CN109881145B - Preparation method of chromium-rich high-temperature corrosion-resistant coating deposited by slurry method - Google Patents
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Abstract
A preparation method of a chromium-rich high-temperature corrosion-resistant coating deposited by a slurry method comprises the steps of preheating a workpiece, and coating chromizing slurry on the surface of the workpiece, wherein the thickness of the coating slurry layer is 0.1-5 mm; then drying and curing, and finally sintering to obtain the chromium-rich high-temperature corrosion-resistant coating; the chromizing slurry comprises, by mass, 10-30% of a binder, 40-60% of a chromizing source, 2-10% of an activating agent, 5-20% of a filler and 10-30% of a diluent. The chromium-rich high-temperature corrosion-resistant coating deposited by the slurry method and the preparation method thereof can be applied to various metal parts such as carbon steel, austenitic stainless steel, high-temperature alloy and the like, are particularly suitable for large-scale pipeline metal parts, heterosexual metal parts, complex parts and the like, and have the advantages of strong practicability, wide application range, high chromizing efficiency, small pollution, moderate thickness, good metallurgical bonding with a matrix and difficult shedding.
Description
Technical Field
The invention belongs to the technical field of material surface coatings, and particularly relates to a preparation method of a chromium-rich high-temperature corrosion-resistant coating deposited by a slurry method.
Background
Thermal power generation accounts for more than 70% of the total generated energy in China, and the corrosion problem of the heating surface of a heat-resistant steel pipeline of a boiler is more prominent along with the trend of thermal power generation towards higher steam temperature and pressure (620-650 ℃/30-35 Mpa); in the actual production process, accidents caused by corrosion failure of boiler pipelines occur sometimes, and huge economic loss and potential safety hazards are caused to the nation and individuals, so that the development of the corrosion resisting technology suitable for the boiler pipelines of the power station has important practical significance under the new operation parameters of a boiler unit.
At present, the most common corrosion resisting technology is the technology of infiltrating corrosion resisting metal on the surface of the alloy, such as infiltrating Al, Si, chromium and the like; the Al-infiltrated alloy has excellent high-temperature oxidation resistance, but has small contribution to corrosion resistance; the Si-infiltrated layer is brittle and easy to crack. Chromium is the most effective element in corrosion resistance, the development of surface chromizing can effectively improve the formation of a protective oxide film on the surface of the alloy so as to improve the high-temperature corrosion resistance, and simultaneously, the high-temperature oxidation resistance and the wear resistance are both achieved, and the formed solid solution has good mechanical property and avoids the generation of brittle phases.
The chromizing technology for metal surfaces has been developed for decades, and the chromizing process is also diversified and generally divided into a powder embedding method, a gas phase method and a liquid phase method. The powder embedding method is realized by embedding a metal workpiece in chromizing agent powder and preserving heat for a long time (more than 4 hours) at high temperature, and has the problems of simple process, low powder utilization rate, low efficiency, high cost, serious dust pollution and the like. The gas-phase chromizing is to hang a workpiece on chromizing agent powder, introduce chlorine gas and the like to react with chromium powder to generate chromizing gas, and the gas is attached to the surface of the workpiece to form active chromium atoms and permeates into a substrate to form a chromizing layer; the method avoids the problems of dust pollution and the like, but the process is complex and requires to be carried out under vacuum, and meanwhile, the emission of toxic gas harms the human health. The liquid phase method generally puts chromium powder into molten salt, and forms a chromium diffusion layer through high-temperature heat preservation, but the molten salt is volatile at high temperature, and has great harm to workpieces, environment and the like. In addition, there are many other new chromizing methods such as mechanical energy-assisted chromizing, high-frequency electric spark chromizing, etc., but these chromizing processes are limited in chromizing efficiency and applicability to large-sized workpieces such as pipes, special-shaped parts, complex parts, etc., and thus there is a need for a new chromizing coating material and a preparation process suitable for various complex workpieces.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a chromium-rich high-temperature corrosion-resistant coating deposited by a slurry method, the method is suitable for metal parts such as various carbon steels, austenitic steels, high-temperature alloys and the like, and is particularly suitable for workpieces such as large boilers, oil and gas field pipeline workpieces, special-shaped parts, complex parts and the like, and the prepared chromium-impregnated coating has good quality, high efficiency and excellent corrosion resistance and oxidation resistance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a chromium-rich high-temperature corrosion-resistant coating deposited by a slurry method comprises the steps of preheating a workpiece, and coating chromizing slurry on the surface of the workpiece, wherein the thickness of the coating slurry layer is 0.1-5 mm; then drying and curing, and finally sintering to obtain the chromium-rich high-temperature corrosion-resistant coating; the chromizing slurry comprises, by mass, 10-30% of a binder, 40-60% of a chromizing source, 2-10% of an activating agent, 5-20% of a filler and 10-30% of a diluent.
