CN106048596B - A kind of cold spraying in-situ preparation preparation method of Ti2AlC phase ceramics coating - Google Patents
A kind of cold spraying in-situ preparation preparation method of Ti2AlC phase ceramics coating Download PDFInfo
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- CN106048596B CN106048596B CN201610210730.3A CN201610210730A CN106048596B CN 106048596 B CN106048596 B CN 106048596B CN 201610210730 A CN201610210730 A CN 201610210730A CN 106048596 B CN106048596 B CN 106048596B
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
Abstract
The present invention relates to ceramic coating and Surface Engineering field, specially a kind of Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings.This method can be applied to the MAX phase material systems of energy pressureless sintering synthesis, specifically with a kind of Ti2The preparation method explanation of AlC ceramic coatings.It will be mixed first for being sintered the material powder of prepares coating in required ratio, it is slurry then to add in organic solvent and bonding agent wet ball grinding.Slurry is dried to spherical raw material powder with spray drying granulation method.On the base material of prepares coating, the base material of deposition and coating are sintered under vacuum atmosphere with regard to that can obtain generated in-situ MAX phase ceramics coating needed for cold air driven spray painter is deposited on for raw material powder.The present invention has the features such as coating layer thickness high quality prepared is good, and powder deposition velocity is fast, and process is reacted without MAX phase decompositions to be occurred, suitable large-scale application easy to use by the method that cold spraying in-situ preparation prepares MAX phase coatings.
Description
Technical field
The present invention relates to ceramic coating and Surface Engineering field, specially a kind of Ti2The cold spraying of AlC phase ceramics coatings is former
Position generation preparation method.
Background technology
MAX phases are a kind of ternary processable ceramics with nanometer laminated structure, and this ceramics have covalent bond, gold simultaneously
Belong to key, ionic bond, thus have both the property of ceramics and metal.Such as：The high-melting-point of ceramic material, anti-oxidant and resistance to corrosion,
Performances, the These characteristics such as electric conductivity, machinability, damage capacitive reactance, the heat shock resistance of metal cause MAX phase coatings to be expected in high temperature
It is applied in the fields such as military service component, protective coating, conducting element.However to by the membrane structure material of MAX phases with going bail for
Shield property coating, then coating must there is preferable quality to have both suitable thickness simultaneously.
The existing method that MAX phase coatings are obtained by physical vapour deposition (PVD) is not only high to equipment requirement, when coating deposits
Between it is long lead to low production efficiency, while by vapor deposition apparatus size limited can not on large-size components prepares coating, and
The coating layer thickness that this method obtains is limited.The excellent inoxidizability of MAX phases is mainly derived from A layers of element integrally outside divergent contour
Into the oxidation film of continuous densification.The MAX phase coating layer thicknesses for the legal system that is vapor-deposited are limited, are on active service under the high temperature conditions, the A in coating
Layer element can be consumed rapidly and lose protectiveness.In addition to the above methods, another MAX phase coating production in the world
It is coating of the thickness up to hundreds of microns to be obtained by supersonic flame spraying method, but since MAX phases are a kind of metastable state phases,
Other decomposition products are easily generated at a high temperature of thermal spraying.To Ti2For AlC phases, in hot-spraying coating can contain TiC and
TixAlyAnd Ti3AlC2Wait Ti2The decomposition product of AlC phases destroys fine and close continuous oxidation film and antioxygenic property is caused to decline.
Invention content
The purpose of the present invention is to provide a kind of Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, in order to
It solves existing vapour deposition process and prepares Ti2AlC coatings are high there are equipment requirement, and low production efficiency, the part dimension of protection to be limited,
The problem of coating layer thickness is limited.And Ti prepared by supersonic flame spraying method2There is thermal decomposition and coating compactness in AlC coatings
It is low, the problem of coating and base material associativity are bad.Coating prepared by the present invention is free of Ti2The decomposition product of AlC phases, coating layer thickness
Up to hundreds of microns, coating is fine and close and is well combined with base material.Coating deposition rate is fast, and production efficiency is high, and method is easy, not by
Part dimension limits, and is easy to industrialize large-scale production and application.
