CN101498648B - Multifunctional in-situ electro-chemical measuring apparatus for tensile test - Google Patents

Multifunctional in-situ electro-chemical measuring apparatus for tensile test Download PDF

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Publication number
CN101498648B
CN101498648B CN200910076351XA CN200910076351A CN101498648B CN 101498648 B CN101498648 B CN 101498648B CN 200910076351X A CN200910076351X A CN 200910076351XA CN 200910076351 A CN200910076351 A CN 200910076351A CN 101498648 B CN101498648 B CN 101498648B
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electrochemical
electrode
multifunctional
chamber
tension test
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CN200910076351XA
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CN101498648A (en
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高克玮
庞晓露
郜明文
李东东
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

A multifunctional in-situ electrochemical measuring device used for the tension test belongs to the electrochemical field. The multifunctional in-situ electrochemical measuring device used for the tension test is characterized in that a reference electrode, an auxiliary electrode and a working electrode are arranged in a top cover of the multifunctional in-situ electrochemical measuring device according to design and measurement requirements; the conductive wires of all the electrodes are connected with an electrochemical workstation; the air input of an air inlet and the air output of an air outlet are adjusted; an installed heating resistor and a thermocouple are connected with a temperature controlling device; the water flow of a water inlet and the water flow of a water outlet are adjusted, and the water inlet and the water outlet are connected with an externally connected water pump. The rotation time of a stepping motor is set, electrochemical parameters of a tensile test sample are measured after the temperature and the pressure are increased to the parameters required by the tension test, and the tension test is conducted after the force of the tensile test sample is adjusted. The multifunctional in-situ electrochemical measuring device used for the tension test has simple and easy method, can measure the electrochemical parameters of the tensile test sample in a long time and can simulate the temperature, the moisture, the gas, the alternation of wetting and drying, the surface scouring, the multiphase medium and complex environment of the tensile test sample.

