CN117230402B - Method for obtaining alumina coating detection sample - Google Patents
Method for obtaining alumina coating detection sample Download PDFInfo
- Publication number
- CN117230402B CN117230402B CN202311490485.2A CN202311490485A CN117230402B CN 117230402 B CN117230402 B CN 117230402B CN 202311490485 A CN202311490485 A CN 202311490485A CN 117230402 B CN117230402 B CN 117230402B
- Authority
- CN
- China
- Prior art keywords
- alumina coating
- coating
- obtaining
- transition layer
- alumina
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000576 coating method Methods 0.000 title claims abstract description 131
- 239000011248 coating agent Substances 0.000 title claims abstract description 129
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 79
- 238000001514 detection method Methods 0.000 title claims abstract description 17
- 230000007704 transition Effects 0.000 claims abstract description 74
- 238000010438 heat treatment Methods 0.000 claims abstract description 51
- 238000007750 plasma spraying Methods 0.000 claims abstract description 35
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims description 77
- 238000005507 spraying Methods 0.000 claims description 58
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 5
- 239000011224 oxide ceramic Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 15
- 229910052751 metal Inorganic materials 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000012805 post-processing Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 77
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 36
- 239000007789 gas Substances 0.000 description 16
- 239000000919 ceramic Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 13
- 238000005524 ceramic coating Methods 0.000 description 12
- 239000002344 surface layer Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000000670 limiting effect Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 230000008642 heat stress Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
Abstract
The application provides a method for obtaining an alumina coating detection sample, and relates to the field of metal surface coatings. A method of obtaining an alumina coating test sample comprising: preparing a transition layer on the surface of a substrate by adopting a low-pressure plasma spraying method, preparing an alumina coating on the surface of the transition layer by adopting an atmospheric plasma spraying method, performing heat treatment and cooling stripping on the obtained composite coating, and obtaining the alumina coating detection sample. The method for obtaining the alumina coating detection sample is simple and convenient to operate, the peeled coating is complete in appearance and controllable in thickness, the chemical composition of the sprayed alumina coating is reserved, and the method can be processed into various required specification shapes through post-processing, so that the requirement of accurate detection of the performance of the alumina coating can be met.
Description
Technical Field
The application relates to the field of metal surface coatings, in particular to a method for obtaining an alumina coating detection sample.
Background
The alumina coating has high hardness, high chemical stability and excellent wear resistance and corrosion resistance, and is widely applied to the industrial field, so that high-end equipment and parts can stably operate in a severe service environment, the damage of matrix materials is reduced, and the service life of the high-end equipment and parts is prolonged. The alumina coating can be used as a low-stress abrasive grain wear, hard surface wear, various chemical media and chemical gas corrosion resistant coating, cavitation resistant coating and erosion resistant coating at normal temperature, and also used as a fuel gas corrosion resistant coating and a high-temperature emission coating at high temperature. Has wide application prospect in the fields of electronics, petroleum, ferrous metallurgy, mechanical chemical industry, equipment manufacturing, aerospace and other industries.
The plasma spraying has the characteristics of high flame flow temperature, simple and convenient process, high efficiency, excellent coating performance and the like, is one of the main methods for preparing the alumina ceramic coating at present, can rapidly deposit the alumina ceramic coating on a substrate by adopting a plasma spraying technology, and can organically combine the advantages of an alumina ceramic material and a metal material, thereby improving the service performance of parts. In the development and production process of the alumina coating by adopting a plasma spraying process, when the related properties of the alumina ceramic coating such as physics, chemistry and the like are required to be evaluated and analyzed with high precision, the alumina coating is required to be peeled off from a substrate when the analysis of chemical components of the alumina coating, the test of physical properties such as thermal conductivity and the like of the alumina coating and the like are carried out by adopting a chemical method.
At present, the existing stripping method of the alumina ceramic coating generally adopts a chemical stripping method, the coating is stripped through electrochemical reaction in alkaline aqueous solution, and the alumina ceramic coating in a spraying state cannot be obtained by adopting the stripping method due to the reaction of the coating. Therefore, there is an urgent need to develop a new peeling method for the alumina coating, which peels the alumina coating from the surface of a specific substrate completely, so as to meet the requirement of coating performance detection.
