CN107267914A - A kind of Ti2The method that AlNb alloy surface two-step methods prepare Si Al Y compisite seeping layers - Google Patents
A kind of Ti2The method that AlNb alloy surface two-step methods prepare Si Al Y compisite seeping layers Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/58—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in more than one step
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Abstract
The present invention relates to a kind of Ti2The method that AlNb alloy surface two-step methods prepare Si Al Y compisite seeping layers, i.e., first in Ti2AlNb based alloys surface embedding co-penetrating Si Y2O3, then pack cementation Al, so that preparing a kind of surface has the resistance to high temperature oxidation infiltration layer of certain Si, Al, Y content.One-step method Si Al Y permeation processes are split into two steps or multistep process, though so that the preparation technology of infiltration layer shows slightly cumbersome, the characteristic for several elements to be penetrated into, the process of more flexible adjustment infiltration element can be directed to.In each procedure, the technological parameter such as catalyst type, temperature, time also can targetedly be selected according to the physics of oozed element, chemical property, so as to be easier to obtain the infiltration layer with design structure.
Description
Technical field
The invention belongs to technical field of metal material surface modification, it is related to a kind of Ti2It is prepared by AlNb alloy surfaces two-step method
The method of Si-Al-Y compisite seeping layers
Background technology
Ti2AlNb based alloys are in α-Ti3Grow up on the basis of Al, it is a kind of based on orderly orthohormbic structure O phases
Intermetallic compound.Relative to the Ti of low Nb content3Al, the O phase alloys of this high Nb contents have higher intensity (particularly
High-temperature yield strength), fracture toughness and creep resistance, and low notch sensitivity.But at high operating temperatures, too high Nb contains
Amount (more than 15%) can cause Al in oxide-film2O3Volume fraction decline, non-protective oxide increases, such as AlNbO4, alloy
Surface can not form stable protective oxide layer.
Apply the important method that protective coating is raising alloy high temperature oxidation resistance in alloy surface, closed relative to titanium
Gold and TiAl-base alloy, at present in Ti2The research of anti oxidation layer prepared by AlNb based alloys surface is few, focuses primarily upon ion
Plate (Li H.Q., Wang Q.M., Jiang S.M., et al.Ion-plated Al-Al2O3 films as diffusion
barriers between NiCrAlY coating and orthorhombic-Ti2AlNb Alloy.Corrosion
Science,2010,52:1168-1674.), magnetron sputtering (Braun R., Leyens C..Protective coatings
on orthorhombic Ti2AlNb Alloy.Material at High Temperatures,2005,22:437–
447.), ion oozes (Liang W.P., Xu Z., Miao Q., et al.Study on Mo diffusion in double
glow plasma surface molybdenizing of Ti2AlNb.Chinese Journal of Aeronautics,
2006,19:255-259.), differential arc oxidation (Wang Y.H., Liu Z.G., Ouyang J.H., Wang Y.M., Zhou
Y..Preparation and high temperature oxidation resistance of microarc
oxidation ceramic coatings formed on Ti2AlNb alloy.Applied Surface Science,
2012,258:8946-8952.) etc..Although existing investigative technique improves Ti2The high temperature oxidation resistance of AlNb alloys, but
There is also some shortcomings, such as coating binding force is poor, and porosity is high, the specific equipment of prepares coating needs, and process costs are higher etc..
Pack cementation method is to prepare the common method of high temperature coatings on high-temperature structural material surface, with required equipment
Simply, cost is low, limit the advantages of small, coating binding force is good to matrix alloy size shape.Wherein, silicide infiltration layer is high temperature
One of structural material research and widely used infiltration layer, silicide infiltration layer density is low, fusing point is high, heat endurance is good, in height
Temperature is lower can to generate the SiO of densification2Infiltration layer, is suitable for the high-temperature oxidation resistant protection of high-temperature structural material.But single silicide
Brittleness is big, the SiO generated during oxidation2Thermal expansion coefficient difference with matrix alloy is larger, can be produced in infiltration layer larger
Internal stress, causes surface film oxide to peel off and lose protectiveness, it is therefore desirable to add other elements and be modified to it.Grind
Study carefully and show, Al elements help to improve the Al formed after the toughness of silicide infiltration layer, and Al oxidations2O3With good anti-oxidation
Diffusion and penetrating power, can be with SiO2Combine to form Al2O3·SiO2Phase, makes the crackle in oxide-film up, increases the viscous of oxide-film
Property, it can keep fine and close and continuous for a long time.And active element Y can be refined significantly in the crystal grain of infiltration layer, reduction oxide-film
Internal stress, so as to effectively improve the anti-strip ability of oxide-film.
