CN113337145B - MXene reinforced silicate adhesive ceramic coating and preparation method thereof - Google Patents
MXene reinforced silicate adhesive ceramic coating and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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Abstract
The invention relates to the technical field of metal surface materials, in particular to an MXene reinforced silicate adhesive ceramic coating and a preparation method thereof, wherein the MXene reinforced silicate adhesive ceramic coating comprises the following components: alumina, silicon phosphate, MXene and silicate adhesive; the chemical formula of MXene is Ti3C2. The coating has the advantages of low shear strength, self-lubricating capability, high mechanical strength and layer-by-layer stacking structure; the preparation process is simple, the curing temperature is low, the time is short, and the method is very suitable for industrial production equipment and places which cannot resist high temperature; the preparation process has low energy consumption, does not need coating equipment with complex and precise structure, and is green and pollution-free.
Description
Technical Field
The invention relates to the technical field of metal surface materials, in particular to an MXene reinforced silicate adhesive ceramic coating and a preparation method thereof.
Background
Under the rapid development of industrial technology, the working environment conditions of engineering equipment and components thereof are increasingly harsh and severe. Interacting machine components, after undergoing friction and wear, eventually result in a power loss and a reduction in service life. At present, reducing material loss caused by friction wear while allowing mechanical parts to operate reliably in a sliding state remains one of the challenges of saving energy consumption. The application of coatings to the surfaces of engineering equipment and parts thereof has become one of the effective ways to protect the engineering machinery and equipment and to save energy consumption.
The inorganic adhesive ceramic coating is a product of a sol-gel technology, mainly comprises an adhesive, an aggregate, a curing agent, a functional additive and the like, and is generally coated by brushing, blade coating and normal-temperature spraying. Since the preparation process is simple and does not need to have a complex structure, precise coating equipment is widely applied in the industrial field. Most of the currently used adhesives are inorganic binders aluminum dihydrogen phosphate, but the curing temperature is high, the curing time is long, the wear resistance under severe real environment needs to be improved, patent CN 106866122 a adopts aluminum dihydrogen phosphate as an adhesive to prepare a coating, and the curing temperature reaches 300 ℃. The inorganic binder potassium silicate has low curing temperature and short curing time, and has the advantages of environmental protection, low cost, strong weather resistance, abundant raw materials and the like, so the inorganic binder potassium silicate is widely applied to zinc-rich primer, building coating, inorganic adhesive and the like, and has been a hot spot of worldwide research in recent years. At present, the application of the potassium silicate binder in preparing wear-resistant antifriction coatings is rarely reported.
In the field of tribology, it is common to utilize one or more organic or inorganic fillers as a lubricating material to improve the tribological wear properties and mechanical properties of the coating material. The two-dimensional MXene material has many excellent characteristics since the first report in 2011, has great research significance in various fields, but has less application in the field of tribology. MXene has some chemical groups on the surface during the chemical etching preparation process, such as-OH, -O and-F. MXene has lower shear strength, self-lubricating ability, higher mechanical strength and a layer-by-layer stacking structure, and the structure is bonded by weaker van der Waals force and can be self-peeled and delaminated under the action of smaller shear force to form a thinner sheet layer with good stability. During the friction process, the sheets and the abrasive dust are easy to form a lubricating film, the friction coefficient between friction pairs is reduced, the abrasion of a friction part is slowed down, and the self-lubricating material is an ideal self-lubricating material and shows great potential in the field of tribology. If MXene can be used as a coating reinforcing material for the surface of any substrate, the MXene has great significance for promoting the industrialization of MXene in the field of friction reduction and wear resistance.
Disclosure of Invention
The invention provides an MXene reinforced silicate adhesive ceramic coating and a preparation method thereof, aiming at solving the problems that in the prior art, an inorganic phosphate adhesive ceramic coating is high in curing temperature, long in curing time and insufficient in wear resistance, and although different lubricating materials are added to improve the frictional wear performance of the inorganic phosphate adhesive ceramic coating, the frictional wear performance of the inorganic phosphate adhesive ceramic coating cannot meet the application requirement of the conventional engineering equipment.
