CN108034922A - Refractory metal surfaces B is modified MoSi2The penetration enhancer and coating production of coating - Google Patents
Refractory metal surfaces B is modified MoSi2The penetration enhancer and coating production of coating Download PDFInfo
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- CN108034922A CN108034922A CN201711340381.8A CN201711340381A CN108034922A CN 108034922 A CN108034922 A CN 108034922A CN 201711340381 A CN201711340381 A CN 201711340381A CN 108034922 A CN108034922 A CN 108034922A
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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 discloses a kind of refractory metal surfaces B to be modified MoSi2The penetration enhancer of coating, by the powder constituent of following mass percent：Alumina powder 5%~65%, boron powder 10%~15%, sodium fluoride powder 1%~8%, surplus are silica flour.The invention also discloses prepare B in refractory metal surfaces using the penetration enhancer to be modified MoSi2Coating process, this method are：First, polished successively the surface of refractory metal surfaces refractory metal, sandblasting, ungrease treatment and pickling；2nd, ball milling mixing powder prepares penetration enhancer；Three obtain B by embedding co-penetrating method in refractory metal surfaces is modified MoSi2Coating.B prepared by the present invention is modified MoSi2Coating forms rich B phases in coating/insoluble metal basal body interface, can effectively reduce the counterdiffusion degree between coating/matrix, so as to reduce the degeneration at high temperature speed of coating, and then extends the high-temperature service service life of coating.
Description
Technical field
The invention belongs to high temperature protection technical field, and in particular to a kind of refractory metal surfaces B is modified MoSi2Coating and its
Preparation method.
Background technology
Refractory alloy possesses excellent elevated temperature strength and toughness and good processing performance, in aerospace industry, aviation work
It is widely used in industry and atomic energy industry.However, refractory alloy application in high-temperature oxidation environment can occur sternly
Re-oxidation and fail, therefore, the high-temperature oxidation resistance for improving refractory metal be ensure its high-temperature service performance key.Relatively
In alloying, applying high-temperature protection coating individually can be designed matrix and coating, while meet mechanical property and high temperature
The requirement of antioxygenic property, is proved to be to ensure that refractory metal is on active service maximally efficient means in high-temperature oxidation environment.
Under high temperature oxidizing conditions, silicide coating generates SiO by the way that the selective oxidations of Si elements occurs2Glass protection
Film, protection is provided for matrix, good high temperature resistance (1000 DEG C~1700 DEG C) oxidation susceptibility has been shown, moreover, SiO2Glass
Film softens at high temperature, can stickiness flowing, the crackle formed in coating preparation process or oxidizing process, hole can be made up
The defects of hole, shown good " self-healing " ability, become the most important high-temperature protection coating of refractory alloy.
In silicide coating material, MoSi2Fusing point is high, medium density, excellent combination property, in high-temperature oxidation process
Due to volatile oxidation product MoO3Timely volatilization, MoSi2Surface can form complete, continuous SiO2Protective film, Ke Yiyou
Effect prevents the diffusion of oxygen, it is considered to be very potential high-temperature protection coating material.However, MoSi2In relatively low oxidizing temperature
Under (300~1000 DEG C) easily occur dusting, low temperature antioxygenic property deficiency；On the other hand, under hot conditions, MoSi2Coating with
High-temperature interface diffusion reaction occurs for refractory alloy matrix, causes coating moderate resistance oxidizing elements Si quickly to consume, greatly reduces
The service life of coating.These problems limit its high temperature application to a certain extent, to MoSi2Coating carries out unitary or polynary
It is modified, its high temperature protection performance is improved, is the hot spot studied at present.
The content of the invention
The technical problems to be solved by the invention are in view of the above shortcomings of the prior art, there is provided a kind of refractory metal
Surface B is modified MoSi2The penetration enhancer of coating.The coating optimizes Si-B co-penetration technologies, and control infusibility by varying the formula of penetration enhancer
The pre-treating technology of metal, can prepare the high quality B that thickness is 5 μm~50 μm in refractory metal surfaces and be modified MoSi2Apply
Layer, the B are modified MoSi2Coating can form rich B phases in coating/basal body interface, can effectively reduce the mutual expansion between coating/matrix
The degree of dissipating, so as to reduce the degeneration at high temperature speed of coating, and then extends the high-temperature service service life of coating.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of refractory metal surfaces B is modified MoSi2
The penetration enhancer of coating, it is characterised in that by the powder constituent of following mass percent：Alumina powder 5%~65%, boron powder 10%~
15%, sodium fluoride powder 1%~8%, surplus is silica flour.
