CN108754399B - Titanium diboride coating resistant to high-temperature fluoride molten salt corrosion and preparation method thereof - Google Patents

Titanium diboride coating resistant to high-temperature fluoride molten salt corrosion and preparation method thereof Download PDF

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CN108754399B
CN108754399B CN201810645798.3A CN201810645798A CN108754399B CN 108754399 B CN108754399 B CN 108754399B CN 201810645798 A CN201810645798 A CN 201810645798A CN 108754399 B CN108754399 B CN 108754399B
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段晓华
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Jiangxi Science and Technology Normal University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C4/134—Plasma spraying
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof

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Abstract

The invention discloses a titanium diboride composite ceramic coating resistant to high temperature fluorination molten salt corrosion and a preparation method thereof, belonging to the field of materials. Hair brushThe method is to compound TiB with the average grain diameter of 3-5 mu m by powder2A layer of rutile TiO with the thickness of 200-500 nm is uniformly assembled on the surface of the particles2The TiO being2The layer melts preferentially in the plasma spraying process and blocks air from the TiB2Oxidation of particles, TiO preferentially melting after deposition on a substrate2Is filled into TiB2The porosity of the coating can be reduced in gaps formed by flatly accumulating the particles, and the titanium diboride composite ceramic coating obtained by the invention has the advantages of uniform components, compact structure and high temperature resistance to corrosion of fluoridized molten salt.

Description

Titanium diboride coating resistant to high-temperature fluoride molten salt corrosion and preparation method thereof
Technical Field
The invention relates to a titanium diboride coating resistant to high temperature fluorination molten salt corrosion and a preparation method thereof, belonging to the field of materials.
Background
Iron diboride (TiB)2) Is a metalloid compound with a structure of type C32 of the hexagonal system, and the structural parameter of the complete crystal is
Figure BDA0001703473510000011
In the whole crystal structure, the surfaces of boron atoms and the surfaces of titanium atoms alternately appear to form a two-dimensional network structure, the titanium atom layers are closely stacked, and the boron atoms are hexa-coordinated and are positioned at the center of a triangular prism of the titanium atoms. Wherein B is-The outer layer has four electrons, each B-And the other three B-And the surplus electrons form a large pi bond with large spatial delocalization by covalent bond combination.
TiB2Has good conductivity (10) comparable to metal-5Omega · m), strong resistance to fluoride salt melt corrosion and excellent wear resistance, have been widely used for surface protection of materials in harsh environments. Preparation of TiB2The coating method comprises chemical vapor deposition, electrode deposition and plasma spraying. In contrast, plasma spraying uses a non-transferred plasma arc as a heat source, having very high energy density and temperature. The plasma spraying has the characteristics of high deposition speed, high production efficiency, good coating uniformity, wide application range and the like.
However, plasma spray produced TiB2Ceramic coatings present some key problems. On the one hand, TiB in the spraying process2The ceramics are easily oxidized and decomposed to form a molten product (B)2O3The melting point is 450 ℃) and can be volatilized greatly above 1000 ℃, so that the coating components are not uniform, and the structural performance is reduced. On the other hand, ceramic particles inevitably generate more cracks during the deposition of the coating layer, and the porosity of the coating layer is high, so that they areThe corrosion resistance cannot be ensured.
In view of this, the invention patent with application number CN201610521817.2, "a process for preparing boronized coating on metal surface", discloses a process for preparing boronized coating combining two technical advantages of plasma spraying and laser remelting treatment. And adopting subsequent laser remelting treatment to obtain a compact coating which is metallurgically bonded with the substrate. However, this patent does not relate to spraying powder TiB2The problem of oxidative decomposition. The invention patent with application number CN201610617312.6 discloses a method for preparing a titanium boride-based coating on the surface of a titanium alloy and titanium-aluminum intermetallic compound, which adopts a thermal spraying method to directly spray the surface of a titanium alloy or titanium-aluminum intermetallic compound workpiece subjected to sand blasting treatment, thereby forming the titanium boride-based coating. The invention aims to solve the problems of complex process, obvious cost increase and the like in the prior art, and does not relate to spraying powder TiB2The oxidative decomposition of the coating and the poor coating compactness.
