CN107267915A - A kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si B Y coatings - Google Patents

A kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si B Y coatings Download PDF

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CN107267915A
CN107267915A CN201710489407.9A CN201710489407A CN107267915A CN 107267915 A CN107267915 A CN 107267915A CN 201710489407 A CN201710489407 A CN 201710489407A CN 107267915 A CN107267915 A CN 107267915A
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oozed
tantalum
penetration enhancer
coatings
alloy surface
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李涌泉
耿桂宏
侯俊峰
李宁
董福元
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North Minzu University
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North Minzu University
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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
    • C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
    • C23C12/02—Diffusion in one step

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Abstract

The invention belongs to high temperature coating technical field, and in particular to a kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si B Y coatings.The invention discloses the composition of penetration enhancer, by weight percentage for：12% 17% are oozed elements Si（Purity >=99%）, 1.0% 2.0% are oozed element Y2O3（Purity >=99%）, 1.0% 2.0% are oozed element B（Purity >=98%）, 5% 8% catalyst n aF（Analysis is pure）, surplus is filler Al2O3.The invention also discloses the preparation method of coating：Specimen surface is pre-processed first, then the penetration enhancer ball milling prepared is refined, then sample and penetration enhancer loading are oozed into tank and sealed, tank will be then oozed and be placed in heating in high temperature furnace, is incubated, cooling, and finally take out sample and clean, dry --.Gained coating structure even compact, is well combined with matrix, is remarkably improved the thermal protective performance of matrix alloy, predominantly high-temperature oxidation resistance, take into account anti-corrosion wear performance, can tolerate 1000 DEG C of high temperature and be up to more than 100h.Equipment needed for the method is simple, process, with low cost, suitable for production application.

Description

A kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si-B-Y coatings
Technical field
The invention belongs to high temperature coating technical field, and in particular to a kind of tantalum and tantalum alloy surface Si-B-Y coatings of preparing Penetration enhancer and method.
Background technology
Tan Shu VB races refractory metal, fusing point is up to 3033 DEG C, and with good elevated temperature strength, is most expected to turn into high temperature The candidate material of structural material.Therefore, controlled and anti-for tantalum alloy technology of preparing, composition design, institutional framework both at home and abroad The work of 20 years of researches is had been carried out in terms of oxidation susceptibility.However, the antioxygenic property of tantalum alloy at high temperature is poor, pure tantalum Even just occurs " pest " oxidative phenomena at 600 DEG C, as one of main bottleneck for restricting its application.
Two aspects are mainly concentrated in the research for improving tantalum-base alloy surface high temperature oxidation resistance at present：1）Alloying changes Property；2）Coat is protected（Tang Yong, Du Jihong, Li Zhengxian etc. tantalum alloy high-temperature oxidation resistant composite coating preparation research [J] Sufacing, 2013,42 (6):59-61.）.Research shows, is entered by adding the elements such as Hf, W, Al, Cr, B, Ge and Y Row is multi-element alloyed can to improve the high-temperature oxidation resistance of tantalum alloy to a certain extent.But this method can't be solved thoroughly The inoxidizability problem of tantalum alloy, because the tantalum alloy after multi-element alloyed mostly generates the oxidation of non-protective after oxidation Thing such as Ta2O5, TiTa2O7And Ti2Ta10O29Deng, meanwhile, low-alloyed high/low temperature power can substantially be dropped by adding excessive alloy element Performance is learned, so with limitation.
Face coat protection is to take into account tantalum alloy high/low temperature mechanical property and the conscientiously effective approach of antioxygenic property. In numerous coating systems, silicide coating fusing point is high, with good heat endurance, and temperature in use is high, with self-healing ability, because And with very strong oxidation resistance.Therefore research both domestic and external is also all concentrated in silicide coating system at present.According to state Inside and outside research level and present situation, the subject matter that the silicide coating of research and development is also present on tantalum alloy at present is：（1） Fragility itself, can cause the generation of a large amount of crackles；（2）SiO2Oxide-film poor fluidity, it is impossible to effectively protect matrix, easily peel off and Lose protectiveness.Therefore addition active element is needed to be modified it, to improve the oxidation resistance of coating.
