CN105758683A - High-temperature-resistant speckle with high adhesion and preparation method thereof - Google Patents
High-temperature-resistant speckle with high adhesion and preparation method thereof Download PDFInfo
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- CN105758683A CN105758683A CN201610132962.1A CN201610132962A CN105758683A CN 105758683 A CN105758683 A CN 105758683A CN 201610132962 A CN201610132962 A CN 201610132962A CN 105758683 A CN105758683 A CN 105758683A
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Abstract
The invention discloses a high-temperature-resistant speckle with high adhesion and a preparation method thereof.The preparation method includes the steps of S1, mixing substance A, high-temperature-resistant oxide and fluxing agent to form emulsion, wherein the substance A is at least one of silica sol, water and ethanol; S2, coating the emulsion in the step S1 on the surface of a substrate, and then drying the substrate to form an initial speckle; S3, burning the substrate with the initial speckle formed on the surface, and cooling to room temperature to obtain the speckle with high adhesion.The prepared speckle has the advantages that the speckle is resistant to high temperature, less prone to breaking and falling off and high in adhesion with the substrate; the speckle can be coordinated with an image processing algorithm to complete the optical measuring of deformation and mechanical performances of materials under a high-temperature environment and various loading states such as being subjected to stretching, compression and heat impact.
Description
Technical field
The invention belongs to the technical fields such as material, optics manufacture, optical measurement mechanics, be specifically related to strong speckle of a kind of adhesiveness and preparation method thereof.
Background technology
In the parts such as the heavy duty gas turbine in Aero-Space electromotor and the field such as firepower, nuclear energy power generation, the true mechanical property under material at high temperature environment is to evaluate part reliability and assess the important parameter in its life-span.At present, most researcheres utilize in optical measurement mechanics and carry out deformation measurement based on the non-contact measurement method of digital image processing method.Wherein, the speckle of parts surface is the ideal carrier of parts surface deformation, can be known by inference the true strain information of parts surface by the deformation of image processing techniques acquisition speckle.Refractory oxide generally has high intensity, high rigidity, wear-resistant, corrosion-resistant washes away the premium properties such as good with chemical stability, such as the oxide such as aluminium oxide, titanium dioxide in high-temperature field extensive uses such as Aero-Space electromotor, car engines, significantly promote the development of exotic material especially based on the ceramic matric composite of refractory oxide.Therefore, refractory oxide is that the ideal material making high-temperature speckle selects.
Manufacturing method of high-temperature speckle conventional at present has etching method and high-temp glue in conjunction with refractory metal oxide method.Etching method is the method that parts surface has destruction, it is easy to affect thermodynamics and the aeroperformance of parts, and easily lures the destruction of material into, should not adopt for comparatively accurate parts；For high-temp glue in conjunction with refractory metal oxide method, the size of the more difficult control speckle of the method, and the situation that metal-oxide at high temperature comes off easily occurs, the cost that secondly high-temp glue is higher makes the method be confined to the other experiment of laboratory-scale, it is impossible to promote to engineering.
Chinese patent literature CN105043835A discloses the manufacture method of a kind of speckle for high temperature deformation test experiments.It comprises the steps: S1, will mix according to mass ratio 3:1 for the ceramic powders gathered materials and liquid binder with aluminium oxide, and the mixed liquor being mixed to get is carried out uniform treatment；S2, the mixed liquor after uniform treatment is sprayed on tested sample surface；S3, to spraying mixed liquor tested sample be dried process, obtain speckle on the surface of tested sample.
Above-mentioned patent documentation is the ceramic powders gathered materials and liquid binder preparation mixed liquor by selective oxidation aluminum, raw material sources are wide, cost is low, operation is succinct, without the utensil of high accuracy high request and equipment, in addition, owing to the fusing point of aluminium oxide is very high, the speckle therefore made according to this patent documentation is stablized in high temperature environments.But, the speckle matter that above-mentioned patent documentation is prepared by dried is crisp, and the poor adhesion on tested sample surface, when tested sample deforms (as stretched) or flows down heating at high velocity heated gas, it is easy to come off from tested sample surface.
