CN107442384B - Preparation method of nano mullite thermal shock resistant ceramic coating - Google Patents

Preparation method of nano mullite thermal shock resistant ceramic coating Download PDF

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CN107442384B
CN107442384B CN201710494899.0A CN201710494899A CN107442384B CN 107442384 B CN107442384 B CN 107442384B CN 201710494899 A CN201710494899 A CN 201710494899A CN 107442384 B CN107442384 B CN 107442384B
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CN107442384A (en
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张博
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Chongqing Zhengfeng Electronic Co ltd
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    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
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    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
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    • C04B35/185—Mullite 3Al2O3-2SiO2
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The invention relates to the technical field of functional ceramics, in particular to a preparation method of a nano mullite thermal shock resistant ceramic coating; comprises 1) selecting steel as a substrate, putting a sample piece into a beaker of acetone, taking out after ultrasonic treatment, and carrying out sand blasting treatment by using brown corundum. 2) Dispersing the nano mullite powder in distilled water to obtain a suspension A, and oscillating the suspension A by an ultrasonic generator; 3) adding silica sol into the suspension A and oscillating in an ultrasonic generator; 4) preheating a high-temperature electric furnace, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace, immersing the heated sample piece into the suspension B, and oscillating in an ultrasonic generator; 5) continuously placing the sample subjected to the ultrasonic treatment into a high-temperature electric furnace, immersing the heated sample piece into the suspension B, taking out the immersed sample, oscillating the immersed sample in an ultrasonic generator, and repeating the step until the required coating thickness is reached; the preparation method of the nano mullite thermal shock resistant ceramic coating has the advantages of simple process, low cost and excellent product performance.

Description

Preparation method of nano mullite thermal shock resistant ceramic coating
Technical Field
The invention belongs to the technical field of functional ceramics, and particularly relates to a preparation method of a nano mullite thermal shock resistant ceramic coating.
Background
Background art: with the continuous development of manufacturing industry, some parts on machinery are damaged by high temperature, temperature change, friction, impact, corrosion and the like for a long time due to the severe working environment, the requirements on the performance of the parts are higher and higher, and the parts are wear-resistant, corrosion-resistant, high-temperature-resistant and the like, but the requirements are difficult to meet only by the treatment of steel, so people begin to reform the surfaces of the parts.
The ceramic coating prepared on the metal surface can have various special properties, such as wear resistance, corrosion resistance, high temperature resistance, fatigue resistance, radiation resistance, special optical, electrical, thermal, magnetic and other properties of the reinforced coating, so that the metal-based ceramic coating technology is increasingly paid more attention as one of important means of material surface treatment technology. In order to more fully exert the advantages of the metal ceramic composite coating, a novel green and environment-friendly coating technology is further developed, the variety of the coating is enriched, the high-tech and industrial modernization high-speed development is adapted, and the level of the modern manufacturing industry is improved.
Because the superfine material (nano material, submicron material, etc.) has special surface effect, small-size effect and quantum effect, when a certain geometric dimension of a certain phase in the material reaches the superfine crystal grade, the structure shows special physical, chemical, electrical, magnetic, thermal, optical and other properties, and has incomparable superiority in the aspects of strength, copper property, corrosion resistance, wear resistance, thermal barrier, thermal fatigue resistance, etc. compared with the large-size crystal grain material. The mullite has an expansion coefficient of 4.4-5.5 × 10–6The melting point is 2000 ℃, the temperature is 1800 ℃ and the corundum phase is still stable, and the corundum phase is decomposed into corundum and liquid phase at 1810 ℃. The mullite is used as a potential reinforcing and toughening material of a ceramic-based, metal-based and polymer-based composite material, and can be widely applied to the fields of high-temperature structural materials, friction materials and the like. Has better high-temperature thermal stability and high-temperature oxidation resistance.
