CN104142293A - Electrochemical experiment device and method for surface thin liquid film of magnesium alloy - Google Patents
Electrochemical experiment device and method for surface thin liquid film of magnesium alloy Download PDFInfo
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Abstract
The invention discloses an electrochemical experiment device and method for a surface thin liquid film of magnesium alloy. The device comprises a base system, an electrolytic cell system and a measurement control system. With adoption of a lever adjusting device, an electrolytic cell bottom plate leveling bolt, a dial indicator adjusting bracket, a peristaltic pump and a series of other technical means, the conditions of thin liquid films of different thicknesses of below 100 microns are obtained; an inner insulated post cavity structure with a porous structure is formed inside the electrolytic cell, the influence of hydrogen, generated by magnesium alloy corrosion, on the thickness of the thin liquid film in a long-term soaking experiment can be avoided, and the thickness of the thin liquid film is kept uniform and stable, so that the real conditions of magnesium/magnesium alloy corrosion in a micro environment inside a human body are simulated. The device is simple in structure and simple and convenient to operate and can meet the experimental requirement on comprehensive research on an electrochemical behavior of magnesium alloy corrosion. The experimental method is simple, and the experimental result is real and accurate.
Description
Technical field
The present invention relates to a kind of surperficial thin liquid film electrochemical experimental device and experimental technique thereof, relate in particular to a kind of Mg alloy surface thin liquid film electrochemical experimental device and experimental technique thereof, belong to electrochemical field.
Background technology
Bio-medical material comprises the upper material of can implantable bioartificial body or can combine with biological tissue of medical treatment, is mainly used in original tissue and organ in treatment or replacement living organism, to revise, to compensate or to improve its function.
In pharmaceutical sanitary field, biodegradable medical material has obtained Devoting Major Efforts To Developing, is widely used in suture line in body tissue rebulding material, body, surgery with bonesetting material etc., has good application prospect.
Biomedical metallic material requires to have following performance, comprising: good histocompatbility, and nontoxicity, teratogenesis is not carcinogenic, does not cause allergic reaction and the immunity of interference body, does not destroy adjacent tissue etc.; Physicochemical property are stable, and intensity, elasticity, size, corrosion-resistant and wearing quality stable; Be easy to machine-shaping, can easily make the shape of various needs.
In the orthopaedics inner implantation material of clinical practice at present, stainless steel and titanium alloy become widely used material with good biocompatibility, corrosion resisting property and mechanical property.But it is poor with the mechanical compatibility of biological bone in the existing metal implant material such as stainless steel and titanium alloy, having a common problem.The tensile strength of stainless steel, titanium alloy etc. is higher more than 5 times than nature bone, and elastic modulus is high more than 10 times especially.After such material implant into body, can produce very large " stress shielding " effect to local bone tissue.Because the suffered stress stimulation of matrix bone declines, there is negative balance in bone remodeling, and causing bone to absorb increases, and bone forms and reduces, and brings out blocking property bone loss.Conventionally, embedded material and biological tissue's mechanical compatibility are poor medically can cause three kinds of serious consequences:
(1), embedded material original biological bone fragilityization around;
(2), embedded material area of new bone undergrowth around;
(3) interface, between embedded material and biological bone occurs that stress concentrates, thereby causes inflammation.
As can be seen here, can not there is too big-difference in the elastic modulus of embedded material and biological bone, and development mechanics and biocompatibility more preferably orthopedic implant material are the fundamental solutions that solves the existing problem of current embedded material.The implants such as while stainless steel, titanium alloy bone plate, nail need by operation taking-up again after bone tissue recovery from illness, have increased patient's misery and medical expense burden.In addition, the intravascular stent of at present clinical practice mainly be take stainless steel and Nitinol as main.These intravascular stents, except existing nickel ion stripping may cause toxic and side effect, cannot carry out the drawbacks such as vascular reconstructive surgery while also there is reangiostenosis and thrombus, vascellum endometrial hyperplasia, appearance accident.
The high medical material tough and that can degrade in vivo of research and development becomes the important development direction of above-mentioned field (orthopedic implant, endovascular stent).Magnesium is biomechanical property and the immediate metal material of human bone in current all metal materials.The elasticity of magnesium alloy is about 45GPa, more approaches the elastic modulus (20GPa) of people's bone than the biomaterial titanium alloy (100GPa) of current widespread use, can effectively reduce " stress-shielding effect ", promotes symphysis.Magnesium alloy has higher yield strength simultaneously, can bear larger load, is applied to bone tissue carrying position, also can be applied to endovascular stent, plays the effect of support blood vessels.Magnesium is one of nutrient important in human body, is in interior the 4th metallic element of human body, cell, to be only second to the kation of the 2nd of K+.
