CN108754399A - A kind of titanium diboride coating and preparation method thereof of high temperature resistant fluorination fused salt corrosion - Google Patents

A kind of titanium diboride coating and preparation method thereof of high temperature resistant fluorination fused salt corrosion Download PDF

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CN108754399A
CN108754399A CN201810645798.3A CN201810645798A CN108754399A CN 108754399 A CN108754399 A CN 108754399A CN 201810645798 A CN201810645798 A CN 201810645798A CN 108754399 A CN108754399 A CN 108754399A
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powder
preparation
titanium
tib
coating
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CN108754399B (en
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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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)

Abstract

The present invention discloses a kind of titanium diboride composite ceramic coating and preparation method thereof of high temperature resistant fluorination fused salt corrosion.The present invention is the TiB for being 3~5 μm in average grain diameter by powder combined processing2Particle surface uniformly assembles the rutile TiO of one layer of 200~500nm thickness2, the TiO2Layer preferentially melts in Plasma Spraying Process Using, and barrier air is to TiB2The oxidation of particle, after depositing to matrix, the TiO that preferentially melts2It is filled into TiB2In the gap of particle flattening accumulation, coating porosity can be reduced, the titanium diboride composite ceramic coating composition that the present invention is obtained is uniform, compact structure, and high temperature resistant is fluorinated fused salt corrosion.

