CN108585897A - A kind of refractory metal high-temperature oxidation resistant Si-Mo-YSZ coatings and preparation method thereof - Google Patents
A kind of refractory metal high-temperature oxidation resistant Si-Mo-YSZ coatings and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to anti-oxidant Si Mo YSZ ceramic coatings of a kind of refractory metal material surface high-temp and preparation method thereof.The coating material includes by percentage to the quality：Si45%~65%, Mo25%~40%, YSZ2%~15%, additive 2%~8%.Coating material is made slurry first and slurry is coated in refractory metal surfaces by the present invention, and coating is made through 1370 DEG C~1530 DEG C sintering 20min~90min.The present invention matches refractory metal basal body coefficient of thermal expansion by rational allocation coating composition, and coating can quickly form ZrSiO in use4‑ZrO2‑SiO2Complex oxide film effectively reduces the diffusion coefficient of coating, realizes long-time anti-oxidant use of all kinds of refractory metal materials in 1700 DEG C or more high temperature.Present invention process is simple, at low cost, and coating is thermally matched preferably with matrix, can effectively improve the high-temperature oxidation resistance of refractory metal.
Description
Technical field
The invention belongs to high-temperature oxidation resistant coating preparing technical fields, and in particular to a kind of refractory metal material high temperature antioxygen
Change Si-Mo-YSZ coatings and preparation method thereof.
Background technology
It is excellent that refractory metal and its alloy have that elevated temperature strength is high, processing plasticity is good, anti-liquid metal corrosion ability is strong etc.
Point, use temperature range are higher than high temperature alloy, therefore be widely used in aerospace industry, nuclear industry up to 1300 DEG C~2300 DEG C
And other high-temperature applications.But refractory metal is since oxygen affinity is high, solubility causes greatly its high-temperature oxidation resistance very poor,
Severe oxidation, mechanical behavior under high temperature just occurs when far below service temperature (700 DEG C or so) drastically to decline, limits it in height
Engineer application in warm aerobic environment.Currently, antioxidant coating is to solve refractory metal and its High Temperature Oxidation protection most
Effective means.
Currently, high-temperature oxidation-resistant coating for refractory includes coat of aluminide, noble coatings, boride coating and silication
Object coating.Coat of aluminide wherein with Al-Cr-Si, Al-Si and Al-Sn etc. for representative is widely used in aerospace neck
Domain has excellent creep, fatigue behaviour and middle low temperature antioxygenic property, but temperature in use is usually no more than 1500 DEG C；With Ir
Have the characteristics that fusing point is high, chemical inertness is good, oxygen permeability is low with the noble coatings that Pt is representative, protection temperature is up to 2200
DEG C, but the bottlenecks such as that there are prices is extremely high, technical threshold is high, requires special equipment, coating radiance low；With ZrB2And HfB2
Have the potentiality of superhigh temperature protection for the boride coating of representative, but can be only used for the short time protection as unit of s at present
And it is generally intended for single use, the long duration protection as unit of h can not be competent at and exists and refractory metal basal body coefficient of thermal expansion
It mismatches, the problems such as thermal shock performance is bad.Silicide coating is that current refractory metal is most widely used, high temperature antioxygen of most study
Change coating, antioxidation mechanism is mainly to form the low high temperature self-healing SiO of oxygen diffusion rate2Glass-film.Due to SiO2
Oxidation film fusing point is only 1600 DEG C of (quartz type)~1710 DEG C (cristobalite type), it is difficult to the Service Environment of competent higher temperature, because
This has carried out a large amount of coating modified researchs for different R＆D targets both at home and abroad, but due to modifying element selection principle, introducing shape
Formula, adding proportion can be directly changed coating structure, phase structure matching, coefficient of thermal expansion, high-temperature oxidation resistance and other are comprehensive
Performance is closed, is a complicated system engineering, in addition SiO2The basic data of the above superhigh temperature of fusing point, oxidation theory, protection machine
System research is still in the stage of fumbling, thus at present the temperature in use of open report be more than 1700 DEG C of silicide coating system still
It is less.
With the fast development of technology, high-temperature oxidation-resistant coating for refractory performance requirement is also stepped up, it would be highly desirable to rich
Richness can be in the high-temperature oxidation resistant coating system that 1700 DEG C and its temperatures above use, to adapt to the demand of different application environment.