325 kinds of enzymes systems of its catalysis or activation body, participate in all energetic supersessions in body.Contraction of muscle, nervimotion function, physiological function and prevention circulation system disease and ischemic heart disease are played an important role.It is 280-300mg that World Health Organization's suggestion per day for adults need to be taken the photograph magnesium amount, and children are 250mg, infant 80mg.
The excretion of magnesium is mainly by urinary system, and magnesium absorbs the obvious rising that can not cause serum magnesium content in human body.Therefore, adopt magnesium alloy with high strength and ductility to there is good medical science security basis as medical degradable biomaterial, be particularly useful for orthopedic implant material and blood vessel inner bracket material.
Yet the corrosion resisting property of magnesium alloy is poor, in the corrosion environment that chlorion exists or when the pH of medium value is less than 11.5, its corrosion is especially serious.As biological implantation material, magnesium alloy must strictly meet necessary mechanics and morphology requirement in-service, so its corrosion degradation rate is unsuitable too fast.Human internal environment's normal ph is in 7.4 left and right, and in body fluid, has a large amount of chlorions, is a complicated corrosion environment in human body in addition, and these all can cause the corrosion rate of magnesium alloy in human body to change.The research that at present degradable medical is implanted magnesium alloy field mainly concentrates on the particularly strong alloy of plastic deformation ability of the good and mechanical property of exploitation corrosion stability, and these 2 be difficult to simultaneously satisfied.The magnesium alloy orthopaedics inner implantation material that enters at present clinical practice exists that intensity is low, the too fast problem of degrading; And as the magnesium alloy of angiocarpy bracket exist plastic deformation ability not, the too fast problem of degrading.In addition, the medical magnesium alloy of research all contains Al element mostly at present, and this element does not belong to the essential trace element of human body, is considered to have neurotoxicity, is the factor that causes alzheimer's disease, and the magnesium alloy tenability limit in human body that contains Al is only 1g/year.
Magnesium and magnesium alloy because of its good biocompatibility and osteoinductive be a kind of promising biomaterial.Can slow degradation after biological medical magnesium alloy implants, can avoid second operation to take out misery that implant brings and high expense.The major obstacle of magnesium alloy clinical practice is its low decay resistance, and this problem can reduce by alloying and process for treating surface the corrosion rate reenlistment of magnesium alloy at present.
But the bioassay standard of relevant Corrosion Behaviors of Magnesium Alloys speed does not also have unified standard at present both at home and abroad.Immersion test in simulated body fluid and have relatively large deviation between body results of animal; Electrochemical results is again because the distinctive negative difference effect of magnesium alloy makes the corrosion rate and the measured result deviation that calculate according to fitting result larger; In body zoopery, be faced with again experimental cost high, the test period is long, and result is not easy to the difficult problem quantizing.
Therefore, in-vitro simulatedly in body experiment, become important research direction of Corrosion Behaviors of Magnesium Alloys research field.
Under actual service condition, magnesium alloy is not to be immersed in body fluid, but forms a microenvironment with human connective tissue, capillary and bone tissue etc., and this microenvironment can be approximated to be a thin liquid film model.
Chinese patent application CN103293094A discloses a kind of simulation test device and using method thereof that can quantitatively change thin liquid film thickness, its simulation test device forms system by corrosive environment, and thickness of liquid film variation control system and electro-chemical test system three parts form.Corrosive environment formation system comprises etchant gas generator, atmosphere case, draft tube, escape pipe and recovery pond; Thickness of liquid film variation control system comprises leveling bolt, peristaltic pump, flexible pipe, numerical control device and signal wire; Electro-chemical test system is placed in atmosphere case, comprises electrolytic cell, sample stage, galvanochemistry sample, electrode cable, support.
Can quantitatively change the electro-chemical measuring apparatus of thickness of liquid film.On the basis of accurate, easy operating, realized the control at regular time and quantity to change procedure.Can carry out electrochemical in-situ polarization curve, ac impedance measurement.
It is said, technique scheme can be to the simulated experiment under different corrosive environment environment; Three-electrode system is packaged together, and can effectively reduce solution resistance, and can realize the electro-chemical test such as polarization curve, AC impedance under thin liquid.Adopt peristaltic pump and outside numerical control device to realize quantitative control to thickness of liquid film, can change thickness of liquid film with certain cycle, speed, realize the electrochemical research to change procedure.
Chinese patent application CN103267488A discloses a kind of device of test waves thickness of liquid film, and it utilizes laser can see through liquid and air but can not see through the principle of solid, generating laser and receiver is formed to loop, and connect reometer.By laser pickoff, change the power of the light signal receiving into current signal.Laser is first irradiated to solid sample, and reometer registration is 0; Move down the height of objective table, while having registration to reometer, on objective table, the scale of micrometer caliper is L1.Keep objective table height constant, generate drop, reometer registration becomes 0 again, moves down objective table height, and when reometer occurs registration again, on objective table, micrometer caliper scale is L2.Thin liquid film height is (L2-L1).
