CN102672150A - Direct control method for titanium-aluminum-niobium alloy lamellar structure - Google Patents
Direct control method for titanium-aluminum-niobium alloy lamellar structure Download PDFInfo
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Abstract
The invention discloses a direct control method for a titanium-aluminum-niobium alloy lamellar structure, and belongs to the technical field of control research of high-temperature alloy structures. The method is a control method for a titanium-aluminum alloy structure based on a full peritectic transformation process. By applying a directional solidification technology, the alloy is controlled to be subjected to full peritectic reaction by changing solidification conditions (temperature gradient G and drawing speed V), so that primary beta phase dendritic crystals are fully dissolved in a solidification process, and adverse effects which may be probably caused by the beta phase to the alloy structure are eliminated; and thus, the aim of controlling the direction of the lamellar structure is fulfilled. The method can be realized only in a normal Bridgman directional solidification system, so that the defects of complex preparation process and non-uniform components and performance in a seed crystal method are overcome; the method is a new method for directly controlling the orientation of titanium-aluminum-niobium alloy directionally solidified lamellas through a non-seed crystal method, and has great significance to improving the performance of the titanium-aluminum alloy; and the industrial application of the directionally solidified titanium-aluminum alloy is promoted.
Description
Technical field
The invention belongs to high temperature alloy organizational controls studying technological domain, relate to a kind of titanium aluminium niobium alloy lamellar structure direction-controlling method.
Background technology
Peritectic Alloy is to use engineering alloy very widely, and many important engineering materials all exist peritectic reaction in the preparation, has therefore caused researcher's very big concern.Titanium-aluminium alloy is as a kind of typical Peritectic Alloy; Have lightweight, height ratio is strong, height ratio is firm, anti-corrosion, wear-resisting, high temperature resistant and excellent advantages such as non-oxidizability; And have excellent normal temperature and a mechanical behavior under high temperature; Serviceability temperature can reach 700-900 ℃, is one of outstanding candidate's high-temperature structural material in fields such as aerospace industry, weapon industry and civilian industry.The titanium-aluminium alloy of high content of niobium receives concern widely because of it has more excellent high-temperature behavior, antioxygenic property and creep-resistant property, and it is the titanium-aluminium alloy that future in engineering applications is arranged most.
Though titanium aluminium base alloy has the performance of more excellence, this type material has essential fragility, generally is difficult to processing, has hindered its practicability.Many scholars attempt through obtaining the oriented freezing organization of titanium-aluminium alloy, make its preferential orientation performance consistent with the carrying direction, the comprehensive mechanical property that obtains.Directional solidification (directional solidification-DS) technology is the control of hot conduction orientation when solidifying through utilization; In frozen metal and solidified melt not, set up the thermograde of specific direction; Reach control process of setting and solidification path, and the control crystal orientation, horizontal crystal boundary eliminated; Obtain the purpose of columanar structure or specific lamella direction, thereby improve other mechanical properties such as its fracture toughness, creep strength, plasticity.Directionally solidifying titanium aluminum alloy is expected to replace directional solidification nickel-base high-temperature alloy, becomes the ideal candidates material of blade of aviation engine.Control to directionally solidifying titanium aluminum alloy lamella microscopic structure has become domestic and international research focus.
The researcher mainly controls directionally solidifying titanium aluminum alloy lamellar structure direction through the seed crystal method both at home and abroad at present, and this method can be obtained the lamellar orientation many twin synthetic crystal (PST) consistent with the direction of growth.It is that the titanium aluminium foundry alloy of α phase prepares seed crystal that the seed crystal method is at first selected first solidifying phase.Solidifying phase is the α phase time in the ban; Lamellar structure preferential direction after the directional solidification is perpendicular to the direction of growth; Johnson D R is at ActaMaterialia; 45 (6): 2523-2533,1997, after cutting seed crystal piece and half-twist, carry out the seed crystal directional solidification among the Alignment of the TiAl/Ti3Al lamellar microstructure in TiAlalloys by growth from a seed material; And control high thermograde G and suitable drawing velocity V, thereby make high temperature α obtain the PST crystal with the plane configuration continued growth.The defective of this method is complicated process of preparation, the seed crystal composition usually and the foundry alloy composition to there are differences the composition and the performance that cause directional solidificating alloy inhomogeneous.In recent years, be the through engineering approaches application and development owing to solidify the mutually polynary titanium-aluminium alloy of β earlier, the researcher urgently wants directly to control the purpose that titanium-aluminium alloy directional solidification process reaches control strip layer tissue direction through non-seed crystal method both at home and abroad.
