Derivation of Parametric Tropical Cyclone Models for Storm Surge Modeling

专利名称：四唑取代的芳基酰胺类
专利类型：发明专利
发明人：L·陈,L·冯,R·C·海利,M·杨,M·P·狄龙申请号：CN200780024141.5
申请日：20070618
公开号：CN101479250A
公开日：
20090708
专利内容由知识产权出版社提供
摘要：式(I)的化合物或其可药用盐，其中R是任选取代的四唑基，R是任选取代的苯基、任选取代的吡啶基或任选取代的噻吩基，且R、R、R和R如本文所定义。

还提供了用这些化合物治疗由P2X和/或P2X受体拮抗剂介导的疾病的方法，以及制备这些化合物的方法。

申请人：弗·哈夫曼-拉罗切有限公司
地址：瑞士巴塞尔
国籍：CH
代理机构：北京市中咨律师事务所
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Wear252(2002)744–754A tribo-electrochemical apparatus for in vitro investigation offretting–corrosion of metallic implant materialsS.Barril,N.Debaud,S.Mischler∗,ndoltLaboratory of Metallurgical Chemistry,Materials Department,Swiss Federal Institute of Technology of Lausanne,EPFL,CH-1015Lausanne,Switzerland Received4October2001;received in revised form22January2002;accepted22January2002AbstractA novel apparatus has been developed for the investigation of fretting–corrosion behaviour of metallic materials used in prosthetic implants.Well-defined micro-movements are achieved through a rigid overall structure and the precise alignment of the components.An electrochemical cell is used for controlling the surface chemistry of the metal in contact and for studying the role of anodic oxidation.During an experiment,the most relevant mechanical and electrochemical parameters are continuously monitored using a computer-based data acquisition system.The apparatus permits,thus,in vitro experiments under well-controlled mechanical and electrochemical conditions. The good time resolution and reproducibility of the measurements permit the observation of correlations between different mechanical and electrochemical quantities.Preliminary results show that the prevailing corrosion conditions critically affect the overall fretting behaviour of Ti6Al4V.©2002Elsevier Science B.V.All rights reserved.Keywords:Fretting–corrosion;Tribo-electrochemical apparatus;Titanium alloy1.IntroductionTissues inflammation caused by degradation of metallic materials used in prosthetic implants can lead to failure of orthopaedic surgical operations.The materials degradation is a consequence of mechanical stresses resulting in small relative displacements(fretting)between prosthesis and sur-rounding bone tissues.The corrosive nature of the physiolog-ical environment exacerbates material degradation leading to fretting–corrosion[1],a situation where materials are exposed to the combined attack by corrosion and fretting. Under such conditions,micro and nanometer size wear par-ticles are formed[2,3]and metallic ions may be released into the body.These wear particles can stimulate cell reactions [4]which lead to tissue inflammation,a phenomenon that affects bone regeneration[5]and the stability of the implant. The release of metallic ions likely provokes allergies,when their concentration exceeds critical values.A better insight into the fretting–corrosion behaviour of metals in biological environments is a prerequisite for the control of biological compatibility of metallic implants.Fretting–corrosion results in metal degradation due to the simultaneous action of mechanical wear and of(electro) chemical oxidation[6].The two mechanisms do not proceed ∗Corresponding author.Tel.:+41-21-693-2954;fax:+41-21-693-3946. E-mail address:stefano.mischler@epfl.ch(S.Mischler).separately,but depend on each other in a complex way.In many cases,corrosion is accelerated by wear and,similarly wear may be affected by corrosion phenomena.Many fac-tors determine the interaction between wear and corrosion. For example,mechanical abrasion of the passivefilm usually leads to wear accelerated corrosion due to high chemical re-activity of the bare metal surface exposed to the environment [7–9].On the other hand,passivefilms seem to decisively influence the surface mechanical response of metals as well as the third-body behaviour[10,11].For the experimental investigation of tribo-corrosion,it is,therefore,essential to control both mechanical and chemical parameters.The control of displacement is particularly important in fretting because displacement accommodation by elastic deformation becomes relevant in case of small amplitude motion.According to the classical analysis[12],by super-posing a tangential force to a ball onflat Hertzian contact, some slip occurs on the outer annular part of the contact area while the centre remains locked(non-slip area).In such partial slip conditions,material damage seems to oc-cur only within the slip area,which becomes larger with increasing displacement.When the imposed displacement exceeds a critical value,slip becomes total and the situation approaches sliding friction.The prevailing slip regime(par-tial or total)must be identified in order to correlate fretting behaviour with mechanical,material and