Invention content
For the problem that the protection temperature of current high-temperature oxidation-resistant coating for refractory is relatively low, it is an object of the invention to carry
For the refractory metal Si-Mo-YSZ coatings and its system that a kind of preparation process is simple, cost is relatively low, superhigh temperature antioxygenic property is excellent
Standby technique, solve the problems, such as refractory metal basal body 1700 DEG C or more hyperthermal environments oxidation protection.
A kind of anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, the coating are raw materials used with quality hundred
It includes following components to divide than meter：
Si powder 45%~65%, preferably 49~59%, further preferably 54~59%；
Mo 25%~40%, preferably 25~35%, further preferably 25~31%；
YSZ 2%~15%, preferably 8~12%, further preferably 9.5~10.5%；Still more preferably it is
10%；
Additive 2%~8%, preferably 3~7.5%, further preferably 3~6%；
The additive is selected from SiO2Powder, NH3At least one of F powder, PVB powder.Preferably, the additive
By SiO2Powder, NH3At least two kinds compositions in F powder, PVB powder.
Wherein YSZ is the zirconium oxide of stabilized with yttrium oxide, and the additive amount of yttrium oxide mass fraction is 3%-10%.It is excellent to be preferably
8%.
A kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, includes the following steps：
Step 1
Match by design component and takes Si powder, Mo powders, YSZ powders, additive；It is uniformly mixed and slurry is made；It obtains spare
Material；
Step 2
Using the refractory metal that surface cleaning is dried as matrix, one layer of standby material is coated in matrix surface；Drying, obtains band
The matrix of standby material；
Step 3
Matrix with standby material obtained by step 2 is placed in sintering furnace, under protective atmosphere, in 1370 DEG C~1530 DEG C
It is sintered, keeps the temperature, it is cooling, obtain the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature.
Preferably, a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, step
In rapid one, matches by design component and take Si powder, Mo powders, YSZ powders, additive as raw material；Using alcoholic solution as ball-milling medium,
The mass ratio for controlling raw material and abrading-ball is 1：5~10, control rotational speed of ball-mill is 200r/min~400r/min；Ball milling 5h~15h,
Obtain standby material.The mass ratio of scheme as a further preference, raw material and ball-milling medium is 2:1~2:5.The ball-milling medium
Preferably ethyl alcohol.
A kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, in step 1, the Si
The average particle diameter size of powder is 0.5~5 μm, preferably 0.5~3 μm, and the average particle diameter size of the Mo powders is 2 μm~10 μ
The average particle diameter size of m, the YSZ powders are 0.1~3 μm, preferably 0.1~0.5 μm, the average grain of other additives
Diameter size is 0.1~10 μm.Si powders, Mo powders, YSZ powders purity be not less than 98%.
Preferably, a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, step
In rapid two, the refractory metal of surface cleaning drying is by made from following proposal：Refractory metal basal body is polished, through pickling,
After alkali cleaning processing, ultrasonic cleaning is clean in alcohol, is put into drying box and dries；Obtain the infusibility gold of surface cleaning drying
Belong to.
Preferably, a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, step
In rapid two, refractory metal is selected from Mo, Mo based alloy, Ta, Ta based alloy, Nb, Nb based alloy, one of W, W based alloy kind.
Preferably, a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, step
In rapid two, standby material obtained by step 1 is evenly applied to the infusibility of surface cleaning drying by the way of dip-coating and/or spraying
Metallic surface forms the coating that thickness is 120 μm~300 μm, is subsequently placed in baking oven and dries 20min in 70~200 DEG C
~120min；Obtain the matrix with standby material.
Preferably, a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention, step
In rapid three, the matrix with standby material obtained by step 2 is placed in sintering furnace, under protective atmosphere, with 5 DEG C/min~50 DEG C/
The heating rate of min is warming up to 1370 DEG C~1530 DEG C, cools down with stove after keeping the temperature 20min~90min, in refractory metal after cooling
Material surface obtains the Si-Mo-YSZ high-temperature oxidation resistant coatings that thickness is 80 μm~200 μm.
In step 3, the protective atmosphere is selected from least one of argon gas, helium, nitrogen.
Designed by of the invention and high-temperature oxidation resistant Si-Mo-YSZ coatings are prepared, are 6 1725 DEG C of static state anti-oxidant service life
~15 hours.