According to the technical scheme of the invention, the MXene reinforced silicate adhesive ceramic coating comprises the following components: alumina, silicon phosphate, MXene and silicate adhesive, wherein the chemical formula of the MXene is Ti3C2。
Further, the mass portion of the aluminum oxide is 20-60, the mass portion of the silicon phosphate is 1-10, the mass portion of the MXene is 0.1-2.5, and the mass portion of the silicate adhesive is 40-80.
Further, the silicate adhesive is prepared by mixing a potassium silicate aqueous solution and a silica sol aqueous solution.
Further, the mass percentage concentration of solute in the silicate adhesive is 35-40%.
Specifically, the silicate adhesive can be prepared by matching a potassium silicate aqueous solution (with the mass percentage concentration of 40%) with a silica sol aqueous solution (with the mass percentage concentration of 30%) in a mass ratio of 2: 1-2.
Further, the surface chemical group of MXene is at least one of-OH, -O and-F.
Further, the alumina has a particle size of 1 μm to 20 μm, and if the particle size is too small, the coating is easily cracked, and if the particle size is too large, the pores of the coating become large and the bonding with the substrate is poor.
The invention also provides a preparation method of the MXene reinforced silicate adhesive ceramic coating, which comprises the following steps,
s1, mixing, dispersing and drying the alumina and MXene, wherein the chemical formula of the MXene is Ti3C2；
S2, adding a silicate adhesive and a curing agent silicon phosphate into the powder obtained by drying the powder in the S1, and uniformly stirring to obtain slurry;
s3, coating the slurry obtained in the step S2 on a pretreated substrate, and curing to obtain the MXene reinforced silicate adhesive ceramic coating.
The specific operation of step S1 is: weighing 20-60 parts of alumina and 0.1-2.5 parts of MXene, mixing, ultrasonically dispersing for 20min by using an ultrasonic cell disruptor, and finally putting into a vacuum drying machine.
The preparation method of the silicate adhesive in the step S2 is as follows: weighing a potassium silicate aqueous solution and a silica sol aqueous solution, mixing and stirring to obtain a silicate adhesive, wherein the silicate adhesive is 40-80 parts by weight; and step S3, the mass portion of the curing agent silicon phosphate is 1-10.
Further, the solvent for dispersion in step S1 is water, and specifically, the dispersion may be performed in deionized water.
Further, the substrate in the step S4 is 304 stainless steel.
Further, the preprocessing in step S4 includes the following steps: firstly, polishing to remove rust marks on the surface of the substrate, then cleaning to remove stains on the surface of the substrate, and carrying out sand blasting treatment on the surface of the substrate after drying.
Further, the curing process in step S4 is: firstly, curing at room temperature (20-30 ℃, the same below), then heating to 150-170 ℃ for 3-6 times, curing after each heating, and finally cooling to room temperature. The method specifically comprises the following steps: firstly, curing at room temperature; then heating to 80-100 ℃ and curing; heating to 110-130 ℃, and curing; heating to 130-150 ℃; heating to 150 ℃ and 170 ℃, solidifying, and finally cooling to room temperature. To ensure that the coating can be prepared at a lower temperature and to ensure its properties, the maximum curing temperature is set at 150 ℃ and 170 ℃. And the gradient temperature rise is adopted, so that the phenomenon that the coating performance is influenced due to nonuniform internal thermal stress caused by rapid heating can be prevented.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. the invention adopts the slurry method to prepare the adhesive ceramic coating, the preparation process is simpler, and coating equipment with complex and precise structure is not needed; the curing temperature of the silicate adhesive ceramic coating is low, the time is short, and the silicate adhesive ceramic coating is very suitable for industrial production equipment and places which cannot resist high temperature;
2. the MXene reinforced silicate adhesive ceramic coating has the advantages of low friction coefficient, long wear resistance and long service life, can realize good wear-resistant and antifriction effects, reduces the wear of metal materials, slows down the wear damage of mechanical equipment and parts, and prolongs the service life of a matrix;
3. the MXene reinforced silicate adhesive ceramic coating has the advantages of low energy consumption in the preparation process, greenness, no pollution and wide coverage of applicable materials.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
FIG. 2 is a wear profile of the coating of comparative example 1.
