CN112225569A - BSAS powder solid-phase synthesis method for environmental barrier coating - Google Patents

BSAS powder solid-phase synthesis method for environmental barrier coating Download PDF

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CN112225569A
CN112225569A CN202011114520.7A CN202011114520A CN112225569A CN 112225569 A CN112225569 A CN 112225569A CN 202011114520 A CN202011114520 A CN 202011114520A CN 112225569 A CN112225569 A CN 112225569A
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powder
bsas
environmental barrier
phase synthesis
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范金娟
贺世美
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AECC Beijing Institute of Aeronautical Materials
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    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
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Abstract

The invention provides a solid-phase synthesis method of BSAS powder for an environmental barrier coating, belonging to the technical field of coating materials. The solid phase synthesis method adopts BaCO3、SrCO3、Al(OH)3And SiO2Mixing raw materials according to a certain molar ratio, ball-milling, drying, sieving and sintering to obtain blocky BSAS; adding a certain proportion of Arabic gum, ammonium citrate and deionized water for ball milling; and performing ball milling again, and performing spray granulation to obtain hollow spherical BSAS powder. The invention has simple process, easy operation, low synthesis temperature and low production cost; the BSAS powder synthesized by the invention has a single-phase structure, the particle size is distributed between 40 and 125 mu m, the structure is stable at a high temperature of 1400 ℃, and the synthesized BSAS powderThe powder has good fluidity and is suitable for preparing the BSAS environmental barrier coating by plasma spraying.