Existing document report controls the growth course of coating by adding B, suppresses the formation of crackle in silicide coating, And form B using oxidation2O3Low melting point improve the mobility of oxide-film, so as to effectively make the method for crackle and hole up. Rare earth element yttrium (Y) and its oxide (Y2O3) there is high fusing point.Yttrium (Y) can improve the high-temperature oxidation resistance of coating Energy；Yittrium oxide has excellent heat-resisting, corrosion-resistant and high-temperature stability.
Chinese patent application 201510917594.7 discloses a kind of tantalum alloy surface and is modified compound Hf-Ta coatings, by with The composition composition of lower mass percent：Ta 19.5%~24.5%, Si 0.5%~2.5%, B 0.5%~1.2%, Al 0.5%~2.5%, Cr 0.5%~2.0%, surplus is Hf；Also disclose simultaneously using stuff paste melting prepares coating.In Patent of invention " high-temperature oxidation-resistant material and the side that high-temperature oxidation resistant coating is prepared by it of state's patent application 201110024938.3 Method ", the component for disclosing high-temperature oxidation-resistant material is：Ta is 1.5-4.8Wt%, and W is 5.2-8.7Wt%, and Cr is 11.2- 15.4Wt%, Ni are 2.3-5.7Wt%, and B is 1.3-1.6Wt%, and NaF is 0.4-0.8Wt%, and Y is 1.1-2.3Wt%, and surplus is Si； Also disclose that simultaneously using stuff paste melting prepares coating；The formula includes 8 kinds of compositions, complex.Above-mentioned two pieces invention is special The prepared coating of profit application can be present compared with multiple hole, and the adhesion with matrix is not good enough, and the high-temperature oxidation resistant life-span is relatively short.Mesh Before, still belong to about tantalum alloy surface B, Y modified silicide coating formula and using the report in terms of pack cementation technology prepares coating Blank.
Therefore, research can overcome silicide coating fragility itself to be also easy to produce crackle and SiO2Oxide-film poor fluidity is asked Topic, can significantly improve silicide coating high-temperature oxidation resistant life-span, and B, Y of the more simple tantalum alloy surface thermal protection of formula again Modified silicide coating and pack cementation technology of preparing, the application to tantalum and tantalum alloy are significant.
The content of the invention
In order to solve the above technical problems, preparing tantalum and tantalum alloy surface Si-B-Y paintings it is an object of the invention to provide one kind The penetration enhancer of layer, the coating prepared by the penetration enhancer is remarkably improved the high-temperature oxidation resistant life-span of tantalum and tantalum alloy, improves high warm anti- Performance is protected, can be the protection that tantalum and tantalum alloy provide the long period in high-temperature oxidation environment and ablation environment.
It is a further object to provide a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings.
To achieve the above object, the technical solution adopted by the present invention is：One kind prepares tantalum and tantalum alloy surface Si-B-Y is applied Layer penetration enhancer, it is characterised in that in percentage by weight consisting of：12%-17% is oozed elements Si, and 1.0%-2.0% is oozed Element Y2O3, 1.0%-2.0% oozed element B, and 5%-8% catalyst n aF, surplus is filler Al2O3。
Above-mentioned a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that according to weight percent Than meter consisting of：13%-16% is oozed elements Si, and 1.0%-1.9% is oozed element Y2O3, 1.0%-1.9% oozed element B, 6%-8% Catalyst n aF, surplus is filler Al2O3。
Above-mentioned a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that according to weight percent Than meter consisting of：12% is oozed elements Si, and 1.0% is oozed element Y2O3, 1.0% is oozed element B, 5% catalyst n aF, and surplus is to fill out Fill thing Al2O3。
Above-mentioned a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that described to be oozed element Si purity >=99%, oozed element Y2O3Purity >=99%, purity >=98% for being oozed element B, catalyst n aF for analyze it is pure； It is described to be oozed elements Si, oozed element Y2O3, oozed element B, catalyst n aF and filler Al2O3Be it is powdered, granularity >= 80 mesh.