A kind of above-mentioned refractory metal surfaces B is modified MoSi2The penetration enhancer of coating, it is characterised in that by following quality percentage
Several powder constituents：Alumina powder 40%~55%, boron powder 10%~15%, sodium fluoride powder 2%~5%, surplus are silica flour.
A kind of above-mentioned refractory metal surfaces B is modified MoSi2The penetration enhancer of coating, it is characterised in that by following quality percentage
Several powder constituents：Aluminium oxide 50%, boron powder 10%, sodium fluoride powder 5%, surplus are silica flour.
In addition, preparing B in refractory metal surfaces using above-mentioned penetration enhancer present invention also offers one kind is modified MoSi2Coating
Method, it is characterised in that this method comprises the following steps：
Step 1: polished successively the surface of refractory metal, sandblasting, ungrease treatment and pickling；The blasting treatment
The sand grains used is emergy or oxidation zircon sand, and the pressure of the blasting treatment is 0.2MPa~0.4MPa, and blast time is
1min~5min；The refractory metal is Mo, Mo alloy, Nb alloys, Ta alloys or W alloy, the Nb alloys, Ta alloys or W
The surface of alloy has Mo layers of the continuous metal not less than 10 μ m-thicks；
Step 2: it is uniform that alumina powder, silica flour, boron powder and sodium fluoride powder be placed in ball milling mixing in ball mill, obtain
Penetration enhancer；
Step 4: the refractory metal after pickling in step 1 is fully embedded the aluminium oxide equipped with penetration enhancer described in step 2
In crucible, it is subsequently placed in vacuum sintering furnace, is 1.0 × 10 in vacuum-3~7.0 × 10-3Under conditions of Pa, with 10 DEG C/
The speed of min~30 DEG C/min is warming up to 900 DEG C~1300 DEG C, and insulation 30min~300min carries out B-Si permeations, furnace cooling
The B for obtaining 5 μm~50 μ m-thicks in refractory metal surfaces afterwards is modified MoSi2Coating.
Above-mentioned method, it is characterised in that the acid solution used in step 2 during pickling by hydrofluoric acid and concentrated nitric acid by (6~
7):The volume ratio of (3~4) mixes, and the mass concentration of the hydrofluoric acid is 40%~60%, and the quality of the concentrated nitric acid is dense
Spend for 65%~68%；The pickling time is 1min~5min.
Above-mentioned method, it is characterised in that the particle diameter of alumina powder, silica flour, boron powder and sodium fluoride described in step 2
Respectively less than 40 μm.
Above-mentioned method, it is characterised in that the rotating speed of ball mill described in step 2 is 280r/min~340r/min, institute
The time for stating ball milling is 10min~60min, ratio of grinding media to material 3：1.
The present invention has the following advantages compared with prior art：
1st, the B that this method obtains is modified MoSi2Coating can significantly improve the crackle of coating surface oxidation generation glass-film
" self-healing " ability, in the more unmodified MoSi of ability of middle low temperature resistant " pest " oxidation2Coating significantly improves.
2nd, the B that this method obtains is modified MoSi2Coating can form rich B phases in coating/basal body interface, can effectively reduce
Counterdiffusion degree between coating/matrix, so as to reduce the degeneration at high temperature speed of coating, and then extends the high-temperature service longevity of coating
Life.
3rd, the B that the present invention obtains on insoluble metal surface is modified MoSi2Coating, the B are modified MoSi2Coating is in 1400 DEG C of perseverances
After temperature oxidation 1h, continuous glass-film is generated in coating surface, which has effectively healed the micro-flaw of coating surface, applies
Layer has shown good high-temperature oxidation resistance.
Technical scheme is described in further detail below by drawings and examples.
