CN104988448B - A kind of Al Ti C systems react the preparation method of powder cored filament material - Google Patents
A kind of Al Ti C systems react the preparation method of powder cored filament material Download PDFInfo
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Abstract
A kind of preparation method of Al Ti C systems reaction powder cored filament material is related to ceramic matric composite preparing technical field.Step of the present invention includes：1) by titanium valve wet-milling in organic solvent medium (absolute ethyl alcohol or acetone), sucrose solution formation mixed material is added；2) dried after mixed material is stirred, be placed in vacuum heat treatment furnace and heat up, sucrose is carbonized, form Ti C mixed systems；3) mixed material after carbonization is crushed, screens out the suitable Ti C composite powders of particle diameter as powder core material；4) by skin material of aluminium strip, Ti C composite powders be powder core material, Al Ti C powder cored filament materials are manufactured using the continuous hot candied tube reducing method of multiple tracks.It is a feature of the present invention that skin material and the constituent element that powder cored filament material is all reaction system, form Al Ti C reaction systems, SHS process (SHS) reaction, fabricated in situ Ti occur in spraying process for the system2AlC base ceramic coatings, using inexpensive raw material, high performance composite ceramic coat is obtained by SHS reactions.
Description
Technical field
The present invention relates to ceramic matric composite preparing technical field, and in particular to one kind is used for reaction thermal spraying ceramics and applied
The preparation method of the powder cored filament material of layer.
Background technology
Ceramic material is due to characteristics such as high-melting-point, high intensity, high rigidity, high-modulus, high chemically stables so that thermal spraying is made pottery
Porcelain coating has the good characteristic such as high temperature resistant, anti-oxidant, wear-resistant, corrosion-resistant.Ceramic coating is generally with ceramic powders or bar
For raw material, prepared using plasma spray technologies such as plasma spraying, detonation flame spraying, HVAFs.But utilize this method
Ceramic coating is prepared, on the one hand because the expensive ceramic powders of needs or bar are as spraying raw material, and can be provided
The plasma spray technology equipment of high-power thermal source, makes ceramic coating prepare cost higher；On the other hand, because ceramic fusing point is very high,
It is prominent to be usually present that ceramic material is difficult to be completely melt, ceramic phase skewness, coating Coating combination are weak in spraying process etc.
Problem, makes coating performance by important adverse effect.Cost is prepared for reduction ceramic coating, ceramic coating performance is improved, grinds
The person of studying carefully develops reaction thermal spraying technology, i.e., using the reaction raw materials of relative low price as sprayed on material, is drawn using thermal source is sprayed
The highly exothermic SHS reactions of spraying system are fired, fabricated in situ target ceramics are reacted by spraying the SHS of system in thermal spray process
Composition, obtains high performance ceramic coating.
Reactive spray material is the key link that ceramic coating is prepared using reaction thermal spraying technology.At present, researcher couple
In terms of the research and development of reaction thermal spraying material are concentrated mainly on dusty spray.But due to carrying out reaction thermal spraying using powder
When, for the reaction uniformity that ensures spraying particle is good, ceramic coating combination property that is preparing is high, it is desirable to the particle diameter model of dusty spray
Enclose very narrow, this make it that the preparation efficiency of reactive spray powder is relatively low, so that having raised ceramic coating indirectly prepares cost.The opposing party
Face, dusty material can not utilize in plasma spray technology the arc spraying technology that cost is minimum, optimum is widely applied to prepare and apply
Layer, also limit the practical implementation of reaction thermal spraying ceramic coating.
Powder cored filament material is the sprayed on material commonly used in plasma spray technology, is especially melted in electric arc spraying infusibility, poorly conductive
Metal, have great importance in terms of alloy or ceramic material.But current powder cored filament material is generally by sheet metal strip bag
Wrap up in different types of powder filler (such as：Metal, alloy, ceramics etc.), to extend the composition of silk material, improve the quality of coating, system
Standby coating is mostly by matrix of metal, hard alloy or ceramic component are to strengthen the metal-based compound coating of phase.Or in gold
Obtain hard particles enhancing metal in category, alloy in a small amount of reaction constituent element of addition, spraying process by reacting synthesis ceramic phase
Base composite coating, to improve the performances such as the wear-resisting of coating, high temperature resistant.Because ceramic phase content is less, the combination property of coating, especially
It is that high temperature wear resistant performance still can not be with being compared favourably with the ceramic base composite coating of ceramic main body.