FIG. 3 is a wear profile of the coating of example 1.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Mixing a potassium silicate aqueous solution with the mass percentage concentration of 40% and a silica sol aqueous solution with the mass percentage concentration of 30% according to the mass ratio of 2:1, preparing the silicate adhesive.
Example 1
A preparation method of MXene reinforced silicate adhesive ceramic coating is shown in figure 1 and comprises the following steps,
(1) matrix pretreatment: and (3) polishing the 304 steel substrate by using sand paper, ultrasonically cleaning the substrate in absolute ethyl alcohol for 15min, removing surface stains, cleaning the substrate by using deionized water, drying the substrate, and finally performing sand blasting on the surface.
(2) Preparing slurry: 4.825g (38.6 wt%) of aggregate alumina, 0.05g (0.4 wt%) of MXene (Ti) were weighed in order according to the preparation procedure3C2) Then pouring the mixture into a beaker, and performing ultrasonic dispersion in deionized water for 20min by using an ultrasonic cell disruptor; weighing 7.5g (60 wt%) of the prepared silicate adhesive, and addingAdding 0.125g (1 wt%) of curing agent silicon phosphate into the mixture subjected to ultrasonic dispersion, and carrying out ultrasonic stirring for 5 min; and finally, uniformly coating the uniformly mixed slurry on the surface of the pretreated 304 steel matrix.
(3) Curing treatment: firstly, curing for 20min at room temperature, then heating to 100 ℃, curing for 1h, then heating to 125 ℃, curing for 1h, then heating to 135 ℃, curing for 1h, and finally heating to 150 ℃, and curing for 1 h. And at the moment, finishing the whole curing process, stopping heating, and naturally cooling the coating to room temperature to obtain the MXene enhanced silicate adhesive ceramic coating.
Example 2
A preparation method of MXene reinforced silicate adhesive ceramic coating is shown in figure 1 and comprises the following steps,
(1) matrix pretreatment: and (3) polishing the 304 steel substrate by using sand paper, ultrasonically cleaning the substrate in absolute ethyl alcohol for 15min, removing surface stains, cleaning the substrate by using deionized water, drying the substrate, and finally performing sand blasting on the surface.
(2) Preparing slurry: 4.775g (38.2 wt%) of aggregate alumina, 0.1g (0.8 wt%) of MXene (Ti) were weighed out in sequence according to the preparation procedure3C2) Then pouring the mixture into a beaker, and performing ultrasonic dispersion in deionized water for 20min by using an ultrasonic cell disruptor; weighing 7.5g (60 wt%) of the prepared silicate adhesive, adding the silicate adhesive into the mixed material after ultrasonic dispersion, adding 0.125g (1 wt%) of curing agent silicon phosphate, and carrying out ultrasonic stirring for 5 min; and finally, uniformly coating the uniformly mixed slurry on the surface of the pretreated 304 steel matrix.
(3) Curing treatment: firstly, curing for 20min at room temperature, then heating to 100 ℃, curing for 1h, then heating to 125 ℃, curing for 1h, then heating to 135 ℃, curing for 1h, and finally heating to 150 ℃, and curing for 1 h. And at the moment, finishing the whole curing process, stopping heating, and naturally cooling the coating to room temperature to obtain the MXene enhanced silicate adhesive ceramic coating.
Example 3
A preparation method of MXene reinforced silicate adhesive ceramic coating is shown in figure 1 and comprises the following steps,
(1) matrix pretreatment: and (3) polishing the 304 steel substrate by using sand paper, ultrasonically cleaning the substrate in absolute ethyl alcohol for 15min, removing surface stains, cleaning the substrate by using deionized water, drying the substrate, and finally performing sand blasting on the surface.
(2) Preparing slurry: 4.725g (37.8 wt%) of aggregate alumina, 0.15g (1.2 wt%) of MXene (Ti) were weighed out in sequence according to the preparation procedure3C2) Then pouring the mixture into a beaker, and performing ultrasonic dispersion in deionized water for 20min by using an ultrasonic cell disruptor; weighing 7.5g (60 wt%) of the prepared silicate adhesive, adding the silicate adhesive into the mixed material after ultrasonic dispersion, adding 0.125g (1 wt%) of curing agent silicon phosphate, and carrying out ultrasonic stirring for 5 min; and finally, uniformly coating the uniformly mixed slurry on the surface of the pretreated 304 steel matrix.