Description

BSAS powder solid-phase synthesis method for environmental barrier coating
Technical Field
The invention belongs to the technical field of environmental barrier coating materials, and particularly relates to a BSAS powder solid-phase synthesis method for an environmental barrier coating.
Background
The SiC-based composite material has excellent performances of high specific strength, high specific modulus, high temperature resistance, oxidation resistance and the like, and is an ideal material for hot end parts of engines. The SiC-based composite material has higher high-temperature oxidation resistance in a dry environment, but has higher high-temperature oxidation resistance in the dry environmentIn the service environment of an engine, the SiC-based composite material reacts with water vapor to generate Si (OH)4Gas, performance degrades rapidly and environmental barrier coatings are the key technology to solve this problem.
The BSAS has stable structure under high-temperature environment, has better high-temperature water oxygen resistance, has a thermal expansion coefficient close to that of a SiC composite material substrate, and is one of main materials of an environmental barrier coating. The BSAS environmental barrier coating is generally prepared by a plasma spraying method, and the environmental barrier coating prepared by the NASA plasma spraying process passes 14000h trial examination, so that the service life of the SiC composite material is greatly prolonged.
Plasma spraying is used to prepare the BSAS coating by melting and accelerating BSAS powder with high-temperature, high-speed and high-enthalpy plasma flame flow and spraying the BSAS powder onto a substrate. The sprayed powder is generally in a hollow spherical shape and has better fluidity. The preparation process of the BSAS powder has less literature, no mature product can be purchased in the domestic market, and the preparation of the BSAS powder is the premise of coating preparation.
Disclosure of Invention
The invention provides a BSAS powder solid-phase synthesis method for an environmental barrier coating, which adopts BaCO3、SrCO3、Al(OH)3And SiO2Mixing raw materials according to a certain molar ratio, ball-milling, drying, sieving and sintering to obtain blocky BSAS; adding a certain proportion of Arabic gum, ammonium citrate and deionized water for ball milling; and performing ball milling again, and performing spray granulation to obtain hollow spherical BSAS powder. The BSAS powder synthesized by the invention has a single-phase structure, the particle size distribution is 40-125 mu m, and the structure is stable at a high temperature of 1400 ℃. The invention has simple process, easy operation, low synthesis temperature and low production cost; the synthesized powder has good fluidity and is suitable for preparing the BSAS environmental barrier coating by plasma spraying.
The technical scheme of the invention is as follows: a BSAS powder solid-phase synthesis method for an environmental barrier coating is characterized by comprising the following steps:
the method comprises the following steps: mixing BaCO3, SrCO3, Al (OH)3 and SiO2 powder according to the molar ratio of (0.7-0.8) to (0.2-0.3) to (0.9-1.1) to (1.9-2.1), adding 400ml of deionized water (convenient for ball milling rotation) and carrying out rapid ball milling for 3-4 h;
step two: drying the ball-milled powder for 11-13h at 90-110 ℃, and sieving the powder with a 40-mesh sieve with the particle size of 280-320 mu m;
step three: placing the powder obtained in the step three in a muffle furnace for sintering at the temperature of 1200-1400 ℃ for 8-10h to obtain blocky BSAS;
step four: grinding the block BSAS by a hand mill to obtain particles with the particle size of 1-3mm, adding Arabic gum, ammonium citrate and deionized water according to the mass ratio of (0.9-1.1): 0.01-0.03): 0.007-0.009): 0.9-1.1), and ball-milling for 20-25 h;
step five: sieving the obtained powder with a 40-mesh sieve, and performing spray granulation to obtain BSAS powder;
step six: and (3) sieving the BSAS powder obtained in the step (a) by a 100-mesh sieve to obtain BSAS powder solid-phase powder particles with the particle size range of 40-125 mu m for plasma spraying.
The raw materials are solid BaCO3, SrCO3, Al (OH)3 and SiO2 powder, the purity is more than or equal to 95%, and the optimal mixing ratio is 0.75:0.25:1: 2.
The optimal sintering temperature is 1200 ℃, and the sintering time is 10 h.
The optimal mass ratio of the added Arabic gum, ammonium citrate and deionized water to the BSAS is 1:0.02:0.008: 1.
And (3) after the powder is sieved by a 40-mesh sieve, carrying out spray granulation.