Technical scheme is as follows：
A kind of Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, using cold air driven spray painter in base
Deposition is used to prepare the material powder of MAX phases on material, and material powder uses TiH2, Al and TiC.
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, material powder TiH2, Al and TiC
Granularity is respectively：TiH20.05~50 micron, 0.04~50 micron of 0.05~50 micron of Al, TiC.
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, material powder TiH2, Al and TiC
Molar ratio is n (TiH2)：n(Al)：N (TiC)=(1~3):(1~5):1.
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, for the original of cold spraying prepares coating
Feed powder body, which need to add bonding agent and organic solvent and is prepared by ball milling or other methods, is mixed into raw material slurry.
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, bonding agent are polyethylene glycol or poly- second
Enol, organic solvent are ethyl alcohol, methanol or acetone, and the weight ratio of bonding agent and organic solvent is 1：(20~200).
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings is for the material powder of cold spraying
The spherical composite granule prepared by raw material slurry spray drying, the granularity of spherical composite granule is 5~150 microns.
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings is sprayed using hyperbaric atmosphere cold air and filled
It is as follows to put progress powder deposition, process parameters range on base material：Spray 1~5MPa of air pressure, gas temperature 100~1000
DEG C, obtain the raw material coating that thickness is 5~300 microns after spraying 5~50 passages.
The Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, in vacuum or has inert gas shielding
Under conditions of carry out Ti2The sintering of AlC phase ceramics coatings, process parameters range are as follows：500~1500 DEG C of sintering temperature is burnt
20~120min of time is tied, obtains the Ti of 5~300 microns of thickness2AlC coatings.
The present invention design philosophy be：
Compared with the conventional method, cold spraying of the present invention is made gas reach very high air pressure and is driven by heat gas
Powder granule passes through nozzle.The heating time that this spraying method powder granule is subject to is short, will not generate apparent hot shadow to powder
It rings.Sprayed particle can be accelerated to several times velocity of sound by air-flow simultaneously, and it is fast that powder deposition and coating prepare speed.Pass through the side of cold spraying
Method will pressureless sintering synthesis MAX phases material powder be deposited on base material, by particle supersonic speed bombarding base material just can obtain
It is fully plastically deformed and with the raw material coating that base material is well combined, which is sintered under vacuum or protective atmosphere
Acquisition is well combined with base material, the fine and close and MAX phase coatings without other impurities.
The present invention has the following advantages and beneficial effects：
1. the present invention prepares MAX phase coatings using the method for cold spraying, MAX phase constituents are without by the height for reaching thermal decomposition
Temperature, the Ti of preparation2AlC coatings are free of TiC and TixAlyDecomposition products are waited, the coating quality of acquisition is good, anti-oxidant and corrosion resistance
It can improve.
2. the present invention prepares spherical material powder using spray drying, the powder fluidity is good, and spraying property is excellent, and should
Composite granule composition separation in cold spray process is not notable.Powder material, by fully plastic deformation, is obtained in substrate surface
Raw material coating it is fine and close and be well combined with base material.
3. the present invention prepares MAX phase coatings using the method for in-situ sintering on base material, sintered coating is produced with base material
Raw is metallurgical binding, interface imporosity and objectionable impurities, and coating is good with base material associativity, and heat resistanceheat resistant cycle and thermal impact are good.
4. the coating layer thickness limitation of vapour deposition process can be broken through using coating prepared by the present invention, thickness can be prepared up to number
Hundred microns of dense coating, the inoxidizability element in coating is more sufficient, can extend effective protecting time of the coating to base material,
And finer and close, continuous protective oxide film can be formed.
