CN108314453A - A method of improving silicon carbide powder dispersion stabilization in water system - Google Patents
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Abstract
The present invention relates to a kind of methods improving silicon carbide powder dispersion stabilization in water system.Silicon carbide powder is scattered in water system by this method is made into slurry, and sucrose ester surfactants solution is added, and so that sucrose ester quality is accounted for 5% the 30% of silicon carbide quality, is mixed evenly, obtains mixed liquor, and adjust the pH value of the mixed liquor between 8~12；In the sucrose ester surfactants solution, sucrose ester is solute, and ethyl alcohol is solvent.This method is easy to operate, uses dispersant is nontoxic, energy conservation and environmental protection, at low cost, the good dispersion of silicon carbide, stability are high in the silicon carbide water system prepared, it can be used as silicon carbide slurry and prepare silicon carbide ceramics by techniques such as injection formings, to improve the dispersion stabilization of silicon carbide ceramics.
Description
Technical field
The present invention relates to silicon carbide ceramics technical field, more particularly to a kind of raising silicon carbide powder disperses surely in water system
Qualitative method.
Background technology
Silicon carbide (SiC) is not only a kind of strongly covalent bond type carbide, but also is a kind of engineering ceramics haveing excellent performance
Material.Silicon carbide has high decomposition temperature, and up to 2600 DEG C, not only the performances such as intensity, hardness, wear-resistant are excellent under room temperature
It is good, and the performances such as inoxidizability, creep resistance are optimal in known ceramic material under high temperature.Currently, silicon carbide is wide
It is general to be applied to the fields such as aerospace, chemical industry, machinery, traffic, the energy and metallurgy, it is considered to be rocket engine, gas turbine
One of optimal candidate materials such as machine, advanced heat engine, heat exchanger, high-temperature wearable part.
Silicon carbide ceramics preparation method is more at present, and slip casting dip forming is one of most common method, wherein preparing height
Solid concentration, stably dispersing, uniform silicon carbide ceramics slurry are the committed steps in this method.But silicon carbide powder is difficult
Stable slurry is formed in water system, easily occur to reunite and is settled, therefore dispersion stabilization of the silicon carbide powder in water system
It is the critical issue of slip casting dip forming.That is, to greatest extent using silicon carbide slurry come injection forming, must just control
The dispersibility and stability of good silicon carbide slurry.
Currently, more to the research of the dispersibility and rheological characteristic of silicon carbide ceramics slurry both at home and abroad, dispersing technology is also various
Various kinds.For example, the primary existing different dispersants of Tang Xue are different to the silicon carbide slurry dispersibility mechanism of action.Intelligence etc. is opened to pass through
Addition Ludox prepares the silicon carbide slurry that solid volume fraction is 69%.Li Wei etc. uses tetramethylammonium hydroxide conduct point
Powder studies its influence to silicon carbide slurry rheological characteristic, and analyzes its reason.Sun etc. is made using polyethyleneimine (PEI)
For dispersant, influence of the research dispersant dosage to silicon carbide slurry mobility.Zhang Qingyong etc. uses graft copolymerization coating modification
Technology forms a strata dielectric film in silicon carbide, and the dispersibility of modified silicon carbide powder is made to greatly improve.
Invention content
Present situation in view of the above technology, the present invention is directed to improve dispersion stabilization of the silicon carbide powder in water system, to for
The silicon carbide ceramics that high quality is made lays the foundation.
In order to solve the above-mentioned technical problem, the technical scheme is that：A kind of raising silicon carbide powder is in water system point
The method of stability is dissipated, it is characterized in that：Silicon carbide powder is scattered in water system, it is 10%-50% to be made into solid volume fraction
Slurry, sucrose ester surfactants solution is added, sucrose ester quality is made to account for the 5%-30% of silicon carbide quality, is mixed equal
It is even, mixed liquor is obtained, and adjust the pH value of the mixed liquor between 8~12；In the sucrose ester surfactants solution,
Sucrose ester is solute, and ethyl alcohol is solvent.
