CN104988448A - Preparation method for Al-Ti-C system reaction cored wire - Google Patents
Preparation method for Al-Ti-C system reaction cored wire Download PDFInfo
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- CN104988448A CN104988448A CN201510290928.2A CN201510290928A CN104988448A CN 104988448 A CN104988448 A CN 104988448A CN 201510290928 A CN201510290928 A CN 201510290928A CN 104988448 A CN104988448 A CN 104988448A
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Abstract
The invention relates to the technical field of ceramic matrix composite preparation, and in particular to a preparation method for an Al-Ti-C system reaction cored wire. The method includes the steps that firstly, titanium powder is wetly ground in an organic solvent medium (absolute ethyl alcohol or acetone), a sucrose solution is added, and therefore a mixed material is generated; secondly, the mixed material is evenly stirred and then dried and placed in a vacuum heat treatment furnace so as to be heated, sucrose is carbonized, and a Ti-C mixed system is formed; thirdly, the carbonized mixed material is crushed, Ti-C composite powder with the proper grain diameter is obtained through screening and serves as a cored material; fourthly, an aluminum belt serves as a skin material, the Ti-C composite powder serves as the cored material, and a multi-stage continuous wire-drawing diameter-reducing method is adopted for preparing the Al-Ti-C cored wire. The method is characterized in that the skin material and the cored wire are both components of the reaction system, the Al-Ti-C reaction system is formed and generates a self-propagating high-temperature synthesis (SHS) reaction in the spraying process, a Ti2AlC-base ceramic coating is synthesized in situ, low-cost raw materials can be used, and a composite ceramic coating with the high performance can be acquired through the SHS reaction.
Description
Technical field
The present invention relates to ceramic matric composite preparing technical field, be specifically related to a kind of preparation method of the powder cored filament material for reaction thermal spraying ceramic coating.
Background technology
Stupalith, due to characteristics such as high-melting-point, high strength, high rigidity, high-modulus, high chemically stables, makes thermal Sperayed Ceramic Coatings have the good characteristics such as high temperature resistant, anti-oxidant, wear-resistant, corrosion-resistant.Ceramic coating usually with ceramic powder or bar for starting material, utilize the hot-spraying techniques preparations such as plasma spraying, detonation flame spraying, hypersonic flame spraying.But utilize the method to prepare ceramic coating, on the one hand because the expensive ceramic powder of needs or bar are as spraying starting material, and the hot-spraying techniques equipment of high-power thermal source can be provided, make ceramic coating preparation cost higher; On the other hand, because ceramic fusing point is very high, usually there is stupalith in spraying process and be difficult to outstanding problems such as melting completely, ceramic phase skewness, coating Coating combination are weak, make coating performance be subject to important disadvantageous effect.For reducing ceramic coating preparation cost, improve ceramic coating performance, software engineering researchers invent reaction thermal spraying technology, namely with the reaction raw materials of relative low price for spray material, the ignite high heat release SHS of spraying system of spraying thermal source is utilized to react, in thermal spray process, react fabricated in situ target ceramics component by the SHS of spraying system, obtain high performance ceramic coating.
Reactive spray material is the key link utilizing reaction thermal spraying technology to prepare ceramic coating.At present, investigator mainly concentrates on dusty spray aspect to the research and development of reaction thermal spraying material.But when carrying out reaction thermal spraying owing to utilizing powder, high for guaranteeing the reaction consistence of spraying particle ceramic coating over-all properties that is good, preparation, require that the particle size range of dusty spray is very narrow, this makes the preparation efficiency of reactive spray powder lower, thus has indirectly raised ceramic coating preparation cost.On the other hand, powdered material cannot utilize the arc spraying technology that is minimum, optimum spread of cost in hot-spraying techniques to prepare coating, also limit the practical implementation of reaction thermal spraying ceramic coating.