SHS process (SHS) technology is to react liberated heat using reaction raw materials own combustion, is made chemical anti-
Answer a kind of spontaneous lasting new material synthetic technology for carrying out, there is specified composition and structured product with acquisition of process.It has
Technique, equipment are simple, and cost is low；Energy consumption and raw materials consumption are few；Reaction temperature is high, and product purity is high；Original can be made full use of
The advantages of position is compound, is particularly suitable for preparing ceramics, cermet and ceramic matric composite etc. with high-melting-point, high rigidity, height
The material of strength characteristic.
Mn+1AXnSerial ceramic layered (abbreviation MAX is ceramic layered) is the class novel ceramic extensively paid close attention in recent years by researcher
Ceramic material, they are possessing the same of the advantages of traditional ceramics strength of materials is high, hardness is high, heat endurance is good, oxidation resistance is strong
When, also possess the advantage that metal material electrical and thermal conductivity performance is good, modulus of elasticity is high.Especially there is plasticity at relatively high temperatures,
The characteristic that can be machined as metal material, becomes military service under the conditions of the bad working environments such as high temperature, abrasion, corrosion
Ideal material, had broad application prospects in high-tech sectors such as Aeronautics and Astronautics, military projects.But prepared by such ceramic material
Condition is harsh, and technique, equipment are complicated, and cost is higher, constrains its practical application.
In known MAX ternary layered ceramics, Ti2AlC is most light (the density 4.1g/cm of weight3), antioxygenic property most
Good one kind.In Ti-Al-C ternary layered ceramics, Ti-C keys are mainly strong covalent bond and ionic bond is combined, and assign material high
The performances such as fusing point, high intensity, high-modulus；And Ti-Al keys have obviously metallic bond feature, material leading well is assigned
Electricity, heat conductivility；Particular, it is important that weak with the Van der Waals force similar to graphite layers between Ti atoms and Al atomic planes layer
Bond is closed so that Ti2AlC materials have layer structure and self-lubricating property.Ti2These ceramic layered AlC characteristics become
The high-performance ceramic coating material that one class has a high potential.
The content of the invention
The present invention provides a kind of available for reaction thermal spraying Ti2The Al-Ti-C powder cored filament materials of AlC base composite ceramic coatings
Preparation method, material foundation is provided for reaction electric arc spraying, wire flame spraying high-performance ceramic coating.In order to ensure what is prepared
Powder cored filament material can prepare Ti by reaction thermal spraying2AlC base composite ceramic coatings, prepared powder core needs to be easy to ignite,
Reaction is quick and can react synthesis target ceramic phase.
The technical solution adopted for the present invention to solve the technical problems：Suitable material system is selected, powder core system is entered
Row composited processing, works out suitable silk material preparation technology, prepares a kind of Al-Ti-C systems reaction powder cored filament material, is characterized in
Comprise the steps：
Step one：Using titanium valve as reaction raw material, the wet-milling in organic solvent medium with sand mill；Claim sucrose, be dissolved in steaming
Distilled water formation sucrose solution, adds in above-mentioned material and continues wet-milling, stirring 1 hour, form mixed slurry；
Step 2：Mixed slurry is poured into container, is placed in 105~110 DEG C of baking oven and dries, is removed in mixed material
Organic solvent and water (noting divulging information in drying course)；Solid material after drying is broken into bulk, 220~225 DEG C are placed in
In vacuum heat treatment furnace, the sucrose in solid material is set to be carbonized (C12H22O11→12C+11H2O1), form Ti-C mixed systems；
Step 3：The block Ti-C mixed materials after carbonization are crushed using pulverizer ,+400~-150 mesh models are screened out
Ti-C composite powders in enclosing are as powder core material；
Step 4：By skin material of aluminium strip, above-mentioned Ti-C composite powders be powder core material, using the continuous hot candied tube reducing of multiple tracks
Method manufactures Al-Ti-C powder cored filament materials.