Disclosure of Invention
The present application aims to provide a method for obtaining an alumina coating test sample, so as to solve the above problems.
In order to achieve the above purpose, the present application adopts the following technical scheme:
a method of obtaining an alumina coating test sample, comprising:
preparing a transition layer on the surface of a substrate by adopting a low-pressure plasma spraying method, preparing an alumina coating on the surface of the transition layer by adopting an atmospheric plasma spraying method, performing heat treatment and cooling stripping on the obtained composite coating to obtain an alumina coating detection sample;
the transition layer comprises 5-10% of aluminum powder by mass percent and the balance of aluminum oxide ceramic powder; the technological parameters of the low-pressure plasma spraying method comprise: the pressure of the vacuum chamber is 1.5-2.0 mbar, the power is 80-120kW, the spraying distance is 700-900mm, ar gas flow is 80-110slpm, he gas flow is 60-150slpm, and the powder feeding speed is 10-20g/min;
the raw materials of the alumina coating are pure alumina ceramic powder, and the technological parameters of the atmospheric plasma spraying method comprise: spraying power is 35kW-42kW, ar gas flow is 38-41slpm, H 2 The air flow is 13-14 slpm, the powder feeding speed is 20-40g/min, and the spraying distance is 100-120mm.
Preferably, the thickness of the transition layer is 20-50 μm.
Preferably, in the raw material of the transition layer, the particle sizes of the aluminum powder and the aluminum oxide ceramic powder are each independently 10-30 μm.
Preferably, the thickness of the alumina coating is not less than 50 μm.
Preferably, the heat treatment comprises:
and placing the substrate with the composite coating in a heating device for heating.
Preferably, the temperature of the heat treatment is 800-1000 ℃ and the time is 3-6h.
Preferably, the cooling comprises:
and immediately putting the sample after the heat treatment into water for ultrasonic treatment until the alumina coating is peeled off.
Preferably, the temperature of the water is 0-10 ℃.
Preferably, the frequency of the ultrasonic treatment is 20-80kHz.
Preferably, the density of the transition layer is 97-99%.
Compared with the prior art, the beneficial effects of this application include:
according to the method for obtaining the alumina coating detection sample, a compact transition layer is prepared on the surface of a substrate by adopting a low-pressure plasma spraying method, then an alumina coating is prepared on the surface of the transition layer by adopting an atmospheric plasma spraying method, the obtained composite coating is subjected to heat treatment, al in the transition layer is oxidized in the heat treatment process, so that the transition layer is subjected to volume expansion to generate stress, and then a larger thermal stress mismatch is generated at the interface of the transition layer and the alumina coating in a cooling mode, so that the alumina coating of the surface layer is peeled off from the surface of the transition layer, and peeling occurs at the interface of the transition layer and the alumina coating to obtain the complete alumina coating detection sample. Aluminum powder and aluminum oxide are used as transition layer materials, so that the transition layer materials can be prevented from polluting the aluminum oxide coating on the surface in the heat treatment process. The method has the advantages of simple operation, complete and uncracked appearance of the stripped coating, controllable thickness of the coating, reserved chemical composition of the sprayed alumina coating, capability of being processed into various required specifications and shapes through post-processing, and the like, and can meet the requirement of accurate detection of the performance of the alumina coating.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate certain embodiments of the present application and therefore should not be considered as limiting the scope of the present application.
FIG. 1 is a physical view of the alumina coating obtained by peeling in example 1.
Detailed Description
First, the technical scheme provided by the application is integrally stated:
a method of obtaining an alumina coating test sample, comprising:
preparing a transition layer on the surface of a substrate by adopting a low-pressure plasma spraying method, preparing an alumina coating on the surface of the transition layer by adopting an atmospheric plasma spraying method, performing heat treatment and cooling stripping on the obtained composite coating to obtain an alumina coating detection sample;
the transition layer comprises 5-10% of aluminum powder by mass percent and the balance of aluminum oxide ceramic powder; the technological parameters of the low-pressure plasma spraying method comprise: the pressure of the vacuum chamber is 1.5-2.0 mbar, the power is 80-120kW, the spraying distance is 700-900mm, ar gas flow is 80-110slpm, he gas flow is 60-150slpm, and the powder feeding speed is 10-20g/min;
the raw materials of the alumina coating are pure alumina ceramic powder, and the technological parameters of the atmospheric plasma spraying method comprise: spraying power is 35kW-42kW, ar gas flow is 38-41slpm, H 2 The air flow is 13-14 slpm, the powder feeding speed is 20-40g/min, and the spraying distance is 100-120mm.
