CN108314453B - Method for improving dispersion stability of silicon carbide powder in water system - Google Patents
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Abstract
The invention relates to a method for improving dispersion stability of silicon carbide powder in a water system. Dispersing silicon carbide powder in a water system to prepare slurry, adding a sucrose ester surfactant solution to enable the mass of sucrose ester to be 5% -30% of that of silicon carbide, uniformly mixing and stirring to obtain a mixed solution, and adjusting the pH value of the mixed solution to be 8-12; in the sucrose ester surfactant solution, sucrose ester is a solute and ethanol is a solvent. The method is simple to operate, the used dispersing agent is non-toxic and harmless, energy-saving and environment-friendly, the cost is low, the silicon carbide in the prepared silicon carbide aqueous system is good in dispersibility and high in stability, and the silicon carbide aqueous system can be used as silicon carbide slurry to prepare silicon carbide ceramics through slip casting and other processes so as to improve the dispersion stability of the silicon carbide ceramics.
Description
Technical Field
The invention relates to the technical field of silicon carbide ceramics, in particular to a method for improving the dispersion stability of silicon carbide powder in a water system.
Background
Silicon carbide (SiC) is not only a strong covalent bond type carbide, but also an engineered ceramic material with excellent properties. The silicon carbide has extremely high decomposition temperature which can reach 2600 ℃, and not only has excellent strength, hardness, wear resistance and other properties at normal temperature, but also has the optimal properties of oxidation resistance, creep resistance and the like at high temperature in the known ceramic materials. At present, silicon carbide has been widely used in the fields of aerospace, chemical engineering, machinery, traffic, energy, metallurgy and the like, and is considered to be one of the best candidate materials for rocket engines, gas turbines, advanced heat engines, heat exchangers, high-temperature wear-resistant parts and the like.
At present, silicon carbide ceramic is prepared by a plurality of methods, and slip casting and dip forming are one of the most common methods, wherein the key steps in the method are to prepare silicon carbide ceramic slurry with high solid content, stable dispersion and uniformity. However, silicon carbide powder is difficult to form stable slurry in a water system, and agglomeration and sedimentation are easy to occur, so that the dispersion stability of the silicon carbide powder in the water system is a key problem of grouting, dipping and molding. That is, in order to maximally perform slip casting using the silicon carbide slurry, it is necessary to control the dispersibility and stability of the silicon carbide slurry.
At present, the dispersibility and rheological property of silicon carbide ceramic slurry are researched more at home and abroad, and the dispersing process is also various. For example, the theory of Tang Dynasty found that different dispersant types acted differently on the dispersion of silicon carbide slurries. Zhangizhi et al prepared a silicon carbide slurry with a solid phase volume fraction of 69% by adding silica sol. Li Rev et al used tetramethylammonium hydroxide as a dispersant, investigated the effect on the rheology of the silicon carbide slurry, and analyzed the cause thereof. Sun et al investigated the effect of dispersant dosage on the flowability of silicon carbide slurries using Polyethyleneimine (PEI) as the dispersant. Zhang Qingyong and the like adopt a graft copolymerization coating modification technology to form a layer of polyelectrolyte film on the surface of silicon carbide, so that the dispersibility of the modified silicon carbide powder is greatly improved.
Disclosure of Invention
In view of the above technical situation, the present invention aims to improve the dispersion stability of silicon carbide powder in a water system, thereby laying a foundation for preparing high-quality silicon carbide ceramics.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for improving dispersion stability of silicon carbide powder in a water system is characterized by comprising the following steps: dispersing silicon carbide powder in a water system to prepare slurry with a solid volume fraction of 10-50%, adding a sucrose ester surfactant solution to enable the mass of sucrose ester to be 5-30% of that of silicon carbide, uniformly mixing and stirring to obtain a mixed solution, and adjusting the pH value of the mixed solution to be 8-12; in the sucrose ester surfactant solution, sucrose ester is a solute and ethanol is a solvent.