Further, the titanium valve of selection is that particle diameter is less than 250 targeted fine powders, and the wet-milling time is 1~24h.Wherein, the wet-milling time
It is related to the titanium valve particle diameter of selection, such as：The titanium valve of the mesh of particle diameter -250 grinds 20~24h；The titanium valve grinding 8 of the mesh of particle diameter -400~
12h；The titanium valve of the mesh of particle diameter -600 grinds 1~2h.
Further, organic solvent medium is absolute ethyl alcohol or acetone.
Further, 10~14mm of aluminium strip width, the 0.2~0.3mm of thickness of selection, the silk material diameter Ф 2.0 of preparation~
3.0mm。
The beneficial effects of the invention are as follows：
1) Ti can be prepared using the reaction powder cored filament material2AlC ceramic layered is matrix, TiC0.2N0.8、Al2O3Deng for second
The composite ceramic coat of phase, due to by means of the SHS process characteristic of sprayed on material, it is possible to use inexpensive former material
Material Al bands, Ti powder and sucrose prepare high performance Ti2AlC base composite ceramic coatings；
2) it is one of constituent element of reaction as the Al of skin material that distinct characteristic of the invention, which is, is participated in spraying process
The SHS reactions of system, when reactive spray is completed, spraying raw material total overall reactions consumption, during the coating of acquisition is spraying process
The ceramic phase of in-situ reactive synthesis, according to this feature, using the powder cored filament material as sprayed on material, using electric arc spraying equipment, line
Material flame spray device prepares composite ceramic coat；
3) during reactive spray, the metal component A l (660 DEG C of fusing point) of low melting point can melt quickly, be carried for spraying system
For mass transfer in liquid phase condition, promote the SHS reactions of spraying system, simultaneously because in spraying process metal Al preferentially and oxygen reaction,
Other spraying ingredient Ti, C can be protected not to be aoxidized, it is to avoid occur the loose phase TiO of influence coating quality in duplex heat treatment2, and
Generation and Ti2The good beneficial ceramic phase Al of AlC compatibilities2O3, it is ensured that the combination property of coating；
4) one aspect of the present invention is less than the purification ultrafine titanium powder of 300 mesh by using particle diameter, and passes through wet-milling tube reducing, makes titanium valve table
Face is activated, on the other hand, can be effective by forming the tight structure of high-activity amorphous carbon (sucrose carbonization is generated) cladding Ti powder
Promote the mass transport process between reaction constituent element in spraying process, it is ensured that SHS reactions quickly occur for spraying system；
5) present invention selection sucrose prepares Ti-C composite powders as reaction constituent element C presoma using sucrose carbonization method,
Rather than as powder core, will can directly prevent that sprayed on material is acted in high pressure draught in spraying process after Ti powder, C powder mechanical mixtures
Lower separation, it is ensured that the SHS reactions of spraying system can be smoothly completed, and obtain target product phase；
6) Ti prepared using the powder cored filament material2In AlC base composite ceramic coatings, each ceramic phase of composition coating is spray
Painting process situ reaction synthesis, dystectic ceramic phase melting is abundant, makes the ceramic coating uniform texture of acquisition, crystal grain
It is tiny, in addition, with Ti2The ceramic layered composite coatings for matrix of AlC have conductive, heat conductivility, and with good machinery
Processing characteristics and from antifriction performance, excellent combination property.
Brief description of the drawings
Fig. 1 is, using -400 mesh titanium valves as raw material, Al-Ti-C systems reaction powder core to be prepared by organic solvent of absolute ethyl alcohol
The process chart of silk material.
Fig. 2 is that the X-ray of the composite coating prepared using electric arc spraying equipment is spread out to react powder cored filament material as sprayed on material
Penetrate analysis (XRD) result.
Fig. 3 is field emission scanning electron microscope (SEM) shape appearance figure of composite coating.(a), (b) is respectively multiplication factor
The SEM photograph of 200 times and 4000 times lower coatings.
Embodiment
With reference to the accompanying drawings and examples, the embodiment to the present invention is further described.