In addition, present invention also offers a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that Comprise the following steps：
1. sample pretreatment：Sample, which is put into after being polished through 200#-400# sand paper in ethanol solution, to be cleaned by ultrasonic, and then drying is treated With；
2. penetration enhancer is prepared：In percentage by weight, weigh 12%-17% and oozed elements Si, 1.0%-2.0% and oozed element Y2O3、 1.0%-2.0% is oozed element B, 5%-8% catalyst ns aF, surplus for filler Al2O3Powder, be placed in ball mill grind；Will Penetration enhancer after ball milling is placed in baking oven and dried, and is subsequently placed at stand-by in drying basin；
3. sample is filled：Penetration enhancer is loaded and oozes tank, and sample is uniformly embedded in penetration enhancer, it is ensured that is in the thickness away from specimen surface 1cm Penetration enhancer；The tank that oozes that will be equipped with sample is capped and sealed with sealant；
4. heat up：Tank will be oozed to be placed in high temperature resistance furnace, high temperature resistance furnace constant heatingrate 1h to 150 DEG C, then with 13 DEG C/min Speed constant heatingrate to 1180 DEG C -1220 DEG C；
5. it is incubated：In 1180 DEG C of -1220 DEG C of insulation 2h-4h, then take out and ooze tank；
6. cool down：Ullage will be oozed and be cooled to room temperature；
7. sample：Opening oozes tank, takes out the sample after pack cementation；
8. cleaning, drying：Sample after pack cementation is put into ethanol and cleaned, is dried in railway carriage or compartment is dried, is obtained in tantalum and the conjunction of tantalum base Gold surface is impregnated with Si-B-Y high-temperature oxidation resistant coating.
A kind of above-mentioned method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that step 1. described in Ethanol solution is absolute ethyl alcohol, preferably analyzes pure, concentration >=99.7%；Step 1. described in be cleaned by ultrasonic the time be 5 min- 10 min。
A kind of above-mentioned method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that step 2. described in Drum's speed of rotation is 30r/min-40r/min, and the milling time is the penetration enhancer granularity after 90min-240min, the ball milling >=300 mesh；Step 2. described in drying temperature be 100 DEG C -120 DEG C, drying time is 1.0h-1.5h.
A kind of above-mentioned method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that step 3. described in The compound method of sealant is：100g high temperature clays are taken, 20ml Ludox is added, stirs into pasty state.
A kind of above-mentioned method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that step 8. described in Ethanol is absolute ethyl alcohol, preferably analyzes pure, concentration >=99.7%, and the drying temperature is 100 DEG C -120 DEG C, and drying time is 4 min-6 min。
A kind of above-mentioned method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that 8. gained is applied step Thickness degree is 20 μm -40 μm.
The present invention has the advantages that compared with prior art：
1st, the present invention in terms of diffusion agent formulation, with the addition of rare earth element y, can play rush ooze, crystal grain thinning, improve oxide-film resist The ability of peeling, while Si elements are as high temperature coating essential element, the SiO formed in oxidizing process2There is self-healing capability, B element can form the B of low melting point in oxidizing process2O3, the mobility of oxide-film can be improved, thus effectively make up crackle and Hole, thus the Si-B-Y coatings being made can overcome silicide coating fragility itself to be also easy to produce crackle and SiO2Aoxidize membrane flow Property difference the problem of, and be formulated it is more simple.