Preferably, the mean particle size range of the silicon carbide powder is 7.5 μm~102.5 μm.
Preferably, sucrose ester quality accounts for the 15%-25% of silicon carbide quality, further preferably 25%.
As a kind of realization method, the sucrose ester surfactants solution is the temperature by sucrose ester at 60~80 DEG C
Then lower dissolving is added ethyl alcohol and prepares to obtain；Preferably, further including third in the sucrose ester surfactants solution
Ketone.
As a kind of realization method, the pH value of the mixed liquor is adjusted using alkali.Preferably, the alkali is hydroxide
One kind in sodium solution and ammonium hydroxide；As further preferred, a concentration of the 5%~10% of sodium hydroxide solution, ammonia spirit
A concentration of 5%~10%.
Preferably, silicon carbide powder is scattered in before water system, silicon carbide powder is started the cleaning processing first.As one
Kind realization method, the cleaning treatment process of silicon carbide powder are：Silicon carbide powder is scattered in the hydrochloric acid solution of 2%-10%,
It is stood after being mixed evenly, supernatant liquid is removed after slurry layering, centrifugation then is carried out to gained slurry and distilled water is clear
It washes, until pH value in neutral range, is finally dried, obtains silicon carbide powder.
A kind of sic powder of polymolecularity can also be made using the method for the present invention, be the method using the present invention
It improves silicon carbide powder to be stood, dried after dispersion stabilization in water system, obtains the sic powder of polymolecularity.
Compared with prior art, beneficial effects of the present invention are as follows：
(1) dispersant sucrose ester is added after silicon carbide powder is scattered in water system.Sucrose ester is uncharged nonionic
Surfactant is rich in hydrophilic hydroxyl, mainly passes through space stability ultimate load to the dispersion of the silicon carbide powder in water system
Mechanism is completed, its one end is adsorbed on silicon-carbide particle surface, and the state of stretching, extension is presented in the strand of the other end, forms space
Barrier provides steric hindrance, and the reunion and sedimentation of silicon carbide powder particle in the slurry, therefore energy can be hindered under its effect
Enough improve dispersion stabilization of the silicon carbide powder in aqueous based systems suspension.
(2) simultaneously, research finds that pH value influences the molecular conformation and degree of ionization of dispersant, and carbonization can be adjusted by adjusting pH value
The charged characteristic on silicon particle surface, makes Particle surface charge increase, and electronic double layer repulsion can increase, to increase silicon carbide water system body
The stability of system；The isoelectric point (IEP) of silicon carbide powder particle is generally pH=3~6 in pulp suspension, in isoelectric point
Place, silicon-carbide particle surface can form stable uncharged silanol, and particle positive and negative charge numerical value is equal in suspension at this time,
Zeta potential is zero, and electrostatic repulsion zero, particle is easy to happen reunion and sedimentation；When pH value is higher, silicon-carbide particle band is negative
Charge, pH value is bigger, and particle surface institute is negatively charged more, and Zeta potential gradually increases, and is conducive to silicon carbide powder particle and exists
Dispersion stabilization in water system.By many experiments exploration discovery, pH value is adjusted when between 8~12, can realize silicon carbide
There is good dispersion stabilization in water system, especially dispersibility is good when pH value is 10.
(3) preparation process of the present invention is easy to operate, uses dispersant is nontoxic, energy conservation and environmental protection, at low cost, prepares
Silicon carbide water system in the good dispersion of silicon carbide, stability it is high, can be used as silicon carbide slurry and pass through the techniques systems such as injection forming
Standby silicon carbide ceramics, can be improved the dispersion stabilization of silicon carbide ceramics.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of silicon carbide powder obtained in comparative example 1；
Fig. 2 is the scanning electron microscopic picture of the silicon carbide powder obtained in embodiment 1 when pH value is 10 in step (1)；
Fig. 3 is the viscosity of suspension section and the relationship of pH value in the silicon carbide slurry that step (1) obtains in embodiment 1；
Fig. 4 is that the volume of distribution of silicon carbide solid phase in the silicon carbide slurry that step (1) obtains in embodiment 1 is (referred to as heavy
Product volume) with the relationship of pH value；
Fig. 5 is the viscosity and dispersant of suspension section in the silicon carbide slurry that step (1) obtains in embodiment 2
Relationship；
Fig. 6 is that the volume of distribution of silicon carbide solid phase in the silicon carbide slurry that step (1) obtains in embodiment 2 is (referred to as heavy
Product volume) with the relationship of dispersant.