Preferably, a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature of the present invention is
It further improves performance, after completing step 3, can be used packet siliconizing treatment processes.The packet siliconizing treatment processes are：Coating will be prepared
Refractory metal samples be placed in the crucible containing packet bleed seal after be placed in vacuum sintering furnace, packet bleed is by mass percent
50%~75% Al2O3, 15%~25% Si and 5~15%NH4F form, under argon atmosphere in 1100 DEG C~
After 1300 DEG C of 2~6h of heat preservation coating sample is can be prepared by with stove cooling.
After optimized, the present invention is designed and prepares high-temperature oxidation resistant Si-Mo-YSZ coatings, in 1725 DEG C of static antioxygen
The change service life is 22.3h, is 10-12 hours 1800 DEG C of static state anti-oxidant service life.It carries out -1800 DEG C of cyclic oxidation examinations of room temperature
It tests, the service life recycles up to 214 times.
The principle of the invention
The coating of the present invention is using three kinds of Si powder, Mo powder and ultra-fine YSZ powder primary raw materials and is aided with NH3F、PVB、SiO2In
One or more additives, through high-temp in-situ reaction-sintered, react (1)~(5) formed with MoSi2、ZrSi2、SiO2For
The coating outer layer of main phase.Wherein NH3F promotes the progress of high-temp in-situ reaction as reacting movable agent；PVB as binder,
The formation for promoting coating idiosome, thickens conducive to coating；SiO2As allotment coating coefficient of thermal expansion.
3Si (l)+5Mo (s)=Mo5Si3(s) (1)
2Si (l)+Mo (s)=MoSi2(s) (2)
7Si(l)+Mo5Si3(s)=5MoSi2(s) (3)
Si(l)+ZrO2(s)=ZrSi (s)+SiO2(s) (4)
Si (l)+ZrSi (s)=ZrSi2(s) (5)
It selects ultra-fine YSZ powder and avoids selecting coarse YSZ powder, be mainly based upon superfines contact surface area
Bigger, the progress that high-temp in-situ can be promoted to react are conducive to formation and MoSi2The more matched ZrSi of main body phase2On the one hand phase may be used
To reduce coat inside stress, the tiny ZrSi of crystal grain is on the other hand formed2Mutually it is embedded in larger-size MoSi2The crystal boundary of phase
Region keeps coating finer and close.ZrSi2It is present in MoSi2Grain boundary area, can blocking crystal boundary, (high temperature oxygen rapidly enters in coating
The channel in portion), it is conducive to promote coating high-temp resistance oxygen permeability, to improve coating high-temp antioxygenic property to a certain degree.Y
On the one hand the introducing of element is conducive to coated grains refinement；On the other hand be conducive to inhibit ZrO2High/low temperature phase transition bring
Volume expansion, be conducive to promoted coating high-temp barrier propterty.
In the superhigh temperature oxidation process higher than 1700 DEG C, refractory metal basal body Si-Mo-YSZ coatings react (6)~
(10) ZrSiO is quickly formed4+ZrO2+SiO2Complex oxide film, due to ZrSiO4And ZrO2Fusing point distinguishes 2550 DEG C and 2715
DEG C, it is higher than SiO21670-1710 DEG C of fusing point, be conducive to improve oxidation film heat resistance；Due to high-melting-point ZrSiO4、ZrO2
The generation of solid particle so that the viscosity of complex oxide film improves, and reduces SiO2Rate of volatilization improves oxidation film resistance to erosion
Ability improves complex oxide film superhigh temperature antioxygenic property.