Summary of the invention
It is an object of the invention to solve the speckle of preparation and base material poor adhesion, the technical problem easily come off from its surface when base material deforms in prior art, and then provide a kind of adhesiveness strong and the preparation method of resistant to elevated temperatures speckle.
For this, the technical solution used in the present invention is,
The preparation method of speckle provided by the present invention, comprises the steps:
S1, by substance A, refractory oxide and flux mix, formed emulsion, wherein, described substance A is at least one in Ludox, water, ethanol；
S2, the emulsion in described step S1 is coated on substrate surface, and the substrate after coating emulsion is dried, form initial speckle；
S3, the substrate that surface in described step S2 forms initial speckle are fired, and are cooled to room temperature, obtain the speckle that adhesiveness is strong.
In described step S3, described in fire the temperature of step be 800 DEG C-1200 DEG C, the time is 10-30min.
In described step S1, the mass ratio of described Ludox, described refractory oxide and described flux is 1:(3～6): 1.5.
In described step S1, described refractory oxide is at least one in aluminium oxide, silicon dioxide, titanium dioxide, zirconium oxide.
Described flux is at least one in lead oxide powder, Zinc oxide powder, magnesium oxide powder, sodium oxide powder, lithium oxide powder, lime powder.
In described step S2, the temperature of described drying steps is 40-50 DEG C.
Further, in described step S1, before mixing, the step adding binding agent is also included.
Described binding agent is latex and/or epoxy resin adhesive；The mass ratio of described binding agent and described refractory oxide is 1:(10-20).
In described step S2, described substrate is alloy sheet or stainless steel substrates；Described coating step is at least one in spin coating, spraying, sputtering.
Present invention also offers the speckle prepared by above-mentioned preparation method.
Compared with prior art, there is advantages that
1) preparation method of the speckle that the embodiment of the present invention provides, by least one in Ludox, water, ethanol, mixes with refractory oxide and flux, forms emulsion；Again emulsion is coated on substrate surface, is dried, be initially formed initial speckle；Eventually pass and fire, obtain the speckle that adhesiveness is strong.Make Ludox can become nanosized silica particles by firing; nanosized silica particles can be entrained in prepared speckle; prevent from drying and firing causing speckle matter crisp; and the problem easily come off from its surface when base material deforms, and nanosized silica particles and fire the existence of step and also enhance speckle and base material adhesiveness；And it is good with base material adhesiveness；Meanwhile, water, ethanol can evaporate in the process fired from speckle, make speckle not easily matter crisp, difficult drop-off, and good with base material adhesiveness；
Furthermore, this neighborhood technique personnel think the existence firing step, the fragility of prepared speckle can be increased, thus easily coming off from its surface when base material deforms, but applicant is found by a large amount of creative works, by by least one in Ludox, water, ethanol, combine with firing, creating unforeseeable technique effect, at least one in Ludox, water, ethanol, has also functioned to synergism between refractory oxide and three kinds of components of flux simultaneously.
2) preparation method of the speckle that the embodiment of the present invention provides, is 800 DEG C-1200 DEG C by restricting the temperature firing step, and the time is 10-30min；And the mass ratio of Ludox, refractory oxide and flux is 1:(3～6): 1.5, Ludox is made to convert nanosized silica particles to, and it is uniformly distributed in speckle with refractory oxide and flux, make the speckle prepared not only high temperature resistant, and good toughness, not easily breaking releasing.
3) preparation method of the speckle that the embodiment of the present invention provides, by adding flux, reduces firing temperature, and flux has part volatilization in sintering procedure simultaneously, makes the crisp degree of matter of speckle reduce further.
4) preparation method of the speckle that the embodiment of the present invention provides, making raw material is conventional chemical reagent, less costly, and the surface speckle being capable of structural member extensive, big makes；Manufacturing process is simple, and speckle size is easily controlled, it is possible to meet the requirement of image procossing.