2nd, the even tissue of Si-B-Y coatings of the present invention, densification, coating are metallurgical binding with matrix, therefore are had well Adhesion, high-temperature oxidation test shows that Si-B-Y coatings have good oxidation-resistance property, is remarkably improved silicide painting In the layer high-temperature oxidation resistant life-span, improve high-temperature hot protection performance, take into account anti-corrosion wear performance, can be tantalum and tantalum alloy in high temperature oxygen Change the protection that the long period is provided in environment and ablation environment, can tolerate 1000 DEG C of high temperature and be up to more than 100h.
3rd, equipment needed for prepared by Si-B-Y coatings of the present invention is simple, with low cost, process stabilizing is reliable, in heating moisturizing It need not be vacuumized in journey, it is easy to operate, be easily achieved, suitable for producing and applying, have to the application of tantalum and tantalum alloy important Meaning.
Below by drawings and examples, technical scheme is described in further detail.
Brief description of the drawings
Fig. 1 (a) is the microstructure figure of the Si-B-Y coating surfaces obtained using the embodiment of the present invention 1；
Fig. 1 (b) is the microstructure figure of the Si-B-Y coating cross sections obtained using the embodiment of the present invention 1；
Fig. 2 (a) is the microstructure figure of the Si-B-Y coating surfaces obtained using the embodiment of the present invention 2；
Fig. 2 (b) is the microstructure figure of the Si-B-Y coating cross sections obtained using the embodiment of the present invention 2；
Fig. 3 (a) is the microstructure figure of the Si-B-Y coating surfaces obtained using the embodiment of the present invention 3；
Fig. 3 (b) is the microstructure figure of the Si-B-Y coating cross sections obtained using the embodiment of the present invention 3；
Fig. 4 is the phase composition figure of the Si-B-Y coating cross sections obtained using the embodiment of the present invention 1；
In figure, 1：Si-B-Y coatings, 2：Base material；
Fig. 5 is Si-B-Y coating productions flow chart of the present invention.
Embodiment
Embodiment 1
A kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings of the present embodiment, it is characterised in that according to weight percent Than meter consisting of：12% is oozed elements Si（Purity >=99%）, 1.0% is oozed element Y2O3（Purity >=99%）, 1.0% is oozed element B（Purity >=98%）, 5% catalyst n aF（Analysis is pure）, surplus is filler Al2O3。
A kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings of the present embodiment, comprises the following steps：
1. it is put into after sample tantalum is polished through 200#, 300# and 400# sand paper in the pure absolute ethyl alcohol of analysis and is cleaned by ultrasonic 5min, with After dry up it is stand-by；
2. penetration enhancer is prepared：In percentage by weight, the 12% of 100 mesh are weighed to be oozed elements Si, 1.0% oozed element Y2O3、 1.0% is oozed element B, 5% catalyst n aF, surplus for filler Al2O3Powder, mixing；The penetration enhancer prepared is placed in ball milling In machine, ground with the r/min of rotating speed 40, milling time is 120min；Penetration enhancer after ball milling is placed in baking oven and dried, drying temperature 100 DEG C of degree, drying time is 1h；
3. sample is filled：Penetration enhancer is loaded and oozes tank, and sample is uniformly embedded in penetration enhancer, it is ensured that is in the thickness away from specimen surface 1cm Penetration enhancer；The tank that oozes that will be equipped with sample is capped and sealed with sealant.The compound method of sealant is：100g high temperature clays are taken, plus Enter 20ml Ludox, stir into pasty state；
4. heat up：Tank will be oozed to be placed in high temperature resistance furnace, high temperature resistance furnace constant heatingrate 1h to 150 DEG C, then with 13 DEG C/min Speed be warming up to 1180 DEG C；
5. it is incubated：Tank is oozed in taking-up after being incubated 2h at 1180 DEG C；
6. cool down：Ullage will be oozed and be cooled to room temperature；
7. sample：Opening oozes tank, and the sample after pack cementation is taken out；
8. cleaning, drying：Use absolute ethyl alcohol（CH3CH2OH≥99.7）Cleaning, dries 5min in drying railway carriage or compartment 100 DEG C, obtains Tantalum surface Si-B-Y high-temperature oxidation resistant coatings.
