CN108002828A - A kind of YSZ ceramic prilling powders used for plasma spraying and preparation method thereof - Google Patents
A kind of YSZ ceramic prilling powders used for plasma spraying and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of YSZ ceramic prilling powders used for plasma spraying and preparation method thereof, by the way that particle diameter is mixed for 0.5~4 μm of the mixed raw material comprising yittrium oxide and zirconium oxide with starch, carry out 1350~1550 DEG C of high-temperature roasting, obtain YSZ clinkers；Then obtained YSZ clinkers are mixed with dispersant and water, ball-milling treatment is carried out, obtains ball milling slurries；Obtained clinker slurries are subjected to sanded treatment again, obtains mixing with binding agent after slurries are sanded, is granulated, obtains YSZ ceramic prilling powders used for plasma spraying.The present invention realizes the solid phase reaction of zirconium oxide and yittrium oxide in the high-temperature calcination process, obtains aoxidizing yttrium partially stabilized zirconium oxide (YSZ), performance is stablized；And acid ion is not introduced, high-temperature roasting temperature is higher, realizes that solid phase reaction can burn micro acid ion while fully progress, so as to improve the batch stability of powder.
Description
Technical field
The present invention relates to ceramic powder technical field, more particularly to a kind of YSZ ceramic prilling powders used for plasma spraying and its
Preparation method.
Background technology
Thermal Barrier Coating Layers Prepared By Plasma Spraying is widely used in the fields such as Aeronautics and Astronautics, machinery, military project, wherein Y2O3It is partially stabilized
ZrO2(YSZ) with its high-melting-point, lower thermal conductivity, of a relatively high thermal coefficient of expansion and good corrosion resistance as current
Most popular thermal barrier coating ceramic material.
With the fast development of science and technology, such as turbo blade, combustion chamber of gas turbine and weaponry propulsion system
The worst hot case parts surface such as hot-end component operating condition it is more and more harsher, plasma spraying conventional micron level ceramic powder
The performance of the thermal barrier coating of acquisition has been difficult to meet the requirements, and there is an urgent need for nanometer scale ceramics powder used for plasma spraying.
Main now to prepare YSZ nano-ceramic powders used for plasma spraying using coprecipitation, the raw material used is such as
The salts substances of the zirconium and yttrium of zirconium oxychloride and yttrium nitrate, inevitably introduce substantial amounts of chlorion, nitrate anion and ammonium root etc.
Pollution ion, is dissolved in after becoming salting liquid in water, adds in the alkaline solution such as ammonium hydroxide or sodium hydroxide, reaction generation hydrogen
Zirconium oxide and yttrium hydroxide precipitation, in conjunction with follow-up 800 DEG C or so of calcination process, obtain YSZ nano-ceramic powders.But altogether
The precipitation method can introduce a large amount of pollution ions, not only need substantial amounts of deionized water in washing process, can also cause environmental pollution,
Increase cost for wastewater treatment, also, inevitably meeting residual fraction acid ion in the powder of coprecipitation preparation, powder will be seriously affected
The stability of body, so that the thermal barrier coating service life being prepared is uneven.
The content of the invention
In view of this, it is an object of the invention to provide YSZ ceramic prilling powders used for plasma spraying and preparation method thereof, sheet
The preparation method provided is invented without zirconium and the salts substances of yttrium, avoids introducing pollution ion in the feed, can obtain
The YSZ ceramic prilling powders used for plasma spraying stablized to performance.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
A kind of preparation method of YSZ ceramic prilling powders used for plasma spraying, comprises the following steps：
(1) mixed raw material comprising yittrium oxide and zirconium oxide is provided；The particle diameter of the mixed raw material is 0.5~4 μm；
(2) mixed raw material is mixed with starch, carries out high-temperature roasting, obtain YSZ clinkers；The temperature of the high-temperature roasting
Spend for 1350~1550 DEG C；
(3) the YSZ clinkers that the step (2) obtains are mixed with dispersant and water, carries out ball-milling treatment, obtain ball milling slurry
Liquid；
(4) the ball milling slurries for obtaining the step (3) carry out sanded treatment, obtain that slurries are sanded；
(5) the sand milling slurries that the step (4) obtains are mixed with binding agent, is granulated, obtained used for plasma spraying
YSZ ceramic prilling powders.
Preferably, the mass ratio of zirconium oxide and yittrium oxide is (900~940) in the mixed raw material：(60~100).
Preferably, the preparation method of the mixed raw material includes：Will be mixed containing zirconium oxide, yittrium oxide, dispersant and water
Close slurry and carry out ball-milling treatment and drying process successively, obtain the mixed raw material comprising yittrium oxide and zirconium oxide；
The mass ratio of the gross mass and water of zirconium oxide and yittrium oxide is (55~65) in the mixed slurry：(35~45)；
The quality of dispersant and the zirconium oxide and the ratio of the gross mass of yittrium oxide are 100 in the mixed slurry:(0.20
~1.0).
Preferably, the time of step (2) the high temperature roasting is 2~6h.
Preferably, starch and mixed raw material mass ratio are (2~6) in the step (2)：100.
Preferably, the dispersant in the step (3) is ammonium polyacrylate, sodium tripolyphosphate, calgon, poly- methyl
One or more in acrylic acid ammonia and polyethylene glycol；
The mass ratio of the dispersant and YSZ clinkers is (0.2~1.0)：100；
The mass ratio of the quality of YSZ clinkers and water is (55~65) in the step (3)：(35~45).