Fig. 1 is, using -400 mesh titanium valves as raw material, Al-Ti-C systems reaction powder core to be prepared by organic solvent of absolute ethyl alcohol
The process chart of silk material.As shown in figure 1, the present invention prepares Al-Ti-C systems reaction powder cored filament material, implement according to the following steps：
Step one：Weigh the mesh of granularity -400, the Ti powder 1150g of purity 99.9%, be placed in sand mill, add 500ml without
Water-ethanol, wet-milling 8 hours according to ethanol volatilization situation during wet-milling, supplements a small amount of ethanol, keeps ethanol in sand mill to infiltrate
Titanium valve.Weighing the pure sucrose of 342g analyses, (titanium valve is 24 with sucrose mol ratio:1), dissolve in 200ml distilled water, and sucrose is molten
Liquid is poured into sand mill, is continued wet-milling 1 hour, mixed material is stirred.
Step 2：Mixed material is poured into and is lined with 3 pallets of aluminium-foil paper (preventing from being mixed into impurity), 105 DEG C are placed in
Dried in baking oven, (baking oven keeps divulging information the absolute ethyl alcohol in removal mixed material during drying, prevents the absolute ethyl alcohol of volatilization with water
Assemble in baking oven, trigger detonation)；Solid material after drying is broken into bulk, in the vacuum heat treatment furnace for being placed in 220 DEG C
(vacuum 2.5Pa), makes the sucrose in solid material be carbonized (C12H22O11→12C+11H2O1), carbonization time 2 hours is formed
Ti-C mixed systems.
Because the unformed charcoal of titanium valve in Ti-C mixed systems and sucrose carbonization generation is respectively provided with very high activity, during carbonization
Carburizing temperature (230 DEG C must not be higher than) must be strictly controlled, prevents carburizing temperature too high, causes mixed system to occur SHS reactions.
Step 3：The block Ti-C mixed materials after carbonization are crushed using pulverizer ,+400~-150 mesh models are screened out
Ti-C composite powders in enclosing are as powder core material.
Step 4：Using width 10mm, thickness 0.2mm aluminium strip as skin material, Ti-C composite powders as powder core material, adopt
Manufacture Al-Ti-C powder cored filament materials with the continuous hot candied tube reducing method of multiple tracks, by silk material diameter by 3.2mm successively tube reducing 0.1mm extremely
2.8mm。
Electric arc spraying equipment used below carries out spray test, is verified with experimental data, the Al- prepared using the present invention
Ti-C systems reaction powder cored filament material is sprayed on material, can prepare Ti2AlC base composite ceramic coatings.Electric arc spraying equipment is base
The automatic high-speed arc spraying system controlled in Motoman robots, spraying matrix is put down for 40mm × 40mm × 5mm 45 steel
Plate sample, spraying parameter setting is as shown in the table.Sample is through blasting treatment before spraying.
| Spray voltage/V | Spray distance/mm | Atomization pressure/MPa |
| 30 | 150 | 0.6 |
Fig. 2 is X-ray diffraction (XRD) analysis result of the composite ceramic coat prepared under above-mentioned process conditions.From figure
As can be seen that there is no the appearance of Ti, Al peak in the XRD results of coating, illustrate that sprayed on material reacts completely in spraying process.
Coating is main by Ti2AlC、TiC0.2N0.8And Al2O3Deng ceramic phase composition, multicomponent composite ceramic coat is formed.Wherein,
Ti2AlC is that Ti, Al, C three react generation；Al2O3Generated for the oxygen reaction in Al and air；TiC0.2N0.8For spraying process
The solid solution of TiC (Ti, C reaction generation) and TiN (Ti is generated with nitrogen reaction in air) formation of middle generation.Demonstrate utilization
Reaction powder cored filament material prepared by the present invention can prepare Ti2AlC base composite ceramic coatings.
Fig. 3 is field emission scanning electron microscope (SEM) photo of coating.Wherein Fig. 3 (a), (b) are respectively multiplication factor
The SEM photograph of 200 times and 4000 times lower coatings.It can be seen that coating structure, even tissue, crystal grain is tiny.Table
Deformation of the composite ceramics molten drop on base material of bright reaction synthesis, sprawl it is in good condition, the composite ceramic coat defect of formation compared with
It is few.
