CN101152776B - Double -gradient composite coating - Google Patents
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- CN101152776B CN101152776B CN200610032331A CN200610032331A CN101152776B CN 101152776 B CN101152776 B CN 101152776B CN 200610032331 A CN200610032331 A CN 200610032331A CN 200610032331 A CN200610032331 A CN 200610032331A CN 101152776 B CN101152776 B CN 101152776B
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Abstract
The invention discloses a dual-gradient composite coating. A coating which is arranged on the surface of a basal body consists of a plurality of sub-coatings, which forms a shock wave moving gradient.The shock wave moving gradient is compounded by two simultaneously existing gradients--a composition gradient and a composition wave centre-value gradient. Every sub-coating consists of two composition gradients with opposite composition changing trends. The composition changing trends of adjacent sub-coatings are similar. From the basal body to the surface, the composition medium value which forms gradient composition in adjacent sub-coatings also changes in gradient, namely the composition wave centre-value gradient. The combined effect of multiple coatings and the designing ability of gradient coating are used, and the dual-gradient coating is arranged on the surface of metal, inorganic non-metallic, polymer and composite and other solid materials. Compared with the ordinary gradient coating, the present invention has the advantage of smaller thermal stress, better thermal stability, high thermal shock resistant ability, no significant macro cracks and good connection performance with the basal body.
Description
Technical field the present invention relates to a kind of high-performance composite coating that is coated on matrix surfaces such as solid metallic, inorganic non-metallic, macromolecule and composite thereof, be mainly used in the protection of material and increase new function, self-defects such as the residual stress of minimizing coating, crackle, improve the heat endurance of coating and the switching performance of coating and matrix, increase the service life.
In the later stage eighties 20th century of background technology, after Japanese scientist had proposed " FGM (Functionally Gradient Materials, FGM) " this notion, the science and technology of FGM just became the focus that receives much concern.FGM is the continuous or quasi-continuous variation of a class by structure and element, comes obtained performance corresponding to the variation of structure and composition and the heterogeneous body composite of gradual change.The emphasis of FGM research mainly concentrates on the FGM of preparation thermal stress mitigation type, in recent years, gradient distribution no longer is confined to the thermal stress alleviating function as a kind of design philosophy and structure control method of material, and it all is being with a wide range of applications aspect the structural material such as wear-resisting, heat-resisting, corrosion-resistant.
In the multiple application of FGM; the FGM coating has unique value; in this technology; the gradient skin is deposited upon on the prefabricated big module component; play the optimization transitional function between big module component and external skin, the remainder of coating protection member avoids being subjected to the effect of the outside abominable conditions such as temperature, corrosion or wearing and tearing of member.The gradient coating The Application of Technology more and more widely, become material protection, improve performance and increase the effective means of new aspects such as function.The method for preparing the functionally gradient material (FGM) coating mainly comprises vapour deposition process, plasma spraying method, powder thermospraying method, laser melting coating synthetic method, composite electrodeposition method etc.
Although gradient coating and multi-layer composite coatings technology have relaxed thermal stress, effectively improved the compatibility of coating and matrix, improved the performance and the life-span of coating and goods, the application that engineering is used under the harsh and unforgiving environments particularly is often still unsatisfactory.Thermal Barrier Coatings is the very fast also coatings art of successful Application of development in recent years, still has the thermal expansion matching problem.Although the researcher improves heat-barrier coating heat-shock resisting performance, antioxygenic property and service life by gradient coating, gradient coating+transition zone methods such as (or claiming cushion), the problem of the thermal mismatching between coating and transition zone (thermal growth oxide), matrix remains the key factor that influences heat barrier coat material heat-mechanical property and durability.The inefficacy of thermal barrier coating is the oxidation under the high temperature and the result of thermal cycle load comprehensive function normally.Failure mode mainly is peeling off of coating and chaps two kinds, and defective pattern then is due to the propagation of expansion, combination and big crackle of micro-crack.The main cause that thermal barrier coating peels off is a stress influence in the thermal cycle process, comprises the stress that do not match thermal stress, coating and matrix thermal expansion that temperature gradient distribution causes the thermal growth oxide of the thermal stress that causes, alloy buffer layer forms and transformation stress etc.
Summary of the invention the object of the present invention is to provide a kind of double-gradient composite coating that is coated on solid metallic, inorganic non-metallic, macromolecule and composite material base surface thereof, and this composite coating has low stress, flawless, the good advantage of thermal shock resistance.
