CN107746267A - A kind of Ba used for plasma sprayingxSr1‑xAl2Si2O8Raw powder's production technology - Google Patents

A kind of Ba used for plasma sprayingxSr1‑xAl2Si2O8Raw powder's production technology Download PDF

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CN107746267A
CN107746267A CN201710941828.0A CN201710941828A CN107746267A CN 107746267 A CN107746267 A CN 107746267A CN 201710941828 A CN201710941828 A CN 201710941828A CN 107746267 A CN107746267 A CN 107746267A
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powder
ball
melting
plasma spraying
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焦健
焦春荣
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AECC Beijing Institute of Aeronautical Materials
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AECC Beijing Institute of Aeronautical Materials
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3215—Barium oxides or oxide-forming salts thereof

Abstract

The invention belongs to field of inorganic nonmetallic material, more particularly to a kind of Ba used for plasma sprayingxSr1‑xAl2Si2O8Raw powder's production technology.The present invention selection Ba, Sr carbonate or oxalates, Al, Si oxide are as raw material, MgO or CaO is as melting auxiliary agent, deionized water is as decentralized medium, ammonium acrylate is as dispersant, above-mentioned material is mixed evenly according to required ratio using ball-grinding machine, it is placed in after discharging in air dry oven to being completely dried, dried powder, which is placed in high temperature melting furnace, carries out high melt, the chunky shape material of glassy state is obtained after quenching, the material mechanical is crushed to certain particle size, obtains can be directly used for the BSAS powders of spraying after screening.Plasma spraying powder is prepared compared to traditional atomizing granulating technology, the present invention can obtain that porosity is lower, more close Environmental Barrier Coatings on Si-based Ceramics is combined with matrix by plasma spray coating process, while this fine and close design feature also substantially increases the high temperature resistant of coating, the barrier propterty such as anti-oxidant, anticorrosive.