Brief description of the drawings
Fig. 1 is that B prepared by the embodiment of the present invention 1 is modified MoSi2The XRD spectrum of coating.
Fig. 2 is that B prepared by the embodiment of the present invention 1 is modified MoSi2The surface SEM photograph of coating.
Fig. 3 is that B prepared by the embodiment of the present invention 1 is modified MoSi2The section SEM photograph of coating.
Fig. 4 is that B prepared by the embodiment of the present invention 1 is modified MoSi2Surface SEM photograph of the coating after 1400 DEG C aoxidize 1h.
Embodiment
Embodiment 1
The refractory metal surfaces B of the present embodiment is modified MoSi2The penetration enhancer of coating by following mass percent powder constituent：
Aluminium oxide 50%, boron powder 10%, sodium fluoride powder 5%, surplus are silica flour.
The refractory metal basal body of the present embodiment is Mo1, and B is modified MoSi2The preparation of coating comprises the following steps：
Step 1: polished successively Mo1 metallic matrixes, sandblasting, ungrease treatment and the pickling of 3min；At the sandblasting
The sand grains used is managed as emergy；The pressure of the blasting treatment is 0.4MPa, blast time 4min；Preferably, by infusibility
Metal, which is immersed in acetone, carries out ungrease treatment；The acid solution that the pickling uses is by hydrofluoric acid and concentrated nitric acid by volume 7:3 mixing
Form, the mass concentration of the hydrofluoric acid is 50%, and the mass concentration of the concentrated nitric acid is 67%；
Step 2: alumina powder, silica flour, boron powder and sodium fluoride powder are weighed in proportion, the raw material powder that then will be weighed
End is placed in ball mill that ball milling mixing is uniform together, obtains penetration enhancer；The rotating speed of the ball mill is 310r/min, the ball milling
Time is 35min, ratio of grinding media to material 3：1, the alumina powder, silica flour, the particle diameter of boron powder and sodium fluoride are respectively less than 40 μm；
Step 3: the Mo1 metallic matrixes handled well in step 1 are fully embedded the oxygen equipped with penetration enhancer described in step 2
Change in aluminium crucible, be then placed in vacuum sintering furnace, be 7.0 × 10 in vacuum-3B-Si permeations are carried out under conditions of Pa,
The B that thickness is 20 μm is obtained in refractory metal surfaces be modified MoSi after furnace cooling2Coating；The detailed process of the high-temperature melting
For：120min is kept the temperature after being warming up to 1200 DEG C with the heating rate of 10 DEG C/min.
The MoSi that the present embodiment is prepared on Mo1 surfaces2Coating, Fig. 1 are the B that the present embodiment is prepared on Mo1 metallic matrixes
Modified MoSi2The XRD spectrum of coating, from figure 1 it appears that the B that the present embodiment is prepared in Mo1 metal surfaces is modified MoSi2Apply
Layer is mainly by MoSi2、MoB2, MoB and SiO2Form.Fig. 2 is that the B that the present embodiment is prepared on Mo1 metallic matrixes is modified MoSi2
The surface SEM photograph of coating, from figure 2 it can be seen that B is modified MoSi2Coating surface is flat, and coating germinates in preparation process
Micro-flaw.Fig. 3 is that the B that the present embodiment is prepared on Mo1 metallic matrixes is modified MoSi2The section SEM photograph of coating,
As can be seen that B is modified MoSi from the pattern photo of Fig. 3 median surfaces2Coating is continuous and thickness is uniform, in coating at basal body interface
Form boron-rich phase.Fig. 4 is modified MoSi for B manufactured in the present embodiment2Surface SEM photograph of the coating after 1400 DEG C of oxidation 1h,
Figure 4, it is seen that after 1400 DEG C of constant temperature oxidation 1h, in MoSi2Coating surface generates continuous glass-film, which has
The micro-flaw for the coating surface that healed is imitated, coating has shown good high-temperature oxidation resistance.
Embodiment 2
The refractory metal surfaces B of the present embodiment is modified MoSi2The penetration enhancer of coating by following mass percent powder constituent：
Aluminium oxide 45%, boron powder 10%, sodium fluoride powder 5%, surplus are silica flour.