5MoSi2(s)+7O2(g)=Mo5Si3(s)+7SiO2(l) (6)
2Mo5Si3(s)+21O2(g)=10MoO3(g)+6SiO2(l) (7)
2MoSi2+7O2(g)=2MoO3(g)+4SiO2(l) (8)
ZrSi2(s)+3O2(g)=ZrSiO4(s)+SiO2(l) (9)
ZrSiO4(s)=ZrO2(s)+SiO2(l) (10)
The advantages of the present invention
1, the present invention is prepared using suitable Mo, Si and YSZ as coated body formula by simple slurry reaction sintering process
Outer layer is the MoSi that Y is modified2+ZrSi2+SiO2, internal layer MSi2+M5Si3(M refers to the member of refractory metal and its alloy base material
Element) composite coating, and the coefficient of thermal expansion of coating can be allocated according to the coefficient of thermal expansion of refractory metal alloy matrix, it is real
Now with the matched well of common refractory metal and its alloy, all kinds of defects caused by thermal stress are greatly reduced.The coating is super
The ZrO of high viscosity, low evaporation rate can be quickly formed in high-temperature oxidation environment2+ZrSiO4+SiO2Complex oxide film.With existing skill
Art ratio, product of the invention has excellent superhigh temperature antioxygenic property, after optimized, 1725 DEG C of static state anti-oxidant service life
10h or more is reached up to 22h or more, 1800 DEG C of static state anti-oxidant service life.
2, the present invention uses fused slurry method prepares coating.Compared with the prior art, preparation method of the invention without
The equipment such as relatively expensive plasma spraying, magnetron sputtering, chemical vapor deposition, preparation process is simple, and production cost is relatively low, fits
For refractory metal base material different, not of uniform size, and coating material is common finished industrial product raw material, and price is relatively low
It is honest and clean.
Description of the drawings：
Fig. 1 is that the original coating cross sections patterns of TZM molybdenum alloys Si-Mo-YSZ and its Surface scan are analyzed
Fig. 2 is Cross Section Morphology and its Surface scan of the TZM molybdenum alloy Si-Mo-YSZ coatings after 1725 DEG C of high-temperature oxydation 8h point
Analysis
The original coating cross sections patterns of Fig. 3 Ta-10W alloys Si-Mo-YSZ and its line scanning：(a) original coating cross sections
Pattern；(b) coating line scanning result
Fig. 4 Ta-10W alloy Si-Mo-YSZ coatings are in 1800 DEG C of oxidizing dynamics curves：(a) coating and uncoated coating
Ta-10W alloy oxidations after macro morphology comparison and its oxidation weight gain situation；(b) coating oxidation weightening square with the time
Fitted figure
Fig. 5 Ta-10W alloy Si-Mo-YSZ coatings aoxidize Cross Section Morphology and surface topography after 10h at 1800 DEG C：(a) it cuts
Face pattern；(b) surface topography
As can be seen from Figure 1 TZM molybdenum alloys Si-Mo-YSZ composite coatings can be divided into two layers, the i.e. MoSi containing Y2+ZrSi2
+SiO2Outer layer and pure MoSi2Internal layer.
As can be seen from Figure 2 TZM molybdenum alloys Si-Mo-YSZ coatings form disperse through 1725 DEG C of high-temperature oxydation rear surfaces
ZrO is distributed with2+ZrSiO4The SiO containing Y of refractory grain2Oxidation film, coating structure develop into the ZrO containing Y2+ZrSiO4+
SiO2MoSi of the oxide layer-containing Y2+ZrSi2+SiO2Coating outer layer-MoSi2Internal layer-Mo5Si3Boundary layer-molybdenum alloy matrix.
As can be seen from Figure 3 the original coating textures of Ta-10W alloys Si-Mo-YSZ are the MoSi containing Y2+ZrSi2+
SiO2Outer layer and TaSi2+WSi2Internal layer.
As can be seen from Figure 4 the Ta-10W alloys of uncoated coating in 1800 DEG C of atmospheric environments only 6 minutes just completely
Dusting, weightening reach 1770.227mg cm-2, and be coated under the same environment of Ta-10W alloys of Si-Mo-YSZ coatings and aoxidize 10h
It does not fail still afterwards, weightening is only 6.729mg cm-2, oxidation weight gain rate KpFor 4.378mg2cm-4h-1。
As can be seen from Figure 5 Ta-10W alloys Si-Mo-YSZ coatings form thick micro- up to 68 after 1800 DEG C aoxidize 10h
The complex oxide film of rice, the visible tiny micro-crack in surface layer, coating structure develop into the ZrO containing Y2+ZrSiO4+SiO2Oxide layer-contains
The MoSi of Y2+ZrSi2+SiO2Coating outer layer-TaSi2+WSi2Internal layer-Ta5Si3+W5Si3Boundary layer-tantalum-tungsten alloy matrix.
