CN109536883A - A kind of antioxidative method of raising Ti-45Al-8.5Nb alloy high-temp - Google Patents
A kind of antioxidative method of raising Ti-45Al-8.5Nb alloy high-temp Download PDFInfo
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Abstract
A kind of antioxidative method of raising Ti-45Al-8.5Nb alloy high-temp, belongs to Ti-Al alloy material field of surface modification, the method for being related to preparing high temperature oxidation resistance coating on titanium-aluminium alloy surface with sufacing.This method is to improve its inoxidizability by coating one layer of crome metal (Cr) coating in Ti-45Al-8.5Nb alloy surface.Ti-45Al-8.5Nb alloy will be prepared and place furnace for double-layer metallic glow ion cementation, using Cr plate as supply source, metallic cementation duration 1-3 h, temperature is 800 DEG C -1000 DEG C, by adjusting metallic cementation temperature and time, change coating layer thickness and the binding ability with Ti-45Al-8.5Nb alloy, obtains the coating being firmly combined with Ti-45Al-8.5Nb alloy.The Ti-45Al-8.5Nb alloy of coating will be made in 900 DEG C of progress isothermal oxidation weight gains the experimental results showed that, when Cr coating oxidation of alloy surface, forms the Cr of a large amount of densifications2O3Protective film results in oxidation weight gain rate significantly lower than not having cated alloy.Therefore, this method can effectively improve Ti-45Al-8.5Nb alloy high-temp inoxidizability, be of great significance to titanium aluminium niobium alloy industrial applications.
Description
Technical field
The invention belongs to titanium-aluminium alloy field of surface modification, it is related to improving titanium-aluminium alloy by surface protection coating technology
High-temperature oxidation resistance method.
Background technique
With industrial development, titanium-aluminium alloy in light alloy has a low-density, high specific strength, high elastic modulus and
The excellent mechanical property such as high creep-resistant property, is widely used in all trades and professions.Wherein there are many machine components and electronics
The working environment of device is very harsh, usually high temperature, high speed, high pressure, heavy duty, the environment such as deep-etching, it is therefore desirable to improve element
The performances such as the wearability of substrate material surface, heat resistance, corrosion resistance and fatigue resistance.To being added in common titanium-aluminium alloy
Suitable niobium (Nb) element, intensity, creep resistance, high-temperature oxidation resistance etc. are optimized.In aerospace field high temperature
Under operating condition, other than needing titanium-aluminium alloy that there is good comprehensive mechanical property, it is also necessary to which titanium-aluminium alloy has higher
Antioxygenic property.Under the high temperature conditions, the Al of formation2O3And TiO2Standard Gibbs free energy very close to therefore not can be carried out
The preferential oxidation of Al can form Al on surface2O3And TiO2Mixed layer, wherein TiO2It is loose porous, cause oxygen atom to spread rapidly
Into alloy substrate, its oxidation resistance can be reduced rapidly under the high temperature conditions.Therefore, the height of lightweight titanium-aluminium alloy how is improved
Warm inoxidizability obtains extensive concern.
Currently, the high-temperature oxidation resistance of raising titanium-aluminium alloy is broadly divided into two methods.The first is alloying, including
Multi-element alloyed and infinitesimal alloying, common multi-element alloyed member, which is known as W, Mo, Cr, Si, Nb etc. and microelement, Zr, Y
Deng the addition elements such as W, Mo can reduce the diffusion rate of Ti, inhibit TiO2Formation, promote Al2O3Formation；Addition is a small amount of
Zr and Y element, the adhesiveness of oxidation film can be improved.University of Science & Technology, Beijing exploitation Ti- (42-45) Al- (0-4) (Cr, Mn,
V)-(5-10) (Nb, Ta, Mo)-(0-1) (W, Si, C, B) alloy shows excellent high-temperature oxidation resistance.But pass through alloy
Change improve titanium-aluminium alloy high-temperature oxidation resistance can the mechanical properties such as toughness, intensity to titanium-aluminium alloy bring detrimental effect.