, both can at a certain temperature, by matrix alloy bag when needing to penetrate into multiple element on matrix alloy surface
In the mixed-powder for being embedded to multiple element, multiple element is disposably deposited on its surface, this method is co-permeation method.It can also adopt
With two steps or multistep process, often walk and only penetrate into one of which or several elements, this method is composite cementation method.At present, using Si-
The method of Al-Y permeations, in NbSi based alloys, (Zhang Chaofeng, Guo likes flat .Nb-Ti-Si based ultra-high temperatures alloy surface Si-Al-Y
Co-penetration layer is organized the formation of, Journal of Inorganic Materials, 2010,25 (11):1209-1216), TiAl-base alloy (Li Y.Q., Xie
F.Q.,Wu X.Q..Effects of Y2O3 on the microstructures and wear resistance of Si-
Al-Y co-deposition coatings prepared on TiAl alloy by pack cementation
technique.Applied Surface Science,2013,278:30-36.) surface is prepared for a variety of anti-oxidant Si-Al-Y
Co-penetration layer, these infiltration layers improve the high temperature oxidation resistance of matrix material in various degree.But using embedding co-penetrating legal system
During standby Si-Al-Y infiltration layers, in order to be able to obtain the infiltration layer of design structure, it is necessary to the ratio between infiltration element powder in penetration enhancer and
Other technological parameters (such as catalyst type, temperature, time) carry out substantial amounts of exploration, even if can be by such as before experiment
The softwares such as ChemSage, HSC or Thermo-Cacl carry out calculation of thermodynamics to permeation process, to be optimized to its parameter, but
Due to each element diffusion in subsequent preparation process and the difference mutually formed between thermodynamics, dynamics, it is still necessary to which test of many times is come
The optimum condition of multicomponent thermochemical treatment is determined, this has resulted in the reduction (Zhang Ping of the waste of resource and benefit in scientific research process
.Nb-Si the tissue of based alloy Si-Al-Y diffusion coatings and antioxygenic property Xi'an:Northwestern Polytechnical University, 2014.).
The content of the invention
The technical problem to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of Ti2AlNb alloy surfaces two-step method prepares Si-
The method of Al-Y compisite seeping layers, first pack cementation Si-Y2O3, then pack cementation Al, in Ti2The generation of AlNb alloy surfaces is fine and close, adhesion
Good Si-Al-Y compisite seeping layers, so as to improve Ti2The oxidation-resistance property of AlNb alloys.