Optionally, the aluminum powder content in the raw materials of the transition layer can be any value between 5%, 6%, 7%, 8%, 9%, 10% or 5-10% by mass percent, and the balance is aluminum oxide ceramic powder.
If the content of the metal Al is too low, the oxidation degree of the transition layer is not obvious, so that the generated thermal expansion mismatch effect is not obvious, and the coating cannot be completely stripped; when the content of the metal Al is too high, explosion is easy to occur in the plasma spraying process to generate danger due to the high activity of the metal Al, and the spraying cannot be performed.
Alternatively, in the process parameters of the low pressure plasma spraying method, the vacuum chamber pressure may be any value of 1.5 mbar, 1.6 mbar, 1.7 mbar, 1.8 mbar, 1.9 mbar, 2.0 mbar or 1.5-2.0 mbar, the power may be any value of 80kW, 90kW, 100kW, 110kW, 120kW or 80-120kW, the spraying distance may be any value of 700mm, 750mm, 800mm, 850mm, 900mm or 700-900mm, ar gas flow can be any value between 80slpm, 90slpm, 100slpm, 110slpm or 80-110slpm, he gas flow can be any value between 60slpm, 70slpm, 80slpm, 90slpm, 100slpm, 110slpm, 120slpm, 130slpm, 140slpm, 150slpm or 60-150slpm, and powder feeding rate can be any value between 10g/min, 11g/min, 12g/min, 13g/min, 14g/min, 15g/min, 16g/min, 17g/min, 18g/min, 19g/min, 20g/min or 10-20g/min;
compared with the traditional atmospheric plasma spraying, the low-pressure plasma spraying is carried out in a low-pressure atmosphere, al is not easy to oxidize in the spraying process, so that the metal Al component in the coating is better reserved, the low-pressure plasma spraying equipment has high power, the spraying material is easy to melt, the spraying speed is high, and the high-pressure plasma spraying can be realizedTransition layer of dense structure (Al/Al 2 O 3 Coating) is prepared, and the subsequent stripping of the alumina layer is facilitated. In the application, when the transition layer is prepared by adopting low-pressure plasma spraying, the spraying parameters are strictly controlled, and the technological parameters are mutually influenced, so that the transition layer with a compact structure can be prepared. The coating is carried out according to specific low-pressure plasma spraying parameters, and particularly, the spraying power is controlled, so that the compactness of the coating can be improved.
The raw materials of the alumina coating are pure alumina ceramic powder, and the technological parameters of the atmospheric plasma spraying method comprise: spraying power is 35kW-42kW, ar gas flow is 38-41slpm, H 2 The air flow is 13-14 slpm, the powder feeding speed is 20-40g/min, and the spraying distance is 100-120mm.
The term "pure alumina ceramic powder" as used herein does not mean absolute pure alumina, but means alumina as a main component, and may contain other trace elements and impurities.
Alternatively, in the process parameters of the atmospheric plasma spraying method, the spraying power may be any value of 35kW, 36kW, 37kW, 38kW, 39kW, 40kW, 41kW, 42kW or 35kW-42kW, and the Ar gas flow may be any value of 38slpm, 40slpm, 41slpm or 38-41slpm, H 2 The air flow can be any value of 13slpm, 13.5slpm, 14slpm or 13-14 slpm, the powder feeding speed can be any value of 20g/min, 25g/min, 30g/min, 35g/min, 40g/min or 20-40g/min, and the spraying distance can be any value of 100mm, 110mm, 120mm or 100-120mm.
Mixing Al powder with Al 2 O 3 The purpose of the uniform mixing of the ceramic powder is to avoid the occurrence of local peeling or cracking of the surface alumina caused by the problem of stress concentration of the transition layer due to local oxidation, thereby being beneficial to obtaining a complete alumina coating.
In an alternative embodiment, the transition layer has a thickness of 20-50 μm.
