CN104568638A - Method for testing binding ability of rust layer and substrate of rusted steel sample, and apparatus thereof - Google Patents

Method for testing binding ability of rust layer and substrate of rusted steel sample, and apparatus thereof Download PDF

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CN104568638A
CN104568638A CN201310469667.1A CN201310469667A CN104568638A CN 104568638 A CN104568638 A CN 104568638A CN 201310469667 A CN201310469667 A CN 201310469667A CN 104568638 A CN104568638 A CN 104568638A
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steel sample
sample
steel
matrix
band rust
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CN104568638B (en
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徐小连
李琳
高鹏
艾芳芳
陈义庆
钟彬
肖宇
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Angang Steel Co Ltd
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Abstract

The invention discloses a method for testing the binding ability of the rust layer and the substrate of a rusted steel sample, and an apparatus thereof. The apparatus is composed of a frame and a clamp, the frame is composed of a pedestal, a supporting frame and a top board, the clamp is composed of a sample carrying platform baseboard, a sample carrying platform surface elastic cushion, an elastic cushion for steel sample upper surface test, a steel sample upper surface pressing board and five same fastening screws, the five same fastening screws are inserted between the top board and the steel sample upper surface pressing board, a pressure measuring induction probe is arranged between the sample carrying platform baseboard and the sample carrying platform elastic cushion, and the probe is connected to a pressure measuring meter. The method includes the following steps: polishing the sample, carrying out corrosion test, weighing the sample after the corrosion, desalting, drying, carrying out rust removal on the testing apparatus, weighing the rust removed sample, and calculating the corrosion rate. The method can quantitatively response the binding ability of the rust layer and the substrate of the rusted steel sample, and provides corrosion resistant bases for researches of new species of steel; and the apparatus has the advantages of simple structure, low cost and easy maintenance.

Description

A kind of with rust steel sample rusty scale and the method for testing of matrix bonding properties and device
Technical field
The invention belongs to steel corrosion detection technique field, relate to a kind of method of testing with rust steel sample rusty scale and matrix bonding properties and device, be specially adapted to quantitative test band and become rusty the combination degree of steel sample Surface Rust and matrix.
Background technology
The corrosion of steel is a general and serious problem, and the loss that wherein atmospheric corrosion causes accounts for the half of whole corrosion loss.And the economic loss caused due to corrosion of steel structure every year accounts for 2% ~ 4% of national economy total output value.At present, the economic loss that causes because of corrosion of steel structure every year of the whole world is up to more than hundreds billion of dollar; Therefore, hold corrosion-prone problem in an atmosphere to solve steel, people have developed weathering steel.Weathering steel has good atmospheric corrosion resistance relative to carbon steel, and one of the main reasons is through long term atmospheric and is exposed to the sun, and define the protective rust being combined firmly, stablizing densification with matrix in its surface, it hinders entering of corrosive medium; And loosen at the rusty scale that steel surface is formed, not firmly, easily come off with matrix bonding properties and have micro-crack to exist, therefore can not play a protective role to matrix.
In order to evaluate weathering steel and carbon steel in dissimilar atmospheric environment form the protective effect of rusty scale to matrix; the particularly bonding properties of rusty scale and matrix; the correlation technique found at present has: " research of Protective Rust Layer Formed on Surface of Weathering Steel Panels and substrate combinating strength " that the people such as Zhang Quancheng deliver, and they are the interface bond strengths measuring weather-resistant steel plate rusty scale/matrix system with indentation method.The method needs to carry out thinning to steel sample Surface Rust, carries out indentation test afterwards with sclerometer under the load that applying is certain, gets its cracking or peels off diameter to investigate weathering steel rusty scale and matrix bonding properties.The method needs fixing sclerometer equipment, can destroy the matrix surface of steel sample after test, can not carry on next step corrosion rate test." impact that the synergy of Cu, Mn is corroded in simulated marine atmosphere environment low alloy steel " that the superfine people of Liu state delivers, they corrode element and chemical state thereof in the weightening finish rule of rusty scale, the growthform of rusty scale, thing phase, rusty scale with the means researchs such as weightening finish method, scanning electron microscope, X-ray diffraction, electron probe and x-ray photoelectron power spectrum 16Mn steel and Cu-Mn weathering steel under simulated marine atmosphere dry wet alternating environment.Weightening finish method is the growth rate embodying rusty scale in its rusty scale forming process, can not embody the bonding properties of rusty scale and matrix; Scanning electron microscope observes the pattern of rusty scale; X-ray diffraction is the phase structure of test rusty scale material; And electron probe and x-ray photoelectron power spectrum are chemical state analysis rusty scale being carried out to element depth analysis and alloying element respectively.They all directly can not react the bonding properties of rusty scale and matrix, and device therefor is very expensive." character of marine environment medium carbon steel Surface Rust and research method " that the people such as Zou Yan deliver, they mainly discuss pattern, the constitution and formation mechanism of steel surface rusty scale, utilize electrochemical impedance method to measure electric conductivity and the poriness of rusty scale respectively, utilize the corrosion speed of gravimetric method and electrochemical techniques measuring metallic materials.Little with the bonding properties relation of test rusty scale and matrix.