5. preparing MAX phases coating using the present invention has the advantages of deposition velocity is fast, and production efficiency is high, and method is easy easily
In grasp and promote.This method prepares MAX phases coating and can not be limited by part dimension, can meet large-size components and large surface
Spraying requirement is easy to industrialize large-scale production and application.
Description of the drawings
Fig. 1 is the X-ray diffracting spectrum of material powder that obtains after 1 mist projection granulating of embodiment.In figure, abscissa
2Theta is the angle of diffraction (deg.), and ordinate Intensity is intensity.
Fig. 2 is the x-ray diffraction pattern of the raw material coating rear surface that cold spraying deposits on TiAl alloy base material of embodiment 1
Spectrum.In figure, abscissa 2Theta is the angle of diffraction (deg.), and ordinate Intensity is intensity.
Fig. 3 is the x-ray diffraction pattern of the raw material coating rear surface that cold spraying deposits on TiAl alloy base material of embodiment 2
Spectrum.In figure, abscissa 2Theta is the angle of diffraction (deg.), and ordinate Intensity is intensity.
Fig. 4 is the X- on the sintered surface of raw material Coatings in Vacuum that cold spraying deposits on TiAl alloy base material of embodiment 1
X ray diffraction collection of illustrative plates.In figure, abscissa 2Theta is the angle of diffraction (deg.), and ordinate Intensity is intensity.
Fig. 5 is the electron scanning photo of spherical material powder that obtains after 1 mist projection granulating of embodiment.
Fig. 6 is the surface electronic scanned photograph of the raw material coating that cold spraying deposits on TiAl alloy base material of embodiment 2.
Fig. 7 is the Ti that embodiment 1 is formed on TiAl alloy base material after vacuum-sintering2The section electron scanning of AlC coatings
Photo.
Specific embodiment
In specific implementation process, the method for the present invention can be applied to the MAX phase material systems of energy pressureless sintering synthesis, specifically
With a kind of Ti2The preparation method explanation of AlC ceramic coatings.It first will be for being sintered the material powder of prepares coating in required ratio
Mixing, it is slurry then to add in organic solvent and bonding agent wet ball grinding.Slurry is dried to spherical shape with spray drying granulation method
Raw material powder.By raw material powder needed for cold air driven spray painter is deposited on the base material of prepares coating, by the base material of deposition
It is sintered under vacuum atmosphere with regard to generated in-situ MAX phase ceramics coating can be obtained with coating.
The present invention is described in further detail with reference to the accompanying drawings and examples, but does not limit the present invention.
Embodiment 1
By TiH2, Al, TiC powder raw material in molar ratio be n (TiH2)：n(Al)：N (TiC)=1:1.1:1 ratio dispensing.
TiH2Powder average grain diameter 800nm, 1 micron of purity 99.9wt%, Al powder average grain diameter, purity 99.9wt%, TiC average grain diameter
500nm, purity 99.8wt%, raw material weight amount to 1Kg, are uniformly mixed with blender stirring 30min.
15g polyethylene glycol is added in into 1.5Kg absolute ethyl alcohols, heating water bath simultaneously stirs and forms mixed solution.It will mix equal
Even powder adds in absolute ethyl alcohol-polyglycol solution, is packed into the stirring ball mill device of 3L.Ball mill mixing stage speed of agitator
300r/min, time 30min.Pelletization stage removes abrading-ball, and adjustment speed of agitator is 50 r/min, maintains to atomization prilling
Stop.It is 10 to be dried slurry atomization with the organic solvent type lab spray dryer with inert gas closed circulation
The spherical composite powder of microns.As shown in Figure 1, the X-ray diffracting spectrum of the material powder obtained after mist projection granulating, it can
It is not changed by spray-drying process powder constituents with finding out.Fig. 5 show the electron scanning image of the spherical powder particles
Photo, it can be seen that powder is made of in spherical the raw material of sub-micron.