The preparation methods of the ceramic coating are various so far, and mainly comprise the following steps: plasma spraying, sol-gel methods, physical vapor deposition, chemical vapor deposition, and the like. The arc theta in the process of preparing the ceramic coating by plasma spraying is as high as more than 1000 ℃, so high residual thermal stress exists at the interface of the metal sample sheet and the coating during cooling, and the material is usually damaged at the interface due to the concentration of interface defects, which is not favorable for the stability of the coating, the interface of the coating and the sample sheet is mainly mechanically occluded, and the bonding strength is correspondingly limited. In addition, the difference of physical properties between the plasma spraying coating and the metal sample piece is larger, and larger internal stress can be generated at the interface, thereby reducing the bonding strength of the coating and the sample piece [ ZHAO X, LiuX, Ding C, et al2,coating aftersodium hydroxide treatment[J].Surface&Coating Technology.2006,200(18-19):5487-5492.]Coatings prepared by sol-gel methods are prone to surface cracking and have inadequate coating thickness [ Adraider Y, Pang Y X, Nabhani F, et al].Interceram InternationalCeramic Review,2013,39(8):9665-9670.]The physical vapor deposition and chemical vapor deposition are adopted, the process is complex and needs to be carried out in a vacuum environment, and the phenomenon of growth and agglomeration of micro-nano particles is easily caused in the coating construction process [ Rujisominapa J, SuringS, Wong panya P.A. comprehensive Study of Wear and oxidation and of End Mill Coated by PVD Coatings [ J].Advanced MaterialsResearch,2013,785-786:858.]Chemical vapor deposition TiN thin film and wear-resisting property thereof]Aeronautical newspaper, 2008, 29 (6): 1687-1691.]。
Disclosure of Invention
The invention aims to provide a method for preparing a nano mullite ceramic coating by adopting an ultrasonic-hot dipping method, overcomes the defects in the prior art, has important significance for protecting metal parts in the manufacturing industry, and has the advantages of simple process, low cost and excellent product performance.
The preparation method of the nano mullite thermal shock resistant ceramic coating comprises the following steps: 1) the base material is made of steel, and is processed into a sample piece with a required size, the sample piece is placed into a beaker filled with acetone in advance, the sample piece is taken out after ultrasonic treatment for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes. 2) Dispersing the nano mullite powder in 200-400 ml of distilled water to obtain a suspension A, ultrasonically oscillating the suspension A for 20-40 min by using an ultrasonic generator, and then magnetically stirring for 3-5 h, wherein the concentration of the nano mullite powder in the suspension A is 100-200 g/L. 3) Adding 40-80 ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into an ultrasonic generator, ultrasonically oscillating for 30-60 min, and then magnetically stirring for 3-5 h while heating at 50-60 ℃; 4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 15-20 min, taking out, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 20-30 s, and oscillating in an ultrasonic generator for 1-2 min; 5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 15-20 min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 20-30 s, oscillating the immersed sample piece in an ultrasonic generator for 1-2 min, and repeating the step until the required coating thickness is reached, thereby obtaining the thermal shock resistant mullite ceramic coating sample.
The invention has the advantages that: 1) the thermal shock resistant mullite ceramic coating prepared by the invention has no cracks on the surface and high bonding strength with a sample piece; 2) the thermal shock resistant mullite ceramic coating with controllable structure thickness and good performance can be obtained at low temperature; 3) the preparation method has the advantages of simple preparation process, convenient operation, easily obtained raw materials and lower preparation cost.
It can be seen from fig. 1 that the mullite coating prepared by the invention is composed of a single mullite crystal phase, and the surface compactness of the prepared coating is good and has no obvious microcrack (a is a back scattering pattern for the surface of the prepared coating, and b is a back scattering pattern under high multiplying power of the prepared coating), and it can be seen from fig. 3 that after the prepared coating is subjected to thermal shock for 50 times at 1200 ℃, the mass loss rate is about 1%, and the thermal shock resistance of the coating is good.
Furthermore, the purity of the nano mullite powder is more than or equal to 99.9%, and the average particle size is 50-70 nm.
Further, in the silica sol, SiO2The solid content of the (B) is 30-31%.
Further, the power of the ultrasonic generator in the steps 1) to 5) is 800-.
Further, in step 2), 300ml of distilled water was used.
Further, in the step 3), 50ml to 70ml of medium silica sol is added.
Further, 60ml of medium silica sol was added in step 3).
Further, in step 1), the size of the sample piece was 30mm × 30mm × 5 mm.
Further, in the step 1), 45 # steel is selected as the base material.
Drawings
FIG. 1 is an XRD pattern of the surface of a mullite overcoat made in example 1 of the present invention;
FIG. 2 is a surface backscattering plot of a mullite coating made in accordance with example 1 of the present invention;
FIG. 3 is a graph of the thermal shock resistance of the mullite coating of this invention made in example 1 at 1200 ℃.
Detailed Description
Example 1
1) The base material is No. 45 steel, processed into a sample piece with the size of 30mm multiplied by 5mm, the sample piece is placed into a beaker filled with 300mL of acetone in advance, and is taken out after being subjected to ultrasonic treatment in an 800W ultrasonic generator for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes.
