CN110668812B - Nano zirconium oxide spraying powder and preparation method thereof - Google Patents
Nano zirconium oxide spraying powder and preparation method thereof Download PDFInfo
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Abstract
The invention provides a non-hollow porous spherical structure powder consisting of yttria partially stabilized nano zirconia (YSZ) aggregates with the mass fraction of (7-8) wt%. The porosity of the powder particles is 40-70%, and the surface of the powder particles is of a porous rough structure. The powder is prepared by adopting a conventional spray granulation process: firstly, dispersing nano YSZ aggregate by using sand grinding, then adding a flocculating agent into the dispersed slurry to enable the nano particles to aggregate to form loose flocculent aggregate, thereby inhibiting the nano particles from migrating to the surface in the spray granulation process, avoiding forming a hollow structure, and finally preparing the non-hollow porous spherical structure powder with high porosity. The YSZ coating with high porosity, high cohesive strength and sintering resistance can be prepared by adopting the powder.
Description
Technical Field
The invention belongs to the field of nano ceramic materials, and particularly relates to nano zirconia spraying powder for preparing a high-porosity, high-cohesion-strength and sintering-resistant coating and a preparation method thereof.
Background
The plasma spraying (7-8) wt% yttria partially stabilized zirconia (YSZ) coating has extremely low thermal conductivity (1.5 w/m.k), high melting point (2700 ℃), high creep temperature (2400 ℃), excellent mechanical property and thermal expansion coefficient similar to that of high temperature alloy, and is widely used for thermal insulation protection of high temperature alloy parts such as aeroengine, gas turbine blades, rocket engine jet pipes and the like. The YSZ coating can be used for reducing the working temperature of the component and prolonging the service life of the component, and meanwhile, the thrust-weight ratio of the engine can be improved by improving the working temperature of the engine on the premise of ensuring the service life of the engine.
The properties of YSZ coatings include mainly thermal insulation capability and service life. The thermal insulation capacity of the coating is mainly determined by the thermal conductivity of the coating, and the service life of the coating is mainly determined by the thermal shock resistance and the sintering resistance of the coating. Research shows that the higher the porosity and the cohesive strength of the coating, the lower the thermal conductivity of the coating, and the better the thermal shock resistance and the sintering resistance, so that the preparation of the coating with high porosity and high cohesive strength is always the research focus in the field.
In the process of preparing the YSZ coating by plasma spraying, spraying powder is firstly melted by plasma flame flow to form molten drops, the molten drops collide with a base material and then spread and solidify to form flat particles, and the flat particles are stacked to form the coating. The porosity in the coating is mainly due to the gas encapsulated in the droplets and to the bridging defects when the flat particles are stacked. The porosity of the YSZ coating can be generally increased by two technical approaches: firstly, through the particle diameter of increase spraying powder, increase the area of spreading of flat particle, increase the overlap joint defect, and then promote the porosity of coating. For example, the current spraying powder is composed of particles with a particle size distribution (10-106) um, and the porosity of the coating prepared by the powder is generally within 12%. If the fine powder with the particle size smaller than 45um is screened out, the coating with the pore size higher than 12 percent can be prepared only by adopting the powder with the particle size larger than 45 um. However, this method has disadvantages in that the lack of easily meltable fine powder in the powder results in a decrease in the cohesive strength of the coating layer, deterioration in the thermal shock resistance, a decrease in the utilization of the powder, and an increase in the production cost.
Another approach is to increase the porosity of the coating by increasing the porosity of the powder particles appropriately. In the early coating preparation, dense granular powder is adopted, and the porosity of the coating is generally within 5 percent; at present, the spray powder for preparing the high-porosity coating is mostly prepared by carrying out spray granulation on micron or submicron YSZ particles, the porosity of the powder particles can be up to 40 percent, and the coating with the porosity of 12 percent can be prepared by adopting the powder. However, due to the size and porosity of the adopted micron or submicron YSZ particles and the particle size of the granulated powder, further increasing the porosity of the powder particles often results in the decrease of the skeleton strength of the powder particles, which are easily broken in high-temperature plasma flame flow, and affect the deposition efficiency of the coating.