other relevant fac-tors.The control of corrosion conditions is best achieved by0043-1648/02/$–see front matter©2002Elsevier Science B.V.All rights reserved. PII:S0043-1648(02)00027-3S.Barril et al./Wear252(2002)744–754745the application,by means of an external source,of a defined potential,measured with respect to a reference electrode. The applied potential determines the reactivity of the metal as well as the presence or not of a passive oxidefilm at the surface and its thickness and composition.In addition, electrochemical techniques allow one to determine in-situ and in real time the rate of electrochemical oxidation during fretting by measuring an electrical current.Of particular importance is the capability of monitoring in real time the relevant mechanical,electrochemical and physical param-eters such as frictional force,normal force,displacement, linear wear,current and temperature in order to follow their evolution during an experiment and to observe correlations between them.This paper describes a novel apparatus developed for the investigation of fretting–corrosion mechanisms of metallic implant materials,which largely fulfils the above require-ments.It includes well-defined displacements,electrochemi-cal control and an advanced computer-based data acquisition system which permits monitoring of critical parameters with good time resolution.The limits and possibilities of the ap-paratus are evaluated by investigating a ball(alumina)on flat(Ti alloy)contact immersed in0.9wt.%NaCl,used asa simple model for bodyfluid.2.Description of the apparatusA rigid square frame made of stainless steel constitutes the main structure of the experimental apparatus(Fig.1). The apparatus is placed on an optical table equipped with pneumatic damping pistons to avoid perturbation by exter-nal vibrations.The calculated frame stiffness in the hori-zontal direction corresponds to109N m−1[13].Two linear roller bearings arefixed on the inside face of the vertical parts of the frame in order to allow for the vertical motion of a horizontal beam.The beam is slightly oversized in or-der to apply an elastic compression of the linear bearings when mounted.This ensures a smooth vertical displacement of the beam as well as its horizontal alignment.A ball screw isfixed on the lower part of the square frame to control the vertical movement of the beam.An elastic bearing(Fig.2) was designed to ensure a well-controlled horizontal motion while minimising any vertical displacement.It consists in two parallel plates connected byfive shafts on each side.The lower plate isfixed on the mobile beam while the upper part supports the lower specimen holder.Motion of the upper plate of the elastic bearing is controlled by a piezo-actuator, whose other extremity isfixed onto the mobile beam.The actuator is equipped with a position sensor and a loop in its electronic controlling system permits to impose well-defined effective displacements.The difference between the com-mand value of the piezo-actuator and the effective displace-ment of the elastic bearing centre was found being<2%up to a slip amplitude of180␮m.Fig.1.Schematic view of the fretting apparatus.The mobile beam sup-porting the elastic bearing is visible in the centre of the structure with the piezo-actuatorfixed on its left side:(1)main structure;(2)elastic bear-ing;(3)mobile beam;(4)screw to move the mobile beam up or down;(5)piezo-actuator;(6)force sensor(hatched part);(7)specimens.The upper specimen holder isfixed on the pre-load piece of a piezo-electric force transducer mounted at the end of a shaft connected to the upper part of the frame by two horizontal spring blades(Fig.3).The two blades maintain the shaft in a vertical position and ensure a high rigid-ity in the horizontal plane and a high compliance in the z-axis(vertical axis).The compliance in the z-axisallows Fig.2.Three-dimensional drawing of the elastic bearing.The upper plate supports the sample holder and the lower plate isfixed onto the mobile beam.746S.Barril et al./Wear 252(2002)744–754Fig.3.Schematic view showing the system used for application of the normal force and for control of the contact stiffness.The upper sample is mounted on a shaft connected to the main frame by two spring blades.The shaft is loaded against the lower specimen (not shown)by compressing an interchangeable spring.the vertical displacement of the upper specimen to follow geometrical changes induced by wear during experiments.The pre-loaded quartz force sensor measures the normal force applied along the z -axis and the tangential force along the x -axis (motion direction).Conversion constants given by manufacturer and used in the pre-amplifiers for normal and tangential force acquisition have been verified.After putting in contact the