2) Dispersing 20g of commercially available nano mullite powder in 200ml of distilled water to obtain a suspension A, ultrasonically oscillating the suspension A for 20min by using an 800W ultrasonic generator, and then magnetically stirring for 3h, wherein the concentration of the nano mullite powder in the suspension A is 100 g/L.
3) Adding 40ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into an 800W ultrasonic generator, ultrasonically oscillating for 30min, and then heating while magnetically stirring for 3h, wherein the heating temperature is 50 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 15min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample after 20s, and oscillating the immersed sample in an 800W ultrasonic generator for 1 min;
5) and (3) continuously placing the sample piece subjected to ultrasonic treatment into a high-temperature electric furnace at 200 ℃, keeping the temperature for 15min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 20s, oscillating the immersed sample piece in an 800W ultrasonic generator for 1min, and repeating the step until the required coating thickness is reached to obtain the nano mullite coating sample.
Example 2
1) The base material is No. 45 steel, processed into a sample piece with the size of 30mm multiplied by 5mm, the sample piece is placed into a beaker filled with 300mL of acetone in advance, and is taken out after being subjected to ultrasonic treatment in a 900W ultrasonic generator for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes.
2) Dispersing 37.5g of commercially available nano mullite powder in 250ml of distilled water to obtain a suspension A, ultrasonically oscillating the suspension A for 25min by using a 900W ultrasonic generator, and then magnetically stirring for 2.5h, wherein the concentration of the nano mullite powder in the suspension A is 150 g/L.
3) Adding 50ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into a 900W ultrasonic generator, ultrasonically oscillating for 35min, and then heating while magnetically stirring for 3.5h at the heating temperature of 55 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 16min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample after 25s, and oscillating the immersed sample in a 900W ultrasonic generator for 1 min;
5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 16min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 25s, oscillating the immersed sample piece in a 900W ultrasonic generator for 1min, and repeating the step until the required coating thickness is reached to obtain the nano mullite ceramic coating sample.
Example 3
1) The base material is No. 45 steel, processed into a sample piece with the size of 30mm multiplied by 5mm, the sample piece is placed into a beaker filled with 300mL of acetone in advance, and is taken out after being subjected to ultrasonic treatment in a 1000W ultrasonic generator for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes.
2) 60g of commercially available nano mullite powder is dispersed in 300ml of distilled water to obtain a suspension A, the suspension A is subjected to ultrasonic oscillation for 30min by using a 1000W ultrasonic generator, and then the suspension A is stirred for 3h by magnetic force, wherein the concentration of the nano mullite powder in the suspension A is 200 g/L.
3) Adding 60ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into a 1000W ultrasonic generator, ultrasonically oscillating for 40min, and then heating while magnetically stirring for 4h at the heating temperature of 55 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 17min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample after 30s, and oscillating the immersed sample in a 1000W ultrasonic generator for 1 min;
5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 17min, taking out, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 30s, oscillating in a 1000W ultrasonic generator for 1min, and repeating the step until the required coating thickness is reached to obtain the nano mullite ceramic coating sample.
Example 4
1) The base material is No. 45 steel, processed into a sample piece with the size of 30mm multiplied by 5mm, the sample piece is placed into a beaker filled with 300mL of acetone in advance, and is taken out after being subjected to ultrasonic treatment in an 1100W ultrasonic generator for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes.
2) 70g of commercially available nano mullite powder is dispersed in 350ml of distilled water to obtain a suspension A, the suspension A is subjected to ultrasonic oscillation for 35min by using an 1100W ultrasonic generator, and then the suspension A is magnetically stirred for 4.5h, wherein the concentration of the nano mullite powder in the suspension A is 200 g/L.
3) Adding 70ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into a 1100W ultrasonic generator, ultrasonically oscillating for 50min, and then heating while magnetically stirring for 4h at the heating temperature of 55 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 18min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample after 30s, and oscillating the immersed sample in an 1100W ultrasonic generator for 1 min;
5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 18min, taking out, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 30s, oscillating in an 1100W ultrasonic generator for 2min, and repeating the step until the required coating thickness is reached to obtain the nano mullite ceramic coating sample.
Example 5
1) The base material is No. 45 steel, processed into a sample piece with the size of 30mm multiplied by 5mm, the sample piece is placed into a beaker filled with 300mL of acetone in advance, and is taken out after being subjected to ultrasonic treatment in a 1200W ultrasonic generator for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes.