Description

A kind of Ba used for plasma sprayingxSr1-xAl2Si2O8Raw powder's production technology
Technical field
The invention belongs to field of inorganic nonmetallic material, more particularly to a kind of Ba used for plasma sprayingxSr1-xAl2Si2O8Powder The preparation method of body.
Background technology
SiC based composites can be stablized under high temperature drying environment to be used, fine and close in one layer of Surface Creation after oxidation SiO2Film plays a protective role to internal material, but contains the corrosion of fuse salt, vapor or hydrogen in aero-engine In property combustion gas environment, SiO2Film can occur chemical reaction with high-temperature water vapor and generate readily volatilized Si (OH)4, cause SiC bases The performance of composite drastically declines, and the appearance of Environmental Barrier Coatings on Si-based Ceramics solves this key issue.
BSAS(BaxSr1-xAl2Si2O8,0<x<1) there is good high temperature resistance water oxygen corrosive nature and and SiC ceramic matrix composite material Heat expansion matching, turn into one of important selection of Environmental Barrier Coatings on Si-based Ceramics material.NASA prepares BSAS environment using plasma spray coating process Barrier coating has already been through test run examination, and the service life of SiC ceramic matrix composite material can be extended as many as three times by the application of the coating. The fresh understatement road of preparation technology of BSAS spraying powders, domestic market can not be directly commercially available, and coating prepares and first has to solve The preparation of high-quality spraying powder.
Plasma spray coating process is current most popular coating production, and its principle is in height by spraying powder Melt and accelerate under the flame stream effect of warm high speed, sprawl, solidify and be stacked into the process of sheet coating after being hit with matrix.Hole Gap and crackle are the faults of construction of Environmental Barrier Coatings on Si-based Ceramics, the failure of meeting acceleration environment barrier coating, in order to reduce coating porosity, it is desirable to Spraying powder has good mobility and heat conductivility.Atomizing granulating technology is to prepare the most frequently used work of plasma spraying powder Skill, spraying powder prepared by this technique is loose hollow microsphere, and the powder fluidity of this shape is relatively good, but is transmitted During heat conduction it is not abundant enough, the Environmental Barrier Coatings on Si-based Ceramics of preparation than it is more loose, hole is more, this is greatly lowered the protection of coating Performance.
The content of the invention
The purpose of the present invention is：In order to solve environment barrier prepared by the BSAS spraying powders of traditional spray prilling preparation The problem of coating porosity is higher, propose a kind of Ba used for plasma sprayingxSr1-xAl2Si2O8Raw powder's production technology.
The technical solution of the present invention is selection synthesis BaxSr1-xAl2Si2O8The compound of powder is Ba, Sr carbon Hydrochlorate or oxalates, Al, Si oxide as raw material, wherein, 0<x<1, raw material are proportionally weighed, melting is helped Agent, dispersant, deionized water and abrading-ball are placed in ball grinder, are mixed evenly using ball-grinding machine, are dried after discharging, dried Powder, which is placed in high temperature melting furnace, carries out melting, and the fragment material of glassy state is obtained after quenching, fragment material mechanical is crushed, is sieved Obtain being directly used in the Ba of plasma spraying after pointxSr1-xAl2Si2O8Powder, specific preparation process are as follows：
(1) dispensing：According to Ba:Sr:Al:Si=x:(1-x):2:2 elemental mole ratios weigh Ba, Sr, Al, Si chemical combination Powder, by powder volume content 40%-60% add deionized water, by powder quality 0.5%-1.2% add MgO or CaO auxiliary agents, ammonium polyacrylate dispersant is added by the 0.5%-1.0% of powder quality；
(2) batch mixing：Above-claimed cpd powder, deionized water, auxiliary agent and dispersant are put into ball mill, by ball material quality Compare 1-4:1 addition abrading-ball carries out being sufficiently mixed ball milling, Ball-milling Time 5-30h, obtains ceramic slurry；
(3) dry：It is placed in after the good slurry of ball milling is taken out in 100-140 DEG C of air dry oven, insulation 5-20h to moisture Volatilization completely；