The thickness for obtaining Si-B-Y coatings by embodiment 1 is 20 μm.
The microstructure figure for obtaining Si-B-Y coating surfaces and section by embodiment 1 is shown in Fig. 1 (a) and Fig. 1 (b) respectively.
The phase composition figure of Si-B-Y coating cross sections is obtained as shown in figure 4, it can be seen that gained coating master by embodiment 1 Will by rich Si Si2Ta phase compositions（Coating electronic probe component analysis show that the chemical composition of the coating is：70.46Si- 1.82Y-2.23B-25.49Ta at.%）, therefore, Si, B, Y element realize compound permeation, and whole coating quality is good.
High-temperature oxydation test result indicates that, Ta matrixes aoxidize 5h at 1000 DEG C, and there is obvious spalling of oxide film on surface, i.e., It there occurs Oxidative demage；120h is aoxidized at 1000 DEG C by the gained infiltration layer of embodiment 1, Si-B-Y coatings are complete, do not peel off, to base Body has protective effect.
Embodiment 2
A kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings of the present embodiment, it is characterised in that according to weight percent Than meter consisting of：15% is oozed elements Si（Purity >=99%）, 1.5% is oozed element Y2O3（Purity >=99%）, 1.5% is oozed element B（Purity >=98%）, 6% catalyst n aF（Analysis is pure）, surplus is filler Al2O3。
A kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings of the present embodiment, comprises the following steps：
1. it is put into after sample tantalum is polished through 200#, 300# and 400# sand paper in the pure absolute ethyl alcohol of analysis and is cleaned by ultrasonic 5min, Then dry up stand-by；
2. penetration enhancer is prepared：In percentage by weight, the 15% of 100 mesh are weighed to be oozed elements Si, 1.5% oozed element Y2O3、 1.5% is oozed element B, 6% catalyst n aF, surplus for filler Al2O3Powder, mixing；The penetration enhancer prepared is placed in ball milling In machine, ground with 35 r/min rotating speed, milling time is 180min；Penetration enhancer after ball milling is placed in baking oven and dried, drying 100 DEG C of temperature, drying time is 1h；
3. sample is filled：Penetration enhancer is loaded and oozes tank, and sample is uniformly embedded in penetration enhancer, it is ensured that is in the thickness away from specimen surface 1cm Penetration enhancer；The tank that oozes that will be equipped with sample is capped and sealed with sealant；The compound method of the sealant is：100g high temperature is taken to stick Soil, adds 20ml Ludox, stirs into pasty state；
4. heat up：Tank will be oozed to be placed in high temperature resistance furnace.High temperature resistance furnace constant heatingrate 1h to 150 DEG C, then with 13 DEG C/min Speed be warming up to 1200 DEG C；
5. it is incubated：Tank is oozed in taking-up after being incubated 3h at 1200 DEG C；
6. cool down：Ullage will be oozed and be cooled to room temperature；
7. sample：Opening oozes tank, and the sample after pack cementation is taken out；
8. cleaning, drying：Use absolute ethyl alcohol（CH3CH2OH≥99.7）Cleaning, dries 5min in drying railway carriage or compartment 100 DEG C, obtains Tantalum surface Si-B-Y high-temperature oxidation resistant coatings.
The thickness for obtaining Si-B-Y coatings by embodiment 2 is 24 μm.
The microstructure figure for obtaining Si-B-Y coating surfaces and section by embodiment 2 is shown in Fig. 2 (a) and Fig. 2 (b) respectively.
The main Si by rich Si of Si-B-Y coatings is obtained by embodiment 22Ta phase compositions（Coating electronic probe component analysis show Show, the chemical composition of the coating is：71.12Si-1.73Y-1.89B-25.26Ta at.%）.High-temperature oxydation test result indicates that, Ta matrixes aoxidize 5h at 1000 DEG C, and there is obvious spalling of oxide film on surface, that is, there occurs Oxidative demage；Applied by the gained of embodiment 2 Layer aoxidizes 130h at 1000 DEG C, and Si-B-Y coatings are complete, do not peel off, have protective effect to matrix.
