CN113624793B - Method for judging whether beta spot defect exists in near beta titanium alloy - Google Patents
Method for judging whether beta spot defect exists in near beta titanium alloy Download PDFInfo
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Abstract
The invention relates to a method for judging whether a near-beta titanium alloy has a beta spot defect or not, which comprises the following steps: (1) Providing a plurality of near-beta titanium alloy standard samples, carrying out heat treatment on each standard sample by adopting different heat treatment temperatures T, and collecting the percentage content P of alpha phase in each standard sample after heat treatment α Fitting P α Providing a near-beta titanium alloy sample to be measured according to the function relation (2) of T, observing the microstructure of the near-beta titanium alloy sample to be measured, and judging whether a suspected region exists in the microstructure; (3) Detecting chemical composition of suspected region and calculating beta phase transition point T corresponding to the chemical composition β1 The method comprises the steps of carrying out a first treatment on the surface of the (4) Judging whether the near-beta titanium alloy has beta spot defect according to the following formula: p (P) α ＝C 1 ×(T‑T β0 )+C 2 。
Description
Technical Field
The invention relates to the field of material detection, in particular to a method for judging whether a near-beta titanium alloy has a beta spot defect or not.
Background
The titanium alloy has excellent comprehensive performance and is widely applied to the aerospace field. The Ti17 alloy is a near beta alloy with excellent comprehensive performance. The alloy has higher strength, fracture toughness, thermal stability and fatigue performance, and has high hardenability and good hot workability. In recent years, commercial aircraft engines increasingly use Ti17 alloys as materials for low temperature section compressor disk forgings. However, since a large amount of alloying elements are added into the Ti17 alloy, cr segregation is extremely easy to occur in the smelting process. Under normal two-phase zone forging conditions, the Cr segregation zone is above the transformation temperature, and after forging, a superheated structure, i.e., beta spots, is formed. The hardness of the beta spot is higher, and the mechanical property of the material can be adversely affected.
In the related art, the beta spot detection procedure of the general Ti17 alloy bar is as follows: for bars in a two-phase forging state, cutting test blocks from cross sections of bar blanks of the same furnace number corresponding to the head and tail parts of an ingot, and heating the test blocks to a beta-phase transition temperature T β The temperature is 25 ℃ below, heat is preserved for 2 hours after heat penetration, and water cooling is carried out. Then preserving heat for 4-8 h at 602-650 ℃ and air cooling. And (3) carrying out microscopic examination on the test block after heat treatment, and judging that the material has beta-plaque defect when a region with the length of more than 0.75mm in any direction and the primary alpha phase of less than 5% exists.
Disclosure of Invention
The inventors found that the prior art detection methods have the potential for erroneous decisions. For example, when the beta spot detection heat treatment is performed, the temperature of the beta spot detection heat treatment shifts due to the measurement error of the phase change point, and when the micro-domain component of the beta stabilization element (Cr, mo, zr, etc.) in the material fluctuates, the primary alpha phase content in the region will be necessarily less than 5% (the primary alpha phase content in the normal Ti17 matrix is about 5%). The above-described case is determined to be a difference between the presence of the β -spot defect and the determination of whether or not the material has component segregation. Therefore, the "area with the primary α phase less than 5% cannot be used as the only standard for judging the β spot defect", and the field needs to find a detection standard capable of correcting the error, so as to perfect the currently practiced Ti17 alloy β spot defect detection method and avoid erroneous judgment.
According to the method, the titanium alloy standard sample is subjected to heat treatment at different temperatures, the content of primary alpha phase in the standard sample is detected, a functional relation between the content of primary alpha phase and the heat treatment temperature difference is fitted, the modified primary alpha phase content of a suspected region in the sample to be detected is further determined by utilizing the functional relation, and whether the sample has the beta-plaque defect is judged according to the modified primary alpha phase content.