Specific implementation mode：
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment 1
(1) base material pre-processes:TZM molybdenum alloys are selected to be carried out with sand paper polishing after surface is smooth as base material
Pickling, alkali cleaning processing, hereafter ultrasonic cleaning is clean in alcohol, is put into drying box and dries.
(2) prepared by slurry：It is matched by the mass fraction of 58.5%Si powder, 29%Mo powder and 9.5%YSZ powder, three
Average grain diameter is respectively 1 μm, 3 μm and 100nm；Select 0.1 μm of SiO2Powder, 2 μm of NH3It is used as and adds in F powder, 5 μm of PVB powder
It is respectively 0.5%, 2% and 0.5% to add agent, mass fraction proportioning；The purity of six kinds of powder is not less than 99%.The painting that will be prepared
In layer raw material merging ball grinder, ball-milling medium is ethyl alcohol, ratio of grinding media to material 8:1, rotating speed 300r/min, Ball-milling Time 10h.
(3) it uniformly coats slurry and dries：Slurry described in (2) is evenly applied in (1) using spray coating method after drying
Molybdenum alloy substrate surface, surface formed thickness be about 140 μm coating idiosome, be subsequently placed in drying box at 110 DEG C dry
Dry 1h.
(4) vacuum-sintering：The molybdenum alloy sample of applying coating in (3) is put into vacuum sintering furnace, in argon gas ceiling
Under part, 1450 DEG C of sintering are warming up to the heating rate of 10 DEG C/min, are cooled down with stove after keeping the temperature 60min, sample is taken out after cooling.
(5) packet siliconising is handled：The sample for preparing coating is placed on after being sealed in the crucible containing packet bleed and is placed in very
Empty stove, packet bleed by mass percent 53% Al2O3, 25% Si and 12%NH4F form, under argon atmosphere in
Cool down with stove after 1150 DEG C of heat preservation 4h, the Si-Mo-YSZ high-temperature oxidation resistants that thickness is 120 μm are obtained in molybdenum alloy surface after cooling
Coating.Original coating cross sections pattern and its Surface scan analysis are as shown in Figure 1.
(6) the anti-oxidant Si-Mo-YSZ coating samples of molybdenum alloy superhigh temperature prepared by embodiment carry out static anti-at 1725 DEG C
Oxidation test, static anti-oxidant service life are 22.3h.Coating aoxidizes the Cross Section Morphology after 8h and its Surface scan analysis at 1725 DEG C
As shown in Figure 2.
Embodiment 2
(1) base material pre-processes:TZM molybdenum alloys are selected to be carried out with sand paper polishing after surface is smooth as base material
Pickling, alkali cleaning processing, hereafter ultrasonic cleaning is clean in alcohol, is put into drying box and dries.
(2) prepared by slurry：It is matched by the mass fraction of 54%Si powder, 25%Mo powder and 15%YSZ powder, three is average
Grain size is respectively 1 μm, 3 μm and 100nm；Select 0.1 μm of SiO2Powder, 2 μm of NH3It is used as additive, mass fraction to match in F powder
Than being respectively 0.5%, 5.5%；The purity of 5 kinds of powder is not less than 99%.The coating material prepared is placed in ball grinder, ball
Grinding media is ethyl alcohol, ratio of grinding media to material 5:1, rotating speed 350r/min, Ball-milling Time 7h.
(3) it uniformly coats slurry and dries：Slurry described in (2) is evenly applied in (1) using spray coating method after drying
Molybdenum alloy substrate surface, surface formed thickness be about 170 μm coating idiosome, be subsequently placed in drying box at 200 DEG C dry
Dry 0.5h.
(4) vacuum-sintering：The molybdenum alloy sample of applying coating in (3) is put into vacuum sintering furnace, in argon gas ceiling
Under part, 1400 DEG C of sintering are warming up to the heating rate of 30 DEG C/min, are cooled down with stove after keeping the temperature 90min, in molybdenum alloy after cooling
Surface obtains the Si-Mo-YSZ high-temperature oxidation resistant coatings that thickness is 120 μm and takes out sample.
(5) the anti-oxidant Si-Mo-YSZ coating samples of molybdenum alloy superhigh temperature prepared by embodiment carry out static anti-at 1725 DEG C
Oxidation test, static anti-oxidant service life are 11.2h.
