CN105353011A - Analyzer for metal oxide film - Google Patents

Analyzer for metal oxide film Download PDF

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Publication number
CN105353011A
CN105353011A CN201510792021.6A CN201510792021A CN105353011A CN 105353011 A CN105353011 A CN 105353011A CN 201510792021 A CN201510792021 A CN 201510792021A CN 105353011 A CN105353011 A CN 105353011A
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China
Prior art keywords
guide rod
oxide film
cover plate
pole plate
metal oxide
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CN201510792021.6A
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CN105353011B (en
Inventor
朱业超
王仁学
周前华
骆忠汉
程祥威
王向欣
郭小龙
林勇
肖光润
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Wuhan Iron and Steel Co Ltd
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Wuhan Iron and Steel Group Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

The invention aims at solving the problems that a silicon steel plate surface oxide layer is long in detection period and investment cost is high, and provides analysis equipment which is based on a primary battery principle and is capable of performing rapid determination on the metal oxide layer. The analysis equipment comprises a potentiometer, a copper guide rod, a cover plate, an acid tank, a water tank, a constant-temperature magnetic stirrer and a porous baffle plate; the constant-temperature magnetic stirrer controls the electrolyte solution temperature stability and concentration uniformity; the copper guide rod is a specially-prepared connecting guide rod, is fixedly disposed on the multifunctional cover plate and is capable of realizing positioning and adjusting of conduction current and a polar plate; and the porous baffle plate is capable of effectively blocking eddy current and guaranteeing the measure stability. The provided equipment is low in cost, low in measure cost, simple to operate and good in measure stability, and is capable of realizing macroscopic rapid measure on the metal oxide film. A figure (5) is the result graphic representation of the apparatus provided by the invention measuring the oriented silicon steel surface oxide layer.