In the directional solidification process, when primary phase is the β phase time, under the lower situation of G/V ratio, nascent β meets and grows with the dendrite pattern as the titanium-aluminium alloy of Peritectic Alloy.Peritectoid α is mutually at first through peritectic reaction forming core and growing up on liquid phase and β interface mutually; Then surround β and intercept itself and the contacting of liquid phase mutually; α internal consumption β phase in opposite directions then outwards consumes liquid phase and grows up peritectoid phase transformation that Here it is; Nascent β has only part to form peritectoid phase α through metatectic transformation mutually usually, and solid-state transformed → α takes place remaining β.Dobler S etc. are at ActaMaterialia, 52 (9): 2795-2808,2004, point out among the Peritectic coupled growth, in solid-state transformed → α process, same position to β dendrite inside can produce a plurality of not coordinatioies to the α variant.And lamella α 2 and γ separate out mutually from high temperature α in full lamella titanium-aluminium alloy; So in the peritectic reaction process; If can make nascent β all change peritectoid α phase mutually into, just may eliminate the generation of the α variant of different directions, just can control its lamella direction.
Therefore; Make titanium aluminium niobium alloy that complete peritectic reaction take place through directional solidification technique; With the superior lamellar structure of obtained performance; Be the new method of directly controlling titanium-aluminium alloy directional solidification lamellar orientation, the performance that improves titanium-aluminium alloy is had very important significance, promoted the industrial applications of directionally solidifying titanium aluminum alloy.
Summary of the invention
The objective of the invention is to provides a kind of method of utilizing complete metatectic transformation effectively to control titanium aluminium niobium alloy lamellar structure direction through changing the directional solidification condition.It specifically is a kind of titanium aluminium niobium alloy lamellar structure direction-controlling method; Adopting titanium aluminium niobium alloy atomic percent is (46-53) Ti-(45-46) Al-(2-8) Nb; Carry out the control of titanium aluminium niobium alloy lamellar structure direction with common Bridgman directional solidification system; Comprise that through changing curing condition thermograde G and drawing velocity V impel titanium aluminium niobium alloy that complete peritectic reaction takes place; Make nascent β phase dendrite in process of setting, dissolved fully, thereby eliminate the purpose that its adverse effect that possibly bring alloy structure has reached control alloy sheet interlayer orientation.
The present invention carries out melting with atomic percent for the raw material of (46-53) Ti-(45-46) Al-(2-8) Nb composition; Form master alloy ingot; Cut into cylindrical alloy bar sample then and carry out directional solidification with Bridgman directional solidification system, concrete grammar is following:
(1) the titanium aluminium niobium alloy sample for said composition range carries out directional solidification, and thermograde G is 10
3K/m ~ 10
4K/m, temperature retention time is 5～15min, and drawing velocity is between 5 μ m/s～200 μ m/s; Continue pull, when the sample directional solidification growth reaches 1/2nd positions of total length, start fast quenching device sample is carried out the fast quenching processing;
(2) alloy bar that above-mentioned steps is obtained carries out the line cutting and with the correlation technique means tissue is analyzed; The growth rhythm of nascent β phase dendrite and pattern thereof and size and the Changing Pattern of volume fraction in each sample of observation analysis step (1) with the directional solidification parameter, and the Nb content of each sample is to the influence of come into being β phase dendritic growth form and characteristic; Sum up the degree that obtains each sample generation peritectic reaction at last.
Further, the scope of the thermograde G that controlled of experiment is 10
3K/m ~ 10
4K/m, the scope of drawing velocity V is 5 μ m/s～200 μ m/s.
Further; Titanium aluminium niobium alloy for special component; The i.e. alloy confirmed of some titanium aluminium niobium compositions in this scope of (46-53) Ti-(45-46) Al-(2-8) Nb; When regulating curing condition thermograde G and drawing velocity V to Al equivalent near the peritectic point composition of phasor, complete peritectic reaction can take place in alloy.