Preferably, the average particle size of the silicon carbide powder is in the range of 7.5 to 102.5. mu.m.
Preferably, the sucrose ester accounts for 15% to 25%, and more preferably 25% by mass of the silicon carbide.
As an implementation mode, the sucrose ester surfactant solution is prepared by dissolving sucrose ester at the temperature of 60-80 ℃ and then adding ethanol; preferably, the sucrose ester surfactant solution further comprises acetone.
As one implementation, the pH of the mixed liquor is adjusted with a base. Preferably, the alkali is one of sodium hydroxide solution and ammonia water; more preferably, the concentration of the sodium hydroxide solution is 5% to 10%, and the concentration of the aqueous ammonia solution is 5% to 10%.
Preferably, the silicon carbide powder is first subjected to a cleaning treatment before being dispersed in an aqueous system. As one implementation mode, the cleaning treatment process of the silicon carbide powder comprises the following steps: dispersing silicon carbide powder in 2% -10% hydrochloric acid solution, mixing and stirring uniformly, standing, removing upper liquid after the slurry is layered, centrifuging and cleaning the obtained slurry with distilled water until the pH value is in a neutral range, and finally drying to obtain the silicon carbide powder.
The method can also be used for preparing the silicon carbide powder with high dispersibility, and the silicon carbide powder with high dispersibility is obtained by standing and drying after the dispersion stability of the silicon carbide powder in a water system is improved by the method.
Compared with the prior art, the invention has the following beneficial effects:
(1) after the silicon carbide powder is dispersed in a water system, a dispersant sucrose ester is added. The sucrose ester is an uncharged nonionic surfactant and is rich in hydrophilic hydroxyl, the dispersion of silicon carbide powder in a water system is mainly completed through a steric hindrance stabilization mechanism, one end of the sucrose ester is adsorbed on the surface of silicon carbide particles, the molecular chain at the other end of the sucrose ester is in a stretched state to form a spatial barrier and provide steric hindrance, and the sucrose ester can hinder the agglomeration and sedimentation of silicon carbide powder particles in slurry under the action of the steric barrier, so that the dispersion stability of the silicon carbide powder in a water-based system suspension can be improved.
(2) Meanwhile, researches find that the pH value influences the molecular morphology and the ionization degree of the dispersing agent, the charging characteristic of the surface of the silicon carbide particle can be adjusted by adjusting the pH value, so that the surface charge of the particle is increased, and the electric double layer repulsion energy is increased, thereby increasing the stability of a silicon carbide water system; the pH value of the isoelectric point (IEP) of the silicon carbide powder particles is generally 3-6 in the slurry suspension, stable uncharged silanol is formed on the surfaces of the silicon carbide particles at the IEP, the positive and negative charges of the particles in the suspension are equal, the Zeta potential is zero, the electrostatic repulsion is zero, and the particles are easy to agglomerate and settle; when the pH value is higher, the silicon carbide particles are negatively charged, the more the pH value is, the more the negative charges are charged on the particle surfaces, and the Zeta potential is gradually increased, so that the dispersion stability of the silicon carbide powder particles in a water system is facilitated. Through a large number of experiments and researches, when the pH value is adjusted to be 8-12, the silicon carbide can have good dispersion stability in a water system, and particularly, the silicon carbide has good dispersion when the pH value is 10.
(3) The preparation process is simple to operate, the used dispersing agent is non-toxic and harmless, energy-saving and environment-friendly, the cost is low, the silicon carbide in the prepared silicon carbide aqueous system is good in dispersibility and high in stability, the silicon carbide slurry can be used as silicon carbide slurry to prepare silicon carbide ceramics through slip casting and other processes, and the dispersion stability of the silicon carbide ceramics can be improved.