two specimens by moving up the mo-bile beam,the desired normal force is imposed via an inter-changeable spring pressed against the end of the shaft by a rotating screw fixed on the frame.In this configuration,the stiffness of the contact is controlled by the rigidity of the spring.Interchangeable springs permit one to carry out ex-periments at different contact stiffness [14].In the present experiments,the rigidity of the spring was of 9.81N mm −1although higher values can be used.A laser distance me-ter (Keyence LC2420)fixed on the optical table measures the vertical displacement of the shaft with a resolution of 0.01␮m.The vertical displacement during fretting corre-sponds in principle to the linear wear.The specimen holders have truncated cone geometry with the part facing the contact finished by grinding in order to obtain a flat surface and a conform contact with the elastic bearing plane.The specimens,either balls or cylinders,are inserted in the upper part of the holder.For systems involving flat contact surfaces,the specimen surface is ground after being inserted to ensure parallelism between contact surface and the bottom surface of the holder.The upper specimen holder has the same geometry as the lower specimen holder but is mounted upside down.Although flat on flat or cylinder on cylinder contacts are possible,in the present experiments only the ball on plate configuration was used.The holders are fixed either on the elastic bearing (lower specimen)or onthe pre-load piece of the force transducer (upper specimen)by means of screwed POM collars.A PMMA liquid cell is fixed around the specimen holder in order to carry out experiments in aqueous media as shown in Fig.4(for sake of clarity this cell has been left out in Fig.1).A three-electrode set-up was implemented with the metallic specimen as working electrode.A counter electrode (made of a platinum wire)as well as areferenceFig.4.The electrochemical cell for tribo-electrochemical measurements.The cell is fixed on the sample holder,which is in turn fixed on the elastic bearing.An alumina disc is used to electrically insulate the lower sample holder from the main frame.S.Barril et al./Wear252(2002)744–754747electrode are connected to a Wenking LB95L potentiostat. The temperature of the test solution is controlled by means of heatingfluid circulating through a circular glass tube fitted in the electrochemical cell.A thermostat controls the temperature of thefluid.A thermocouple is used to mea-sure the solution temperature close(1mm distance)to the specimen.During the test,the normal force,the frictional force,the horizontal position of the elastic bearing,the linear wear and the electrochemical parameters current and potential are con-tinuously monitored using a Macintosh computer running under Labview software.Each parameter is acquired at a sampling rate of1000points per second.In parallel,every second,the mean value is calculated.Both mean values and instantaneous values are stored at regular intervals of1and 60s,respectively.The coefficient of friction is determined during each stroke by dividing the frictional force by the normal force measured in the centre of the oscillation path.3.Experimental method for studying fretting–corrosion of Ti6Al4V against aluminaFretting between an alumina ball(upper specimen)and a Ti6Al4V,plate(lower specimen)was investigated in order to demonstrate the possibilities of the apparatus and explore its range of application.Ti6Al4V was chosen because it is widely used in orthopaedic devices.Al2O3was chosen as sliding partner because of its chemical inertness and high hardness.Thus,Al2O3is expected to suffer negligible degra-dation when fretting against Ti6Al4V.The Ti6Al4V spec-imens were of cylindrical shape(4mm in radius)and the alumina counter piece of spherical shape(5mm in radius). The Ti6Al4V alloy(Siber and Hegner,Switzerland)of hard-ness323HV5[7]was supplied in form of hot rolled,an-nealed and ground bars of10mm diameter.The as received Ti6Al4V bars were cut in smaller parts of8mm in diame-ter and approximately16mm height.After insertion in the holder,the exposedflat surface of the cylinder was ground down to a R a value of0.6␮m according to a well-defined and controlled procedure.The reproducibility of results among different specimens was found to be critically affected by small deviations in the grinding procedure.Sliding direction was always perpendicular to the grinding grooves.The alu-mina balls were supplied by Saphirwerke AG with a surface finish of grade G10according to AFBMA standard(R q< 0.02␮m).An aerated NaCl solution of0.9wt.