The present invention utilizes the complex effect of multi-element coating and the designability of coating, the composite coating that goes out to have two kinds of gradients of composition gradient and composition ripple central value gradient in the surface preparation of solid materials such as metal, inorganic non-metallic, macromolecule and composite thereof.
Technical solution of the present invention is: double-gradient composite coating, form by a plurality of sub-coatings in the coating of matrix surface, and constitute the gradient of concussion fluctuation, this gradient is by simultaneous two kinds of gradients---and composition gradient and composition ripple central value gradient are composited; Each sub-coating all has two kinds of opposite composition gradients of composition variation tendency, the composition gradient variation tendency of adjacent sub-coating is similar, to the surface, the composition mean value that constitutes gradient material in the adjacent sub-coating also has graded, i.e. composition ripple central value gradient by matrix.
The excursion of the peak swing of composition ripple is 0～100%, generally changes better between 5～50%, and the excursion of composition ripple central value gradient is 0～100%.
Coating and matrix are solid materials such as metal, inorganic non-metallic, macromolecule and composite thereof.
From integral body, coating is made of a plurality of sub-coatings with composition ripple, and to the surface, the composition mean value of adjacent sub-coating forms graded, i.e. composition ripple central value gradient by matrix; From the part, each sub-coating all has the version of similar composition ripple, in each sub-coating a kind of composition from high to low, (another kind of composition is then opposite) continuous or quasi-continuous graded more from low to high, form two kinds of composition gradients that version is opposite, but two kinds of version amplitude differences, be that sub-coating composition ripple exists two amplitudes, it is exactly that the composition of composition ripple central value on this sub-coating layer thickness changes size and change direction that peak swing and minimum amplitude exist difference DELTA C and change direction.In brief, double-gradient composite coating is the gradient coating with concussion fluctuation.
Characteristics of the present invention are: 1) kinds of processes can realize the present invention, preparation technology mainly contains technologies such as chemical vapour deposition (CVD), physical vapour deposition (PVD), electrochemical deposition, laser melting coating, high temperature insostatic pressing (HIP), thermal spraying, pricker are coated with, sol-gel technology, brushing technology, sintering, or the compound formation of kinds of processes.2) key issue that is solved is the problem of the mechanical compatibility between coating and matrix, promptly coefficient of expansion mismatch, internal stress big, be prone to crackle, be coated with matrix or other that connectivity of interlayer is poor, the problem of thermal shock resistance difference.3) can increase new function, except that the performance with former gradient coating, two gradient coatings have also increased some new functions, form the bonding strength that strengthens coating and material as bearing stress, and anti-wear performance improves; Two gradient coatings help coating uniform wear or homogeneous corrosion (ablation); Improve the service life of coating.4) widely applicable.
Description of drawings:
The schematic diagram of Fig. 1 double-gradient composite coating; Wherein: the 1-matrix; The coordinate of 2-composition A; The 3-coating; The 4-coating surface; 5-coating layer thickness coordinate; 6-wavelet center; 7-composition A is with the varied in thickness curve; 8-coating;
Fig. 2 has the double-gradient composite coating schematic diagram of multiple variation; Wherein: the 1-matrix; The coordinate of 2-composition A; The 3-coating; The 4-coating surface; 5-coating layer thickness coordinate; 6-wavelet center; 7-composition A is with the varied in thickness curve; 8-coating;
The cross-section morphology SEM photo of Fig. 3 TaC/SiC coating;
The two gradient multilayer TaC/SiC composite coating SEM photos of Fig. 4.