Technical scheme
A kind of Ti2The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, it is characterised in that step is such as
Under：
The preparation of step 1, Si-Y co-penetration layers：Penetration enhancer A is loaded into crucible, and the Ti of pretreatment2AlNb based alloys are embedded to
In penetration enhancer, using elevated-temperature seal mud by crucible and crucible cover sealing joint, it is placed in high temperature resistance furnace；Then heat to 940~
1060 DEG C, it is incubated afterwards after 6~9h, crucible is taken out, room temperature is air-cooled to；
By the Ti after pack cementation2AlNb based alloys are taken out, and are rinsed, are cleaned with absolute ethyl alcohol ultrasonic wave using circulating water, then
Dried, complete the preparation of Si-Y co-penetration layers；
The Ti2AlNb based alloys surface covering penetration enhancer thickness is not less than 10mm；
The Ti2AlNb based alloys are not less than 10mm away from crucible bottom distance；
The penetration enhancer A：According to percentage by weight by 10~20% Si, 1~3% Y2O3, 5~10% NaF, surplus
For Al2O3Ground and mixed in ball mill is placed in, is placed in baking oven and is incubated and dries；
Step 2, aluminizing：
The alloy of Si-Y co-penetration layers is cleaned using absolute ethyl alcohol ultrasonic wave, then is embedded in the penetration enhancer B of crucible, then is warming up to
850~950 DEG C, it is incubated afterwards after 2~4h, crucible is taken out, room temperature is air-cooled to；
Alloy after pack cementation is taken out, is rinsed, is cleaned with absolute ethyl alcohol ultrasonic wave using circulating water, then is dried,
Complete to Ti2The aluminizing of AlNb based alloy Si-Y co-penetration layers, so far, in Ti2AlNb alloy surface two-step methods Si-Al-Y is answered
The preparation for closing infiltration layer is completed；
The alloy surface covering penetration enhancer thickness of the Si-Y co-penetration layers is not less than 10mm；
The alloy of the Si-Y co-penetration layers is not less than 10mm away from crucible bottom distance；
The penetration enhancer B：According to percentage by weight by 10~20% Al, 3~8% AlCl3·6H2O, surplus is Al2O3
Ground and mixed in ball mill is placed in, is placed in baking oven and is incubated and dries.
The Ti2AlNb based alloys are pre-processed：Polish Ti2AlNb based alloys surface, ultrasonic wave is cleaned in absolute ethyl alcohol
After dry.
Si powder and Y in the penetration enhancer A2O3The particle diameter of powder is no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh.
The particle diameter of Al powder is no more than 100 mesh, Al in the penetration enhancer B2O3The particle diameter of powder is no more than 200 mesh.
The penetration enhancer A and penetration enhancer B grind 2~4h in ball mill, are placed in insulation 1h in the baking oven that temperature is 100 DEG C and carry out
Drying.
The elevated-temperature seal mud：Ludox and Al2O3The Al of l~l.2kg is added according to every 1L Ludox2O3Ratio mixing
Elevated-temperature seal mud is made.
Beneficial effect
A kind of Ti proposed by the present invention2The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, i.e., first exist
Ti2AlNb based alloys surface embedding co-penetrating Si-Y2O3, then pack cementation Al, so that preparing a kind of surface has certain Si, Al, Y
The resistance to high temperature oxidation infiltration layer of content.One-step method Si-Al-Y permeation processes are split into two steps or multistep process, though so that infiltration layer
Preparation technology shows slightly cumbersome, but can be directed to the characteristic for several elements to be penetrated into, and the work of element is penetrated into more flexible adjustment
Sequence.In each procedure, physics that the technological parameter such as catalyst type, temperature, time also can be according to oozed element, chemical property
Targetedly selected, so as to be easier to obtain the infiltration layer with design structure.
Beneficial effect is：
(1) first in Ti2AlNb alloy surfaces prepare Si-Y co-penetration layers, Si-Y co-penetration layers are carried out again oozing at Al afterwards
Reason.It is ternary co-osmosized relative to Si-Al-Y, Si-Y two-spots permeation and individually to ooze Al techniques more ripe and easily controllable；
(2) prepared by infiltration layer uses common high temperature furnace, and without inert gas shielding, the practical work piece of complicated shape is still
It can be surface-treated using this technique, therefore process costs are low, it is practical；
(3) infiltration layer and matrix are chemical bonds, and adhesion is detected using methods such as file side method, scarifications, oozed
Layer and basal body binding force are good；
(4) the Si-Al-Y infiltration layers prepared using the technique have excellent oxidation-resistance property, through 900 DEG C of high temperature oxygens
Change after 100h, layer surface oxide-film is compact and complete, without substantially coming off and crackle, unit area weightening is 0.25~0.39mg/
cm2, and Ti2The weightening of AlNb alloy substrates unit area is 4.08mg/cm2。
Brief description of the drawings
Fig. 1 is Technology Roadmap of the invention.