(4) melting：Dried powder is placed in high temperature melting furnace and carries out high melt, obtains melten glass state BaxSr1-xAl2Si2O8, 1600-1800 DEG C of smelting temperature, smelting time 1-5h；
(5) it is quenched：Melten glass state is poured into cold water to be quenched, obtains chunky shape BaxSr1-xAl2Si2O8；
(6) crush：By chunky shape BaxSr1-xAl2Si2O8It is 50-100 μm to carry out mechanical crushing to median grain diameter；
(7) sieve：The powder that above-mentioned steps are obtained sieves, and takes Ba of the particle size range at 30-80 μmxSr1-xAl2Si2O8 Powder granule is standby as spraying.
(8) if crushing, granularity still greater than 80 μm, repeats (6)-(7) step, until particle size range is in 30-80 μ after sieving m。
When selecting Ba, Sr, Al, Si compound powder raw material, selection Ba, Sr carbonate or oxalates, and Al, Si oxide.
Smelting technology temperature is 1700 DEG C, is BaO, SrO, Al2O3、SiO2The eutectic point of mixed oxide, smelting time 2- 3h。
The melting auxiliary agent of selection is MgO, and dosage must not be more than the 1.0% of powder quality.
Advantages of the present invention and feature：
(1) raw material sources of the present invention are convenient, and cost is low, easy to operate, and environmental pollution is small；
(2) BSAS spraying powders are prepared compared to traditional atomizing granulating technology, process of the present invention is simple, and process cycle is short；
(3) BSAS powders prepared by the present invention have the characteristics of fine and close, block, multi-angular, in plasma spray coating process mistake Faster, melting is abundant for heat conduction in journey, and deposition efficiency is high；
(4) the BSAS powders that prepare of the present invention can obtain that porosity is lower, is combined with matrix by plasma spray coating process More close Environmental Barrier Coatings on Si-based Ceramics, while this design feature also substantially increases the high temperature resistant, anti-oxidant, anticorrosive etc. anti-of coating Protect performance.
The present invention selection Ba, Sr carbonate or oxalates, Al, Si oxide are as raw material, MgO or CaO conducts Auxiliary agent is melted, deionized water is as decentralized medium, and ammonium acrylate is as dispersant, using ball-grinding machine by above-mentioned material according to institute Need ratio to be mixed evenly, be placed in after discharging in air dry oven to being completely dried, dried powder is placed in high temperature melting furnace High melt is carried out, the chunky shape material of glassy state is obtained after quenching, the material mechanical is crushed to certain particle size, after screening To the BSAS powders that can be directly used for spraying.This technical process is fairly simple, and the BSAS powders of preparation are with fine and close, block, more The characteristics of corner angle, faster, melting is abundant, can be sunk by plasma spray coating process for heat conduction during plasma spray coating process Product is more efficient, porosity is lower, more close Environmental Barrier Coatings on Si-based Ceramics is combined with matrix, while this design feature also greatly improves The barrier propterty such as the high temperature resistant of coating, anti-oxidant, anticorrosive.
Brief description of the drawings
BSAS spraying powders prepared by Fig. 1 prior arts spray granulation；
Fig. 2 is BSAS powders prepared by present invention melting crush method；
Environmental Barrier Coatings on Si-based Ceramics prepared by Fig. 3 prior arts spray granulation BSAS powders used for plasma spraying；
Fig. 4 is Environmental Barrier Coatings on Si-based Ceramics prepared by present invention melting crush method BSAS powders used for plasma spraying.
Embodiment
Selection does not produce or seldom produced Ba, Sr of pernicious gas carbonate or oxalates, Al, Si oxide powder As raw material powder, proportionally weigh above-mentioned material, melting auxiliary agent, dispersant, deionized water and abrading-ball and be placed in ball grinder It is interior, it is mixed evenly using ball-grinding machine, is dried after discharging, dried powder, which is placed in high temperature melting furnace, carries out melting, quenching The fragment material of glassy state is obtained afterwards, the material mechanical is crushed to certain particle size, obtains can be directly used for spraying after screening BSAS powders.Specific preparation method is as follows：