In sum, also do not have to destroy metal base surface at present, and can simple and easy to do, calibration tape rust steel sample rusty scale and the method for matrix bonding properties and device quantitatively, with the satisfied research different rusty scale of steel grade surface formation and the bonding properties of matrix in different environments, the therefrom corrosion stability of reaction material in its respective environment.
Summary of the invention
Not only for Problems existing during above-mentioned measurement metal base surface band rust steel sample rusty scale, the invention provides and a kind ofly do not destroy metal base surface but also can simple and easy to do, calibration tape rust steel sample rusty scale and matrix bonding properties and take into account the method and apparatus that simultaneously can test out the corrosion rate of its steel sample quantitatively.
The concrete technical scheme that the present invention takes is as follows:
The first step: the test steel sample of polishing of learning from else's experience carries out degreasing and neutralisation treatment, measures sample length, width and height after cleaning and dehydration, and to calculate its surface area be that S(is accurate to 0.01mm 2), weighing its quality is M 0(being accurate to 0.1mg).
Second step: steel sample is put into the corrosion environments such as alternate-immersion equipment and carry out corrosion test.
3rd step: after some cycles test, carefully taken out from corrosion environment by band rust steel sample, avoiding colliding with is attached to the corrosion product on steel sample surface.
4th step: deionized water band rust steel sample being put into temperature>=40 DEG C, swings with the speed of 20 ± 2 times/min., dissolve the material being taken to steel sample surface by the salt in corrosion environment, as NaCl, Na 2sO 4, Na 2sO 3, Na 2cO 3, NaHCO 3, NaF, MgCl 2, CaCl 2, KCl, KBr etc., avoid these materials to bring in steel sample rusty scale and form impurity, affect the accuracy of test data.Deionized water temperature <40 DEG C, the salt on steel sample surface is not soluble; Swing speed is higher than 22 times/min., and the corrosion product on band rust steel sample surface can be made to come off, and swing speed is lower than 18 times/min., and the salt on its steel sample surface corrosion product is difficult to remove.
5th step: the band rust steel sample surface plate after desalination has been contained the constant temperature oven putting into 105 ± 1 DEG C, insulation 2h, has removed the moisture in steel sample Surface Rust.
6th step: careful taking-up is with rust steel sample from constant temperature oven, puts into exsiccator and is cooled to room temperature, then the quality of the band rust steel sample that weighs with scale is M 11(being accurate to 0.1mg).
7th step: again band rust steel sample surface plate has been contained the constant temperature oven putting into 105 ± 1 DEG C, insulation 2h, removed the moisture in steel sample Surface Rust further; Put into exsiccator afterwards to room temperature, then the quality of the band rust steel sample that weighs with scale is M 12(being accurate to 0.1mg); Repeat the 5th step ~ the 7th step, the quality obtaining being with rust steel sample is M 1n, multiplicity is to M 1n-1-M 1n≤ 0.2mg.
8th step: by the band rust steel sample cohesive strength>=2.4N/cm through drying also constant weight 2adhesive tape spread on band rust steel sample upper and lower surface respectively, two ends reserve certain surplus with the upper lower clamp of fixing card sample, drive the residual air between rust sample surface and adhesive tape out of.Cohesive strength <2.4N/cm 2adhesive tape pair do not have the effect of stripping with matrix in conjunction with insecure rusty scale.
9th step: upper and lower surface is placed in up and down with the fixture of cushion by the band rust steel sample that adhesive tape is deposited with, guarantees that steel sample surface all can be stressed with cushion.
Tenth step: screwing fastening screw successively to steel sample surface pressing according to clockwise and middle part is 400 ± 5Pa, leaves standstill >=3min..Pressure <395Pa, adhesive tape is deposited with insufficient strength with matrix in conjunction with insecure rusty scale to steel sample surface; Pressure >405Pa, steel sample Surface Rust institutional framework can be destroyed.Standing <3min. also can cause adhesive tape not reach requirement with matrix in conjunction with the intensity that is deposited with of insecure rusty scale to steel sample surface.