The nano powder has large specific surface area and low apparent density, and can theoretically prepare spraying powder with higher particle porosity. However, many studies have shown that nanoparticles are small in mass, and thus when spray granulation is performed, nanoparticles migrate to the particle surface by capillary force generated by water evaporation, and form a thin-walled hollow powder, which cannot form a porous structure. When the powder is used for preparing a coating, because gas in the powder is concentrated in the center of the particles, thin-wall molten drops similar to balloons are formed after the particles are melted. According to related researches, during the process that the thin-wall molten drop collides with a matrix and is solidified to form flat particles, most of gas in the thin-wall molten drop escapes, and finally, a coating with a porosity of less than 12% and a high flat particle interface is formed. Although the coating has low thermal conductivity, the interface of flat particles is easy to sinter at high temperature, and after the coating is used at high temperature for a short time, the thermal conductivity is rapidly increased, so that the heat insulation capability is reduced.
Although research shows that spherical powder with porosity of more than 40% can be prepared by using nano YSZ as raw material and adopting Spray freezing method (Spray freezing), the Spray freezing method needs to slowly remove ice in the powder in a sublimation way under low temperature and vacuum conditions, so that equipment investment is large, efficiency is low, production cost is extremely high, and related reports for preparing high-porosity Spray powder do not exist at present.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a high-porosity nano zirconia spray powder and a preparation method thereof, aiming at the defects of the prior art. By adopting the powder, the sintering-resistant YSZ coating with high porosity and high cohesive strength can be prepared.
In order to achieve the purpose, the technical scheme of the invention is as follows: a nano zirconia spraying powder is a non-hollow porous spherical structure consisting of nano YSZ aggregates containing (7-8) wt% of yttria, the porosity of powder particles is between 40-70%, the surface of the powder particles is a porous rough structure, and the powder is prepared by adopting a spray granulation process.
A preparation method of nano zirconia spraying powder comprises the following steps:
step one, uniformly mixing nano YSZ powder with yttrium oxide content of 7-8%, deionized water and a dispersing agent to obtain slurry;
step two, adopting a sand mill to grind the slurry until the particle size is less than 300 nm;
step three, adding a flocculating agent into the ground slurry, and uniformly stirring at a low speed;
step four, adding the adhesive into the uniformly stirred slurry in the step three, and continuously stirring at a low speed until the slurry is uniform;
step five, carrying out spray drying treatment on the slurry obtained in the step four to obtain granulated materials;
sixthly, placing the granulated material in a sintering furnace, keeping the temperature at 400 ℃ for 1-2 h at a temperature rise rate of not higher than 300 ℃/h, keeping the temperature at 1300 ℃ for 1-2 h, and naturally cooling after the temperature is kept;
and seventhly, screening the sintered powder, and reserving the powder with the particle size of (20-90) um to obtain the nano zirconia spraying powder.
As an improvement of the invention, in the first step, the grain size of the nano YSZ agglomerated powder is (20-80) nm, and the solid content of the nano YSZ powder in the slurry is (20-35)%; the dispersant is ammonium polyacrylate, and the dosage of the dispersant is 0.5-1.0 percent of the weight of the nano YSZ powder.
As an improvement of the invention, the flocculant in the third step is anionic polyacrylamide, the molecular weight of the flocculant is 8000-12000, and the dosage of the flocculant is (0.05-0.2)% of the weight of the nano YSZ powder; the stirring speed is (10-30) revolutions per minute.
As an improvement of the invention, the adhesive in the fourth step is acrylic resin, and the amount of the adhesive is 1-3% of the weight of the nano YSZ powder; the stirring speed is (10-30) revolutions per minute.
As an improvement of the invention, in the fifth step, during spray granulation, the inlet temperature is 300-400 ℃ and the outlet temperature is 110-120 ℃.
The basic principle of the invention is that nano YSZ is firstly prepared into a loose and porous flocculating constituent, then the flocculating constituent is prepared into spherical spraying powder with high porosity by utilizing spray granulation, and the increase of the porosity of the spraying powder particles is mainly beneficial to the porosity in the loose flocculating constituent. Compared with the prior art, the invention has the following advantages: 1) compared with the technical scheme of preparing the high-porosity coating by adopting powder of more than 45um at the present stage, the powder of the invention reserves the more easily-melted fine powder due to the increase of the porosity of the powder particles, the phenomenon of obvious decrease of the cohesive strength of the coating is avoided, and the YSZ coating with high porosity and high cohesive strength can be prepared.