Alternatively, the thickness of the transition layer may be any value between 20 μm, 30 μm, 40 μm, 50 μm, or 20-50 μm.
If the thickness of the transition layer is too thin, partial areas may not be completely coated, and the subsequent stripping of the surface layer alumina is affected; the transition layer need not be made too thick in view of cost and efficiency.
In an alternative embodiment, the particle size of the aluminum powder and the alumina ceramic powder in the raw material of the transition layer is 10-30 μm independently.
The powder material has the advantages of fine granularity, poor fluidity, adverse effect on the powder conveying effect in the plasma spraying process and uneven obtained coating structure; the transition layer prepared by the low-pressure plasma spraying is not compact in structure, the thermal stress generated after the subsequent heat treatment is oxidized is small, the thermal expansion mismatch effect is not obvious, and the stripping of the surface layer aluminum oxide coating is affected.
In an alternative embodiment, the alumina coating has a thickness of not less than 50 μm.
Too small a thickness of the alumina coating can result in cracking of the coating during stripping, failing to obtain a complete alumina coating.
In an alternative embodiment, the heat treatment comprises:
and placing the substrate with the composite coating in a heating device for heating.
In an alternative embodiment, the heat treatment is carried out at a temperature of 800-1000 ℃ for a time of 3-6 hours.
If the heat treatment temperature is too low, the metal Al is insufficiently oxidized; when the heat treatment temperature is too high, metal Al is melted, and in addition, the matrix material cannot bear the too high temperature, so that the matrix material is damaged; too short a heat treatment time cannot ensure sufficient oxidation of the metallic Al. Therefore, the heat treatment temperature and the heat treatment time need to be strictly controlled, which is favorable for generating enough heat stress so as to enable the alumina coating to be better stripped.
Alternatively, the temperature of the heat treatment may be 800 ℃, 900 ℃, 1000 ℃, or any value between 800 and 1000 ℃ and the time may be 3 hours, 4 hours, 5 hours, 6 hours, or any value between 3 and 6 hours.
In an alternative embodiment, the cooling comprises:
and immediately putting the sample after the heat treatment into water for ultrasonic treatment until the alumina coating is peeled off.
In an alternative embodiment, the water temperature is 0-10 ℃.
Alternatively, the temperature of the water may be any value between 0 ℃, 1 ℃, 2 ℃, 3 ℃, 4 ℃, 5 ℃, 6 ℃, 7 ℃, 8 ℃, 9 ℃, 10 ℃, or 0-10 ℃.
In an alternative embodiment, the frequency of the sonication is in the range of 20-80kHz.
Alternatively, the frequency of the ultrasonic treatment may be 20kHz, 30kHz, 40kHz, 50kHz, 60kHz, 70kHz, 80kHz, or any value between 20 and 80kHz.
The high-temperature sample is rapidly cooled, and the alumina coating can be rapidly peeled off by utilizing a larger temperature difference and combining ultrasonic treatment with specific frequency.
In an alternative embodiment, the density of the transition layer is 97-99%.
Alternatively, the density of the transition layer may be any value between 97%, 98%, 99% or 97-99%.
The proper compactness can make the coating interface more easily generate larger thermal stress mismatch (amplification effect), thereby stripping the surface layer alumina ceramic coating and obtaining the complete alumina coating.
Embodiments of the present application will be described in detail below with reference to specific examples, but it will be understood by those skilled in the art that the following examples are only for illustration of the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a method for obtaining an alumina coating detection sample, which specifically comprises the following steps:
(1) Metal Al powder and Al 2 O 3 Fully and uniformly mixing the ceramic powder to obtain Al mixed Al 2 O 3 Spraying a powder material on the transition layer; adopting a low-pressure plasma spraying process to uniformly mix Al powder and Al 2 O 3 Powder spraying forms a transition layer on the high temperature alloy. Wherein Al is mixed with Al 2 O 3 The chemical components of the spraying material are as follows: the content of the metal Al powder is 5wt percent, and the balance is Al 2 O 3 Ceramic powder, al powder and Al 2 O 3 The granularity of the ceramic powder is 15-30 μm, and the thickness of the transition layer is 20 μm. The spraying technological parameters of the transition layer are as follows: the vacuum chamber pressure is 1.5 mbar, the power is 120kW, the spraying distance is 900mm, the Ar gas flow is 110slpm, the He flow is 120slpm, and the powder feeding speed is 20g/min.