Fig. 2 is embodiment 1 in Ti2Si-Y co-penetration layers (a) and two-step method Si- prepared by the AlNb based alloys surface first step
The photomacrograph of Al-Y compisite seeping layers (b).
Fig. 3 is embodiment 1 in Ti2Si-Y co-penetration layers (a) and two-step method Si- prepared by the AlNb based alloys surface first step
Surface second electronics (SE) collection of illustrative plates of Al-Y compisite seeping layers (b).
Fig. 4 is embodiment 1 in Ti2Si-Y co-penetration layers (a) and two-step method Si- prepared by the AlNb based alloys surface first step
Surface X-ray diffraction (XRD) collection of illustrative plates of Al-Y compisite seeping layers (b).
Fig. 5 is embodiment 1 in Ti2The cross section back scattering of Si-Y co-penetration layers prepared by the AlNb based alloys surface first step
(BSE) collection of illustrative plates (a) and the concentration profile (b) of each element in the co-penetration layer that draws is analyzed according to power spectrum (EDS).
Fig. 6 is embodiment 1 in Ti2The cross section back of the body of two-step method Si-Al-Y compisite seeping layers prepared by AlNb based alloys surface
Scattering (BSE) collection of illustrative plates (a) and the concentration profile (b) that each element in the compisite seeping layer drawn is analyzed according to power spectrum (EDS).
Fig. 7 is Ti2Ti in AlNb matrix alloys (a), embodiment 12AlNb based alloys surface two-step method Si-Al-Y composite cementations
Layer (b) aoxidizes the photomacrograph after 100h under 900 DEG C of atmospheric environments.
Fig. 8 is Ti2Ti in AlNb matrix alloys, embodiment 12AlNb based alloys surface two-step method Si-Al-Y compisite seeping layers exist
The unit area weightening curve map after 100h is aoxidized under 900 DEG C of atmospheric environments.
Embodiment
In conjunction with implementation
Example, the invention will be further described for accompanying drawing：
The first step：The preparation of Si-Y co-penetration layers：(1) by Ti2Each surface of AlNb based alloy samples is with 80~1500#SiC water sands
Paper is polished step by step, in absolute ethyl alcohol after ultrasonic wave cleaning, dry for standby；(2) penetration enhancer is configured, according to certain percentage by weight
Weigh Si powder, Y2O3, NaF, Al2O3；(3) penetration enhancer prepared is placed in 2~4h of grinding in ball mill, is sufficiently mixed it；
(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to be dried；(5) penetration enhancer dried is loaded crucible, and handle
In sample embedment penetration enhancer, the distance between adjacent, parallel sample is not less than 8mm, and alloy surface covering penetration enhancer thickness and sample are away from earthenware
Crucible bottom distance is not less than 10mm；(5) crucible that will be equipped with sample is capped and uses Ludox and Al2O3Add according to every 1L Ludox
Enter the Al of l~l.2kg2O3Ratio mixing after seal, be placed in high temperature resistance furnace；(6) high temperature resistance furnace is warming up to 940~1060
DEG C, it is incubated afterwards after 6~9h, crucible is taken out, room temperature is air-cooled to；(7) sample after pack cementation is rinsed using circulating water, used
Absolute ethyl alcohol ultrasonic wave is cleaned, then is dried.
Second step：Aluminizing：(1) alloy sample for there are Si-Y co-penetration layers prepared in the first step is surpassed with absolute ethyl alcohol
Sound wave is cleaned, dry for standby；(2) penetration enhancer is configured, Al powder, AlCl are weighed according to certain percentage by weight3·6H2O, Al2O3；
(3) penetration enhancer prepared is placed in 2~4h of grinding in ball mill, is sufficiently mixed it；(4) penetration enhancer is placed in temperature for 100 DEG C
Baking oven in insulation 1h dried；(5) penetration enhancer dried is loaded crucible, and sample is embedded in penetration enhancer, it is adjacent, parallel
The distance between sample is not less than 8mm, and alloy surface covering penetration enhancer thickness and sample are not less than 10mm away from crucible bottom distance；
(6) crucible that will be equipped with sample is capped and uses Ludox and Al2O3The Al of l~l.2kg is added according to every 1L Ludox2O3Ratio
Seal, be placed in high temperature resistance furnace after mixing；(7) high temperature resistance furnace is warming up to 850~950 DEG C, is incubated afterwards after 2~4h, will
Crucible takes out, and is air-cooled to room temperature；(8) sample after pack cementation is rinsed using circulating water, cleaned with absolute ethyl alcohol ultrasonic wave, then
Dried, preparation process terminates.