Further specify below in conjunction with schematic diagram:
Fig. 1 is the schematic diagram of double-gradient composite coating of the present invention. Coating on matrix 1 is composited by two kinds of materials of A, B, wherein, substance A be base matter or for the extraordinary material of matrix phase capacitive (as, expansion characteristics is very approaching, chemical compatibility is good), the substance A composition represents that with coordinate 2 B is the another kind of material different from the substance A characteristic. On the thickness direction of coating 3 from matrix surface until the spacing of coating outer surface 4 represent with coordinate 5, for common gradient coating, the composition of coating changes such as Fig. 1 dotted line 6, namely, by the outer surface of matrix surface to coating, the composition of substance A is continuous or quasi-continuously be reduced to 0% by 100%, and the composition of substance B is continuous or quasi-continuously bring up to 100% by 0%. The composition of double-gradient composite coating changes then such as Fig. 1 solid line 7, changes similar sub-coating 8 by several compositions and consists of, and the composition vibrating type fluctuation of coating changes, and is comprising two kinds of gradients. First kind of gradient is local composition gradient, the composition of exactly every sub-coating is continuous or quasi-continuous graded, different from general gradient coating variation tendency is that every sub-coating comprises two opposite variation tendencies, namely falls after rising, or rear liter falls earlier, but the amplitude of lifting is different, and every sub-coating ingredient change amount of each on thickness direction is Δ C, such as Fig. 1, composition A reduces Δ C, and composition B increases Δ C. The second gradient is composition ripple central value gradient, and to the surface, the composition mean value (such as the dotted line among Fig. 1) that consists of gradient material in the adjacent sub-coating also changes in gradient by matrix. Position on composition ripple central value (being composition mean value) and the coating layer thickness direction linearly or curvilinear motion, the excursion of composition ripple central value gradient is 0～100%. The amplitude of sub-coating can be constant, also can change, and the composition excursion is greater than 0%, less than 100%, namely/Δ C can be definite value, also can be changing value. In brief, common gradient coating shows as straight (song) line style gradual change of composition, and two gradient coatings then show as the gradual change of composition fluctuation-type.
Fig. 2 is the double-gradient composite coating schematic diagram that multiple variation is arranged, the composition ripple central value of coating is curve, the shock range of coating and concussion frequency are all changing, can be divided into three districts along the coating layer thickness direction, the sub-coating amplitude that 1. coating is distinguished is little, and thickness is also little, the sub-coating amplitude that 2. coating is distinguished increases, thickness is also bigger, the sub-coating amplitude maximum that 3. coating is distinguished, and thickness is also maximum. These variations can be satisfied different needs.
K
1、K
2For two amplitudes (in %) of coating composition ripple, work as K1＝K
2The time, composition ripple central value is constant, is the sustained oscillation coating; Work as K1＝K
2In the time of=100%, composition is periodic vibration between A, B, is exactly the A/B multi-layer composite coatings; Work as K1＝K
2=0 o'clock, be common gradient coating, composition A drops to 0 by 100%, and B is raised to 100% by 0 simultaneously, otherwise or; As 0＜K1＝K
2, be A-B codeposition cyclic swing coating at＜100 o'clock. Work as K1≠K
2, namely | K1-K
2|=Δ C＞0 o'clock is two gradient coatings; K1、K
2The size of size, Δ C and the thickness of sub-coating be the important indicator of two gradient coatings designs. And the thickness of coating=n Δ C (n is the number of sub-coating). When the thickness of group coating is identical, be equifrequent concussion (such as Fig. 1), the thickness of group coating is the Frequency concussion not simultaneously. When Δ C is definite value, for waiting luffing concussion (1. distinguishing such as Fig. 1, Fig. 2 coating). K1、K
2More big, the composition amplitude of variation in the sub-coating is more big, and Δ C is more big, and it is more few that son is coated with number of layers, and composition ripple central value gradient is more big. Its concrete numerical value will determine according to two aspects, that is, 1) substance A, the corresponding relation of B properity and the composition and structure of A-B codeposition coating, the corresponding relation of performance; 2) environment for use requirement. Basic premise is: guarantee to be lower than in preparation and internally coated residual stress of time limit in service life or internal stress the limit stress of coating material, be lower than simultaneously the bonding strength of coating and matrix.
Compare with common gradient coating, the two gradient coatings of this composition fluctuation-type gradual change have significant advantage: have low internal stress and fluctuation-type and reduce, no Interlaminar Crack and through-wall crack, densification and with matrix bonding strength height, thermal shock resistance is good.
The principle of this excellent specific property is: 1) utilized the variation of composition fluctuation and structure that the inside of whole coating is among the little continuous STRESS VARIATION of STRESS VARIATION amplitude, presented the alternately nonlinear change of concussion of tensile stress, compression. Reduced significantly increasing progressively in the transitive set of ess-strain that the unicity of stress direction causes, thereby can be with Stress Control within the limit stress of material. 2) stress is concentrated be distributed to whole coating. Not only stress, the concentrated interface of should becoming different are separated into and have certain thickness each sub-coating, and by the second heavy gradient stress, ess-strain is distributed to each position of coating. 3) inner actual relative gradient (the gradient rate of coating, be that composition changes and thickness ratio) greater than apparent gradient (also being the relative gradient of common gradient coating), the variation that the composition of a plurality of sub-coatings shakes fluctuation and lattice structure fast also can produce more atom vacancy iso-stress absorption region; Change simultaneously the coefficient of expansion and the elastic modelling quantity of coating material, thereby, structural stress and thermal stress can be reduced. The compression strength that particularly can take full advantage of ceramic material is higher than tensile strength, utilizes two gradient coatings to produce new compression variation tendency, progressively offsets the shortcoming that the coating coefficient of expansion is big, elastic modelling quantity is high. Therefore, coating has the characteristics of low stress, flawless and heat shock resistance.