Further, be under the condition of determined value in thermograde and drawing velocity, through regulating the content of aluminium and niobium, when making alloying component, obtain complete peritectic reaction more easily for (46-53) Ti-(45-46) Al-(2-8) Nb alloy near peritectic point.
Further, in the said step 1), continue pull, during to the 45mm extension position, sample is carried out the fast quenching processing up to the sample directional solidification growth.
It is to start the fast quenching treating apparatus that said fast quenching is handled, and sample moment is drawn in the gallium indium cooling fluid, is a kind of method for rapid cooling, and purpose is in order to keep the solid liquid interface of high temperature.
Said step (1) is to reach 10 when vacuum
-3Pa ~ 10
-4After the Pa, feed inert protective gas make vacuum reach-0.07～-0.05MPa, send electrical heating subsequently, raise the temperature to and carry out under the above condition of titanium-aluminium alloy fusing point.
Further, said step (1) is to reach 5x10 when vacuum
-3Behind the Pa, feed the protective gas high-purity argon gas make vacuum reach-0.07～-0.05MPa, send electrical heating subsequently, raise the temperature to and carry out under the above condition of titanium-aluminium alloy fusing point.
Correlation technique means in the said step 2 are some microscopic examination methods; For example the backscattered electron pattern (BSE) of light microscope (OM) and ESEM (SEM) to solidify earlier β mutually dendrite analyze; Utilize an emission Electronic Speculum (FEM) to analyze the hand down direction of growth and of a quench zone peritectoid perpendicular to the growing state on the directional solidification direction; Utilize the changes in distribution rule of each element in electron probe (EPMA) the analysis package crystalline phase change process; Adopt transmission electron microscope (TEM) to analyze phase structure, adopt the grain size and the crystal orientation of EBSD (EBSD) technical Analysis peritectoid phase transition process, X-ray energy spectrum (EDS) is analyzed phase constituent; X-ray diffraction (XRD) carries out facies analysis, utilizes the high Nb-TiAl alloy sheet interlayer of OM and SEM check directional solidification tissue.Further; Said method is that atomic percent is carried out melting for the raw material of (46-53) Ti-(45-46) Al-(2-8) Nb composition; Form master alloy ingot, the alloy bar sample that cuts into Φ (6-10) x100mm then carries out directional solidification with Bridgman directional solidification system.
In the said step (1) the sample Microstructure characteristics being carried out observation analysis finds: (1) part sample sees that the β that has in various degree is inclined to one side in backscattered electron microscopically room temperature texture; The lamella direction and the direction of growth exist the angle number more; β dendrite does not have the complete reaction fusion in this explanation process of setting; In solid-state phase changes subsequently, cause the generation of a plurality of α variants, promptly complete peritectic reaction does not take place in sample, and the alloy sheet interlayer orientation fails to be effectively controlled.(2) quite a spot of β segregation is only arranged in the minority sample, this explanation has only the not dissolving when high temperature of a spot of nascent β phase dendrite, and approximate complete peritectic reaction has taken place alloy.(3) individual sample can't see the β segregation at normal temperatures, and there are the angle minimum number in the lamella direction and the direction of growth, and complete peritectic reaction has taken place this explanation sample, has effectively controlled titanium aluminium niobium alloy lamellar structure direction.This shows under the identical situation of sample constituents and solidify parameter, can impel alloy that complete peritectic reaction takes place, reach the purpose that control lamella structure optimization alloy structure improves material property through suitable adjustment.
In the said step (2) the sample microstructure compared and find also to have eliminated the β segregation fully for some sample, complete peritectic reaction has taken place in alloy, and lamella has obtained effective control, has obtained PST crystal grain.Explanation is being solidified under the situation of parameter constant thus, through suitable adjustment alloying component, can impel alloy that complete peritectic reaction takes place equally, reaches the purpose of control lamella.
Characteristic part of the present invention is: with directional solidification technique control titanium aluminium niobium alloy complete peritectic reaction takes place; Control first solidifying phase β and optimize high temperature peritectoid phase α then; Reach control room temperature lamellar orientation, optimize the purpose of tissue, promote the performance of titanium-aluminium alloy in this way and expand its application.
The application takes the lead in effectively having controlled lamellar orientation through the metatectic transformation in the control directional solidification process.