The diffusion agent formulation that the present invention is provided：
(1) Si-Y is oozed2O3：Percentage by weight is 10~20%Si, 1~3%Y2O3, 5~10%NaF, surplus is Al2O3,
Si powder and Y2O3The particle diameter of powder is no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh；
(2) Al is oozed：Percentage by weight is 10~20%Al, 3~8%AlCl3·6H2O, surplus is Al2O3, wherein, Al powder
Particle diameter be no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh；
Specific embodiment：
From the Ti that atomic percent is 55%Ti-22%Al-23%Nb2AlNb based alloys are base material, are used thereon
Two-step method elder generation pack cementation Si-Y2O3, then pack cementation Al, in Ti2AlNb alloy surfaces generate Si-Al-Y compisite seeping layers.And it is entered
900 DEG C/100h of row atmospheric environment oxidation experiment.
Embodiment 1：
The first step：The preparation of Si-Y co-penetration layers
(1) by Ti2AlNb based alloy sample lines are cut into 10mm × 10mm × 5mm cuboid sample, and each surface uses 80
~1500#SiC waterproof abrasive papers are polished step by step, in absolute ethyl alcohol after ultrasonic wave cleaning 10min, are dried standby；(2) penetration enhancer is configured.
Penetration enhancer each component is 15%Si-2%Y according to percentage by weight2O3- 8%NaF-75%Al2O3, wherein, Si powder and Y2O3The grain of powder
Footpath is 100 mesh, Al2O3The particle diameter of powder is 200 mesh；(3) penetration enhancer prepared is placed in ball mill and ground under 200r/min
3h, is sufficiently mixed it；(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to be dried；(5) drying
Penetration enhancer half loads crucible and is compacted, and the sample after cleaning, drying is embedded in penetration enhancer, is covered and pressed again with second half penetration enhancer
It is real, when placing sample, it need to ensure that the distance between adjacent, parallel sample is not less than 8mm, alloy surface covering penetration enhancer thickness and examination
Sample is not less than 10mm away from crucible bottom distance；(6) the crucible capping of sample is will be equipped with, the seam crucible and crucible cover is molten with silicon
Glue and Al2O3The elevated-temperature seal mud sealing being modulated into, the proportioning of elevated-temperature seal mud adds 60g Al according to 50ml Ludox2O3；
(7) crucible after sealing is placed in high temperature resistance furnace, high temperature resistance furnace is warming up to 980 DEG C, Zhi Houbao with 7 DEG C/min speed
After warm 6h, crucible is taken out, room temperature is air-cooled to；(8) sample after pack cementation is taken out, is rinsed using circulating water, use anhydrous second
Alcohol ultrasonic wave cleans 20min, then is dried, and completes the preparation of Si-Y co-penetration layers.