5) speckle that the embodiment of the present invention provides, it has high temperature resistant, good toughness, not easily breaking releasing, strong with base material adhesiveness；Meanwhile, the algorithm of image procossing can be coordinated to complete the optical measurement of deformation and mechanical property under the multiple stress states such as material Tensile, compression, thermal shock under hot environment.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the speckle that a kind of adhesiveness is strong.
Fig. 2 prepares on high temperature alloy sheet in embodiment 1 that adhesiveness is strong and resistant to elevated temperatures speckle pattern.
Fig. 3 be in embodiment 1 speckle in the high temperature test lab diagram of temperature (A) T=1200 DEG C, (B) T=1400 DEG C.
Fig. 4 be in embodiment 1 speckle stretch under different stretch power after speckle pattern, wherein, tensile force from left to right is followed successively by 0 μ ε, 10000 μ ε, 15000 μ ε, 20000 μ ε and 25000 μ ε.
Fig. 5 is the speckle pattern prepared on high temperature alloy sheet in comparative example 2.
Detailed description of the invention
In order to the object, technical solutions and advantages of the present invention are better described, below in conjunction with the drawings and specific embodiments, the present invention is described further.The present invention can be embodied in many different forms, and should not be construed as limited to embodiment set forth herein.On the contrary, it is provided that these embodiments so that the disclosure will be thorough and complete, and the design of the present invention being fully conveyed to those skilled in the art, the present invention will only be defined by the appended claims.
In each embodiment following and comparative example, the experimental technique of speckle high temperature test is as follows: be positioned in quartz lamp heating furnace by surface with the test specimen 1 of speckle, and heating is to 1200 DEG C and is incubated 30min, test specimen is cooled to room temperature afterwards, and observes phenomenon.Again being positioned in quartz lamp heating furnace by test specimen 1 afterwards, heating is to 1400 DEG C and is incubated 30min, test specimen is cooled to room temperature afterwards, and observes phenomenon.After being again positioned in quartz lamp heating furnace by test specimen 1 afterwards, test specimen is cooled to room temperature, and observes phenomenon.
In each embodiment following and comparative example, the experimental technique of extension test (Y-direction strain) is as follows: fired by speckle on the standard tensile test specimen of Inconel751 high-temperature alloy material or stainless steel substrates, afterwards test specimen is arranged on mechanical stretch testing machine and carries out extension test, elongation strain starts Slow loading from 0 μ ε until surface of test piece speckle comes off, captured image recording phenomenon in loading procedure.
Embodiment 1,
The present embodiment provides high temperature resistant speckle that a kind of adhesiveness is strong and preparation method thereof, and by the flow chart of Fig. 1, its preparation method comprises the steps:
S1, in the 1g Ludox being placed in beaker, add 1g alumina powder, 2g SiO 2 powder, 0.5g Zinc oxide powder and 1g magnesium oxide powder, after adding a kind of powder, it is sufficiently stirred for Glass rod so that it is mix homogeneously, add lower a kind of powder, the emulsion being uniformly mixed；
S2, to the emulsion in described step S1 adding 0.2g latex, and be sufficiently stirred for Glass rod so that it is mix homogeneously；Being sprayed at by emulsion after mix homogeneously and be of a size of 40mm × 40mm × 2mm and through cleaning and dried Inconel751 high temperature alloy sheet surface, then oven drying at low temperature at 40 DEG C, forms initial speckle；
S3, the alloy sheet that surface in described step S2 forms initial speckle are put in high temperature furnace, it is warming up to 800 DEG C, and fire 20min at 800 DEG C, stopping heating afterwards, alloy sheet is naturally down to room temperature in high temperature furnace, obtains that adhesiveness is strong and resistant to elevated temperatures speckle, corresponding speckle pattern is as shown in Figure 2, can learn from Fig. 2: speckle is uniform in Inconel751 high temperature alloy sheet surface distributed, is tightly combined, it does not have come off region because combining the large stretch of speckle closely not occurred.