11 step: fastening screw of outwarding winding successively, takes out band rust steel sample, takes adhesive tape off.
12 step: weigh and be only greater than 2.4N/cm with bond matrix intensity 2band rust steel sample quality be M 21(being accurate to 0.1mg).
13 step: repeat the 8th step ~ the 12 step, to M 2n-1-M 2n≤ 0.2mg, ensures allly all to be stripped in conjunction with insecure rusty scale with matrix.
14 step: band rust steel sample is put into 15% ~ 18% hydrochloric acid being added with 20g/L urotropine, and temperature is room temperature, removes all rusty scales on steel sample surface, with the naked steel sample of washed with de-ionized water, and with dehydration of alcohol, dries up with hair-dryer, put into exsiccator 2h.
15 step: weighing naked steel sample quality is M 3(precision is 0.1mg).
16 step: design following formula and carry out CHARACTERISATION TESTS steel and forms the quality of rusty scale and matrix bonding properties in its surface institute of specific environment, namely calculating and matrix are in conjunction with the number percent R of overall rusty scale shared by insecure rusty scale.
Computing formula is: R = M 1 n - M 2 n M 1 n - M 3 &times; 100 %
In formula: R---and the mass percent (%) of matrix in conjunction with the shared overall rusty scale of insecure rusty scale;
M 1n---band rust steel sample gross mass (g);
M 2n---stick out through adhesive tape the quality (g) being with the steel sample that becomes rusty with matrix after insecure rusty scale;
M 3---wash the quality (g) of steel sample after all rusty scales in steel sample surface off.
R value is high, and illustrate that test steel surface institute forms the bonding properties of rusty scale and matrix poor, the protective capacities of its rusty scale to steel matrix is weak, i.e. test steel corrosion-resistant; Vice versa.
Note: utilize above data to pass through formula calculates the corrosion rate (CR) of its test steel sample simultaneously.
Concrete pick-up unit of the present invention is made up of framework and fixture, framework is made up of pedestal, bracing frame and top board, fixture is made up of load sample platform base plate, load sample table top cushion, steel sample upper surface test cushion and steel sample upper surface pressing plate, 5 identical fastening screws, fastening screw assigns between top board and steel sample upper surface pressing plate, between load sample platform base plate and load sample table top cushion, settle pressure measurement inductive probe, probe is connected to pressure gauge.
Advantage of the present invention and effect are that the method can the bonding properties of quantitative reaction band rust steel sample rusty scale and matrix, provide corrosion stability foundation for studying new steel grade; Institute's contrive equipment structure is simple, cost is low, be easy to maintenance.
Accompanying drawing explanation
Fig. 1 is tested steel sample rusty scale and matrix bonding properties device schematic diagram.
In Fig. 1,1 is device pedestal, and 2 is device support stand, 3 is device frame top board, 4 is load sample platform base plate, and 5 is load sample table top cushion, and 6 is steel sample lower surface test tape, 7 is steel sample upper surface test tape, 8 is steel sample upper surface test cushion, and 9 is steel sample upper surface pressing plate, and 10 ~ 14 is fastening screw, 15 is pressure gauge, and 16 is band rust steel sample.
Embodiment
Below in conjunction with Fig. 1, the present invention is described in detail: proving installation of the present invention is made up of framework and fixture, framework is by pedestal 1, bracing frame 2 and top board 3 form, fixture is by load sample platform base plate 4, load sample table top cushion 5, steel sample upper surface test cushion 8, steel sample upper surface pressing plate 9 and 5 identical fastening screws 10, fastening screw 11, fastening screw 12, fastening screw 13, fastening screw 14 forms, fastening screw assigns between top board 3 and steel sample upper surface pressing plate 9, pressure measurement inductive probe is settled between load sample platform base plate 4 and load sample table top cushion 5, probe is connected to pressure gauge 15.
Get one group of 50mm × 50mm × 5mm Kesternich test steel sample through polishing and carry out degreasing and neutralisation treatment, after cleaning and dehydration, by miking sample length, width and height, and to calculate its surface area be S, and weighing its quality respectively with the electronic balance that precision is 0.1mg is M 0.Afterwards test steel sample is put into alternate-immersion test machine, carry out test according to the design of simulated marine atmosphere alternation of wetting and drying corrosion test.
Behind 7 days, 15 days, 30 days and 60 day test period, rust steel sample is with carefully to take out from alternate-immersion test machine respectively, put into the deionized water container filling temperature >=40 DEG C, swing with the speed of 20 ± 2 times/min., dissolve the salts such as the NaCl brought to steel sample surface by corrosion environment; Band rust steel sample surface plate after desalination is contained the constant temperature oven putting into 105 ± 1 DEG C, insulation 2h, removes the moisture in steel sample Surface Rust.