Preferably, the rotating speed of ball-milling treatment is 40~80r/min in the step (3), and the time of the ball-milling treatment is
12~24h.
Preferably, the rotating speed of sanded treatment is 800~1200r/min in the step (4), the time of the sanded treatment
For 2~6h.
Preferably, the dosage of binding agent is described in terms of the quality of YSZ clinkers in the sand milling slurries in the step (5)
The mass ratio of YSZ clinkers and binding agent is 100:(0.3~1.5).
Present invention also offers the YSZ ceramic prillings used for plasma spraying that preparation method described in above-mentioned technical proposal obtains
Powder, including：The stabilized with yttrium oxide agent of the zirconium oxide and 6~10wt% of 90~94wt%；The particle diameter of the YSZ ceramic prilling powders is
30~150 μm.
The present invention provides a kind of preparation method of YSZ ceramic prilling powders used for plasma spraying, comprise the following steps：By grain
The mixed raw material comprising yittrium oxide and zirconium oxide that footpath is 0.5~4 μm is mixed with starch, carries out 1350~1550 DEG C of high temperature roasting
Burn, obtain YSZ clinkers；Then obtained YSZ clinkers are mixed with dispersant and water, ball-milling treatment is carried out, obtains ball milling slurries；
Obtained clinker slurries are subjected to sanded treatment again, obtains mixing with binding agent after slurries are sanded, is granulated, obtains plasma
YSZ ceramic prilling powders are used in spraying.
The present invention realizes the solid phase reaction of zirconium oxide and yittrium oxide in the high-temperature calcination process, obtains yittrium oxide part
Stable zirconium oxide (YSZ), that is, allow yittrium oxide to be dissolved into the lattice of zirconium oxide, obtains Tetragonal and cube mutually knot mixed
Structure, the stable structure, and then performance are stablized.And the present invention does not introduce acid ion, and the high-temperature roasting temperature is higher, realize
Solid phase reaction can burn remaining micro acid ion in commercially available zirconium oxide and yittrium oxide while fully progress, effectively more
Mend in coprecipitation preparation process because acid ion content is high and caused by powder characteristic it is unstable the defects of, so as to improve powder
Batch stability.Embodiment the result shows that, YSZ ceramic prilling powders performance used for plasma spraying is prepared in the present invention
Stablize so that the service life for the thermal barrier coating that same batch is prepared is homogeneous.
Brief description of the drawings
Fig. 1 is the XRD diagram through 1450 DEG C of sintering obtained YSZ clinkers of 4h in the embodiment of the present invention 3；
The field emission electron that the obtained YSZ ceramic powders of 3h are sanded through 1100r/min in Fig. 2 embodiment of the present invention 4 is swept
Retouch microscope photograph；
Fig. 3 is the optical microscope picture of the preparation-obtained YSZ ceramic prilling powders of the embodiment of the present invention 4；
Fig. 4 is cutting for the thermal barrier coating a that the YSZ granulation powders obtained in the embodiment of the present invention 1 are prepared through plasma spraying
Face shape appearance figure；
Fig. 5 is the section for the thermal barrier coating b that the YSZ granulation powders that the embodiment of the present invention 1 obtains are prepared through plasma spraying
Optical microphotograph shape appearance figure；
Fig. 6 is the section for the thermal barrier coating c that the YSZ granulation powders that the embodiment of the present invention 1 obtains are prepared through plasma spraying
Optical microphotograph shape appearance figure；
Fig. 7 is the section for the thermal barrier coating d that the YSZ granulation powders that the embodiment of the present invention 1 obtains are prepared through plasma spraying
Optical microphotograph shape appearance figure.
Embodiment
The present invention provides a kind of preparation method of YSZ ceramic prilling powders used for plasma spraying, comprise the following steps：
(1) mixed raw material comprising yittrium oxide and zirconium oxide is provided；The particle diameter of the mixed raw material is 0.5~4 μm；
(2) mixed raw material is mixed with starch, carries out high-temperature roasting, obtain YSZ clinkers；The temperature of the high-temperature roasting
Spend for 1350~1550 DEG C；
(3) the YSZ clinkers that the step (2) obtains are mixed with dispersant and water, carries out ball-milling treatment, obtain ball milling slurry
Liquid；
(4) the ball milling slurries for obtaining the step (3) carry out sanded treatment, obtain that slurries are sanded；
(5) the sand milling slurries that the step (4) obtains are mixed with binding agent, is granulated, obtained used for plasma spraying
YSZ ceramic prilling powders.
Mixed raw material provided by the invention comprising yittrium oxide and zirconium oxide, zirconium oxide and yittrium oxide in the mixed raw material
Mass ratio be preferably (900~940)：(60~100), more preferably (915~935)：(65~85), more preferably
930：70.In the present invention, the particle diameter of the mixed raw material is 0.5~4 μm, is preferably 1~3 μm, more preferably 1.5~2 μm.
In the present invention, the preparation method of the mixed raw material preferably includes：Zirconium oxide, yittrium oxide, dispersant will be contained
Ball-milling treatment and drying process are carried out successively with the mixed slurry of water, obtain the mixed raw material comprising yittrium oxide and zirconium oxide.
The present invention does not have particular/special requirement to the source of the zirconium oxide and yittrium oxide, and use is well known to those skilled in the art
Zirconium oxide and yittrium oxide commercial goods.In the present invention, total matter of zirconium oxide and yittrium oxide in the mixed slurry
The mass ratio of amount and water is preferably (55~65)：(35~45), more preferably (56~62)：(38~44), more preferably
(58~61)：(39~42), are most preferably 60：40.