(2) Spraying pure Al on the surface of the transition layer prepared in the step (1) 2 O 3 Coating to obtain Al mixed Al 2 O 3 Transition layer and pure Al 2 O 3 A double-layer structure coating of the surface layer. Wherein, pure Al 2 O 3 The coating thickness was 300 μm. Al (Al) 2 O 3 The spraying technological parameters of the layer are as follows: spraying power 35kW, ar flow 38slpm, H 2 The flow rate is 13slpm, the powder feeding rate is 20g/min, and the spraying distance is 100mm.
(3) And carrying out high-temperature heat treatment on the sample with the double-layer structure coating, and rapidly cooling the sample after heat treatment, so that the surface layer alumina ceramic coating can be completely peeled off, and the complete alumina ceramic coating is obtained. The heat treatment process parameters of the samples were as follows: the heat treatment temperature is 1000 ℃, and the heat treatment time is 3 hours; the cooling process parameters of the test specimens were as follows: the high-temperature heating state coating is rapidly placed into low temperature water at 0 ℃ and is subjected to ultrasonic treatment, and the ultrasonic frequency is 20KHz. Finally, the peeled alumina coating is obtained.
A physical diagram of the resulting alumina coating is shown in FIG. 1.
The appearance of the aluminum oxide coating peeled by the method is observed and analyzed, the appearance of the coating is complete, the cracking phenomenon does not occur, the chemical components of the peeled aluminum oxide coating are tested and analyzed, and the coating chemistry is that: al (Al) 2 O 3 （wt%）≥99.9%, na (wt%): 0.004, mg (wt%): 0.001, K (wt%): 0.002, ca (wt%): 0.004, fe (wt%): 0.002, the alumina coating has low impurity content and high purity.
Example 2
The embodiment provides a method for obtaining an alumina coating detection sample, which specifically comprises the following steps:
(1) Metal Al powder and Al 2 O 3 Fully and uniformly mixing the ceramic powder to obtain Al mixed Al 2 O 3 Spraying a powder material on the transition layer; adopting a low-pressure plasma spraying process to uniformly mix Al powder and Al 2 O 3 Powder spraying forms a transition layer on the substrate. Wherein Al is mixed with Al 2 O 3 The chemical components of the spraying material are as follows: the content of the metal Al powder is 5wt percent, and the balance is Al 2 O 3 Ceramic powder, al powder and Al 2 O 3 The granularity of the ceramic powder is 15-30 μm, and the thickness of the transition layer is 20 μm. The spraying technological parameters of the transition layer are as follows: the vacuum chamber pressure is 2.0 mbar, the power is 100kW, the spraying distance is 800mm, the Ar gas flow is 90slpm, the He flow is 100slpm, and the powder feeding speed is 15g/min.
(2) Spraying pure Al on the surface of the transition layer prepared in the step (1) 2 O 3 Coating to obtain Al mixed Al 2 O 3 Transition layer and pure Al 2 O 3 A double-layer structure coating of the surface layer. Wherein, pure Al 2 O 3 The coating thickness was 50 μm. Al (Al) 2 O 3 The spraying technological parameters of the layer are as follows: spraying power 35kW, ar flow 38slpm, H 2 The flow rate is 13slpm, the powder feeding rate is 20g/min, and the spraying distance is 100mm.
(3) And carrying out high-temperature heat treatment on the sample with the double-layer structure coating, and rapidly cooling the sample after heat treatment, so that the surface layer alumina ceramic coating can be completely peeled off, and the complete alumina ceramic coating is obtained. The heat treatment process parameters of the samples were as follows: the heat treatment temperature is 1000 ℃, and the heat treatment time is 3 hours; the cooling process parameters of the test specimens were as follows: the high-temperature heating state coating is rapidly placed into low temperature water at 0 ℃ and is subjected to ultrasonic treatment, and the ultrasonic frequency is 20KHz. Finally, the peeled alumina coating is obtained.