Disclosure of Invention
Aiming at the defects explained in the background technology, the invention provides a reasonable and efficient preparation scheme of the titanium diboride composite ceramic coating aiming at high temperature resistant fluoridation molten salt corrosion, which comprises the following steps: TiB having an average particle diameter of 3 to 5 μm2A layer of rutile TiO with the particle size of 200-500 nm is uniformly assembled on the surface of the particle2Then agglomerated and sprayed with a coating. In one aspect, the TiO2The layer melts preferentially in the atmospheric plasma spraying process and blocks air from the TiB2Oxidation of the particles; on the other hand, TiO, which is preferentially melted after deposition on a substrate2Is filled into TiB2In the gaps of the flat accumulation of the particles, the porosity is reduced, and the thermal shock property, the compactness and the high temperature resistance molten salt corrosion property of the coating are improved.
The invention is realized by the following technical scheme: the titanium diboride composite ceramic coating resisting high temperature fluorination molten salt corrosion is prepared from 95-99% of TiB by mass 21 to 5 mass% of TiO2The coating can resist corrosion of the fluoride molten salt with the temperature not more than 1000 ℃.
The preparation method of the titanium diboride composite ceramic coating resisting high molten salt corrosion comprises the following steps:
firstly, compounding raw material powder;
(1) pre-treated TiB2Adding powder, titanium alkoxide and an inhibitor into an alcohol solution, and performing ultrasonic dispersion for more than 1h to prepare a dispersion liquid with the mass percent of 0.2-15%; (2) slowly adding deionized water of titanium alkoxide with the molar ratio of 0.2-0.4 into the dispersion liquid, adjusting the pH to 2-3, controlling the reaction temperature to be 25-30 ℃, violently stirring, and aging for 48-72 hours after the reaction is finished; (3) and washing and separating the reactant in the last step by using absolute ethyl alcohol, drying at 80 ℃ for 2 hours, and then calcining at 300-500 ℃ for 0.5-2 hours to obtain the required powder.
Secondly, agglomerating and granulating the powder;
(2) dispersing the powder obtained in the last step into deionized water, sequentially adding a dispersing agent and a binder, performing mechanical ball milling dispersion for 4-8 hours to prepare stable slurry, and performing high-speed centrifugal spray granulation to obtain agglomerated powder;
thirdly, preparing a titanium diboride composite ceramic coating;
(3) and (3) decontaminating and cleaning the substrate, blasting sand on the surface for coarsening, taking the agglomerated powder in the second step as a feed, and spraying a coating on the surface of the substrate by adopting an atmospheric plasma spraying technology.
The pretreated TiB2The powder is prepared by performing surface activation treatment on one or more of hydrochloric acid, sulfuric acid, nitric acid, lauric acid, oleic acid, cetyl trimethyl ammonium bromide, sodium hexametaphosphate and sodium tripolyphosphate, and performing surface treatment on the surface treated powder to obtain TiB2The average particle size of the powder is 3-5 μm, and the surface potential is 30-60 mV.
The titanium alkoxide is one or a mixture of more of titanium tert-butoxide, titanium isopropoxide, titanium n-butoxide, titanium n-propoxide, tetrabutyl titanate, titanium isopropyl ester and titanium tetraisopropyl ester.
The inhibitor is one or a mixture of more of glacial acetic acid, acetylacetone, acetic acid and hydrochloric acid, and the molar ratio of the inhibitor to the titanate is 0.5-1.5.
The TiB after composite treatment2A layer of compact rutile TiO is uniformly assembled on the surface of the powder particles2The thickness is 200 to 500 nm.
The agglomerated powder has a loose structure and a particle size of 15-40 mu m.