The refractory metal basal body of the present embodiment is the Nb521 niobium alloys of Mo layers of the continuous metal with 10 μ m-thicks, in utilization
State penetration enhancer and B modifications MoSi is prepared on Nb521 niobium alloys surface2The method of coating comprises the following steps：
Step 1: to thickness for 10 μm of o layer of continuous Ns Nb521 niobium alloys matrix polished successively, sandblasting, take off
Fat processing and the pickling of 2min；The sand grains that the blasting treatment uses is emergy；The pressure of the blasting treatment is 0.2MPa,
Blast time is 2min；Preferably, refractory metal basal body is immersed in acetone and carries out ungrease treatment；The acid solution that the pickling uses
By hydrofluoric acid and concentrated nitric acid by volume 6:3 mix, and the mass concentration of the hydrofluoric acid is 40%, the matter of the concentrated nitric acid
It is 68% to measure concentration；
Step 2: alumina powder, silica flour, boron powder and sodium fluoride powder are weighed in proportion, the raw material powder that then will be weighed
End is placed in ball mill that ball milling mixing is uniform together, obtains penetration enhancer；The rotating speed of the ball mill is 280r/min, the ball milling
Time is 60min, ratio of grinding media to material 3：1, the alumina powder, silica flour, the particle diameter of boron powder and sodium fluoride are respectively less than 40 μm；
Step 3: by what is handled well in step 1 there is thickness to be fully embedded for the Nb521 niobium alloys of 10 μm of o layers of continuous Ns
In alumina crucible equipped with penetration enhancer described in step 2, be then placed in vacuum sintering furnace, vacuum for 4.0 ×
10-3B-Si permeations are carried out under conditions of Pa, obtaining the B that thickness is 25 μm in refractory metal surfaces after furnace cooling is modified MoSi2
Coating；The detailed process of the high-temperature melting is：300min is kept the temperature after being warming up to 900 DEG C with the heating rate of 20 DEG C/min.
The present embodiment is main for MoSi2 coatings prepared by the Nb521 niobium alloys surface of 10 μm of o layers of continuous Ns with thickness
By MoSi2、MoB2, MoB and SiO2Form, B is modified MoSi2Coating surface is flat, and coating is continuous and thickness is uniform, and coating is being made
Micro-flaw is germinated during standby, and boron-rich phase is formd at basal body interface in coating.B manufactured in the present embodiment is modified
MoSi2Coating generates continuous glass-film after 1400 DEG C aoxidize 1h, in coating surface oxidation, which has effectively healed painting
The micro-flaw of layer surface, coating have shown good high-temperature oxidation resistance.
Embodiment 3
The refractory metal surfaces B of the present embodiment is modified MoSi2The penetration enhancer of coating by following mass percent powder constituent：
Aluminium oxide 55%, boron powder 12%, sodium fluoride powder 2%, surplus are silica flour.
The refractory metal basal body of the present embodiment has the Ta10W alloys of Mo layers of the continuous metal of 15 μ m-thicks, is oozed using above-mentioned
Agent prepares B in Ta10W alloy surfaces and is modified MoSi2The method of coating comprises the following steps：
Step 1: to thickness for 15 μm of o layers of continuous Ns Ta10W alloy substrates polished successively, sandblasting, degreasing
Processing and the pickling of 1min；The sand grains that the blasting treatment uses is emergy；The pressure of the blasting treatment is 0.3MPa, spray
The sand time is 3min；Preferably, refractory metal basal body is immersed in acetone and carries out ungrease treatment；The acid solution that the pickling uses by
Hydrofluoric acid and concentrated nitric acid by volume 7:4 mix, and the mass concentration of the hydrofluoric acid is 60%, the quality of the concentrated nitric acid
Concentration is 67%；
Step 2: alumina powder, silica flour, boron powder and sodium fluoride powder are weighed in proportion, the raw material powder that then will be weighed
End is placed in ball mill that ball milling mixing is uniform together, obtains penetration enhancer；The rotating speed of the ball mill is 340r/min, the ball milling
Time is 10min, ratio of grinding media to material 3：1, the alumina powder, silica flour, the particle diameter of boron powder and sodium fluoride are respectively less than 40 μm；
Step 3: by what is handled well in step 1 there is thickness to be fully embedded dress for the Ta10W alloys of 15 μm of o layers of continuous Ns
In the alumina crucible for having penetration enhancer described in step 2, then it is placed in vacuum sintering furnace, is 1.0 × 10 in vacuum- 3B-Si permeations are carried out under conditions of Pa, obtaining the B that thickness is 30 μm in refractory metal surfaces after furnace cooling is modified MoSi2Apply
Layer；The detailed process of the high-temperature melting is：30min is kept the temperature after being warming up to 1300 DEG C with the heating rate of 30 DEG C/min.