Powder cored filament material is spray material conventional in hot-spraying techniques, especially melts at electric arc spraying infusibility, has great importance in the metal of poorly conductive, alloy or stupalith.But current powder cored filament material is generally wrap up dissimilar powder filler (as: metal, alloy, pottery etc.) by sheet metal strip, carry out the composition of expansion wire material, improve the quality of coating, the metal-based compound coating that it be matrix, Wimet or ceramics component is wild phase that the coating of preparation mostly is with metal.Or add in metal, alloy and react constituent element on a small quantity, obtain hard particles mutually by reacting to synthesize ceramic in spraying process and strengthen metal-based compound coating, to improve the performance such as wear-resisting, high temperature resistant of coating.Because ceramic phase content is less, the over-all properties of coating, especially high temperature wear resistant performance still cannot compare favourably with the ceramic base compound coating with ceramic main body.
SHS process (SHS) technology utilizes reaction raw materials own combustion to react liberated heat, and spontaneous the continuing of chemical reaction process is carried out, to obtain a kind of type material synthetic technology having and specify composition and structured product.It has technique, equipment is simple, and cost is low; Energy consumption and raw materials consumption few; Temperature of reaction is high, and product purity is high; Can the advantages such as In-situ reaction be made full use of, be particularly suitable for preparing the material that pottery, sintering metal and ceramic matric composite etc. have high-melting-point, high rigidity, high strength characteristics.
M
n+1aX
nseries ceramic layered (being called for short MAX ceramic layered) is in recent years extensively by the class new ceramic material that investigator pays close attention to, they, while possessing the advantages such as the traditional ceramics strength of materials is high, hardness is high, Heat stability is good, resistance of oxidation are strong, also possess the advantage that metallic substance electrical and thermal conductivity performance is good, Young's modulus is high.Especially at relatively high temperatures there is plasticity, the characteristic of mechanical workout can be carried out as metallic substance, the ideal material of being on active service under becoming the bad working environments conditions such as high temperature, wearing and tearing, corrosion, has broad application prospects in the high-tech sector such as Aeronautics and Astronautics, military project.But such stupalith preparation condition is harsh, technique, equipment are complicated, and cost is higher, constrains its practical application.
In known MAX ternary layered ceramic, Ti
2alC is the lightest (the density 4.1g/cm of weight
3), the best one of antioxidant property.In Ti-Al-C ternary layered ceramic, Ti-C key mainly strong covalent bond and ionic linkage combines, and gives the performances such as material high-melting-point, high strength, high-modulus; And Ti-Al key has obviously metallic bond feature, give conduction, heat conductivility that material is good; Significantly, combine with the Van der Waals force weak bond being similar to graphite layers between Ti atom and Al atomic plane layer, make Ti
2alC material has laminate structure and self-lubricating property.Ti
2ceramic layered these characteristics of AlC become the high-performance ceramic coated material that a class has a high potential.
Summary of the invention
The invention provides one and can be used for reaction thermal spraying Ti
2the preparation method of the Al-Ti-C powder cored filament material of AlC base composite ceramic coating, for reaction electric arc spraying, wire flame spraying high-performance ceramic coating provide material foundation.In order to ensure that the powder cored filament material prepared can prepare Ti by reaction thermal spraying
2alC base composite ceramic coating, prepared powder core needs to be easy to ignite, react fast and can Reactive Synthesis target ceramic phase.
The technical solution adopted for the present invention to solve the technical problems: select suitable material system, carries out composited processing to powder core architecture, works out suitable silk material preparation technology, prepares a kind of Al-Ti-C system reaction powder cored filament material, is characterized in comprising the steps:
Step one: take titanium valve as reaction starting material, with sand mill wet-milling in organic solvent medium; Claim sucrose, be dissolved in distilled water and form sucrose solution, add in above-mentioned material and continue wet-milling, stirring 1 hour, form mixed slurry;
Step 2: pour mixed slurry into container, the baking oven being placed in 105 ~ 110 DEG C is dried, and removes the organic solvent in mixture and water (noting in drying course ventilating); Solid materials after drying is broken into bulk, is placed in the vacuum heat treatment furnace of 220 ~ 225 DEG C, makes the sucrose carbonization (C in solid materials
12h
22o
11→ 12C+11H
2o
1), form Ti-C mixed system;
Step 3: utilize pulverizer that the block Ti-C mixture after carbonization is broken, sieves out Ti-C composite powder within the scope of+400 ~-150 orders as powder core material;
Step 4: take aluminium strip as skin material, above-mentioned Ti-C composite powder is powder core material, adopts the continuous hot candied tube reducing method of multiple tracks to manufacture Al-Ti-C powder cored filament material.