Technique scheme it is said can carry out the measurement of 10 μ m-999 μ m thin liquid film thickness, can be used for the electrochemical behavior of measuring metallic materials under thin liquid film.
But, the device of this test waves thickness of liquid film, on the one hand, installation composition and complex structure, equipment investment are larger; On the other hand, its scope of application, mainly for the relevant research of metal corrosion rate in atmosphere, is unsuitable for the modeling effort of Corrosion Behaviors of Magnesium Alloys speed under internal milieu.
Summary of the invention
One of object of the present invention is, provide a kind of simple structure, compact conformation reasonable, in experimental implementation process, adjustment operation is easy, and the Mg alloy surface thin liquid film electrochemical experimental device of the truth of magnesium/magnesium alloy corrosion under can analogue simulation inside of human body microenvironment.
The technical scheme that the present invention adopted is for achieving the above object that a kind of Mg alloy surface thin liquid film electrochemical experimental device, is characterized in that, comprises support system, electrolytic cell system and Measurement and Control System;
Described support system comprises rigid frame and sleeve; Described rigid frame integral body is the hexahedral shape that four sides is opened wide, sealed up and down all around, and its top board central part offers through hole, and the interior also part of described through hole is inserted through described top board in the bottom of described sleeve;
Described electrolytic cell system is arranged on the central authorities of the internal cavities of described rigid frame;
Described electrolytic cell system comprises electrolytic bath and working electrode;
Described working electrode is magnesium/magnesium alloy electrode;
On the arranged on left and right sides wall of described electrolytic bath, be respectively arranged with the feed liquor mouth of pipe and the fluid mouth of pipe, the position of the described fluid mouth of pipe is higher than the described feed liquor mouth of pipe;
The base plate center of described electrolytic bath inside is provided with a columniform sample stage, and the top of described sample stage is provided with a slot, and described working electrode inserts described slot;
Four drift angle places of base plate of described electrolytic bath outside are also respectively arranged with leveling bolt, and described leveling bolt is for adjusting the level of electrolytic bath;
Described Measurement and Control System comprises insulation cylinder;
Described insulation cylinder is right cylinder, and it is from up to down deep into the upper surface top of described sample stage through described sleeve;
Described insulation cylinder be take its center of circle, bottom surface and as the center of circle, is offered vertically blind hole; Described blind hole is covered by porous ceramic plate from inside to outside successively, then the hydrophobic membrane of being made by one deck teflon is coated seals, and forms an insulation cylinder internal cavities;
Before wrapping up by hydrophobic membrane, first with ear washing bulb, pump out the air in above-mentioned cavity, so that be negative pressure state in insulation cylinder internal cavities;
It is one circular to electrode that described sample stage top is set with;
In described electrolytic tank, be also provided with a contrast electrode, the bottom of described contrast electrode through the top board of described rigid frame, extend in electrolytic tank from top to bottom;
Described insulation cylinder is also provided with a ring groove at the place, top position of described sleeve;
The top of described insulation cylinder is also provided with a clock gauge, and the end of probe of described clock gauge is positioned at the top surface top of described insulation cylinder, and the adjusting support of described clock gauge is fixed on the top board of described rigid frame;
On described rigid frame top board, be also provided with one for regulating the lever adjusting device of described insulation cylinder in the vertical direction displacement;
Described lever adjusting device comprises left and right two screw rod pillars and an adjuster bar; Wherein, left screw rod pillar is fixed on the upper surface of described sleeve, right screw rod pillar is fixed on the top board of described rigid frame, on described adjuster bar, offer the first through hole and the second through hole, and be connected with described right screw rod pillar, left screw rod pillar respectively from right to left with the second through hole by described the first through hole, the end of described adjuster bar inserts described ring groove; On described left and right two screw rod pillars, be separately installed with the first setting nut and the second setting nut; The end that prizes of above-mentioned lever adjusting device is respectively left screw rod pillar and right screw rod pillar for the end of adjuster bar, two fulcrums from inside to outside.
The technique effect that technique scheme is directly brought is, whole device simple structure, compact conformation are reasonable, in experimental implementation process, can fully meet required adjusting requirement, and adjustment operation are very easy; Wherein, circularly to electrode, make distribution of current more even, effectively reduce the solution ohmmic drop that diffusion control is brought, can realize the electro-chemical test such as polarization curve, AC impedance and electrochemistry noise under thin liquid film condition;
Magnesium alloy working electrode is immersed in solution completely, avoids the interference of surface tension of liquid, maintains thin liquid film thickness stable time, also obtains the liquid film as thin as a wafer below 100 μ m.