Description

A kind of metal oxide film analyser
Technical field:
The present invention relates to a kind of species analysis equipment, particularly relate to a kind of metal oxide film analyser.
Background technology:
Orientation silicon steel being widely used industrially, but may the bad problems such as surface quality defect be there is in orientation silicon steel is produced, as revealed crystalline substance, leak gold, piebald, interface resistance are low, surface quality problems can improve bottom concession rate on the one hand, improve iron loss on the other hand, also damage the image of product simultaneously.The quality of oxide layer that decarburizing annealing is formed has conclusive impact to final surface quality, but after final painting insulating layer coating, find surface quality problems from decarburizing annealing, arrive problem analysis again and find solution, about need several weeks, produce the bad product of exhibiting high surface quality at this few Zhou Lihui.Therefore, detect quality of oxide layer at decarburizing annealing production line, timely Surface Quality makes anticipation, makes the incidence that technique adjustment can reduce the bad problem of surface quality greatly early.
The domestic analysis to oxide layer at present detects and mainly adopts the micro-analysis means such as scanning electron microscope (SEM), x-ray photoelectron power spectrum (XPS), X-ray diffractometer (XRD) and Auger electron spectroscopy (AES), as magazine " atomic energy science and technology ", the article of volume supplementary issue publication May the 49th in 2015: the double layer oxide film that " the corrosion oxidation layer analysis of cladding materials 316Ti in liquid lead bismuth " report is formed after adopting sem analysis lead base research experiment heap candidate cladding materials 316Ti corrosion; Magazine " Special Processes of Metal Castings and non-ferrous metal ", the article that 25th volume the 3rd periodical in 2005 is stepped on: " the form and structure analysis of magnesium alloy dipulse differential arc oxidization surface rete " report adopts the methods such as XRD, SEM, EDX, have studied pure magnesium and AZ91D magnesium alloy at hexafluoro sodium aluminate (Na 3alF 6), potassium hydroxide (KOH), sodium hexametaphosphate ((NaPO 3) 6) and triethanolamine quaternary component electrolytic solution in the formation of dipulse differential arc oxidation film layer, film shape and constituent structure; Magazine " Chinese corrosion and protection journal ", calendar year 2001 the 21st article stepped on of volume the 3rd periodical: " structure analysis of aluminium surface high pressure anode oxidation membrane " report adopts XRD, SEM and XPS comprehensively to analyze the composition of the high voltage anodization film that aluminium is formed in phosphoric acid and sodium tungstate system, pattern and structure.Disclose in JP 2004-11217 publication and adopt Fourier transform infrared line spectrum (FT-IR) to measure FeO and SiO in the surface oxidation bottom of steel plate 2content ratio.The advantage of these methods is to carry out detailed qualitative analysis and quantitative test to the composition of oxide layer, pattern, structure, therefore scientific research is adapted to especially, but these analytical cycles are long, analyze the little and equipment investment of area and testing cost high, be not suitable in commercial production and need long-term, continuous, large batch of macroscopic view to detect.
Summary of the invention:
For solving the problem, the present invention utilizes galvanic principles, and provide a kind of analytical equipment can carrying out macroscopic view, Quick Measurement to metal oxide film, this equipment manufacturing cost is low, testing cost is low, and easy and simple to handle, Measurement sensibility good.
The present invention for solving the problems of the technologies described above adopted technical scheme is:
A set of metal oxide film analyser, comprise potential difference meter, copper guide rod, cover plate, acid tank, tank and constant temperature blender with magnetic force, it is characterized in that: acid tank upper end securing cover plate, two guide rods pass from the groove of cover plate centre, and fix on the cover board, two lower end of the guide rod are connected with the first pole plate and the second pole plate respectively, and pole plate is immersed in the acid solution of acid tank, two guide rod upper ends are connected with potential difference meter by wire, form loop.
By technique scheme, splendid attire acid and magneton in described acid tank, arrange heat-insulation system outside acid tank, comprise tank and constant temperature blender with magnetic force, wherein tank is placed in constant temperature blender with magnetic force inside.
By technique scheme, cover plate surrounding has 4 spacing holes, and also corresponding aperture on acid tank, is fixed on acid tank by bolt by cover plate, cover plate also has acid-filling mouth, is convenient to supplement acid solution in acid tank.
By technique scheme, guide rod is preferably copper guide rod.
By technique scheme, two copper guide rods pass from the groove of cover plate centre, and copper guide rod is bolted on cover plate by upper and lower two diverse locations; The relative distance of pole plate and the height of pole plate can be regulated by regulating the bolt on copper guide rod.
By technique scheme, two copper guide rod tops are bolted wire, and bottom is cut open and holed, and pole plate is also holed, and be connected with pole plate by copper guide rod by bolt, pole plate is immersed in the acid solution of acid tank.
By technique scheme, pole plate comprises decarburizing annealing plate to be measured and removes the substrate of oxide film.
By technique scheme, in acid tank, establish porous baffle-wall, effectively can intercept eddy current.
The present invention is based on galvanic interaction principle, utilize the different oxide of metal different from the electrode potential that metallic matrix is formed, the macroscopic view completing tenor measures.Copper guide rod used is special bind copper guide rod, can conduction current, and can regulate the relative distance of pole plate and the height of pole plate by regulating the bolt on copper guide rod; Constant temperature blender with magnetic force used can control electrolyte solution temperature stability and even concentration; Porous baffle-wall in acid tank effectively can intercept eddy current, ensures the stability measured.