Carefully from constant temperature oven take out band rust steel sample, put into exsiccator and be cooled to room temperature, then with precision be 0.1mg electronic balance respectively the become rusty quality of steel sample of weigh belt be M 11.
Again band rust steel sample surface plate is contained the constant temperature oven putting into 105 ± 1 DEG C, insulation 2h, remove the moisture in steel sample Surface Rust further; Put into exsiccator afterwards to room temperature, then the quality of the band rust steel sample that weighs with scale is M 12(being accurate to 0.1mg).Repeat constant temperature, cooling, weighing to M 1n-1-M 1n≤ 0.2mg.
By the band rust steel sample cohesive strength>=2.4N/cm through drying also constant weight 2for steel sample lower surface adhesive tape 6, for steel sample upper surface adhesive tape 7, spread on the band rust upper and lower surface of steel sample respectively, two ends reserve certain surplus with fixing load sample platform base plate 4, load sample table top cushion 5 and steel sample upper surface test cushion 8, steel sample upper surface pressing plate 9, and drive the residual air between rust sample surface and adhesive tape out of.The band rust steel sample 16 being covered with adhesive tape is placed in the middle of the upper and lower steel sample upper surface test cushion 8 with sponge bullet and load sample table top cushion 5, when to screw fastening screw 10 ~ 14 to steel sample surface pressing table 15 pressure be successively 400 ± 5Pa according to screw rod that is clockwise and middle part, leave standstill 3min..To outward winding successively fastening screw 10 ~ 14, take out band rust steel sample, take steel sample lower surface adhesive tape 6 off, upper surface adhesive tape 7.
Weigh and be only greater than 2.4N/cm with bond matrix intensity 2band rust steel sample quality be M 21(being accurate to 0.1mg).Repeat to be deposited with adhesive tape, clamp, take off adhesive tape and weigh to M 2n-1-M 2n≤ 0.2mg, ensures allly all to be stripped in conjunction with insecure rusty scale with matrix.
At room temperature put into rust steel sample 15% ~ 18% hydrochloric acid being added with 20g/L urotropine respectively, remove all rusty scales on steel sample surface, with the naked steel sample of washed with de-ionized water, and with dehydration of alcohol, dry up with hair-dryer, put into exsiccator 2h.
The quality weighing naked steel sample with the electronic balance that precision is 0.1mg is respectively M 3.
Use formula calculate respectively and the number percent of matrix in conjunction with the shared overall rusty scale of insecure rusty scale, pass through simultaneously formulae discovery goes out the corrosion rate of its respective steel sample, the results are shown in Table 1.
Table 1 is with rust steel sample and the corrosion rate of matrix in conjunction with insecure rusty scale shared totally rusty scale number percent and steel sample thereof
Test piece number (Test pc No.) 1 2 3 4
S/mm 2 6203.85 6199.80 6197.97 6144.67
M 0/g 104.7719 104.1538 104.1243 104.4805
M 1/g 105.6452 104.2836 103.8562 104.4610
M 2/g 101.3975 98.9359 100.1861 104.2459
M 3/g 100.5874 97.3095 93.0037 87.8005
T/ days 7 15 30 60
R/% 83.98 76.68 33.82 1.29
CR/(g.m -2.h -1) 4.0149 306665 2.4920 1.8851
Note: T--corrosion test time.