%(0.15M)was used in the present preliminary experiments,although more com-plex solutions containing other salts and organic compounds exist for simulating the physiologicalfluid in the human body[15].All experiments were performed at room temper-ature(21±1◦C)to avoid problems related to achieving ther-mal stabilisation of the apparatus when heating the solution.A few experiments carried out at37◦C did not reveal ma-jors differences in fretting–corrosion behaviour compared to room temperature experiments.A saturated Ag/AgCl refer-ence electrode(standard potential of+0.222V versus SHE) was used and,in the present paper,all potentials are given with respect to this reference electrode.Unless otherwise indicated,all experiments were carried out at an applied po-tential of0.5V corresponding to the passive state of the ti-tanium alloy.The applied load was10N(maximum contact pressure of860MPa according to Hertz)and the oscillation frequency was1Hz.After fretting–corrosion experiments,laser profilometry (UBM instrument)was used to measure the volume of re-moved metal.Surface scans were performed,on square areas of typically1.7mm×1.7mm.Resolution was1000points per mm in x-direction and80lines scans per mm in the y-direction.Afterwards,the wear volume was determined using an UBM software routine by measuring the air vol-ume below the reference plane defined by the surface outside the contact.The topography of the wear traces was charac-terised using a Philips XL30scanning electron microscope or a Leitz optical microscope.4.Results4.1.Time dependence and reproducibility of measured mechanical and electrical quantitiesFig.5shows a typical set of mean values for an exper-iment performed at a displacement amplitude of150␮m, 1Hz oscillation frequency,a normal force of10N,and under an applied potential of+0.5V.A spring of rigidity 9.81N mm−1was used to apply the normal load.Rubbing starts at200s and stops at900s.The initial coefficient of friction is close to0.4(Fig.5a).After a running in period of approximately100s,the coefficient of friction displays a plateau at a value close to0.6characterised by somefluc-tuations ranging from0.45to0.65.The current markedly increases as soon as fretting starts(Fig.5b).This confirms that rubbing interferes with passivity and leads to anodic metal oxidation.After few seconds of rubbing,the position of the contact(Fig.5c)rises indicating material build-up in the contact.Afterwards,the descent of the contact indicates progressive material removal from the contact(wear). Fluctuation observed for all three quantities during rub-bing are of particular interest.Indeed,the data demonstrate a close correlation between the current peaks,the friction coefficient variations and the linear wear rate.A sudden decrease in friction coefficient corresponds to an increase in current and a rise in the position of the contact.Thesefluc-tuations are attributed to the formation of wear particles and to their ejection from the contact[16].A detailed mechanis-tic interpretation of the results lies beyond the scope of the present paper,however.The results of Fig.5clearly demon-strate that the described apparatus is able to detect time dependent variations and,thus,permits one tofind correla-tions between different mechanical and electrical quantities.748S.Barril et al./Wear 252(2002)744–754Fig.5.Evolution of the (a)coefficient of friction,(b)current and (c)vertical position of the contact during a fretting experiment.Test conditions:NaCl 0.9wt.%solution;displacement amplitude 150␮m;rubbing time 600s;oscillation frequency 1Hz;load 10N;spring rigidity 9.81N mm −1;applied potential 0.5V/Ag/AgCl.Rubbing starts at 300s.Small variations in the specimen surface preparation by grinding were found to have a deleterious influence on the reproducibility.This confirms the relevant role played by surface finish on fretting.In the present study,good repro-ducibility was achieved by strictly following a pre-defined grinding protocol for the preparation of the Ti 6Al 4V spec-imens.To demonstrate the reproducibility achieved under the present experimental conditions,four identical exper-iments were carried out using virgin Ti 6Al 4V and Al 2O 3specimens.Slip amplitude was 150␮m,duration of rub-bing was 600s,the oscillation frequency was 1Hz and the normal force was 10N.A potential of +0.5V was applied to the Ti 6Al 4V specimen immersed in the NaCl solution.Fig.6shows the evolution of the coefficient of friction for the four experiments.Rubbing starts at approximately 300s and stops at 900s .At the onset of rubbing the co-efficient of friction is close to 0.4,then it increases during a run in period of approximately 100s.The time evolu-tion of the coefficient of friction during this period shows good reproducibility.Interestingly,a temporary decrease of the coefficient of friction (approximately between 400and 500s)is observed in all experiments at the beginning of the plateau corresponding to the steady-state value of about 0.6.The behaviour indicates that a systematic event related toS.Barril et al./Wear 252(2002)744–754749Fig.6.Evolution of the coefficient of friction with time measured in four independent tests.Test conditions as in Fig.5.Fig.8.Fretting log diagrams for experiments carried out at displacement amplitudes of (a)3␮m;(b)10␮m;(c)30␮m,respectively.Test conditions:NaCl 0.9wt.