The parameters for preparing the coating are as follows: the net power of plasma spraying is 30-60 kW, argon gas in plasma gas is 20-60 slpm, hydrogen gas is 10-30 slpm, the powder feeding and gas carrying amount is 2-5L/min, and the spraying distance is 100-150 mm.
The invention has the advantages of
The coating prepared by the method can effectively reduce the porosity, and improve the thermal shock property, the compactness and the high temperature resistance molten salt corrosion property of the coating.
Drawings
FIG. 1 SEM back-scattered mode photograph of a cross-section of a sprayed titanium diboride composite ceramic coating of example 1: (1)316l stainless steel substrate; (2) TiB2And (3) composite ceramic coating.
FIG. 2 is an SEM secondary electron photograph of a cross-section of a titanium diboride composite ceramic coating after molten fluoride salt corrosion: (1) a graphite matrix; (2) TiB2A composite ceramic coating; (3) and (3) a molten fluoride salt.
Detailed Description
Example 1
Firstly, compounding raw material powder;
(1) 200g of TiB subjected to sodium hexametaphosphate activation treatment2Adding 200mL of tetrabutyl titanate and glacial acetic acid (the molar ratio of the tetrabutyl titanate to the glacial acetic acid is 1:1) into 1000mL of absolute ethanol solution, and ultrasonically dispersing for more than 1 h; (2) slowly adding deionized water (0.2 molar ratio of butyl titanate) into the dispersion, adjusting the pH value to 2.5 with hydrochloric acid, controlling the reaction temperature to be 25 ℃, violently stirring, and aging for 48 hours after the reaction is finished; (3) washing the reactant in the last step with absolute ethyl alcohol, separating, drying at 80 ℃ for 2h, and then calcining at 500 ℃ for 2h to obtain the required powder.
Secondly, agglomerating and granulating the powder;
(2) dispersing the powder obtained in the last step into deionized water, sequentially adding a dispersing agent and a binder, performing mechanical ball milling and dispersing for 4 hours to prepare stable slurry, and then performing high-speed centrifugal spray granulation to obtain agglomerated powder;
thirdly, preparing a titanium diboride composite ceramic coating;
(3) and (3) decontaminating and cleaning a 316l stainless steel substrate, blasting sand on the surface for coarsening, taking the agglomerated powder in the second step as a feed, and spraying a coating on the surface of the substrate by adopting an atmospheric plasma spraying technology. The spray parameters used were: the net power of plasma spraying is 35kW, the argon in the plasma gas is 45slpm, the hydrogen is 10slpm, the powder feeding and gas carrying amount is 5L/min, the spraying distance is 120mm, and the microstructure of the prepared composite ceramic coating is shown in the attached drawing 1 of the specification.
Example 2
Firstly, compounding raw material powder;
(1) 200g of TiB activated with lauric acid2Adding 200mL of isopropyl titanate and a proper amount of acetylacetone (the molar ratio of butyl titanate to glacial acetic acid is 1:1) into 1000mL of absolute ethanol solution, and ultrasonically dispersing for more than 1 h; (2) slowly adding deionized water (0.3 molar ratio isopropyl titanate) into the dispersion, adjusting the pH value to 2.5 with hydrochloric acid, controlling the reaction temperature to be 25 ℃, violently stirring, and aging for 48 hours after the reaction is finished; (3) washing the reactant in the last step with absolute ethyl alcohol, separating, drying at 80 ℃ for 2h, and then calcining at 450 ℃ for 2h to obtain the required powder.
Secondly, agglomerating and granulating the powder;
dispersing the powder obtained in the last step into deionized water, sequentially adding a dispersing agent and a binder, performing mechanical ball milling and dispersing for 4 hours to prepare stable slurry, and then performing high-speed centrifugal spray granulation to obtain agglomerated powder;
thirdly, preparing a titanium diboride composite ceramic coating;
and (3) decontaminating and cleaning a 316l stainless steel substrate, blasting sand on the surface for coarsening, taking the agglomerated powder in the second step as a feed, and spraying a coating on the surface of the substrate by adopting an atmospheric plasma spraying technology. The spray parameters used were: the net power of plasma spraying is 35kW, the argon gas in the plasma gas is 45slpm, the hydrogen gas is 10slpm, the powder feeding and gas carrying amount is 5L/min, and the spraying distance is 120 mm.