In the present invention, it is preferably ammonium polyacrylate, sodium tripolyphosphate, six inclined phosphorus to prepare the mixed raw material with dispersant
One or more in sour sodium, polymethylacrylic acid ammonia and polyethylene glycol.It is not of the same race in the present invention when selecting a variety of dispersants
Class dispersant preferably according to etc. mass parts add.The present invention does not have particular/special requirement to the source of the dispersant, using this area
Known to technical staff.
In the present invention, the quality of dispersant and the zirconium oxide and the ratio of the gross mass of yittrium oxide in the mixed slurry
Preferably 100:(0.20~1.0), more preferably 100：(0.25~0.85), more preferably 100：(0.5~0.55).
In the present invention, the dispersant is organic matter, and usage amount is less, the drawbacks of not introducing acid ion.
The present invention preferably carries out ball-milling treatment and drying process successively to the mixed slurry, obtains including yittrium oxide and oxygen
Change the mixed raw material of zirconium.In the present invention, the rotating speed of the ball-milling treatment is preferably 120~160r/min, more preferably
125~155r/min, more preferably 130~140r/min.In the present invention, the time of the ball-milling treatment is preferably 2~6h,
More preferably 2.5~5.5h, more preferably 3~5h.In the present invention, abrasive body used in the ball milling is preferably oxygen
Change zirconium ball；The particle diameter of the abrasive body is preferably 3~8mm, more preferably 3.5~7mm, more preferably 4~5mm.
In the present invention, the ball-milling treatment preferably carries out in the ball mill；The ball mill is preferably agitating ball mill
Or roller mill.
In the present invention, the ball milling can realize the refinement to zirconium oxide and yittrium oxide, easy to obtain target grain size
Mixed raw material containing zirconium oxide and yittrium oxide, and then ensure in follow-up roasting process, the progress of solid phase reaction；And the ball
Mill contributes to the uniform mixing of zirconium oxide and yittrium oxide, and abundant easy to follow-up solid phase reaction carries out.
After the ball-milling treatment, the present invention processing preferably is dried to the ball milling slurry, obtain comprising yittrium oxide with
The mixed raw material of zirconium oxide.In the present invention, the moisture content of the mixed raw material is preferably below 0.5wt%.In the present invention,
The mode of the drying process is preferably in spray drying, Electric heat oven drying, evaporator dry, centrifugal dehydration and filter-press dehydration
One or more.The present invention does not have particular/special requirement to the embodiment of the centrifugal dehydration and filter-press dehydration, using this
Known to field technology personnel.In the present invention, when by the way of Electric heat oven drying or evaporator dry, institute
The temperature for stating drying process is preferably 80~100 DEG C, more preferably 85~95 DEG C, more preferably 90~95 DEG C；It is described dry
The time of dry processing is preferably 5~15h, more preferably 8~12h, more preferably 9~10h.In the present invention, use is worked as
During the mode of spray drying, the atomization frequency of the spray drying is preferably 40~50Hz, more preferably 45Hz.In this hair
In bright, the inlet air temperature of the spray drying is preferably 220~250 DEG C, more preferably 230~240 DEG C；The spraying is dry
Dry leaving air temp is preferably 85~100 DEG C, more preferably 90~95 DEG C.Specific side of the present invention to the spray drying
Formula does not have particular/special requirement, using spray drying well-known to those skilled in the art.
After obtaining the mixed raw material, the present invention mixes the mixed raw material with starch, carries out high-temperature roasting, obtains
YSZ clinkers.
In the present invention, the mass ratio of the mixed raw material and starch is preferably (2~6)：100, more preferably
(2.5~5.5)：100, more preferably (3~4.5)：100.The present invention does not have particular/special requirement to the source of the starch, using this
Starch known to field technology personnel.After the present invention mixes the starch and mixed raw material, the starch is in high temperature
Volatilization can be decomposed in roasting process, leaves stomata, can effectively prevent that material is blocking, during being conducive to subsequent ball milling, YSZ
The refinement of clinker.
The present invention does not have particular/special requirement to the hybrid mode of the mixed raw material and starch, using those skilled in the art institute
Well known material hybrid mode, can realize the uniform mixing of mixed raw material and starch.
After completing the mixing, the present invention carries out high-temperature roasting to mixture, obtains YSZ clinkers.In the present invention, it is described
The temperature of high-temperature roasting is 1350~1550 DEG C, is preferably 1400~1500 DEG C, more preferably 1420~1480 DEG C；At this
In the embodiment of invention, the temperature of the roasting is specially 1370 DEG C, 1410 DEG C, 1430 DEG C, 1470 DEG C or 1520 DEG C.In this hair
In bright, the time of the roasting is preferably 2~6h, more preferably 3~5h；In an embodiment of the present invention, the roasting
Time be specially 2.5h, 3.5h, 4.0h, 4.5h or 5.5h.The present invention realized in the high-temperature calcination process zirconium oxide and
The solid phase reaction of yittrium oxide, obtains aoxidizing yttrium partially stabilized zirconium oxide (YSZ), that is, allows yittrium oxide to be dissolved into the lattice of zirconium oxide
In, obtain Tetragonal and cube phase structure mixed, the stable structure, and then performance and stablize；And the high-temperature roasting temperature
Degree is higher, realizes that solid phase reaction can be by remaining micro acid ion in commercially available zirconium oxide and yittrium oxide while fully progress
Burn, avoid influence of the acid ion to the service life of thermal barrier coating；The high-temperature roasting, which is also avoided that temperature is excessive, to be caused
Roasting material overvulcanization and particle excessively grow up.