Description

A kind of titanium diboride coating and preparation method thereof of high temperature resistant fluorination fused salt corrosion
Technical field
The present invention relates to the titanium diboride coatings and preparation method thereof that a kind of high temperature resistant is fluorinated fused salt corrosion, belong to material neck Domain.
Background technology
Two iron boride (TiB2) be hexagonal crystal system C32 type structures metalloid compound, the structural parameters of perfect crystal ForIn entire crystal structure, boron atom face and titanium atom face are alternately present composition two-dimensional mesh Shape structure, titanium atom layer is tightly packed, and boron atom is the center of hexa-coordinate and the triangular prism positioned at titanium atom.Wherein B-Outer layer There are four electronics, each B-With the other three B-It is combined with covalent bond, extra one electronically forms space delocalization large Π bond.
TiB2With the satisfactory electrical conductivity (10 that can be compared with metal-5Ω m), the stronger melt of resistance to fluoride salt corrosive nature And excellent wearability, it is widely used in the surfacecti proteon of material in harsh environment all the time.Prepare TiB2The side of coating Method includes chemical vapor deposition, electrode deposition, plasma spraying.Under relatively, plasma spraying uses non-transferred plasma arc As heat source, there is very high energy density and temperature.Plasma spraying is with deposition velocity is fast, production efficiency is high, coating The features such as uniformity is good, applied widely.
But TiB prepared by plasma spraying2There are some critical issues for ceramic coating.On the one hand, in spraying process TiB2The oxidizable decomposition of ceramics, the melting product (B generated2O3, fusing point is 450 DEG C) and it can largely volatilize at 1000 DEG C or more, it causes Keep coating composition uneven, structural behaviour declines.On the other hand, ceramic particle is formed in accumulation in coating procedure, unavoidably Ground generates more crackle, and coating porosity is higher, thus its corrosion resistance can not ensure.
In consideration of it, application No. is the patent of invention of CN201610521817.2, " one kind preparing boronation coating in metal surface Process " disclose a kind of preparation boronation coating for combining plasma spraying and laser remolten and handling two kinds of technological merits Process.It is handled, is obtained with matrix in metallurgical binding, fine and close coating using subsequent laser remolten.But the patent is not It is related to spraying powder TiB2Oxygenolysis problem.Application No. is the patent of invention of CN201610617312.6 " titanium alloy and titaniums The preparation method of Al intermetallic surface boronation ti-based coating " is using heat spraying method direct spraying by blasting treatment Titanium alloy or Intermatallic Ti-Al compound workpiece surface, to form boronation ti-based coating.The invention is intended to simplify prior art The problems such as complicated, cost obviously increases, is not directed to spraying powder TiB2Oxygenolysis and the problems such as poor coating compactness.
Invention content
The present invention is directed to the deficiency illustrated in background above technology, proposes that a kind of high temperature resistant that is directed to is fluorinated fused salt corrosion The reasonable efficient preparation method of titanium diboride composite ceramic coating：The TiB for being 3~5 μm in average grain diameter2Particle surface is uniform Assemble one layer of 200~500nm rutile TiO2, then reunite, then spray-on coating.On the one hand, the TiO2Layer is in atmospheric plasma It is preferentially melted in spraying process, barrier air is to TiB2The oxidation of particle；On the other hand, it after depositing to matrix, preferentially melts TiO2It is filled into TiB2In the gap of particle flattening accumulation, porosity is reduced, the thermal shock resistance of coating, compactness and resistance to height are promoted Temperature molten salt corrosive nature.
The present invention is achieved by the following technical solutions：A kind of titanium diboride composite ceramic of high temperature resistant fluorination fused salt corrosion Porcelain coating, the coating material by 95~99% mass TiB2, the TiO of 1~5% mass2Composition, the coating is resistant to not surpass Cross the corrosion of the fluorination fused salt of 1000 DEG C of degree.
A kind of preparation method of the titanium diboride composite ceramic coating of high temperature resistant melt salt corrosion, this method step packet It includes：
The first step, the combined processing of raw material powder；
(1) by pretreated TiB2Powder, Titanium alkoxides are added with inhibitor in alcoholic solution, ultrasonic disperse 1h or more, configuration The dispersion liquid for being 0.2~15% at mass percent；(2) deionized water of 0.2~0.4 molar ratio Titanium alkoxides is slowly added to point Dispersion liquid adjusts pH to 2~3, while controlling reaction temperature is 25~30 DEG C and is vigorously stirred, and is aged 48~72h after completion of the reaction； (3) reactant of previous step is washed into separation with absolute ethyl alcohol, then 80 DEG C of dry 2h are forged at a temperature of 300~500 DEG C again It burns 0.5~2 hour, obtains required powder.
