CN101148749A - Ti-Fe-Ni-C series reaction thermal spraying composite powder and preparation technique thereof - Google Patents
Ti-Fe-Ni-C series reaction thermal spraying composite powder and preparation technique thereof Download PDFInfo
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Abstract
The present invention is one kind of composite hot sprayed Ti-Fe-Ni-C powder capable of forming composite TiC/Fe-Ni alloy coating and its preparation process. The composite Ti-Fe-Ni-C powder containing Ni in the amount of 32-45 wt% of Fe+Ni content and Ti+C in over 70 wt% is prepared with sucrose as the precursor of C. The TiC/Fe-Ni alloy coating formed through hot spraying with Fe-Ni alloy as the adhering phase has the advantages of small stress, low porosity, high bonding strength between the Fe-Ni alloy and TiC, excellent high temperature antiwear and anticorrosion performance and small TiC grain size.
Description
Technical field
The invention belongs to metal material field, particularly a kind of Ti-Fe-Ni-C series reaction thermal spraying composite powder and preparation technology thereof are used for TiC/Fe-Ni alloy compound coating.
Background technology
Ceramic/metal compound coating, especially carbide/metal composite coating have the excellent abrasive energy, and civilian and national defense industry field has purposes widely in metallurgy, the energy, petrochemical complex, automobile, aerospace etc.Research and development high-quality, efficiently, ceramic/metal compound coating technology of preparing is one of most active research topic of high-abrasive material and Surface Engineering field in recent years always cheaply.The performance of ceramic/metal compound coating is main relevant with preparation technology of coating with wild phase, bonding phase.
Aspect wild phase, with WC and Cr commonly used in traditional ceramics/metal composite coating
3C
2Ceramic phase is compared, TiC thermostability better (1100 ℃ are not decomposed yet), hardness and antioxidant property are higher, and density is low, frictional coefficient is little, the ideal that is the ceramic/metal compound coating strengthens body, by bonding phase metal (alloy) is designed, can also make coating have both performances such as high temperature resistant, corrosion-resistant, wear-resistant, have higher using value and application prospect widely.
Aspect the bonding phase, elemental metals or alloy, Co for example, Fe, Ni, Ni-Cr, Fe-Cr-Al and Fe-Al etc., it is the bonding phase of generally using in the present ceramic/metal compound coating, but they can not satisfy the requirements at the higher level of coating for bonding phase performance: 1) thermal expansivity of ceramic/metal compound coating bonding phase should be approaching with ceramic enhancement phase, otherwise can produce the influence of two aspects: on the one hand, metal sticking is bigger with the volumetric shrinkage gap that ceramic enhancement phase produces during deposited coatings, cause to produce fine crack between the interface, the coating unrelieved stress is big, porosity increases, and coating internal bond strength and wear and corrosion behavior descend; On the other hand, the whole volumetric shrinkage that produces of process of cooling floating coat is bigger, and may be because of thermal stresses cracks between the spraying substrate, even comes off, thereby coating and significantly reduction of high base strength, and can not prepare thicker coating.2) wear-resisting and high-temperature behavior is the important performance indexes of ceramic/metal compound coating, this just requires the coating bonding to have good wear resistance and high-temperature oxidation resistant erosion resistance mutually, otherwise coating bonds in actual applications and is easy to earlier destroyedly mutually, causes coming off of ceramic phase, and whole coating lost efficacy.At present, Cr3C2/Ni-Cr and Cr3C2/Fe-Cr-Al etc. is the high-temperature wear resistant coating of using always, but Cr3C2 will decarburization under comparatively high temps, has limited the use of coating under higher temperature.3) the relative ceramic phase of bonding will have good wettability, and ceramic phase particles just is not easy to assemble grows up, but the work-ing life of wild phase ability uniform distribution and significant prolongation coating.Bonding phase problem becomes the bottleneck that restriction ceramic/metal composite coating improves, and studies self to have good Wear-resistant, high-temperature resistant performance, and mates good bonding mutually with ceramic phase heat, can effectively widen the application prospect of ceramic/metal compound coating.