Description of drawings
Fig. 1 is the normal packet crystal structure sketch in the directional solidification process for β solidifies titanium-aluminium alloy earlier.Nascent β meets and grows with the dendrite pattern.Peritectoid α is mutually at first through peritectic reaction forming core and growing up on liquid phase and β interface mutually, surrounds β then and intercepts itself and the contacting of liquid phase mutually, and α internal consumption β phase in opposite directions then outwards consumes liquid phase L and grows up.
Fig. 2 is high undercooling district quenching backscattered electron microscopic structure in the alloy directionally solidified process of the present invention.
Fig. 3 is an alloy sample directional solidification vertical section organization chart of the present invention.
Fig. 4 is an alloy sample directional solidification of the present invention cross section organization chart.
Fig. 5 is the longitudinal section micro-organization chart of Ti-46Al-5Nb alloy sample.
Fig. 6 is Ti-45Al-8Nb alloy sample lamellar structure figure.
The specific embodiment
Use plasma-arc or vacuum induction melting that atomic ratio is carried out melting for some raw alloys of (46-53) Ti-(45-46) Al-(2-8) Nb composition; And be cast into master alloy ingot; Female ingot is taken out from metal mold; Warp cutting and rough turn external peripheral surface obtain regular alloy pig, and cut the thin cylinder bar of Φ (6-10) x100mm from the edge, specimen surface is polished remove the oxide layer and the impurity on surface; The crucible of packing into then is incorporated with it in Bridgman directional solidification system of high-purity argon gas protection and carries out the directional solidification experiment.
Embodiment 1
The research composition is the alloy of Ti-46Al-5Nb (49Ti-46Al-5Nb), and typical B ridgman method is adopted in experiment, when vacuum reaches 5x10
-3Behind the Pa, feed the protective gas high-purity argon gas vacuum is reached-0.068MPa, send electrical heating subsequently, raise the temperature to more than the titanium-aluminium alloy fusing point, be incubated 8 minutes, then with the speed pull of 30 μ m/s, G=5.2 under this experiment condition * 10
3K/m when pull length is two of specimen length/for the moment, start fast quenching device, keeps the solid liquid interface form under this withdrawing rate.Cut sample from the directional solidification sample then and carry out microstructure observation; To solidifying the hand down direction of growth and analyze of β phase dendritic growth situation, quench zone peritectoid earlier perpendicular to the grain size of the growing state on the directional solidification direction, peritectoid phase transition process and crystal orientation etc.; Find that complete metatectic transformation takes place its tissue, as shown in Figure 5, complete peritectic reaction has taken place in this tissue; Lamellar orientation is controlled, and is in full accord with the direction of growth; Successfully obtained the lamellar structure oriented freezing organization parallel with the direction of growth.
Fig. 1 is the normal packet crystal structure sketch in the directional solidification process for β solidifies titanium-aluminium alloy earlier.Nascent β meets and grows with the dendrite pattern.Peritectoid α is mutually at first through peritectic reaction forming core and growing up on liquid phase and β interface mutually, surrounds β then and intercepts itself and the contacting of liquid phase mutually, and α internal consumption β phase in opposite directions then outwards consumes liquid phase L and grows up.Fig. 2 is high undercooling district quenching backscattered electron microscopic structure in the alloy directionally solidified process of the present invention.This figure shows the universal law in the process of setting.Line 1 is expressed as the position before the metatectic transformation, online 1 front and back, and primary phase β volume fraction is relatively stable; Line 2 is the center line of phase region L+ β+α, so its position should be in the metatectic transformation; After line 3 is confirmed as metatectic transformation, because the terminal point of metatectic transformation is when being defined in the liquid phase complete obiteration usually.Change because the β in the quenching process on the dendrite with the remaining β of metatectic transformation β → α can take place, cause white β to be segregated in that β is inner to be formed, so in the BSE micro-organization chart of quenching, could confirm not molten β alpha region.Fig. 3 is an alloy sample directional solidification vertical section organization chart of the present invention.The figure illustrates lamella and can cross over each dendrite and keep orientation not change, can control lamellar orientation for peritectic reaction experimental basis is provided.Fig. 4 is an alloy sample directional solidification of the present invention cross section organization chart.Still can find out lamella each crystal grain of leap and keep orientation not change from this figure.