And sieving the powder subjected to spray granulation by a 140-mesh sieve to ensure that the particle size distribution range is 40-125 mu m.
The synthesized BSAS powder was hollow spherical. The invention has the beneficial effects that: BaCO of the invention3、SrCO3、Al(OH)3And SiO2Uniformly mixing raw materials in proportion, performing ball milling, drying, sieving and sintering to obtain blocky BSAS; adding a certain proportion of Arabic gum, ammonium citrate and deionized water, ball milling, and spray granulating to obtain hollow spherical BSAS powder. The invention has simple process, easy operation, low synthesis temperature and low production cost; the synthesized BSAS powder has a single-phase structure, the particle size distribution is 40-125 mu m, the structure is stable at the high temperature of 1400 ℃, the powder flowability is good, and the BSAS powder is suitable for being used for the likeAnd preparing the BSAS environmental barrier coating by ion spraying.
Drawings
FIG. 1 shows the morphology of BSAS powder;
FIG. 2 is a BSAS powder structure;
fig. 3 shows the coefficient of thermal expansion of the BSAS powder structure.
Detailed Description
Example 1
The invention relates to a BSAS powder solid-phase synthesis method for an environmental barrier coating, which comprises the following steps:
the method comprises the following steps: selecting BaCO with purity more than or equal to 95%3、SrCO3、Al(OH)3And SiO2Powder as raw material, weighing BaCO3Powder 300g, SrCO364g of powder, Al (OH)3Powder 304g and SiO2248g of powder, uniformly mixing, adding 400ml of deionized water, and rapidly ball-milling for 3 hours;
step two: drying the ball-milled powder for 13h at 90 ℃, and sieving the powder with a 40-mesh sieve, wherein the granularity is 280-300 mu m;
step three: sintering the powder obtained in the step three in a muffle furnace at 1200 ℃ for 10h to obtain blocky BSAS;
step four: grinding the block BSAS by hand to 1-3mm, adding Arabic gum, ammonium citrate and deionized water, and ball-milling for 22h, wherein the mass ratio of the Arabic gum to the ammonium citrate to the deionized water to the BSAS is 9:0.1:0.07: 9;
step five: sieving the obtained powder with a 40-mesh sieve, and performing spray granulation to obtain BSAS powder;
step six: and (3) sieving the powder obtained in the step (a) by a 140-mesh sieve to obtain BSAS powder particles with the particle size range of 40-125 mu m for plasma spraying.
Example 2
The method comprises the following steps: selecting BaCO with purity more than or equal to 95%3、SrCO3、Al(OH)3And SiO2Powder as raw material, weighing BaCO3321g of powder SrCO3Powder 80.1g, Al (OH)3338.2g powder and SiO2260.6g of powder, uniformly mixing, adding 500ml of deionized water, and rapidly ball-milling for 3 hours;
step two: drying the ball-milled powder at 100 ℃ for 12h, and sieving the powder with a 40-mesh sieve to obtain powder with the particle size of 300-320 mu m;
step three: placing the powder obtained in the step three in a muffle furnace, and sintering for 9 hours at 1300 ℃ to obtain blocky BSAS;
step four: manually grinding the block BSAS to 1-3mm, adding Arabic gum, ammonium citrate and deionized water, wherein the mass ratio of the Arabic gum, the ammonium citrate, the deionized water to the BSAS is 1:0.02:0.008:1, and ball-milling for 25 hours;
step five: sieving the obtained powder with a 40-mesh sieve, and performing spray granulation to obtain BSAS powder;
step six: and (3) sieving the powder obtained in the step (a) by a 140-mesh sieve to obtain BSAS powder particles with the particle size range of 40-125 mu m for plasma spraying.
Example 3
The method comprises the following steps: selecting BaCO with purity more than or equal to 95%3、SrCO3、Al(OH)3And SiO2Powder as raw material, weighing BaCO3342g of powder SrCO3Powder 96g, Al (OH)3Powder 372g and SiO2274g of powder is uniformly mixed, and 600ml of deionized water is added for rapid ball milling for 3 hours;
step two: drying the ball-milled powder for 11h at 110 ℃, and sieving the powder with a 40-mesh sieve to obtain powder with the particle size of 300-320 mu m;
step three: placing the powder obtained in the step three in a muffle furnace, and sintering for 8 hours at 1400 ℃ to obtain blocky BSAS;
step four: manually grinding the block BSAS to 1-3mm, adding Arabic gum, ammonium citrate and deionized water, wherein the mass ratio of the Arabic gum to the ammonium citrate to the deionized water to the BSAS is 1.1:0.03:0.009:1.1, and ball-milling for 25 h;
step five: sieving the obtained powder with a 40-mesh sieve, and performing spray granulation to obtain BSAS powder;
step six: and (3) sieving the powder obtained in the step (a) by a 140-mesh sieve to obtain BSAS powder particles with the particle size range of 40-125 mu m for plasma spraying.