The high temperature test lab diagram that Fig. 3 is speckle prepared by the present embodiment at temperature (A) T=1200 DEG C and (B) T=1400 DEG C.Can learning from Fig. 3: speckle is carried out high temperature test, under different high temperature, speckle pattern is unchanged or almost without change, surface speckle resistance to elevated temperatures is good, obscission will not occurs because of high temperature.
Fig. 4 is the speckle pattern after the speckle prepared by the present embodiment stretches under different stretch power, and wherein, tensile force from left to right is followed successively by 0 μ ε, 10000 μ ε, 15000 μ ε, 20000 μ ε and 25000 μ ε.Can learn from Fig. 4: speckle is gradually increased tensile force, speckle pattern is unchanged or almost without change, it was shown that the adhesion of speckle and substrate is strong, not easily breaking releasing, this performance is just resulting from adopting Ludox, combines the synergism brought with sintering procedure.
Embodiment 2,
The present embodiment provides high temperature resistant speckle that a kind of adhesiveness is strong and preparation method thereof, and by the flow chart of Fig. 1, its preparation method comprises the steps:
S1, in the 1g deionized water being placed in beaker, add 2g alumina powder, 2g SiO 2 powder, 2g titanium dioxide powder and 1.5g lead oxide powder, after adding a kind of powder, it is sufficiently stirred for Glass rod, make its mix homogeneously, add lower a kind of powder, the emulsion being uniformly mixed；
S2, to the emulsion in described step S1 adding 0.3g liquid epoxies adhesive, and be sufficiently stirred for Glass rod so that it is mix homogeneously；Again the emulsion after mix homogeneously is sprayed at and is of a size of 40mm × 40mm × 3mm and through cleaning and dried stainless steel substrates surface, then naturally dry at 25 DEG C, form initial speckle；
S3, the stainless steel substrates that surface in described step S2 forms initial speckle are put in high temperature furnace, it is warming up to 1200 DEG C, and fires 15min at 1200 DEG C, stop heating afterwards, stainless steel substrates is naturally down to room temperature in high temperature furnace, obtains that adhesiveness is strong and resistant to elevated temperatures speckle.
Test according to the corresponding detection method in embodiment 1, learn that the speckle that the present embodiment prepares is uniform in stainless steel substrates surface distributed, be tightly combined, it does not have come off region because combining the large stretch of speckle closely not occurred；Speckle is carried out high temperature test, and under different high temperature, speckle pattern is unchanged or almost without change, surface speckle resistance to elevated temperatures is good, obscission will not occurs because of high temperature；Speckle is gradually increased tensile force, speckle pattern is unchanged or almost without change, show that the adhesion of speckle and substrate is strong, not easily breaking releasing, this performance is just resulting from adopting deionized water, the synergism brought is combined with sintering procedure, because water can evaporate in the process fired from speckle, make speckle matter pine, good toughness, difficult drop-off, and good with base material adhesiveness.
Embodiment 3,
The present embodiment provides high temperature resistant speckle that a kind of adhesiveness is strong and preparation method thereof, and by the flow chart of Fig. 1, its preparation method comprises the steps:
S1, in the 1g ethanol being placed in beaker, add 2g alumina powder, 2g Zirconium oxide powder, 1g lithium oxide powder and 0.5g lime powder, after adding a kind of powder, it is sufficiently stirred for Glass rod so that it is mix homogeneously, add lower a kind of powder, the emulsion being uniformly mixed；
S2, to the emulsion in described step S1 adding 0.4g latex, and be sufficiently stirred for Glass rod so that it is mix homogeneously；Being spun on by emulsion after mix homogeneously and be of a size of 40mm × 40mm × 2mm and through cleaning and dried Inconel751 high temperature alloy sheet surface, then oven drying at low temperature at 20 DEG C, forms initial speckle；
S3, the alloy sheet that surface in described step S2 forms initial speckle are put in high temperature furnace, are warming up to 1000 DEG C, and fire 18min at 1000 DEG C, stop heating afterwards, and alloy sheet is naturally down to room temperature in high temperature furnace, obtain that adhesiveness is strong and resistant to elevated temperatures speckle.