Drawings
FIG. 1 is a scanning electron micrograph of a silicon carbide powder obtained in comparative example 1;
FIG. 2 is a scanning electron microscope photograph of the silicon carbide powder obtained in example 1 when the pH value in step (1) was 10;
FIG. 3 is a graph showing the relationship between the viscosity and pH of the suspension portion of the silicon carbide slurry obtained in step (1) in example 1;
FIG. 4 is a graph showing the relationship between the distribution volume of a silicon carbide solid phase (hereinafter referred to as deposition volume) in the silicon carbide slurry obtained in step (1) in example 1 and the pH value;
FIG. 5 is a graph showing the relationship between the viscosity of the suspension portion and the content of the dispersing agent in the silicon carbide slurry obtained in step (1) of example 2;
FIG. 6 is a graph showing the relationship between the distribution volume of the silicon carbide solid phase (hereinafter referred to as "deposition volume") in the silicon carbide slurry obtained in step (1) in example 2 and the content of the dispersant.
Detailed Description
The present invention is described in further detail below with reference to examples, which are intended to facilitate the understanding of the present invention without limiting it in any way.
Example 1:
in this embodiment, the preparation method of the silicon carbide ceramic powder is as follows:
(1) dispersing silicon carbide powder in distilled water, wherein the mass ratio of the silicon carbide powder to the distilled water is 1:1, adding a sucrose ester surfactant solution to enable the sucrose ester to account for 25% of the silicon carbide, and mixing and stirring for 5 hours under the condition of 750r/min to obtain silicon carbide slurry;
the sucrose ester in the surfactant solution is used as a dispersing agent, and the ethanol and the acetone are used as solvents, and the sucrose ester is dissolved at the temperature of 60-80 ℃, and then the sucrose ester is prepared by adding the ethanol and the acetone;
then, adjusting the pH value of the silicon carbide slurry by using ammonia water and hydrochloric acid to obtain six groups of slurry with the pH values of 2, 4, 6, 8, 10 and 12, continuously stirring for 1h under the condition of 300r/min, and adjusting the pH value of the silicon carbide slurry again after stirring is finished to ensure that the pH value is unchanged; then standing the silicon carbide slurry, observing the distribution space of a silicon carbide solid phase after the silicon carbide slurry is stabilized, sampling the suspension liquid on the upper part, and measuring the viscosity of the suspension liquid to obtain the solid phase content information of the silicon carbide;
(2) taking out the silicon carbide slurry, standing for 24h, and finally drying in a constant-temperature drying oven at 50 ℃ for 24h to obtain silicon carbide ceramic powder.
Comparative example 1:
this example is a comparative example to example 1 above.
In this embodiment, the preparation method of the silicon carbide ceramic powder is as follows:
(1) dispersing silicon carbide powder in distilled water, and mixing and stirring the silicon carbide powder and the distilled water for 5 hours under the conditions that the mass ratio of the silicon carbide powder to the distilled water is 1:1 and 750r/min, so as to obtain silicon carbide slurry;
(2) same as in step (2) in example 1.
FIG. 1 is a scanning electron micrograph of the silicon carbide powder obtained in comparative example 1. FIG. 2 is a scanning electron micrograph of the silicon carbide powder obtained in example 1 at a pH of 10 in step (1). The comparison of the two shows that the silicon carbide powder modified by the sucrose ester surfactant solution in example 1 has a reduced agglomeration and a good dispersibility, compared to the silicon carbide powder not modified by the sucrose ester surfactant solution in comparative example 1.
Fig. 3 is a graph of the viscosity of the suspension portion of the silicon carbide slurry obtained in step (1) of example 1, as a function of pH, showing that the viscosity of the suspension tends to increase and decrease with increasing pH, and most of the silicon carbide is deposited at the bottom when the pH is 2, and the viscosity of the suspension is the smallest; with the increase of the pH value, the dispersibility of the silicon carbide is gradually improved, the deposition volume at the bottom is gradually reduced, the content of the silicon carbide in the suspension at the upper part is gradually increased, and the viscosity of the suspension is gradually increased; when the pH is 8, the viscosity of the suspension is maximum; when the pH value continues to increase, the viscosity of the suspension decreases, because ammonia is added continuously, although the dispersibility of the silicon carbide is still improved when the pH value continues to increase, the volume of the suspension is increased simultaneously, and the solid content of the silicon carbide in the suspension decreases, but even if the viscosity decreases, the viscosity is still higher when the pH is 12.