Embodiment 3
A kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings of the present embodiment, it is characterised in that according to weight percent Than meter consisting of：17% is oozed elements Si（Purity >=99%）, 2.0% is oozed element Y2O3（Purity >=99%）, 2.0% is oozed element B（Purity >=98%）, 8% catalyst n aF（Analysis is pure）, surplus is filler Al2O3。
A kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings of the present embodiment, comprises the following steps：
1. it is put into after sample tantalum is polished through 200#, 300# and 400# sand paper in the pure absolute ethyl alcohol of analysis and is cleaned by ultrasonic 5min, Then dry up stand-by；
2. penetration enhancer is prepared：In percentage by weight, the 17% of 100 mesh are weighed to be oozed elements Si, 2.0% oozed element Y2O3、 2.0% is oozed element B, 8% catalyst n aF, surplus for filler Al2O3Powder, mixing；The penetration enhancer prepared is placed in ball milling In machine, ground with 35r/min rotating speed, milling time is 180min；Penetration enhancer after ball milling is placed in baking oven and dried, drying temperature 100 DEG C of degree, drying time is 1h；
3. sample is filled：Penetration enhancer is loaded and oozes tank, and sample is uniformly embedded in penetration enhancer, it is ensured that is in the thickness away from specimen surface 1cm Penetration enhancer；The tank that oozes that will be equipped with sample is capped and sealed with sealant；The compound method of the sealant is：100g high temperature is taken to stick Soil, adds 20ml Ludox, stirs into pasty state；
4. heat up：Tank will be oozed to be placed in high temperature resistance furnace, high temperature resistance furnace constant heatingrate 1h to 150 DEG C, then with 13 DEG C/min Speed heat up 1.5h to 1220 DEG C；
5. it is incubated：Tank is oozed in taking-up after being incubated 4h at 1220 DEG C；
6. cool down：Ullage will be oozed and be cooled to room temperature；
7. sample：Opening oozes tank, and the sample after pack cementation is taken out；
8. cleaning, drying：Use absolute ethyl alcohol（CH3CH2OH≥99.7）Cleaning, dries 5min in drying railway carriage or compartment 100 DEG C, obtains Tantalum surface Si-B-Y high-temperature oxidation resistant coatings.
The thickness for obtaining Si-B-Y coatings by embodiment 3 is 30 μm.
The microstructure figure for obtaining Si-B-Y coating surfaces and section by embodiment 3 is shown in Fig. 3 (a) and Fig. 3 (b) respectively.
The main Si by rich Si of Si-B-Y coatings is obtained by embodiment 32Ta phase compositions（Coating electronic probe component analysis show Show, the chemical composition of the coating is：73.81Si-1.77Y-2.07B-22.35Ta at.%）.
High-temperature oxydation test result indicates that, Ta matrixes 1000 DEG C aoxidize 5h, there is obvious spalling of oxide film on surface, that is, sent out Oxidative demage is given birth to；125h is aoxidized at 1000 DEG C by the gained coating of embodiment 3, Si-B-Y coatings are complete, do not peel off, have to matrix Protective effect.
Above-described embodiment is only the present invention preferably embodiment, and embodiments of the present invention are not by above-described embodiment Limitation, it is noted that for those skilled in the art, do not departing from the premise of the technology of the present invention principle Under, a lot of other modification or optimal enforcement mode are can be designed that, these modifications or optimal enforcement mode will fall in the application Within scope of disclosure.