%solution;rubbing time 3600s;scillation frequency 1Hz;load 10N;spring rigidity 9.81N mm −1;applied potential 0.5V/Ag/AgCl.Fig.7.Evolution of the current with time measured in four independent tests.Test conditions as in Fig.5.750S.Barril et al./Wear 252(2002)744–754the build-up and accommodation of third-body particles oc-curs after accommodation of the two surfaces.Discontinuous ejection of third-body particles leads to continuing fluctua-tions in the plateau region.When rubbing stops the friction coefficient does not instantaneously decrease to zero,as one would expect.The behaviour is attributed to an artefact cre-ated by the signal discharge in the force sensor preamplifier with respect to the time constant imputed in the settings.For the same series of experiments,Fig.7displays the measured anodic currents versus time.Immediately after rubbing starts,the current sharply increases to a maximum and then slowly stabilises towards a lower plateau value.The current increase arises from the metal oxidation follow-ing fretting enhanced de-passivation.The current stabilisa-tion suggests that,after the run in period,the removal rate of the passive layer decreases,possibly due to the formation of protective third-body.The current plateau exhibits sev-eral spikes.A major peak is always observed at the begin-ning of the plateau,approximately between 400and 500s.The time evolution of the current shows reproducible sim-ilarities with the coefficient of friction.The initial current peak corresponds well with the run in period for friction.Furthermore,the secondary current peaks observed attheFig.9.SEM images of the Ti 6Al 4V alloy after fretting experiment performed in NaCl 0.9wt.%at two different applied potentials (−1V Ag/AgCl (a,b)and 0.5V Ag/AgCl (c,d)).Test conditions:NaCl 0.9wt.%solution;displacement amplitude 50␮m;rubbing time 3600s;oscillation frequency 1Hz;load 10N;spring rigidity 9.81N mm −1.beginning of the plateau correspond well with minima of the coefficient of friction.4.2.Effect of fretting regime on electrochemical oxidation Acquisition of transient values permits one to anal-yse data in terms of so called “friction logs”[17],i.e.three-dimensional graphical representation of the time evo-lution of the frictional force-displacement loops (Fig.8).Such diagrams are shown in Fig.8for tests carried out under identical conditions as previously mentioned but at displacement amplitudes of 3,10and 30␮m and duration is 3600s.In Fig.8,one can easily identify the dominating fretting regimes [12,18].For example,Fig.8a exhibits a closed loop representative of a stick regime,where elastic deformation of the device and of the contact accommo-dates the entire imposed displacement.Fig.8c shows a rectangular loop where both elastic deformation and slip contribute to displacement (gross slip regime).Note that the real displacement (approximately 20␮m)is smaller than the imposed one (30␮m).Fig.8b shows an intermediate situation where elastic accommodation prevails over slip (partial slip regime).S.Barril et al./Wear252(2002)744–754751 The fretting regime has a marked effect on the mate-rial loss by electrochemical oxidation.Under slip or partialslip conditions periodic passivefilm removal followed byre-passivation of the metal surface leads to metal loss ac-cording to the anodic reaction:Ti+2H2O→TiO2+4H++4e−The metal volume V anod oxidised during a given timecan be determined from the measured anodic current usingFaraday’s law:V anod=(I rubbing t rubbing)MnFρin this equation,t rubbing is the rubbing time,I rubbing the current measured due to rubbing,F the Faraday constant (96500C mol−1),M the atomic weight,ρthe molar density of Ti and n=4the number of electron transferred dur-ing oxidation.I rubbing is determined here by averaging the current measured during rubbing and subtracting the mean value of the current measured just before and just after rub-bing.In this way,it is possible to compensate for the part of the current that does not depend on rubbing.The calcula-tion implies that titanium oxidation to the four valent state is the only anodic reaction.More complex calculations could take into account the minor alloy elements present but for the purposes of the present study this is not needed.The anodic volumes,V anod,listed in Table1together with the overall wear values,V tot,were determined for experiments