The research composition is that Ti-45Al-8Nb (test and adopt typical B ridgman method, when vacuum reaches 5x10 for W, B by the Y) titanium-aluminium alloy of (47Ti-45Al-8Nb)
-3Behind the Pa, feed the protective gas high-purity argon gas vacuum is reached-0.06MPa, send electrical heating subsequently, raise the temperature to more than the titanium-aluminium alloy fusing point, be incubated 10 minutes, then with the speed pull of 10 μ m/s, G=3.8 under this experiment condition * 10
3K/m when pull length is two of specimen length/for the moment, start fast quenching device, keeps the solid liquid interface form under this withdrawing rate.Treat that system cools is to room temperature; Take out the processing of polishing of sample and multilist face; Cut sample from the directional solidification sample and carry out microstructure observation; To solidifying the hand down direction of growth and analyze of β phase dendritic growth situation, quench zone peritectoid earlier perpendicular to the grain size of the growing state on the directional solidification direction, peritectoid phase transition process and crystal orientation etc., find that complete metatectic transformation takes place its tissue, as shown in Figure 6; Because complete peritectic reaction has taken place in process of setting, lamellar structure has obtained better controlled.
Embodiment 3
The research composition is the titanium-aluminium alloy of Ti-46Al-2Nb (52Ti-46Al-2Nb), and typical B ridgman method is adopted in experiment, when vacuum reaches 5x10
-3Behind the Pa, feed the protective gas high-purity argon gas vacuum is reached-0.05MPa, send electrical heating subsequently, raise the temperature to more than the titanium-aluminium alloy fusing point, be incubated 15 minutes, then with the speed pull of 100 μ m/s, G=7.7 under this experiment condition * 10
3K/m when pull length is 45mm, starts fast quenching device, keeps the solid liquid interface form under this withdrawing rate.Treat that system cools is to room temperature; Take out the processing of polishing of sample and multilist face; Cut sample from the directional solidification sample and carry out microstructure observation; To solidifying the hand down direction of growth and analyze of β phase dendritic growth situation, quench zone peritectoid earlier, find that complete metatectic transformation takes place its tissue perpendicular to the grain size of the growing state on the directional solidification direction, peritectoid phase transition process and crystal orientation etc.
Embodiment 4
The research composition is the titanium-aluminium alloy of Ti-46Al-7Nb (47Ti-46Al-7Nb), and typical B ridgman method is adopted in experiment, when vacuum reaches 5x10
-3Behind the Pa, feed the protective gas high-purity argon gas make vacuum reach-0.07～-0.05MPa, send electrical heating subsequently, raise the temperature to more than the titanium-aluminium alloy fusing point, be incubated 10 minutes, then with the speed pull of 150 μ m/s, G=9.4 under this experiment condition * 10
3K/m when pull length is 45mm, starts fast quenching device, keeps the solid liquid interface form under this withdrawing rate.Treat that system cools is to room temperature; Take out the processing of polishing of sample and multilist face; Cut sample from the directional solidification sample and carry out microstructure observation; To solidifying the hand down direction of growth and analyze of β phase dendritic growth situation, quench zone peritectoid earlier, find that complete metatectic transformation takes place its tissue perpendicular to the grain size of the growing state on the directional solidification direction, peritectoid phase transition process and crystal orientation etc.
Claims (7)
1. titanium aluminium niobium alloy lamellar structure direction-controlling method; It is characterized in that: adopting titanium aluminium niobium alloy atomic percent is (46-53) Ti-(45-46) Al-(2-8) Nb; Carry out the control of titanium aluminium niobium alloy lamellar structure direction with common Bridgman directional solidification system; Comprise that through changing curing condition thermograde G and drawing velocity V impel titanium aluminium niobium alloy that complete peritectic reaction takes place; Make nascent β phase dendrite in process of setting, dissolved fully, thereby eliminate the purpose that its adverse effect that possibly bring alloy structure has reached control alloy sheet interlayer orientation.
