CN116969765A - Precursor ceramic high-temperature sensing material containing in-situ antioxidation coating and preparation method thereof - Google Patents
Precursor ceramic high-temperature sensing material containing in-situ antioxidation coating and preparation method thereof Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 52
- 238000000576 coating method Methods 0.000 title claims abstract description 52
- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 239000002243 precursor Substances 0.000 title claims abstract description 40
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 35
- 239000011540 sensing material Substances 0.000 title claims abstract description 26
- 230000003064 anti-oxidating effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 46
- 230000003647 oxidation Effects 0.000 claims abstract description 34
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 34
- 230000007704 transition Effects 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000000465 moulding Methods 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims abstract description 7
- 238000006722 reduction reaction Methods 0.000 claims abstract description 7
- 230000009471 action Effects 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 238000000197 pyrolysis Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000004093 laser heating Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000000016 photochemical curing Methods 0.000 claims description 2
- 230000008646 thermal stress Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5603—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides with a well-defined oxygen content, e.g. oxycarbides
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Abstract
The application belongs to the technical field of sensor materials, and discloses a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating and a preparation method thereof, wherein the precursor ceramic high-temperature sensing material comprises a raw material layer, and a transition layer and an oxidation-resistant coating are sequentially arranged on the outer side of the raw material layer; the preparation method comprises the following steps: the raw material layer is prepared by molding and pyrolysis of a polymer precursor; the transition layer is obtained through a temperature gradient constructed by laser; the antioxidation coating is obtained by an in-situ carbothermal reduction reaction under the heating action of the laser surface; the application constructs a surface gradient temperature field based on the surface heating effect of laser, and combines the carbothermal reduction reaction of the precursor ceramic at high temperature to consume surface free carbon, thereby realizing the in-situ preparation of the high-temperature-resistant and high-electrical-resistance oxidation coating. The gradient temperature field constructed by the laser not only can realize the in-situ preparation of the antioxidation coating, but also can ensure the gradient transition of the components, and can effectively relieve the thermal stress caused by the mismatch of the thermal expansion coefficients.
Description
Technical Field
The application relates to the technical field of sensor materials, in particular to a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating and a preparation method thereof.
Background
The accurate quantification of the pneumatic heating energy transmission process is the basis for developing the design of a new generation of high Mach number heat protection system of the near space aircraft, and is also a key technology for further optimizing the structural efficiency of the near space aircraft and improving the flight performance. Among them, measurement of temperature and heat flow in the high-speed flight process is always an important point of attention in the field of near space aircrafts, however, the severe flight environment presents serious challenges for direct measurement of parameters such as temperature and heat flow in a thermal protection system.
The surface temperature, heat flow and other parameter tests of the current near space aircraft heat protection system are mainly realized through thermocouples, and the defects of high price, large volume, insufficient test precision and stability, poor matching property with heat protection materials and high assembly difficulty are overcome. The development of microelectromechanical systems (MEMS) has provided the possibility to embed micro sensors in thermal protection systems. However, existing MEMS sensor testing capabilities typically do not exceed 500 ℃.
The precursor conversion ceramic (PDC) technology is a method for preparing inorganic ceramic through high-temperature pyrolysis of organic high-molecular polymers, and has excellent formability, high-temperature stability, oxidation/corrosion resistance and high-temperature semiconductor characteristics, so that the method becomes one of the most potential material systems for solving the temperature sensing problem in the severe high-temperature environment in the future. Research has shown that precursor-converted SiCNO ceramics still have better semiconductor properties at 1300 ℃ than any of the presently known materials. Under inert atmosphere, the highest use temperature of the known PDC temperature sensor reaches 1800 ℃; however, under aerobic conditions, the maximum use temperature is only 800 ℃, and oxidation of the PDC sensitive material will significantly increase its resistance, thereby affecting the accuracy of the temperature sensor.
Disclosure of Invention
The application aims to provide a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating and a preparation method thereof, wherein a surface gradient temperature field is constructed based on the surface heating effect of laser, and the in-situ preparation of the high-temperature-resistant high-electrical-resistance oxidation coating is realized by combining the carbothermal reduction reaction of the precursor ceramic at high temperature to consume surface free carbon. The gradient temperature field constructed by the laser not only can realize the in-situ preparation of the antioxidation coating, but also can ensure the gradient transition of the components, and can effectively relieve the thermal stress caused by the mismatch of the thermal expansion coefficients.
In order to achieve the above object, the present application provides the following technical solutions:
the precursor ceramic high-temperature sensing material containing the in-situ oxidation-resistant coating comprises a raw material layer, wherein a transition layer and an oxidation-resistant coating are sequentially arranged on the outer side of the raw material layer.
Further, the raw material layer is a precursor converted silicon-based ceramic which can undergo carbothermic reduction reaction at high temperature.
Further, the precursor converts the silicon-based ceramic to one of SiCN, siOC, siBCN, siBOC.
Further, the thickness of the raw material layer is 0.1-3 mm, the thickness of the transition layer is 1-50 μm, and the thickness of the antioxidation coating is 1-100 μm.