carried out at different displacements under otherwise iden-tical conditions at an applied potential0.5V.The very small volumes involved and difficulties in the assessment of the reference plane of the unworn surface, render imprecise the determination of the overall wear vol-ume by profilometry.The poor reproducibility of the V tot values listed in Table1reflects this imprecision.The anodic volumes show much less scattering because the current can be measured with good sensitivity.The data of Table1show that the overall wear and the anodic volume depend differ-ently on displacement amplitude.In the stick regime,wear is detectable but no significant current due to electrochemical Table1Chemical and mechanical wear volumes at different slip amplitude(3600s, 1Hz,10N,9.81N mm−1,room temperature,+0.5V/Ag/AgCl)Amplitude (␮m)DisplacementaccommodationV tot(10−3mm3)V anod(10−3mm3)V anod/V tot(%)3Elastic0.02700 30.01900 10Partial slip0.01600 100.01500 30Gross slip0.0730.0079 300.0380.00925 50Gross slip0.1560.06541 500.1270.06954 100Gross slip0.3740.22760 1000.2820.19970oxidation is measured.This suggests that elastic deforma-tion does not lead to passivefilm removal.Electrochemical oxidation becomes significant only when gross slip occurs and becomes dominant at higher amplitudes as indicated by the V anod/V tot ratios listed in the table.4.3.Effect of applied potential on fretting behaviour Experiments were carried out under identical conditions but at two distinct applied potentials of−1.0and+0.5V. From a thermodynamic point of view in neutral solution titanium oxide,TiO2,is the stable species[19].However,the thickness of the passive oxidefilm is likely to be different, since,it depends on the applied potential[20,21].For the present alloy thefilm composition could also slightly change with potential[21].The wear morphology and the wear rate were found to vary considerably with the applied potential.At−1V (Fig.9a and b),the wear trace on the alloy is elliptical with a width of approximately140␮m and a length of180␮m. Some wear particles accumulate at the end of the wearscar Fig.10.Cross-section profiles of wear traces formed on the Ti6Al4V specimen after rubbing at(a)−1V Ag/AgCl and(b)0.5V Ag/AgCl.Test conditions as in Fig.9.752S.Barril et al./Wear 252(2002)744–754Fig.11.Fretting log representations for experiments performed in NaCl 0.9wt.%at (a)−1V Ag/AgCl and (b)0.5V Ag/AgCl.Test conditions as in Fig.9.(Fig.9),while the wear scar itself is covered with smeared material.The profilometer trace measured across the contact area (Fig.10)does not show evidence of material removal,but indicates some decrease of the roughness within the contact.According to Hertz contact theory,the contact area diameter is 148␮m (maximum pressure of 860MPa).The Hertz contact diameter corresponds well with the width of the fretting trace.Further,as shown by the friction logs (Fig.11),the slip distance is approximately 26␮m.Thesum Fig.12.Optical microscope images of the alumina balls after fretting against Ti 6Al 4V at (a)−1V Ag/AgCl and (b)0.5V Ag/AgCl.Test conditions as in Fig.9.of the elastic area diameter and the slip amplitude corre-sponds to the contact distance,i.e.the theoretical length of the fretted trace.In the present situation,one obtains a value of 174␮m,which corresponds well with the trace length observed in the SEM images as well as in the profilometer trace.At an applied potential of +0.5V ,the fretting scar is larger (Fig.9c)and exhibits different features in the cen-tre with respect to the edges,the latter being covered byS.Barril et al./Wear252(2002)744–754753smeared material(Fig.9d).The dimensions of the scar are approximately280␮m(width)by350␮m(length).Because significant metal removal has taken place,as evidenced by the profilometer trace(Fig.10),these dimensions rather re-late to the ball geometry than to the Hertzian contact area. Indeed,optical microscope observations(Fig.12)reveal thatflattening by wear of the alumina sphere in the con-tact area occurred.The diameter of theflattened area was larger at0.5V(300␮m)compared to the lower potential (170␮m).Alumina wear,therefore,depends on the elec-trochemical conditions prevailing in the contact.A similar potential dependence of alumina wear was previously ob-served during rubbing against various metals under sliding wear conditions[7].The information provided by fretting-log diagrams (Fig.11)is of particular interest.In fact,the slope of the loop is more pronounced at the negative potential than at0.5V.The slip amplitude varies consequently from 26to36␮m at−1.0and0.5V,respectively.The coeffi-cient of friction is higher at lower potential(0.62V)than at higher(0.45V)potential.These results show that the prevailing electrochemical conditions interfere not only with