Example 3
The embodiment provides a method for obtaining an alumina coating detection sample, which specifically comprises the following steps:
(1) Metal Al powder and Al 2 O 3 Fully and uniformly mixing the ceramic powder to obtain Al mixed Al 2 O 3 Spraying a powder material on the transition layer; adopting a low-pressure plasma spraying process to uniformly mix Al powder and Al 2 O 3 Powder spraying forms a transition layer on the substrate. Wherein Al is mixed with Al 2 O 3 The chemical components of the spraying material are as follows: the content of the metal Al powder is 5wt percent, and the balance is Al 2 O 3 Ceramic powder, al powder and Al 2 O 3 The granularity of the ceramic powder is 15-30 μm, and the thickness of the transition layer is 20 μm. The spraying technological parameters of the transition layer are as follows: the vacuum chamber pressure is 2.0 mbar, the power is 80kW, the spraying distance is 700mm, the Ar gas flow is 80slpm, the He flow is 70slpm, and the powder feeding speed is 10g/min.
(2) Spraying pure Al on the surface of the transition layer prepared in the step (1) 2 O 3 Coating to obtain Al mixed Al 2 O 3 Transition layer and pure Al 2 O 3 A double-layer structure coating of the surface layer. Wherein, pure Al 2 O 3 The coating thickness was 50 μm. Al (Al) 2 O 3 The spraying technological parameters of the layer are as follows: spraying power 35kW, ar flow 38slpm, H 2 The flow rate is 13slpm, the powder feeding rate is 20g/min, and the spraying distance is 100mm.
(3) And carrying out high-temperature heat treatment on the sample with the double-layer structure coating, and rapidly cooling the sample after heat treatment, so that the surface layer alumina ceramic coating can be completely peeled off, and the complete alumina ceramic coating is obtained. The heat treatment process parameters of the samples were as follows: the heat treatment temperature is 1000 ℃, and the heat treatment time is 3 hours; the cooling process parameters of the test specimens were as follows: the high-temperature heating state coating is rapidly placed into low temperature water at 0 ℃ and is subjected to ultrasonic treatment, and the ultrasonic frequency is 20KHz. Finally, the peeled alumina coating is obtained.
Comparative example 1
Comparative example 1 differs from example 3The method comprises the following steps: in comparative example 1, the uniformly mixed Al powder and Al powder were applied by an atmospheric plasma spray process 2 O 3 Powder spraying forms a transition layer on the substrate. Wherein Al is mixed with Al 2 O 3 The chemical components of the spraying material are as follows: the content of the metal Al powder is 5wt percent, and the balance is Al 2 O 3 Ceramic powder, al powder and Al 2 O 3 The granularity of the ceramic powder is 15-30 μm, and the thickness of the transition layer is 20 μm. The spraying technological parameters of the transition layer are as follows: the spraying power is 32kW, the main air flow is 32slpm, the auxiliary air flow is 11 slpm, the powder feeding speed is 30g/min, and the spraying distance is 110mm. The remainder remained the same as in example 3.
The density of the transition layer prepared by the process is lower than 87%, and after the obtained composite coating is subjected to heat treatment and cooling, the generated thermal expansion mismatch degree is smaller, so that the alumina coating is difficult to peel off.
Comparative example 2
Comparative example 2 differs from example 3 in that: in comparative example 2, during the preparation of the transition layer, metallic Al powder and Al were mixed 2 O 3 Fully and uniformly mixing the ceramic powder to obtain Al mixed Al 2 O 3 Spraying a powder material on the transition layer; adopting a low-pressure plasma spraying process to uniformly mix Al powder and Al 2 O 3 Powder spraying forms a transition layer on the substrate. Wherein Al is mixed with Al 2 O 3 The chemical components of the spraying material are as follows: the content of the metal Al powder is 1wt%, and the balance is Al 2 O 3 The ceramic powder was the same as in example 3.
The transition layer prepared by the process has low aluminum content, and the generated thermal expansion mismatch degree is small after the obtained composite coating is subjected to heat treatment and cooling, so that the aluminum oxide coating is difficult to strip.
Comparative example 3
Comparative example 3 differs from example 3 in that: in comparative example 3, in the preparation process of the transition layer, the spraying process parameters of the transition layer are as follows: the vacuum chamber pressure was 2.0 mbar, power 80kW, spray distance 700mm, ar gas flow 80slpm, he flow 70slpm, powder feed rate 50g/min, and the remainder remained consistent with example 3.