The invention has the further improvement that the preheating temperature is 60-100 ℃ and the time is 30-60 min.
The invention has the further improvement that the adhesive is sodium silicate, the seepage source is pure chromium powder, the activating agent is sodium chloride, the filling agent is alumina, and the diluting agent is distilled water.
The invention further improves the preparation method of the chromizing slurry, which comprises the following steps: weighing 10-30% of sodium silicate, 40-60% of chromium powder, 2-10% of sodium chloride, 5-20% of alumina and 10-30% of distilled water in percentage by mass, and dividing the distilled water into three parts; dissolving sodium silicate in the first part of distilled water to obtain a sodium silicate solution, and dissolving sodium chloride in the second part of distilled water to obtain a sodium chloride solution; adding chromium powder into a sodium silicate solution, stirring uniformly, adding a sodium chloride solution, mixing uniformly, adding alumina, stirring uniformly, adding a third part of distilled water, and finally carrying out ball milling to obtain a chromizing slurry.
The ball milling method is further improved in that the ball milling is carried out in a star-type ball milling tank, the rotating speed is 350-400 r/min, and the ball milling time is 5-10 h.
The invention further improves the method that the chromizing slurry is applied to the surface of the workpiece in a spraying or brushing mode.
The further improvement of the invention is that the drying and curing adopt a sectional gradient curing process, which specifically comprises the following steps: pre-drying at 75-85 ℃ for 5-30 min, then drying at 140-160 ℃ for 30-60 min, and finally curing at 250-300 ℃ for 30-60 min.
The invention has the further improvement that the sintering temperature is 900-1100 ℃, and the time is 5-30 min.
The invention has the further improvement that during sintering, the temperature is increased from room temperature to 900-1100 ℃ at the temperature increase rate of more than 1000 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the rapid chromizing slurry is suitable for various metal workpieces with surfaces needing to be strengthened, comprises carbon steel, austenitic stainless steel, high-temperature alloy and other workpieces, can be used for preparing chromizing layers particularly for large boilers, oil and gas field pipeline workpieces, special-shaped parts, complex parts and the like, and has wide application range and strong practicability.
(2) The chromium-rich high-temperature corrosion-resistant coating deposited by the slurry method and the preparation method thereof do not need to be carried out under the protection of vacuum or atmosphere, the sintering process is simple, the sintering time is short, meanwhile, the chromium-permeated layer is high in preparation efficiency, small in pollution, moderate in thickness, high in hardness of more than 45HRC, good in wear resistance, and especially excellent in high-low temperature corrosion resistance and steam oxidation resistance.
Furthermore, the segmented curing process effectively solves the problems of microcracks and tiny holes generated by stress cracking of a slurry layer under a one-step drying curing method while ensuring the slurry curing, and the slurry is combined with the surface of a workpiece more compactly.
Furthermore, in order to prevent volatilization of components in the slurry at high temperature, rapid sintering diffusion chromizing is carried out on the workpiece in a rapid heating mode.
Drawings
FIG. 1 is a photograph showing the cross-sectional morphology of a Cr-rich HTC coating prepared on the surface of austenitic steel in example 5 of the present invention;
FIG. 2 is a photograph showing the cross-sectional morphology of the Cr-rich HTC corrosion-resistant coating prepared on the surface of the superalloy in example 9 of the present invention;
FIG. 3 shows the distribution of the Cr elements in the Cr-rich HTC corrosion-resistant coating prepared on the surface of the superalloy in example 9 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to the attached drawings.
The invention respectively takes large boiler pipes prepared from carbon steel, austenitic steel and high-temperature alloy as examples to prepare the chromium-infiltrated layer, and the specifications of the pipes are 55mm in outer diameter, 8mm in wall thickness and 4000mm in length.
The chromizing slurry of the invention: the adhesive comprises, by mass, 10-30% of sodium silicate as an adhesive, 40-60% of source-infiltrated pure chromium powder, 2-10% of sodium chloride as an activating agent, 5-20% of alumina as a filler and 10-30% of distilled water as a diluent.