Description

The multifunctional in-situ electro-chemical measuring apparatus that a kind of tension test is used
Technical field
The invention belongs to electrochemical field, mainly be that sample when dynamic tensile is tested carries out temperature, humidity, gas and alternation of wetting and drying, surface erosion, the simulation of complex environments such as multiphase medium, and utilize the electrochemical in-situ detection technique to carry out on-line measurement, particularly under long-time unmanned state, the stretching sample is carried out electrochemical measurement.
Background technology
Traditional cupping machine can stretch to sample according to request for utilization, compression, bending, creep, lax wait test, be mainly used in test, study metal, nonmetal, compound substance and manufactured goods corrode in various media and stress under mechanical property.Although traditional drawing machine can apply multiple mechanical property to test specimen, and can select different anchor clamps to carry out imposed load according to different samples, but can not simulate the needed external environment of sample, as temperature, humidity, solution, gas etc., limited the research technique of experiment material under the plus load situation, and lack the tracking measurement that corresponding external device comes the sample of bearing load is carried out electrochemical parameter, lack the characterization parameter of verifying material mechanical performance, can not further understand the corrosion behavior of material and the mechanism that corrosion takes place, test is existed certain restriction.
Generally the electrochemical measurement of sample then is after the sample imposed load finishes, and the electrochemical measurement system of normal temperature and pressure is put in its taking-up, utilizes three-electrode system that electrode potential and electric current are controlled respectively and measured again.The numerical value of gained only is that sample carries out the performance that mechanical property military service back is showed, performance and variation in the time of can not characterizing its military service process like this.After eliminating load, change has to a certain degree more likely taken place in the mechanics of material and chemical property, and therefore this measurement lacks for the guidance of practice meaning.
Summary of the invention
The objective of the invention is to solve the problems such as error imperfect and that cause owing to experimental system is different that original stretching instrument and electrochemical appliance separate the experimental data that produced of experimentizing.On drawing machine, sample is carried out the measurement and the analysis of electrochemical parameter, realize dynamic online detection, obtain the partial data of laboratory sample electrochemical parameter under longer etching time, and in the measuring process of original three-electrode system, realize the simulation of multiple environmental factor, increased the integrality of data in tension test diversity and the test process.
The multifunctional in-situ electro-chemical measuring apparatus that a kind of tension test is required is made up of electrochemical appliance, environment simulator and drawing machine three parts.Electrochemical appliance comprises that partly auxiliary electrode, contrast electrode and working electrode are tensile sample.Environment simulator comprises thermopair, heating resistor, air intake opening, gas outlet, water inlet, water delivering orifice, rubber plug, fixed spiro, top cover and cavity.Drawing machine comprises upper and lower chuck.
With the multifunctional in-situ electro-chemical measuring apparatus drawing machine of packing into, its middle chamber drops on the lower chuck.The tensile sample and the chuck that are welded with lead are sealed up for safekeeping with 704 silica gel, reserved the area that numerical value is subscribed in test; With salt bridge, thermopair, the rubber plug top cover of packing into, and auxiliary electrode inserted in the rubber plug; With the rubber plug chamber of packing into, and tensile sample passed rubber plug in chamber and the top cover; Rotating cap and chamber closure; With pack into cavity bottom and tightening of heating resistor, open air intake opening and insert gas cylinder, adjust the size of giving vent to anger of gas port; Close water delivering orifice, open water inlet and close water inlet after with solution injecting chamber; After inserting contrast electrode in the salt bridge, with contrast electrode, tensile sample, the lead of auxiliary electrode inserts electrochemical workstation, the lead cut-in temperature control device of thermopair, heating resistor; Stretch behind the stress load of adjustment tensile sample; On the stretching instrument, sample is carried out the measurement and the analysis of electrochemical parameter, realize dynamic online detection, obtain the partial data of laboratory sample electrochemical parameter under longer etching time, and in the measuring process of original three-electrode system, realize the simulation of multiple environmental factor, increased the integrality of data in tension test diversity and the test process.
Because tensile sample should be simulated extraneous environmental baseline and be guaranteed sample again do not have plus load except that the load of the drawing machine that is subjected to when the singularity of testing has determined carrying out tension test, if in solution environmental, want in addition to guarantee between tensile sample and the anchor clamps leakproofness, prevent that it from bimetallic corrosion taking place influence test findings.Therefore anchor clamps and test specimen to be sealed up for safekeeping with 704 silica gel near the part of anchor clamps, only be stayed the definite stretched portion of area and carry out electrochemical test.As shown in Figure 1
Electrochemical appliance partly adopts traditional three-electrode system to measure.Used auxiliary electrode is a platinum electrode, and contrast electrode is a mercurous chloride electrode, and it is selected that working electrode is looked experiment material.Wherein relative with auxiliary electrode in the working electrode, contrast electrode is positioned at salt bridge, and salt bridge and working electrode distance are close, and distribution situation as shown in Figure 2.
Introduce workstation from the three electrode lead that device extracts.Then will install the interior environment solution that injects as needs simulated environment temperature, with thermopair, heating resistor acromere such as attemperating unit.Environment as need simulation specific gas then inserts gas cylinder with air intake opening, and by the size of gas admittance valve control air inflow, gas is discharged from the gas outlet.Then water inlet and water delivering orifice are external to water pump as need simulation dry wet alternating environment, inject the simulation that solution is realized dry wet alternating environment interval time.
Line Measurement Technique is the variation of the electrochemical characteristic of tracking test sample better, and is especially longer at etching time, and under the more condition of measurement data, line Measurement Technique can embody its advantage better, significantly improves work efficiency.
The temperature control principle of this device is as follows, and heating resistor is positioned at the chamber inboard, and the solution of entire reaction chamber is heated, and thermopair has constituted the temperature hierarchy of control with heating resistor, by external electronic device control reaction chamber indoor temperature.Thereby the air inflow in the reaction chamber obtains required Temperature numerical of experimenter and ambiance by inlet, outlet control.
The required multifunctional in-situ electro-chemical measuring apparatus of the tension test that the present invention relates to has been compared following characteristics with traditional tension test:
1. realized the electrochemical on-line measurement of material under the plus load state.
2. reduce laboratory sample and under different condition, measured the error of its electrochemical parameter.
3. can simulate multiple external environmental condition, enrich the diversity of tension test at research material military service aspect of performance, means are simple, realize easily.
Compared with prior art, the method of the multifunctional in-situ electro-chemical measuring apparatus that the tension test that this device adopts is required, make the measurement data complete and accurate, avoided in two different systems because the influence that environmental error brought, and real simulated site environment more, make experimental data reliable, and tracking measurement makes data point more complete for a long time, for the experimenter grasps data as much as possible under time-limited situation, the electrochemical mechanism of further probing in the corrosion process provides convenience.Simultaneously more measurement data, the time interval that makes measurement point, the curve of time and electrochemical parameter was complete credible accurately and reliably.This device has structural safety, easy operating, and measurement data is enriched characteristics such as accurate.
Description of drawings
Fig. 1 multifunctional in-situ electro-chemical measuring apparatus structural drawing
Tensile sample 1, salt bridge 2, auxiliary electrode 3, thermopair 4, heating resistor 5, water inlet 6, water delivering orifice 7, air intake opening 8, gas outlet 9, rubber plug 10, fixed spiro 11, top cover 12, chamber 13, upper grip 14, lower chuck 15
Fig. 2 multifunctional in-situ electro-chemical measuring apparatus vertical view
Embodiment
With reference to the accompanying drawings and in conjunction with example structure of the present invention and implementation result are done further explanation below.
Embodiment 1: the required multifunctional in-situ electro-chemical measuring apparatus of tension test is installed is carried out three-electrode system electrochemical test (feeding the simulation of specific gas environment in the solution)
1. the drawing machine of multifunctional in-situ electro-chemical measuring apparatus being packed into, its middle chamber 13 drops on the lower chuck 15.
2. the tensile sample 1 that will be welded with lead is sealed up for safekeeping with last lower chuck 14,15 usefulness 704 silica gel, reserves the area that numerical value is subscribed in test.
3. the top cover 12 of salt bridge 2, thermopair 4, rubber plug 10 being packed into, and metal platinum system auxiliary electrode 3 inserted in the rubber plugs 10.
4. the chamber 13 of rubber plug 10 being packed into, and tensile sample 1 passed rubber plug in chamber 13 and the top cover 12.Rotating cap 12 and chamber 13 closures,
5. the cavity bottom of heating resistor 5 being packed into is also tightened, and opens air intake opening 8 and inserts gas cylinder, adjusts the size of giving vent to anger of gas port 9
6. close water delivering orifice 7, open water inlet 6 and close water inlet 6 after with solution injecting chamber.
7. after contrast electrode being inserted in the salt bridge 2, with contrast electrode, tensile sample 1, the lead of metal platinum system auxiliary electrode 3 inserts electrochemical workstation, thermopair 4, the lead cut-in temperature control device of heating resistor 5
8. stretch behind the stress load of adjustment tensile sample.
Embodiment 2: the required multifunctional in-situ electro-chemical measuring apparatus of tension test is installed is carried out three-electrode system electrochemical test (simulation of dry wet alternating environment)
1. the drawing machine of multifunctional in-situ electro-chemical measuring apparatus being packed into, its middle chamber 13 drops on the lower chuck 15.
2. the tensile sample 1 that will be welded with lead is sealed up for safekeeping with last lower chuck 14,15 usefulness 704 silica gel, reserves the area that numerical value is subscribed in test.
3. the top cover 12 of salt bridge 2, thermopair 4, rubber plug 10 being packed into, and metal platinum system auxiliary electrode 3 inserted in the rubber plugs 10.
4. the chamber 13 of rubber plug 10 being packed into, and tensile sample 1 passed rubber plug in chamber 13 and the top cover 12.Rotating cap 12 and chamber 13 closures,
5. close air intake opening 8, the position of heating resistor 5 is screwed sealing with bolt.
6. open water inlet 6, adjust the aquifer yield size at the mouth of a river 7, guarantee that aquifer yield is much smaller than inflow.
7. the external water circulation system controls by water pump, guarantees to add unanimity interval time of water.
8. after contrast electrode being inserted in the salt bridge 2, with the lead access electrochemical workstation of contrast electrode, tensile sample 1, auxiliary electrode 3,
9. stretch behind the stress load of adjustment tensile sample.