(3) Curing treatment: firstly, curing for 20min at room temperature, then heating to 100 ℃, curing for 1h, then heating to 125 ℃, curing for 1h, then heating to 135 ℃, curing for 1h, and finally heating to 150 ℃, and curing for 1 h. And at the moment, finishing the whole curing process, stopping heating, and naturally cooling the coating to room temperature to obtain the MXene enhanced silicate adhesive ceramic coating.
Example 4
A preparation method of MXene reinforced silicate adhesive ceramic coating is shown in figure 1 and comprises the following steps,
(1) matrix pretreatment: and (3) polishing the 304 steel substrate by using sand paper, ultrasonically cleaning the substrate in absolute ethyl alcohol for 15min, removing surface stains, cleaning the substrate by using deionized water, drying the substrate, and finally performing sand blasting on the surface.
(2) Preparing slurry: 4.675g (37.4 wt%) of aggregate alumina, 0.2g (1.6 wt%) of MXene (Ti) were weighed out in sequence according to the preparation procedure3C2) Then pouring the mixture into a beaker, and performing ultrasonic dispersion in deionized water for 20min by using an ultrasonic cell disruptor; weighing 7.5g (60 wt%) of the prepared silicate adhesive, adding the silicate adhesive into the mixed material after ultrasonic dispersion, adding 0.125g (1 wt%) of curing agent silicon phosphate, and carrying out ultrasonic stirring for 5 min; and finally, uniformly coating the uniformly mixed slurry on the surface of the pretreated 304 steel matrix.
(3) Curing treatment: firstly, curing for 20min at room temperature, then heating to 100 ℃, curing for 1h, then heating to 125 ℃, curing for 1h, then heating to 135 ℃, curing for 1h, and finally heating to 150 ℃, and curing for 1 h. And at the moment, finishing the whole curing process, stopping heating, and naturally cooling the coating to room temperature to obtain the MXene enhanced silicate adhesive ceramic coating.
Example 5
Based on example 3, the mass of alumina was adjusted to 7.5g, the mass of silicate adhesive was adjusted to 10g, and the mass of curing agent silicon phosphate was adjusted to 1.25 g.
Example 6
Based on example 3, the mass of alumina was adjusted to 2.5g, the mass of silicate adhesive was adjusted to 5g, and the mass of curing agent silicon phosphate was adjusted to 0.625 g.
Comparative example 1
A preparation method of a silicate adhesive ceramic coating comprises the following steps,
(1) matrix pretreatment: polishing a 304 steel substrate by using sand paper, ultrasonically cleaning the substrate in absolute ethyl alcohol for 15min, removing surface stains, cleaning the substrate by using deionized water, drying the substrate, and finally performing sand blasting on the surface;
(2) preparing slurry: weighing 4.875g (39 wt%) of aggregate alumina, pouring into a beaker, and performing ultrasonic dispersion in deionized water for 20min by using an ultrasonic cell disruptor; weighing 7.5g (60 wt%) of the prepared silicate adhesive, adding the silicate adhesive into the mixed material after ultrasonic dispersion, adding 0.125g (1 wt%) of curing agent silicon phosphate, and carrying out ultrasonic stirring for 5 min; finally, uniformly coating the uniformly mixed slurry on the surface of the pretreated 304 steel substrate;
(3) curing treatment: firstly, curing for 20min at room temperature, then heating to 100 ℃, curing for 1h, then heating to 125 ℃, curing for 1h, then heating to 135 ℃, curing for 1h, and finally heating to 150 ℃, curing for 1h, at this moment, finishing the whole curing process, stopping heating, and naturally cooling the coating to room temperature, thus obtaining the MXene reinforced silicate adhesive ceramic coating.