Claims (10)

1. a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that its group in percentage by weight Turn into：12%-17% is oozed elements Si, and 1.0%-2.0% is oozed element Y2O3, 1.0%-2.0% oozed element B, 5%-8% catalyst NaF, surplus is filler Al2O3。
2. a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 1, it is characterised in that according to Percentage by weight meter consisting of：13%-16% is oozed elements Si, and 1.0%-1.9% is oozed element Y2O3, 1.0%-1.9% oozed element B, 6%-8% catalyst n aF, surplus are filler Al2O3。
3. a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 1, it is characterised in that according to Percentage by weight meter consisting of：12% is oozed elements Si, and 1.0% is oozed element Y2O3, 1.0% is oozed element B, 5% catalyst n aF, Surplus is filler Al2O3。
4. a kind of penetration enhancer for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 1, it is characterised in that described Oozed purity >=99% of elements Si, oozed element Y2O3Purity >=99%, purity >=98% for being oozed element B, catalyst n aF be Analysis is pure；It is described to be oozed elements Si, oozed element Y2O3, oozed element B, catalyst n aF and filler Al2O3Be it is powdered, The mesh of granularity >=80.
5. a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings, it is characterised in that comprise the following steps：
1. sample pretreatment：Sample, which is put into after being polished through 200#-400# sand paper in ethanol solution, to be cleaned by ultrasonic, and then drying is treated With；
2. penetration enhancer is prepared：Si, Y are weighed according to the penetration enhancer proportion of composing described in claim 12O3, B, NaF and Al2O3Powder, Mixing；It is subsequently placed in ball mill and grinds；Penetration enhancer after ball milling is placed in baking oven and dried, is subsequently placed at stand-by in drying basin；
3. sample is filled：Penetration enhancer is loaded and oozes tank, and sample is uniformly embedded in penetration enhancer, it is ensured that is in the thickness away from specimen surface 1cm Penetration enhancer；The tank that oozes that will be equipped with sample is capped and sealed with sealant；
4. heat up：Tank will be oozed to be placed in high temperature resistance furnace, high temperature resistance furnace constant heatingrate 1h to 150 DEG C, then with 13 DEG C/min Speed constant heatingrate to 1180 DEG C -1220 DEG C；
5. it is incubated：In 1180 DEG C of -1220 DEG C of insulation 2h-4h, then take out and ooze tank；
6. cool down：Ullage will be oozed and be cooled to room temperature；
7. sample：Opening oozes tank, takes out the sample after pack cementation；
8. cleaning, drying：Sample after pack cementation is put into ethanol and cleaned, is dried in railway carriage or compartment is dried, is obtained in tantalum and the conjunction of tantalum base Gold surface is impregnated with Si-B-Y high-temperature oxidation resistant coating.
6. a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 5, it is characterised in that step 1. ethanol solution described in is absolute ethyl alcohol, concentration >=99.7%；Step 1. described in be cleaned by ultrasonic the time be 5 min -10 min。
7. a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 5, it is characterised in that step 2. drum's speed of rotation described in is 30r/min-40r/min, and the milling time is 90min-240min, after the grinding The mesh of penetration enhancer granularity >=300；Step 2. described in drying temperature be 100 DEG C -120 DEG C, drying time is 1.0h-1.5h.
8. a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 5, it is characterised in that step 3. the compound method of sealant described in is：100g high temperature clays are taken, 20ml Ludox is added, stirs into pasty state.
9. a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 5, it is characterised in that step 8. ethanol described in is absolute ethyl alcohol, and concentration >=99.7%, the drying temperature is 100 DEG C -120 DEG C, and drying time is 4 min- 6 min。
10. a kind of method for preparing tantalum and tantalum alloy surface Si-B-Y coatings as claimed in claim 5, it is characterised in that step Suddenly 8. gained coating layer thickness is 20 μm -40 μm.