The present embodiment with thickness for the Ta10W alloy surfaces preparation of 15 μm of o layer of continuous Ns MoSi2 coatings mainly by
MoSi2、MoB2, MoB and SiO2Form, B is modified MoSi2Coating surface is flat, and coating is continuous and thickness is uniform, prepared by coating
During germinated micro-flaw, and boron-rich phase is formd at basal body interface in coating.B manufactured in the present embodiment is modified
MoSi2Coating generates continuous glass-film after 1500 DEG C aoxidize 1h, in coating surface oxidation, which has effectively healed painting
The micro-flaw of layer surface, coating have shown good high-temperature oxidation resistance.
Embodiment 4
The refractory metal surfaces B of the present embodiment is modified MoSi2The penetration enhancer of coating by following mass percent powder constituent：
Aluminium oxide 65%, boron powder 10%, sodium fluoride powder 1%, surplus are silica flour.
The refractory metal basal body of the present embodiment is the W1 alloys of Mo layers of the continuous metal with 20 μ m-thicks, utilizes above-mentioned penetration enhancer
B, which is prepared, in W1 alloy surfaces is modified MoSi2The method of coating comprises the following steps：
Step 1: to thickness for 20 μm of o layers of continuous Ns W1 alloy substrates polished successively, sandblasting, ungrease treatment
With the pickling of 3min；The sand grains that the blasting treatment uses is oxidation zircon sand；The pressure of the blasting treatment is 0.3MPa, sandblasting
Time is 5min；Preferably, refractory metal basal body is immersed in acetone and carries out ungrease treatment；The acid solution that the pickling uses is by hydrogen
Fluoric acid and concentrated nitric acid by volume 6:4 mix, and the mass concentration of the hydrofluoric acid is 40%, and the quality of the concentrated nitric acid is dense
Spend for 68%；
Step 2: alumina powder, silica flour, boron powder and sodium fluoride powder are weighed in proportion, the raw material powder that then will be weighed
End is placed in ball mill that ball milling mixing is uniform together, obtains penetration enhancer；The rotating speed of the ball mill is 300r/min, the ball milling
Time is 30min, ratio of grinding media to material 3：1, the alumina powder, silica flour, the particle diameter of boron powder and sodium fluoride are respectively less than 40 μm；
Step 3: by what is handled well in step 1 there is thickness to be fully embedded for the W1 alloys of 20 μm of o layers of continuous Ns equipped with step
Described in rapid two in the alumina crucible of penetration enhancer, then it is placed in vacuum sintering furnace, is 3.0 × 10 in vacuum-3Pa's
Under the conditions of carry out B-Si permeations, after furnace cooling refractory metal surfaces obtain thickness be 48 μm B be modified MoSi2Coating；Institute
The detailed process for stating high-temperature melting is：200min is kept the temperature after being warming up to 1000 DEG C with the heating rate of 20 DEG C/min.
The present embodiment with thickness for the W1 alloy surfaces preparation of 20 μm of o layer of continuous Ns MoSi2 coatings mainly by
MoSi2、MoB2, MoB and SiO2Form, B is modified MoSi2Coating surface is flat, and coating is continuous and thickness is uniform, prepared by coating
During germinated micro-flaw, and boron-rich phase is formd at basal body interface in coating.B manufactured in the present embodiment is modified
MoSi2Coating generates continuous glass-film after 1500 DEG C aoxidize 2h, in coating surface oxidation, which has effectively healed painting
The micro-flaw of layer surface, coating have shown good high-temperature oxidation resistance.