Second step：Aluminizing
(1) alloy sample for there are Si-Y co-penetration layers prepared in the first step is dried with after absolute ethyl alcohol ultrasonic wave 10min
It is standby；(2) penetration enhancer is configured.Penetration enhancer each component is 15%Al-5%AlCl according to percentage by weight3·6H2O-80%Al2O3, its
In, the particle diameter of Al powder is no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh；(3) penetration enhancer prepared is placed in ball mill
In grind 3h under 200r/min, be sufficiently mixed it；(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to carry out
Drying；(5) the penetration enhancer half dried is loaded crucible and be compacted, the sample after cleaning, drying is embedded in penetration enhancer, with another
Half penetration enhancer is covered and is compacted again, when placing sample, need to ensure that the distance between adjacent, parallel sample is not less than 8mm, alloy table
Face covers penetration enhancer thickness and sample and is not less than 10mm away from crucible bottom distance；(6) will be equipped with the crucible capping of sample, crucible and
The seam Ludox and Al of crucible cover2O3The elevated-temperature seal mud sealing being modulated into, the proportioning of elevated-temperature seal mud is molten according to 50ml silicon
Glue adds 60g Al2O3；(7) crucible after sealing is placed in high temperature resistance furnace, high temperature resistance furnace is with 7 DEG C/min speed liter
Temperature is incubated after 3h to 900 DEG C, crucible is taken out, room temperature is air-cooled to afterwards；(8) sample after pack cementation is taken out, uses flowing
Water is rinsed, and 20min is cleaned with absolute ethyl alcohol ultrasonic wave, then is dried, and completes the preparation of aluminide coating.
900 DEG C/100h atmospheric environment oxidation experiment is carried out to infiltration layer, as a result shows that oxide-film is compact and complete, no peeling
Phenomenon, unit area weightening is 0.25mg/cm2。
Embodiment 2：
The first step：The preparation of Si-Y co-penetration layers
(1) by Ti2AlNb based alloy sample lines are cut into 10mm × 10mm × 5mm cuboid sample, and each surface uses 80
~1500#SiC waterproof abrasive papers are polished step by step, in absolute ethyl alcohol after ultrasonic wave cleaning 10min, are dried standby；(2) penetration enhancer is configured.
Penetration enhancer each component is 10%Si-3%Y according to percentage by weight2O3- 8%NaF-79%Al2O3, wherein, Si powder and Y2O3The grain of powder
Footpath is 100 mesh, Al2O3The particle diameter of powder is 200 mesh；(3) penetration enhancer prepared is placed in ball mill and ground under 200r/min
3h, is sufficiently mixed it；(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to be dried；(5) drying
Penetration enhancer half loads crucible and is compacted, and the sample after cleaning, drying is embedded in penetration enhancer, is covered and pressed again with second half penetration enhancer
It is real, when placing sample, it need to ensure that the distance between adjacent, parallel sample is not less than 8mm, alloy surface covering penetration enhancer thickness and examination
Sample is not less than 10mm away from crucible bottom distance；(6) the crucible capping of sample is will be equipped with, the seam crucible and crucible cover is molten with silicon
Glue and Al2O3The elevated-temperature seal mud sealing being modulated into, the proportioning of elevated-temperature seal mud adds 60g Al according to 50ml Ludox2O3；
(7) crucible after sealing is placed in high temperature resistance furnace, high temperature resistance furnace is warming up to 1060 DEG C with 7 DEG C/min speed, afterwards
It is incubated after 9h, crucible is taken out, room temperature is air-cooled to；(8) sample after pack cementation is taken out, rinsed using circulating water, with anhydrous
EtOH Sonicate ripple cleans 20min, then is dried, and completes the preparation of Si-Y co-penetration layers.
Second step：Aluminizing
(1) alloy sample for there are Si-Y co-penetration layers prepared in the first step is dried with after absolute ethyl alcohol ultrasonic wave 10min
It is standby；(2) penetration enhancer is configured.Penetration enhancer each component is 10%Al-5%AlCl according to percentage by weight3·6H2O-85%Al2O3, its
In, the particle diameter of Al powder is no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh；(3) penetration enhancer prepared is placed in ball mill
In grind 3h under 200r/min, be sufficiently mixed it；(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to carry out
Drying；(5) the penetration enhancer half dried is loaded crucible and be compacted, the sample after cleaning, drying is embedded in penetration enhancer, with another
Half penetration enhancer is covered and is compacted again, when placing sample, need to ensure that the distance between adjacent, parallel sample is not less than 8mm, alloy table
Face covers penetration enhancer thickness and sample and is not less than 10mm away from crucible bottom distance；(6) will be equipped with the crucible capping of sample, crucible and
The seam Ludox and Al of crucible cover2O3The elevated-temperature seal mud sealing being modulated into, the proportioning of elevated-temperature seal mud is molten according to 50ml silicon
Glue adds 60g Al2O3；(7) crucible after sealing is placed in high temperature resistance furnace, high temperature resistance furnace is with 7 DEG C/min speed liter
Temperature is incubated after 4h to 850 DEG C, crucible is taken out, room temperature is air-cooled to afterwards；(8) sample after pack cementation is taken out, uses flowing
Water is rinsed, and 20min is cleaned with absolute ethyl alcohol ultrasonic wave, then is dried, and completes the preparation of aluminide coating.