Aspect the preparation technology of coating, hot-spraying techniques is the important method of efficient production ceramic/metal compound coating.During traditional hot spraying preparation ceramic/metal compound coating, the carbide wild phase adopts usually and adds the compound mode in advance in spraying starting material (powder, silk material etc.), ceramic phase skewness in the coating, particle are thick, and ceramic/metal bonding interface vulnerable to pollution influences coating performance greatly.The reaction thermal spraying technology is the type coating technology of preparing that development in recent years is got up, it combines the reaction in synthetic technology of material with traditional hot-spraying techniques, utilize in the spraying process reaction original position synthetic coating material between the spray material constituent element and be deposited as coating simultaneously, thereby one step of synthetic and deposition of coated material is finished.Compare with the traditional hot spraying technology, the reaction thermal spraying technology has following characteristics: 1) can utilize the exothermic heat of reaction between constituent element in the spraying process to increase substantially the temperature of paint particles, reduce coating porosity, improve coating and the combination that bonds mutually; 2) coated material (ceramic phase with metal bonding mutually) is synthetic by the reaction original position between spraying starting material constituent element, ceramic phase particles tiny (can reach nano level), is evenly distributed and the interface cleaning, helps improving the weave construction of coating; 3) because spray material self heat release that responds in the spraying process, and hard is synthetic for reaction in mutually, can reduce the degree of dependence of spraying process to thermal source greatly, makes the common flame plating of application just can obtain fine ceramic/metal compound coating; 4) coated material system utilizes cheap starting material reaction in synthetic, can reduce cost significantly etc.The shortcoming of ceramic coated/metal composite coating technology that reaction thermal spraying has overcome traditional hot has incomparable advantage aspect the preparation ceramic/metal compound coating.Simultaneously because titanium is accompanied by a large amount of heat release (43.85 kcal/mol), synthetic mutually single with the synthetic TiC of carbon reaction, and the synthetic TiC of original position can reduce the wettability requirement to bonding phase metal (alloy) to a certain extent, therefore, the TiC/ metal composite coating is considered to one of typical coating that is suitable for reaction thermal spraying, and reaction thermal spraying also is considered to obtain the most potential method of high-quality TiC/ metal composite coating.
But, no matter analyze from the principle of reaction thermal spraying, still from the actual effect of existing research, the granulation technique of dusty spray is the key that obtains high quality reaction thermal spraying coating.At present, the powder method of granulating that is adopted when compound coatings such as reaction thermal spraying TiC/ metal all is to add Chemical Felter to granulate both at home and abroad, reaction constituent element particle separate easily causes the system reaction not exclusively under high temperature, the effect of high speed flame stream, and coating quality is relatively poor and stable inadequately.How guaranteeing to react between constituent element fully by powder process, reaction is a difficult problem of powdered reaction technical field of hot always.
Preparation problem at reaction thermal spraying composite powder, " Study of TiC/Fe metal ceramic composite coatingby reactive flame spray " (China YouSe Acta Metallurgica Sinica, 2004, Vol (14) 8, p1389～1393) propose to utilize pitch to prepare the higher Ti-Fe-C series reaction thermal spraying composite powder of raw material powder bonding strength as the presoma of carbon, can effectively solve the isolating problem of raw material powder in the spraying process (reaction constituent element particle), prepare TiC/Fe compound coating with excellent abrasive resistance.But because the pitch complicated component, carbonization temperature height (about 600 ℃) is unfavorable for the easily adding of the alloying element of oxidation under the hot conditions, is not suitable for preparing the more compound coating of alloying element, and this will influence the composition design of coating and widening of product category.