2) Compared with other processes for preparing spraying powder by adopting nano YSZ at the present stage, the method adopts a sand milling process and an ammonium polyacrylate dispersant to disperse nano YSZ aggregates, and simultaneously, polyacrylamide is added into the slurry. After the polyacrylamide is dissociated in water, one end of a high molecular group of the polyacrylamide is adsorbed on the surface of the nano-particles, and the other end of the high molecular group of the polyacrylamide is mutually wound to connect the nano-particles in the slurry into loose and flocculent aggregates. During spray granulation, on one hand, nanoparticles are mutually held by macromolecular groups, and loose flocculent aggregates are mutually rubbed to form a barrier, so that the nanoparticles are inhibited from migrating to the surface, and hollow-structure powder is prevented from being formed; on the other hand, the loose flocculent aggregate is a loose porous structure, compared with the conventional granulation adopting nano powder or an aggregate thereof, the porosity of the granulated powder particles can be increased, so that porous network structure powder with higher porosity is formed, and the size of the flocculent aggregate can be controlled by controlling the addition of the dispersing agent and the flocculating agent and controlling the stirring speed, so that the spraying powder with different particle porosities is prepared;
3) the invention can lead the porosity of the spraying powder particles to be between 40 and 70 percent by optimizing the addition of the dispersing agent, the addition of the flocculating agent and the stirring speed. On one hand, the porosity of the particles is improved to be more than 40%, the high-porosity coating can be prepared under the condition that fine powder is not screened out, on the other hand, the porosity of the particles is controlled within 70%, the situation that after the powder is melted, gas in molten drops is combined to form large bubbles can be avoided, a coating structure similar to hollow structure powder is finally formed, and the sintering-resistant coating with high porosity cannot be obtained.
4) The anionic polyacrylamide used in the invention is a flocculant commonly used in daily industry, has low price and low dosage, and does not obviously increase the cost.
5) Because the nano particles in the slurry are flocculated into the porous flocculent aggregates, compared with the conventional spraying powder, the powder prepared by the invention has a porous rough surface, the flowing property is slightly reduced compared with the conventional spraying powder, and the flowing property requirement of the spraying process on the powder can be still well met.
Drawings
FIG. 1 is a surface SEM photograph of a nano zirconia spray powder of the present invention;
FIG. 2 is a SEM image of a cross section of a nano zirconia spray powder according to the present invention;
FIG. 2A is a coating prepared from a nano zirconia spray powder of the present invention;
fig. 2B shows a high porosity coating prepared using a commercially available powder having a particle size of 45um or greater.
Detailed Description
For the purpose of enhancing an understanding of the present invention, the following detailed description is given in conjunction with examples.
Example 1:
referring to fig. 1 and 2, a method for preparing nano zirconia spray powder includes the following steps:
the method comprises the following steps: nano YSZ powder with the grain size of 40nm and the yttrium oxide content of 7.2 wt% and deionized water are mixed according to the weight ratio of 1: 3, mixing, adding a dispersing agent accounting for 1 percent of the weight of the YSZ powder, and uniformly mixing to obtain slurry;
step two: grinding the slurry by a sand mill until the particle size in the slurry is less than 200 nm;
step three: adding anionic polyacrylamide with molecular weight of 8000 into the ground slurry, wherein the addition amount is 0.1% of the weight of the nano YSZ powder, and stirring uniformly at a stirring speed of 30 r/min;
step four: continuously adding acrylic resin into the slurry, wherein the adding amount is 2% of the weight of the nano YSZ powder, and continuously stirring the mixture to be uniform at a stirring speed of 30 revolutions per minute;
step five: carrying out spray drying treatment on the slurry to obtain a granulation material; the inlet temperature during granulation is 340 ℃, and the outlet temperature is 110 ℃;
step six: placing the granulated material in a sintering furnace, keeping the temperature at 400 ℃ for 2h and 1300 ℃ for 2h, and naturally cooling after sintering;
step seven: and screening the sintered powder to remove the powder with the particle size smaller than 20um and larger than 90um, and finally obtaining the nano zirconia spraying powder.
SEM photographs of the surface and the section of the nano zirconia spraying powder prepared by the embodiment of the invention are shown in attached figures 1 and 2. As can be seen from the attached drawings, the powder prepared by the invention has a spherical porous structure and a relatively rough surface, unlike the powder with a hollow structure prepared by common nano powder.
The porosity of the powder particles was 60.7% as measured by mercury intrusion method, the powder flow rate was 41s/50g as measured by Hall flow meter, and the apparent density was 1.96g/cm3The flowability of the common spraying powder is less than 60s/50g, and the apparent density is more than 1.8g/cm3The technical requirements of (1).