The specific embodiment:
Embodiment 1: chemical vapour deposition (CVD) prepares in TaC and the SiC composite coating on C/C composite or graphite, and two gradient TaC/SiC composite coatings are low stress, flawless, thermal shock-resistant coating, also is high temperature resistant, anti-oxidant, antiscour, ablative cork coatings.
Because the thermal coefficient of expansion of SiC and TaC is all than C/C composite height, be about 2 times, 4 times of the C/C matrix coefficient of expansion respectively, and the both is the very high fragile material of elastic modelling quantity, single coating on the C/C composite material surface, when surpassing certain thickness, the through-wall crack that dense coating all is prone to.After the MULTILAYER COMPOSITE, the TaC/SiC composite coating is still many greatly than the coefficient of expansion of C/C composite, and TaC is coated with SiC and belongs to chemical bonding being connected of interlayer, the bonding strength height, so after cooling still cracking easily, as TaC during, show the most outstanding on top layer.Fig. 3 is a TaC/SiC composite coating cross-section morphology.Fig. 3-a is no gradient multi-layer composite coatings, TaC and SiC codeposition coating that 15～20 μ m are arranged near matrix, be that thickness in monolayer is TaC and the SiC multi-layer composite coatings separately of 1～5 μ m then, be coated with interlayer and do not carry out gradient transition, EDS shows that the composition of C is highly stable, illustrate that depositing operation control is stable, the composition of Ta and Si is alternately concussion variation fast, shows that the number of plies of TaC/SiC composite coating is many, thickness in monolayer is little.Because the thickness of every individual layer is less, coating is all fine and close aplitic texture, and the connection that respectively is coated with interlayer is tight, is connected finely with matrix, but has some to grow, run through more deeply the face crack of coating, and a spot of interlayer crackle is arranged at the through-wall crack place.The residual stress that this coating is described is still bigger, ftractures in the process of cooling in coating preparation back.Also has the perfoliate crackle of some crackle right and wrong.TaC coating and SiC are coated with interlayer and have coefficient of expansion difference, and certain interlayer internal stress is arranged, also can inducing layer when face crack occurs between crackle occur, and the position of not having a face crack does not generally have the interlayer crackle.
Fig. 3-b is for there being certain interlayer gradient TaC/SiC multi-layer composite coatings.Promptly by a kind of when being coated with the another kind of coating transition of course, the codeposition district that has composition to change is so change shape in coating and color are variation.Composition changes tangible step of appearance at the interface or interlayer crackle greatly, and the contrast of color is also bigger.An outstanding feature of this coating is: coating has face crack, but crackle does not run through whole coating, but is separated into several tiny crackles gradually, and cracks has the interlayer crackle to follow.
Fig. 4 is two gradient multilayer TaC/SiC composite coating SEM photos, the multilayer TaC/SiC composite coating of two gradients be organized as the needle-like aplitic texture, and do not change with the fluctuation and the change of composition.The inner C elementary composition of coating is constant substantially, and from inside to outside, Si elementary composition fluctuation formula increases, and Ta elementary composition fluctuation formula reduces, and shows that inner TaC of coating and SiC have constituted two gradients.Coating is made of the sub-coating of a plurality of structural similarities, and TaC or SiC composition more from high to low, form repeatedly the composition gradient fluctuation alternately from low to high, are similar to sine or cosine function ripple (the composition ripple of no gradient multilayer TaC/SiC composite coating is a standing wave); From inside to outside coating on the whole the composition mean value of TaC, SiC certain gradient is arranged, promptly the central value of TaC composition ripple from high to low, the central value of SiC composition ripple is from low to high.
Repeatedly observe by naked eyes, body formula mirror, ESEM, this pair of gradient coating do not have any cracking obscission, both do not had face crack, do not have the interlayer crackle yet, and be fine with the connectivity of substrate.Thereby this coating process is that flawless is coated with layer model.
