3与电位差计1连接，极板4和5通过螺栓固定在铜导杆3上，铜导杆3通过螺栓固定在盖板3上；3. Connect the copper guide rod 3 to the potentiometer 1 with the wire 7, the pole plates 4 and 5 are fixed on the copper guide rod 3 by bolts, and the copper guide rod 3 is fixed on the cover plate 3 by bolts;
4、盖板3盖在酸槽10上，同时极板浸入酸中，用螺栓将盖板固定在酸槽上；4. The cover plate 3 is covered on the acid tank 10, while the polar plate is immersed in the acid, and the cover plate is fixed on the acid tank with bolts;
5、打开电位差计1开始测量，当电位差计上显示值稳定在0mV时，反应完成，关闭电源，结束测量。5. Turn on the potentiometer 1 to start measurement. When the value displayed on the potentiometer is stable at 0mV, the reaction is completed, and the power is turned off to end the measurement.
实施例5Example 5
1、水槽11中注入约4000ml水，酸槽10中注入600ml，浓度为12％的硫酸，并将酸槽10浸入水中；1, inject about 4000ml water in the water tank 11, inject 600ml in the acid tank 10, the concentration is 12% sulfuric acid, and the acid tank 10 is immersed in water;
2、恒温磁力搅拌器8通电，对酸预热，设定温度55℃，磁子9转速为50转/分钟；2. The constant temperature magnetic stirrer 8 is energized, the acid is preheated, the set temperature is 55°C, and the rotation speed of the magnet 9 is 50 rpm;
3、用导线7将铜导杆3与电位差计1连接，极板4和5通过螺栓固定在铜导杆3上，铜导杆3通过螺栓固定在盖板2上；3. Connect the copper guide rod 3 to the potentiometer 1 with the wire 7, the pole plates 4 and 5 are fixed on the copper guide rod 3 by bolts, and the copper guide rod 3 is fixed on the cover plate 2 by bolts;
4、盖板2盖在酸槽上，同时极板4和5浸入酸中，用螺栓将盖板2固定在酸槽10上；4. The cover plate 2 is covered on the acid tank, while the pole plates 4 and 5 are immersed in the acid, and the cover plate 2 is fixed on the acid tank 10 with bolts;
5、打开电位差计1开始测量，当电位差计上显示值稳定在0mV时，反应完成，关闭电源，结束测量。5. Turn on the potentiometer 1 to start measurement. When the value displayed on the potentiometer is stable at 0mV, the reaction is completed, and the power is turned off to end the measurement.
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