CN105606492B - A kind of interdiffusion coefficient measurement method eliminating cooling procedure and influencing - Google Patents
A kind of interdiffusion coefficient measurement method eliminating cooling procedure and influencing Download PDFInfo
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Abstract
The invention discloses a kind of interdiffusion coefficient measurement methods that elimination cooling procedure influences, it is characterized in that carrying out as follows: 1 carries out isothermal diffusion experiment using the big diffusion couple of Semi-infinite One-dimensional of the counterdiffusion equipment to alloy melt, obtains component spectrum；2 obtain the interdiffusion coefficient of the big diffusion couple of Semi-infinite One-dimensional；3 obtain the diffusion length of the big diffusion couple of Semi-infinite One-dimensional；4 obtain interdiffusion coefficient and diffusion length of the big diffusion couple of Semi-infinite One-dimensional in isothermal diffusion process.The present invention can be on the basis of sliding shearing technique easy to operate, accurately, the influence of cooling procedure diffusion is reasonably eliminated, improve the measurement accuracy of counterdiffusion experiment, so as to obtain accurate counterdiffusion data, for the foundation of alloy melt counterdiffusion database, the development in associated alloys melt field and the design of metal material and application contribute.
Description
Technical field
It is specifically a kind of to be disappeared using the dependence of diffusion length at any time the present invention relates to alloy melt counterdiffusion field
Except the diffusion of cooling procedure, interdiffusion coefficient is obtained, the method for improving interdiffusion coefficient measurement accuracy.
Background technique
It spreads as important dynamic phenomena a kind of in alloy melt, has to mass transport processes numerous in melt significant
Influence, as melt solidification and crystallization process in, the size of solutes accumulation coefficient directly determines the component distributing of solidified structure, life
Long mode and microscopic appearance.Although alloy melt generally wants fast 2~3 orders of magnitude relative to the diffusion of solid alloy, with
Chemical reaction rate is compared to very slowly, therefore, melt spreads again the often important limiting factor of chemical reaction again.It is resonable
By aspect is calculated, the diffusion of melt is not only the important inspection of important an input parameter and analog result of computer simulation
Standard, and be to establish melt structure, kinetic model, the essential data source of theory of development and verifying newly.Currently,
The diffusion theory of liquid metals and alloy is still far from perfect, and basic reason is in addition to structure is complicated, diffusion coefficient data for melt
It is outer that library amount is insufficient, another important reason is exactly that the measurement accuracy of existing diffusion coefficient is not high, how to be obtained high-precision
Diffusion coefficient also becomes the focus of numerous scholars and Experts ' Attention.
Experimentally, obtaining high-precision melt interdiffusion coefficient still has many difficulties, especially for traditional length
Capillary tube method, due to there is the influence of the factors such as diffusion in heating process and cooling procedure, error range can reach 50%~
100%.It is cumbersome and can not largely carry out counterdiffusion experiment since structure is complicated for measuring accurate cut unit method.?
On the basis of traditional long capillary method and cut unit method, the independent research of this seminar has gone out carry out alloy melt counterdiffusion measurement
Equipment and slide shearing method accordingly, relative to traditional long capillary method, what it can effectively avoid spreading in heating process
It influences, therefore error significantly reduces, measurement accuracy is higher；Cut unit method is compared simultaneously, its equipment operation is simple, and it is low in cost,
Therefore be conducive to carry out a large amount of counterdiffusion measurement, but the influence for temperature-fall period diffusion not can avoid but.Unquestionably,
Temperature-fall period has a certain impact to the measurement accuracy tool of experiment, and existing some experimental results also show this point, especially
When shorter for isothermal diffusion time, this influence is more significant.
Accurate interdiffusion coefficient be not only the new melt diffusion theory of building alloy melt counterdiffusion database, creation,
The basis of computer Simulation calculation is carried out, and is to disclose, characterize and explain the melts dynamics such as Liquid liquid transition, Liquid-solid Transition
The important parameter of phenomenon.In addition, the brand-new materials such as either traditional metal material or glassy metal, high-entropy alloy, accurately
Interdiffusion coefficient for the molding control of material, technological design, ingredient design, Defect prevention and structure transformation etc. processes all have
There is extremely important directive function.Therefore, mutually expand to further be improved on the basis of sliding shearing technique easy to operate
The measurement accuracy for dissipating experiment, obtains accurate counterdiffusion data quickly, in large quantities, it is necessary to reasonably correct cooling procedure diffusion couple
The influence of whole counterdiffusion process.