The coatings obtained in examples 1 to 4 and comparative example 1 were subjected to a coefficient of friction test, the results of which are shown in Table 1:
TABLE 1 Friction coefficient of MXene enhanced silicate adhesive ceramic coatings
As can be seen from Table 1, the friction coefficient of the coating added with MXene is small, and the friction coefficient is the smallest when the MXene content is 1.2wt%, so that the MXene has a very good antifriction effect, once friction is generated in the use process of the coated substrate, the sheet layer and the abrasive dust generated by the layer-by-layer stacked structure form a lubricating film, the friction coefficient between friction pairs is reduced, the abrasion of a friction piece is slowed down, the direct contact between the adhesive ceramic coating and other objects is prevented, and the adhesive ceramic coating plays a role of a solid lubricant, so that the friction coefficient of the ceramic coating can be effectively reduced, the wear-resistant antifriction performance of the coating is improved, and the adhesive ceramic coating is ensured to have good strength and toughness. This phenomenon can also be demonstrated from the comparison of the wear profiles of the comparative example 1 and example 1 coatings in fig. 2, fig. 1. When the MXene content reaches 1.6 wt% or more, the friction coefficient rises.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (9)
1. The MXene reinforced silicate adhesive ceramic coating is characterized by comprising the following components in parts by weight: 20-60 parts of aluminum oxide, 1-10 parts of silicon phosphate, 0.1-2.5 parts of MXene and 40-80 parts of silicate adhesive; the chemical formula of MXene is Ti3C2The MXene content was 0.4 wt%, 0.8 wt% or 1.2 wt%.
2. The MXene reinforced silicate cementitious ceramic coating of claim 1, wherein the silicate cement is obtained by mixing an aqueous potassium silicate solution with an aqueous silica sol solution.
3. The MXene enhanced silicate adhesive ceramic coating of claim 2, wherein the concentration of solute in the silicate adhesive is 35-40% by mass.
4. The MXene enhanced silicate adhesive ceramic coating of claim 1, wherein the surface chemical group of MXene is at least one of-OH, -O and-F.
5. The MXene enhanced silicate adhesive ceramic coating of claim 1, wherein the alumina has a particle size of 1 μm to 20 μm.
6. A method of making the MXene enhanced silicate cementitious ceramic coating of any one of claims 1-5 comprising the steps of,
s1, mixing 20-60 parts of alumina and 0.1-2.5 parts of MXene by weight, dispersing and drying, wherein the MXene has a chemical formula of Ti3C2；
S2, adding 40-80 parts of silicate adhesive and 1-10 parts of curing agent silicon phosphate into the powder obtained by drying the powder in the S1, and uniformly stirring to obtain slurry;
s3, coating the slurry obtained in the step S2 on a pretreated substrate, and curing to obtain the MXene reinforced silicate adhesive ceramic coating.
7. The method of preparing the MXene-reinforced silicate adhesive ceramic coating of claim 6, wherein the dispersed solvent in step S1 is water.
8. The method for preparing the MXene enhanced silicate adhesive ceramic coating according to claim 6, wherein the curing treatment in the step S3 is: firstly, curing at room temperature, then heating to 150-170 ℃ for 3-6 times, curing after each heating, and finally cooling to room temperature.
9. The method for preparing the MXene enhanced silicate adhesive ceramic coating according to claim 6, wherein the curing treatment in the step S3 is: firstly, curing at room temperature; then heating to 80-100 ℃ and curing; heating to 110-130 ℃, and curing; heating to 130-150 ℃; heating to 150 ℃ and 170 ℃, solidifying, and finally cooling to room temperature.
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| CN106007678B (en) * | 2016-05-18 | 2019-02-01 | 南京亮而彩新材料有限公司 | A kind of high temperature wear resistant ceramic coating and preparation method thereof |
| CN110357666B (en) * | 2018-10-08 | 2021-12-28 | 湖南德智新材料有限公司 | Ceramic composite coating and preparation method thereof |
| CN113337145B (en) * | 2021-06-03 | 2022-03-01 | 苏州大学 | MXene reinforced silicate adhesive ceramic coating and preparation method thereof |
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| US4018616A (en) * | 1974-09-13 | 1977-04-19 | Mizusawa Kagaku Kogyo Kabushiki Kaisha | Water glass composition |
| CN106810916A (en) * | 2015-11-30 | 2017-06-09 | 中国科学院金属研究所 | A kind of aqueous environment protection inorganic high-temperature resistant self-lubricating coating and preparation method and application |
| CN110105711A (en) * | 2019-05-23 | 2019-08-09 | 大连理工大学 | A kind of epoxy resin tribological property ameliorative way |
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