In some aspects, a method of determining whether a near-beta titanium alloy has a beta spot defect is provided, comprising the steps of:
(1) Providing a plurality of near-beta titanium alloy standard samples, carrying out heat treatment on each standard sample by adopting different heat treatment temperatures T, and collecting the percentage content P of alpha phase in each standard sample after heat treatment α Fitting P α The functional relationship with T is as follows:
P α ＝C 1 ×(T-T β0 )+C 2 ；
wherein T is β0 The beta transformation point of the standard sample is in units of ℃;
wherein C is 1 And C 2 Is a constant;
(2) Providing a near-beta titanium alloy sample to be detected, observing the microstructure of the near-beta titanium alloy sample to be detected, and judging whether a suspected region exists in the microstructure, wherein the suspected region refers to a region with the percentage content of primary alpha phase in the microstructure less than 5% and the size of more than 0.75mm in at least one direction;
if the suspected region does not exist in the microstructure, judging that the beta spot defect does not exist in the sample to be detected;
if the suspected region exists in the microstructure, executing the next step;
(3) Detecting chemical composition of suspected region and calculating beta phase transition point T corresponding to the chemical composition β1 ；
(4) Judging whether the near-beta titanium alloy has beta spot defect according to the following formula:
P α ’＝C 1 ×(T β0 -T β1 -25)+C 2 ；
if P α And (5) judging that the near-beta alloy sample to be detected does not have the beta spot defect;
if P α And if' < 5%, judging that the near-beta alloy sample to be detected has the beta spot defect.
In some embodiments, the near-beta titanium alloy is a Ti17 titanium alloy.
In some embodiments, the near beta titanium alloy is a Ti17 titanium alloy, wherein
C 1 ＝-0.459，C 2 ＝-2.22。
In some embodiments, the near-beta titanium alloy is a Ti17 titanium alloy, wherein T β0 ＝897℃。
In some embodiments, in step (1), the different heat treatment temperatures T refer to: at (T) β0 -30) DEG C to (T β0 -5) different heat treatment temperatures in the range of c.
In some embodiments, in step (1), the heat treatment comprises: heating the sample to a heat treatment temperature T, preserving heat for 2 hours after heat penetration, cooling with water, preserving heat for 4 to 8 hours at 602 to 650 ℃, and cooling with air.
In some embodiments, in step (3), T β1 Obtained by calculation of the following formula:
Δ＝-19.3(Cr)-4.7(Zr)-16.8(Fe)-10.0(Mo)+23.1(Al)+154.5(O)
wherein Δ=t β1 -T β0
Wherein, (Cr) =P Cr1 -P Cr0 ，P Cr1 The weight percentage of Cr element and P in the suspected region of the sample to be detected Cr0 The Cr element weight percentage content of the standard sample.
In some embodiments, the suspected region refers to a region in the microstructure having a percentage of primary alpha phase of < 5% and a dimension of 0.75mm or more in two directions, a first direction and a second direction that are perpendicular to each other.
In some embodiments, the standard sample of titanium alloy and the sample to be measured of titanium alloy are produced and obtained by smelting furnaces with the same furnace number.
In some embodiments, the near-beta titanium alloy is a Ti17 titanium alloy, and the titanium alloy standard sample comprises the following alloying elements: 4.5 to 5.5 weight percent of Al, 1.5 to 2.5 weight percent of Sn, 1.5 to 2.5 weight percent of Zr, 3.5 to 4.5 weight percent of Mo and 3.5 to 4.5 weight percent of Cr.
In some embodiments, the near-beta titanium alloy is a Ti17 titanium alloy, and the titanium alloy standard sample comprises the following alloying elements: al 5wt%, sn 2wt%, zr 2wt%, mo 4wt% and Cr 4wt%.
In some embodiments, the Cr element content at different locations in the titanium alloy standard sample does not fluctuate by more than 1%.
In some embodiments, the titanium alloy standard sample has no more than 1% variation in the content of each element at different locations.
In some embodiments, no suspected region is present in the titanium alloy standard.
In some embodiments, the titanium alloy standard and the titanium alloy standard are (α+β) two-phase wrought titanium alloy samples.
Description of the terminology:
"near beta titanium alloy" means a titanium alloy having a beta stabilizing element content slightly above the critical concentration (the lowest concentration that will retain the high temperature beta phase to room temperature upon rapid cooling)
"Ti17 titanium alloy" is also called Ti-5Al-2Sn-2Zr-4Mo-4Cr titanium alloy, and the theoretical alloy element content is as follows:
| major alloying elements | Weight percent wt% |
| Al | 4.5-5.5wt％ |
| Sn | 1.6-2.4wt％ |
| Zr | 1.6-2.4wt％ |
| Mo | 3.5-4.5wt％ |
| Cr | 3.5-4.5wt％ |
"primary alpha phase" (primary alpha) refers to the alpha phase that remains from the upper portion of the last alpha-beta phase region by heating, and has a light-colored circular or oval morphology under an optical microscope. The percentage of primary alpha phase refers to the volume percentage of primary alpha phase.