According to the preparation method of the precursor ceramic high-temperature sensing material containing the in-situ oxidation-resistant coating, the raw material layer is prepared by forming and pyrolyzing a polymer precursor; the transition layer is obtained through a temperature gradient constructed by laser; the antioxidation coating is obtained by in-situ carbothermal reduction reaction under the heating action of the laser surface.
The preparation method of the precursor ceramic high-temperature sensing material containing the in-situ oxidation-resistant coating comprises the following specific steps:
s1, preparation of raw materials: the precursor ceramic with excellent formability is selected for forming, after forming, the temperature is raised to 1000 ℃ to 1600 ℃ under vacuum or inert environment, the temperature is kept for 4 hours, then the temperature is lowered to room temperature, the raw materials for the needed high-temperature sensor are obtained, and then pretreatment is carried out;
s2, preparing a transition layer: adopting continuous or pulse laser to irradiate the surface of the raw material in an inert gas environment, constructing continuous temperature gradients by the surface heating effect of the laser, reacting the material with different degrees along with the change of temperature, and preparing a transition layer by the continuous gradients of the surface components caused by the continuous gradients of the temperature;
s3, preparing an antioxidation coating: and (3) irradiating the surface of the raw material by adopting continuous or pulse laser in an inert gas environment, wherein the surface heating effect of the laser enables the surface temperature of the material to be the highest, free carbon in the material is consumed by the carbothermic reaction, and the compact antioxidation coating is prepared after repeated dipping and laser heating.
Further, in S1, the molding method is one of powder molding, liquid molding, and photo-curing molding.
Further, in S1, the preprocessing includes the following processes: grinding the raw material layer by metallographic sand paper with the mesh number of 200#, 500#, 1000# respectively, ultrasonically cleaning by acetone for 5-15 min, ultrasonically cleaning by alcohol for 5-15 min, and drying at 100-150 ℃ for 20-60 min.
Further, in S2, when preparing the transition layer, the laser irradiation raw material adopts continuous laser beam, and the laser power is 40W-200W; the laser irradiation raw material adopts a pulse laser beam, and the laser power is 0.01W-10W; the temperature gradient is thus established to produce the transition layer.
Further, in S3, when preparing the antioxidation coating, continuous laser beams are adopted as laser irradiation raw materials, and the laser power is 40W-200W; the laser irradiation raw material adopts a pulse laser beam, and the laser power is 0.01W-10W; thereby the raw materials are subjected to in-situ reaction to prepare the antioxidation coating.
The technical proposal has the beneficial effects that:
1. the application provides a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating and a preparation method thereof, wherein continuous component gradient of the oxidation-resistant coating is realized through continuous temperature gradient generated by laser irradiation, the prepared oxidation-resistant coating has excellent high-temperature stability and high-resistance characteristics, and a continuous gradient transition layer can effectively relieve thermal stress caused by unmatched thermal expansion coefficients, so that the use temperature of the precursor ceramic high-temperature sensing material under high-temperature aerobic conditions can be greatly expanded;
2. the preparation method of the precursor ceramic high-temperature sensing material containing the in-situ oxidation-resistant coating has the advantages of simple process flow, suitability for all precursor ceramics capable of undergoing carbothermic reaction, good stability of the prepared material and easiness in large-scale popularization and application.
Drawings
FIG. 1 is a schematic structural diagram of a precursor ceramic high temperature sensing material containing an in-situ oxidation resistant coating of the present application;
FIG. 2 is a schematic illustration of a precursor ceramic high temperature sensing material preparation process comprising an in situ oxidation resistant coating of the present application;
the names of the corresponding marks in the drawings are:
a raw material layer 1, a transition layer 2, an antioxidation coating 3, a high-temperature electrode 4, a vacuum environment 5 and a laser irradiation source 6.
Detailed Description
The application is described in further detail below with reference to the attached drawings and embodiments:
as shown in fig. 1, a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating comprises a raw material layer 1, wherein a transition layer 2 and an oxidation-resistant coating 3 are sequentially arranged on the outer side of the raw material layer 1; the raw material layer 1 is ceramic SiCN with the thickness of 0.1 mm-3 mm; the thickness of the transition layer 2 is 0.5-2 mu m; the thickness of the antioxidation coating 3 is 2-3 μm.
As shown in fig. 2, a preparation method of a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating is shown, and a raw material layer 1 is prepared by forming and pyrolyzing a polymer; the transition layer 2 is prepared by a temperature gradient constructed by laser; the antioxidation coating 3 is obtained by in-situ reaction under the action of laser.