Second step, the agglomeration granulation of powder；
(2) powder that previous step obtains is scattered in deionized water, sequentially adds dispersant and binder, mechanical ball mill Dispersion 4~8 hours, is configured to stable slurry, then by high speed centrifugation mist projection granulating, obtains reunion powder；
Third walks, the preparation of titanium diboride composite ceramic coating；
(3) matrix is decontaminated and is cleaned, surface sand-blasting roughening, using the reunion powder in second step as feeding, using air etc. Plasma-spray technique, in matrix surface spray-on coating.
The pretreatment TiB2Powder is through persalt, sulfuric acid, nitric acid, lauric acid, oleic acid, cetyl trimethyl bromine The surface activation process for changing the mixtures of the one or more of ammonium, calgon, sodium tripolyphosphate, after surface treatment, TiB2 The average particle size of powder is 3~5 μm, and surface potential is 30~60mV.
The Titanium alkoxides be titanium tert butoxide, titanium isopropoxide, titanium n-butanol salt, titanium normal propyl alcohol salt, butyl titanate, One or more of mixtures of isopropyl titanate, tetraisopropyl titanate.
The inhibitor is one or more of mixtures of glacial acetic acid, acetylacetone,2,4-pentanedione, acetic acid, hydrochloric acid, inhibitor with The molar ratio of titanate is 0.5~1.5.
TiB after the combined processing2Powder particle surface uniformly assembles one layer of fine and close rutile TiO2, thickness is 200~500nm.
The reunion powder is loosely organized, and grain size is 15~40 μm.
The parameter of the prepares coating is：Plasma spraying net power is 30~60kW, and argon gas is 20 in plasma gas ~60slpm, hydrogen are 10~30slpm, powder feeding 2~5L/min of load volume, 100~150mm of spray distance.
Beneficial effects of the present invention
Coating prepared by the present invention can effectively reduce porosity, promote the thermal shock resistance of coating, compactness and high temperature resistant Fused salt corrosion performance.
Description of the drawings
The SEM back ofs the body for the titanium diboride composite ceramic coating section that Fig. 1 embodiments 1 spray dissipate pattern photo：(1) 316l is stainless Steel matrix；(2)TiB2Composite ceramic coat.
Fig. 2 comparative examples 1 are fluorinated the SEM secondary electron photos of titanium diboride composite ceramic coating section after fused salt corrosion：(1) Graphite matrix；(2)TiB2Composite ceramic coat；(3) it is fluorinated fused salt.
Specific implementation mode
Embodiment 1
The first step, the combined processing of raw material powder；
(1) take 200g through the TiB of calgon activation process2Powder, 200mL butyl titanates and glacial acetic acid (metatitanic acid The molar ratio of butyl ester and glacial acetic acid is 1:1) it is added in 1000mL ethanol solutions, ultrasonic disperse 1h or more；(2) by deionization Water (0.2 molar ratio butyl titanate) be slowly added to dispersion liquid, salt acid for adjusting pH to 2.5, while controlling reaction temperature be 25 DEG C simultaneously It is vigorously stirred, is aged 48 hours after completion of the reaction；(3) reactant of previous step is washed into separation, 80 DEG C of dryings with absolute ethyl alcohol Then 2h is calcined 2 hours at a temperature of 500 DEG C again, obtain required powder.
Second step, the agglomeration granulation of powder；
(2) powder that previous step obtains is scattered in deionized water, sequentially adds dispersant and binder, mechanical ball mill Dispersion 4 hours, is configured to stable slurry, then by high speed centrifugation mist projection granulating, obtains reunion powder；
Third walks, the preparation of titanium diboride composite ceramic coating；
(3) 316l stainless steel bases are decontaminated and is cleaned, surface sand-blasting roughening, using the reunion powder in second step as feeding, Using atmospheric plasma spraying technology, in matrix surface spray-on coating.Spray parameters used are：Plasma spraying net power is 35kW, argon gas is 45slpm in plasma gas, hydrogen 10slpm, powder feeding load volume 5L/min, spray distance 120mm, institute The heterogeneous microstructure of the composite ceramic coat of preparation is shown in Figure of description 1.
Embodiment 2
The first step, the combined processing of raw material powder；
(1) take 200g through the TiB of lauric acid activation process2Powder, 200mL isopropyl titanates and suitable acetylacetone,2,4-pentanedione (molar ratio of butyl titanate and glacial acetic acid is 1:1) it is added in 1000mL ethanol solutions, ultrasonic disperse 1h or more；(2) will Deionized water (0.3 molar ratio isopropyl titanate) is slowly added to dispersion liquid, salt acid for adjusting pH to 2.5, while controlling reaction temperature It for 25 DEG C and is vigorously stirred, is aged 48 hours after completion of the reaction；(3) reactant of previous step is washed into separation with absolute ethyl alcohol, 80 DEG C of dry 2h, are then calcined 2 hours at a temperature of 450 DEG C again, obtain required powder.
