CN116879287A - Evaluation method for micro-component uniformity of titanium alloy cast ingot - Google Patents
Evaluation method for micro-component uniformity of titanium alloy cast ingot Download PDFInfo
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- CN116879287A CN116879287A CN202310634499.0A CN202310634499A CN116879287A CN 116879287 A CN116879287 A CN 116879287A CN 202310634499 A CN202310634499 A CN 202310634499A CN 116879287 A CN116879287 A CN 116879287A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 52
- 238000011156 evaluation Methods 0.000 title claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 42
- 230000007797 corrosion Effects 0.000 claims abstract description 30
- 238000005260 corrosion Methods 0.000 claims abstract description 30
- 238000005204 segregation Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 15
- 238000005520 cutting process Methods 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000007689 inspection Methods 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 107
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003518 caustics Substances 0.000 claims description 12
- 239000012459 cleaning agent Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 230000007704 transition Effects 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000003746 surface roughness Effects 0.000 claims description 5
- 239000008399 tap water Substances 0.000 claims description 5
- 235000020679 tap water Nutrition 0.000 claims description 5
- 230000009466 transformation Effects 0.000 claims description 5
- 230000005856 abnormality Effects 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 5
- 208000004350 Strabismus Diseases 0.000 claims 2
- 101000686227 Homo sapiens Ras-related protein R-Ras2 Proteins 0.000 abstract description 6
- 102100025003 Ras-related protein R-Ras2 Human genes 0.000 abstract description 6
- 238000012790 confirmation Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- 238000003723 Smelting Methods 0.000 abstract 1
- 230000002159 abnormal effect Effects 0.000 abstract 1
- 238000012545 processing Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005242 forging Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- -1 TA15 Proteins 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses an evaluation method of micro-component uniformity of a titanium alloy cast ingot, which comprises the steps of sampling a sample sheet and cutting a phase-change ring test sample in an unprocessed state of the cast ingot after finished product smelting is completed, and detecting a phase-change point by a metallographic method; then carrying out heat treatment on the sample in a mode of 'low and high' nearby the phase change point; and then the scale is removed by a vehicle in a low-power mode, vertical alternate corrosion and the like are processed, finally the low-power inspection is carried out by a multi-angle observation method, and microcosmic composition confirmation is carried out on the low-power abnormal position. The evaluation method of the invention directly samples and detects on the cast ingot, which not only can evaluate slight-level micro-component segregation which cannot be evaluated in the prior art, such as cast ingot streamline, but also can realize the micro-segregation problem possibly generated in the process of predicting the cast ingot; in addition, the invention is not only applicable to titanium alloy ingots produced by any equipment, as long as the shape of the titanium alloy ingots is cylindrical, but also applicable to all titanium alloy brands, such as TA15, TC4, TC21 and the like.
Description
Technical Field
The invention belongs to the technical field of titanium alloy material processing, and particularly relates to an evaluation method for microcomponent uniformity of titanium alloy ingots, which is not only suitable for titanium alloy ingots produced by all vacuum consumable arc furnaces, but also suitable for titanium alloy ingots produced by other equipment (such as vacuum non-consumable arc furnaces, electron beam furnaces and the like) as long as the titanium alloy ingots are cylindrical in shape, and is suitable for all titanium alloy brands such as TA15, TC4, TC21 and the like
Background
Titanium and titanium alloy have excellent specific strength, specific rigidity, corrosion resistance and other performances, so that the titanium and titanium alloy is widely applied to various fields such as aerospace, conventional weapons, ships and oceanographic engineering, nuclear power and thermal power generation, chemical industry and petrochemical industry, metallurgy, construction, transportation, sports, articles for daily use and the like.
At present, common production modes of titanium and titanium alloy include vacuum consumable arc melting, cold hearth melting, electron beam melting and the like, but no matter which melting mode is used, the obtained cast ingot has micro segregation to a certain extent, and the only difference is that the degree of segregation of each element is inconsistent under different brands and different melting modes. However, actual production is hindered by various factors, and it is difficult to evaluate microscopic uniformity from the ingot.