After the high-temperature roasting, the present invention mixes the YSZ clinkers with dispersant and water, carries out ball-milling treatment, obtains
Ball milling slurries.In the present invention, the dispersant is preferably ammonium polyacrylate, sodium tripolyphosphate, calgon, poly- methyl-prop
One or more in olefin(e) acid ammonia and polyethylene glycol；The specific source of dispersant of the present invention does not have particular/special requirement, using this
Commercial goods known to field technology personnel.In the present invention, the water is preferably distilled water or deionized water.
In the present invention, the mass ratio of the dispersant and YSZ clinkers is preferably (0.2~1.0)：100, further preferably
For (0.3~0.9)：100, more preferably (0.5~0.7)：100.In the present invention, the quality of the YSZ clinkers is preferably YSZ
The 55~65% of the gross mass of clinker and water, more preferably 58~62%, more preferably 60~61%.
Hybrid mode of the invention to the YSZ clinkers and dispersant and water, without particular/special requirement, using art technology
The hybrid mode of material and water known to personnel.
After the mixing, the present invention carries out ball-milling treatment to the clinker slurries being mixed to get, and obtains ball milling slurries.
In the present invention, the rotating speed of the ball-milling treatment is preferably 40~80r/min, more preferably 45~75r/min, further excellent
Elect 50~60r/min as；The time of the ball-milling treatment is preferably 12~24h, more preferably 15~20h, more preferably
16~18h.In the present invention, abrasive body used in the ball milling is preferably zirconia ball；The particle diameter of the abrasive body is preferred
For 10~30mm, more preferably 15~28mm, more preferably 20~25mm.
In the present invention, the starch can decompose volatilization in high-temperature calcination process, leave stomata, can effectively prevent
Material is blocking, contributes in the mechanical milling process of YSZ clinkers effectively to refine, and not only reduces energy consumption, moreover it is possible to ensure the suitable of mechanical milling process
Profit carries out.
In the present invention, the particle diameter of YSZ clinkers is preferably less than 4 μm in the ball milling slurries after the YSZ clinkers ball milling, into
One step is preferably 0.5~4 μm.
The present invention does not have particular/special requirement to the concrete mode of the ball-milling treatment, and use is well-known to those skilled in the art
The mode of ball-milling treatment.
After the ball-milling treatment, the present invention carries out sanded treatment to the obtained ball milling slurries, obtains that slurries are sanded.Institute
Before stating sanded treatment, the present invention is preferably adjusted the mass ratio of YSZ clinkers and water in the ball milling slurries, obtains pre- sand milling
Processing slurries；The pre- sanded treatment with the 45 of the gross mass that the quality of YSZ clinkers in slurries is YSZ clinkers and water~
55%, more preferably 46~52%, more preferably 48~50%.In the present invention, the adjustment of the mass ratio is preferably logical
The addition for crossing water is realized.
In the present invention, the rotating speed of the sanded treatment is preferably 800~1200r/min, more preferably 850~
1150r/min, more preferably 900~1100r/min, are most preferably 1000~1050r/min.In the present invention, the sand milling
The time of processing is preferably 2~6h, more preferably 2.5~5.5h, more preferably 3~5h, is most preferably 4~4.5h.
In the present invention, abrasive body used in the sand milling is preferably zirconia ball；The particle diameter of the abrasive body is preferably 0.1~
0.8mm, more preferably 0.2~0.5mm, more preferably 0.3~0.4mm.
In the present invention, the sanded treatment carries out preferably in sand mill；The present invention does not have the source of the sand mill
There is particular/special requirement, using sand mill well-known to those skilled in the art；In an embodiment of the present invention, the sand mill
Model the total amount of slurry of sanded treatment carried out needed for determine.
In the present invention, the particle diameter that YSZ clinkers in slurries are sanded is preferably below 100nm, more preferably
Below 80nm.
The present invention does not have particular/special requirement to the concrete mode of the sanded treatment, and use is well-known to those skilled in the art
The mode of sanded treatment.
The process that hardening and crystal grain in afore-said hot roasting process of the present invention there are material are grown up, is sanded again by ball milling
Processing mode, the advantage of sanded treatment can be given full play to, realize the refinement of roasting material.
After the sanded treatment, the present invention mixes the obtained sand milling slurries with binding agent, is granulated, obtained
Plasma spray YSZ ceramic prilling powders.The present invention does not have particular/special requirement to the species of the binding agent, selects people in the art
Ceramics binding agent known to member, it is specific such as polyvinyl alcohol.In the present invention, the dosage of the binding agent preferably with
The quality meter of YSZ clinkers in the sand milling slurries, the mass ratio of the YSZ clinkers and binding agent is preferably 100:(0.3~
1.5) it is more preferably, 100:(0.4~1.2), more preferably 100:(0.5~1.0), more preferably 100:(0.75~
0.8)。
The present invention does not have particular/special requirement to the hybrid mode of the sand milling slurries and binding agent, using those skilled in the art
Known slurry hybrid mode.