Technological process of the present invention is: fill water in tank, dress acid, magneton and porous baffle-wall in acid tank, and tank put into by acid tank, open constant temperature blender with magnetic force to sour preheating, be fixed on by pole plate on copper guide rod, copper guide rod, through the groove in the middle of cover plate, is fixed on the cover board, after temperature stabilization, pole plate is immersed in acid, securing cover plate, open potential difference meter and start to measure, when potential difference meter numerical stability is at 0mV, measures and terminate.
Beneficial effect of the present invention:
(1) equipment manufacturing cost is low, and testing cost is low.
(2) easy and simple to handle, Measurement sensibility is good.
(3) measuring period is short, can realize metal oxide film macroscopic view, measure fast; Timely Surface Quality makes anticipation, makes the incidence that technique adjustment can reduce the bad problem of surface quality greatly in time.
Accompanying drawing illustrates:
Fig. 1 is complete machine structure schematic diagram of the present invention;
Fig. 2 is covering plate structure figure of the present invention;
Fig. 3 is special bind copper guide rod figure of the present invention;
Fig. 4 is porous baffle-wall structural drawing of the present invention;
Fig. 5 for adopt this kind of analytical instrument provided by the invention, test in a kind of silicon steel oxide film result figure figure: 1-potential difference meter, 2-cover plate, 3-copper guide rod, 4-first pole plate substrate, 5-second pole plate decarburizing annealing plate, 6-porous baffle-wall, 7-wire, 8-constant temperature blender with magnetic force, 9-magneton, 10-acid tank, 11-tank, 12-slot cover, 13-acid filling hole, 14-spacing hole.
Can see that from the experiment curv of Fig. 5 the peak of FeO is very sharp-pointed, illustrate that FeO comparision contents is few, Fe 2siO 4peak wider, SiO 2also there is an obvious peak, but compare Fe 2siO 4peak slightly narrow.
Embodiment:
Embodiment 1
1, inject about 3000ml water in tank 11, inject 400ml in acid tank 10, concentration is the sulfuric acid of 8%, and is immersed in the water by acid tank;
2, constant temperature blender with magnetic force 8 is energized, to sour preheating, and design temperature 40 DEG C, magneton 9 rotating speed is 30 revs/min;
3, be connected with potential difference meter 1 by copper guide rod 3 with wire 7, pole plate 4 and 5 is bolted on copper guide rod 3, and copper guide rod 3 is bolted on cover plate 2;
4, cover plate 2 covers on acid tank 10, and pole plate 4 and 5 immerses in acid simultaneously, is fixed on acid tank 10 with bolt by cover plate 2;
5, open potential difference meter 1 to start to measure, when on potential difference meter, displayed value is stabilized in 0mV, reaction completes, powered-down, terminates to measure.
Embodiment 2
1, inject about 4000ml water in tank 11, inject 500ml in acid tank 10, concentration is the sulfuric acid of 10%, and is immersed in the water by acid tank 10;
2, constant temperature blender with magnetic force 8 is energized, to sour preheating, and design temperature 40 DEG C, magneton 9 rotating speed is 40 revs/min;
3, be connected with potential difference meter 1 by copper guide rod 3 with wire 7, pole plate 4 and 5 is bolted on copper guide rod 3, and copper guide rod 3 is bolted on cover plate 2;
4, cover plate 2 covers on acid tank 10, and pole plate 4 and 5 immerses in acid simultaneously, is fixed on acid tank 10 with bolt by cover plate 2;
5, open potential difference meter 1 to start to measure, when on potential difference meter, displayed value is stabilized in 0mV, reaction completes, powered-down, terminates to measure.
Embodiment 3
1, inject about 4000ml water in tank 11, inject 600ml in acid tank 10, concentration is the sulfuric acid of 12%, and is immersed in the water by acid tank 10;
2, constant temperature blender with magnetic force 8 is energized, to sour preheating, and design temperature 40 DEG C, magneton 9 rotating speed is 40 revs/min;
3, be connected with potential difference meter 1 by copper guide rod 3 with wire 7, pole plate 4 and 5 is bolted on copper guide rod 3, and copper guide rod 3 is bolted on cover plate 2;
4, cover plate 2 covers on acid tank 10, and pole plate 4 and 5 immerses in acid simultaneously, is fixed on acid tank 10 with bolt by cover plate 2;
5, open potential difference meter 1 to start to measure, when on potential difference meter, displayed value is stabilized in 0mV, reaction completes, powered-down, terminates to measure.
Embodiment 4
1, inject about 4000ml water in tank 11, inject 600ml in acid tank 10, concentration is the sulfuric acid of 12%, and is immersed in the water by acid tank 10;
2, constant temperature blender with magnetic force 8 is energized, to sour preheating, and design temperature 50 DEG C, magneton 9 rotating speed is 50 revs/min;
3, be connected with potential difference meter 1 by copper guide rod 3 with wire 7, pole plate 4 and 5 is bolted on copper guide rod 3, and copper guide rod 3 is bolted on cover plate 3;
4, cover plate 3 covers on acid tank 10, and pole plate immerses in acid simultaneously, is fixed on acid tank with bolt by cover plate;
5, open potential difference meter 1 to start to measure, when on potential difference meter, displayed value is stabilized in 0mV, reaction completes, powered-down, terminates to measure.
Embodiment 5
1, inject about 4000ml water in tank 11, inject 600ml in acid tank 10, concentration is the sulfuric acid of 12%, and is immersed in the water by acid tank 10;
2, constant temperature blender with magnetic force 8 is energized, to sour preheating, and design temperature 55 DEG C, magneton 9 rotating speed is 50 revs/min;
3, be connected with potential difference meter 1 by copper guide rod 3 with wire 7, pole plate 4 and 5 is bolted on copper guide rod 3, and copper guide rod 3 is bolted on cover plate 2;
4, cover plate 2 covers on acid tank, and pole plate 4 and 5 immerses in acid simultaneously, is fixed on acid tank 10 with bolt by cover plate 2;
5, open potential difference meter 1 to start to measure, when on potential difference meter, displayed value is stabilized in 0mV, reaction completes, powered-down, terminates to measure.