In the prior art, in order to ensure that the microcosmic uniformity can meet the basic requirements of materials, the microcosmic component uniformity is generally evaluated under the condition of deforming titanium alloy, and common deformation modes include forging, rolling and extrusion. The evaluation mode in the prior art is to adopt heat treatment at the temperature of about 25 ℃ below the phase transition point to check whether the beta spot meets the standard or not, but the method is only applicable to some easily segregated alloys, and cannot effectively evaluate the micro-uniformity of conventional titanium alloys such as TC21, TA15, TC4 and the like, and even cannot evaluate the micro-uniformity of some specific micro-components. The reason is mainly because the beta spot is a common micro segregation in the titanium alloy, once formed, the beta spot is difficult to eliminate in the subsequent forging, extrusion, rolling and other processing processes, and various mechanical properties of the material are seriously affected, but other types of micro segregation are rarely reported. In addition, for some slight-level micro segregation, some micro segregation can be eliminated through subsequent processing, and some micro segregation can be inherited, so that the importance of the micro segregation is insufficient in the industry, and few people study how to perform characterization evaluation, particularly evaluation on cast ingots.
In view of the above, the present inventors have provided a method for evaluating the uniformity of micro-components of a titanium alloy ingot to solve the above-mentioned problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides an evaluation method for the micro-component uniformity of a titanium alloy cast ingot, which can evaluate micro-component segregation at a slight level which cannot be evaluated in the prior art, and simultaneously can realize the problem of micro-segregation possibly generated in the process of predicting the cast ingot, thereby providing effective reference for the subsequent processing technology and avoiding the processing cost and the material loss cost caused by the micro-segregation which can only be judged in a deformed state in a conventional mode.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a method for evaluating the uniformity of microcomponents of a titanium alloy cast ingot, which specifically comprises the following steps:
sampling a sample sheet in a raw state of a titanium alloy ingot, wherein the sample sheet comprises a longitudinal low-power sample sheet and a transverse low-power sample sheet;
step two, cutting a phase transformation ring test sample on the titanium alloy cast ingot, and detecting a phase transformation point by using a metallographic method;
thirdly, carrying out 'low-high-low' heat treatment on the longitudinal low-power sample piece and the transverse low-power sample piece obtained in the first step in a resistance furnace, and then discharging the materials from the furnace to cool the materials to room temperature;
fourthly, carrying out low-power treatment on the sample wafer subjected to the heat treatment in the third step to remove oxide scales generated by the heat treatment;
fifthly, carrying out low-power corrosion on the sample wafer by adopting a vertical alternate corrosion method;
step six, cleaning the corrosive on the low-power sample wafer;
step seven, performing low-power inspection by adopting a multi-angle observation method to confirm whether low-power abnormality exists; if the low power is normal, ending the evaluation flow; if there is a low-power abnormality, a high-power sample piece at a corresponding position is cut, and the high-power sample piece is observed on a high-power display device to confirm the degree of microscopic component segregation.
Further, in the first step, when the sheet is sampled, the surface of the titanium alloy cast ingot is not peeled; when a sample is specifically taken, firstly, sawing a cylinder with the thickness of more than or equal to 20mm at the head end and the tail end of a titanium alloy cast ingot to serve as a transverse low-power sample piece, and simultaneously sawing a cylinder blank with the thickness of more than or equal to 200mm, wherein the sawing skewness is less than or equal to 5mm; and sawing a longitudinal low-power sample wafer with the width of more than or equal to 20mm and the thickness of more than or equal to 200mm along the axial direction at the middle part of the cylindrical blank, wherein the sawing deflection is required to be less than or equal to 5mm. .
Further, in the second step, when the phase-change ring test sample is cut on the titanium alloy cast ingot, the sampling depth is at least 10mm.
Further, in the third step, when the sample wafer is subjected to heat treatment, a temperature-reaching and placing mode is adopted, and the heating error of the resistance furnace is required to be less than 5 ℃. The temperature reaching and placing mode means that after the temperature of the resistance furnace is raised to the target temperature, a sample wafer is placed in the furnace after the furnace is opened for heat preservation; the commonly used furnace-following heating means that the sample wafer is directly placed at room temperature or the original temperature of the furnace, and then is heated to the target temperature and then is kept warm.