Test according to the corresponding detection method in embodiment 1, learn that the speckle that the present embodiment prepares is uniform in Inconel751 high temperature alloy sheet surface distributed, be tightly combined, it does not have come off region because combining the large stretch of speckle closely not occurred；Speckle is carried out high temperature test, and under different high temperature, speckle pattern is unchanged or almost without change, surface speckle resistance to elevated temperatures is good, obscission will not occurs because of high temperature；Speckle is gradually increased tensile force, speckle pattern is unchanged or almost without change, show that the adhesion of speckle and substrate is strong, not easily breaking releasing, this performance is just resulting from adopting ethanol, the synergism brought is combined with sintering procedure, because ethanol can evaporate in the process fired from speckle, make speckle matter pine, good toughness, difficult drop-off, and good with base material adhesiveness.
Embodiment 4,
The present embodiment provides high temperature resistant speckle that a kind of adhesiveness is strong and preparation method thereof, and its preparation method comprises the steps:
S1, in the 1g Ludox being placed in beaker, add 2g alumina powder, 2g SiO 2 powder, 2g titanium dioxide powder and 1.5g lead oxide powder, after adding a kind of powder, it is sufficiently stirred for Glass rod so that it is mix homogeneously, add lower a kind of powder, the emulsion being uniformly mixed；
S2, the emulsion in described step S1 is sputtered in be of a size of 40mm × 40mm × 3mm and through cleaning and dried stainless steel substrates surface, then naturally dry at 50 DEG C, form initial speckle；
S3, the stainless steel substrates that surface in described step S2 forms initial speckle are put in high temperature furnace, it is warming up to 1100 DEG C, and fires 16min at 1100 DEG C, stop heating afterwards, stainless steel substrates is naturally down to room temperature in high temperature furnace, obtains that adhesiveness is strong and resistant to elevated temperatures speckle.
Test according to the corresponding detection method in embodiment 1, learn that the speckle that the present embodiment prepares is uniform in stainless steel substrates surface distributed, be tightly combined, it does not have come off region because combining the large stretch of speckle closely not occurred；Speckle is carried out high temperature test, and under different high temperature, speckle pattern is unchanged or almost without change, surface speckle resistance to elevated temperatures is good, obscission will not occurs because of high temperature；Speckle is gradually increased tensile force, and speckle pattern is unchanged or almost without change, it was shown that the adhesion of speckle and substrate is strong, not easily breaking releasing, and this performance is just resulting from adopting Ludox, combines the synergism brought with sintering procedure.
Comparative example 1,
This comparative example provides a kind of speckle and preparation method thereof, and its preparation method comprises the steps:
S1, in the 0.2g latex being placed in beaker, add 1g alumina powder, 2g SiO 2 powder, 0.5g Zinc oxide powder and 1g magnesium oxide powder, after adding a kind of powder, it is sufficiently stirred for Glass rod so that it is mix homogeneously, add lower a kind of powder, the emulsion being uniformly mixed；
S2, the emulsion in described step S1 is sprayed at be of a size of 40mm × 40mm × 2mm and through cleaning and dried Inconel751 high temperature alloy sheet surface, then oven drying at low temperature at 40 DEG C, forms initial speckle；
S3, the alloy sheet that surface in described step S2 forms initial speckle are put in high temperature furnace, are warming up to 800 DEG C, and fire 20min at 800 DEG C, stop heating afterwards, and alloy sheet is naturally down to room temperature in high temperature furnace, obtains speckle.
Test according to the corresponding detection method in embodiment 1, learn when the speckle that the present embodiment prepares carries out stretching under different stretch power, when tensile force reaches 20000 μ ε, there is partial exfoliation in speckle, expose Inconel751 high temperature alloy sheet, show, do not add Ludox and cause that the adhesiveness of speckle and Inconel751 high temperature alloy sheet declines.