CN201710489407.9A 2017-06-24 2017-06-24 A kind of penetration enhancer and method for preparing tantalum and tantalum alloy surface Si B Y coatings Pending CN107267915A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108823525A (en) * 2018-06-15 2018-11-16 金堆城钼业股份有限公司 A kind of preparation method of pure two step of molybdenum surface embedding silicon boron yttrium anti-oxidation composite coating
CN108914054A (en) * 2018-07-17 2018-11-30 北方民族大学 The preparation process and its penetration enhancer of nickel-base alloy surface oxidation-resistant heat and corrosion resistant Cr-Si-B-Y coating
CN110863172A (en) * 2019-11-16 2020-03-06 北方民族大学 Cr-Si-Zr-B permeating agent and application method thereof on tantalum and tantalum alloy surface
CN112941459A (en) * 2021-01-29 2021-06-11 中国人民解放军军事科学院国防科技创新研究院 Refractory high-entropy alloy surface oxidation-resistant coating and preparation method thereof
CN113025951A (en) * 2021-03-02 2021-06-25 南昌大学 Molybdenum alloy containing antioxidant composite coating and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58177458A (en) * 1982-04-12 1983-10-18 Sumitomo Metal Ind Ltd Cementation method of nickel-chromium alloy
CN102534469A (en) * 2011-11-25 2012-07-04 厦门虹鹭钨钼工业有限公司 High temperature anti-oxidation coating molybdenum material and preparation method thereof
CN102912290A (en) * 2012-09-06 2013-02-06 西北工业大学 Preparation method of antioxidation Si-Zr-Y seepage coating on Nb-Ti-Si-base alloy surface
RU2011145048A (en) * 2011-11-07 2013-05-20 Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" METHOD FOR APPLYING MULTICOMPONENT PROTECTIVE COATING ON PRODUCTS FROM STEEL OR TITANIUM
CN104911537A (en) * 2015-06-09 2015-09-16 西北工业大学 Nb-Ti-Si-base alloy surface B-Y modified silicide coating and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58177458A (en) * 1982-04-12 1983-10-18 Sumitomo Metal Ind Ltd Cementation method of nickel-chromium alloy
RU2011145048A (en) * 2011-11-07 2013-05-20 Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" METHOD FOR APPLYING MULTICOMPONENT PROTECTIVE COATING ON PRODUCTS FROM STEEL OR TITANIUM
CN102534469A (en) * 2011-11-25 2012-07-04 厦门虹鹭钨钼工业有限公司 High temperature anti-oxidation coating molybdenum material and preparation method thereof
CN102912290A (en) * 2012-09-06 2013-02-06 西北工业大学 Preparation method of antioxidation Si-Zr-Y seepage coating on Nb-Ti-Si-base alloy surface
CN104911537A (en) * 2015-06-09 2015-09-16 西北工业大学 Nb-Ti-Si-base alloy surface B-Y modified silicide coating and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曲江龙: "钼表面B,Y改性包埋渗Si涂层研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108823525A (en) * 2018-06-15 2018-11-16 金堆城钼业股份有限公司 A kind of preparation method of pure two step of molybdenum surface embedding silicon boron yttrium anti-oxidation composite coating
CN108914054A (en) * 2018-07-17 2018-11-30 北方民族大学 The preparation process and its penetration enhancer of nickel-base alloy surface oxidation-resistant heat and corrosion resistant Cr-Si-B-Y coating
CN108914054B (en) * 2018-07-17 2020-07-10 北方民族大学 Preparation process of oxidation-resistant hot corrosion-resistant Cr-Si-B-Y coating on surface of nickel-based alloy and penetrating agent thereof
CN110863172A (en) * 2019-11-16 2020-03-06 北方民族大学 Cr-Si-Zr-B permeating agent and application method thereof on tantalum and tantalum alloy surface
CN112941459A (en) * 2021-01-29 2021-06-11 中国人民解放军军事科学院国防科技创新研究院 Refractory high-entropy alloy surface oxidation-resistant coating and preparation method thereof
CN113025951A (en) * 2021-03-02 2021-06-25 南昌大学 Molybdenum alloy containing antioxidant composite coating and preparation method thereof
CN113025951B (en) * 2021-03-02 2022-06-07 南昌大学 Molybdenum alloy containing antioxidant composite coating and preparation method thereof

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