Further, the titanium valve chosen is that particle diameter is less than 250 object fine powders, and the wet-milling time is 1 ~ 24h.Wherein, the wet-milling time is relevant to the titanium valve particle diameter chosen, as: particle diameter-250 object titanium valve grinding 20 ~ 24h; Particle diameter-400 object titanium valve grinding 8 ~ 12h; Particle diameter-600 object titanium valve grinding 1 ~ 2h.
Further, organic solvent medium is dehydrated alcohol or acetone.
Further, the aluminium strip width 10 ~ 14mm, the thickness 0.2 ~ 0.3mm that choose, the silk material diameter Ф 2.0 ~ 3.0mm of preparation.
The invention has the beneficial effects as follows:
1) this reaction powder cored filament material is adopted to prepare Ti
2alC is ceramic layered is matrix, TiC
0.2n
0.8, Al
2o
3deng the composite ceramic coat for second-phase, owing to by means of the SHS process characteristic of spray material, can utilize that the starting material Al of low cost is with, Ti powder and sucrose prepares high performance Ti
2alC base composite ceramic coating;
2) distinct characteristic of the present invention is, Al as skin material is one of constituent element of reaction, the SHS reaction of system is participated in spraying process, when reactive spray completes, spraying starting material total overall reaction consumes, and the coating of acquisition is the ceramic phase of spraying process situ Reactive Synthesis, according to this feature, with this powder cored filament material for spray material, electric arc spraying equipment can be utilized, wire flame spraying equipment prepares composite ceramic coat;
3) in reactive spray process; the metal component A l (fusing point 660 DEG C) of low melting point can melt very soon; for spraying system provides mass transfer in liquid phase condition; promote the SHS reaction of spraying system; simultaneously because metal A l in spraying process is preferential and oxygen reaction; other spraying ingredient Ti, C can be protected not oxidated, avoid the loose phase TiO occurring affecting coating quality in duplex heat treatment
2, and generate and Ti
2the useful ceramic phase Al that AlC consistency is good
2o
3, ensure that the over-all properties of coating;
4) one aspect of the present invention is less than 300 object purification ultrafine titanium powders by adopting particle diameter, and through wet-milling tube reducing, make titanium valve surface active, on the other hand, by forming the imporosity of high-activity amorphous carbon (sucrose carbonization generation) coated Ti powder, effectively can promote the mass transfer process of reacting in spraying process between constituent element, ensure that SHS reaction occurs spraying system fast;
5) the present invention selects sucrose as the presoma of reaction constituent element C, sucrose carbonization method is utilized to prepare Ti-C composite powder, instead of directly using after Ti powder, C powder mechanically mixing as powder core, spray material in spraying process can be prevented to be separated under high pressure draft effect, ensure that the SHS reaction of spraying system can complete smoothly, obtain target product phase;
6) Ti prepared by this powder cored filament material is utilized
2in AlC base composite ceramic coating, each ceramic phase of composition coating is spraying process situ Reactive Synthesis, and dystectic ceramic phase melting is abundant, and make the ceramic coating uniform texture of acquisition, crystal grain is tiny, in addition, with Ti
2the ceramic layered compound coating for matrix of AlC has conduction, heat conductivility, and has good machining property and from antifriction performance, excellent combination property.
Accompanying drawing explanation
Fig. 1 is with-400 order titanium valves for starting material, take dehydrated alcohol as the process flow sheet that organic solvent prepares Al-Ti-C system reaction powder cored filament material.
Fig. 2 is to react powder cored filament material for spray material, X-ray diffraction analysis (XRD) result of the compound coating utilizing electric arc spraying equipment to prepare.
Fig. 3 is field emission scanning electron microscope (SEM) shape appearance figure of compound coating.A (), (b) are respectively the SEM photo of magnification 200 times and 4000 times lower coatings.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.