The preparation method of the chromizing slurry comprises the following steps: respectively weighing 10-30% of sodium silicate, 40-60% of chromium powder, 2-10% of sodium chloride, 5-20% of filler alumina and 10-30% of distilled water according to mass percentage, and dividing the distilled water into three parts; adding chromium powder into the sodium silicate solution, uniformly stirring, adding the sodium chloride solution into the mixed solution, fully mixing, adding alumina powder into the mixed solution, uniformly stirring, adding a third part of distilled water, and adjusting the slurry to a proper viscosity as required; and finally, putting the mixed slurry into a planetary ball milling tank for ball milling for 5-10 h at the rotating speed of 350-400 r/min, and standing for 12h to obtain the rapid chromizing slurry.
The preparation method of the chromium diffusion layer comprises the following steps:
1) workpiece surface cleaning
Cleaning oil stains, dust and the like on the surface of the workpiece by using alcohol/acetone, and removing surface oxide skin by using a steel brush; the specific surface area of the uneven workpiece surface after being brushed by the steel brush is increased, which is beneficial to the coating of subsequent slurry and the diffusion of chromium atoms.
2) Slurry coating of workpiece surfaces
Preheating a workpiece at 60-100 ℃ for 30-60 min, and then coating the slurry to a proper thickness in one step in a spraying or brushing mode, wherein multiple layered coating cannot be performed; the thickness of the coating slurry layer is 0.1-5 mm. A slurry layer that is too thin may not provide a sufficient source of bleed, and too thick may crack and flake, which may be detrimental to the uniformity of the chromized layer thickness.
3) Drying and curing
The drying and curing adopt a sectional gradient curing process, namely: pre-drying at a low temperature of 75-85 ℃ for 5-30 min, then drying at a low temperature of 140-160 ℃ for 30-60 min, and finally curing at a medium temperature of 250-300 ℃ for 30-60 min. The segmented curing process effectively solves the problems of microcracks and tiny holes generated by stress cracking of a slurry layer under a one-step drying curing method while ensuring the slurry curing, and simultaneously the slurry is combined with the surface of a workpiece more compactly.
4) Rapid sintering of
In order to prevent the volatilization of the components in the high-temperature blanking slurry, the workpiece is rapidly sintered, diffused and chromized by adopting a rapid heating mode, and then air-cooled to room temperature; wherein the heating rate is more than or equal to 1000 ℃/min, the heat preservation temperature is 900-1100 ℃, and the heat preservation time is 5-30 min; the thickness of the chromizing layer obtained by the process is about 10-100 mu m.
The deposited chromium-rich high-temperature corrosion-resistant coating contains not less than 30 percent (mass fraction) of chromium.
Example 1
1) Cleaning the surface of the pipeline
The method is characterized in that oil stains, dust and the like on the surface of the pipeline are cleaned by alcohol/acetone, and meanwhile, the surface oxide skin is removed by a steel brush.
2) Slurry coating of pipeline surfaces
Preheating the pipeline for 30min at 60 ℃, and then coating the slurry to a proper thickness in one step in a spraying (or brushing and other modes) mode, wherein multiple layered coating can not be performed; the thickness of the coating slurry layer is 0.1-5 mm.
Wherein the slurry is prepared by the following processes: respectively weighing 12% of sodium silicate, 58% of chromium powder, 5% of sodium chloride, 15% of filler alumina and 10% of distilled water according to mass percentage, and dividing the distilled water into three parts; adding chromium powder into the sodium silicate solution, uniformly stirring, adding the sodium chloride solution into the mixed solution, fully mixing, adding alumina powder into the mixed solution, uniformly stirring, adding a third part of distilled water, and adjusting the slurry to a proper viscosity as required; and finally, ball-milling the mixed slurry in a planetary ball-milling tank for 5 hours at the rotating speed of 400r/min, and standing for 12 hours to obtain the rapid chromizing slurry.
3) Drying and curing
Pre-drying the metal pipeline coated with the chromizing material at the low temperature of 80 ℃ for 5min, then drying at the low temperature of 150 ℃ for 55min, and finally curing at the medium temperature of 250 ℃ for 30 min.
4) Rapid sintering of
Rapidly sintering, diffusing and chromizing the pipeline in a rapid heating mode, and then air-cooling to room temperature; wherein the heating rate is set to 1000 ℃/min, the heat preservation temperature is 900 ℃, and the heat preservation time is 30 min.