900 DEG C/100h atmospheric environment oxidation experiment is carried out to infiltration layer, as a result shows that oxide-film is compact and complete, no peeling
Phenomenon, unit area weightening is 0.39mg/cm2。
Embodiment 3：
The first step：The preparation of Si-Y co-penetration layers
(1) by Ti2AlNb based alloy sample lines are cut into 10mm × 10mm × 5mm cuboid sample, and each surface uses 80
~1500#SiC waterproof abrasive papers are polished step by step, in absolute ethyl alcohol after ultrasonic wave cleaning 10min, are dried standby；(2) penetration enhancer is configured.
Penetration enhancer each component is 15%Si-3%Y according to percentage by weight2O3- 8%NaF-74%Al2O3, wherein, Si powder and Y2O3The grain of powder
Footpath is 100 mesh, Al2O3The particle diameter of powder is 200 mesh；(3) penetration enhancer prepared is placed in ball mill and ground under 200r/min
3h, is sufficiently mixed it；(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to be dried；(5) drying
Penetration enhancer half loads crucible and is compacted, and the sample after cleaning, drying is embedded in penetration enhancer, is covered and pressed again with second half penetration enhancer
It is real, when placing sample, it need to ensure that the distance between adjacent, parallel sample is not less than 8mm, alloy surface covering penetration enhancer thickness and examination
Sample is not less than 10mm away from crucible bottom distance；(6) the crucible capping of sample is will be equipped with, the seam crucible and crucible cover is molten with silicon
Glue and Al2O3The elevated-temperature seal mud sealing being modulated into, the proportioning of elevated-temperature seal mud adds 60g Al according to 50ml Ludox2O3；
(7) crucible after sealing is placed in high temperature resistance furnace, high temperature resistance furnace is warming up to 1020 DEG C with 7 DEG C/min speed, afterwards
It is incubated after 6h, crucible is taken out, room temperature is air-cooled to；(8) sample after pack cementation is taken out, rinsed using circulating water, with anhydrous
EtOH Sonicate ripple cleans 20min, then is dried, and completes the preparation of Si-Y co-penetration layers.
Second step：Aluminizing
(1) alloy sample for there are Si-Y co-penetration layers prepared in the first step is dried with after absolute ethyl alcohol ultrasonic wave 10min
It is standby；(2) penetration enhancer is configured.Penetration enhancer each component is 20%Al-5%AlCl according to percentage by weight3·6H2O-75%Al2O3, its
In, the particle diameter of Al powder is no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh；(3) penetration enhancer prepared is placed in ball mill
In grind 3h under 200r/min, be sufficiently mixed it；(4) penetration enhancer is placed in into insulation 1h in the baking oven that temperature is 100 DEG C to carry out
Drying；(5) the penetration enhancer half dried is loaded crucible and be compacted, the sample after cleaning, drying is embedded in penetration enhancer, with another
Half penetration enhancer is covered and is compacted again, when placing sample, need to ensure that the distance between adjacent, parallel sample is not less than 8mm, alloy table
Face covers penetration enhancer thickness and sample and is not less than 10mm away from crucible bottom distance；(6) will be equipped with the crucible capping of sample, crucible and
The seam Ludox and Al of crucible cover2O3The elevated-temperature seal mud sealing being modulated into, the proportioning of elevated-temperature seal mud is molten according to 50ml silicon
Glue adds 60g Al2O3；(7) crucible after sealing is placed in high temperature resistance furnace, high temperature resistance furnace is with 7 DEG C/min speed liter
Temperature is incubated after 2h to 900 DEG C, crucible is taken out, room temperature is air-cooled to afterwards；(8) sample after pack cementation is taken out, uses flowing
Water is rinsed, and 20min is cleaned with absolute ethyl alcohol ultrasonic wave, then is dried, and completes the preparation of aluminide coating.