Embodiment 5
The refractory metal surfaces B of the present embodiment is modified MoSi2The penetration enhancer of coating by following mass percent powder constituent：
Aluminium oxide 5%, boron powder 15%, sodium fluoride powder 8%, surplus are silica flour.
The refractory metal basal body of the present embodiment is the C103 alloys of Mo layers of the continuous metal with 10 μ m-thicks, is oozed using above-mentioned
Agent prepares B in C103 alloy surfaces and is modified MoSi2The method of coating comprises the following steps：
Step 1: to being polished successively for the C103 alloy substrates of 10 μm of o layers of continuous Ns with thickness, sandblasting, at degreasing
The pickling of reason and 5min；The sand grains that the blasting treatment uses is emergy；The pressure of the blasting treatment is 0.3MPa, sandblasting
Time is 3min；Preferably, refractory metal basal body is immersed in acetone and carries out ungrease treatment；The acid solution that the pickling uses is by hydrogen
Fluoric acid and concentrated nitric acid by volume 6.5:3.5 mix, and the mass concentration of the hydrofluoric acid is 50%, the matter of the concentrated nitric acid
It is 67% to measure concentration；
Step 2: alumina powder, silica flour, boron powder and sodium fluoride powder are weighed in proportion, the raw material powder that then will be weighed
End is placed in ball mill that ball milling mixing is uniform together, obtains penetration enhancer；The rotating speed of the ball mill is 310r/min, the ball milling
Time is 45min, ratio of grinding media to material 3：1, the alumina powder, silica flour, the particle diameter of boron powder and sodium fluoride are respectively less than 40 μm；
Step 3: the C103 alloys with 10 μm of o layers of continuous Ns handled well in step 1 are fully embedded equipped with step 2
Described in penetration enhancer alumina crucible in, be then placed in vacuum sintering furnace, vacuum be 4.0 × 10-3The condition of Pa
Lower progress B-Si permeations, obtain the B that thickness is 5 μm in refractory metal surfaces after furnace cooling and are modified MoSi2Coating；The high temperature
The detailed process fused is：120min is kept the temperature after being warming up to 1200 DEG C with the heating rate of 15 DEG C/min.
The present embodiment with thickness for the C103 alloy surfaces preparation of 10 μm of o layer of continuous Ns MoSi2 coatings mainly by
MoSi2、MoB2, MoB and SiO2Form, B is modified MoSi2Coating surface is flat, and coating is continuous and thickness is uniform, prepared by coating
During germinated micro-flaw, and boron-rich phase is formd at basal body interface in coating.B manufactured in the present embodiment is modified
MoSi2Coating generates continuous glass-film after 1400 DEG C aoxidize 2h, in coating surface oxidation, which has effectively healed painting
The micro-flaw of layer surface, coating have shown good high-temperature oxidation resistance.
The above, is only presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art substantially makees above example, still fall within technical solution of the present invention
Protection domain in.
Claims (7)
1. a kind of refractory metal surfaces B is modified MoSi2The penetration enhancer of coating, it is characterised in that by the powder group of following mass percent
Into：Alumina powder 5%~65%, boron powder 10%~15%, sodium fluoride powder 1%~8%, surplus are silica flour.
2. refractory metal surfaces B described in accordance with the claim 1 is modified MoSi2The penetration enhancer of coating, it is characterised in that by following matter
Measure the powder constituent of percentage：Alumina powder 40%~55%, boron powder 10%~15%, sodium fluoride powder 2%~5%, surplus
For silica flour.
3. refractory metal surfaces B described in accordance with the claim 2 is modified MoSi2The penetration enhancer of coating, it is characterised in that by following matter
Measure the powder constituent of percentage：Aluminium oxide 50%, boron powder 10%, sodium fluoride powder 5%, surplus are silica flour.