Example 3
Firstly, compounding raw material powder;
(1) 200g of TiB activated by hexadecyl trimethyl ammonium bromide are taken2Adding 200mL of butyl titanate and glacial acetic acid (the molar ratio of the butyl titanate to the glacial acetic acid is 1:1) into 1000mL of absolute ethanol solution, and performing ultrasonic dispersion for more than 1 h; (2) slowly adding deionized water (0.2 molar ratio of butyl titanate) into the dispersion, adjusting the pH value to 2.5 with hydrochloric acid, controlling the reaction temperature to be 25 ℃, violently stirring, and aging for 48 hours after the reaction is finished; (3) washing the reactant in the last step with absolute ethyl alcohol, separating, drying at 80 ℃ for 2h, and then calcining at 500 ℃ for 2h to obtain the required powder.
Secondly, agglomerating and granulating the powder;
dispersing the powder obtained in the last step into deionized water, sequentially adding a dispersing agent and a binder, performing mechanical ball milling and dispersing for 4 hours to prepare stable slurry, and then performing high-speed centrifugal spray granulation to obtain agglomerated powder;
thirdly, preparing a titanium diboride composite ceramic coating;
and (3) decontaminating and cleaning the graphite matrix, blasting sand on the surface for coarsening, taking the agglomerated powder in the second step as a feed, and spraying a coating on the surface of the matrix by adopting an atmospheric plasma spraying technology. The spray parameters used were: the net power of plasma spraying is 35kW, the argon gas in the plasma gas is 45slpm, the hydrogen gas is 10slpm, the powder feeding and gas carrying amount is 5L/min, and the spraying distance is 120 mm.
Example 4
Firstly, compounding raw material powder;
(1) 200g of TiB subjected to mixed activation treatment of nitric acid and hexadecyl trimethyl ammonium bromide are taken2Adding 200mL of butyl titanate and glacial acetic acid (the molar ratio of the butyl titanate to the glacial acetic acid is 1:1) into 1000mL of absolute ethanol solution, and performing ultrasonic dispersion for more than 1 h; (2) slowly adding deionized water (0.2 molar ratio of butyl titanate) into the dispersion, adjusting the pH value to 2.5 with hydrochloric acid, controlling the reaction temperature to be 25 ℃, violently stirring, and aging for 48 hours after the reaction is finished; (3) using absolute ethyl alcohol to make the above-mentioned material undergo the process of one-step reactionThe reaction mass is washed and separated, dried at 80 ℃ for 2h and then calcined at 500 ℃ for 2h to obtain the desired powder.
Secondly, agglomerating and granulating the powder;
dispersing the powder obtained in the last step into deionized water, sequentially adding a dispersing agent and a binder, performing mechanical ball milling and dispersing for 4 hours to prepare stable slurry, and then performing high-speed centrifugal spray granulation to obtain agglomerated powder;
thirdly, preparing a titanium diboride composite ceramic coating;
and (3) decontaminating and cleaning a 316l stainless steel substrate, blasting sand on the surface for coarsening, taking the agglomerated powder in the second step as a feed, and spraying a coating on the surface of the substrate by adopting an atmospheric plasma spraying technology. The spray parameters used were: the net power of plasma spraying is 35kW, the argon gas in the plasma gas is 45slpm, the hydrogen gas is 10slpm, the powder feeding and gas carrying amount is 5L/min, and the spraying distance is 120 mm.