The antioxidative method of second of improvement titanium-aluminium alloy is process for modifying surface, including surface alloying and surface covering.Table
It is divided into ion implanting, diffusion infiltration, chemical surface treatment etc. inside surface alloying again.Research find to titanium-aluminium alloy surface by from
The elements such as son injection Nb+Al, Nb+C or Nb+Si pass through diffusion carburizing or silicon etc., and the high temperature antioxygen of titanium-aluminium alloy can be improved
The property changed, but the depth of ion implanting and constituent content are limited, and alloying layer thickness and the high temperature internal oxidition for spreading carburizing are not easy to control,
Therefore their high-temperature oxidation resistance is limited.Lacquer systems include NiCrAlY, TiAlCr coating system, TiAl base
Coating, ceramic coating etc..Research shows that TiAl3Coating, ceramic coating etc. significantly improve the high-temperature oxidation resistance of titanium-aluminium alloy,
But occur between coating and substrate combinating strength, coating and matrix it is different degrees of react and counterdiffusion be still there are the problem of.
Therefore depending merely on alloying material or depend merely on sufacing is that can not solve our problems faceds.
Under the overall background of current scientific and technological high speed development, the engine power in aerospace field is increasing, work
Temperature is also higher and higher, for traditional titanium-aluminium alloy metallic cementation, to the metallic cementation chromium of titanium-aluminium alloy containing Nb
It (Cr) is a kind of antioxidative new method of raising.And double glow plasma surface alloying technique has the advantages that its uniqueness.Metal from
It will form thicker alloy-layer when son diffusion, the tenor of alloy-layer is gradual change, has gradient, with coating, film is compared
It is stronger in conjunction with matrix, it is not easily to fall off；There is the ion of high-speed mobile in glow discharging process, meeting striking work surface makes gold
Workpiece surface can preferably be goed deep by belonging to ion；Double glow plasma surface alloying technique use scope is wide, metallic cementation material, temperature,
The parameters such as time are all adjustable, can control coating material and coating layer thickness, infiltration layer form etc. by adjusting these parameters；From environment
Technology is nontoxic for angle, free from environmental pollution.By improving the presence of alloy high-temp inoxidizability to Cr is added in titanium-aluminium alloy
Some problems, the Cr content of addition can promote Ti in oxidation film (Cr, Al) when being greater than 7%2 The formation of Laves phase, to alloy
Toughness is unfavorable, can promote TiO when Cr content is less than 4%2It is formed, it is unfavorable to alloy inoxidizability.But Cr can be formed at high temperature
Compare Al2O3Finer and close Cr2O3Oxidation film, its thermostabilization and chemical property are also very stable.Therefore pass through dual-layer glow ion skill
Art seeps Cr to Ti-45Al-8.5Nb alloy surface, and Cr coating is made to form fine and close Cr at high temperature2O3Protective film can be used as one
Kind improves the new method of titanium-aluminium alloy high-temperature oxidation resistance.
Summary of the invention
The object of the present invention is to provide a kind of high temperature for improving titanium-aluminium alloy using double glow plasma surface alloying technique is anti-
The method of oxidisability.Combination between the metal infiltration layer and matrix of technology preparation belongs to metallurgical bonding, coating and Ti-45Al-
8.5Nb alloy combines the lofty interface of no performance, and in conjunction with more secured, coating metal content is gradual change, chemical property
It is more stable.Ti-45Al-8.5Nb alloy forms fine and close Cr in alloy surface in 900 DEG C of long-time isothermal oxidations2O3Oxygen
Change film, oxidation weight gain rate is also significantly lower than when not doing coating as a result, effectively raising the high-temperature oxidation resistance of alloy.Its
Specific process step are as follows:
(1), use vacuum arc furnace melting at matter high purity Ti (> 99.99%), Al (> 99.95%), Nb (> 99.95%)
The titanium-aluminium alloy that score is Ti-45Al-8.5Nb is measured, is then cast as alloy pig with copper mold；
(2), alloy pig is cut into the square alloy sample that size is 10 × 10 × 5mm with wire cutting, and will be closed with SiC sand paper
Golden sample surrounding is polishing to 2000# from 600#, is put into ultrasonic wave to be cleaned with alcohol and dry, does for double-layer metallic glow ion cementation
Prepare；
(3), Ti-45Al-8.5Nb metallic cementation Cr is given by double glow plasma surface alloying technique.Used equipment is
Furnace for double-layer metallic glow ion cementation is placed into sample in double-deck glow metal leakage furnace, and is 99.99% to purity is filled in furnace
Argon gas；
(4), metallic cementation duration 1-3h is set, and temperature is 800 DEG C -1000 DEG C, obtains the coating of different shape；
(5), cated Ti-45Al-8.5Nb alloy and cated Ti-45Al-8.5Nb alloy will not be had to be put into togerther 900 DEG C
High temperature furnace carry out isothermal oxidation, record weight gain quality calculates oxidation weight gain curve, with the object phase composition of XRD characterization oxidation film,
With the micromorphology of SEM observation oxidation film；
(6), oxidation weight gain curve, oxide form are analyzed, research show that cated alloy high-temp inoxidizability obtains obviously
Improve.