Claims (7)

1. A BSAS powder solid-phase synthesis method for an environmental barrier coating is characterized by comprising the following steps:
the method comprises the following steps: mixing BaCO3、SrCO3、Al(OH)3And SiO2Mixing the powder according to the molar ratio of (0.7-0.8) to (0.2-0.3) to (0.9-1.1) to (1.9-2.1), adding 400ml of deionized water (convenient for ball milling rotation) and rapidly ball milling for 3-4 h;
step two: drying the ball-milled powder for 11-13h at 90-110 ℃, and sieving the powder with a 40-mesh sieve with the particle size of 280-320 mu m;
step three: placing the powder obtained in the step three in a muffle furnace for sintering at the temperature of 1200-1400 ℃ for 8-10h to obtain blocky BSAS;
step four: grinding the block BSAS by a hand mill to obtain particles with the particle size of 1-3mm, adding Arabic gum, ammonium citrate and deionized water according to the mass ratio of (0.9-1.1): 0.01-0.03): 0.007-0.009): 0.9-1.1), and ball-milling for 20-25 h;
step five: sieving the obtained powder with a 40-mesh sieve, and performing spray granulation to obtain BSAS powder;
step six: and (3) sieving the BSAS powder obtained in the step (a) by a 100-mesh sieve to obtain BSAS powder solid-phase powder particles with the particle size range of 40-125 mu m for plasma spraying.
2. The method of solid phase synthesis of BSAS powder for environmental barrier coatings of claim 1 wherein in step one, the starting material is solid BaCO3、SrCO3、Al(OH)3And SiO2The purity of the powder is more than or equal to 95 percent, and the optimal mixing ratio is 0.75:0.25:1: 2.
3. The method for solid phase synthesis of BSAS powder for environmental barrier coatings of claim 1 wherein in step three, the optimum sintering temperature is 1200 ℃ and the sintering time is 10 hours.
4. The solid-phase synthesis method of BSAS powder for environmental barrier coatings according to claim 1, wherein in step six, the optimal mass ratio of added gum arabic, ammonium citrate and deionized water to BSAS is 1:0.02:0.008: 1.
5. The method for solid phase synthesis of BSAS powder for environmental barrier coatings of claim 1, where in step five, the powder is passed through a 40 mesh sieve and then spray granulated.
6. The method of solid phase synthesis of BSAS powder for environmental barrier coatings of claim 1, in which the powder after spray granulation is passed through a 140 mesh sieve to ensure a particle size distribution in the range of 40 to 125 μm.
7. The method of solid phase synthesis of BSAS powder for environmental barrier coatings according to claim 1, in which the BSAS powder synthesized is in the form of hollow spheres.
CN202011114520.7A 2020-10-16 2020-10-16 BSAS powder solid-phase synthesis method for environmental barrier coating Pending CN112225569A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090202735A1 (en) * 2008-02-13 2009-08-13 Saint-Gobain Centre De Recherches Et D'etudes Europeen Bsas powder
CN104003697A (en) * 2014-06-10 2014-08-27 中南大学 Preparation method of BSAS composite ceramic powder
CN106116702A (en) * 2016-06-27 2016-11-16 中国科学院长春应用化学研究所 A kind of Cfthe preparation method of/SiC ceramic matrix composite material surface high-temp oxidation-inhibited thermal barrier coating
CN107746267A (en) * 2017-10-11 2018-03-02 中国航发北京航空材料研究院 A kind of Ba used for plasma sprayingxSr1‑xAl2Si2O8Raw powder's production technology
CN109485396A (en) * 2017-12-29 2019-03-19 西安航天复合材料研究所 A kind of preparation method of Environmental Barrier Coatings on Si-based Ceramics BSAS ceramic powders
CN109485387A (en) * 2017-12-29 2019-03-19 西安航天复合材料研究所 A kind of preparation method of Environmental Barrier Coatings on Si-based Ceramics hollow ball shape BSAS powder

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090202735A1 (en) * 2008-02-13 2009-08-13 Saint-Gobain Centre De Recherches Et D'etudes Europeen Bsas powder
CN104003697A (en) * 2014-06-10 2014-08-27 中南大学 Preparation method of BSAS composite ceramic powder
CN106116702A (en) * 2016-06-27 2016-11-16 中国科学院长春应用化学研究所 A kind of Cfthe preparation method of/SiC ceramic matrix composite material surface high-temp oxidation-inhibited thermal barrier coating
CN107746267A (en) * 2017-10-11 2018-03-02 中国航发北京航空材料研究院 A kind of Ba used for plasma sprayingxSr1‑xAl2Si2O8Raw powder's production technology
CN109485396A (en) * 2017-12-29 2019-03-19 西安航天复合材料研究所 A kind of preparation method of Environmental Barrier Coatings on Si-based Ceramics BSAS ceramic powders
CN109485387A (en) * 2017-12-29 2019-03-19 西安航天复合材料研究所 A kind of preparation method of Environmental Barrier Coatings on Si-based Ceramics hollow ball shape BSAS powder

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