Embodiment 3
(1) base material pre-processes:Select Ta-10W alloys as base material, with sand paper polishing after surface is smooth, into
Row pickling, alkali cleaning processing, hereafter ultrasonic cleaning is clean in alcohol, is put into drying box and dries.
(2) prepared by slurry：It is matched by the mass fraction of 56%Si powder, 30%Mo powder and 10%YSZ powder, three is average
Grain size is respectively 1 μm, 2 μm and 200nm；Select 0.5 μm of SiO2It is used as additive, mass fraction to match in powder, 5 μm of PVB powder
Than being respectively 3% and 1%；The purity of five kinds of powder is not less than 99%.The coating material prepared is placed in ball grinder, ball milling
Medium is ethyl alcohol, ratio of grinding media to material 10:1, rotating speed 400r/min, Ball-milling Time 6h.
(3) it uniformly coats slurry and dries：Slurry described in (2) is evenly applied in (1) using spray coating method after drying
Ta-10W alloy base materials surface, it is 180 μm of coating to form thickness on surface, is subsequently placed in vacuum drying chamber at 100 DEG C
Vacuum drying 1h.
(4) vacuum-sintering：The Ta-10W alloy samples of applying coating in (3) are put into vacuum sintering furnace, are protected in argon gas
Under the conditions of shield, 1450 DEG C of sintering are warming up to the heating rate of 10 DEG C/min, are cooled down with stove after keeping the temperature 60min, are taken out after cooling
Sample.
(5) packet siliconising is handled：The sample for preparing coating is placed on after being sealed in the crucible containing packet bleed and is placed in very
Empty stove, packet bleed by mass percent 70% Al2O3, 20% Si and 10%NH4F form, under argon atmosphere in
Ta-W alloy Si-Mo-YSZ high-temperature oxidation resistant coating samples are can be prepared by with stove cooling after 1200 DEG C of heat preservation 5h, coating layer thickness is about
It it is 154 μm, original coating cross sections pattern and constituent analysis are as shown in Figure 3.
(6) the anti-oxidant Si-Mo-YSZ coating samples of Ta-10W alloy superhigh temperature that prepared by embodiment are quiet in 1800 DEG C of progress
State Oxidation Resistance Test, oxidizing dynamics curve are as shown in Figure 4；Its static anti-oxidant service life is more than that 10h does not fail yet, is applied after oxidation
Layer cross section is as shown in Figure 5 with surface topography；- 1800 DEG C of cyclic oxidation tests of room temperature are carried out to it, the service life recycles up to 214 times.
Embodiment 4
(1) base material pre-processes:Select Nb521 niobium alloys as base material, with sand paper polishing after surface is smooth, into
Row pickling, alkali cleaning processing, hereafter ultrasonic cleaning is clean in alcohol, is put into drying box and dries.
(2) prepared by slurry：It is matched by the mass fraction of 49.5%Si powder, 40%Mo powder and 5%YSZ powder, San Zheping
Equal grain size is respectively 3 μm, 5 μm and 500nm；Select 2 μm of NH3It is used as additive, mass fraction to match in F powder, 10 μm of PVB powder
Than being respectively 5% and 0.5%；Purity >=99% of 4 kinds of powder.The coating material prepared is placed in ball grinder, ball-milling medium
For ethyl alcohol, ratio of grinding media to material 10:1, rotating speed 250r/min, Ball-milling Time 15h.
(3) it uniformly coats slurry and dries：Slurry described in (2) is evenly applied in (1) using spray coating method after drying
Nb521 niobium alloy substrate surfaces, surface formed thickness be about 150 μm coating idiosome, be subsequently placed in drying box 150
DEG C drying 0.5h.
(4) vacuum-sintering：The Nb521 niobium alloy samples of applying coating in (3) are put into vacuum sintering furnace, are protected in argon gas
Under the conditions of shields, 1500 DEG C of sintering are warming up to the heating rate of 20 DEG C/min, are cooled down with stove after keeping the temperature 40min, it is cooling after
Nb521 niobium alloys surface obtains the Si-Mo-YSZ high-temperature oxidation resistant coatings that thickness is 100 μm.
(5) the anti-oxidant Si-Mo-YSZ coating samples of Nb521 niobium alloy superhigh temperature that prepared by embodiment are quiet in 1725 DEG C of progress
State Oxidation Resistance Test, static anti-oxidant service life are 13.5h, are 4.1h 1800 DEG C of protection service life.