Surface residual stress spreads out and measures the TaC/SiC composite coating (Fig. 3-b) surface residual stress is a tensile stress, and size is+12.56MPa, and TaC/SiC coating (Fig. 4) surface residual stress of two gradients is a compression, and size is-7.64MPa with changeing the target X-ray diffraction.Evidence: in TaC and SiC composite coating, anti-oxidant, antiscour, the anti-ablation of the TaC/SiC coating of two gradients are best.
Embodiment 2: carry out Fe on Q235 steel surface
3Al/Al
2O
3The gradient coating plasma spraying is handled, and to improve the performance such as wear-resisting, anti-oxidant of material, thermal shock performance of coatings is the key that prolongs the service life of material.By the appearance of matrix, be prepared into Fe to coating
3Al by 100% be reduced to 0 gradually, Al
2O
3Be increased to 100% gradient coating gradually by 0, when thickness was 80～100 μ m, size 50mm * 50mm sample carried out the thermal shock resistance test, and the number of times that coating shedding occurs is about 110～130 times.The thermal shock resistance test condition: in the box electrothermal furnace under 800 ℃ of temperature conditions, insulation 20minm takes out then, and blowing compressed air is cooled to room temperature, and so circulation obscission occurs up to coating.
Carry out Fe on Q235 steel surface
3Al/Al
2O
3When two gradient coatings are handled, two gradient peak swing k
1=25%, minimum amplitude k
2=15%, the thickness 10 μ m of sub-coating, size 50mm * 50mm sample carry out same thermal shock resistance test, and the number of times that coating shedding occurs is about 650～700 times.Thermal shock resistance improves 5～6 times than gradient coating, all improves with high base strength, non-oxidizability.
Claims (3)
1. double-gradient composite coating, it is characterized in that: the coating at matrix surface is made up of a plurality of sub-coatings, constitutes the gradient of concussion fluctuation, and this gradient is by simultaneous two kinds of gradients---and composition gradient and composition ripple central value gradient are composited; Each sub-coating all has two kinds of opposite composition gradients of composition variation tendency, the composition gradient variation tendency of adjacent sub-coating is similar, to the surface, the composition mean value that constitutes gradient material in the adjacent sub-coating also has graded, i.e. composition ripple central value gradient by matrix;
The excursion of composition ripple central value gradient is 0～100%.
2. double-gradient composite coating according to claim 1 is characterized in that: the composition excursion of sub-coating is 0～100%.
3. double-gradient composite coating according to claim 1 is characterized in that: coating and matrix are metal, inorganic non-metallic, macromolecule and composite thereof.
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| CN106383203B (en) * | 2016-08-31 | 2019-06-25 | 中国建材检验认证集团股份有限公司 | The method for measuring coating elasticity modulus |
| CN108411242B (en) * | 2018-01-31 | 2020-12-18 | 广东省新材料研究所 | Thermal barrier coating with particle erosion resistant surface layer and preparation method thereof |
| CN112374891B (en) * | 2020-11-16 | 2021-11-23 | 南京工业大学 | Graphite base plate surface gradient TaC coating |
| CN113582713B (en) * | 2021-09-29 | 2022-01-28 | 中南大学 | Ceramic coating protective gradient carbon-ceramic composite material and preparation method thereof |
| CN114605173B (en) * | 2022-04-18 | 2023-02-03 | 中南大学 | Ablation-resistant and thermal shock-resistant zirconium silicate-high-alumina glass/HTBS high-entropy ceramic coating and preparation method and application thereof |
| CN114853507B (en) * | 2022-07-06 | 2022-10-14 | 湖南泰坦未来科技有限公司 | Composite carbon material and preparation method and application thereof |
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| JP2001152263A (en) * | 1999-11-18 | 2001-06-05 | Ueda Seni Kagaku Shinkokai | Hybrid functionally gradient material and its manufacturing method |
| CN1302456A (en) * | 1999-04-29 | 2001-07-04 | 赛姆特里克斯公司 | Ferroelectric field effect transistor having compositionally graded ferroelectric material and method of making the same |
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| CN1302456A (en) * | 1999-04-29 | 2001-07-04 | 赛姆特里克斯公司 | Ferroelectric field effect transistor having compositionally graded ferroelectric material and method of making the same |
| JP2001152263A (en) * | 1999-11-18 | 2001-06-05 | Ueda Seni Kagaku Shinkokai | Hybrid functionally gradient material and its manufacturing method |
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