As preferably, the above-mentioned feed liquor mouth of pipe is connected respectively a peristaltic pump that flow is adjustable with the fluid mouth of pipe, for controlling electrolytic bath electrolyte inside flow velocity.
The technique effect that this optimal technical scheme is directly brought is, by peristaltic pump, regulate and control flowing of simulated body fluid in electrolytic tank, can carry out very easily the state simulation under true body fluid environment in human body, and, by thin liquid film condition simulation internal milieu musculature, connective tissue, the impact of epithelial tissue on Corrosion Behaviors of Magnesium Alloys, further guarantee authenticity and the accuracy of experimental result more truly.
Further preferably, above-mentioned rigid frame material is organic glass; The base plate material of described electrolytic tank is glass.
The technique effect that this optimal technical scheme is directly brought is, the material of rigid frame and electrolytic tank base plate is transparent material, is convenient to carry out in experimentation omnibearing in good time observation.
Further preferably, the screw thread of above-mentioned left screw rod pillar and described the first setting nut is fine thread; The screw thread of described right screw rod pillar and described the second setting nut is coarse thread.
The technique effect that this optimal technical scheme is directly brought is, two fulcrums of left screw rod pillar and right these two leverages of screw rod pillar adopt respectively different pitch, in carrying out the operating process of insulation cylinder vertical direction up-down adjustment, adjusting cooperatively interacts, both convenient and swift, can guarantee obtained degree of regulation again.
Further preferably, above-mentioned circular to electrode, be pure platinum manufacture; Described insulation cylinder is made by teflon.
The technique effect that this optimal technical scheme is directly brought is, insulation cylinder 9 is made by teflon, mainly considers, the friction factor of teflon is extremely low, has the characteristic of good pre-good antiscale property.
Two of object of the present invention is that a kind of method of utilizing above-mentioned Mg alloy surface thin liquid film electrochemical experimental device to carry out simulated experiment in Corrosion Behaviors of Magnesium Alloys body is provided.
The technical scheme that the present invention adopted is for achieving the above object that a kind of experimental technique of Mg alloy surface thin liquid film electrochemical experimental device, is characterized in that, comprises the following steps:
The first step, respectively by magnesium alloy working electrode, circular electrode and contrast electrode be connected and put in place with electrochemical workstation outside device by wire respectively;
Second step injects the lower end that simulated body fluid to liquid level did not have insulation cylinder in electrolytic tank,, the leveling bolt on regulating electrolytic tank base plate, to electrolytic tank level;
Whole device is placed in CO2gas incubator, maintains the condition of 4% gas concentration lwevel at 37.5 ℃, the simulation human body liquid pH value stabilization in assurance electrolytic bath is in 7.4～7.6 left and right;
The peristaltic pump that startup is connected with effluent pipe mouth with water inlet pipe mouth respectively;
Adjustment (adjusting) lever regulating device, make hydrophobic membrane and circular to the spacing between electrode to required separation distance;
Regulate again the adjusting support of clock gauge until the end of probe of clock gauge holds out against the top surface at described insulation cylinder;
The 3rd step, reads the registration of milscale, starts electrochemical workstation and also by electrochemical workstation, detects polarization curve and electrochemical impedance spectroscopy;
The 4th step, adjustment (adjusting) lever regulating device, make hydrophobic membrane and circular to the spacing between electrode to another required separation distance, again read the registration of milscale, and again start electrochemical workstation and detect polarization curve and electrochemical impedance spectroscopy by electrochemical workstation;
The 5th step, repeats the 4th step, until finish.
The technique effect that technique scheme is directly brought is, by under thin liquid film environment, the impact of microenvironment on Corrosion Behaviors of Magnesium Alloys such as human connective tissue, capillary and bone tissue under simulated in vivo environment, body internal corrosion microenvironment is reduced to a kind of ideal conditions, a kind of new electrochemical test method that can qualitative and quantitative analysis Corrosion Behaviors of Magnesium Alloys speed is provided;
Above-mentioned experimental technique can original position carry out activation polarization, AC impedance or electrochemistry noise test to magnesium alloy sample, and obtains and in the experimental result of the comparatively identical external corrosion rate of magnesium alloy of body experimental result.
Be preferably above-mentioned hydrophobic membrane and the circular thickness that spacing between electrode is to Mg alloy surface thin liquid film; Above-mentioned simulated body fluid is Hank ' s solution.