Advantageous effects
One or more technical solutions of the present disclosure have one or more of the following beneficial effects:
1. the method reduces the misjudgment condition generated by judging the waste materials by judging whether the alpha phase content is the beta-spot segregation defect or not only depending on the content of the primary alpha phase;
2. according to the method, through analysis of the stable and consistent performance of the titanium alloy bar, the repeated detection procedure and cost of the beta spots are reduced, and the accuracy of the beta spot segregation detection is improved.
Drawings
FIG. 1 is a photograph of a microstructure of a sample to be tested;
FIGS. 2 (a) and (c) are a scanning electron microscope photograph and an energy spectrum (EDS) detection selection region photograph, respectively, of a suspected region; FIGS. 2 (b) and (d) are a scanning electron microscope photograph and an energy spectrum (EDS) detection selected region photograph of a normal region, respectively;
fig. 3 is a schematic diagram of the corresponding curves of the formulas (1) and (3) to (5).
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The drugs or instruments used were conventional products available commercially without the manufacturer's attention.
Providing the titanium alloy obtained by smelting in the same furnace.
1. Build-up of the percentage of primary alpha phase P α With heat treatment temperature TFunctional relationship
A plurality of Ti17 alloy standard samples without Cr segregation (Cr component difference of the alloy is less than 1 percent) of the furnace are provided. Wherein the main alloy element content is as follows: al (4.5-5.5 wt.%), sn (1.5-2.5 wt.%), zr (1.5-2.5 wt.%), mo (3.5-4.5 wt.%) and Cr (3.5-4.5 wt.%).
At T β0 -30 ℃ to from T β0 Within-5 ℃ C (Ti 17 alloy standard, T β0 The Ti17 alloy standard samples are respectively processed at different heat treatment temperatures of (897 ℃), heat-insulated for 2 hours after heat penetration, and water-cooled. Then preserving heat for 4-8 h at 602-650 ℃ and air cooling. Carrying out surface corrosion treatment on the test block after heat treatment, observing under an optical microscope, and recording the percentage content P of primary alpha phase in each standard sample α 。
Fitting the relation between the primary alpha phase content and the heat treatment temperature T to obtain the following fitting empirical relation (1):
P α ＝-0.459×(T-T β0 )-2.22 (1)
at a primary alpha phase content (P α ) On the ordinate, the heat treatment temperature and T β0 Is the difference (T-T) β0 ) On the abscissa, formula (1) is plotted as a curve, which is a "Ti17 matrix" curve in fig. 3.
According to the beta spot test program, the test block is heated to T in a simulation mode β0 -25 ℃ (i.e. 872 ℃), heat-insulating for 2 hours after heat penetration, and water-cooling. Then preserving heat for 4-8 h at 602-650 ℃ and air cooling. At this time, if t=t β0 The value of 25 is taken into formula (1), and P is obtained by solving α ＝9.255(％)。
From the above calculation results, the Ti17 alloy standard sample was subjected to T β0 P after heat treatment at-25 DEG C α =9.255 (%), greater than 5%, no β plaques are present.
2. Calculating the influence of component segregation on beta phase transition point deviation
When there is a segregation of components in the material, the beta transus point may deviate according to empirical formulas known in the art:
Δ＝-19.3(Cr)-4.7(Zr)-16.8(Fe)-10.0(Mo)+23.1(Al)+154.5(O)
wherein Δ=t β1 -T β0
Wherein, (Cr) =P Cr1 -P Cr0 ，P Cr1 The weight percentage (wt%) of Cr element and P of the sample to be tested Cr0 The Cr element weight percent (wt%) is the Cr element weight percent (wt%) of the standard sample. The other elements are calculated in the same way.