The metallic cementation source electrode that the present invention narrates is Cr plate, when metallic cementation a length of 1-3h, temperature is 800 DEG C -1000 DEG C.
The advantage of the invention is that the tenor of metallic cementation layer has gradient, coating and Ti-45Al-8.5Nb alloy
Between combine stronger, stable chemical performance.It adjusts metallic cementation temperature and duration, available different-thickness, different metal contains
The coating of amount.Cr is seeped in alloy surface, is not had a significant impact to the mechanical property of alloy.Cr2O3Oxidation film it is fine and close, growth
Speed is slow, and performance is more stable, and Cr element also has a significant impact to heat erosion, therefore metallic cementation source electrode is selected as Cr.It is this
New method is safe from harm to environment, and technical operation is simple, can also save preparation cost.
Detailed description of the invention
Cross Section Morphology after 800 DEG C of double-layer glow ion penetration Cr of Fig. 1；
Oxidizing dynamics curve of Fig. 2 Ti-45Al-8.5Nb in 900 DEG C of isothermal oxidation 90h；
800 DEG C of Fig. 3 seep Cr alloy in the oxidizing dynamics curve of 900 DEG C of isothermal oxidation 90h；
800 DEG C of Fig. 4 seep the XRD spectrum that Cr alloy aoxidizes 90h at 900 DEG C；
Fig. 5 Ti-45Al-8.5Nb aoxidizes the microscopic appearance of sample surfaces after 90h；
The microscopic appearance of sample surfaces after 800 DEG C of Fig. 6 infiltration Cr alloy oxidation 90h；
The oxidizing dynamics curve of Fig. 7 Ti-45Al-8.5Nb alloy isothermal oxidation 300h；
800 DEG C of Fig. 8 seep Cr alloy in the oxidizing dynamics curve of 900 DEG C of isothermal oxidation 300h；
800 DEG C of Fig. 9 seep the XRD spectrum that Cr alloy aoxidizes 300h at 900 DEG C；
Figure 10 Ti-45Al-8.5Nb aoxidizes the microscopic appearance of sample surfaces after 300h；
The microscopic appearance of sample surfaces after 800 DEG C of Figure 11 infiltration Cr alloy oxidation 300h；
Cross Section Morphology after 1000 DEG C of double-layer glow ion penetration Cr of Figure 12；
The oxidizing dynamics curve of 1000 DEG C of Figure 13 infiltration Cr alloy isothermal oxidation 90h；
1000 DEG C of Figure 14 seep the XRD spectrum that Cr alloy aoxidizes 90h at 900 DEG C；
The microscopic appearance of sample surfaces after 1000 DEG C of Figure 15 infiltration Cr alloy oxidation 90h；
The oxidizing dynamics curve of 1000 DEG C of Figure 16 infiltration Cr alloy isothermal oxidation 300h；
1000 DEG C of Figure 17 seep the XRD spectrum that Cr alloy aoxidizes 300h at 900 DEG C；
The microscopic appearance of sample surfaces after 1000 DEG C of Figure 18 infiltration Cr alloy oxidation 300h.