The specific heat treatment process comprises the following steps: firstly, carrying out heat treatment at the temperature of 5-20 ℃ below the phase transition point for 1-2 h, then heating up to the temperature of 5-15 ℃ above the phase transition point along with a furnace, then carrying out heat treatment for 0.5-1.5 h, then cooling down to the temperature of 5-20 ℃ below the phase transition point along with the furnace, carrying out heat treatment for 1-2 h, and finally directly discharging from the furnace for water cooling to room temperature.
Further, in the fourth step, when the sample wafer is subjected to the low-power treatment, any surface is selected to be subjected to the low-power treatment, the turning depth is more than 3mm, the heat treatment oxide skin is ensured to be removed, and meanwhile, the surface roughness is controlled to be less than or equal to 3.2 mu m, so that the low-power tissue can be conveniently observed. .
Further, in the step five, when the sample wafer is corroded, the adopted corrosive agent is formed by mixing hydrofluoric acid, nitric acid and water, and the volume ratio of the hydrofluoric acid to the nitric acid is as follows: nitric acid: water=1:1:3;
the whole corrosion process is carried out for 4 times, specifically, the 1 st time and the 3 rd time are corroded along the direction parallel to the length direction of the ingot, all positions are guaranteed to be uniformly covered with corrosive agents, the 2 nd time and the 4 th time are corroded along the direction perpendicular to the length direction of the ingot, all positions are guaranteed to be uniformly covered with corrosive agents, and each time of corrosion is completed for 1min, and the method is used for corrosion reaction.
Further, in the step six, when the low-power sample wafer is cleaned, the cleaning agent adopts tap water, and the cleaning of all areas of the low-power surface is gradually carried out by using a laminar cooling mode, wherein the cleaning time is at least 5min, so that the residual acid liquid is thoroughly removed; and after the cleaning is finished, the cleaning agent is uniformly dried by high-pressure air, so that no residual cleaning agent is ensured for the low-power sample wafer.
Further, the multiple angles in the seventh step are five angles, which are respectively a top view angle of the sample wafer, a vertical 45 ℃ oblique view angle of the sample wafer and a left and right 45 ℃ oblique view angle of the sample wafer.
Further, the high power display device in the seventh step is a high power scanning electron microscope or a transmission electron microscope or an electron probe microscope.
Further, the titanium alloy ingot is cylindrical in shape.
Compared with the prior art, the invention has the following beneficial effects:
the invention relates to an evaluation method for micro-component uniformity of a titanium alloy ingot, which comprises the steps of directly carrying out sampling detection on the ingot, observing the whole original appearance of the ingot without peeling during evaluation, carrying out low-high heat treatment on the sample, fully utilizing titanium alloy phase transformation to further eliminate other interference factors, confirming component inheritance instead of tissue inheritance, and adopting a corrosion technology not only to evaluate micro-component segregation which cannot be evaluated in the prior art, such as an ingot streamline, but also to realize the problem of micro-segregation possibly generated in the process of predicting the ingot. Compared with the prior art, the method has the advantages that the microcomponent uniformity is required to be evaluated under the deformed titanium alloy, the material cost and the production and processing cost can be greatly saved, and the method can provide basis for subsequent processing processes, such as a high-temperature homogenization process, a forging process, a rolling process and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate principles of the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to a person skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a flow chart of an evaluation method of micro-component uniformity of a titanium alloy ingot according to the invention;
FIG. 2 is a schematic diagram of the process of taking a longitudinal low-power sample and a transverse low-power sample from the head and the tail of a titanium alloy ingot according to the embodiment 1 of the invention;
FIG. 3 is a tail portion real object diagram of the low-power evaluation result (cast ingot streamline) of the embodiment 1-TA15 of the invention;
FIG. 4 is a diagram showing the tail portion of the low-power evaluation result (flow line of ingot) of example 2-TC21 of the present invention;
FIG. 5 is a graph showing the low-power evaluation results (normal) of the tail portion of examples 3 to TC4 according to the present invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are not intended to represent all embodiments consistent with the invention. Rather, they are merely examples of devices that are consistent with aspects of the invention that are set forth in the following claims.
The present invention will be described in further detail with reference to examples for better understanding of the technical aspects of the present invention by those skilled in the art.