This seminar is in " a kind of titanium-nickel-carbon reacting spraying composite powder and preparation technology thereof " (patent publication No.: CN1614072A), proposed sucrose and prepared the Ti-Ni-C series reaction thermal spraying composite powder as the presoma of carbon.The adding that sucrose heat of carbonization decomposition temperature is low, be easy to alloying element, composition is simple, it is little to pollute in the carbonization process, the composite powder bonding strength height of preparation.But, contain oxygen element in the sucrose, in the composite powder preparation process sucrose heat of carbonization decompose the O element discharge be easy to powder in Ti exothermic oxidation reaction takes place and cause the reaction of Ti and C, in composite powder, generate TiC and titanyl compound impurity.Present carbonization technique can only prepare the composite powder of the total content of Ti, C element less than 53wt%, otherwise owing to sucrose content in the mixed powder is too high, exothermic oxidation reaction can't be avoided in the carbonization process.TiC wild phase content is less in the coating of the composite powder spraying back deposition gained of low Ti, C content, and much smaller than the ceramic phase volume ratio of WC/Co wear-resistant coating about 90% commonly used, abrasion property is not high.It is the system composition design of presoma preparation feedback thermospray composite powder with sucrose that original carbonization technique has limited greatly, is unfavorable for using the performance of the prepared coating of this powder to improve.
Summary of the invention
The present invention seeks to develop a kind of high performance alloys suspension that is used for compact disk laser reading head.Improve sensitivity, further strengthen the tracking characteristic.
A kind of Ti-Fe-Ni-C series reaction thermal spraying composite powder and preparation technology thereof mainly comprise two aspects:
(1) at first be the Ti-Fe-Ni-C series reaction thermal spraying composite powder, it is characterized in that: with TiFe powder, Ti powder, Fe powder, Ni powder is raw material, and sucrose is the presoma of carbon; The mass percent that nickel content in the composite powder accounts for iron, nickel total content is 32%～45%; The one-tenth of composite powder is grouped into by mass percentage, Ti:15%～60%; Fe:15%～50%; Ni:10%～30%; C:4%～15%.
(2) secondly be the technology of preparation Ti-Fe-Ni-C series reaction thermal spraying composite powder, comprise raw material powder particle size, the batch mixing oven dry, charging thickness, holding temperature and time, temperature rise rate etc. in the carbonization process, it is characterized in that: 1) utilize the presoma of sucrose as carbon, TiFe powder (2～10 μ m), Ti powder (2～10 μ m), Ni powder (2～5 μ m), Fe powder (2～5 μ m) and sucrose mix wet-milling by proportioning, and the mass percent of sucrose is 10%～35%; 2) slurry that mixes was dried 4～12 hours in 45～60 ℃ of scopes; 3) the block mixed powder after the slurry oven dry is packed in the heat treatment furnace of nitrogen protection, charging thickness is 2～10cm; 4) adopt three holding stages that the sucrose heat of carbonization is decomposed: 200～250 ℃ are incubated 1～2 hour; 300 ℃ are incubated 0.5～1 hour; 350 ℃ are incubated 0.5～1 hour.5) adopt different heating rate to be warming up to each holding stage: the heating rate with 10～15 ℃/min is warming up to 200～250 ℃; Heating rate with 7～10 ℃/min is warming up to 300 ℃; Heating rate with 4～7 ℃/min is warming up to 350 ℃.
The principal feature of this Ti-Fe-Ni-C series reaction thermal spraying composite powder just is to design the powder composition, and to make spraying back gained coating be TiC/Fe-Ni alloy compound coating, in the hope of satisfying the ceramic/metal compound coating to bonding phase performance demands.Experimental study shows: 1) the coating bonding after the spraying of this Ti-Fe-Ni-C series reaction thermal spraying composite powder is the Fe-Ni alloy mutually.The thermal expansivity of Fe-Ni alloy and TiC ceramic enhancement phase differs very little on the one hand, metal sticking is better with the hot matching of ceramic enhancement phase during deposited coatings, two-phase is shunk evenly, the interface shrinkage cavity is few, unrelieved stress is little, and coating densification, porosity are low, internal bond strength and wear and corrosion behavior improve; On the other hand, the Fe-Ni alloy has low thermal expansivity, and very little in the whole volumetric shrinkage that produces of spraying process of cooling floating coat, thermal stresses is little between coating and spraying matrix, bonding strength is high, can prepare thicker coating.2) in the coated material after the composite powder spraying, TiC ceramic phase frictional coefficient is little, wear resistance good, high-temperature stability obviously is better than WC and Cr
3C
2Ceramic phase, the Fe-Ni alloy bonding also has wear-resisting, the anti-oxidant and corrosion resistance of good high-temperature mutually simultaneously, and the high-temperature behavior of TiC/Fe-Ni alloy compound coating must be better than general high temperature wearable anti-corrosion coating.3) the Fe-Ni alloy is good to TiC ceramic phase wettability in the composite powder spraying process, and the TiC particle is difficult for assembling grows up, and can obviously reduce the appearance of larger particles TiC aggregate.The tiny TiC particle that TiC is evenly distributed and exists a large amount of disperses to distribute in the prepared TiC/Fe-Ni alloy compound coating has improved the abrasion property energy greatly.