The technique effect that this optimal technical scheme is directly brought is,
In sum, the present invention, with respect to prior art, has following beneficial effect:
1, whole device simple structure, compact conformation are reasonable, in experimental implementation process, can fully meet required adjusting requirement, and adjustment operation are very easy; By thin liquid film structure and regulate the flow velocity of electrolytic solution by peristaltic pump, inside of human body microenvironment is simulated in emulation in vitro, particularly simulated muscle tissue phantom, connective tissue and the epithelial tissue impact on Corrosion Behaviors of Magnesium Alloys behavior, has further guaranteed authenticity and the accuracy of experimental result;
2, magnesium alloy working electrode is immersed in solution and can avoids the impact of solution surface tension on thin liquid film thickness, produces thickness lower than the liquid film as thin as a wafer of 100 μ m;
3, at the insulation cylinder that is formed with porous structure of electrolytic cell inside, can avoid the impact on thin liquid film thickness of hydrogen that Corrosion Behaviors of Magnesium Alloys in long-time immersion test produces, guarantee thin liquid film thickness homogeneous, stable.
4, this device is applicable to a series of Electrochemical Measurement Technology such as open circuit potential, electrokinetic potential polarization curve, linear polarization curve, ac impedance spectroscopy and electrochemistry noise, can meet the requirement of experiment of the corrosion electrochemical action of comprehensive research magnesium alloy.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is under bulk solution and different thin liquid film thickness condition, the electrokinetic potential polarization curve of pure magnesium in Hank ' s simulated body fluid is (in figure, curve A is the polarization curve under bulk solution condition, curve B is the polarization curve under 200 μ m thin liquid film thickness condition, and curve C is the polarization curve under 70 μ m thin liquid film thickness condition);
Fig. 3 is under bulk solution and different thin liquid film thickness condition, the electrokinetic potential polarization curve of Mg alloy AZ91 D in Hank ' s simulated body fluid is (in figure, curve A is the polarization curve under bulk solution condition, curve B is the polarization curve under 200 μ m thin liquid film thickness condition, and curve C is the polarization curve under 1000 μ m thin liquid film thickness condition).
Description of reference numerals: 1 clock gauge, 2 adjustable supports, 3 sleeves, 4 contrast electrodes, 5 electrolytic baths, 6 circular to electrode, the 7 feed liquor mouths of pipe, 8 leveling bolts, 9 insulation cylinders, 10 left screw rod pillars, 11 adjuster bars, 12 right screw rod pillars, the 13 fluid mouths of pipe, 14 insulation cylinder internal cavities, 15 porous ceramic plates, 16 hydrophobic membrane, 17 thin liquid films, 18 working electrodes, 19 sample stages, 20 rigid frames.
Embodiment
Below in conjunction with drawings and Examples, to of the present invention, further illustrate.
As shown in Figure 1, Mg alloy surface thin liquid film electrochemical experimental device of the present invention, comprises support system, electrolytic cell system and Measurement and Control System;
Above-mentioned support system comprises rigid frame 20 and sleeve 3; Above-mentioned rigid frame 20 integral body are the hexahedral shape that four sides is opened wide, sealed up and down all around, and its top board central part offers through hole, and the interior also part of above-mentioned through hole is inserted through above-mentioned top board in the bottom of above-mentioned sleeve 3;
Electrolytic cell system is arranged on the central authorities of the internal cavities of above-mentioned rigid frame 20;
Above-mentioned electrolytic cell system comprises electrolytic bath 5 and working electrode 18; On the arranged on left and right sides wall of electrolytic bath 5, be respectively arranged with the feed liquor mouth of pipe 7 and the fluid mouth of pipe 13, the position of the above-mentioned fluid mouth of pipe 13 is higher than the feed liquor mouth of pipe 7;
Above-mentioned working electrode 18 is magnesium/magnesium alloy electrode, and described magnesium/magnesium alloy electrode is respectively skin and is enclosed with the magnesium/magnesium alloy right cylinder that the diameter of epoxy resin is 20mm;
The base plate center of above-mentioned electrolytic bath inside is provided with a columniform sample stage 19, and the top of sample stage 19 is provided with a slot, and working electrode 18 is arranged on described slot and goes out slot;
Four drift angle places of base plate of above-mentioned electrolytic bath outside are also respectively arranged with leveling bolt 8, and leveling bolt 8 is for adjusting the level of electrolytic bath;
Measurement and Control System comprises insulation cylinder 9;
Above-mentioned insulation cylinder 9 is right cylinder, and it is from up to down deep into the upper surface top of sample stage through above-mentioned sleeve 3;
Above-mentioned insulation cylinder 9 be take its center of circle, bottom surface and as the center of circle, is offered vertically blind hole; Blind hole is covered by porous ceramic plate 15 from inside to outside successively, more coated the sealing of hydrophobic membrane 16 of being made by one deck teflon, forms an insulation cylinder internal cavities 14;