Example 1 (evaluation of micro-composition uniformity of TA15 titanium alloy ingot)
1) And sawing a sample piece with the thickness of 20mm and 200mm at the head part and the tail part of the TA15 cast ingot with the specification of phi 720, wherein the sawing deflection is less than or equal to 5mm. Wherein two samples with the specification of phi 720mm x 20mm are used as transverse low-power sample pieces; and the two cylindrical sample pieces with the specification of phi 720mm and 200mm are longitudinally cut along the diameter position of the circular section respectively, and the longitudinal low-power sample pieces with the specification of 720mm and 200mm and 20mm (length and thickness (height) and width, wherein the thickness is parallel to the axis of an ingot) are cut, and the sawing skewness of the longitudinal cutting is less than or equal to 5mm, as shown in figure 2.
2) And cutting a phase-change ring test sample from the residual material of the longitudinal section of the ingot, and measuring the phase-change point of the ingot to 990 ℃ by using a metallographic method.
3) Heating the resistance heating furnace to 970 ℃, and heating the four sample pieces (comprising two transverse low-power sample pieces with the specification of phi 720mm by 20mm; two longitudinal low-power sample sheets with the specification of 720mm and 200mm and 20 mm) are placed into a heating furnace, and are kept for 2 hours; then the temperature of the heating furnace is raised to 1005 ℃, and the temperature is kept for 1.5h; then the temperature of the heating furnace is reduced to 970 ℃, and the temperature is kept for 2 hours; finally, taking the sample out of the furnace, and directly quenching in a water tank until the temperature is reduced to room temperature.
4) And (3) carrying out turning low-power treatment on the sample wafer cooled to room temperature, wherein the turning depth is more than 3mm, so that the removal of heat-treated oxide skin is ensured, and meanwhile, the surface roughness is controlled to be less than or equal to 3.2 mu m, so that the observation of low-power tissues is facilitated.
5) The corrosive agent is adopted (the corrosive agent is formed by mixing hydrofluoric acid, nitric acid and water, and the volume ratio of the hydrofluoric acid to the nitric acid is: nitric acid: water=1:1:3), the whole corrosion process is performed for 4 times, specifically, the 1 st and 3 rd times are corroded along the direction parallel to the length direction of the ingot, the corrosion agent is uniformly covered at all positions, the 2 nd and 4 th times are corroded along the direction perpendicular to the length direction of the ingot, the corrosion agent is uniformly covered at all positions, and each time of corrosion is completed for 1min, so that the corrosion reaction is performed.
6) Cleaning agent (tap water) is adopted, and a laminar cooling mode is utilized to gradually clean all areas of the low-power sample, wherein the cleaning time lasts for at least 5min, so that the residual acid liquid is thoroughly removed; and after the cleaning is finished, the cleaning is uniformly dried by high-pressure air, and the purging time is at least 5min, so that no residual cleaning agent is ensured for the low-power sample.
7) The samples were observed low power. The sample is subjected to low-power observation according to the overlooking angle of the sample, the up-down 45 ℃ squinting angle of the sample and the left-right 45 ℃ squinting angle of the sample, and the result is that: the head samples were all normal, and cast ingot streamlines were observed only in the tail longitudinal section samples, as shown in fig. 3.
8) Microcomponent identification. Taking a high-power sample of the streamline position of the cast ingot, carrying out tissue and component confirmation by using a high-power scanning electron microscope after sample grinding, polishing and corrosion, and the results are shown in the following table 1:
TABLE 1 TA15 ingot streamline position Spectrum microcomponent results
Example 2 (evaluation of micro-composition uniformity of TC21 titanium alloy ingot)
1) And sawing a sample piece with the thickness of 30mm and 100mm at the head part and the tail part of the TC21 cast ingot with the specification phi 720, wherein the sawing deflection is less than or equal to 5mm. Wherein two samples with the specification of phi 720mm and 30mm are taken as transverse low-power sample sheets; and the two cylindrical sample sheets with the specification phi 720mm and 100mm are longitudinally cut along the diameter position of the circular section respectively, and the longitudinal low-power sample sheets with the specification phi 720mm and 30mm (length and thickness (height) and width, wherein the thickness is parallel to the axis of the ingot) are cut, and the longitudinally cut sawing deviation is less than or equal to 5mm, similar to the sawing mode shown in fig. 2.