The above, only section Example of the invention, therefore cannot limit the scope of implementation of the present invention according to this, i.e.,
According to equivalent changes and modifications made by the scope of the claims of the present invention and description, all should still belong in the range of the present invention covers.
The comparison of YSZ contents, all process steps and raw material are same as Example 1, and only Mo, YSZ ratio are adjusted,
When Mo is 34%, YSZ is 4.5%, Si-Mo-YS coatings are 13.5h in 1725 DEG C of static state high-temperature antioxygenic properties, when Mo is
34%, when YSZ is 14.5%, it is 14.2h in 1725 DEG C of static state high-temperature antioxygenic properties, has compared with the 22.3h of embodiment 1 larger
Gap.
Comparative example 1：
(1) base material pre-processes:TZM molybdenum alloys are selected to be carried out with sand paper polishing after surface is smooth as base material
Pickling, alkali cleaning processing, hereafter ultrasonic cleaning is clean in alcohol, is put into drying box and dries.
(2) prepared by slurry：It is matched by the mass fraction of 58.5%Si powder, 15%Mo powder and 25%YSZ powder, San Zheping
Equal grain size is respectively 1 μm, 3 μm and 100nm；Select 0.1 μm of SiO2Additive, mass fraction are used as in powder, 10 μm of PVB powder
Proportioning is respectively 1%, 0.5%；The purity of 5 kinds of powder is not less than 99%.The coating material prepared is placed in ball grinder, ball
Grinding media is ethyl alcohol, ratio of grinding media to material 5:1, rotating speed 350r/min, Ball-milling Time 7h.
(3) it uniformly coats slurry and dries：Slurry described in (2) is evenly applied in (1) using spray coating method after drying
Molybdenum alloy substrate surface, surface formed thickness be about 150 μm coating idiosome, be subsequently placed in drying box at 200 DEG C dry
Dry 0.5h.
(4) vacuum-sintering：The molybdenum alloy sample of applying coating in (3) is put into vacuum sintering furnace, in argon gas ceiling
Under part, 1400 DEG C of sintering are warming up to the heating rate of 30 DEG C/min, are cooled down with stove after keeping the temperature 60min, in molybdenum alloy after cooling
Surface obtains the Si-Mo-YSZ high-temperature oxidation resistant coatings that thickness is 100 μm and takes out sample.
(5) the anti-oxidant Si-Mo-YSZ coating samples of molybdenum alloy superhigh temperature prepared by comparative example carry out static anti-at 1725 DEG C
Oxidation test, the static anti-oxidant service life is about 0.4h.
Comparative example 2：
(1) base material pre-processes:Select Ta-10W alloys as base material, with sand paper polishing after surface is smooth, into
Row pickling, alkali cleaning processing, hereafter ultrasonic cleaning is clean in alcohol, is put into drying box and dries.
(2) prepared by slurry：It is matched by the mass fraction of 56%Si powder, 10%Mo powder and 30%YSZ powder, three is average
Grain size is respectively 1 μm, 2 μm and 200nm；Select 0.5 μm of SiO2It is used as additive, mass fraction to match in powder, 5 μm of PVB powder
Than being respectively 3% and 1%；The purity of five kinds of powder is not less than 99%.The coating material prepared is placed in ball grinder, ball milling
Medium is ethyl alcohol, ratio of grinding media to material 10:1, rotating speed 400r/min, Ball-milling Time 6h.
(3) it uniformly coats slurry and dries：Slurry described in (2) is evenly applied in (1) using spray coating method after drying
Ta-10W alloy base materials surface, it is 180 μm of coating to form thickness on surface, is subsequently placed in vacuum drying chamber at 100 DEG C
Vacuum drying 1h.
(4) vacuum-sintering：The Ta-10W alloy samples of applying coating in (3) are put into vacuum sintering furnace, are protected in argon gas
Under the conditions of shield, 1450 DEG C of sintering are warming up to the heating rate of 10 DEG C/min, are cooled down with stove after keeping the temperature 60min, is made after cooling
The sample that thickness is 130 μm.
(5) the anti-oxidant Si-Mo-YSZ coating samples of Ta-10W alloy superhigh temperature that prepared by embodiment are quiet in 1800 DEG C of progress
State Oxidation Resistance Test, static anti-oxidant service life are 0.1h.