2. method according to claim 1 is characterized in that: said titanium aluminium niobium alloy lamellar structure direction-controlling method comprises the steps:
(1) the titanium aluminium niobium alloy rod sample for said composition range carries out directional solidification, and thermograde G is 10
3K/m ~ 10
4K/m, temperature retention time is 5～15min, and drawing velocity V is between 5 μ m/s～200 μ m/s; Continue pull, when the sample directional solidification growth reaches 1/2nd positions of total length, start fast quenching device sample is carried out the fast quenching processing;
(2) alloy bar that above-mentioned steps is obtained carries out the line cutting and with the correlation technique means tissue is analyzed; The growth rhythm of nascent β phase dendrite and pattern thereof and size and the Changing Pattern of volume fraction in each sample of observation analysis step (1) with the directional solidification parameter, and the Nb content of each sample is to the influence of come into being β phase dendritic growth form and characteristic; Sum up the degree that obtains each sample generation peritectic reaction at last.
3. method according to claim 2 is characterized in that: said step (1) is to reach 10 when vacuum
-3Pa ~ 10
-4After the Pa, feed inert protective gas make vacuum reach-0.07～-0.05MPa, send electrical heating subsequently, raise the temperature to and carry out under the above condition of titanium-aluminium alloy fusing point, the scope of the thermograde G that experiment is controlled is 10
3K/m ~ 10
4K/m, the scope of drawing velocity V is 5 μ m/s～200 μ m/s.
4. according to each described method in the claim 1 ~ 3; It is characterized in that: for the titanium aluminium niobium alloy of special component; The i.e. alloy confirmed of some titanium aluminium niobium compositions in this scope of (46-53) Ti-(45-46) Al-(2-8) Nb; When regulating curing condition thermograde G and drawing velocity V to Al equivalent near the peritectic point composition of phasor, complete peritectic reaction can take place in alloy.
5. method according to claim 1 and 2; It is characterized in that: in thermograde and drawing velocity is under the condition of determined value; For the content of (46-53) Ti-(45-46) Al-(2-8) Nb alloy through adjusting aluminium and niobium; When making alloying component, obtain complete peritectic reaction more easily near peritectic point.
6. method according to claim 1 and 2 is characterized in that: in the said step 1), continue pull, during to the 45mm extension position, sample is carried out the fast quenching processing up to the sample directional solidification growth.
7. method according to claim 3 is characterized in that: said step (1) is to reach 5x10 when vacuum
-3Behind the Pa, feed the protective gas high-purity argon gas make vacuum reach-0.07～-0.05MPa, send electrical heating subsequently, raise the temperature to and carry out under the above condition of titanium-aluminium alloy fusing point.
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| PCT/CN2012/083373 WO2013170585A1 (en) | 2012-05-14 | 2012-10-23 | Direction control method of tial-nb alloys lamellar structure |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013170585A1 (en) * | 2012-05-14 | 2013-11-21 | 北京科技大学 | Direction control method of tial-nb alloys lamellar structure |
| CN103472085A (en) * | 2013-09-29 | 2013-12-25 | 哈尔滨工业大学 | Experimental equipment and experimental method for Ti-Al base alloy directional solidification under action of direct current |
| CN103969277A (en) * | 2014-04-29 | 2014-08-06 | 江苏省沙钢钢铁研究院有限公司 | Characterization method for distinguishing multi-phase sinter in hot-rolled silicon steel |
| CN104357783A (en) * | 2014-10-20 | 2015-02-18 | 中国人民解放军装甲兵工程学院 | Titanium-aluminum alloy powder material for thermal spraying and preparation method thereof |
| CN104328501B (en) * | 2014-10-09 | 2017-06-27 | 南京理工大学 | TiAl single crystal alloy with fully controllable lamellar orientation and preparation method thereof |
| JP2017536327A (en) * | 2014-10-09 | 2017-12-07 | 南京理工大学Ｎａｎｊｉｎｇ Ｕｎｉｖｅｒｓｉｔｙ Ｏｆ Ｓｃｉｅｎｃｅ Ａｎｄ Ｔｅｃｈｎｏｌｏｇｙ | Single crystal material of TiAl intermetallic compound and method for producing the same |
| CN110090942A (en) * | 2019-06-06 | 2019-08-06 | 西安建筑科技大学 | The method that the multifunctional integrated material of Fe-Al-Ta is prepared using Bridgman directional solidification technique |
| CN112071375A (en) * | 2020-06-01 | 2020-12-11 | 南京工业大学 | TiAl-based high-temperature alloy material design method |
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