The coating prepared in example 3 is placed in a molten fluoride salt, and the mass fraction of the molten salt is as follows: na (Na)3AlF6，90％；CaF25 percent, the temperature of fused salt is 970 ℃, and the corrosion time is 8 hours; after the corrosion test was completed, the sample was cooled to room temperature and taken out, and cut in the corrosion direction for analysis. As shown in the attached figure 2 of the specification, after molten salt corrosion, the coating is well combined with the graphite substrate, and no peeling or other defects are generated. The coating section is observed, and the coating still remains intact and does not crack or generate fine cracks.
It should be noted that the above-mentioned embodiments can enable those skilled in the art to more fully understand the present invention, but do not limit the present invention in any way. Thus, while the invention has been described in detail in this specification, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all technical solutions and modifications that do not depart from the spirit of the invention are intended to be included within the scope of the invention.

Claims (8)

1. A titanium diboride composite ceramic coating resisting high temperature fluorination molten salt corrosion is characterized in that: the coating material consists of 95 ℃ to99% mass fraction of TiB21-5% by mass of TiO2The coating can resist corrosion of the fluoride molten salt of not more than 1000 ℃.
2. A preparation method of a titanium diboride composite ceramic coating resisting high temperature molten salt corrosion is characterized by comprising the following steps: the method comprises the following steps:
firstly, compounding raw material powder;
(1) pre-treated TiB2Adding the powder, titanium alkoxide and an inhibitor into an absolute ethyl alcohol solution, and ultrasonically dispersing for more than 1h to prepare a dispersion liquid with the mass percent of 0.2-15%; (2) slowly adding deionized water of titanium alkoxide with the molar ratio of 0.2-0.4 into the dispersion liquid, adjusting the pH to 2-3, controlling the reaction temperature to be 25-30 ℃, violently stirring, and aging for 48-72 hours after the reaction is finished; (3) washing and separating the reactant in the last step by absolute ethyl alcohol, drying at 80 ℃ for 2h, and then calcining at 300-500 ℃ for 0.5-2 h to obtain the required powder;
secondly, agglomerating and granulating the powder;
(2) dispersing the powder obtained in the last step into deionized water, sequentially adding a dispersing agent and a binder, performing mechanical ball milling dispersion for 4-8 hours to prepare stable slurry, and performing high-speed centrifugal spray granulation to obtain agglomerated powder;
thirdly, preparing a titanium diboride composite ceramic coating;
(3) and (3) decontaminating and cleaning the substrate, blasting sand on the surface for coarsening, taking the agglomerated powder in the second step as a feed, and spraying a coating on the surface of the substrate by adopting an atmospheric plasma spraying technology.
3. The method of claim 2, wherein: pretreatment of TiB in (1) in the first step2The powder is as follows: activating the surface of one or more of hydrochloric acid, sulfuric acid, nitric acid, lauric acid, oleic acid, cetyl trimethyl ammonium bromide, sodium hexametaphosphate and sodium tripolyphosphate, and controlling TiB after surface treatment2The average particle size of the powder is 3-5 μm, and the surface potential is 30-60 mV.
4. The method of claim 2, wherein: the titanium alkoxide in the first step (1) is one or a mixture of more of titanium tert-butoxide, titanium isopropoxide, titanium n-butoxide, titanium n-propoxide, tetrabutyl titanate, isopropyl titanate and tetraisopropyl titanate.
5. The method of claim 2, wherein: the inhibitor is one or a mixture of more of glacial acetic acid, acetylacetone, acetic acid and hydrochloric acid, and the molar ratio of the inhibitor to the titanium alkoxide is 0.5-1.5.
6. The method of claim 2, wherein: the TiB after composite treatment2A layer of compact rutile TiO is uniformly assembled on the surface of the powder particles2The thickness is 200 to 500 nm.
7. The method of claim 2, wherein: the agglomerated powder has a loose structure and a particle size of 15-40 mu m.
8. The method of claim 2, wherein: the parameters for preparing the coating are as follows: the net power of plasma spraying is 30-60 kW, argon gas in plasma gas is 20-60 slpm, hydrogen gas is 10-30 slpm, the powder feeding and gas carrying amount is 2-5L/min, and the spraying distance is 100-150 mm.
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