Following table is the Main Mechanical test result of composite ceramic coat.Wherein, surveyed using Wilson microhardnesses instrument
Determine the microhardness of coating, test load 200g, load time 15s take 10 test point average values hard as the Vickers of coating
Degree；Modulus of elasticity is determined using Nano Indenter XP multifunctional nanos impress tester, test parameters：Maximum depth of cup
500 μm, maximum load 600mN takes 5 groups of samples to measure average value as the modulus of elasticity of coating；Coating is resistance to the steel of matrix 45
Mill performance is determined on UMT-2 friction wear testing machines, test parameters：Load 100N, time 30min, frequency 10Hz；Corresponding mill
Damage amount is observed and calculated using the three-dimensional white light interference surface topographic apparatus fos of Phase Shift MicroWav-3D, takes 3 groups of samples
Average value is measured as the wear extent of coating.The wear extent of composite ceramic coat is only matrix material under as shown by data, the same terms
Nearly the 1/9 of material, shows the Ti prepared2AlC base composite ceramic coatings have been obviously improved the anti-wear performance of material.
| Vickers hardness/HV0.2 | Modulus of elasticity/GPa | Wear extent (coating)/mm3 | Wear extent (45 steel)/mm3 |
| 1125±189 | 352±47 | 3.8±0.7 | 33.6±0.5 |
Claims (1)
1. a kind of Al-Ti-C systems react the preparation method of powder cored filament material, it is characterised in that complete according to the following steps：
1) using titanium valve as reaction raw material, with sand mill wet-milling in absolute ethyl alcohol or medium-acetone；Sucrose is weighed, distillation is dissolved in
Water formation sucrose solution, adds in above-mentioned material and continues wet-milling, stirring 1 hour, form mixed slurry；Mole of titanium valve and sucrose
It is 22 than scope:1~26:1；
2) mixed slurry is poured into container, is placed in 105~110 DEG C of baking oven and dries, remove the organic solvent in mixed material
With water；Solid material after drying is broken into bulk, in the vacuum heat treatment furnace for being placed in 220~225 DEG C, made in solid material
Sucrose is carbonized 1-2 hours, forms Ti-C mixed systems；
3) the block Ti-C mixed materials after carbonization are crushed using pulverizer, screens out the Ti-C in the range of+400~-150 mesh
Composite powder is used as powder core material；
4) by skin material of aluminium strip, above-mentioned Ti-C composite powders be powder core material, manufactured using the continuous hot candied tube reducing method of multiple tracks
Al-Ti-C powder cored filament materials；
Wherein, the titanium valve of selection is that particle diameter is less than 250 targeted fine powders, and the wet-milling time is 1~24h；Wet-milling time and the titanium chosen
Powder footpath is related, and the titanium valve of the mesh of particle diameter -250 grinds 20~24h；The titanium valve of the mesh of particle diameter -400 grinds 8~12h；The mesh of particle diameter -600
Titanium valve grind 1~2h；10~14mm of aluminium strip width, the 0.2~0.3mm of thickness of selection, the silk material diameter Ф 2.0 of preparation~
3.0mm。
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| CN104988448B (en) * | 2015-05-31 | 2017-11-03 | 中国人民解放军装甲兵工程学院 | A kind of Al Ti C systems react the preparation method of powder cored filament material |
| 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 |
| CN111451490B (en) * | 2020-05-25 | 2021-04-20 | 华中科技大学 | Metal type powder core wire material and preparation method and application thereof |
| CN111690892B (en) * | 2020-07-09 | 2022-03-22 | 长沙理工大学 | Preparation method of MAX phase-based coating |
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| CN104988448A (en) * | 2015-05-31 | 2015-10-21 | 中国人民解放军装甲兵工程学院 | Preparation method for Al-Ti-C system reaction cored wire |
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| CN104988448A (en) * | 2015-05-31 | 2015-10-21 | 中国人民解放军装甲兵工程学院 | Preparation method for Al-Ti-C system reaction cored wire |
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| 自反应电弧喷涂复相陶瓷涂层工艺研究;刘宏伟等;《装甲兵工程学院学报》;20131231;第27卷(第6期);第85页-第89页 * |
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