Claims (2)

1. the method for testing with become rusty steel sample rusty scale and matrix bonding properties, is characterized in that,
Concrete technology step is as follows:
The first step: the test steel sample of polishing of learning from else's experience carries out degreasing and neutralisation treatment, measures sample length, width and height after cleaning and dehydration, and to calculate its surface area be S, and weighing its quality is M 0;
Second step: steel sample is put into alternate-immersion equipment and carries out corrosion test;
3rd step: after test, takes out band rust steel sample from corrosion environment;
4th step: deionized water band rust steel sample being put into temperature >=40 DEG C, swings with the speed of 20 ± 2 times/min.;
5th step: the band rust steel sample surface plate after desalination has been contained the constant temperature oven putting into 105 ± 1 DEG C, insulation 2h;
6th step: take out band rust steel sample from constant temperature oven, put into exsiccator and be cooled to room temperature, then the quality of the band rust steel sample that weighs with scale is M 11;
7th step: again band rust steel sample surface plate has been contained the constant temperature oven putting into 105 ± 1 DEG C, insulation 2h, removed the moisture in steel sample Surface Rust further; Put into exsiccator afterwards to room temperature, then the quality of the band rust steel sample that weighs with scale is M 12; Repeat the 5th step ~ the 7th step, the quality obtaining being with rust steel sample is M 1n, multiplicity is to M 1n-1-M 1n≤ 0.2mg;
8th step: by the band rust steel sample cohesive strength>=2.4N/cm through drying also constant weight 2adhesive tape spread on band rust steel sample upper and lower surface respectively, two ends reserve surplus with the upper lower clamp of fixing card sample;
9th step: upper and lower surface is placed in up and down with the fixture of cushion by the band rust steel sample that adhesive tape is deposited with;
Tenth step: screwing fastening screw successively to steel sample surface pressing according to screw rod that is clockwise and middle part is 400 ± 5Pa, leaves standstill >=3min;
11 step: fastening screw of outwarding winding successively, takes out band rust steel sample, takes adhesive tape off;
12 step: weigh and be only greater than 2.4N/cm with bond matrix intensity 2band rust steel sample quality be M 21;
13 step: repeat the 8th step ~ the 12 step, to M 2n-1-M 2n≤ 0.2mg;
14 step: band rust steel sample is put into 15% ~ 18% hydrochloric acid being added with 20g/L urotropine, and temperature is room temperature, removes all rusty scales on steel sample surface, with the naked steel sample of washed with de-ionized water, and with dehydration of alcohol, dries up with hair-dryer, put into exsiccator 2h;
15 step: weighing naked steel sample quality is M 3;
16 step: design following formula and carry out CHARACTERISATION TESTS steel and forms the quality of rusty scale and matrix bonding properties in its surface institute of specific environment, namely calculating and matrix are in conjunction with the number percent R of overall rusty scale shared by insecure rusty scale;
Computing formula is: R = M 1 n - M 2 n M 1 n - M 3 &times; 100 %
In formula: R---and the mass percent (%) of matrix in conjunction with the shared overall rusty scale of insecure rusty scale;
M 1n---band rust steel sample gross mass (g);
M 2n---stick out through adhesive tape the quality (g) being with the steel sample that becomes rusty with matrix after insecure rusty scale;
M 3---wash the quality (g) of steel sample after all rusty scales in steel sample surface off;
R value is high, and illustrate that test steel surface institute forms the bonding properties of rusty scale and matrix poor, the protective capacities of its rusty scale to steel matrix is weak, i.e. test steel corrosion-resistant; Vice versa;
Meanwhile, above data are utilized to pass through formula calculates the corrosion rate of its test steel sample simultaneously, CR---corrosion rate.
2. one kind is applied to the device of the method for testing of band rust steel sample rusty scale according to claim 1 and matrix bonding properties, it is characterized in that, it is made up of framework and fixture, framework is by pedestal (1), bracing frame (2) and top board (3) composition, fixture is by load sample platform base plate (4), load sample table top cushion (5), steel sample upper surface test cushion (8) and steel sample upper surface pressing plate (9) and 5 identical fastening screws compositions, fastening screw assigns between top board (3) and steel sample upper surface pressing plate (9), pressure measurement inductive probe is settled between load sample platform base plate (4) and load sample table top cushion (5), probe is connected to pressure gauge (15).
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CN113640216A (en) * 2021-09-14 2021-11-12 鞍钢股份有限公司 Device and method for evaluating adhesive force of rust layer of rusted steel sample
CN113686764A (en) * 2021-07-27 2021-11-23 中联先进钢铁材料技术有限责任公司 Corrosive liquid for simulating corrosion of steel in south sea environment and simulation method
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CN112161923A (en) * 2020-09-03 2021-01-01 燕山大学 Method for detecting bonding strength between weathering steel rust layer and substrate
CN113686764A (en) * 2021-07-27 2021-11-23 中联先进钢铁材料技术有限责任公司 Corrosive liquid for simulating corrosion of steel in south sea environment and simulation method
CN113686764B (en) * 2021-07-27 2024-05-10 中联先进钢铁材料技术有限责任公司 Corrosive liquid for simulating steel corrosion in south China sea environment and simulation method
CN113702276A (en) * 2021-07-28 2021-11-26 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) Corrosion environment and corrosion characteristic dynamic acquisition device
CN113702276B (en) * 2021-07-28 2023-12-05 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) Corrosion environment and corrosion characteristic dynamic acquisition device
CN113640216A (en) * 2021-09-14 2021-11-12 鞍钢股份有限公司 Device and method for evaluating adhesive force of rust layer of rusted steel sample
CN114323842A (en) * 2021-12-14 2022-04-12 北京科技大学 Rusty metal cultural relic simulation sample and manufacturing method thereof

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