The alloy that the trade mark is Ti-45Al-2Nb-2Mn is cut into the small sample block of 20 × 10 × 3mm, the aluminium oxide through 80 mesh
Sand surface sand-blasting process.Powder deposition is carried out on base material using hyperbaric atmosphere cold air spray equipment, sprays air pressure 1.2MPa, gas
250 DEG C of temperature obtains the raw material coating that thickness is 5 microns after spraying 10 passages.As shown in Fig. 2, there is raw material coating on surface
TiAl sample X-ray diffracting spectrums, since the raw material figure layer is relatively thin, visible base material TiAl alloy peak spectrum in collection of illustrative plates, and meanwhile it is different
Material powder deposition capability on base material is also variant, crisp and hard material such as TiH2Deposition is poor.The sample is sealed
Enter to be passed through the quartz ampoule inner tube of argon gas protection, quartz ampoule is sintered in Muffle furnace, 1200 DEG C of sintering temperature, sintering time
60min.As shown in figure 4, the coating X-ray diffracting spectrum finally obtained, X-ray diffraction breaks through coating, so removing
Ti2Outside AlC coatings, diffracting spectrum also has base material peak spectrum, and in addition to this sintering also has a small amount of Ti in quartz ampoule5Si3Generation.Figure
7 be the coating and the section electron scanning image photograph of base material, understands coating and base material metallurgical binding by picture, associativity is very
It is good.
Embodiment 2
By TiH2, Al, TiC powder raw material in molar ratio be n (TiH2)：n(Al)：N (TiC)=1:1.1:1 ratio dispensing.
TiH2Powder average grain diameter 800nm, 1 micron of purity 99.9wt%, Al powder average grain diameter, purity 99.9wt%, TiC average grain diameter
500nm, purity 99.8wt%, raw material weight amount to 1Kg, are uniformly mixed with blender stirring 30min.
10g polyethylene glycol is added in into 1.5Kg absolute ethyl alcohols, heating water bath simultaneously stirs and forms mixed solution.It will mix equal
Even powder adds in absolute ethyl alcohol-polyglycol solution, is packed into the vibratory milling device of 3L, vibration frequency 50Hz, amplitude 5mm,
Ball-milling Time 30 minutes.Slurry after ball milling is poured out and is packed into the beaker of 5L while is stirred with blender, speed of agitator 50r/
Min maintains to atomization prilling to stop.Slurry is dried with the centrifugal atomizing drying machine with closed circulation, is used
Centrifugal atomizing nozzle, is atomized disk diameter 50mm, and atomizer rotating speed 20000r/min intake air temperatures are set as 150 DEG C, go out wind-warm syndrome
90 DEG C of degree control.Wriggling revolution speed 30r/min, heating power 9KW.
The alloy that the trade mark is Ti-45Al-2Nb-2Mn is cut into the small sample block of 20 × 10 × 3mm, the aluminium oxide through 80 mesh
Sand surface sand-blasting process.Powder deposition is carried out on base material using hyperbaric atmosphere cold air spray equipment, sprays air pressure 1.8MPa, gas
400 DEG C of temperature obtains the raw material coating that thickness is 150 microns after spraying 20 passages.As shown in figure 3, deposition has raw material coating
TiAl specimen surface X-ray diffracting spectrums, since the thicker X-ray diffraction of raw material coating fails to penetrate coating, in coating not
It composes at peak containing base material.As shown in fig. 6, there is the electron scanning image photograph of the TiAl samples of raw material coating on surface, understood by picture
The powder material effect of being hit when substrate surface deposits generates apparent plastic deformation in cold spray process.The sample is packed into
Alumina crucible is sintered in a vacuum furnace, and 1200 DEG C, sintering time 60min of sintering temperature can obtain thickness up to 150 microns
Ti2AlC coatings.
Embodiment the result shows that, the present invention MAX phase coatings are prepared by cold spraying in-situ preparation method, with cold spraying
Depositing powders raw material, in-situ sintering prepare MAX phase ceramics coatings, have the coating layer thickness high quality prepared good, powder deposits speed
The features such as degree is fast, and process is reacted without MAX phase decompositions to be occurred, suitable large-scale application easy to use.