friction but with the elastic behaviour of the con-tact as well.To what extent third-body particles are in-volved in the different behaviour can not be judged at present.5.DiscussionThe present apparatus was developed to investigate fretting–corrosion mechanisms relevant for biomedical im-plants.The results obtained demonstrate the usefulness of the device and of the data acquisition system for such stud-ies,and they provide evidence for the complexity of the phe-nomena involved in fretting–corrosion.Fretting–corrosion experiments performed under electrochemical control with a Ti6Al4V/Al2O3contact revealed clear correlations be-tween mechanical and electrochemical quantities.In partic-ular,the close correlation between currentfluctuations and linear displacement illustrated in Fig.5indicates that the electrochemical activity depends to a large extent on the third-body behaviour in the contact.In fact,current peaks are always associated with simultaneous peaks in position of the contact.The latter are due to material accumulation in the contact causing the counter piece to move up.Thus, current peaks are associated with third-body accumula-tion in the contact.This suggests that third-body particle formation(probably by fatigue wear)is associated with a local de-passivation of the metal which dissolves and re-passivates at high instantaneous current density.In addi-tion,dissolution and passivation of freshly formed particles may also contribute to the current peaks.Periodically the oxidised third-body particles are ejected from the contact leading to correspondingfluctuations in linear wear and friction coefficient.The increase in chemical reactivity of a passive metal resulting from rubbing in a fretting experiment is expected to depend on the displacement amplitude,because the latter should affect the rate of de-passivation due to mechanical damage of the oxidefilm.Thus,an increased electrochemi-cal reactivity would be expected with increasing displace-ment amplitude.This is indeed confirmed by the data of Table1but only for amplitudes>10␮m,i.e.when the gross slip fretting regime dominates.In case of partial slip and elastic accommodation,no evidence for changes in elec-trochemical activity are detected.Thus,one can conclude that slip is necessary to promote metal activation.However, mechanical wear is observed even at low amplitudes.One would expect that this wear should lead to exposure of fresh metal surface and,hence,a measurable anodic cur-rent due to re-oxidation.The fact that no such current is observed can be explained by considering that at very low displacement amplitude,the extent of de-passivated area is small and the corresponding electrochemical response may be below the detection limit.An other explanation could be that in the absence of slip no electrolyte is present at the contacting surfaces(except when a wear fragment is released),thus excluding an electrochemical reaction. More studies will be necessary to elucidate the observed behaviour.Several works discuss wear of titanium alloys under fret-ting conditions.Among others,Blanchard reports that wear fragments under certain fretting-wear conditions arise from a tribologically transformed structure(TTS)[22].On one hand,Sauger et al.also reports that TTS formation in dry conditions strictly depends on mechanical parameters and that no oxidation phenomenon influences the amount of TTS formed[23].Under the present experimental conditions a distinct influence of the applied potential on the magnitude of the wear volume and on the elasticity behaviour of the contact was observed,which supports the notion that fret-ting in corrosive environments strongly depends on elec-trochemical parameters.Therefore,other mechanisms than TTS formation are likely to determine fretting–corrosion. Wear enhancement due to surface oxidefilms formed at different potential has previously been reported for slid-ing contacts[7,24,25].The thickness of passivefilms is known to increase with the applied potential[20].More-over,a potential dependence of the chemical composition of the surface oxidefilm on Ti6Al4V has been observed [21].These observations provide evidence for the important role played by the surface state of the metal.The present data show that any interpretation of the wear process should also include the possible degradation of the antagonist as evidenced in Fig.11.Surprisingly,the electrochemical con-ditions were found to also affect the elastic behaviour of the tribological system,as indicated by the different slopes in the friction–displacement loops in Fig.11.The slope K slope is usually associated with the rigidity of the contact K contact and of the device K device.Blanchard et ed[18] a model based on two springs in series to determine the。