The density of the transition layer prepared by the process is lower than 89%, and after the obtained composite coating is subjected to heat treatment and cooling, the generated thermal expansion mismatch degree is smaller, so that the alumina coating is difficult to peel off.
Comparative example 4
Comparative example 4 differs from example 3 in that: in comparative example 4, in the preparation process of the transition layer, the spraying process parameters of the transition layer are as follows: the vacuum chamber pressure was 2.0 mbar, power 35kW, spray distance 700mm, ar gas flow 80slpm, he flow 70slpm, powder feed rate 10g/min, and the remainder remained consistent with example 3.
The density of the transition layer prepared by the process is lower than 88%, and after the obtained composite coating is subjected to heat treatment and cooling, the generated thermal expansion mismatch degree is smaller, so that the alumina coating is difficult to peel off.
Comparative example 5
Comparative example 5 differs from example 3 in that: in comparative example 5, al powder and Al during the preparation of the transition layer 2 O 3 The particle size of the ceramic powder is 45-90 μm, and the thickness of the transition layer is 50 μm. The remainder remained the same as in example 3.
The density of the transition layer prepared by the process is lower than 87%, and after the obtained composite coating is subjected to heat treatment and cooling, the generated thermal expansion mismatch degree is smaller, so that the alumina coating is difficult to peel off.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.
Claims (10)
1. A method of obtaining an alumina coating test sample, comprising:
preparing a transition layer on the surface of a substrate by adopting a low-pressure plasma spraying method, preparing an alumina coating on the surface of the transition layer by adopting an atmospheric plasma spraying method, performing heat treatment and cooling stripping on the obtained composite coating to obtain an alumina coating detection sample;
the transition layer comprises 5-10% of aluminum powder by mass percent and the balance of aluminum oxide ceramic powder; the technological parameters of the low-pressure plasma spraying method comprise: the pressure of the vacuum chamber is 1.5-2.0 mbar, the power is 80-120kW, the spraying distance is 700-900mm, ar gas flow is 80-110slpm, he gas flow is 60-150slpm, and the powder feeding speed is 10-20g/min;
the raw materials of the alumina coating are pure alumina ceramic powder, and the technological parameters of the atmospheric plasma spraying method comprise: spraying power is 35kW-42kW, ar gas flow is 38-41slpm, H 2 The air flow is 13-14 slpm, the powder feeding speed is 20-40g/min, and the spraying distance is 100-120mm.
2. The method of obtaining a test sample of alumina coating according to claim 1, wherein the transition layer has a thickness of 20-50 μm.
3. The method for obtaining a sample for alumina coating according to claim 1, wherein the particle size of the aluminum powder and the alumina ceramic powder in the raw material of the transition layer is 10 to 30 μm independently.
4. The method for obtaining a test sample of an alumina coating according to claim 1, wherein the thickness of the alumina coating is not less than 50 μm.
5. The method of obtaining an alumina coating test sample of claim 1, wherein the heat treating comprises:
and placing the substrate with the composite coating in a heating device for heating.
6. The method for obtaining a test sample of an alumina coating according to claim 5, wherein the heat treatment is performed at a temperature of 800-1000 ℃ for a time of 3-6 hours.
7. The method of obtaining an alumina coating test sample of claim 1, wherein the cooling comprises:
and immediately putting the sample after the heat treatment into water for ultrasonic treatment until the alumina coating is peeled off.
8. The method for obtaining a test sample of an alumina coating according to claim 7, wherein the water is at a temperature of 0-10 ℃.
9. The method for obtaining a test sample of an alumina coating according to claim 7, wherein the frequency of the ultrasonic treatment is 20-80kHz.