If the influence of the component segregation is taken into consideration, the beta transverter of the component segregation site is deviated, T β1 ＝T β0 +Δ, then translation of formula (1) will occur, yielding formula (2)
Pα＝-0.459(T-T β0 )+0.459(T β1 -T β0 )-2.22 (2)
When Δ=t, calculated according to equation (2) β1 -T β0 At = -9.27 ℃, if t=t β0 The value of 25 is taken into formula (2), and P is obtained by solving α =5 (%). In other words, when the beta transus point due to component segregation deviates to-9.27 ℃, the percentage of primary alpha phase P α Will be reduced to 5%.
It follows that when the segregation of the constituents is so severe that it results in a delta < -9.27 c, it results in a reduction of the percentage of primary alpha phase to less than 5%.
When Δ= -9.27 ℃, formula (2) can be written as formula (3):
Pα＝-0.459×(T-T β0 )-6.475 (3)
fig. 3 shows a curve represented by formula (3), and the region to the left of the curve is a β -patch region.
2. Observing the microstructure of the sample to be measured
And cutting test blocks from the cross sections of the furnace number bar blank corresponding to the head and tail of the ingot, and taking the test blocks as samples to be tested. In one beta spot test, the sample to be tested is heated to T in a simulation mode β0 -25 ℃ (i.e. 872 ℃), heat-insulating for 2 hours after heat penetration, and water-cooling. Then preserving heat for 4-8 h at 602-650 ℃ and air cooling. Carrying out surface corrosion treatment on the test block after heat treatment, and observing the microstructure of the test block under an optical microscope:
the preliminary detection result is: the head of the bar had a region (1.2% of the detection result) of about 1.7mm with less than 5% of the primary alpha phase content, and was judged as a suspected region, see fig. 1. The primary alpha phase content of the normal region around the suspected region was 5.6%.
The suspected region and the normal region were each subjected to energy spectrum (EDS) detection. Fig. 2 (a) and (c) show scanning electron microscope photographs and energy spectrum (EDS) detection selective area photographs of a local position of a suspected region. Fig. 2 (b) and (d) show scanning electron microscope photographs and energy spectrum (EDS) detection selective area photographs of a local position of a normal area.
The two positions (position 1 and position 2) on the suspected region were subjected to spectrum detection, and one position (position 3) on the normal region was subjected to spectrum detection, and the results are shown in table 1 below:
TABLE 1 EDS detection results of suspected and Normal regions
For suspected region position 1: delta= -5.5 ℃ is more than or equal to-9.27 ℃, namely T β1 =897-5.5= 891.5 ℃. In this case, the formula (2) can be written as the formula (4):
P α ＝-0.459×(T-T β0 )-4.74 (4)
fig. 3 shows a curve represented by formula (4), which is located on the right side of the curve represented by formula (3). If T=T β0 -25 is brought into formula (4), solved for, and obtained, P α ＝6.7(％)≥5(％)
For suspected region position 2: delta= -2.75 ℃ is more than or equal to-9.27 ℃, namely T β1 =897-2.75= 894.25 ℃. In this case, the formula (2) can be written as formula (5):
P α ＝-0.459×(T-T β0 )-3.48 (5)
fig. 3 shows a curve represented by formula (5), which is located on the right side of the curve represented by formula (3). If T=T β0 -25 is brought into formula (5), and the obtained, P α ＝8.0(％)≥5(％)。
According to the conclusion of the last step, the delta values of positions 1 and 2 of the suspected region are both greater than-9.27 ℃, their P α The values are also not less than 5 percent, therefore, neitherIs a beta spot defect.
3. Verification of accuracy of determination results
(1) The determination conclusion of the above embodiment was verified by the hardness test.
The hardness of the suspected region positions 1 and 2 was measured by a durometer, and the measurement results are shown in table 2:
TABLE 2
| Vickers hardness HV | Deviation from normal region | |
| Normal region | 386 | \ |
| Suspected region position 1 | 387 | 0.2％ |
| Suspected region position 2 | 392 | 1.5％ |
The hardness test showed no significant difference in hardness at positions 1 and 2 of the suspected region from the normal region. The hardness test results are consistent with the above determination that neither of the suspected region positions 1 and 2 is a beta spot defect.