Examples 2-9 the process of example 9 is the same as example 1, the specific conditions are detailed in table 1, table 1 shows the specific parameters of examples 1-9 of the preparation method of the chromium-rich hte-corrosion resistant coating deposited by the slurry method, and according to the preparation steps in the above example 1 and the specific preparation parameters in the table, the chromium-rich hte-corrosion resistant coating on the surface of different metal materials and large metal parts and the thickness thereof can be obtained.
TABLE 1
The above embodiments are analyzed and studied, and the thickness of the chromizing layer is measured to be about 10-100 μm, and the specific results are shown in table 1, and the cross-sectional morphology of the chromizing layer is shown in fig. 1-2. The numerical references in fig. 2 correspond to the abscissa in fig. 3, and the distribution of chromium elements can be seen from fig. 3.
As can be seen from the microscopic morphology diagrams 1-2 of the chromizing layers of the embodiments, the whole chromizing layer has uniform structure and moderate thickness, is well combined with the matrix metallurgy and is not easy to fall off.
Example 10
1) Pipe surface cleaning
The method is characterized in that oil stains, dust and the like on the surface of the pipeline are cleaned by alcohol/acetone, and meanwhile, the surface oxide skin is removed by a steel brush.
2) Slurry coating of pipe surfaces
Preheating the pipeline at 60 ℃ for 60min, and then coating the chromizing slurry to a proper thickness in one step in a spraying mode, wherein multiple times of layered coating cannot be performed; the thickness of the coating slurry layer is 0.1-5 mm.
Wherein the slurry is prepared by the following processes: respectively weighing 10% of sodium silicate, 60% of chromium powder, 5% of sodium chloride, 5% of filler alumina and 20% of distilled water according to mass percentage, and dividing the distilled water into three parts; adding chromium powder into the sodium silicate solution, uniformly stirring, adding the sodium chloride solution into the mixed solution, fully mixing, adding alumina powder into the mixed solution, uniformly stirring, adding a third part of distilled water, and adjusting the slurry to a proper viscosity as required; and finally, ball-milling the mixed slurry in a planetary ball-milling tank for 5 hours at the rotating speed of 400r/min, and standing for 12 hours to obtain the rapid chromizing slurry.
3) Drying and curing
Pre-drying the metal pipeline coated with the chromizing material at the low temperature of 75 ℃ for 30min, then drying at the low temperature of 140 ℃ for 60min, and finally curing at the medium temperature of 250 ℃ for 60 min.
4) Rapid sintering of
Rapidly sintering, diffusing and chromizing the pipeline in a rapid heating mode, and then air-cooling to room temperature; wherein the heating rate is set to 1000 ℃/min, the heat preservation temperature is 900 ℃, and the heat preservation time is 30 min.
Example 11
1) Pipe surface cleaning
The method is characterized in that oil stains, dust and the like on the surface of the pipeline are cleaned by alcohol/acetone, and meanwhile, the surface oxide skin is removed by a steel brush.
2) Slurry coating of pipe surfaces
Preheating the pipeline for 50min at 80 ℃, and then coating the chromizing slurry to a proper thickness in one step by adopting a row brush mode, wherein the chromizing slurry cannot be coated in layers for multiple times; the thickness of the coating slurry layer is 0.1-5 mm.
Wherein the slurry is prepared by the following processes: weighing 15% of sodium silicate, 40% of chromium powder, 5% of sodium chloride, 10% of filler alumina and 30% of distilled water according to mass percentage, and dividing the distilled water into three parts; adding chromium powder into the sodium silicate solution, uniformly stirring, adding the sodium chloride solution into the mixed solution, fully mixing, adding alumina powder into the mixed solution, uniformly stirring, adding a third part of distilled water, and adjusting the slurry to a proper viscosity as required; and finally, ball-milling the mixed slurry in a planetary ball-milling tank for 5 hours at the rotating speed of 400r/min, and standing for 12 hours to obtain the rapid chromizing slurry.
3) Drying and curing
Pre-drying the metal pipeline coated with the chromizing material at the low temperature of 80 ℃ for 5min, then drying at the low temperature of 150 ℃ for 40min, and finally curing at the medium temperature of 300 ℃ for 30 min.
4) Rapid sintering of
Rapidly sintering, diffusing and chromizing the pipeline in a rapid heating mode, and then air-cooling to room temperature; wherein the heating rate is set to 1000 ℃/min, the heat preservation temperature is 1100 ℃, and the heat preservation time is 20 min.
Example 12
1) Pipe surface cleaning
The method is characterized in that oil stains, dust and the like on the surface of the pipeline are cleaned by alcohol/acetone, and meanwhile, the surface oxide skin is removed by a steel brush.