Summary of the invention
The present invention is to propose a kind of mutual expansion that elimination cooling procedure influences to overcome the shortcomings of the prior art place
Coefficient measuring method is dissipated, to accurately, reasonably eliminate cooling procedure on the basis of sliding shearing technique easy to operate and expand
Scattered influence improves the measurement accuracy of counterdiffusion experiment, is alloy melt counterdiffusion so as to obtain accurate counterdiffusion data
The foundation of database, the development in associated alloys melt field and the design of metal material and application contribute.
The present invention adopts the following technical scheme that in order to solve the technical problem
The present invention is to carry out as follows a kind of the characteristics of eliminating the interdiffusion coefficient measurement method that cooling procedure influences:
Step 1, at set diffusion temperature T, utilize the big expansion of Semi-infinite One-dimensional of the counterdiffusion equipment to alloy melt
Scattered idol carries out M isothermal diffusion experiment respectively, and obtaining isothermal diffusion time is respectively t1,
t2..., tm..., tMComponent spectrum C (t1), C (t2) ..., C (tm) ..., C (tM)；tmIndicate the big diffusion couple of the Semi-infinite One-dimensional m-th of isothermal diffusion time at the diffusion temperature T；1≤m≤M；C(tm) described in expression
The big diffusion couple of Semi-infinite One-dimensional is in m-th of isothermal diffusion time tmComponent spectrum, and haveIndicate the Semi-infinite One-dimensional
Big diffusion couple is in m-th of isothermal diffusion time tmPosition on concentration；NmIndicate institute
State the m time isothermal diffusion experiment of the big diffusion couple of Semi-infinite One-dimensional at the diffusion temperature T
The middle number measured into branch；1≤nm≤Nm；A, B respectively indicates the constituent element of the big diffusion couple of the Semi-infinite One-dimensional；Respectively indicate the atomic percent of the big diffusion couple of Semi-infinite One-dimensional A constituent element on the position+∞ and on the position-∞
Specific concentration,
Step 2 obtains the big diffusion couple of Semi-infinite One-dimensional using formula (1)In the expansion
Dissipate the interdiffusion coefficient D of the m times isothermal diffusion experiment under temperature Tm, to obtain the mutual expansion under M different isothermal diffusion times
Dissipate coefficient D1, D2..., Dm..., DM:
In formula (1), C (x, tm) indicate the big diffusion couple of Semi-infinite One-dimensionalAt m-th
Isothermal diffusion time tmXth position on concentration；Indicate the big diffusion couple of the Semi-infinite One-dimensionalThe position at interface is spread in the m times isothermal diffusion experiment at the diffusion temperature T；erf()
Indicate error function；
Step 3 obtains the big diffusion couple of Semi-infinite One-dimensional using formula (2)In the expansion
Dissipate the diffusion length L of the m times isothermal diffusion experiment under temperature Tm, so that the diffusion obtained under M different isothermal diffusion times is long
Spend L1, L2..., Lm..., LM:
Step 4, using formula (3) to the 4D in formula (2)mtmIt is decomposed:
In formula (3),Indicate the big diffusion couple of the Semi-infinite One-dimensionalIn the diffusion
Under temperature T the m times counterdiffusion experiment in isothermal diffusion process interdiffusion coefficient；Indicate the big diffusion of the Semi-infinite One-dimensional
It is evenThe average counterdiffusion for the diffusion process that cools down in the m times counterdiffusion experiment at diffusion temperature T
Coefficient, t 'mIt indicates to drop to room temperature temperature fall time experienced from the diffusion temperature T in the m times counterdiffusion experiment；
Step 5, by the interdiffusion coefficient of the isothermal diffusion processIt is denoted as D；By being averaged for the cooling diffusion process
Interdiffusion coefficientWith temperature fall time t 'mIt is denoted as respectivelyWith t '；Then formula (3) is rewritten are as follows:
Step 6, the function table that the diffusion length L as shown in formula (5) and isothermal diffusion time t are obtained according to formula (2) and (4)
Up to formula L2(t):
Step 7, the function expression L that t=0 moment isothermal diffusion time is obtained using formula (6)2(0):
Formula (6) are substituted into formula (5) acquisition formula (7) by step 8:
L2(t)=4Dt+L2(0) (7)
Step 9 is fitted formula (7), to obtain the big diffusion couple of the Semi-infinite One-dimensionalAt the diffusion temperature T in the m times isothermal diffusion experiment isothermal diffusion process counterdiffusion
The coefficient D and diffusion length L at isothermal diffusion time t=0 moment (0).