Before wrapping up by hydrophobic membrane 16, first with ear washing bulb, pump out the air in above-mentioned cavity, so that be negative pressure state in insulation cylinder internal cavities 14;
It is one circular to electrode 6 that above-mentioned sample stage top is set with;
In above-mentioned electrolytic tank, be also provided with a contrast electrode 4, the bottom of contrast electrode 4 through the top board of rigid frame 20, extend in electrolytic tank from top to bottom;
Above-mentioned insulation cylinder 9 is also provided with a ring groove at the place, top position of sleeve 3;
The top of above-mentioned insulation cylinder 9 is also provided with a clock gauge 1, and the end of probe of clock gauge 1 is positioned at the top surface top of above-mentioned insulation cylinder 9, and the adjusting support 2 of clock gauge is fixed on the top board of rigid frame 20;
On above-mentioned rigid frame 20 top boards, be also provided with one for regulating the lever adjusting device of insulation cylinder 9 in the vertical direction displacements;
Above-mentioned lever adjusting device comprises left and right two screw rod pillars and an adjuster bar 11; Wherein, left screw rod pillar 10 is fixed on the upper surface of described sleeve, right screw rod pillar 12 is fixed on the top board of rigid frame 20, on adjuster bar 11, offer the first through hole and the second through hole, and be connected with described right screw rod pillar 12, left screw rod 10 pillars respectively from right to left with the second through hole by described the first through hole, the end of adjuster bar 10 inserts above-mentioned ring groove; On above-mentioned left and right two screw rod pillars, be separately installed with the first setting nut and the second setting nut; The end that prizes of above-mentioned lever adjusting device is respectively left screw rod pillar 10 and right screw rod pillar 12 for the end of adjuster bar, two fulcrums from inside to outside.
The above-mentioned feed liquor mouth of pipe 7 is connected respectively a peristaltic pump that flow is adjustable with the fluid mouth of pipe 13, for controlling electrolytic bath electrolyte inside flow velocity.
Above-mentioned rigid frame 20 materials are organic glass; The base plate material of electrolytic tank is glass.
The screw thread of above-mentioned left screw rod pillar and described the first setting nut is fine thread; The screw thread of right screw rod pillar and described the second setting nut is coarse thread.
Above-mentioned circular to electrode 6, be pure platinum manufacture; Insulation cylinder 9 is made by teflon.
The experimental technique of above-mentioned Mg alloy surface thin liquid film electrochemical experimental device, is characterized in that, comprises the following steps:
The first step, respectively by working electrode 18, circular electrode 6 and contrast electrode 4 be connected and put in place with electrochemical workstation outside device by wire respectively;
Second step injects the lower end that simulated body fluid to liquid level did not have insulation cylinder 9 in electrolytic tank, and the leveling bolt on regulating electrolytic tank base plate, to electrolytic tank level;
Whole device is placed in CO2gas incubator, maintains the condition of 4% gas concentration lwevel at 37.5 ℃, the simulation human body liquid pH value stabilization in assurance electrolytic bath is in 7.4～7.6 left and right;
Start respectively the peristaltic pump being connected with effluent pipe mouth 13 with water inlet pipe mouth 7;
Adjustment (adjusting) lever regulating device, make hydrophobic membrane 16 and circular to the spacing between electrode 6 to required separation distance;
Regulate again the adjusting support of clock gauge until the end of probe of clock gauge holds out against the top surface at described insulation cylinder 9;
The 3rd step, reads the registration of milscale 1, starts electrochemical workstation and also by electrochemical workstation, detects polarization curve and electrochemical impedance spectroscopy;
The 4th step, adjustment (adjusting) lever regulating device, make hydrophobic membrane 16 and circular to the spacing between electrode 6 to another required separation distance, again read the registration of milscale 1, and again start electrochemical workstation and detect polarization curve and electrochemical impedance spectroscopy by electrochemical workstation;
The 5th step, repeats the 4th step, until finish.
Preferably mode is, above-mentioned hydrophobic membrane 16 and the circular thickness that spacing between electrode 6 is to Mg alloy surface thin liquid film 17; Above-mentioned simulated body fluid is Hank ' s solution.
For understanding better the present invention, existing the present invention is described in detail in conjunction with the accompanying drawings and embodiments.Embodiment 1
Working electrode is magnesium electrode
Experimental technique:
After Mg alloy surface thin liquid film electrochemical experimental device is in place, pass through lever adjusting device, insulation cylinder is regulated down to working electrode and is contacted, by electrolytic tank adjusting bolt, progressively regulate until insulation cylinder lower surface contacts completely with working electrode again, regulate subsequently adjustable support that clock gauge is contacted with insulation cylinder, write down registration and be decided to be zero point.