Original is the composite powder that the carbonization technique of the precursor preparation feedback hot spray powder of carbon can not prepare high Ti, C content with sucrose, trace it to its cause: when sucrose content is higher in the mixed powder, if processing condition can not effectively be controlled sucrose carbonization pyrolysated speed and ensure the sufficient loss of degradation production, just will inevitably the initiated oxidation thermopositive reaction behind a certain amount of oxygen element of gathering in the mixed powder.The present invention has carried out significant improvement to original carbonization technique process when preparation Ti-Fe-Ni-C series reaction thermal spraying composite powder: 1) strict control charging thickness is between 2～10cm.2) adopt three holding stages: 200～250 ℃ are incubated 1～2 hour; 300 ℃ are incubated 0.5～1 hour; 350 ℃ are incubated 0.5～1 hour.3) adopt different heating rate to be warming up to each holding stage: the heating rate with 10～15 ℃/min is warming up to 200～250 ℃; Heating rate with 7～10 ℃/min is warming up to 300 ℃ again; Heating rate with 4～7 ℃/min is warming up to 350 ℃ at last.4) heat of carbonization decomposition course of sucrose is all finished under nitrogen protection, compares with original process using argon shield, has reduced cost.After carbonization was finished, gained porous block solid furnace cooling and with its fragmentation, screening was prepared the reaction thermal spraying composite powder that requires granularity.
Evidence: the carbonization technique after the improvement can prepare Ti, C content and be higher than the above composite powder of 70wt%, behind the powder spraying in the gained coating TiC wild phase content can significantly improve, coating abrasion performance increases significantly.The design that is improved to the reaction thermal spraying composite powder system of carbonization technique, the further raising of coating performance is laid a good foundation.
Compared with prior art, the invention has the advantages that:
1, Zhi Bei Ti-Fe-Ni-C series reaction thermal spraying composite powder forms the carbon clad structure around raw material powder, make the cohesive strength height of raw material powder and carbon, and not easily separated in spraying process, what help reacting finishes.
2, the carbonization technique after the improvement can prepare Ti, the higher reaction thermal spraying composite powder of C content, and TiC wild phase content can reach more than the 70wt% in the TiC/ metal composite coating of spraying back.
3, the coating bonding after the spraying of Ti-Fe-Ni-C series reaction thermal spraying composite powder is the very little Fe-Ni alloy of thermal expansivity mutually, and the coating unrelieved stress is little, porosity is low, coating is inner and coating and spraying high base strength height; Fe-Ni alloy and TiC wetting behavior are better, have reduced the appearance of larger particles TiC aggregate, and coating structure is even.
4, utilize the high-temperature wearable stability of the anti-corrosion oxidation-resistance of high temperature of Fe-Ni alloy in the TiC/Fe-Ni alloy compound coating of composite powder preparation and TiC all very excellent, coating can have the good high-temperature wear and corrosion behavior.
Description of drawings
Fig. 1 is a Ti-Fe-Ni-C series reaction thermal spraying composite powder structure photo.
Fig. 2 is a Ti-Fe-Ni-C series reaction thermal spraying composite powder XRD figure spectrum.
Fig. 3 is the TiC/Fe-Ni compound coating back scattering pattern that utilizes the plasma spraying preparation.