Fig. 1 is with-400 order titanium valves for starting material, take dehydrated alcohol as the process flow sheet that organic solvent prepares Al-Ti-C system reaction powder cored filament material.As shown in Figure 1, the present invention prepares Al-Ti-C system reaction powder cored filament material, implements according to the following steps:
Step one: the Ti powder 1150g taking granularity-400 order, purity 99.9%, is placed in sand mill, adds 500ml dehydrated alcohol, 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.Take 342g analytical pure sucrose (titanium valve and sucrose mol ratio are 24:1), dissolve in 200ml distilled water, and sucrose solution is poured in sand mill, continue wet-milling 1 hour, mixture is stirred.
Step 2: mixture is poured into be lined with aluminium-foil paper (preventing from being mixed into impurity) 3 pallets in, the baking oven being placed in 105 DEG C is dried, (during oven dry, baking oven keeps ventilating for dehydrated alcohol in removal mixture and water, prevent the dehydrated alcohol volatilized from assembling in baking oven, cause detonation); Solid materials after drying is broken into bulk, is placed in the vacuum heat treatment furnace (vacuum tightness 2.5Pa) of 220 DEG C, makes the sucrose carbonization (C in solid materials
12h
22o
11→ 12C+11H
2o
1), carbonization time 2 hours, forms Ti-C mixed system.
The unformed charcoal generated due to titanium valve in Ti-C mixed system and sucrose carbonization all has very high activity, strictly must control carbonization temperature (must not higher than 230 DEG C), prevent carbonization temperature too high, cause mixed system that SHS reaction occurs during carbonization.
Step 3: utilize pulverizer that the block Ti-C mixture after carbonization is broken, sieves out Ti-C composite powder within the scope of+400 ~-150 orders as powder core material.
Step 4: using the aluminium strip of width 10mm, thickness 0.2mm be skin material, Ti-C composite powder as powder core material, adopt the continuous hot candied tube reducing method of multiple tracks to manufacture Al-Ti-C powder cored filament material, by silk material diameter by 3.2mm successively tube reducing 0.1mm to 2.8mm.
Below use electric arc spraying equipment to carry out spray test, with experimental data checking, the Al-Ti-C system utilizing the present invention to prepare reaction powder cored filament material is spray material, can prepare Ti
2alC base composite ceramic coating.Electric arc spraying equipment is the automatic high-speed arc spraying system based on Motoman robot controlling, and spraying matrix is the 45 steel plane plate specimens of 40mm × 40mm × 5mm, and spraying parameter is set as follows shown in table.Before spraying, sample is through sandblasting.
| Spray voltage/V | Spray distance/mm | Atomization pressure/MPa |
| 30 | 150 | 0.6 |
Fig. 2 is X-ray diffraction (XRD) analytical results of the composite ceramic coat prepared under above-mentioned processing condition.As can be seen from the figure, in the XRD result of coating, do not have Ti, Al peak to occur, spray material complete reaction all in spraying process is described.Coating is primarily of Ti
2alC, TiC
0.2n
0.8and Al
2o
3deng ceramic phase composition, form multicomponent composite ceramic coat.Wherein, Ti
2alC is that Ti, Al, C three reacts generation; Al
2o
3for the oxygen reaction in Al and air generates; TiC
0.2n
0.8for the sosoloid that the TiC (Ti, C react generation) that generates in spraying process and TiN (in Ti and air, nitrogen reacts and generates) are formed.Demonstrate the reaction powder cored filament material utilizing the present invention to prepare and can prepare Ti
2alC base composite ceramic coating.
Fig. 3 is field emission scanning electron microscope (SEM) photo of coating.Wherein Fig. 3 (a), (b) are respectively the SEM photo of magnification 200 times and 4000 times lower coatings.As can be seen from the figure, coating structure is tight, and homogeneous microstructure, crystal grain is tiny.Show the distortion of composite ceramics molten drop on base material of Reactive Synthesis, sprawl in good condition, the composite ceramic coat defect of formation is less.