By working electrode, contrast electrode with circular electrode is connected to electrochemical workstation, start electrochemical workstation respectively, start electro-chemical test.
Again by lever adjusting device, regulate the height and position of insulation cylinder, change the thickness (now the thickness of thin liquid film can read by clock gauge) of thin liquid film; And peristaltic pump is connected on the feed liquor mouth of pipe, the rotating speed by regulating peristaltic pump is with different parts in analogue body, different velocity of blood flow, and above-mentioned simulated body fluid flows out electrolytic bath through thin liquid film, the fluid mouth of pipe successively under the driving of peristaltic pump.
Band thickness of liquid film and velocity of flow adjust are complete, again start new electro-chemical test.
As shown in Figure 2, curve A is the polarization curve under bulk solution condition, and bulk solution ie in solution flows freely under condition, is equivalent to thin liquid film thickness for infinitely great, now the corrosion potential of magnesium is-1.544V (vs.SCE), and corrosion current density is 8.81 * 10
-6a/cm
2.
According to Faraday's law, can be by the corrosion current density i of polarization curve
corrbe converted to corrosion rate CR, formula is as follows:
In above formula, CR represents corrosion rate, and t represents soak time, and M is relative molecular mass, i
corrfor corrosion current density, n is valence state, and F is Faraday constant, and ρ is density.
The corrosion rate that calculates pure magnesium under bulk solution condition according to formula (1) is 12.06mm/;
Curve B is the polarization curve under 200 μ m thin liquid film thickness condition, and now the corrosion potential of magnesium is-1.52V (vs.SCE), and corrosion current density is 1.51 * 10
-6a/cm
2.
The corrosion rate that calculates pure magnesium under 200 μ m thin liquid film thickness condition according to formula (1) is 2.1mm/;
Curve C is the polarization curve under 70 μ m thin liquid film thickness condition, and now the corrosion potential of magnesium is-1.50V (vs.SCE), and corrosion current density is 1.22 * 10
-6a/cm
2.
The corrosion rate that calculates pure magnesium under 200 μ m thin liquid film thickness condition according to formula (1) is 1.68mm/.
Embodiment 2
Working electrode is Mg alloy AZ91 D electrode
Experimental technique is with embodiment 1.
As shown in Figure 3, curve A is the polarization curve under bulk solution condition, and now the corrosion potential of magnesium is-1.442V (vs.SCE), and corrosion current density is 2.39 * 10
-6a/cm
2.
The corrosion rate that calculates pure magnesium under bulk solution condition according to formula (1) is 3.3mm/;
Curve B is the polarization curve under 200 μ m thin liquid film thickness condition, and now the corrosion potential of magnesium is-1.456V (vs.SCE), and corrosion current density is 8.68 * 10
-7a/cm
2.
The corrosion rate that calculates pure magnesium under 200 μ m thin liquid film thickness condition according to formula (1) is 1.2mm/;
Curve C is the polarization curve under 100 μ m thin liquid film thickness condition, and now the corrosion potential of magnesium is-1.549V (vs.SCE), and corrosion current density is 5.90 * 10
-7a/cm
2.
The corrosion rate that calculates pure magnesium under 200 μ m thin liquid film thickness condition according to formula (1) is 0.78mm/.
Body animal, contrast experiment shows, in big white mouse body, the corrosion rate of Mg alloy AZ91 D is 0.7 ± 0.5mm/.
Show that external Electrochemical results that Mg alloy surface thin liquid film electrochemical experimental device of the present invention carries out is with substantially identical at body results of animal, experimental result is true, accurately.