2) Slurry coating of pipe surfaces
Preheating the pipeline for 30min at 100 ℃, and then coating the chromizing slurry to a proper thickness in one step in a spraying (or brushing and other modes) mode, wherein the chromizing slurry cannot be coated in layers for multiple times; the thickness of the coating slurry layer is 0.1-5 mm.
Wherein the slurry is prepared by the following processes: respectively weighing 30% of sodium silicate, 40% of chromium powder, 5% of sodium chloride, 5% of filler alumina and 20% of distilled water according to mass percentage, and dividing the distilled water into three parts; adding chromium powder into the sodium silicate solution, uniformly stirring, adding the sodium chloride solution into the mixed solution, fully mixing, adding alumina powder into the mixed solution, uniformly stirring, adding a third part of distilled water, and adjusting the slurry to a proper viscosity as required; and finally, ball-milling the mixed slurry in a planetary ball-milling tank for 5 hours at the rotating speed of 400r/min, and standing for 12 hours to obtain the rapid chromizing slurry.
3) Drying and curing
Pre-drying the metal pipeline coated with the chromizing material at 75 ℃ for 20min, then drying at 160 ℃ for 30min, and finally curing at 270 ℃ for 50 min.
4) Rapid sintering of
Rapidly sintering, diffusing and chromizing the pipeline in a rapid heating mode, and then air-cooling to room temperature; wherein the heating rate is set to 1000 ℃/min, the heat preservation temperature is 1000 ℃, and the heat preservation time is 20 min.
The chromium-rich high-temperature corrosion-resistant coating deposited by the slurry method and the preparation method thereof can be applied to various metal parts such as carbon steel, austenitic stainless steel, high-temperature alloy and the like, are particularly suitable for large-scale pipeline metal parts, heterosexual metal parts, complex parts and the like, and have the advantages of strong practicability, wide application range, high chromizing efficiency, small pollution, moderate thickness, good metallurgical bonding with a matrix and difficult shedding.
Claims (4)
1. A preparation method of a chromium-rich high-temperature corrosion-resistant coating deposited by a slurry method is characterized in that a workpiece is preheated, and then chromizing slurry is coated on the surface of the workpiece, wherein the thickness of the coating slurry layer is 0.1-5 mm; then drying and curing, and finally sintering to obtain the chromium-rich high-temperature corrosion-resistant coating; wherein the chromizing slurry comprises, by mass, 10-30% of a binder, 40-60% of a penetration source, 2-10% of an activating agent, 5-20% of a filler and 10-30% of a diluent; wherein the adhesive is sodium silicate, the seepage source is pure chromium powder, the activating agent is sodium chloride, the filling agent is alumina, and the diluting agent is distilled water; sintering at 900-1100 ℃ for 5-30 min;
the preparation method of the chromizing slurry comprises the following steps: weighing 10-30% of sodium silicate, 40-60% of chromium powder, 2-10% of sodium chloride, 5-20% of alumina and 10-30% of distilled water in percentage by mass, and dividing the distilled water into three parts; dissolving sodium silicate in the first part of distilled water to obtain a sodium silicate solution, and dissolving sodium chloride in the second part of distilled water to obtain a sodium chloride solution; adding chromium powder into a sodium silicate solution, stirring uniformly, adding a sodium chloride solution, mixing uniformly, adding alumina, stirring uniformly, adding a third part of distilled water, and finally performing ball milling to obtain chromizing slurry;
the drying and curing adopts a sectional gradient curing process, which specifically comprises the following steps: pre-drying at 75-85 ℃ for 5-30 min, then drying at 140-160 ℃ for 30-60 min, and finally curing at 250-300 ℃ for 30-60 min;
and during sintering, heating to 900-1100 ℃ from room temperature at a heating rate of more than or equal to 1000 ℃/min.
2. The preparation method of the chromium-rich high-temperature corrosion-resistant coating deposited by the slurry method according to claim 1, wherein the preheating temperature is 60-100 ℃ and the preheating time is 30-60 min.
3. The preparation method of the chromium-rich high-temperature corrosion-resistant coating according to claim 1, wherein ball milling is carried out in a star-shaped ball milling tank, the rotating speed is 350-400 r/min, and the ball milling time is 5-10 h.
4. A method for preparing a cr-rich htcorrosionproof coating according to claim 1, wherein the chromizing slurry is applied to the surface of the workpiece by spraying or brushing.
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