Claims (10)
1. a kind of anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature, it is characterised in that：The coating is raw materials used with quality
Percentages include following components：
Si powder 45%~65%；
Mo 25%~40%；
YSZ 2%~15%；
Additive 2%~8%；
The additive is selected from SiO2Powder, NH3At least one of F powder, PVB powder.
2. the anti-oxidant Si-Mo-YSZ coatings of a kind of refractory metal superhigh temperature according to claim 1, it is characterised in that：Institute
It includes following components by percentage to the quality that it is raw materials used, which to state coating,：
3. the anti-oxidant Si-Mo-YSZ coatings of a kind of refractory metal superhigh temperature according to claim 2, it is characterised in that：Institute
It includes following components by percentage to the quality that it is raw materials used, which to state coating,：
4. a kind of preparation side of the anti-oxidant Si-Mo-YSZ coatings of the refractory metal superhigh temperature as described in claim 1-3 any one
Method, it is characterised in that；Include the following steps：
Step 1
Match by design component and takes Si powder, Mo powders, YSZ powders, additive；It is uniformly mixed and slurry is made；Obtain standby material；
Step 2
Using the refractory metal that surface cleaning is dried as matrix, one layer of standby material is coated in matrix surface；Drying, obtains with spare
The matrix of material；
Step 3
Matrix with standby material obtained by step 2 is placed in sintering furnace, under protective atmosphere, in 1370 DEG C~1530 DEG C progress
Sintering is kept the temperature, cooling, obtains the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature.
5. a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature according to claim 4；It is special
Sign is：In step 1, matches by design component and take Si powder, Mo powders, YSZ powders, additive as raw material；Using alcoholic solution as
Ball-milling medium, the mass ratio for controlling raw material and abrading-ball is 1：5~10, control rotational speed of ball-mill is 200r/min~400r/min；Ball
5h~15h is ground, standby material is obtained.The mass ratio of scheme as a further preference, raw material and ball-milling medium is 2:1~2:5.Institute
It is preferably ethyl alcohol to state ball-milling medium.
6. a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature according to claim 4；It is special
Sign is：In step 1, the average particle diameter size of the Si powder is 0.5~5 μm, preferably 0.5~3 μm, the Mo powders
Average particle diameter size is 2 μm~10 μm, and the average particle diameter size of the YSZ powders is 0.1~3 μm, preferably 0.1~0.5 μm,
The average particle diameter size of other additives is 0.1~10 μm.Si powders, Mo powders, YSZ powders purity be not less than
98%.
7. a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature according to claim 4；It is special
Sign is：In step 2, refractory metal is selected from Mo, Mo based alloy, Ta, Ta based alloy, Nb, Nb based alloy, it in W, W based alloy
It is a kind of.
8. a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature according to claim 4；It is special
Sign is：In step 2, standby material obtained by step 1 is evenly applied to surface cleaning by the way of dip-coating and/or spraying and is done
The surface of dry refractory metal forms the coating that thickness is 120 μm~300 μm, is subsequently placed in baking oven and is dried in 70~200 DEG C
Dry 20min~120min；Obtain the matrix with standby material.
9. a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature according to claim 4；It is special
Sign is：In step 3, the matrix with standby material obtained by step 2 is placed in sintering furnace, under protective atmosphere, with 5 DEG C/min
The heating rate of~50 DEG C/min is warming up to 1370 DEG C~1530 DEG C, cools down with stove after keeping the temperature 20min~90min, it is cooling after
Refractory metal material surface obtains the Si-Mo-YSZ high-temperature oxidation resistant coatings that thickness is 80 μm~200 μm.
10. a kind of preparation method of the anti-oxidant Si-Mo-YSZ coatings of refractory metal superhigh temperature according to claim 4；Its
It is characterized in that：After completing step 3, packet siliconizing treatment processes can be used；The packet siliconizing treatment processes are：The infusibility gold of coating will be prepared
Belong to sample be placed on sealed in the crucible containing packet bleed after is placed in vacuum sintering furnace, packet bleed by mass percent 50%~
75% Al2O3, 15%~25% Si and 5~15%NH4F is formed, in 1100 DEG C~1300 DEG C guarantors under argon atmosphere
After 2~6h of temperature coating sample is can be prepared by with stove cooling.
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