The present invention is granulated the slurry being mixed to get, and obtains YSZ ceramic prilling powders used for plasma spraying.At this
In invention, described be granulated is preferably mist projection granulating.In the present invention, the atomization frequency of the mist projection granulating be preferably 36~
48Hz, more preferably 38~45Hz, more preferably 40.5~41.5Hz.In the present invention, the inlet air of the mist projection granulating
Temperature is preferably 220~230 DEG C, more preferably 222~228 DEG C, more preferably 225~226 DEG C；The mist projection granulating
Leaving air temp is preferably 85~100 DEG C, more preferably 88~98 DEG C, more preferably 90~95 DEG C.The present invention is to the spray
The concrete mode that mist is granulated does not have particular/special requirement, using mist projection granulating well-known to those skilled in the art.
The present invention avoids introducing the pollutions such as a large amount of acid groups, ammonium root in the feed without zirconium and the salts substances of yttrium
Ion, though contain a small amount of acid ion in raw material, and calcination temperature is high, and also can be whole by the acid ion in raw material
Burn, effectively make up in coprecipitation preparation process because acid ion content is high and caused by powder characteristic it is unstable the defects of, from
And improve the batch and stability of powder.The present invention need to be only sanded by wet ball grinding and wet method can be by powder refining
To nanoscale (below 100nm), preparation process simple and convenient, cost is low, and the cycle is short, reproducible, is more suitable for industrial production, solution
The problems such as energy consumption and of high cost in coprecipitation of having determined, environmental pollution is big, meet the demand for development of following new material preparation process.
Present invention also offers the YSZ used for plasma spraying ceramics that the preparation method described in a kind of above-mentioned technical proposal obtains
Pelletizing, including：The stabilized with yttrium oxide agent of the zirconium oxide and 6~10wt% of 90~94wt%；The grain of the YSZ ceramic prilling powders
Footpath is 30~150 μm.In the present invention, the YSZ ceramic prilling powders used for plasma spraying are the yttrium partially stabilized oxidation of oxidation
Zirconium, is Tetragonal and cube phase structure mixed, i.e. yittrium oxide is dissolved into the lattice structure of zirconium oxide.In the present invention, institute
The particle diameter for stating YSZ ceramic prilling powders used for plasma spraying is 30~150 μm, is preferably 50~130 μm, or preferably 80~150 μ
m；Or preferably 60~130 μm.In the present invention, the plasma spray, which scribbles YSZ ceramic prilling powders, includes 90~94wt%'s
Zirconium oxide, is preferably 91.5~93.5wt%, more preferably 93wt%；The plasma spray, which scribbles YSZ ceramic prilling powders, includes 6
The stabilized with yttrium oxide agent of~10wt%, is preferably 6.5~8.5wt%, more preferably 7wt%.
YSZ ceramic prilling powders used for plasma spraying provided by the invention and preparation method thereof are carried out with reference to embodiment
Detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, it is 940 parts accurately to weigh zirconium oxide, yittrium oxide 60
Part, dispersant polymethylacrylic acid ammonia is 2 parts, adds deionized water, adjusts the quality of zirconium oxide and yittrium oxide in mixed slurry
By agitating ball mill ball milling 2h, abrasive body it is grain by material with 55% for zirconium oxide, yittrium oxide and deionized water gross mass
The zirconia ball of 3~4mm of footpath, rotational speed of ball-mill 160r/min.
Slurry after stirring ball-milling is subjected to spraying drying, it is 45Hz to adjust atomization frequency, 240 DEG C of inlet air temperature, outlet air
90 DEG C of temperature, obtains yttria zirconia mixed raw material.
It is accurate to weigh 20 parts of 1000 parts of yttria zirconia mixed raw material and starch, the two is mixed thoroughly after 1350 DEG C of sintering
6h, obtains YSZ clinkers.XRD analysis are carried out to obtained YSZ clinkers, it is known that, the YSZ clinkers that high-temperature calcination obtains have synthesized
The mixing phase structure of Tetragonal and Emission in Cubic, occurs without monoclinic phase, illustrates that stabilizer yittrium oxide has been dissolved into zirconium oxide crystalline substance
Among lattice.
1000 parts of YSZ clinkers are accurately weighed respectively, and dispersant polymethylacrylic acid ammonia is 2 parts, adds deionized water, obtains
Clinker slurries；It is the 55% of YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in clinker slurries, and clinker slurries are passed through
Ball mill ball milling 24h, abrasive body are the zirconia ball of 10~20mm of particle diameter, and rotational speed of ball-mill 40r/min, obtains ball milling slurries.
Slurry after ball milling is imported in sand mill, it is YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in slurry
45%, continue be sanded 6h, abrasive body be 0.6~0.8mm of particle diameter zirconium oxide bead, sand milling rotating speed is 800r/min, obtains sand
Grinding slurry.Field emission electron flying-spot microscope detection is carried out to the obtained YSZ ceramic powders being sanded in slurries, it is known that, it is sanded
YSZ ceramic powders have been refined to Nano grade, uniform particle sizes, less than 100 nanometers afterwards.
Slurries will be sanded to export and add 1.5% polyvinyl alcohol adhesive of YSZ clinker gross masses, carry out spraying and make
Grain, you can the YSZ ceramic prilling powders used for plasma spraying that particle diameter is 60~150 μm, sphericity and good fluidity are obtained, wherein
It is that atomization frequency is 36Hz to set Spray granulation equipment technological parameter, 220 DEG C of inlet air temperature, 85 DEG C of leaving air temp.
The YSZ ceramic prilling powders used for plasma spraying being prepared using embodiment 1 carry out the preparation of thermal barrier coating, obtain
A thermal barrier coatings, b thermal barrier coatings, c thermal barrier coatings and d thermal barrier coatings；Its Cross Section Morphology figure is respectively such as Fig. 4, Fig. 5, Fig. 6 and Fig. 7 institute
Show, as seen from the figure, powder melting degree under the action of plasma jet is more consistent, and nano-powder melts the particle to be formed
It is evenly distributed and size is close, has no large-sized and do not melt field trash and crackle, tissue is more uniformly distributed and densification, and 4
The institutional framework of a thermal barrier coating is consistent；And the service life of 4 thermal barrier coatings is suitable.YSZ ceramic prilling powders provided by the invention
Performance is stablized, and the service life for the thermal barrier coating that same batch is prepared is homogeneous.
Embodiment 2
Using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, it is 930 parts accurately to weigh zirconium oxide, yittrium oxide 70
Part, dispersants ammonium polyacrylate is 4 parts, adds deionized water, adjusts the quality of zirconium oxide and yittrium oxide in mixed slurry and is
The 58% of zirconium oxide, yittrium oxide and deionized water gross mass, by material by agitating ball mill ball milling 3h, abrasive body is particle diameter 4
The zirconia ball of~5mm, rotational speed of ball-mill 150r/min.
Slurry after stirring ball-milling is obtained into yttria zirconia mixing life directly through Electric heat oven in 90 DEG C of dry 12h
Material.
It is accurate to weigh 30 parts of 1000 parts of yttria zirconia mixed raw material and starch, the two is mixed thoroughly after 1400 DEG C of sintering
5h, obtains YSZ clinkers.XRD analysis are carried out to obtained YSZ clinkers, it is known that, the YSZ clinkers that high-temperature calcination obtains have synthesized
The mixing phase structure of Tetragonal and Emission in Cubic, occurs without monoclinic phase, illustrates that stabilizer yittrium oxide has been dissolved into zirconium oxide crystalline substance
Among lattice.
1000 parts of YSZ clinkers are accurately weighed respectively, and dispersants ammonium polyacrylate is 4 parts, adds deionized water, obtains clinker
Slurries；It is the 58% of YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in clinker slurries, and clinker slurries are passed through ball milling
Machine ball milling 21h, abrasive body are the zirconia ball of 15~20mm of particle diameter, and rotational speed of ball-mill 50r/min, obtains ball milling slurries.
Slurry after ball milling is imported in sand mill, it is YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in slurry
48%, continue be sanded 5h, abrasive body be 0.5~0.6mm of particle diameter zirconium oxide bead, sand milling rotating speed is 900r/min, obtains sand
Grinding slurry.Field emission electron flying-spot microscope detection is carried out to the obtained YSZ ceramic powders being sanded in slurries, it is known that, it is sanded
YSZ ceramic powders have been refined to Nano grade, uniform particle sizes, less than 100 nanometers afterwards.
Slurries will be sanded to export and add 1.2% polyvinyl alcohol adhesive of YSZ clinker gross masses, carry out spraying and make
Grain, you can the YSZ ceramic prilling powders used for plasma spraying that particle diameter is 50~130 μm, sphericity and good fluidity are obtained, wherein
It is that atomization frequency is 39Hz to set Spray granulation equipment technological parameter, 240 DEG C of inlet air temperature, 90 DEG C of leaving air temp.
The YSZ ceramic prilling powders used for plasma spraying being prepared are carried out to the preparation of thermal barrier coating, obtain the painting of a thermal boundarys
Layer, b thermal barrier coatings, c thermal barrier coatings and d thermal barrier coatings；The institutional framework of 4 thermal barrier coatings is consistent；And 4 thermal barrier coatings
Service life is suitable.YSZ ceramic prilling powders performance provided by the invention is stablized, and the thermal barrier coating that same batch is prepared uses the longevity
Order homogeneous.
Embodiment 3
Using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, it is 920 parts accurately to weigh zirconium oxide, yittrium oxide 80
Part, pentasodium triphosphate of dispersing agent is 6 parts, adds deionized water, adjusts the quality of zirconium oxide and yittrium oxide in mixed slurry and is
The 60% of zirconium oxide, yittrium oxide and deionized water gross mass, by material by agitating ball mill ball milling 4h, abrasive body is particle diameter 5
The zirconia ball of~6mm, rotational speed of ball-mill 140r/min.
Slurry after stirring ball-milling is obtained into yttria zirconia mixed raw material through evaporator in 80 DEG C of dry 8h.
It is accurate to weigh 40 parts of 1000 parts of yttria zirconia mixed raw material and starch, the two is mixed thoroughly after 1450 DEG C of sintering
4h, obtains YSZ clinkers.XRD analysis are carried out to obtained YSZ clinkers, the results are shown in Figure 1.As shown in Figure 1, high-temperature calcination obtains
To YSZ clinkers synthesized the mixing phase structure of Tetragonal and Emission in Cubic, occur without monoclinic phase, illustrate stabilizer yittrium oxide
It has been dissolved among zirconia crystal lattice.
1000 parts of YSZ clinkers are accurately weighed respectively, and pentasodium triphosphate of dispersing agent is 6 parts, adds deionized water, obtains clinker
Slurries；It is the 60% of YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in clinker slurries, and clinker slurries are passed through ball milling
Machine ball milling 18h, abrasive body are the zirconia ball of 15~25mm of particle diameter, and rotational speed of ball-mill 60r/min, obtains ball milling slurries.
Slurry after ball milling is imported in sand mill, it is YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in slurry
50%, continue be sanded 4h, abrasive body be 0.4~0.5mm of particle diameter zirconium oxide bead, sand milling rotating speed is 1000r/min, obtains sand
Grinding slurry.Field emission electron flying-spot microscope detection is carried out to the obtained YSZ ceramic powders being sanded in slurries, it is known that, it is sanded
YSZ ceramic powders have been refined to Nano grade, uniform particle sizes, less than 100 nanometers afterwards.
Slurries will be sanded to export and add 0.9% polyvinyl alcohol adhesive of YSZ clinker gross masses, carry out spraying and make
Grain, you can the YSZ ceramic prilling powders used for plasma spraying that particle diameter is 40~120 μm, sphericity and good fluidity are obtained, wherein
It is that atomization frequency is 42Hz to set Spray granulation equipment technological parameter, 270 DEG C of inlet air temperature, 95 DEG C of leaving air temp.
The YSZ ceramic prilling powders used for plasma spraying being prepared are carried out to the preparation of thermal barrier coating, obtain the painting of a thermal boundarys
Layer, b thermal barrier coatings, c thermal barrier coatings and d thermal barrier coatings；The institutional framework of 4 thermal barrier coatings is consistent；And 4 thermal barrier coatings
Service life is suitable.YSZ ceramic prilling powders performance provided by the invention is stablized, and the thermal barrier coating that same batch is prepared uses the longevity
Order homogeneous.
Embodiment 4
Using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, it is 910 parts accurately to weigh zirconium oxide, yittrium oxide 90
Part, sodium hexametaphosphate dispersant is 8 parts, adds deionized water, adjusts the quality of zirconium oxide and yittrium oxide in mixed slurry and is
The 62% of zirconium oxide, yittrium oxide and deionized water gross mass, by material by agitating ball mill ball milling 5h, abrasive body is particle diameter 6
The zirconia ball of~7mm, rotational speed of ball-mill 130r/min.
Slurry after stirring ball-milling is subjected to centrifugal dehydration, then yittrium oxide oxygen is obtained in 90 DEG C of dry 5h through Electric heat oven
Change zirconium mixed raw material.
It is accurate to weigh 50 parts of 1000 parts of yttria zirconia mixed raw material and starch, the two is mixed thoroughly after 1500 DEG C of sintering
3h, obtains YSZ clinkers.XRD analysis are carried out to obtained YSZ clinkers, it is known that, the YSZ clinkers that high-temperature calcination obtains have synthesized
The mixing phase structure of Tetragonal and Emission in Cubic, occurs without monoclinic phase, illustrates that stabilizer yittrium oxide has been dissolved into zirconium oxide crystalline substance
Among lattice.
1000 parts of YSZ clinkers are accurately weighed respectively, and sodium hexametaphosphate dispersant is 8 parts, adds deionized water, obtains clinker
Slurries；It is the 62% of YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in clinker slurries, and clinker slurries are passed through ball milling
Machine ball milling 15h, abrasive body are the zirconia ball of 20~25mm of particle diameter, and rotational speed of ball-mill 70r/min, obtains ball milling slurries.
Slurry after ball milling is imported in sand mill, it is YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in slurry
52%, continue be sanded 3h, abrasive body be 0.3~0.4mm of particle diameter zirconium oxide bead, sand milling rotating speed is 1100r/min, obtains sand
Grinding slurry.Field emission electron flying-spot microscope detection is carried out to the obtained YSZ ceramic powders being sanded in slurries, as a result such as Fig. 2
It is shown.As shown in Figure 2, YSZ ceramic powders have been refined to Nano grade, uniform particle sizes, less than 100 nanometers after sand milling.
Slurries will be sanded to export and add 0.6% polyvinyl alcohol adhesive of YSZ clinker gross masses, carry out spraying and make
Grain, you can obtain the YSZ ceramic prilling powders used for plasma spraying that particle diameter is 30~100 μm, be provided with Spray granulation equipment work
Skill parameter is that atomization frequency is 45Hz, 300 DEG C of inlet air temperature, 95 DEG C of leaving air temp.Carried out to YSZ ceramic prilling powders are prepared
Optical micro analysis, the results are shown in Figure 3.From the figure 3, it may be seen that by after nano-powder mist projection granulating, sphericity, mobility have been obtained
Well, the granulation powder of 30~100um of uniform particle sizes.
The YSZ ceramic prilling powders used for plasma spraying being prepared are carried out to the preparation of thermal barrier coating, obtain the painting of a thermal boundarys
Layer, b thermal barrier coatings, c thermal barrier coatings and d thermal barrier coatings；The institutional framework of 4 thermal barrier coatings is consistent；And 4 thermal barrier coatings
Service life is suitable.YSZ ceramic prilling powders performance provided by the invention is stablized, and the thermal barrier coating that same batch is prepared uses the longevity
Order homogeneous.
Embodiment 5
Using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, it is 900 parts accurately to weigh zirconium oxide, yittrium oxide 100
Part, dispersant polyethylene glycol is 10 parts, adds deionized water, adjusts the quality of zirconium oxide and yittrium oxide in mixed slurry and is oxygen
Change zirconium, the 65% of yittrium oxide and deionized water gross mass, by material by agitating ball mill ball milling 6h, abrasive body for particle diameter 7~
The zirconia ball of 8mm, rotational speed of ball-mill 120r/min.
Slurry after stirring ball-milling is subjected to filter-press dehydration, then yittrium oxide oxygen is obtained in 90 DEG C of dry 5h through Electric heat oven
Change zirconium mixed raw material.
It is accurate to weigh 60 parts of 1000 parts of yttria zirconia mixed raw material and starch, the two is mixed thoroughly after 1550 DEG C of sintering
2h, obtains YSZ clinkers.XRD analysis are carried out to obtained YSZ clinkers, it is known that, the YSZ clinkers that high-temperature calcination obtains have synthesized
The mixing phase structure of Tetragonal and Emission in Cubic, occurs without monoclinic phase, illustrates that stabilizer yittrium oxide has been dissolved into zirconium oxide crystalline substance
Among lattice.
1000 parts of YSZ clinkers are accurately weighed respectively, and dispersant polyethylene glycol is 10 parts, adds deionized water, obtains clinker
Slurries；It is the 65% of YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in clinker slurries, and clinker slurries are passed through ball milling
Machine ball milling 12h, abrasive body are the zirconia ball of 20~30mm of particle diameter, and rotational speed of ball-mill 80r/min, obtains ball milling slurries.
Slurry after ball milling is imported in sand mill, it is YSZ clinkers and deionized water gross mass to adjust YSZ clinkers in slurry
55%, continue be sanded 2h, abrasive body be 0.1~0.2mm of particle diameter zirconium oxide bead, sand milling rotating speed is 1200r/min, obtains sand
Grinding slurry.Field emission electron flying-spot microscope detection is carried out to the obtained YSZ ceramic powders being sanded in slurries, it is known that, it is sanded
YSZ ceramic powders have been refined to Nano grade, uniform particle sizes, less than 100 nanometers afterwards.
Slurries will be sanded to export and add 0.3% polyvinyl alcohol adhesive of YSZ clinker gross masses, carry out spraying and make
Grain, you can the YSZ ceramic prilling powders used for plasma spraying that particle diameter is 30~80 μm, sphericity and good fluidity are obtained, wherein
It is that atomization frequency is 48Hz to set Spray granulation equipment technological parameter, 320 DEG C of inlet air temperature, 100 DEG C of leaving air temp.
The YSZ ceramic prilling powders used for plasma spraying being prepared are carried out to the preparation of thermal barrier coating, obtain the painting of a thermal boundarys
Layer, b thermal barrier coatings, c thermal barrier coatings and d thermal barrier coatings；The institutional framework of 4 thermal barrier coatings is consistent；And 4 thermal barrier coatings
Service life is suitable.YSZ ceramic prilling powders performance provided by the invention is stablized, and the thermal barrier coating that same batch is prepared uses the longevity
Order homogeneous.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of YSZ ceramic prilling powders used for plasma spraying, comprises the following steps：
(1) mixed raw material comprising yittrium oxide and zirconium oxide is provided；The particle diameter of the mixed raw material is 0.5~4 μm；
(2) mixed raw material is mixed with starch, carries out high-temperature roasting, obtain YSZ clinkers；The temperature of the high-temperature roasting is
1350~1550 DEG C；
(3) the YSZ clinkers that the step (2) obtains are mixed with dispersant and water, carries out ball-milling treatment, obtain ball milling slurries；
(4) the ball milling slurries for obtaining the step (3) carry out sanded treatment, obtain that slurries are sanded；
(5) the sand milling slurries that the step (4) obtains are mixed with binding agent, is granulated, obtain YSZ potteries used for plasma spraying
Porcelain pelletizing.
2. preparation method according to claim 1, it is characterised in that the matter of zirconium oxide and yittrium oxide in the mixed raw material
It is (900~940) to measure ratio：(60~100).
3. preparation method according to claim 1 or 2, it is characterised in that the preparation method of the mixed raw material includes：Will
Mixed slurry containing zirconium oxide, yittrium oxide, dispersant and water carries out ball-milling treatment and drying process successively, obtains comprising oxidation
The mixed raw material of yttrium and zirconium oxide；
The mass ratio of the gross mass and water of zirconium oxide and yittrium oxide is (55~65) in the mixed slurry：(35~45)；
The quality of dispersant and the zirconium oxide and the ratio of the gross mass of yittrium oxide are 100 in the mixed slurry:(0.20~
1.0)。
4. preparation method according to claim 1, it is characterised in that the time of step (2) high temperature roasting for 2~
6h。
5. the preparation method according to claim 1 or 4, it is characterised in that starch and mixed raw material in the step (2)
Mass ratio is (2~6)：100.
6. preparation method according to claim 1, it is characterised in that the dispersant in the step (3) is polyacrylic acid
One or more in ammonium, sodium tripolyphosphate, calgon, polymethylacrylic acid ammonia and polyethylene glycol；
The mass ratio of the dispersant and YSZ clinkers is (0.2~1.0)：100；
The mass ratio of the quality of YSZ clinkers and water is (55~65) in the step (3)：(35~45).
7. the preparation method according to claim 1 or 6, it is characterised in that the rotating speed of ball-milling treatment is in the step (3)
40~80r/min, the time of the ball-milling treatment is 12~24h.
8. preparation method according to claim 1, it is characterised in that the rotating speed of sanded treatment is 800 in the step (4)
~1200r/min, the time of the sanded treatment is 2~6h.
9. preparation method according to claim 1, it is characterised in that the dosage of binding agent is with described in the step (5)
The quality meter of YSZ clinkers in slurries is sanded, the mass ratio of the YSZ clinkers and binding agent is 100:(0.3~1.5).
10. the YSZ ceramic prilling powders used for plasma spraying that the preparation method described in claim 1~9 any one obtains, bag
Include：The stabilized with yttrium oxide agent of the zirconium oxide and 6~10wt% of 90~94wt%；The particle diameter of the YSZ ceramic prilling powders for 30~
150μm。
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