2) And cutting a phase-change ring test sample from the residual material of the longitudinal section of the ingot, and measuring the phase-change point of the ingot to 960 ℃ by using a metallographic method.
3) Heating the resistance heating furnace to 950 ℃, and heating the four sample plates (comprising two transverse low-power sample plates with the specification of phi 720mm and 30mm; two longitudinal low-power sample sheets with the specification of 720mm and 100mm and 30 mm) are placed into a heating furnace, and the temperature is kept for 1.5h; then the temperature of the heating furnace is raised to 970 ℃, and the temperature is kept for 1.0h; then the temperature of the heating furnace is reduced to 950 ℃, and the temperature is kept for 1.0h; finally, taking the sample out of the furnace, and directly quenching in a water tank until the temperature is reduced to room temperature.
4) And (3) carrying out turning low-power treatment on the sample wafer cooled to room temperature, wherein the turning depth is more than 3mm, so that the removal of heat-treated oxide skin is ensured, and meanwhile, the surface roughness is controlled to be less than or equal to 3.2 mu m, so that the observation of low-power tissues is facilitated.
5) The corrosive agent is adopted (the corrosive agent is formed by mixing hydrofluoric acid, nitric acid and water, and the volume ratio of the hydrofluoric acid to the nitric acid is: nitric acid: water=1:1:3), the whole corrosion process is performed for 4 times, specifically, the 1 st and 3 rd times are corroded along the direction parallel to the length direction of the ingot, the corrosion agent is uniformly covered at all positions, the 2 nd and 4 th times are corroded along the direction perpendicular to the length direction of the ingot, the corrosion agent is uniformly covered at all positions, and each time of corrosion is completed for 1min, so that the corrosion reaction is performed.
6) Cleaning agent (tap water) is adopted, and a laminar cooling mode is utilized to gradually clean all areas of the low-power sample, wherein the cleaning time lasts for at least 5min, so that the residual acid liquid is thoroughly removed; and after the cleaning is finished, the cleaning is uniformly dried by high-pressure air, and the purging time is at least 5min, so that no residual cleaning agent is ensured for the low-power sample.
7) The samples were observed low power. The sample is subjected to low-power observation according to the overlooking angle of the sample, the up-down 45 ℃ squinting angle of the sample and the left-right 45 ℃ squinting angle of the sample, and the result is that: the head samples were all normal, and cast ingot streamlines were observed only in the tail longitudinal section samples, as shown in fig. 4.
8) Microcomponent identification. Taking a high-power sample of the streamline position of the cast ingot, carrying out tissue and component confirmation by using a high-power scanning electron microscope after sample grinding, polishing and corrosion, and the results are shown in the following table 2:
TABLE 2 energy spectrum microcomponent results for the streamline position of TC21 ingots
Example 3 (evaluation of micro-composition uniformity of TC4 titanium alloy ingot)
1) And sawing a sample piece with the thickness of 30mm and 300mm at the head part and the tail part of the TC4 cast ingot with the specification of phi 920, wherein the sawing deflection is less than or equal to 5mm. Wherein two samples with the specification of phi 920mm are taken as transverse low-power sample sheets; and the two cylindrical sample pieces with the specification phi 920mm are longitudinally cut along the diameter position of the circular section respectively, and the longitudinal low-power sample pieces with the specification phi 920mm, 300mm, 30mm (length, thickness (height), width, thickness which is parallel to the axis of the ingot) are cut, wherein the inclination of longitudinally cut saw cutting is less than or equal to 5mm, and the saw cutting mode is similar to that shown in fig. 2.
2) And cutting a phase change test sample from the residual material of the longitudinal section of the ingot, and measuring the phase change point of the ingot to be 1000 ℃ by using a metallographic method.