毕业设计(论文)外文资料翻译系别：机电信息系专业：机械设计制造及其自动化班级：姓名：学号：外文出处：International Journal of Engineering, Science andTechnologyVol. 1, No. 1, 2009, pp. 254-271附件： 1. 原文； 2. 译文2013年03月一个复杂的特征值分析与设计相结合的方法实验（DOE）研究盘式制动器制动尖叫摘要：本文提出了研究结合有限元模拟与统计回归技术的制动片上的盘式制动器制动尖叫的影响因素探讨。

复杂的特征值分析（CEA）已被广泛用于在制动系统模型预测的不稳定频率、有限元模型与实验模态试验的相关性。

“制动器和制动盘的几何形状之间的输入输出关系的构建可以利用各种几何配置预测盘式制动器的尖叫。

影响的各种因素，即；杨氏模量背板，背板厚度，槽，两槽间的距离，槽的宽度和角度，槽所使用的设计研究实验（DOE）技术等。

预测在数学模型的基础上已开发的最有影响的因素验证，仿真实验证明了它的充分性。

预测结果表明，制动尖叫倾向可以通过增加的杨氏模量的背板和添加修改倒角形状减少摩擦材料双方的摩擦。

通过引入槽结构，制动尖叫使用建模相结合的方法CEA和美国能源部被发现通过验证试验的统计学足够。

这种组合方式会有用到盘式制动器的设计阶段。

关键词：盘式制动器的制动尖叫，有限元分析，实验模态分析，实验设计1、引言：制动器尖叫是因为摩擦力能够诱导的动态不稳定性引起的振动引起的噪声问题（Akay，2002）。

制动操作期间，垫和盘之间的摩擦力可以诱导系统中的动态不稳定性。

通常制动尖叫发生在1和20千赫之间的频率范围。

尖叫声是一个复杂的现象，部分原因是因为它的强烈的依赖于许多参数，部分原因是因为这些机械相互作用在制动系统。

机械的相互作用被认为是由于在摩擦界面接触的非线性影响非常复杂。

发生尖叫是间歇性的或随机的。

在一定的条件下，即使当汽车是全新的，它也往往产生尖叫噪声，以消除噪声为目标进行广泛的研究。

人参皂苷合成途径中催化达玛烯二醇合成原人参二醇的细胞色素P450酶——CYP716A47摘要：人参是一种有名的中药，且在它的根中含有药理活性成分——人参皂苷。

人参皂苷是四环三萜皂苷的一种，被认为是由达玛烯二醇经过细胞色素P450羟化和糖基转移酶糖基化后形成的。

然而，还没有编码羟基化和糖基化的基因被鉴定出来。

本文，我们鉴定了一个原人参二醇合酶，该酶为细胞色素酶，通过对达玛烯二醇的碳12位进行羟化作用形成原人参二醇。

从由茉莉酸甲酯诱导后的人参不定根的EST序列中筛选到9个假定的细胞色素序列。

因为CYP716A47不止在茉莉酸甲酯诱导后表达量提高，且在过表达角鲨烯合酶，皂苷高产的转基因人参中表达量也很高，因此被认为是原人参二醇合酶。

体外实验证明CYP716A47催化达玛烯二醇合成原人参二醇。

在酿酒酵母WAT21中异源表达CYP716A47，可催化达玛烯二醇合成原人参二醇。

另外，在不添加达玛烯二醇的情况下，在酵母中共表达，达玛烯二醇合酶基因和CYP716A47基因，能生成原人参二醇。

由达玛烯二醇形成的原人参二醇结构式通过液相色谱联合大气压化学电离质谱进行分析鉴定。

因此，CYP716A47是一个催化达玛烯二醇合成原人参二醇的达玛烯C12羟化酶。

关键词：CYP716A47；细胞色素P450；达玛烯二醇；人参皂苷；原人参二醇1、前言三萜皂苷是高等植物中异戊二烯类的次生代谢产物。

在不同种类的植物中它表现出结构和生物活性的多样性。

这些分子具有可观的商业价值且很多已被用作药物。

植物中人参皂苷的天然功能被认为可能与防御病原菌和害虫攻击有关。

三萜皂苷的基本骨架有齐墩果烷型，乌苏果烷型，羽扇豆醇型和达玛烷型。

人参因为它对癌症，糖尿病和神经退行性等疾病有显著的药理活性而闻名。

人参皂苷是人参根中的主要生物活性成分。

人参根中至少含有其干重4%的皂苷。

人参皂苷的主要成分是七个达玛烷型的四环三萜皂苷（人参皂苷Rb1, Rb2, Rc, Rd, Re, Rf 和Rg1）和一个含量很少的齐墩果烷型皂苷Ro。

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