Claims (2)

1. a tension test multifunctional in-situ electro-chemical measuring apparatus is characterized in that being made of electrochemical appliance, environment simulator and drawing machine three parts; Electrochemical appliance is made up of tensile sample (1), salt bridge (2) and auxiliary electrode (3); Environmental simulation system is made up of thermopair (4), heating resistor (5), water inlet (6), water delivering orifice (7), air intake opening (8), gas outlet (9), first, second, third rubber plug, fixed spiro (11), top cover (12), chamber (13): drawing machine comprises upper grip (14), lower chuck (15); Its middle chamber (13) drops on lower chuck (15); The tensile sample (1) that is welded with lead is sealed up for safekeeping with 704 silica gel with upper grip (14), lower chuck (15), reserved the area that numerical value is subscribed in test; With salt bridge (2), thermopair (4), first and second rubber plugs top cover (12) of packing into, and auxiliary electrode (3) inserted in second rubber plug; With the 3rd rubber plug chamber (13) of packing into, and tensile sample (1) passed the 3rd rubber plug and the first interior rubber plug of top cover (12) in the chamber (13); Rotating cap (12) and chamber (13) closure with pack into chamber (13) bottom and tightening of heating resistor (5), are opened air intake opening (8) and are inserted gas cylinder, adjust the size of giving vent to anger of gas port (9); Close water delivering orifice (7), open water inlet (6) and close water inlet (6) after with solution injecting chamber; After inserting contrast electrode in the salt bridge (2), with contrast electrode, tensile sample (1), the lead of auxiliary electrode (3) inserts electrochemical workstation, the lead cut-in temperature control device of thermopair (4), heating resistor (5); Stretch behind the stress load of adjustment tensile sample; On the stretching instrument, sample is carried out the measurement and the analysis of electrochemical parameter, realize dynamic online detection, obtain the partial data of laboratory sample electrochemical parameter under longer etching time, and in the measuring process of original three-electrode system, realize the simulation of multiple environmental factor, increased the integrality of data in tension test diversity and the test process.
2. a kind of tension test multifunctional in-situ electro-chemical measuring apparatus as claimed in claim 1 is characterized in that used auxiliary electrode is a platinum electrode, and contrast electrode is a mercurous chloride electrode.
CN200910076351XA 2009-01-14 2009-01-14 Multifunctional in-situ electro-chemical measuring apparatus for tensile test Expired - Fee Related CN101498648B (en)

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CN104458559B (en) * 2014-11-24 2017-12-19 辽宁石油化工大学 Stress electrochemical corrosion test device
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