Claims (7)
1. a Mg alloy surface thin liquid film electrochemical experimental device, is characterized in that, comprises support system, electrolytic cell system and Measurement and Control System;
Described support system comprises rigid frame and sleeve; Described rigid frame integral body is the hexahedral shape that four sides is opened wide, sealed up and down all around, and its top board central part offers through hole, and the interior also part of described through hole is inserted through described top board in the bottom of described sleeve;
Described electrolytic cell system is arranged on the central authorities of the internal cavities of described rigid frame;
Described electrolytic cell system comprises electrolytic bath and working electrode;
Described working electrode is magnesium/magnesium alloy electrode;
On the arranged on left and right sides wall of described electrolytic bath, be respectively arranged with the feed liquor mouth of pipe and the fluid mouth of pipe, the position of the described fluid mouth of pipe is higher than the described feed liquor mouth of pipe;
The base plate center of described electrolytic bath inside is provided with a columniform sample stage, and the top of described sample stage is provided with a slot, and described working electrode inserts described slot;
Four drift angle places of base plate of described electrolytic bath outside are also respectively arranged with leveling bolt, and described leveling bolt is for adjusting the level of electrolytic bath;
Described Measurement and Control System comprises insulation cylinder;
Described insulation cylinder is right cylinder, and it is from up to down deep into the upper surface top of described sample stage through described sleeve;
Described insulation cylinder be take its center of circle, bottom surface and as the center of circle, is offered vertically blind hole; Described blind hole is covered by porous ceramic plate from inside to outside successively, then the hydrophobic membrane of being made by one deck teflon is coated seals, and forms an insulation cylinder internal cavities;
Before wrapping up by hydrophobic membrane, first with ear washing bulb, pump out the air in above-mentioned cavity, so that be negative pressure state in insulation cylinder internal cavities;
It is one circular to electrode that described sample stage top is set with;
In described electrolytic tank, be also provided with a contrast electrode, the bottom of described contrast electrode through the top board of described rigid frame, extend in electrolytic tank from top to bottom;
Described insulation cylinder is also provided with a ring groove at the place, top position of described sleeve;
The top of described insulation cylinder is also provided with a clock gauge, and the end of probe of described clock gauge is positioned at the top surface top of described insulation cylinder, and the adjusting support of described clock gauge is fixed on the top board of described rigid frame;
On described rigid frame top board, be also provided with one for regulating the lever adjusting device of described insulation cylinder in the vertical direction displacement;
Described lever adjusting device comprises left and right two screw rod pillars and an adjuster bar; Wherein, left screw rod pillar is fixed on the upper surface of described sleeve, right screw rod pillar is fixed on the top board of described rigid frame, on described adjuster bar, offer the first through hole and the second through hole, and be connected with described right screw rod pillar, left screw rod pillar respectively from right to left with the second through hole by described the first through hole, the end of described adjuster bar inserts described ring groove; On described left and right two screw rod pillars, be separately installed with the first setting nut and the second setting nut; The end that prizes of above-mentioned lever adjusting device is respectively left screw rod pillar and right screw rod pillar for the end of adjuster bar, two fulcrums from inside to outside.
2. Mg alloy surface thin liquid film electrochemical experimental device according to claim 1, is characterized in that, the described feed liquor mouth of pipe is connected respectively a peristaltic pump that flow is adjustable with the fluid mouth of pipe, for controlling electrolytic bath electrolyte inside flow velocity.
3. Mg alloy surface thin liquid film electrochemical experimental device according to claim 1, is characterized in that, described rigid frame material is organic glass;
The base plate material of described electrolytic tank is glass.
4. Mg alloy surface thin liquid film electrochemical experimental device according to claim 1, is characterized in that, the screw thread of described left screw rod pillar and described the first setting nut is fine thread;
The screw thread of described right screw rod pillar and described the second setting nut is coarse thread.
5. Mg alloy surface thin liquid film electrochemical experimental device according to claim 1, is characterized in that, described circular to electrode, be pure platinum manufacture;
Described insulation cylinder is made by teflon.
6. the experimental technique of Mg alloy surface thin liquid film electrochemical experimental device as claimed in claim 1, is characterized in that, comprises the following steps:
The first step, respectively by magnesium alloy working electrode, circular electrode and contrast electrode be connected and put in place with electrochemical workstation outside device by wire respectively;
Second step injects the lower end that simulated body fluid to liquid level did not have insulation cylinder in electrolytic tank,, the leveling bolt on regulating electrolytic tank base plate, to electrolytic tank level;
Whole device is placed in CO2gas incubator, maintains the condition of 4% gas concentration lwevel at 37.5 ℃, the simulation human body liquid pH value stabilization in assurance electrolytic bath is in 7.4～7.6 left and right;
The peristaltic pump that startup is connected with effluent pipe mouth with water inlet pipe mouth respectively;
Adjustment (adjusting) lever regulating device, make hydrophobic membrane and circular to the spacing between electrode to required separation distance;
Regulate again the adjusting support of clock gauge until the end of probe of clock gauge holds out against the top surface at described insulation cylinder 9;
The 3rd step, reads the registration of milscale, and detects polarization curve and electrochemical impedance spectroscopy by electrochemical workstation;
The 4th step, adjustment (adjusting) lever regulating device, make hydrophobic membrane 16 and circular to the spacing between electrode 6 to another required separation distance, again read the registration of milscale, and again by electrochemical workstation, detect polarization curve and electrochemical impedance spectroscopy;
The 5th step, repeats the 4th step, until finish.
7. according to the experimental technique of the Mg alloy surface thin liquid film electrochemical experimental device described in claim, it is characterized in that described hydrophobic membrane and the circular thickness that spacing between electrode is to Mg alloy surface thin liquid film; Described simulated body fluid is Hank ' s solution.
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