Second step, the agglomeration granulation of powder；
The powder that previous step obtains is scattered in deionized water, dispersant and binder, mechanical ball mill point are sequentially added It dissipates 4 hours, is configured to stable slurry, then by high speed centrifugation mist projection granulating, obtain reunion powder；
Third walks, the preparation of titanium diboride composite ceramic coating；
316l stainless steel bases are decontaminated and are cleaned, surface sand-blasting roughening is used using the reunion powder in second step as feeding Atmospheric plasma spraying technology, in matrix surface spray-on coating.Spray parameters used are：Plasma spraying net power is 35kW, argon gas is 45slpm, hydrogen 10slpm, powder feeding load volume 5L/min, spray distance 120mm in plasma gas.
Embodiment 3
The first step, the combined processing of raw material powder；
(1) take 200g through the TiB of cetyl trimethylammonium bromide activation process2Powder, 200mL butyl titanates and ice vinegar (molar ratio of butyl titanate and glacial acetic acid is 1 to acid:1) it is added in 1000mL ethanol solutions, ultrasonic disperse 1h or more；(2) Deionized water (0.2 molar ratio butyl titanate) is slowly added to dispersion liquid, salt acid for adjusting pH to 2.5, while controlling reaction temperature It for 25 DEG C and is vigorously stirred, is aged 48 hours after completion of the reaction；(3) reactant of previous step is washed into separation with absolute ethyl alcohol, 80 DEG C of dry 2h, are then calcined 2 hours at a temperature of 500 DEG C again, obtain required powder.
Second step, the agglomeration granulation of powder；
The powder that previous step obtains is scattered in deionized water, dispersant and binder, mechanical ball mill point are sequentially added It dissipates 4 hours, is configured to stable slurry, then by high speed centrifugation mist projection granulating, obtain reunion powder；
Third walks, the preparation of titanium diboride composite ceramic coating；
Graphite matrix is decontaminated and is cleaned, surface sand-blasting roughening, using the reunion powder in second step as feeding, using air etc. Plasma-spray technique, in matrix surface spray-on coating.Spray parameters used are：Plasma spraying net power be 35kW, wait from Argon gas is 45slpm, hydrogen 10slpm, powder feeding load volume 5L/min, spray distance 120mm in sub- gas.
Embodiment 4
The first step, the combined processing of raw material powder；
(1) TiB for taking 200g to be handled through nitric acid and cetyl trimethylammonium bromide admixture activation2Powder, 200mL metatitanic acids (molar ratio of butyl titanate and glacial acetic acid is 1 to butyl ester with glacial acetic acid:1) it is added in 1000mL ethanol solutions, ultrasonic disperse 1h or more；(2) deionized water (0.2 molar ratio butyl titanate) is slowly added to dispersion liquid, salt acid for adjusting pH to 2.5, same to time control Reaction temperature processed is 25 DEG C and is vigorously stirred, and is aged 48 hours after completion of the reaction；(3) with absolute ethyl alcohol by the reactant of previous step Then washing separation, 80 DEG C of dry 2h are calcined 2 hours at a temperature of 500 DEG C again, obtain required powder.
Second step, the agglomeration granulation of powder；
The powder that previous step obtains is scattered in deionized water, dispersant and binder, mechanical ball mill point are sequentially added It dissipates 4 hours, is configured to stable slurry, then by high speed centrifugation mist projection granulating, obtain reunion powder；
Third walks, the preparation of titanium diboride composite ceramic coating；
316l stainless steel bases are decontaminated and are cleaned, surface sand-blasting roughening is used using the reunion powder in second step as feeding Atmospheric plasma spraying technology, in matrix surface spray-on coating.Spray parameters used are：Plasma spraying net power is 35kW, argon gas is 45slpm, hydrogen 10slpm, powder feeding load volume 5L/min, spray distance 120mm in plasma gas.
Painting prepared by example 3 is placed on fluorination fused salt, the mass fraction of fused salt is：Na3AlF6, 90%；CaF2, 5%, temperature of molten salt is 970 DEG C, and etching time is 8 hours；After corrosion experiment, sample is cooled to room temperature and is taken out, edge Corrosion position incision is analyzed.See shown in Figure of description 2, after fused salt corrosion, coating is combined intact with graphite matrix, is not produced Raw stripping or other defect.Coating cross sections are observed, coating still remains intact, and does not crack or generate fine cracks.
It should be pointed out that the above embodiment can make those skilled in the art be more completely understood the present invention, but not with Any mode limits the present invention.Therefore, although this specification is to present invention has been detailed description, art technology Personnel should be appreciated that and still can modify or equivalently replace the present invention；And all do not depart from the skill of essence of the invention Art scheme and its improvement should all be covered in the protection domain of patent of the present invention.