The coating prepared from the nano zirconia spray powder of the invention is compared with a high porosity coating prepared from powder with the particle size of more than 45um sold in the market. The spraying equipment is a Metco 9MB plasma spraying system. The lower graph is a cross-sectional SEM of both coatings, from which it can be seen that the porosity of both coatings is around 19%.
FIG. 2A shows that the porosity of the coating prepared from the nano zirconia powder of the present invention is 19.2%
FIG. 2B shows a high porosity coating prepared from a commercially available powder having a particle size of 45um or more, the porosity of which is 18.6%
The bonding strength of the coating was tested using the ASTM C633 standard, the thermal shock resistance of the coating was tested using water cooling at 1050 ℃, and the thermal conductivity of the coating was tested using the laser pulse method, with the results shown in table 1.
Table 1 comparison of performance tests of two powder coatings
As can be seen from table 1, the porosity and thermal conductivity of the two powder coatings are similar, but since the average cohesive strength of the coatings prepared from the powder of the invention is much higher than that of the comparative powder coating, the thermal shock resistance of the powder coating of the invention is close to 1.8 times that of the comparative powder. By adopting the powder disclosed by the invention, the YSZ coating with high porosity and high cohesive strength can be prepared.
Example 2:
the preparation method of the nano zirconia spraying powder comprises the following steps:
the method comprises the following steps: nano YSZ powder with the grain size of 30nm and the content of yttrium oxide of 7.5 wt% and deionized water are mixed according to the weight ratio of 1: 2.5, adding a dispersant accounting for 0.8 percent of the weight of the YSZ powder, and uniformly mixing to obtain slurry;
step two: grinding the slurry by a sand mill until the particle size in the slurry is less than 100 nm;
step three: adding anionic polyacrylamide with the molecular weight of 10000 into the ground slurry, wherein the addition amount of the anionic polyacrylamide is 0.18 percent of the weight of the nano YSZ powder, and stirring the mixture to be uniform at the stirring speed of 20 r/min;
step four: continuously adding acrylic resin into the slurry, wherein the adding amount is 1.5 percent of the weight of the nano YSZ powder, and continuously stirring the mixture to be uniform at the stirring speed of 30 revolutions per minute;
step five: carrying out spray drying treatment on the slurry to obtain a granulation material; the inlet temperature during granulation is 380 ℃, and the outlet temperature is 120 ℃;
step six: placing the granulated material in a sintering furnace, keeping the temperature at 400 ℃ for 1h and 1300 ℃ for 1.5h at the heating rate of 150 ℃/h, and naturally cooling after sintering;
step seven: and screening the sintered powder to remove the powder with the particle size smaller than 20um and larger than 90um, and finally obtaining the nano zirconia spraying powder.
The porosity of the powder particles was 64.3% as measured by mercury intrusion method, the powder flow rate was 43s/50g as measured by Hall flow meter, and the apparent density was 2.03g/cm3The flowability of the common spraying powder is less than 60s/50g, and the apparent density is more than 1.8g/cm3The technical requirements of (1). The coating prepared from the nano zirconia spray powder of the present invention was compared with a coating using a commercially available hollow powder. The spraying equipment is a Metco 9MB plasma spraying system, the performances of the two powder coatings are shown in the table 2, and the thermal conductivity after the heat treatment is that the coating is sintered for 100 hours at 1350 ℃, and then the thermal conductivity test is carried out.
Table 2 comparison of the performance tests of two powder coatings
As can be seen from table 2, although the porosity of the two powder coatings differs greatly, the two powder coatings have similar cohesive strength, thermal shock resistance, and initial thermal conductivity. However, after heat treatment, the thermal conductivity of the powder coating of the invention only increased slightly, compared to a large increase in the thermal conductivity of the hollow powder coating, indicating that the powder coating of the invention is more resistant to sintering.