Compared with the prior art, the invention has the advantages that:
1, the present invention is based on sliding shearing technique, and compared to complicated cut unit method, present invention experiment is set
Standby building is simple, it is easy to accomplish, it is low in cost, conducive to long-term, a large amount of measurement for carrying out interdiffusion coefficient is carried out；Simultaneously originally
The experimental implementation of invention is convenient far beyond cumbersome cut unit method, and measurement experiment is easy to carry out, and is convenient for promotion and application.
2, the present invention sliding shearing technique basis on, by same diffusion couple ingredient under same diffusion temperature into
At least the counterdiffusion experiment acquisition of different isothermal diffusion times diffuses into open score accordingly to row more than three times, utilizes measured expansion
Component spectrum is dissipated, obtains and diffuses into open score accordingly；By the dependence of diffusion length at any time, will can rationally, effectively melt
The diffusion of body cooling procedure and the diffusion of melt constant temperature process are separated, and the counterdiffusion at the corresponding temperature of corresponding diffusion couple is obtained
Coefficient；Therefore, the present invention overcomes the shadows that traditional long capillary method and general sliding shearing method can not eliminate cooling procedure diffusion
Loud disadvantage can quickly and easily obtain accurate interdiffusion coefficient, to significantly improve interdiffusion coefficient measurement accuracy.
3, the present invention has good versatility, theoretically, can also be with traditional length other than in conjunction with sliding shearing method
Capillary tube method is combined, and under the premise ofs the operation of specification, accurate measurement etc., eliminates two processes diffusions of heating and cooling
It influences, greatly improves the interdiffusion coefficient measurement accuracy of this method.
Detailed description of the invention
Fig. 1 is diffusion couple of embodiment of the present invention Al75Cu25-Al65Cu35The fingerprints of middle Cu element；
Fig. 2 is diffusion couple of embodiment of the present invention Al75Cu25-Al65Cu35Middle diffusion length and result figure.
Specific embodiment
In order to be discussed to the present invention is further, below in conjunction with diffusion couple Al75Cu25-Al65Cu35Dispersal behavior into
Row illustrates.According to selected diffusion couple ingredient, Al-Cu binary alloy phase diagram is consulted, according to liquidus temperature, is determined real
The isothermal diffusion temperature tested is 1023K in this example.The diffusion sample of diffusion couple ingredient is prepared, former material used in sample in this example
Material is the Al and Cu of purity 99.99%.The rod-like samples that casting diameter is 2mm are inhaled using vacuum melting furnace, casting process is inhaled and uses argon
Gas shielded, in order to guarantee that ingredient is uniform, sample is at vacuum melting furnace domestic demand at least melting 5 times.
It carries out solving diffusion couple Al using the present invention75Cu25-Al65Cu35Interdiffusion coefficient in 1023K includes following step
It is rapid:
Step 1, at set diffusion temperature T, using be able to use sliding shearing technique (granted patent
The counterdiffusion equipment for 201210105224.X) measuring melt interdiffusion coefficient carries out M isothermal diffusion experiment to the big diffusion couple of the Semi-infinite One-dimensional of alloy melt respectively, and obtaining isothermal diffusion time is respectively t1, t2...,
tm..., tMComponent spectrum C (t1), C (t2) ..., C (tm) ..., C (tM), in this example, T=1023K；Counterdiffusion experiment is being closed
It completes on golden melt diffusion facilities (granted patent 201210105060.0), before being diffused experiment, sample is polishing to directly
Diameter is 1.5mm.In experimentation, the upper and lower temperature difference for spreading platform is controlled within ± 3K.Sample after experiment is cut, is beaten
It is milled to middle position, then determines diffusion couple sample along the component spectrum in the direction length x using energy-spectrum scanning.tmIndicate one-dimensional half nothing
Limit big diffusion couple m-th of isothermal diffusion time at diffusion temperature T；M indicates that diffusion couple is expanding
Dissipate the total degree that counterdiffusion experiment is carried out under temperature T, 1≤m≤M, M=4, t in this example1=480s, t2=600s, t3=
720s, t4=840s；C(tm) indicate that the big diffusion couple of Semi-infinite One-dimensional is spread in m-th of isothermal
Time tmComponent spectrum, and haveIn this example
Diffusion couple Al75Cu25-Al65Cu35T is spread in T=1023K isothermal3The Cu element obtained after=720s diffuses into open score C (t3)
As shown in Figure 1；Indicate that the big diffusion couple of Semi-infinite One-dimensional is spread in m-th of isothermal
Time tmPosition on concentration, shown in the dot in this example as shown in figure 1；NmIndicate that Semi-infinite One-dimensional is big
Diffusion couple measures at branch in the m times isothermal diffusion experiment at diffusion temperature T
Number, 1≤nm≤Nm, N in this example1=N2=N3=N4=32；A, B respectively indicates the constituent element of the big diffusion couple of Semi-infinite One-dimensional, this
A=Cu in example, B=Al；Respectively indicate the big diffusion couple of Semi-infinite One-dimensional on the position+∞ and the position-∞ on A
The atom percentage concentration of constituent element, in this example
Step 2 obtains the big diffusion couple of Semi-infinite One-dimensional using formula (1)In diffusion temperature T
The interdiffusion coefficient D of lower the m times isothermal diffusion experimentm, to obtain the interdiffusion coefficient D under M different isothermal diffusion times1,
D2..., Dm..., DM, D in this example1=(10.4 ± 1.2) 10-9m2/ s, D2=(10.1 ± 0.6) 10-9m2/ s, D3=
(9.7±1.0)·10-9m2/ s, D4=(9.8 ± 1.1) 10-9m2/ s:
In formula (1), C (x, tm) indicate the big diffusion couple of Semi-infinite One-dimensionalIn m-th of isothermal
Diffusion time tmXth position on concentration, C (x, t in this example3) as shown by the solid lines of fig. 1,；Indicate one-dimensional half nothing
Limit big diffusion coupleThe position at interface is spread in the m times isothermal diffusion experiment at diffusion temperature T,
In this example,Erf () indicates error function；
Step 3 obtains the big diffusion couple of Semi-infinite One-dimensional using formula (2)In diffusion temperature T
The diffusion length L of lower the m times isothermal diffusion experimentm, to obtain the diffusion length L under M different isothermal diffusion times1,
L2..., Lm..., LM, in this exampleNumerical value it is as shown in table 1:
Step 4, using formula (3) to the 4D in formula (2)mtmIt is decomposed:
In formula (3),Indicate the big diffusion couple of Semi-infinite One-dimensionalAt diffusion temperature T
The interdiffusion coefficient of isothermal diffusion process in m counterdiffusion experiment,Indicate the big diffusion couple of Semi-infinite One-dimensionalAt diffusion temperature T in the m times isothermal diffusion experiment isothermal diffusion process to 4DmtmTribute
It offers；Indicate the big diffusion couple of Semi-infinite One-dimensionalThe m times counterdiffusion is tested at diffusion temperature T
The average interdiffusion coefficient of middle cooling diffusion process, t 'mIt indicates to drop to room temperature institute from diffusion temperature T in the m times counterdiffusion experiment
The temperature fall time of experience；Indicate that diffusion couple the m times counterdiffusion at specified diffusion temperature T cools down diffusion process in testing
To 4DmtmContribution,
Step 5, by the interdiffusion coefficient of isothermal diffusion processIt is denoted as D；By the average counterdiffusion system for the diffusion process that cools down
NumberWith temperature fall time t 'mIt is denoted as respectivelyWith t '；Then formula (3) is rewritten are as follows:
According to the property of interdiffusion coefficient it is found that in M diffusion experiment isothermal diffusion process interdiffusion coefficientPhase
Together, it is denoted as D；Meanwhile the cooling procedure of M diffusion experiment of the diffusion couple at specified diffusion temperature T is all from specified diffusion temperature
Degree drops to room temperature, and cooling condition is all consistent, and solid-state diffusion is slower than liquid state diffusion very much, it can thus be assumed that this M times diffusion is real
Cooling procedure having the same is tested, therefore in M diffusion experiment of diffusion couple, the average counterdiffusion having the same of cooling diffusion process
Coefficient and identical temperature fall time, are denoted as respectivelyWith t '；
Step 6, according to formula (2) and (4) it is found that stating the diffusion length L that diffusion couple tests measurement at specified diffusion temperature T
It is made of isothermal diffusion part and cooling diffusion two parts, therefore the diffusion length L as shown in formula (5) and isothermal diffusion can be obtained
The function expression L of time t2(t):
Step 7, by formula (5) it is found thatEssence correspond to diffusion couple at specified diffusion temperature T it is a certain have it is as follows
The diffusion length of the diffusion process of feature: the isothermal diffusion time of this diffusion process is 0, it may be assumed that
The function expression L at t=0 moment isothermal diffusion time is obtained using formula (6)2(0):
By (6) it is found that diffusion couple cooling procedure at specified diffusion temperature T can be seen as to the contribution of diffusion length and isothermal
Diffusion time unrelated constant；
Formula (6) are substituted into formula (5) acquisition formula (7) by step 8:
L2(t)=4Dt+L2(0) (7)
Step 9 is fitted formula (7), to obtain the big diffusion couple of Semi-infinite One-dimensional
At diffusion temperature T in the m times isothermal diffusion experiment when the interdiffusion coefficient D of isothermal diffusion process and isothermal diffusion time t=0
The diffusion length L (0) at quarter, in this example, L2(0)=3.1 ± 1.1mm2, D=(8.8 ± 0.3) m2/s.Accordingly, according to step 3 institute
Diffusion length L under M times obtained different isothermal diffusion times1, L2..., Lm..., LM, D and L can be acquired using formula (7)2(0)
Size；L2It (0) is the diffusion couple influence that the diffusion couple whole system of cooling procedure is spread at specified diffusion temperature T；Mutually expand
Dissipating coefficient D is that diffusion couple eliminates the resulting interdiffusion coefficient of cooling procedure influence at specified diffusion temperature T.So this
Method can effectively separate the diffusion of constant temperature process and the diffusion of temperature-fall period, to eliminate cooled in propagation measurement
The influence of journey significantly improves the measurement accuracy of counterdiffusion.
Table 1 is using sliding shearing technique to diffusion coupleWhen the diffusion of 1023K isothermal is different
Between tmThe diffusion length obtained afterwardsAnd corresponding interdiffusion coefficient Dsingle.
The interdiffusion coefficient D and single experiment gained interdiffusion coefficient D that table 2 is obtained using formula (4)singleDeviation to D
Δ.
In table 2: Δ=(Dsingle- D)/D100%.
It can be obtained from Fig. 2 and the analysis of table 2, consistent with the technical solution of front, experimental result and formula (7) meet very well, and
And with isothermal diffusion time tmIncrease, single diffusion experiment interdiffusion coefficient D obtainedsingleReally it becomes closer to
In the interdiffusion coefficient D obtained using Time Dependent method proposed by the present invention, the corresponding Δ that deviates is also smaller and smaller, theoretically
Work as tmWhen tending to infinity, DsingleD will be accurately equal to, and for isothermal diffusion time tmWhen smaller, since cooling procedure expands
Scattered influence, DsingleDeviate considerably from D.By this example it is found that proposed by the present invention obtain melt counterdiffusion system by Time Dependent
Several methods can actually rationally, effectively eliminate cooling procedure diffusion influence, significantly improve interdiffusion coefficient measurement accuracy.
Therefore, by this method in conjunction with simple, convenient sliding shearing technique and low-cost alloy melt diffusion facilities phase
In conjunction with, can not only be rapidly performed by counterdiffusion measurement, obtain a large amount of counterdiffusion data, while can guarantee surveyed counterdiffusion data
Precision.Largely lack for current diffusion data, the status that data precision is not high, the acquisition interdiffusion coefficient that the present invention provides
Method have very important significance of scientific research and practical value.
Claims (1)
1. a kind of interdiffusion coefficient measurement method eliminating cooling procedure and influencing, it is characterized in that carrying out as follows:
Step 1, at set diffusion temperature T, carry out M isothermal diffusion experiment respectively using the big diffusion couple of Semi-infinite One-dimensional of the counterdiffusion equipment to alloy melt, obtaining isothermal diffusion time is respectively t1, t2...,
tm..., tMComponent spectrum C (t1), C (t2) ..., C (tm) ..., C (tM)；tmIndicate the big diffusion couple of the Semi-infinite One-dimensional m-th of isothermal diffusion time at the diffusion temperature T；1≤m≤M；C(tm) described in expression
The big diffusion couple of Semi-infinite One-dimensional is in m-th of isothermal diffusion time tmComponent spectrum, and haveIndicate the Semi-infinite One-dimensional
Big diffusion couple is in m-th of isothermal diffusion time tmPosition on concentration；NmIndicate institute
State the m time isothermal diffusion experiment of the big diffusion couple of Semi-infinite One-dimensional at the diffusion temperature T
The middle number measured into branch；1≤nm≤Nm；A, B respectively indicates the constituent element of the big diffusion couple of the Semi-infinite One-dimensional；Respectively indicate the atomic percent of the big diffusion couple of Semi-infinite One-dimensional A constituent element on the position+∞ and on the position-∞
Specific concentration,
Step 2 obtains the big diffusion couple of Semi-infinite One-dimensional using formula (1)In the diffusion temperature
Spend the interdiffusion coefficient D of the m times isothermal diffusion experiment under Tm, to obtain the counterdiffusion system under M different isothermal diffusion times
Number D1, D2..., Dm..., DM:
In formula (1), C (x, tm) indicate the big diffusion couple of Semi-infinite One-dimensionalExpand in m-th of isothermal
Dissipate time tmXth position on concentration；Indicate the big diffusion couple of the Semi-infinite One-dimensional?
The position at interface is spread under the diffusion temperature T in the m times isothermal diffusion experiment；Erf () indicates error function；
Step 3 obtains the big diffusion couple of Semi-infinite One-dimensional using formula (2)In the diffusion temperature
Spend the diffusion length L of the m times isothermal diffusion experiment under Tm, to obtain the diffusion length L under M different isothermal diffusion times1,
L2..., Lm..., LM:
Step 4, using formula (3) to the 4D in formula (2)mtmIt is decomposed:
In formula (3),Indicate the big diffusion couple of the Semi-infinite One-dimensionalIn the diffusion temperature T
The interdiffusion coefficient of isothermal diffusion process in lower the m times counterdiffusion experiment；Indicate the big diffusion couple of the Semi-infinite One-dimensionalThe average counterdiffusion system for the diffusion process that cools down in the m times counterdiffusion experiment at diffusion temperature T
Number, t 'mIt indicates to drop to room temperature temperature fall time experienced from the diffusion temperature T in the m times counterdiffusion experiment；
Step 5, by the interdiffusion coefficient of the isothermal diffusion processIt is denoted as D；Average by the cooling diffusion process is mutually expanded
Dissipate coefficientWith temperature fall time t 'mIt is denoted as respectivelyWith t '；Then formula (3) is rewritten are as follows:
Step 6, the function expression that the diffusion length L as shown in formula (5) and isothermal diffusion time t are obtained according to formula (2) and (4)
L2(t):
Step 7, the function expression L that t=0 moment isothermal diffusion time is obtained using formula (6)2(0):
Formula (6) are substituted into formula (5) acquisition formula (7) by step 8:
L2(t)=4Dt+L2(0) (7)
Step 9 is fitted formula (7), to obtain the big diffusion couple of the Semi-infinite One-dimensional
The interdiffusion coefficient D of isothermal diffusion process and isothermal diffusion time t in the m times isothermal diffusion experiment at the diffusion temperature T
The diffusion length L (0) at=0 moment.
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