3) Heating a resistance heating furnace to 995 ℃, and heating the four sample plates (comprising two transverse low-power sample plates with the specification of phi 920mm by 30mm; two longitudinal low-power sample sheets with the specification of 920mm, 300mm and 30 mm) are placed into a heating furnace, and the temperature is kept for 1.0h; then the temperature of the heating furnace is raised to 1005 ℃, and the temperature is kept for 0.5h; then the temperature of the heating furnace is reduced to 995 ℃ and the temperature is kept for 2 hours; finally, taking the sample out of the furnace, and directly quenching in a water tank until the temperature is reduced to room temperature.
4) And (3) carrying out turning low-power treatment on the sample wafer cooled to room temperature, wherein the turning depth is more than 3mm, so that the removal of heat-treated oxide skin is ensured, and meanwhile, the surface roughness is controlled to be less than or equal to 3.2 mu m, so that the observation of low-power tissues is facilitated.
5) The corrosive agent is adopted (the corrosive agent is formed by mixing hydrofluoric acid, nitric acid and water, and the volume ratio of the hydrofluoric acid to the nitric acid is: nitric acid: water=1:1:3), the whole corrosion process is performed for 4 times, specifically, the 1 st and 3 rd times are corroded along the direction parallel to the length direction of the ingot, the corrosion agent is uniformly covered at all positions, the 2 nd and 4 th times are corroded along the direction perpendicular to the length direction of the ingot, the corrosion agent is uniformly covered at all positions, and each time of corrosion is completed for 1min, so that the corrosion reaction is performed.
6) Cleaning agent (tap water) is adopted, and a laminar cooling mode is utilized to gradually clean all areas of the low-power sample, wherein the cleaning time lasts for at least 5min, so that the residual acid liquid is thoroughly removed; and after the cleaning is finished, the cleaning is uniformly dried by high-pressure air, and the purging time is at least 5min, so that no residual cleaning agent is ensured for the low-power sample.
7) The samples were observed low power. The sample is subjected to low-power observation according to the overlooking angle of the sample, the up-down 45 ℃ squinting angle of the sample and the left-right 45 ℃ squinting angle of the sample, and the result is that: the low power is normal without high power confirmation, as shown in fig. 5.
The foregoing is only a specific embodiment of the invention to enable those skilled in the art to understand or practice the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
It will be understood that the invention is not limited to what has been described above and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (10)
1. The evaluation method for the micro-ingredient uniformity of the titanium alloy cast ingot is characterized by specifically comprising the following steps of:
sampling a sample sheet in a raw state of a titanium alloy ingot, wherein the sample sheet comprises a longitudinal low-power sample sheet and a transverse low-power sample sheet;
step two, cutting a phase transformation ring test sample on the titanium alloy cast ingot, and detecting a phase transformation point by using a metallographic method;
thirdly, carrying out 'low-high-low' heat treatment on the longitudinal low-power sample piece and the transverse low-power sample piece obtained in the first step in a resistance furnace, and then discharging the materials from the furnace to cool the materials to room temperature;
fourthly, carrying out low-power treatment on the sample wafer subjected to the heat treatment in the third step to remove oxide scales generated by the heat treatment;
fifthly, carrying out low-power corrosion on the sample wafer by adopting a vertical alternate corrosion method;
step six, cleaning the corrosive on the low-power sample wafer;
step seven, performing low-power inspection by adopting a multi-angle observation method to confirm whether low-power abnormality exists; if the low power is normal, ending the evaluation flow; if there is a low-power abnormality, a high-power sample piece at a corresponding position is cut, and the high-power sample piece is observed on a high-power display device to confirm the degree of microscopic component segregation.
2. The method for evaluating the micro-component uniformity of a titanium alloy ingot according to claim 1, wherein in the first step, the surface of the titanium alloy ingot is not peeled off during the sampling of the sheet;
when a sample is specifically taken, firstly, sawing a cylinder with the thickness of more than or equal to 20mm at the head end and the tail end of a titanium alloy cast ingot to serve as a transverse low-power sample piece, and simultaneously sawing a cylinder blank with the thickness of more than or equal to 200mm, wherein the sawing skewness is less than or equal to 5mm; and sawing a longitudinal low-power sample wafer with the width of more than or equal to 20mm and the thickness of more than or equal to 200mm along the axial direction at the middle part of the cylindrical blank, wherein the sawing deflection is required to be less than or equal to 5mm.