Claims (7)

1. a metal oxide film analyser, comprise acid tank (10), first pole plate (4), second pole plate (5) and potential difference meter (1), it is characterized in that: acid tank (10) upper end securing cover plate (2), two guide rods (3) are passed from the groove (12) of cover plate (2) centre, and be fixed on cover plate (2), two guide rod (3) lower ends are connected with the first pole plate (4) and the second pole plate (5) respectively, pole plate is immersed in the acid solution of acid tank (10), two guide rod (3) upper ends are connected with potential difference meter (1) by wire (7), form loop.
2. a kind of metal oxide film analyser according to claim 1, it is characterized in that: described cover plate (2) surrounding has 4 spacing holes (14), by bolt, cover plate (2) is fixed in the corresponding aperture of acid tank (10), cover plate (2) also has acid filling hole (13).
3. a kind of metal oxide film analyser according to claim 2, is characterized in that: described guide rod (3) is copper guide rod, is bolted on cover plate (2).
4. a kind of metal oxide film analyser according to claim 3, it is characterized in that: described copper guide rod (3) bottom is cut open and holes, first pole plate (4) and the boring of the second pole plate (5) upper end, pole plate and guide rod are bolted.
5. a kind of metal oxide film analyser according to claim 4, is characterized in that: described first pole plate (4) and the second pole plate (5) comprise decarburizing annealing plate and remove oxide film substrate.
6. a kind of metal oxide film analyser according to claim 1, is characterized in that: be provided with porous baffle-wall (6) in acid tank (2).
7. a kind of metal oxide film analyser according to claim 1, it is characterized in that: described acid tank arranges heat-insulation system outside (10), comprise tank (11) and constant temperature blender with magnetic force (8), wherein tank is placed in constant temperature blender with magnetic force.
CN201510792021.6A 2015-11-17 2015-11-17 A kind of metal oxide film analyzer Expired - Fee Related CN105353011B (en)