The method comprises the following specific steps:
s1, preparing and preprocessing a raw material layer 1: heating precursor ceramic SiCN to 1200-1600 ℃ under vacuum environment 5, preserving heat for 4h, cooling to room temperature, grinding into powder, tabletting, repeatedly dipping and pyrolyzing to obtain a raw material layer 1, and carrying out pretreatment; wherein, the pretreatment comprises the following steps: grinding the raw material layer 1 by metallographic sand paper with the mesh number of 2000#, 3000# and 5000# for 0.5-2 hours respectively, ultrasonically cleaning by using acetone for 5-15 min, ultrasonically cleaning by using alcohol for 5-15 min, ultrasonically cleaning by using water for 5-15 min, and drying at 100-150 ℃ for 20-60 min;
s2, preparing a transition layer 2: irradiating raw materials by a laser irradiation source 6 in an inert gas environment, and constructing a temperature gradient by laser to prepare a transition layer 2; wherein, the conditions of the laser irradiation raw materials are: adopting a continuous laser beam, wherein the laser power is 40-200W;
s3, preparing an antioxidation coating 3: under the inert gas environment, the raw material layer 1 is connected with a laser irradiation source 6 through a high-temperature electrode 4, the laser irradiation source 6 is started to irradiate raw materials, and an in-situ reaction is carried out under the action of laser to prepare an antioxidation coating 3; wherein, the conditions of the laser irradiation raw materials are: the continuous laser beam is adopted, and the laser power is 40W-200W.
The foregoing is merely exemplary embodiments of the present application, and detailed technical solutions or features that are well known in the art have not been described in detail herein. It should be noted that, for those skilled in the art, several variations and modifications can be made without departing from the technical solution of the present application, and these should also be regarded as the protection scope of the present application, which does not affect the effect of the implementation of the present application and the practical applicability of the patent. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (10)
1. The precursor ceramic high-temperature sensing material containing the in-situ oxidation-resistant coating is characterized by comprising a raw material layer, wherein a transition layer and the oxidation-resistant coating are sequentially arranged on the outer side of the raw material layer.
2. The precursor ceramic high-temperature sensing material containing the in-situ oxidation-resistant coating according to claim 1, wherein the raw material layer is a precursor converted silicon-based ceramic subjected to carbothermal reduction reaction at high temperature.
3. The precursor ceramic high temperature sensing material comprising an in-situ oxidation resistant coating of claim 2, wherein the precursor converts a silicon-based ceramic to one of SiCN, siOC, siBCN, siBOC.
4. The precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating according to claim 1, wherein the thickness of the raw material layer is 0.1-3 mm, the thickness of the transition layer is 1-50 μm, and the thickness of the oxidation-resistant coating is 1-100 μm.
5. The method for preparing a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating according to any one of claims 1 to 4, wherein the raw material layer is prepared by molding and pyrolysis of a polymer precursor; the transition layer is obtained through a temperature gradient constructed by laser; the antioxidation coating is obtained by in-situ carbothermal reduction reaction under the heating action of the laser surface.
6. The method for preparing the precursor ceramic high-temperature sensing material containing the in-situ oxidation resistant coating according to claim 5, which is characterized by comprising the following specific steps:
s1, preparation of raw materials: the precursor ceramic with excellent formability is selected for forming, after forming, the temperature is raised to 1000 ℃ to 1600 ℃ under vacuum or inert environment, the temperature is kept for 4 hours, then the temperature is lowered to room temperature, the raw materials for the needed high-temperature sensor are obtained, and then pretreatment is carried out;
s2, preparing a transition layer: adopting continuous or pulse laser to irradiate the surface of the raw material in an inert gas environment, constructing continuous temperature gradients by the surface heating effect of the laser, reacting the material with different degrees along with the change of temperature, and preparing a transition layer by the continuous gradients of the surface components caused by the continuous gradients of the temperature;
s3, preparing an antioxidation coating: and (3) irradiating the surface of the raw material by adopting continuous or pulse laser in an inert gas environment, wherein the surface heating effect of the laser enables the surface temperature of the material to be the highest, free carbon in the material is consumed by the carbothermic reaction, and the compact antioxidation coating is prepared after repeated dipping and laser heating.
7. The method for preparing a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating according to claim 6, wherein in the step S1, the molding method is one of powder molding, liquid molding and photo-curing molding.
8. The method for preparing a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating according to claim 6, wherein in S1, the pretreatment comprises the following steps: grinding the raw material layer by metallographic sand paper with the mesh number of 200#, 500#, 1000# respectively, ultrasonically cleaning by acetone for 5-15 min, ultrasonically cleaning by alcohol for 5-15 min, and drying at 100-150 ℃ for 20-60 min.
9. The method for preparing a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating, according to claim 6, wherein in the step S2, when preparing the transition layer, a continuous laser beam is adopted as a laser irradiation raw material, and the laser power is 40W-200W; the laser irradiation raw material adopts a pulse laser beam, and the laser power is 0.01W-10W; the temperature gradient is thus established to produce the transition layer.
10. The method for preparing a precursor ceramic high-temperature sensing material containing an in-situ oxidation-resistant coating according to claim 6, wherein in the step S3, when the oxidation-resistant coating is prepared, a continuous laser beam is adopted as a laser irradiation raw material, and the laser power is 40W-200W; the laser irradiation raw material adopts a pulse laser beam, and the laser power is 0.01W-10W; thereby the raw materials are subjected to in-situ reaction to prepare the antioxidation coating.
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