Specific embodiment
Embodiment 1
(1), use vacuum arc furnace melting at matter high purity Ti (> 99.99%), Al (> 99.95%), Nb (> 99.95%)
The high Nb titanium-aluminium alloy that score is Ti-45Al-8.5Nb is measured, is then cast as alloy pig with copper mold；
(2), alloy is cut into the square alloy sample that size is 10 × 10 × 5mm with wire cutting, and with SiC sand paper by sample
Surrounding is polishing to 2000# from 600#, is put into ultrasonic wave to be cleaned with alcohol and dry, prepares for double-layer metallic glow ion cementation；
(3), Cr is seeped to the surface Ti-45Al-8.5Nb by double glow plasma surface alloying technique, sample is placed into the double-deck brightness
In light metal leakage furnace, and to be filled in furnace purity be 99.99% argon gas；
(4) a length of 2h when metallic cementation, temperature are 800 DEG C, and the both ends when actual temperature reaches setting temperature to grid are passed through low
Voltage high-current obtains the coating (Fig. 1) with a thickness of 2 μm, and coating is fine and close and is firmly combined with Ti-45Al-8.5Nb alloy, table
Face Cr content also reaches the Cr to form single densification2O3Critical concentration；
(5), cated Ti-45Al-8.5Nb alloy and cated Ti-45Al-8.5Nb alloy will not be had to be put into togerther 900 DEG C
High temperature furnace in isothermal oxidation 90h and 300h, characterized with XRD, SEM etc.；
(6), comparative study discovery their rate of rise of oxidation initial stage is all very fast, aoxidizes 90h, they parabolically increase (figure
2), with the extension of oxidization time, the advantage of cated Ti-45Al-8.5Nb alloy is more and more obvious, its oxidation weight gain
Rate is significantly lower than result when not doing coating, and (Fig. 5 does not have the rate 1.98mg/cm of cated Ti-45Al-8.5Nb alloy2·
The rate of h, cated Ti-45Al-8.5Nb (800 DEG C of infiltration Cr) alloy are 1.17mg/cm2While cated Ti- h),
45Al-8.5Nb alloy surface forms fine and close Cr2O3Oxidation film (Fig. 3,4,6,7), effectively prevent oxygen in air into
Enter alloy substrate, this is also the reason for having the oxidation rate of coating alloy more and more stable why.
Embodiment 2
(1), use vacuum arc furnace melting at matter high purity Ti (> 99.99%), Al (> 99.95%), Nb (> 99.95%)
The titanium-aluminium alloy that score is Ti-45Al-8.5Nb is measured, is then cast as alloy pig with copper mold；
(2), alloy pig is cut into the square alloy sample that size is 10 × 10 × 5mm with wire cutting, and will be closed with SiC sand paper
Golden sample surrounding is polishing to 2000# from 600#, is put into ultrasonic wave to be cleaned with alcohol and dry, does for double-layer metallic glow ion cementation
Prepare；
(3), Cr is seeped to the surface Ti-45Al-8.5Nb by double glow plasma surface alloying technique, sample is placed into the double-deck brightness
In light metal leakage furnace, and to the argon gas for being filled with high-purity in furnace；
(4) a length of 2h when metallic cementation, temperature are 1000 DEG C, and the both ends when actual temperature reaches setting temperature to grid are passed through low
Voltage high-current obtains the coating (Fig. 8) that thickness is about 10 μm, and coating is fine and close and is firmly combined with Ti-45Al-8.5Nb alloy,
Surface C r content also reaches the Cr to form single densification2O3Critical concentration；
(5), cated Ti-45Al-8.5Nb alloy and cated Ti-45Al-8.5Nb alloy will not be had to be put into togerther 900 DEG C
High temperature furnace in isothermal oxidation aoxidize 90h and 300h, characterized with XRD, SEM；
(6), comparative study discovery their rate of rise of oxidation initial stage is all very fast, aoxidizes 90h, they parabolically increase (figure
9), with the extension of oxidization time, the advantage of cated Ti-45Al-8.5Nb alloy is more and more obvious, its oxidation weight gain
Rate is significantly lower than result when not doing coating, and (Figure 12 does not have the rate 1.98mg/cm of cated Ti-45Al-8.5Nb alloy2·
H, cated Ti-45Al-8.5Nb (1000 DEG C of infiltration Cr) rate are 1.03mg/cm2H), while in cated alloy table
Face forms finer and close Cr2O3Oxidation film (Fig. 9,10,12,13), oxidation rate, which is significantly lower than, does not have cated Ti-45Al-
The oxidation rate of 8.5Nb alloy, and it is also lower than the oxidation rate of Ti-45Al-8.5Nb alloy cated in embodiment 1,
High-temperature oxidation resistance is more preferable.