(1) dispensing：According to Ba:Sr:Al:Si=x:(1-x):2:2 elemental mole ratios weigh Ba, Sr, Al, Si chemical combination Powder, by powder volume content 40%-60% add deionized water, by powder quality 0.5%-1.2% add MgO or CaO auxiliary agents, ammonium polyacrylate dispersant is added by the 0.5%-1.0% of powder quality；
(2) batch mixing：Above-claimed cpd powder, deionized water, auxiliary agent and dispersant are put into ball mill, by ball material quality Compare 1-4:1 addition abrading-ball carries out being sufficiently mixed ball milling, Ball-milling Time 5-30h, is uniformly dispersed, suspension is good, viscosity Moderate ceramic slurry；
(3) dry：It is placed in after the good slurry of ball milling is taken out in 100-140 DEG C of air dry oven, insulation 5-20h to moisture Volatilization completely；
(4) melting：Dried powder is placed in high temperature melting furnace and carries out high melt, obtains melten glass state BaxSr1-xAl2Si2O8, 1600-1800 DEG C of smelting temperature, smelting time 1-5h；
(5) it is quenched：Molten product is poured into cold water to be quenched, obtained because volume acutely shrinks the fragment for causing to ftracture Shape BSAS；
(6) crush：It it is 50-100 μm by the further mechanical crushing of BSAS fragments to median grain diameter；
(7) sieve：The powder sieving that above-mentioned steps obtain, takes BSAS powder granule conduct of the particle size range at 30-80 μm Spray standby.
(8) if crushing, granularity still greater than 80 μm, repeats (6)-(7) step, until particle size range is in 30-80 μ after sieving M, to improve yield.
In order to be better understood from the present invention, present disclosure, but this is expanded on further with reference to specific embodiment The content of invention is not limited solely to the following examples：
Embodiment 1
(1) dispensing：Barium carbonate 493.4g, strontium carbonate 369g, aluminum oxide 510g, silica 600g are weighed, 300ml is added and goes Ionized water, 15gMgO auxiliary agents, 20g ammonium acrylate dispersants；
(2) batch mixing：Above-mentioned material is put into ball mill, 4Kg aluminum oxide abrading-balls is added and is sufficiently mixed ball milling 20h, obtain It is uniformly dispersed, suspension is good, the ceramic slurry of modest viscosity；
(3) dry：The good slurry of ball milling is placed in into 120 DEG C of air dry oven inside holding 10h after discharging to wave completely to moisture Hair；
(4) melting：Dried powder is placed in high temperature melting furnace and carries out high melt, obtains melten glass state Ba0.5Sr0.5Al2Si2O8, 1700 DEG C of smelting temperature, smelting time 3h；
(5) it is quenched：Molten product is poured into cold water to be quenched, obtained because volume acutely shrinks the fragment for causing to ftracture Shape Ba0.5Sr0.5Al2Si2O8；
(6) crush：By Ba0.5Sr0.5Al2Si2O8The further mechanical crushing of fragment to median grain diameter is 50-100 μm；
(7) sieve：The powder that above-mentioned steps are obtained sieves, and takes Ba of the particle size range at 30-80 μm0.5Sr0.5Al2Si2O8 Powder granule is standby as spraying.
(8) if crushing, granularity still greater than 80 μm, repeats (6)-(7) step, until particle size range is in 30-80 μ after sieving m。
Embodiment 2
(1) dispensing：Barium oxalate 1690g, strontium carbonate 369g, aluminum oxide 1020g, silica 1200g are weighed, adds 500ml Deionized water, 30gMgO auxiliary agents, 30g ammonium acrylate dispersants；
(2) batch mixing：Above-mentioned material is put into ball mill, 15Kg aluminum oxide abrading-balls is added and is sufficiently mixed ball milling 30h, obtain It is uniformly dispersed, suspension is good, the ceramic slurry of modest viscosity；
(3) dry：The good slurry of ball milling is placed in into 120 DEG C of air dry oven inside holding 20h after discharging to wave completely to moisture Hair；
(4) melting：Dried powder is placed in high temperature melting furnace and carries out high melt, obtains melten glass state Ba0.75Sr0.25Al2Si2O8, 1700 DEG C of smelting temperature, smelting time 5h；
(5) it is quenched：Molten product is poured into cold water to be quenched, obtained because volume acutely shrinks the fragment for causing to ftracture Shape Ba0.75Sr0.25Al2Si2O8；
(6) crush：By Ba0.75Sr0.25Al2Si2O8The further mechanical crushing of fragment to median grain diameter is 50-100 μm；
(7) sieve：The powder that above-mentioned steps are obtained sieves, and takes particle size range at 30-80 μm Ba0.75Sr0.25Al2Si2O8Powder granule is standby as spraying.
(8) if crushing, granularity still greater than 80 μm, repeats (6)-(7) step, until particle size range is in 30-80 μ after sieving m。