Claims (8)

1. a kind of titanium diboride composite ceramic coating of high temperature resistant fluorination fused salt corrosion, it is characterised in that：The coating material is by 95 The TiB of~99% mass fraction2, the TiO of 1~5% mass fraction2Composition, the coating is resistant to the fluorination no more than 1000 DEG C The corrosion of fused salt.
2. a kind of preparation method of the titanium diboride composite ceramic coating of high temperature resistant melt salt corrosion, it is characterised in that：By following several A step composition：
The first step, the combined processing of raw material powder；
(1) by pretreated TiB2Powder, Titanium alkoxides are added with inhibitor in ethanol solution, ultrasonic disperse 1h or more, configuration The dispersion liquid for being 0.2~15% at mass percent；(2) deionized water of 0.2~0.4 molar ratio Titanium alkoxides is slowly added to point Dispersion liquid adjusts pH to 2~3, while controlling reaction temperature is 25~30 DEG C and is vigorously stirred, and is aged 48~72h after completion of the reaction； (3) reactant of previous step is washed into separation with absolute ethyl alcohol, then 80 DEG C of dry 2h are forged at a temperature of 300~500 DEG C again It burns 0.5~2 hour, obtains required powder；
Second step, the agglomeration granulation of powder；
(2) powder that previous step obtains is scattered in deionized water, sequentially adds dispersant and binder, mechanical ball mill dispersion 4~8 hours, it is configured to stable slurry, then by high speed centrifugation mist projection granulating, obtains reunion powder；
Third walks, the preparation of titanium diboride composite ceramic coating；
(3) matrix is decontaminated and is cleaned, surface sand-blasting roughening, using the reunion powder in second step as feeding, using atmospheric plasma Spraying technology, in matrix surface spray-on coating.
3. preparation method as claimed in claim 2, it is characterised in that：Pretreatment TiB in the first step in (1)2Powder For：Through persalt, sulfuric acid, nitric acid, lauric acid, oleic acid, cetyl trimethylammonium bromide, calgon, sodium tripolyphosphate One or more of mixtures surface activation process, after surface treatment, control TiB2The average particle size of powder is 3~5 μm, Surface potential is 30~60mV.
4. preparation method as claimed in claim 2, it is characterised in that：Titanium alkoxides in the first step in (1) are the tertiary fourths of titanium The one of alkoxide, titanium isopropoxide, titanium n-butanol salt, titanium normal propyl alcohol salt, butyl titanate, isopropyl titanate, tetraisopropyl titanate Kind or several mixtures.
5. preparation method as claimed in claim 2, it is characterised in that：The inhibitor is glacial acetic acid, acetylacetone,2,4-pentanedione, second The molar ratio of one or more of mixtures of acid, hydrochloric acid, inhibitor and Titanium alkoxides is 0.5~1.5.
6. preparation method as claimed in claim 2, it is characterised in that：TiB after the combined processing2Powder particle surface is equal One layer of fine and close rutile TiO of even assembling2, thickness is 200~500nm.
7. preparation method as claimed in claim 2, it is characterised in that：The reunion powder is loosely organized, grain size be 15~ 40μm。
8. preparation method as claimed in claim 2, it is characterised in that：The parameter of the prepares coating is：Plasma spraying is net Power is 30~60kW, and argon gas is 20~60slpm in plasma gas, and hydrogen is 10~30slpm, 2~5L/ of powder feeding load volume Min, 100~150mm of spray distance.
CN201810645798.3A 2018-06-21 2018-06-21 Titanium diboride coating resistant to high-temperature fluoride molten salt corrosion and preparation method thereof Active CN108754399B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115283666A (en) * 2022-06-23 2022-11-04 江苏岐铭新材料科技发展有限公司 Aluminum alloy powder spheroidizing process

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KR20030054077A (en) * 2001-12-24 2003-07-02 서울대학교 공과대학 교육연구재단 Method to coat ceramic powder with TiO2 and Method to improve wettability of B4C-Al composite material
CN104630769A (en) * 2015-01-28 2015-05-20 辽宁工程技术大学 Active argon arc cladding Ni-based aluminum oxide-titanium diboride compound coating of coal ash and preparation method
CN105695917A (en) * 2016-03-24 2016-06-22 中国科学院上海硅酸盐研究所 High-temperature and ablation resistance TiB2-MoSi2 composite coating and preparation method thereof
CN105734555A (en) * 2016-02-17 2016-07-06 柳州职业技术学院 Surface coating for AZ91 alloy for automobile engine

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Publication number Priority date Publication date Assignee Title
KR20030054077A (en) * 2001-12-24 2003-07-02 서울대학교 공과대학 교육연구재단 Method to coat ceramic powder with TiO2 and Method to improve wettability of B4C-Al composite material
CN104630769A (en) * 2015-01-28 2015-05-20 辽宁工程技术大学 Active argon arc cladding Ni-based aluminum oxide-titanium diboride compound coating of coal ash and preparation method
CN105734555A (en) * 2016-02-17 2016-07-06 柳州职业技术学院 Surface coating for AZ91 alloy for automobile engine
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115283666A (en) * 2022-06-23 2022-11-04 江苏岐铭新材料科技发展有限公司 Aluminum alloy powder spheroidizing process

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