Claims (5)
1. a kind of Ti2The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, which is characterized in that using cold air power spraying and coating
Device is used to prepare the material powder of MAX phases in deposited on substrates, and material powder uses TiH2, Al and TiC, in vacuum or inertia
Sintering obtains generated in-situ MAX phase ceramics coating under gas shield；
Material powder TiH2, Al and TiC granularity be respectively：TiH20.05~50 micron, 0.05~50 micron of Al, TiC
0.04~50 micron；
Material powder TiH2, Al and TiC molar ratio be n (TiH2)：n(Al)：N (TiC)=(1~3):(1~5):1；
Powder deposition is carried out on base material using hyperbaric atmosphere cold air spray equipment, process parameters range is as follows：Spray air pressure 1
~5MPa, 100~1000 DEG C of gas temperature obtain the raw material coating that thickness is 5~300 microns after spraying 5~50 passages.
2. Ti according to claim 12The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, which is characterized in that
For cold spraying prepares coating material powder need to add bonding agent and organic solvent be prepared by ball milling or other methods it is mixed
It closes uniformly into raw material slurry.
3. Ti according to claim 22The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, which is characterized in that
Bonding agent is polyethylene glycol or polyvinyl alcohol, and organic solvent is the weight ratio of ethyl alcohol, methanol or acetone, bonding agent and organic solvent
It is 1：(20~200).
4. Ti according to claim 12The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, which is characterized in that
Material powder for cold spraying is by the spherical composite granule of raw material slurry spray drying preparation, the granularity of spherical composite granule
It is 5~150 microns.
5. Ti according to claim 12The cold spraying in-situ preparation preparation method of AlC phase ceramics coatings, which is characterized in that
In vacuum or have and carry out Ti under conditions of inert gas shielding2The sintering of AlC phase ceramics coatings, process parameters range are as follows：
500~1500 DEG C, 20~120min of sintering time of sintering temperature obtains the Ti of 5~300 microns of thickness2AlC coatings.
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| CN108080628A (en) * | 2016-11-23 | 2018-05-29 | 中国科学院金属研究所 | The high-throughput preparation method of particles reiforced metal-base composition under a kind of low temperature solid-state |
| CN110396687A (en) * | 2018-04-24 | 2019-11-01 | 中国科学院金属研究所 | A kind of Ti2AlC MAX phase ceramics coating and its cold spraying preparation method |
| CN109957757B (en) * | 2019-04-04 | 2021-06-08 | 中国核动力研究设计院 | Method for preparing ultra-thick Ti-Al-C ternary coating by two-step PVD (physical vapor deposition) technology |
| CN111005024B (en) * | 2019-12-04 | 2021-12-17 | 天津大学 | Thermal barrier coating resistant to molten CMAS corrosion and preparation method thereof |
| CN111116211A (en) * | 2019-12-27 | 2020-05-08 | 中铭瓷(苏州)纳米粉体技术有限公司 | Preparation method of ternary nano lamellar MAX phase powder and product thereof |
| CN111763939B (en) * | 2020-07-18 | 2022-04-01 | 新余学院 | Multi-scale TiC ceramic phase reinforced TiAl3TiAl biphase composite coating and preparation method thereof |
| CN115491629A (en) * | 2022-10-17 | 2022-12-20 | 河北工业大学 | Method for preparing Ti-Al-C-based composite coating by using plasma spraying |
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| Cold Spraying of Ti2AlC MAX-Phase Coatings;H.Gutzmann etal.;《Journal of Thermal Spray Technology》;20121110;第22卷(第2/3期);第406-412页 * |
| TiH2做Ti原合成Ti2AlC/Ti3AlC2及热分析;李良等;《硅酸盐通报》;20130131;第32卷(第1期);第132-137页 * |
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