Claims (4)

  1. A kind of 1. Ba used for plasma sprayingxSr1-xAl2Si2O8Raw powder's production technology, it is characterised in that selection synthesis BaxSr1- xAl2Si2O8The compound of powder is Ba, Sr carbonate or oxalates, Al, Si oxide as raw material, wherein, 0<x< 1, raw material are proportionally weighed, melting auxiliary agent, dispersant, deionized water and abrading-ball are placed in ball grinder, set using ball milling It is standby to be mixed evenly, dried after discharging, dried powder, which is placed in high temperature melting furnace, carries out melting, and glassy state is obtained after quenching Fragment material, fragment material mechanical is crushed, obtain being directly used in the Ba of plasma spraying after screeningxSr1-xAl2Si2O8Powder Body, specific preparation process are as follows：
    (1) dispensing：According to Ba:Sr:Al:Si=x:(1-x):2:2 elemental mole ratios weigh Ba, Sr, Al, Si compound powder Body, deionized water is added by powder volume content 40%-60%, adding MgO or CaO by the 0.5%-1.2% of powder quality helps Agent, ammonium polyacrylate dispersant is added by the 0.5%-1.0% of powder quality；
    (2) batch mixing：Above-claimed cpd powder, deionized water, auxiliary agent and dispersant are put into ball mill, by ball material mass ratio 1- 4:1 addition abrading-ball carries out being sufficiently mixed ball milling, Ball-milling Time 5-30h, obtains ceramic slurry；
    (3) dry：It is placed in after the good slurry of ball milling is taken out in 100-140 DEG C of air dry oven, insulation 5-20h is complete to moisture Volatilization；
    (4) melting：Dried powder is placed in high temperature melting furnace and carries out high melt, obtains melten glass state BaxSr1- xAl2Si2O8, 1600-1800 DEG C of smelting temperature, smelting time 1-5h；
    (5) it is quenched：Melten glass state is poured into cold water to be quenched, obtains chunky shape BaxSr1-xAl2Si2O8；
    (6) crush：By chunky shape BaxSr1-xAl2Si2O8It is 50-100 μm to carry out mechanical crushing to median grain diameter；
    (7) sieve：The powder that above-mentioned steps are obtained sieves, and takes Ba of the particle size range at 30-80 μmxSr1-xAl2Si2O8Powder Grain is standby as spraying.
    (8) if crushing, granularity still greater than 80 μm, repeats (6)-(7) step, until particle size range is at 30-80 μm after sieving.
  2. A kind of 2. Ba used for plasma spraying according to claim 1xSr1-xAl2Si2O8Raw powder's production technology, its feature exist In, when selecting Ba, Sr, Al, Si compound powder raw material, selection Ba, Sr carbonate or oxalates, and Al, Si Oxide.
  3. A kind of 3. Ba used for plasma spraying according to claim 1xSr1-xAl2Si2O8Raw powder's production technology, its feature exist In smelting technology temperature is 1700 DEG C, is BaO, SrO, Al2O3、SiO2The eutectic point of mixed oxide, smelting time 2-3h.
  4. A kind of 4. Ba used for plasma spraying according to claim 1xSr1-xAl2Si2O8Raw powder's production technology, its feature exist In the melting auxiliary agent of selection is MgO, and dosage must not be more than the 1.0% of powder quality.
CN201710941828.0A 2017-10-11 2017-10-11 A kind of Ba used for plasma sprayingxSr1‑xAl2Si2O8Raw powder's production technology Pending CN107746267A (en)

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CN112225569A (en) * 2020-10-16 2021-01-15 中国航发北京航空材料研究院 BSAS powder solid-phase synthesis method for environmental barrier coating
CN112521150A (en) * 2020-11-02 2021-03-19 广西科技大学 Preparation method of perovskite-like structure ceramic coating
CN113800910A (en) * 2021-09-24 2021-12-17 太原理工大学 Preparation method of composite perovskite type spherical powder for spraying
CN115180806A (en) * 2022-08-03 2022-10-14 南京高新经纬电气有限公司 Glass state material manufacturing process

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CN112225569A (en) * 2020-10-16 2021-01-15 中国航发北京航空材料研究院 BSAS powder solid-phase synthesis method for environmental barrier coating
CN112521150A (en) * 2020-11-02 2021-03-19 广西科技大学 Preparation method of perovskite-like structure ceramic coating
CN113800910A (en) * 2021-09-24 2021-12-17 太原理工大学 Preparation method of composite perovskite type spherical powder for spraying
CN115180806A (en) * 2022-08-03 2022-10-14 南京高新经纬电气有限公司 Glass state material manufacturing process

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