XRD is X ray diffracting spectrum；SEM is scanning electron microscope；
It is the related effective embodiment explanation of the present invention above.Here, needing to declare a bit, this method is not limited to
Above embodiments.
Claims (4)
1. a kind of method for the high-temperature oxidation resistance for improving Ti-45Al-8.5Nb alloy, it is characterized in that the following steps are included:
(1), use vacuum arc furnace melting at mass fraction for Ti-45Al-8.5Nb's Ti, Al, Nb of purity > 99.95%
Then alloy is cast as alloy pig with copper mold, alloy pig is cut into the square sample that size is 10 × 10 × 5mm, polishing is washed
Only；
(2), sample is placed into double-deck glow metal leakage furnace, and to be filled in furnace purity be 99.99% argon gas, metallic cementation
Material is Cr；
(3), metallic cementation temperature and time is adjusted, the infiltration layer being firmly combined from Ti-45Al-8.5Nb alloy but form is different is obtained；
(4), cated Ti-45Al-8.5Nb alloy and cated Ti-45Al-8.5Nb alloy will not be had to be put into togerther 900 DEG C
High temperature furnace in isothermal oxidation, sample oxidation behavior is characterized with XRD, SEM, analyzes the high-temperature oxydation of two kinds of laboratory samples
Row.
2. a kind of antioxidative method of raising Ti-45Al-8.5Nb alloy high-temp as described in claim 1, feature exist
In the matrix alloy of selection is Ti-45Al-8.5Nb alloy, by carrying out double-layer metallic glow ion cementation to alloy surface, is come
Improve the inoxidizability of titanium-aluminium alloy.
3. a kind of antioxidative method of raising Ti-45Al-8.5Nb alloy high-temp as described in claim 1, it is characterised in that
When carrying out metallic cementation Cr to sample, a length of 1-3 h when metallic cementation is set, and metallic cementation temperature is 800 DEG C -1000 DEG C, when practical temperature
Be passed through low-voltage and high-current to the both ends of grid when degree reaches setting temperature, obtain the coating of different-thickness, coating it is fine and close and with
Ti-45Al-8.5Nb alloy is firmly combined.
4. a kind of antioxidative method of raising Ti-45Al-8.5Nb alloy high-temp as described in claim 1, it is characterised in that
After sample is put into 900 DEG C of high temperature furnace isothermal oxidations, cated alloy forms one layer of Cr on surface2O3Fine and close oxidation film,
Oxidation weight gain rate is caused to be significantly lower than when not doing coating as a result, to improve the inoxidizability of Ti-45Al-8.5Nb alloy.
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Cited By (3)
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| CN113186505A (en) * | 2021-04-17 | 2021-07-30 | 太原理工大学 | Method for preparing WC coating on surface of gamma-TiAl alloy |
| CN114657501A (en) * | 2022-02-28 | 2022-06-24 | 太原理工大学 | Method for improving high-temperature oxidation resistance of high Nb-TiAl alloy |
| CN116444284A (en) * | 2023-04-13 | 2023-07-18 | 武汉理工大学 | Antioxidant composite material screening preparation method based on thermodynamic calculation |
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| CN113186505A (en) * | 2021-04-17 | 2021-07-30 | 太原理工大学 | Method for preparing WC coating on surface of gamma-TiAl alloy |
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