Following table is the Main Mechanical test result of composite ceramic coat.Wherein, utilize Wilson microhardness instrument to measure the microhardness of coating, test load 200g, loading time 15s, get the Vickers' hardness of 10 test point mean values as coating; Young's modulus utilizes Nano Indenter XP multifunctional nano impress tester to measure, test parameter: maximum depth of indentation 500 μm, and ultimate load 600mN, gets 5 groups of samples and measure the Young's modulus of mean value as coating; The wear resisting property of coating and matrix 45 steel measures on UMT-2 friction wear testing machine, test parameter: load 100N, time 30min, frequency 10Hz; Corresponding abrasion loss utilizes the three-dimensional white light interference surface topographic apparatus fo of Phase Shift MicroWav-3D observe and calculate, and gets 3 groups of samples and measures the abrasion loss of mean value as coating.Data show, under the same terms, the abrasion loss of composite ceramic coat is only nearly 1/9 of body material, show the Ti prepared
2alC base composite ceramic coating significantly improves the wear resisting property of material.
| Vickers' hardness/HV0.2 | Young's modulus/GPa | Abrasion loss (coating)/mm 3 | Abrasion loss (45 steel)/mm 3 |
| 1125±189 | 352±47 | 3.8±0.7 | 33.6±0.5 |
Claims (3)
1. a preparation method for Al-Ti-C system reaction powder cored filament material, is characterized in that, complete according to the following steps:
1) take titanium valve as reaction starting material, with sand mill wet-milling in organic solvent medium; Take sucrose, be dissolved in distilled water and form sucrose solution, add in above-mentioned material and continue wet-milling, stirring 1 hour, form mixed slurry; The molar ratio range of titanium valve and sucrose is 22:1 ~ 26:1;
2) pour mixed slurry into container, the baking oven being placed in 105 ~ 110 DEG C is dried, and removes the organic solvent in mixture and water; Solid materials after drying is broken into bulk, is placed in the vacuum heat treatment furnace of 220 ~ 225 DEG C, makes the sucrose carbonization 1-2 hour in solid materials, form Ti-C mixed system;
3) utilize pulverizer that the block Ti-C mixture after carbonization is broken, sieve out Ti-C composite powder within the scope of+400 ~-150 orders as powder core material;
4) take aluminium strip as skin material, above-mentioned Ti-C composite powder is powder core material, adopts the continuous hot candied tube reducing method of multiple tracks to manufacture Al-Ti-C powder cored filament material.
2. Al-Ti-C system reacts the preparation method of powder cored filament material according to claim 1, it is characterized in that: the titanium valve chosen is that particle diameter is less than 250 object fine powders, and the wet-milling time is 1 ~ 24h.3, Al-Ti-C system reacts the preparation method of powder cored filament material according to claim 1, it is characterized in that: organic solvent medium is dehydrated alcohol or acetone.
3. Al-Ti-C system reacts the preparation method of powder cored filament material according to claim 1, it is characterized in that: the aluminium strip width 10 ~ 14mm, the thickness 0.2 ~ 0.3mm that choose, the silk material diameter Ф 2.0 ~ 3.0mm of preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109957757A (en) * | 2019-04-04 | 2019-07-02 | 中国核动力研究设计院 | A kind of method of two-step method PVD technique preparation super thick Ti-Al-C ternary coating |
| CN111451490A (en) * | 2020-05-25 | 2020-07-28 | 华中科技大学 | Metal type powder core wire material and preparation method and application thereof |
| CN111690892A (en) * | 2020-07-09 | 2020-09-22 | 长沙理工大学 | Preparation method of MAX phase-based coating |
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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 |
-
2015
- 2015-05-31 CN CN201510290928.2A patent/CN104988448B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 刘宏伟等: "自反应电弧喷涂复相陶瓷涂层工艺研究", 《装甲兵工程学院学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109957757A (en) * | 2019-04-04 | 2019-07-02 | 中国核动力研究设计院 | A kind of method of two-step method PVD technique preparation super thick Ti-Al-C ternary coating |
| CN111451490A (en) * | 2020-05-25 | 2020-07-28 | 华中科技大学 | Metal type powder core wire material and preparation method and application thereof |
| CN111690892A (en) * | 2020-07-09 | 2020-09-22 | 长沙理工大学 | Preparation method of MAX phase-based coating |
| 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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