2) 80g of commercially available nano mullite powder is dispersed in 400ml of distilled water to obtain a suspension A, the suspension A is subjected to ultrasonic oscillation for 35min by using a 1200W ultrasonic generator, and then the suspension A is stirred for 4.5h by magnetic force, wherein the concentration of the nano mullite powder in the suspension A is 200 g/L.
3) Adding 80ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into a 1200W ultrasonic generator, ultrasonically oscillating for 50min, and then heating while magnetically stirring for 4h at the heating temperature of 55 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 20min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample after 30s, and oscillating the immersed sample in a 1200W ultrasonic generator for 1 min;
5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 20min, taking out, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 30s, oscillating for 2min in a 1200W ultrasonic generator, and repeating the step until the required coating thickness is reached to obtain the nano mullite ceramic coating sample.
Example 6
1) The base material is No. 45 steel, processed into a sample piece with the size of 30mm multiplied by 5mm, the sample piece is placed into a beaker filled with 300mL of acetone in advance, and is taken out after being subjected to ultrasonic treatment in a 1000W ultrasonic generator for 30min, and after the sample piece is dried, the sample piece is subjected to sand blasting treatment by using brown corundum with 24 meshes.
2) 60g of commercially available nano mullite powder is dispersed in 400ml of distilled water to obtain a suspension A, the suspension A is subjected to ultrasonic oscillation for 35min by using a 1200W ultrasonic generator, and then the suspension A is magnetically stirred for 5h, wherein the concentration of the nano mullite powder in the suspension A is 150 g/L.
3) Adding 80ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into a 1000W ultrasonic generator, ultrasonically oscillating for 60min, and then heating while magnetically stirring for 5h at the heating temperature of 60 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 20min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample after 30s, and oscillating the immersed sample in a 1000W ultrasonic generator for 2 min;
5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 20min, taking out, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 30s, oscillating for 2min in a 1000W ultrasonic generator, and repeating the step until the required coating thickness is reached to obtain the nano mullite ceramic coating sample.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.

Claims (9)

1. A preparation method of a nano mullite thermal shock resistant ceramic coating is characterized by comprising the following steps: comprises the following steps
1) Selecting steel as a base material, processing the steel into a sample piece with a required size, putting the sample piece into a beaker which is pre-filled with 300ml of acetone, carrying out ultrasonic treatment for 30min, taking out the sample piece, drying the sample piece, and carrying out sand blasting treatment by using brown corundum with 24 meshes;
2) dispersing 20g-80g of nano mullite powder in 200 ml-400 ml of distilled water to obtain a suspension A, ultrasonically oscillating the suspension A for 20-40 min by using an ultrasonic generator, and then magnetically stirring for 3-5 h, wherein the concentration of the nano mullite powder in the suspension A is 100-200 g/L;
3) adding 40-80 ml of silica sol into the suspension A to obtain a suspension B, placing the suspension B into an ultrasonic generator, ultrasonically oscillating for 30-60 min, and then magnetically stirring for 3-5 h while heating at 50-60 ℃;
4) preheating a high-temperature electric furnace to 200 ℃ in advance, keeping the temperature at 200 ℃, taking out the sample piece subjected to sand blasting, placing the sample piece into the electric furnace at 200 ℃, keeping the temperature for 15-20 min, taking out, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 20-30 s, and oscillating in an ultrasonic generator for 1-2 min;
5) and (3) continuously placing the sample piece subjected to the ultrasonic treatment into a high-temperature electric furnace at the temperature of 200 ℃, keeping the temperature for 15-20 min, taking out the sample piece, immersing the heated sample piece into the suspension B, taking out the immersed sample piece after 20-30 s, oscillating the immersed sample piece in an ultrasonic generator for 1-2 min, and repeating the step until the required coating thickness is reached, thereby obtaining the thermal shock resistant mullite ceramic coating sample.
2. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: the purity of the nano mullite powder is more than or equal to 99.9%, and the average particle size is 50-70 nm.
3. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: in the silica sol, SiO2The solid content of the (B) is 30-31%.
4. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: the power of the ultrasonic generator in the steps 1) to 5) is 800-1200W.
5. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: in step 2), 300ml of distilled water was used.
6. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: in the step 3), 50ml to 70ml of silica sol is added.
7. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 6, which is characterized in that: in step 3), 60ml of silica sol was added.
8. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: in step 1), the size of the test piece was 30mm × 30mm × 5 mm.
9. The preparation method of the nano mullite thermal shock resistant ceramic coating according to claim 1, which is characterized in that: in the step 1), the base material is No. 45 steel.
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