Example 3:
the preparation method of the nano zirconia spraying powder comprises the following steps:
the method comprises the following steps: nano YSZ powder with the grain size of 80nm and the content of yttrium oxide of 7.25 wt% and deionized water are mixed according to the weight ratio of 1: 2, mixing, adding a dispersing agent accounting for 0.5 percent of the weight of the YSZ powder, and uniformly mixing to obtain slurry;
step two: grinding the slurry by a sand mill until the particle size in the slurry is less than 300 nm;
step three: adding anionic polyacrylamide with the molecular weight of 12000 into the ground slurry, wherein the addition amount of the anionic polyacrylamide is 0.06 percent of the weight of the nano YSZ powder, and stirring the mixture to be uniform at the stirring speed of 20 r/min;
step four: continuously adding acrylic resin into the slurry, wherein the adding amount is 1.5 percent of the weight of the nano YSZ powder, and continuously stirring the mixture to be uniform at the stirring speed of 30 revolutions per minute;
step five: carrying out spray drying treatment on the slurry to obtain a granulation material; the inlet temperature during granulation is 360 ℃, and the outlet temperature is 120 ℃;
step six: placing the granulated material in a sintering furnace, keeping the temperature at 400 ℃ for 1h and 1300 ℃ for 1.5h at the heating rate of 150 ℃/h, and naturally cooling after sintering;
step seven: and screening the sintered powder to remove the powder with the particle size smaller than 20um and larger than 90um, and finally obtaining the nano zirconia spraying powder.
The porosity of the powder particles was 47.5% as measured by mercury intrusion method, the powder flow rate was 45s/50g as measured by Hall flow meter, and the apparent density was 1.91g/cm3The flowability of the common spraying powder is less than 60s/50g, and the apparent density is more than 1.8g/cm3The technical requirements of (1). The properties of the coating prepared by using the nano zirconia spray powder of the invention are shown in table 3 by adopting a Metco 9MB plasma spray system as spray equipment, and the thermal conductivity after heat treatment is that the coating is sintered for 100 hours at 1350 ℃ and then is subjected to thermal conductivity test.
TABLE 3 Properties of the coatings of the examples of the invention
It can be seen from table 3 that with the spray powder according to the invention, a sintering-resistant coating can be produced which combines a high porosity and a high cohesive strength, in comparison with the properties of the comparative powder coatings in examples 1 and 2.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (6)
1. The nano zirconia spraying powder is characterized in that the powder is a non-hollow porous spherical structure consisting of nano YSZ aggregates containing 7-8 wt% of yttria, the porosity of powder particles is 40-70%, the surface of the powder particles is a porous rough structure, the powder is prepared by adopting a spray granulation process, and a flocculating agent is added into slurry before the spray granulation process.
2. The preparation method of the nano zirconia spraying powder is characterized by comprising the following steps:
step one, uniformly mixing nano YSZ agglomerated powder with yttrium oxide content of 7-8 wt%, deionized water and a dispersing agent to obtain slurry;
step two, adopting a sand mill to grind the slurry until the particle size is less than 300 nm;
step three, adding a flocculating agent into the ground slurry, and uniformly stirring at a low speed;
step four, adding the adhesive into the uniformly stirred slurry in the step three, and continuously stirring at a low speed until the slurry is uniform;
step five, carrying out spray drying treatment on the slurry obtained in the step four to obtain granulated materials;
sixthly, placing the granulated material in a sintering furnace, keeping the temperature at 400 ℃ for 1-2 h at a temperature rise rate of not higher than 300 ℃/h, keeping the temperature at 1300 ℃ for 1-2 h, and naturally cooling after the temperature is kept;
and seventhly, screening the sintered powder, and reserving the powder with the particle size of 20-90 um to obtain the nano zirconia spraying powder.
3. The method for preparing nano zirconia spray powder according to claim 2, wherein in the first step, the grain size of the nano YSZ agglomerated powder is less than 80nm, and the solid content of the nano YSZ powder in the slurry is 20-35%; the dispersant is ammonium polyacrylate, and the dosage of the dispersant is 0.5-1.0% of the weight of the nano YSZ powder.
4. The method for preparing nano zirconia spray powder according to claim 2, wherein the flocculant in step three is anionic polyacrylamide, the molecular weight of which is 8000-12000, and the amount of the flocculant is 0.05-0.2% of the weight of the nano YSZ powder; the stirring speed is 10-30 r/min.
5. The method for preparing nano zirconia spray powder according to claim 2, wherein the adhesive in the fourth step is acrylic resin, and the amount of the adhesive is 1-3% of the weight of the nano YSZ powder; the stirring speed is 10-30 r/min.
6. The method for preparing nano zirconia spray powder according to claim 2, wherein in the fifth step, the inlet temperature is 300-400 ℃ and the outlet temperature is 110-120 ℃ during spray granulation.
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| CN110845233A (en) | 2020-02-28 |
| CN110668813A (en) | 2020-01-10 |
| CN110451957A (en) | 2019-11-15 |
| CN110668812A (en) | 2020-01-10 |
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