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Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4229264A (en) * 1978-11-06 1980-10-21 The Boeing Company Method for measuring the relative etching or stripping rate of a solution
CN85200979U (en) * 1985-04-01 1986-06-18 田振武 Flaw detector for coating film
CN86100248A (en) * 1986-01-10 1986-09-03 机械工业部沈阳仪器仪表工艺研究所 Measure the admittance instrument of alumilite process membrane closure quality
EP0282332A2 (en) * 1987-03-11 1988-09-14 Sogo Pharmaceutical Company Limited Method of detecting bitter or odor substances and apparatus therefor
JPH0211783A (en) * 1988-06-30 1990-01-16 Furukawa Alum Co Ltd Method of monitoring contact corrosion of different metals and corrosion resistance tester
EP0760473A1 (en) * 1995-08-24 1997-03-05 Matsushita Electric Industrial Co., Ltd. Metal surface state evaluation method and semiconductor device production method
EP1956357A1 (en) * 2007-02-06 2008-08-13 Royal Scientific Society Galvanic Corrosion Monitoring And Analysis System
US20080257729A1 (en) * 2007-02-05 2008-10-23 Saeed Farqad F M Galvanic corrosion monitoring and analyzing system
CN201464415U (en) * 2009-07-01 2010-05-12 上海宝钢工业检测公司 Electrode device for determining oxidation film potential difference curve on strip steel surfaces
CN102134718A (en) * 2009-11-30 2011-07-27 韦特柯格雷控制系统有限公司 Method of monitoring cathode protection
KR20120073680A (en) * 2010-12-27 2012-07-05 주식회사 포스코 Apparatus for measuring corrosion of aluminium passivity metal and method for testing corrosion of aluminium passivity metalal using the same
CN203299161U (en) * 2013-03-04 2013-11-20 上海宝钢工业技术服务有限公司 Multifunctional tin plate surface property testing device
CN203965379U (en) * 2014-07-18 2014-11-26 上海电缆研究所 Electrician uses copper bar oxide thickness proving installation

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4229264A (en) * 1978-11-06 1980-10-21 The Boeing Company Method for measuring the relative etching or stripping rate of a solution
CN85200979U (en) * 1985-04-01 1986-06-18 田振武 Flaw detector for coating film
CN86100248A (en) * 1986-01-10 1986-09-03 机械工业部沈阳仪器仪表工艺研究所 Measure the admittance instrument of alumilite process membrane closure quality
EP0282332A2 (en) * 1987-03-11 1988-09-14 Sogo Pharmaceutical Company Limited Method of detecting bitter or odor substances and apparatus therefor
JPH0211783A (en) * 1988-06-30 1990-01-16 Furukawa Alum Co Ltd Method of monitoring contact corrosion of different metals and corrosion resistance tester
EP0760473A1 (en) * 1995-08-24 1997-03-05 Matsushita Electric Industrial Co., Ltd. Metal surface state evaluation method and semiconductor device production method
US20080257729A1 (en) * 2007-02-05 2008-10-23 Saeed Farqad F M Galvanic corrosion monitoring and analyzing system
EP1956357A1 (en) * 2007-02-06 2008-08-13 Royal Scientific Society Galvanic Corrosion Monitoring And Analysis System
CN201464415U (en) * 2009-07-01 2010-05-12 上海宝钢工业检测公司 Electrode device for determining oxidation film potential difference curve on strip steel surfaces
CN102134718A (en) * 2009-11-30 2011-07-27 韦特柯格雷控制系统有限公司 Method of monitoring cathode protection
KR20120073680A (en) * 2010-12-27 2012-07-05 주식회사 포스코 Apparatus for measuring corrosion of aluminium passivity metal and method for testing corrosion of aluminium passivity metalal using the same
CN203299161U (en) * 2013-03-04 2013-11-20 上海宝钢工业技术服务有限公司 Multifunctional tin plate surface property testing device
CN203965379U (en) * 2014-07-18 2014-11-26 上海电缆研究所 Electrician uses copper bar oxide thickness proving installation

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