(2) Compositional testing verifies the decision of the above examples:
as shown in Table 1, EDS measurements showed that the Cr element content in the suspected region positions 1 and 2 was 5.03wt% and 5.11wt%, respectively, and the Cr element content in the normal region was 5.00wt%. It can be seen that the suspected region and the normal region are at the same level of Cr element, the difference is not more than 1%, and there is no component segregation. The beta spot region and normal region Cr content, which are generally segregated, show a content difference of about 1% to 1.5% under EDS. The component test results are identical to the above determination results that the positions 1 and 2 of the suspected region are not beta-plaque defects.
Although specific embodiments of the invention have been described in detail, those skilled in the art will appreciate that: many modifications and variations of details may be made to the disclosed embodiments in light of the overall teachings of the invention and remain within its scope. The full scope of the invention is given by the appended claims and any equivalents thereof.
Claims (10)
1. A method of determining whether a near-beta titanium alloy has beta spot defects comprising the steps of:
(1) Providing a plurality of near-beta titanium alloy standard samples, carrying out heat treatment on each standard sample by adopting different heat treatment temperatures T, and collecting the percentage content P of alpha phase in each standard sample after heat treatment α Fitting P α The functional relationship with T is as follows:
P α ＝C 1 ×(T-T β0 )+C 2 ；
wherein T is β0 The beta transformation point of the standard sample is in units of ℃;
wherein C is 1 And C 2 Is a constant;
(2) Providing a near-beta titanium alloy sample to be detected, observing the microstructure of the near-beta titanium alloy sample to be detected, and judging whether a suspected region exists in the microstructure, wherein the suspected region refers to a region with the percentage content of primary alpha phase in the microstructure less than 5% and the size of more than 0.75mm in at least one direction;
if the suspected region does not exist in the microstructure, judging that the beta spot defect does not exist in the sample to be detected;
if the suspected region exists in the microstructure, executing the next step;
(3) Detecting chemical composition of suspected region and calculating beta phase transition point T corresponding to the chemical composition β1 ；
(4) Judging whether the near-beta titanium alloy has beta spot defect according to the following formula:
P α ’＝C 1 ×(T β0 -T β1 -25)+C 2 ；
if P α And (5) judging that the near-beta alloy sample to be detected does not have the beta spot defect;
if P α And if' < 5%, judging that the near-beta alloy sample to be detected has the beta spot defect.
2. The method of claim 1, the near-beta titanium alloy being a Ti17 titanium alloy.
3. The method of claim 1, the near-beta titanium alloy being a Ti17 titanium alloy, wherein
C 1 ＝-0.459，C 2 ＝-2.22。
4. The method of claim 1, the near-beta titanium alloy being a Ti17 titanium alloy, wherein T β0 ＝897℃。
5. The method of claim 1, wherein in step (1), the different heat treatment temperatures T are: at (T) β0 -30) DEG C to (T β0 -5) different heat treatment temperatures in the range of c.
6. The method of claim 1, in step (1), the heat treatment comprising: heating the sample to a heat treatment temperature T, preserving heat for 2 hours after heat penetration, cooling with water, preserving heat for 4 to 8 hours at 602 to 650 ℃, and cooling with air.
7. The method of claim 1, wherein in step (3), T β1 Obtained by calculation of the following formula:
Δ＝-19.3(Cr)-4.7(Zr)-16.8(Fe)-10.0(Mo)+23.1(Al)+154.5(O)
wherein Δ=t β1 -T β0
Wherein, (Cr) =P Cr1 -P Cr0 ，P Cr1 The weight percentage of Cr element and P in the suspected region of the sample to be detected Cr0 The weight percentage of Cr element in the standard sample is the same as that of other elements.
8. The method of claim 1, wherein the suspected region is a region having a percentage of primary alpha phase of less than 5% and a dimension of 0.75mm or more in two directions, the two directions being a first direction and a second direction perpendicular to each other.
9. The method according to claim 1, wherein the standard sample of the titanium alloy and the sample to be measured of the titanium alloy are produced and obtained by smelting furnaces with the same furnace number.
10. The method of claim 1, the near-beta titanium alloy being a Ti17 titanium alloy, the titanium alloy standard sample comprising the following alloying elements:
Al 4.5～5.5wt％，Sn 1.5～2.5wt％，Zr 1.5～2.5wt％，Mo 3.5～4.5wt％，Cr 3.5～4.5wt％。
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