Comparative example 2,
This comparative example provides a kind of speckle and preparation method thereof, and its preparation method comprises the steps:
S1, in the 1g Ludox being placed in beaker, add 1g alumina powder, 2g SiO 2 powder, 0.5g Zinc oxide powder and 1g magnesium oxide powder, after adding a kind of powder, it is sufficiently stirred for Glass rod so that it is mix homogeneously, add lower a kind of powder, the emulsion being uniformly mixed；
S2, to the emulsion in described step S1 adding 0.2g latex, and be sufficiently stirred for Glass rod so that it is mix homogeneously；Being sprayed at by emulsion after mix homogeneously and be of a size of 40mm × 40mm × 2mm and through cleaning and dried Inconel751 high temperature alloy sheet surface, then oven drying at low temperature at 80 DEG C, obtains speckle.The speckle obtained is carried out adhesiveness test, by scrub-brush polish-brush surface of test piece, obtain corresponding speckle pattern as shown in Figure 5, can learn: speckle is not strong at Inconel751 high temperature alloy sheet surface adhesion occur after polish-brush test exposing Inconel751 high temperature alloy sheet in large stretch of region without speckle from Fig. 5, reason is in that, unfired step, the adhesion between speckle and Inconel751 high temperature alloy sheet is weak, occurs that sheet comes off after polish-brush.
Obviously, above-described embodiment is only for clearly demonstrating example, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.And the apparent change thus extended out or variation are still among the protection domain of the invention.
Claims (10)
1. a preparation method for the high temperature resistant speckle that adhesiveness is strong, comprises the steps:
S1, by substance A, refractory oxide and flux mix, formed emulsion, wherein, described substance A is at least one in Ludox, water, ethanol；
S2, the emulsion in described step S1 is coated on substrate surface, and the substrate after coating emulsion is dried, form initial speckle；
S3, the substrate that surface in described step S2 forms initial speckle are fired, and are cooled to room temperature, obtain the speckle that adhesiveness is strong.
2. preparation method according to claim 1, it is characterised in that: in described step S3, described in fire the temperature of step be 800 DEG C-1200 DEG C, the time is 10-30min.
3. preparation method according to claim 1 and 2, it is characterised in that: in described step S1, the mass ratio of described Ludox, described refractory oxide and described flux is 1:(3～6): 1.5.
4. the preparation method according to any one of claim 1-3, it is characterised in that: in described step S1, described refractory oxide is at least one in aluminium oxide, silicon dioxide, titanium dioxide, zirconium oxide.
5. the preparation method according to any one of claim 1-4, it is characterised in that: described flux is at least one in lead oxide powder, Zinc oxide powder, magnesium oxide powder, sodium oxide powder, lithium oxide powder, lime powder.
6. the preparation method according to any one of claim 1-5, it is characterised in that: in described step S2, the temperature of described drying steps is 40-50 DEG C.
7. the preparation method according to any one of claim 1-6, it is characterised in that: in described step S1, before mixing, also include the step adding binding agent.
8. preparation method according to claim 7, it is characterised in that: described binding agent is latex and/or epoxy resin adhesive；
The mass ratio of described binding agent and described refractory oxide is 1:(10-20).
9. the preparation method according to any one of claim 1-8, it is characterised in that: in described step S2, described substrate is alloy sheet or stainless steel substrates；
Described coating step is at least one in spin coating, spraying, sputtering.
10. the speckle that the preparation method according to any one of a claim 1-9 prepares.
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| CN109959543A (en) * | 2019-05-05 | 2019-07-02 | 中国人民解放军陆军装甲兵学院 | The method of speckle labeling method and detection coating material damage |
| CN112556976A (en) * | 2020-12-09 | 2021-03-26 | 中国航天空气动力技术研究院 | Speckle manufacturing method for deformation measurement of special wind tunnel experiment model |
| CN113029805A (en) * | 2021-03-04 | 2021-06-25 | 武汉科技大学 | Visual detection method for high-temperature performance of material with external magnetic field |
| CN116144263A (en) * | 2023-04-17 | 2023-05-23 | 兰州大学 | Preparation process of low-temperature large-deformation speckle, speckle and optical path observation system |
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