900 DEG C/100h atmospheric environment oxidation experiment is carried out to infiltration layer, as a result shows that oxide-film is compact and complete, no peeling
Phenomenon, unit area weightening is 0.29mg/cm2。
Claims (6)
1. a kind of Ti2The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, it is characterised in that step is as follows：
The preparation of step 1, Si-Y co-penetration layers：Penetration enhancer A is loaded into crucible, and the Ti of pretreatment2AlNb based alloys are embedded to penetration enhancer
In, using elevated-temperature seal mud by crucible and crucible cover sealing joint, it is placed in high temperature resistance furnace；Then heat to 940~1060
DEG C, it is incubated afterwards after 6~9h, crucible is taken out, room temperature is air-cooled to；
By the Ti after pack cementation2AlNb based alloys are taken out, and are rinsed, are cleaned with absolute ethyl alcohol ultrasonic wave, then dried using circulating water
It is dry, complete the preparation of Si-Y co-penetration layers；
The Ti2AlNb based alloys surface covering penetration enhancer thickness is not less than 10mm；
The Ti2AlNb based alloys are not less than 10mm away from crucible bottom distance；
The penetration enhancer A：According to percentage by weight by 10~20% Si, 1~3% Y2O3, 5~10% NaF, surplus is
Al2O3Ground and mixed in ball mill is placed in, is placed in baking oven and is incubated and dries；
Step 2, aluminizing：
The alloy of Si-Y co-penetration layers is cleaned using absolute ethyl alcohol ultrasonic wave, then is embedded in the penetration enhancer B of crucible, then is warming up to 850
~950 DEG C, it is incubated afterwards after 2~4h, crucible is taken out, room temperature is air-cooled to；
Alloy after pack cementation is taken out, is rinsed, is cleaned with absolute ethyl alcohol ultrasonic wave using circulating water, then is dried, is completed
To Ti2The aluminizing of AlNb based alloy Si-Y co-penetration layers, so far, in Ti2AlNb alloy surface two-step method Si-Al-Y composite cementations
The preparation of layer is completed；
The alloy surface covering penetration enhancer thickness of the Si-Y co-penetration layers is not less than 10mm；
The alloy of the Si-Y co-penetration layers is not less than 10mm away from crucible bottom distance；
The penetration enhancer B：According to percentage by weight by 10~20% Al, 3~8% AlCl3·6H2O, surplus is Al2O3It is placed in
Ground and mixed in ball mill, is placed in baking oven and is incubated and dries.
2. Ti according to claim 12The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, its feature exists
In：The Ti2AlNb based alloys are pre-processed：Polish Ti2AlNb based alloys surface, dries in the air in absolute ethyl alcohol after ultrasonic wave cleaning
It is dry.
3. Ti according to claim 12The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, its feature exists
In：Si powder and Y in the penetration enhancer A2O3The particle diameter of powder is no more than 100 mesh, Al2O3The particle diameter of powder is no more than 200 mesh.
4. Ti according to claim 12The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, its feature exists
In：The particle diameter of Al powder is no more than 100 mesh, Al in the penetration enhancer B2O3The particle diameter of powder is no more than 200 mesh.
5. Ti according to claim 12The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, its feature exists
In：The penetration enhancer A and penetration enhancer B grind 2~4h in ball mill, are placed in insulation 1h in the baking oven that temperature is 100 DEG C and are dried.
6. Ti according to claim 12The method that AlNb alloy surface two-step methods prepare Si-Al-Y compisite seeping layers, its feature exists
In：The elevated-temperature seal mud：Ludox and Al2O3The Al of l~l.2kg is added according to every 1L Ludox2O3Ratio be mixed
Elevated-temperature seal mud.
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