3. The method for evaluating the micro-component uniformity of a titanium alloy ingot according to claim 1, wherein the sampling depth is at least 10mm when the phase-change ring test sample is cut from the titanium alloy ingot in the second step.
4. The method for evaluating the micro-ingredient uniformity of a titanium alloy ingot according to claim 1, wherein in the third step, when a sample is subjected to heat treatment, a temperature-reaching and placing mode is adopted, and a heating error of a resistance furnace is required to be less than 5 ℃;
the specific heat treatment process comprises the following steps: firstly, carrying out heat treatment at the temperature of 5-20 ℃ below the phase transition point for 1-2 h, then heating up to the temperature of 5-15 ℃ above the phase transition point along with a furnace, then carrying out heat treatment for 0.5-1.5 h, then cooling down to the temperature of 5-20 ℃ below the phase transition point along with the furnace, carrying out heat treatment for 1-2 h, and finally directly discharging from the furnace for water cooling to room temperature.
5. The method for evaluating the micro-component uniformity of the titanium alloy cast ingot according to claim 1, wherein in the fourth step, when the sample wafer is subjected to the low-power treatment, any surface is selected to be subjected to the low-power treatment, the turning depth is more than 3mm, the heat treatment oxide skin is ensured to be removed, and meanwhile, the surface roughness is controlled to be less than or equal to 3.2 mu m, so that the observation of the low-power tissue is facilitated.
6. The method for evaluating the micro-component uniformity of a titanium alloy ingot according to claim 1, wherein in the fifth step, when a sample is corroded, the adopted corrosive agent is formed by mixing hydrofluoric acid, nitric acid and water, and the volume ratio of the hydrofluoric acid to the nitric acid is: nitric acid: water=1:1:3;
the whole corrosion process is carried out for 4 times, specifically, the 1 st time and the 3 rd time are corroded along the direction parallel to the length direction of the ingot, all positions are guaranteed to be uniformly covered with corrosive agents, the 2 nd time and the 4 th time are corroded along the direction perpendicular to the length direction of the ingot, all positions are guaranteed to be uniformly covered with corrosive agents, and each time of corrosion is completed for 1min, and the method is used for corrosion reaction.
7. The method for evaluating the micro-ingredient uniformity of the titanium alloy cast ingot according to claim 1, wherein in the step six, when the low-power sample wafer is cleaned, tap water is adopted as a cleaning agent, and a laminar cooling mode is utilized to gradually clean all areas of the low-power surface, wherein the cleaning time is at least 5min, so that the residual acid liquid is completely removed; and after the cleaning is finished, the cleaning agent is uniformly dried by high-pressure air, so that no residual cleaning agent is ensured for the low-power sample wafer.
8. The method for evaluating the uniformity of micro-ingredients of a titanium alloy ingot according to claim 1, wherein the multi-angles in the seventh step are five angles, namely a top view angle of a sample wafer, a top and bottom 45 ℃ strabismus angle of the sample wafer and a left and right 45 ℃ strabismus angle of the sample wafer.
9. The method for evaluating the uniformity of micro components of a titanium alloy ingot according to claim 1, wherein the high power display device in the seventh step is a high power scanning electron microscope or a transmission electron microscope or an electron probe microscope.
10. The method for evaluating the uniformity of micro-ingredients of a titanium alloy ingot according to any one of claims 1 to 9, wherein the titanium alloy ingot is cylindrical in shape.
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| CN117949278A (en) * | 2024-03-26 | 2024-04-30 | 有研工程技术研究院有限公司 | Method for evaluating homogenization effect of 7xxx series aluminum alloy cast ingot |
| CN119413548A (en) * | 2024-09-29 | 2025-02-11 | 重庆金世利航空材料有限公司 | A method for evaluating the composition uniformity of titanium alloy ingots |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117949278A (en) * | 2024-03-26 | 2024-04-30 | 有研工程技术研究院有限公司 | Method for evaluating homogenization effect of 7xxx series aluminum alloy cast ingot |
| CN119413548A (en) * | 2024-09-29 | 2025-02-11 | 重庆金世利航空材料有限公司 | A method for evaluating the composition uniformity of titanium alloy ingots |
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