Fig. 4 utilizes equally distributed tiny TiC particle photo in the TiC/Fe-Ni compound coating of plasma spraying preparation.
Fig. 5 is an XRD figure spectrum of utilizing the TiC/Fe-Ni compound coating of plasma spraying preparation.
The reaction thermal spraying composite powder that can see preparation from Fig. 1 (Ti-Fe-Ni-C series reaction thermal spraying composite powder structure photo) has formed carbon and has been coated on clad structure around the tiny material powder, the adhesion strength of material powder and carbon is high, not easily separated in spraying process, what be conducive to react finishes; Can see from Fig. 2 (Ti-Fe-Ni-C series reaction thermal spraying composite powder XRD collection of illustrative plates), adopt sucrose as presoma, not contain any other impurity in the composite powder of the carbonization technique preparation after the improvement; Can see that from Fig. 3 (the TiC/Fe-Ni composite coating back scattering pattern of plasma spraying preparation) coating that obtains has typical thermal spraying lamellar structure, it is less that TiC assembles lamella in the coating, and tissue evenly; Fig. 4 is equally distributed tiny TiC particle photo in the TiC/Fe-Ni composite coating of plasma spraying preparation, and the Fe-Ni alloy is good to the TiC wetability, in conjunction with closely, and TiC is evenly distributed; Fig. 5 is the XRD collection of illustrative plates of the TiC/Fe-Ni composite coating of plasma spraying preparation, and institute's coating composition that obtains is simple, only by TiC and (Fe-Ni) two phase compositions, generates without other impurity phase.
Embodiment
Raw material powder of the present invention is TiFe powder, Ti powder, Ni powder, Fe powder and sucrose, and prepared Ti-Fe-Ni-C series reaction thermal spraying composite powder composition is as shown in table 1, and its concrete technical process is:
1) TiFe powder (2～10 μ m), Ti powder (2～10 μ m), Ni powder (2～5 μ m), Fe powder (2～5 μ m) and sucrose mix by proportioning;
2) mixed raw material powder wet-milling 24～72 hours on ball mill, the volume ratio of used steel ball and raw mix is 4: 1, and drum's speed of rotation is 120rpm, and ball-milling medium is an alcohol;
3) slurry that mixes behind the ball milling was dried 4～12 hours in 45～60 ℃ of scopes;
4) the block mixed powder after the slurry oven dry is put into the heat treatment furnace of nitrogen protection, charging thickness is 2～10cm;
5) feed nitrogen protection 5～10 minutes earlier, flow is 5～15ml/min, so can begin heating again;
6) elder generation is warming up to 200～250 ℃ of insulations 1～2 hour with the heating rate of 10～15 ℃/min, heating rate with 7～10 ℃/min is warming up to 300 ℃ of insulations 0.5～1 hour again, and the heating rate with 4～7 ℃/min is warming up to 350 ℃ of insulations 0.5～1 hour at last;
7) stop heating, furnace cooling is cooled to 100 ℃ under nitrogen protection, close nitrogen, treats to take out blocky composite powder to room temperature;
8) the porous block solid that obtains after the carbonization is carried out fragmentation, screening, prepare the reaction thermal spraying composite powder that requires granularity.