10. The method of obtaining a test sample of an alumina coating according to any one of claims 1 to 9, wherein the density of the transition layer is 97 to 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311490485.2A CN117230402B (en) | 2023-11-10 | 2023-11-10 | Method for obtaining alumina coating detection sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311490485.2A CN117230402B (en) | 2023-11-10 | 2023-11-10 | Method for obtaining alumina coating detection sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117230402A CN117230402A (en) | 2023-12-15 |
| CN117230402B true CN117230402B (en) | 2024-04-02 |
Family
ID=89088305
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311490485.2A Active CN117230402B (en) | 2023-11-10 | 2023-11-10 | Method for obtaining alumina coating detection sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117230402B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637030A (en) * | 2015-10-28 | 2017-05-10 | 三菱日立电力系统株式会社 | Thermal barrier coating stripping method and thermal barrier coating repair method |
| CN112697550A (en) * | 2020-11-18 | 2021-04-23 | 天津力神电池股份有限公司 | Sample preparation method for pole piece magnetic substance test |
| CN113640117A (en) * | 2021-08-13 | 2021-11-12 | 中国航发沈阳黎明航空发动机有限责任公司 | Method for testing elastic modulus of coating |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109682702B (en) * | 2018-12-10 | 2020-03-20 | 湘潭大学 | Turbine blade thermal barrier coating working condition simulation experiment test system |
-
2023
- 2023-11-10 CN CN202311490485.2A patent/CN117230402B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637030A (en) * | 2015-10-28 | 2017-05-10 | 三菱日立电力系统株式会社 | Thermal barrier coating stripping method and thermal barrier coating repair method |
| CN112697550A (en) * | 2020-11-18 | 2021-04-23 | 天津力神电池股份有限公司 | Sample preparation method for pole piece magnetic substance test |
| CN113640117A (en) * | 2021-08-13 | 2021-11-12 | 中国航发沈阳黎明航空发动机有限责任公司 | Method for testing elastic modulus of coating |
Non-Patent Citations (1)
| Title |
|---|
| 热障涂层服役环境模拟实验方法;师俊东;何箐;;航空材料学报;20180404(02);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117230402A (en) | 2023-12-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2133422C (en) | Process for producing a strong bond between copper layes and ceramic | |
| JP4740932B2 (en) | Method for forming black yttrium oxide sprayed coating and black yttrium oxide sprayed coating member | |
| JP2004332081A (en) | Plasma resistant member, and its production method | |
| JP2009235558A (en) | Member coated with aluminum nitride by thermal splaying and its manufacturing method | |
| CN106591820B (en) | A kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating | |
| CN111235511A (en) | Preparation method of multi-element ceramic composite coating | |
| CN117230402B (en) | Method for obtaining alumina coating detection sample | |
| CN113462911B (en) | Preparation method of tough corrosion-resistant AZ80 magnesium alloy | |
| CN110872713B (en) | Y/Y2O3Cold spraying preparation method of metal ceramic protective coating | |
| JP5412290B2 (en) | Corrosion resistant material | |
| CN114231917B (en) | Preparation method of high-purity rare earth and alloy target material | |
| JP3829935B2 (en) | High voltage resistance member | |
| CN110791726B (en) | Method for spraying abradable coating capable of reducing abradable component loss rate | |
| CN114686794A (en) | Preparation method of nano YSZ/NiCoCrAlYTa composite coating on TiAl alloy surface | |
| Wang et al. | Improvement of Microstructure and Properties of Cu Coatings Prepared with Cold Spraying by Plasma Heating | |
| CN115094365B (en) | High-temperature acid corrosion resistant insulating coating and preparation method thereof | |
| CN111455370A (en) | Preparation method of cold spraying metal deposit body with high deposition efficiency and high performance | |
| Yamada et al. | Influence of substrate materials upon fabrication of aluminum nitride coatings by reactive RF plasma spraying | |
| RU2219145C1 (en) | Method for metallic coating of ceramics under soldering | |
| CN114686803B (en) | Ternary nitride coating prepared by microwave plasma chemical vapor deposition and method thereof | |
| Mrdak et al. | Characterization of vacuum plasma spray VPS-W coating deposited on stainless steel substrates | |
| CN114686872A (en) | Strong corrosion-resistant Ta alloy coating and preparation method thereof | |
| CN115896775A (en) | Copper-coated graphite modified copper-based gradient composite material and preparation method thereof | |
| JP3059250B2 (en) | Method for forming composite of alumina and aluminum nitride | |
| CN117821884A (en) | Adhesive layer powder material suitable for atmospheric plasma spraying preparation and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |