CN106769304A - 2099 aluminium lithium alloy standard sample preparation methods - Google Patents
2099 aluminium lithium alloy standard sample preparation methods Download PDFInfo
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- CN106769304A CN106769304A CN201611167543.8A CN201611167543A CN106769304A CN 106769304 A CN106769304 A CN 106769304A CN 201611167543 A CN201611167543 A CN 201611167543A CN 106769304 A CN106769304 A CN 106769304A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of 2099 aluminium lithium alloy standard sample preparation method, in the preparation method, the chemical composition in 2099 aluminium lithium alloy standard samples is have devised in advance, prepare raw material according to the Design of Chemical Composition value afterwards, by obtaining 2099 aluminium lithium alloy standard samples after the operations such as melting, casting, heat treatment, extruding, machining, and the analysis of ingot casting inspection, uniformity testing and definite value is carried out to the standard sample, finally prepare 2099 qualified aluminium lithium alloy standard samples of all technical.The preparation method of 2099 aluminium lithium alloy standard samples is simple to operate in the present invention, it is easy to accomplish, and for the production of 2099 aluminium lithium alloys provides technical support.
Description
Technical field
The present invention relates to aluminium lithium alloy field, more specifically to a kind of 2099 aluminium lithium alloy standard sample preparation side
Method.
Background technology
2099 aluminium lithium alloys compared with conventional aluminum alloys, with density it is low, specific strength is high, specific stiffness is high, the spy such as solderable
Point, is described as the ideal structure material of current aircraft industry.But, rarely have in the prior art on preparing 2099 aluminium lithium alloy marks
The method of quasi- sample.
Therefore, a kind of preparation method of 2099 aluminium lithium alloy standard sample how is developed, so as to be 2099 aluminium lithium alloys
Production provides technical support, is those skilled in the art's critical problem urgently to be resolved hurrily.
The content of the invention
It is an object of the invention to provide a kind of preparation method of 2099 aluminium lithium alloy standard sample.
To reach above-mentioned purpose, the present invention provides following technical scheme：
A kind of preparation method of 2099 aluminium lithium alloy standard sample, including：
The chemical composition in 2099 aluminium lithium alloy standard samples is designed, Design of Chemical Composition value is drawn, wherein：
Si:0.04%-0.06%, Fe:0.06%-0.08%, Cu:2.4%-2.8%, Mn:0.25%-0.35%, Mg:
0.25%-0.35%, Zn:0.65%-0.75%, Ti:0.02%-0.04%, Zr:0.08%-0.12%Li:1.6%-2%,
Be:0.0008%-0.0012%, Na:0.004%-0.006%, remaining is A1；
Raw material needed for preparing 2099 aluminium lithium alloys includes：Al99.90 aluminium ingots, Li, Mg, Na and Al-Si, Al-Fe, Al-
Cu, Al-Mn, Al-Ti, Al-Zr, Al-Be, Al-5Ti-1B, burdening calculation is carried out according to the Design of Chemical Composition value, it is accurate
Standby above-mentioned raw materials；
Prepare flux LiF+LiCl, mixing tool, slag hitting utensil, sampling instrument, bet pipe, funnel, crystallizer；
Melting is carried out to the raw material；
Casting；
It is heat-treated, extrudes, is machined into 2099 aluminium lithium alloy standard samples；
2099 aluminium lithium alloy standard samples are carried out with the analysis of ingot casting inspection, uniformity testing and definite value.
Preferably, when melting is carried out to the raw material, the temperature of melt is 740 DEG C -760 DEG C.
Preferably, when melting is carried out to the raw material, first added except Mg, Li, Na according to the Design of Chemical Composition value
With other metals outside Al-5Ti-1B, stirring sampling after fusing is good carries out on-the-spot sample analysis, to all units in addition to Mg, Li, Na
Cellulose content is adjusted, and Mg, Li, Na metal are added by burdening calculation value after adjusting, and is sprinkled into LiF+LiCl flux to described molten
Body carries out covering protection, stirs sampling analysis, carries out final composition adjustment, prepares toward interior addition Al-5Ti-1B of melt
Stove casts.
Preferably, be sprinkled into LiF+LiCl flux in the ratio of 10Kg/t carries out covering protection to melt.
Preferably, casting of coming out of the stove is prepared for Al-5Ti-1B toward addition in melt in the ratio of 2Kg/t.
Preferably, during casting, the melt temperature control is at 720 DEG C -740 DEG C.
Preferably, during casting, casting speed 70mm/min-75mm/min.
Preferably, during casting, cooling water pressure is controlled in 0.06MPa-0.08MPa.
Preferably, during casting, a diameter of 140mm-200mm of casting of 2099 aluminium lithium alloy standard samples.
From above-mentioned technical proposal as can be seen that the present invention in advance have devised 2099 aluminium lithium alloy standard samples in chemistry
Composition, prepares raw material, by works such as melting, casting, heat treatment, extruding, machinings according to the Design of Chemical Composition value afterwards
2099 aluminium lithium alloy standard samples are obtained after sequence, and ingot casting inspection, uniformity testing and definite value point are carried out to the standard sample
Analysis, finally prepares 2099 qualified aluminium lithium alloy standard samples of all technical.2099 aluminium lithium alloy standard in the present invention
The preparation method of sample is simple to operate, it is easy to accomplish, and for the production of 2099 aluminium lithium alloys provides technical support.
Brief description of the drawings
Scheme in order to illustrate more clearly the embodiments of the present invention, will use required described in embodiment below
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for ability
For field technique personnel, on the premise of not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
The technological process of the preparation method of the 2099 aluminium lithium alloy standard samples that Fig. 1 is provided for a specific embodiment of the invention
Figure；
Fig. 2 is the schematic diagram at ingot quality check sampling position in the present invention；
Fig. 3 is the schematic diagram that component segregation inspection takes a position in the present invention.
Specific embodiment
The invention provides a kind of preparation method of 2099 aluminium lithium alloy standard sample, so as to be the life of 2099 aluminium lithium alloys
Produce and provide technical support.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Base
In embodiments of the invention, those of ordinary skill in the art obtained on the premise of creative work is not made it is all its
Its embodiment, belongs to the scope of protection of the invention.
Refer to accompanying drawing 1- Fig. 3.In a specific embodiment of the invention, the preparation method of 2099 aluminium lithium alloy standard samples
Comprise the following steps：
The chemical composition in 2099 aluminium lithium alloy standard samples is designed, Design of Chemical Composition value is drawn, wherein：
Si:0.04%-0.06%, Fe:0.06%-0.08%, Cu:2.4%-2.8%, Mn:0.25%-0.35%
Mg:0.25%-0.35%, Zn:0.65%-0.75%, Ti:0.02%-0.04%, Zr:0.08%-0.12%,
Li:1.6%-2%, Be:0.0008%-0.0012%, Na:0.004%-0.006%, remaining is A1；
Have devised the chemical composition in 2099 aluminium lithium alloy standard samples in advance in this step, draw chemical composition
Design load.Further, the composition ratio of above-mentioned each element can be preferably：Si:0.05, Fe：0.07, Cu:2.6, Mn:
0.3, Mg:0.3, Zn:0.7, Ti：0.03, Zr：0.1, Li:1.8, Be：0.001, Na：0.005.
Raw material needed for preparing 2099 aluminium lithium alloys includes：Al99.90 aluminium ingots, Li, Mg, Na and Al-Si, Al-Fe, Al-
Cu, Al-Mn, Al-Ti, Al-Zr, Al-Be, Al-5Ti-1B, burdening calculation is carried out according to above-mentioned Design of Chemical Composition value, it is accurate
Standby above-mentioned raw materials.
Prepare flux LiF+LiCl, mixing tool, slag hitting utensil, sampling instrument, bet pipe, funnel, crystallizer.
Melting is carried out to the raw material.
Baked chute, bet pipe, flow table etc. are installed in place, is cast, cast out 2099 aluminium lithium alloy ingot castings.
2099 aluminium lithium alloy ingot castings and its standard sample are carried out with the analysis of ingot casting inspection, uniformity testing and definite value.
This specific embodiment have devised the chemical composition in 2099 aluminium lithium alloy standard samples in advance, afterwards according to the change
Study and set up evaluation preparation raw material separately, closed by obtaining 2099 aluminium lithiums after the operations such as melting, casting, heat treatment, extruding, machining
Goldstandard sample, and the analysis of ingot casting inspection, uniformity testing and definite value is carried out to the standard sample, finally prepare every skill
2099 aluminium lithium alloy standard samples of art qualified.The preparation method operation letter of 2099 aluminium lithium alloy standard samples in the present invention
It is single, it is easy to accomplish, and for the production of 2099 aluminium lithium alloys provides technical support.
In a specific embodiment of the invention, when melting is carried out to raw material, the temperature control of melt is at 740 DEG C -760
℃.Preferably Smelting Effect can be accessed in the temperature range.
In a specific embodiment of the invention, in order to ensure the content value of each element in 2099 aluminium lithium alloy standard samples exists
In the range of Design of Chemical Composition value, when melting is carried out to raw material, be first according to Design of Chemical Composition value first add except Mg,
Other metals outside Li, Na and Al-5Ti-1B, stirring sampling after fusing is good carries out on-the-spot sample analysis, in addition to Mg, Li, Na
All elements content is adjusted, and according to chemical composition design load adds Mg, Li, Na metal after adjusting, and is sprinkled into LiF+LiCl and melts
Agent carries out covering protection to the melt, stirs sampling analysis, carries out final composition adjustment, last toward addition Al- in melt
5Ti-1B carries out micronization processes, finally prepares casting of coming out of the stove.
Further, when LiF+LiCl flux is sprinkled into, carried out according to the ratio of 10Kg/t, i.e., be sprinkled into according to melt per ton
The ratio of 10KgLiF+LiCl flux is carried out.
Preferably, stokehold is being melted out, according to the ratio of 2Kg/t to adding Al-5Ti-1B in melt, i.e., according to per ton
The ratio of melt addition 2Kg adds Al-5Ti-1B, and the ratio is obtained in that excellent thinning effect.
During casting, by the temperature control of melt at 720 DEG C -740 DEG C, it is possible to further by the temperature of melt
Degree priority acccess control is at 735 DEG C.
In order to further optimize casting technological parameter, so as to obtain expected 2099 aluminium lithium alloy standard sample, can be by
Casting speed control further, is controlled in 72mm/min in 70mm/min-75mm/min；Cooling water pressure control is existed
0.06MPa-0.08MPa, further, controls in 0.07MPa.
In the present embodiment, it is contemplated that the follow-up detection to 2099 aluminium lithium alloy standard samples, by 2099 aluminium lithium alloy marks
The casting diameter design of quasi- sample is 140mm-200mm, and further, the diameter value can be preferably 162mm.
Following detection is carried out after preparing 2099 aluminium lithium alloy standard samples using the technical scheme in the present invention：
First, the ingot casting inspection of 2099 aluminium lithium alloy standard samples：
Ingot casting inspection test piece is cut as shown in Figure 2, end to end sawing amount：Bottom >=350mm, gate part >=200mm, sequentially takes
Metallographic specimen and component segregation test piece.Standard sample ingot casting must after the assay was approved can through microstructure examination and component segregation
Into subsequent handling.
1st, the ingot casting metallographic structure of 2099 aluminium lithium alloy standard samples is checked
By to No. 1 in Fig. 2, high and low times of inspection of No. 4 test pieces, as a result show that ingot structure is fine and closely woven, uniform, pore-free, folder
It is miscellaneous to wait metallurgical imperfection.
2nd, the ingot casting component segregation of 2099 aluminium lithium alloy standard samples is checked
In order to ensure the uniformity of standard sample composition, we to No. 2 in every ingot casting such as Fig. 2, No. 3 test pieces carry out composition
Segregation is checked.Taking as shown in Figure 3 a little carries out spectrum analysis, and every number takes five groups of data of A1~A5, every group of number from center to edge
According to the average result for secondary spark.Ingot casting radial direction component segregation degree is represented with the size of five groups of data component differences, with casting
No. 2 of ingot, the size of the respective five groups of differences of statistical average of No. 3 test pieces represent ingot casting longitudinal direction degree of segregation.Particular exam method
It is as follows：
1. radial segregation checks (Da Weite (DARVID) inspections)
Radially there is segregation if R/S ＞ d α .n
The radial direction segregation-free if R/S≤d α .n
R- extreme differences S- standard deviations in formula
Statistical constant (d α .n=2.753 here) d α .n- relevant with α .n
2. (t inspections) is checked in longitudinal segregation：If t0 ＞ t α v, there is segregation longitudinal direction；If t0≤t α v, longitudinal unbiased
Analysis.
In formula：
--- the respective average value of two test pieces；N --- take points (n=5)；
S1、S2--- the standard deviation of two test pieces；
ta.v--- the statistical constant (t here determined by α v=n-1a.vTake 2.306)
Ingotism assay illustrates radially, longitudinally equal segregation-free.
2nd, the uniformity testing of 2099 aluminium lithium alloy standard samples：
Standard sample uniformity is one of most critical index of standard sample, and standard sample chemical composition must be uniform.Root
Specify that we employ variance method and carry out uniformity testing to random sampling according to GB/T15000 and YS/T409.To eliminate instrument
Drift and the influence of light source fluctuation, the continuous operation method that we employ before blocked operation method is substituted carry out uniformity testing.
M (taking 24 by technical specification) sample is randomly selected, high precision assay method is used, in same experimental conditions
Under, each sample replication n times (being determined 3 times by technical specification) measures m group equally accurate determination datas：
x11, x12... ... x1n, average value
x21, x22... ... x2n, average value
... ... ... ... ... ...；
xm1, xm2, xmn, average value
Calculate overall average
Sum of square of deviations between calculating group(Q in formula1=MSamong)
Sum of square of deviations in calculating group(Q in formula2=MSwithin)
Calculate free degree ν1=m-1；ν2=m (n-1)
Counting statistics amount
According to taken level of significance α and free degree ν1, ν2, F is checked in from F inspections tables of critical valuesα.Compare F and FαSentenced
It is disconnected：
If 1) F ＜ Fα, then it is assumed that the interior no significant difference and between group of group, sample is uniform.
If 2) F >=Fα, then have systematic error, i.e. sample room there is some difference between suspecting each group, but it is actually used not
It is impacted.Now calculate inhomogeneities variance, and contributed to characteristic quantity standard value expanded uncertainty：
If 3) F ＞ FαThen think that sample is uneven.
Extracting 16 and 24 samples respectively to the woollen of 2099 aluminium lithium alloy standard samples carries out uniformity testing.Uniformly
Property assay is shown in Table 1.Each element uniformity is all qualified as seen from Table 1.
Table 1：K2099 aluminium lithium alloy standard sample uniformity testing results
3rd, the definite value analysis of 2099 aluminium lithium alloy standard samples：
Adopt processing definite value sample with the following method：From the every head of extruded rod, middle part, afterbody (after cutting away material head material tail)
Three segment standard sample rods (per segment length 200mm) are cut, bits shape is processed into drilling and milling machine and special cutter, mix packing.According to GB/
The regulation of T15000 and YS/T409, we entrust 8 laboratory cooperating analysis such as national light metal Quality Supervision and Inspection Center to determine
Value.Each laboratory analysis methodologies are shown in Table 2：
Table 2：Each cooperation experiment room definite value analysis method
4th, data processing
1st, having a large amount of initial data during research and production of metallurgical standard sample will carry out mathematical statistics, inspection and calculating.We are with newly
The software developed《StndMtrl systems》The data that constituent parts are quoted are counted and checked.
The method of inspection is as follows：
1. Figure correction：By GB/T 8170-2008《The expression and judgement of Figure correction rule and limiting figure》Carry out,
Error ending method.
2. Rod Dixon inspection：The result that each cooperation experiment room is quoted is tested by average value with Rod Dixon test criterion
And accept or reject, Rod Dixon assay is shown in Table 3.As seen from Table 3, assay is as good as constant value.
3. Normal distribution test：The normality of each cell mean is checked with Xia Piluo-Weir gram, assay is shown in Table 4.From table 4
It can be seen that, assay is normal distribution.
4. equally accurate inspection：With Cochran criterion judge each group of data whether equally accurate, assay is shown in Table 5.Can from table 5
See, assay is equally accurate.
2nd, the standard deviation and expanded uncertainty of standard value, single measurement are counted
Specified according to GB/T 15000 and YS/T409, this standard sample each element all meets normal distribution.By following public affairs
Formula calculates standard value and standard deviation：
Standard value
The standard deviation of single measurement
Synthetic standards deviation (S)：(S02, SL2, SW2 result of calculation are shown in Table 6)
In formula：
--- chemical numeraire variance；
SL2 --- uneven variance between block；SW2 --- uneven variance expanded uncertainty U in block：
K is the Coverage factor determined by fiducial probability and the free degree in formula, herein K=2.365 (α=0.05, conspicuousness water
It is flat；ν=m-1=7, the free degree).Stability uncertainty is ignored.
The standard definite value result (standard value, single measurement standard deviation, expanded uncertainty) of this standard sample is shown in Table 7.
In order to check the application effect of this standard sample, with this standard sample in two import spectrum of QSG750, ARL4460
2099 alloy samples are analyzed on instrument.Its analysis result is consistent with chemical results, is shown in Table 8.
Conclusion：
The development of 2099 aluminum alloy standard samples after the time more than a year, by composition design, founding, extruding etc. more than 30
Individual operation, satisfactory to complete development task, all technical reaches design objective.By trial application analyze, its result with change
Value is consistent.This standard sample can meet well 2099 aluminium alloys and its similar alloy composition analysis during to control sample
Demand, can significantly improve such alloy analysis speed and the degree of accuracy, economic benefit, social benefit are notable.
Table 3：2099 aluminium alloy standard specimen Rod Dixon assay w/%
Table 4：2099 aluminium alloy standard specimen Xia Piluo assays w/%
Table 5：2099 aluminium alloy single-point standard sample equally accurate assays
Table 6：2099 aluminium alloy single-point standard sample synthetic standards deviations are calculated
Table 7:2099 aluminium alloy standard specimen definite value results, %
Note：Expanded uncertainty isK=2.365 (α=0.05, significance；ν=m-1=7,
The free degree).
Table 8：2099 production result of appraisal %
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or uses the present invention.
Various modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The scope most wide for causing.
Claims (9)
1. a kind of preparation method of 2099 aluminium lithium alloy standard sample, it is characterised in that including：
The chemical composition in 2099 aluminium lithium alloy standard samples is designed, Design of Chemical Composition value is drawn, wherein：
Si:0.04%-0.06%, Fe:0.06%-0.08%, Cu:2.4%-2.8%, Mn:0.25%-0.35%, Mg:
0.25%-0.35%, Zn:0.65%-0.75%, Ti:0.02%-0.04%, Zr:0.08%-0.12%, Li:1.6%-
2%, Be:0.0008%-0.0012%, Na:0.004%-0.006%, remaining is A1；
Raw material needed for preparing 2099 aluminium lithium alloys includes：Al99.90 aluminium ingots, Li, Mg, Na and Al-Si, Al-Fe, Al-Cu,
Al-Mn, Al-Ti, Al-Zr, Al-Be, Al-5Ti-1B, burdening calculation is carried out according to the Design of Chemical Composition value, in preparation
State raw material；
Prepare flux LiF+LiCl, mixing tool, slag hitting utensil, sampling instrument, bet pipe, funnel, crystallizer；
Melting is carried out to the raw material；
Casting；
It is heat-treated, extrudes, is machined into 2099 aluminium lithium alloy standard samples；
2099 aluminium lithium alloy standard samples are carried out with the analysis of ingot casting inspection, uniformity testing and definite value.
2. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 1, it is characterised in that to the original
When material carries out melting, the temperature of melt is 740 DEG C -760 DEG C.
3. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 1, it is characterised in that to the original
When material carries out melting, other metals in addition to Mg, Li, Na and Al-5Ti-1B are first added according to the Design of Chemical Composition value,
Sampling is stirred after fusing is good carries out on-the-spot sample analysis, and all elements content in addition to Mg, Li, Na is adjusted, after adjusting by
Burdening calculation value adds Mg, Li, Na metal, and being sprinkled into LiF+LiCl flux carries out covering protection, stirring sampling point to the melt
Analysis, carries out final composition adjustment, and toward melt interior addition, Al-5Ti-1B prepares casting of coming out of the stove.
4. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 3, it is characterised in that by 10Kg/t's
Ratio is sprinkled into LiF+LiCl flux and carries out covering protection to melt.
5. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 3, it is characterised in that by 2Kg/t's
Ratio prepares casting of coming out of the stove for Al-5Ti-1B toward addition in melt.
6. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 1, it is characterised in that in the mistake of casting
Cheng Zhong, the melt temperature control is at 720 DEG C -740 DEG C.
7. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 6, it is characterised in that in the mistake of casting
Cheng Zhong, casting speed 70mm/min-75mm/min.
8. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 7, it is characterised in that in the mistake of casting
Cheng Zhong, cooling water pressure is controlled in 0.06MPa-0.08MPa.
9. the preparation method of 2099 aluminium lithium alloy standard sample according to claim 1, it is characterised in that in the mistake of casting
Cheng Zhong, a diameter of 140mm-200mm of casting of 2099 aluminium lithium alloy standard samples.
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