Table 1 has provided the several preferred embodiments that the Ti-Fe-Ni-C series reaction thermal spraying composite powder that utilizes the present invention to prepare passes through plasma spraying depositing Ti C/Fe-Ni alloy compound coating:
Table 1
| Preferred embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
|
Embodiment 6 | Embodiment 7 | |
| Ti-Fe-Ni-C series reaction thermal spraying composite powder composition | The mass percent of Ti (%) | 17.96 | 33.60 | 47.82 | 56.00 | 33.60 | 33.60 | 33.60 |
| The mass percent of Fe (%) | 49.63 | 37.12 | 25.75 | 19.20 | 39.44 | 33.64 | 31.90 | |
| The mass percent of Ni (%) | 27.92 | 20.88 | 14.48 | 10.80 | 18.56 | 24.36 | 26.10 | |
| The mass percent of C (%) | 4.49 | 8.40 | 11.95 | 14.00 | 8.40 | 8.40 | 8.40 | |
| The mass percent (%) that sucrose adds | 12.50 | 21.70 | 29.09 | 32.97 | 21.70 | 21.70 | 21.70 | |
| Coating bonding phase | Fe36Ni | Fe36Ni | Fe36Ni | Fe36Ni | Fe32Ni | Fe42Ni | Fe45Ni | |
| Coating hardness (HR15N) | 73.20 | 89.50 | 93.40 | 102.50 | 91.00 | 88.20 | 87.30 | |
| Anchoring strength of coating (all from the glue-line fracture) | ＞62.31 (MPa ) | ＞62.31 (MPa ) | ＞62.31 (MPa ) | ＞62.31 (MPa ) | ＞62.31 (MPa ) | ＞62.31 (MPa ) | ＞62.31 (MPa ) | |
| Coating porosity (%) | 1.10 | 1.40 | 1.60 | 1.90 | 1.20 | 1.60 | 2.1 | |
| Coating relative wear resistance (comparing) (doubly) with conventional Ni60 coating | 4.20 | 7.90 | 12.00 | 14.60 | 9.00 | 7.80 | 7.30 | |
Claims (2)
1. Ti-Fe-Ni-C series reaction thermal spraying composite powder, it is characterized in that: with TiFe powder, Ti powder, Fe powder, Ni powder is raw material, sucrose is the presoma of carbon; To account for the mass percent of iron, nickel total content be 32%～45% to nickel content in the composite powder; The one-tenth of composite powder is grouped into by mass percentage, Ti:15%～60%; Fe:15%～50%; Ni:10%～30%; C:4%～15%.
2. the technology of preparation Ti-Fe-Ni-C series reaction thermal spraying composite powder comprises raw material powder particle size, the batch mixing oven dry, and charging thickness, holding temperature and time in the carbonization process, temperature rise rate is characterized in that:
1) utilize the presoma of sucrose as carbon, TiFe powder (2～10 μ m), Ti powder (2～10 μ m), Ni powder (2～5 μ m), Fe powder (2～5 μ m) and sucrose mix wet-milling by proportioning, and the mass percent of sucrose is 10%～35%;
2) slurry that mixes was dried 4～12 hours in 45～60 ℃ of scopes;
3) the block mixed powder after the slurry oven dry is packed in the heat treatment furnace of nitrogen protection, charging thickness is 2～10cm;
4) adopt three holding stages that the sucrose heat of carbonization is decomposed: 200～250 ℃ are incubated 1～2 hour; 300 ℃ are incubated 0.5～1 hour; 350 ℃ are incubated 0.5～1 hour;
5) adopt different heating rate to be warming up to each holding stage: the heating rate with 10～15 ℃/min is warming up to 200～250 ℃; Heating rate with 7～10 ℃/min is warming up to 300 ℃; Heating rate with 4～7 ℃/min is warming up to 350 ℃.
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| CN102166652A (en) * | 2011-03-30 | 2011-08-31 | 北京科技大学 | Preparation method of titanium carbide-based cermet powder material for thermal spraying |
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| CN110434327A (en) * | 2019-08-29 | 2019-11-12 | 西安交通大学 | A kind of reproducible great friction coefficient wear-resistant coating of high roughness and preparation method thereof |
| CN111593289A (en) * | 2020-05-22 | 2020-08-28 | 有研资源环境技术研究院(北京)有限公司 | Corrosion-resistant coating for aluminum electrolysis temperature thermocouple and preparation method thereof |
| CN112479744A (en) * | 2020-11-27 | 2021-03-12 | 北京工业大学 | Method and device for preparing active metal connecting layer on surface of carbon fiber reinforced silicon carbide composite material matrix |
| CN113894461A (en) * | 2021-10-12 | 2022-01-07 | 广州汉源新材料股份有限公司 | Glass-based sealing composition, sealing slurry, and preparation method and application thereof |
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