4. one kind prepares B in refractory metal surfaces using the penetration enhancer of claim 1,2 or 3 and is modified MoSi2The method of coating, its
It is characterized in that, this method comprises the following steps：
Step 1: polished successively the surface of refractory metal, sandblasting, ungrease treatment and pickling；The blasting treatment uses
Sand grains be emergy or oxidation zircon sand, the pressure of the blasting treatment be 0.2MPa~0.4MPa, blast time be 1min~
5min；The refractory metal is Mo, Mo alloy, Nb alloys, Ta alloys or W alloy, the Nb alloys, Ta alloys or W alloy
Surface has Mo layers of the continuous metal not less than 10 μ m-thicks；
Step 2: it is uniform that alumina powder, silica flour, boron powder and sodium fluoride powder be placed in ball milling mixing in ball mill, penetration enhancer is obtained；
Step 3: the refractory metal after pickling in step 1 is fully embedded the alumina crucible equipped with penetration enhancer described in step 2
In, it is subsequently placed in vacuum sintering furnace, is 1.0 × 10 in vacuum-3~7.0 × 10-3Under conditions of Pa, with 10 DEG C/min~
The speed of 30 DEG C/min is warming up to 900 DEG C~1300 DEG C, and insulation 30min~300min carries out B-Si permeations, after furnace cooling
The B that refractory metal surfaces obtain 5 μm~50 μ m-thicks is modified MoSi2Coating.
5. in accordance with the method for claim 4, it is characterised in that the acid solution used in step 2 during pickling is by hydrofluoric acid and dense
Nitric acid presses (6~7):The volume ratio of (3~4) mixes, and the mass concentration of the hydrofluoric acid is 40%~60%, the dense nitre
The mass concentration of acid is 65%~68%；The pickling time is 1min~5min.
6. in accordance with the method for claim 4, it is characterised in that alumina powder described in step 2, silica flour, boron powder and fluorination
The particle diameter of sodium is respectively less than 40 μm.
7. in accordance with the method for claim 4, it is characterised in that the rotating speed of ball mill described in step 2 for 280r/min~
340r/min, time of the ball milling are 10min~60min, ratio of grinding media to material 3：1.
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Cited By (5)
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| CN109666886A (en) * | 2018-12-28 | 2019-04-23 | 河南科技大学 | A kind of preparation method of molybdenum base material surface oxidation-resistant coating |
| CN109972081A (en) * | 2019-05-05 | 2019-07-05 | 中国人民解放军空军工程大学 | A kind of molybdenum silicon boron powder for metal part surface infiltration layer and preparation method thereof and infiltration layer preparation method |
| CN114107888A (en) * | 2021-11-19 | 2022-03-01 | 中南大学 | Novel tantalum-based Si-Mo-ZrB containing TaB diffusion barrier layer2Composite coating and three-step preparation method thereof |
| CN114892163A (en) * | 2022-05-09 | 2022-08-12 | 宁夏东方钽业股份有限公司 | High-temperature antioxidant protective coating material, preparation method and application |
| CN117448808A (en) * | 2023-10-31 | 2024-01-26 | 北京工业大学 | Nb-Si-based alloy surface high-temperature oxidation-resistant gradient structure coating material and preparation method thereof |
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| CN109666886A (en) * | 2018-12-28 | 2019-04-23 | 河南科技大学 | A kind of preparation method of molybdenum base material surface oxidation-resistant coating |
| CN109972081A (en) * | 2019-05-05 | 2019-07-05 | 中国人民解放军空军工程大学 | A kind of molybdenum silicon boron powder for metal part surface infiltration layer and preparation method thereof and infiltration layer preparation method |
| CN114107888A (en) * | 2021-11-19 | 2022-03-01 | 中南大学 | Novel tantalum-based Si-Mo-ZrB containing TaB diffusion barrier layer2Composite coating and three-step preparation method thereof |
| CN114892163A (en) * | 2022-05-09 | 2022-08-12 | 宁夏东方钽业股份有限公司 | High-temperature antioxidant protective coating material, preparation method and application |
| CN114892163B (en) * | 2022-05-09 | 2023-11-21 | 宁夏东方钽业股份有限公司 | High-temperature antioxidant protective coating material, preparation method and application |
| CN117448808A (en) * | 2023-10-31 | 2024-01-26 | 北京工业大学 | Nb-Si-based alloy surface high-temperature oxidation-resistant gradient structure coating material and preparation method thereof |
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