Fig. 4 is a graph of the distribution volume of the silicon carbide solid phase in the silicon carbide slurry obtained in step (1) in example 1 above as a function of pH, showing that the distribution volume is low when pH is 2 because most of the silicon carbide is deposited at the bottom; with the increase of the pH value, the dispersibility of the silicon carbide in the suspension liquid is improved, and the distribution space volume of the silicon carbide is gradually increased; when the pH value is 10, the distribution space volume of the silicon carbide solid phase is the largest and reaches 100ml, which indicates that the silicon carbide powder particles have the best dispersibility and stability in a water-based system; as the pH continues to increase progressively, the volume of the silicon carbide solid phase in the distribution space decreases, but is still higher when the pH is 12.
Example 2:
in this embodiment, the preparation method of the silicon carbide ceramic powder is as follows:
(1) dispersing silicon carbide powder in distilled water, wherein the mass ratio of the silicon carbide powder to the distilled water is 1:1, adding a sucrose ester surfactant solution to enable the sucrose esters to respectively account for 5%, 10%, 15%, 20%, 25% and 30% of the silicon carbide, and mixing and stirring for 5 hours under the condition of 750r/min to obtain six groups of silicon carbide slurry;
the sucrose ester in the surfactant solution is used as a dispersing agent, and the ethanol and the acetone are used as solvents, and the sucrose ester is dissolved at the temperature of 60-80 ℃, and then the sucrose ester is prepared by adding the ethanol and the acetone;
then, adjusting the pH value of the silicon carbide slurry by using ammonia water and hydrochloric acid to obtain the pH value of 10, continuously stirring for 1h under the condition of 300r/min, and adjusting the pH value of the silicon carbide slurry again after stirring is finished to ensure that the pH value is unchanged; then standing the silicon carbide slurry, observing the distribution space of a silicon carbide solid phase after the silicon carbide slurry is stabilized, sampling the suspension liquid on the upper part, and measuring the viscosity of the suspension liquid to obtain the solid phase content information of the silicon carbide;
(2) taking out the silicon carbide slurry, standing for 24h, and finally drying in a constant-temperature drying oven at 50 ℃ for 24h to obtain silicon carbide ceramic powder.
FIG. 5 is a graph showing the relationship between the viscosity of the suspension portion and the content of the dispersing agent in the silicon carbide slurry obtained in the step (1) in example 2. FIG. 6 is a graph showing the relationship between the distribution volume of the silicon carbide solid phase in the silicon carbide slurry obtained in step (1) in example 2 and the dispersant content. From FIGS. 3 and 4, it is shown that the amount of sucrose ester added has a large influence on the viscosity of the suspension portion and the volume of distribution of the silicon carbide solid phase. When the content of the dispersing agent is 5%, the viscosity of the suspension part and the distribution volume of the silicon carbide solid phase are minimum; when the content of the dispersing agent is increased, the general trend of the viscosity of the suspending agent suspension and the distribution volume of the silicon carbide solid phase is increased along with the increase of the content of the dispersing agent; when the content of the dispersing agent reaches 25%, the distribution volume of the silicon carbide solid phase reaches the maximum; when the content of the dispersing agent continues to increase, the viscosity of the suspension liquid part continues to increase, and the distribution volume of the silicon carbide solid phase does not change any more, because the adsorption of the sucrose ester and the surfaces of the silicon carbide particles has a critical value, when the content of the sucrose ester reaches 25%, the silicon carbide particles can be completely dispersed in the suspension liquid of the water system, and the steric hindrance effect is the best. When the content of the sucrose ester is continuously increased, a supersaturated state can be achieved, the sucrose ester has certain viscosity when dissolved in water, and the increase of the content can cause the viscosity of the slurry to be continuously increased, the particles to be agglomerated and flocculated, and the fluidity to be poor. Therefore, when the dispersant content is 25%, the slurry dispersibility and stability are optimized.
Example 3:
(1) substantially the same as in step (1) in example 1, except that the sucrose ester accounted for 5% by mass of the silicon carbide, and that the pH of the silicon carbide slurry was adjusted to 10 with ammonia and hydrochloric acid;
(2) same as in step (2) in example 1.
Example 4:
(1) substantially the same as in step (1) in example 1, except that the sucrose ester accounted for 10% by mass of the silicon carbide, and that the pH of the silicon carbide slurry was adjusted to 10 with ammonia and hydrochloric acid;
(2) same as in step (2) in example 1.
Example 5:
(1) substantially the same as in step (1) in example 1, except that the sucrose ester accounted for 20% by mass of the silicon carbide, and that the pH of the silicon carbide slurry was adjusted to 10 with ammonia and hydrochloric acid;
(2) same as in step (2) in example 1.
Example 6:
this example is essentially the same as example 3, except that prior to step (1), the silicon carbide powder was treated as follows:
dispersing silicon carbide powder in 5% hydrochloric acid solution, respectively preparing suspensions with the solid volume fraction of 20%, mixing and stirring for 1h under the condition of 750r/min, standing, removing upper-layer liquid after the suspensions are layered, centrifuging and washing the obtained suspensions with distilled water until the pH value of the suspensions is within a neutral range, and finally drying in a constant-temperature drying oven at 100 ℃ for 12h to obtain the silicon carbide powder.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for improving dispersion stability of silicon carbide powder in a water system is characterized by comprising the following steps: dispersing silicon carbide powder in a water system to prepare slurry with the solid volume fraction of 10-50%, adding a sucrose ester surfactant solution to enable the mass of sucrose ester to be 5-30% of the mass of silicon carbide, uniformly mixing and stirring to obtain a mixed solution, and adjusting the pH value of the mixed solution to be 10-12;
in the sucrose ester surfactant solution, sucrose ester is a solute and ethanol is a solvent.
2. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 1, wherein: the average grain size range of the silicon carbide powder is 7.5-102.5 mu m.
3. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 1, wherein: the mass of the sucrose ester accounts for 15-25% of the mass of the silicon carbide.
4. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 1, wherein: the sucrose ester surfactant solution is prepared by dissolving sucrose ester at the temperature of 60-80 ℃ and then adding ethanol.
5. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 1, wherein: the sucrose ester surfactant solution also comprises acetone.
6. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 1, wherein: adjusting the pH value of the mixed solution by using alkali; the alkali is one of sodium hydroxide solution and ammonia water.
7. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 6, wherein: the concentration of the sodium hydroxide solution is 5-10%, and the concentration of the ammonia water solution is 5-10%.
8. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 1, wherein: before the silicon carbide powder is dispersed in an aqueous system, the silicon carbide powder is first subjected to a cleaning treatment.
9. The method for improving the dispersion stability of silicon carbide powder in an aqueous system according to claim 8, wherein: the cleaning treatment process of the silicon carbide powder comprises the following steps: dispersing silicon carbide powder in 2% -10% hydrochloric acid solution, mixing and stirring uniformly, standing, removing upper liquid after the slurry is layered, centrifuging and cleaning the obtained slurry with distilled water until the pH value is in a neutral range, and finally drying to obtain the silicon carbide powder.
10. A method for preparing high-dispersibility silicon carbide powder, which comprises the steps of improving the dispersion stability of silicon carbide powder in an aqueous system by the method according to any one of claims 1 to 9, standing, and drying to obtain the high-dispersibility silicon carbide powder.
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