Specific implementation mode
With reference to embodiment, present invention is further described in detail, it should be pointed out that embodiment described below purport
Convenient for the understanding of the present invention, and any restriction effect is not played to it.
Embodiment 1：
In the present embodiment, the preparation method of silicon carbide ceramics powder is as follows：
(1) silicon carbide powder is scattered in distilled water, silicon carbide powder quality is 1 with distilled water mass ratio:1, then
Sucrose ester surfactants solution is added, sucrose ester quality is made to account for the 25% of silicon carbide quality, is mixed under conditions of 750r/min
Stirring 5h is closed, silicon carbide slurry is obtained；
For sucrose ester as dispersant, ethyl alcohol, as solvent, is by sucrose ester with acetone in the surfactant solution
It is dissolved at a temperature of 60~80 DEG C, ethyl alcohol and acetone then is added and prepares to obtain；
Then, the pH value that silicon carbide slurry is adjusted with ammonium hydroxide and hydrochloric acid, obtains six groups that pH is respectively 2,4,6,8,10,12
Slurry continues to stir 1h under conditions of 300r/min, the pH value of silicon carbide slurry is adjusted after stirring again, to ensure pH
It is worth constant；The silicon carbide slurry is stood later, the distribution space of wherein silicon carbide solid phase is observed after stablizing, and samples top
Suspension, by the solid concentration information for measuring the available wherein silicon carbide of its viscosity；
(2) it takes out silicon carbide slurry to stand for 24 hours, is finally putting into drying in 50 DEG C of constant temperature drying boxes and for 24 hours, obtains silicon carbide pottery
Ceramic powder.
Comparative example 1：
The present embodiment is the comparative example of above-described embodiment 1.
In the present embodiment, the preparation method of silicon carbide ceramics powder is as follows：
(1) silicon carbide powder is scattered in distilled water, silicon carbide powder quality is 1 with distilled water mass ratio:1,
5h is mixed under conditions of 750r/min, obtains silicon carbide slurry；
(2) identical as step (2) in embodiment 1.
Fig. 1 is the scanning electron microscopic picture of silicon carbide powder obtained in comparative example 1.Fig. 2 is to work as step in embodiment 1
Suddenly the scanning electron microscopic picture of the silicon carbide powder obtained when pH value is 10 in (1).The two compares, in display and comparative example 1
It is compared without the silicon carbide powder of sucrose ester surfactants solution modification, sucrose ester surfactants is passed through in embodiment 1
The reunion of silicon carbide powder reduces after solution modification, favorable dispersibility.
Fig. 3 is the viscosity of suspension section and the pass of pH value in the silicon carbide slurry that step (1) obtains in above-described embodiment 1
System, display is with the increase of pH value, and suspension viscosity, which is presented, first increases the trend subtracted afterwards, the major part depositing SiC as pH=2
In bottom, suspension viscosity is minimum；As pH value increases, silicon carbide dispersibility is gradually increased, and the deposition volume of bottom gradually subtracts
Small, carborundum content gradually rises in the suspension of top, and suspension viscosity gradually increases；As pH=8, suspension viscosity is most
Greatly；When pH value continues growing, suspension viscosity declines, this is because ammonium hydroxide continuously adds, although pH value continues growing, carbon
SiClx dispersibility still improves, but increases suspension vol simultaneously, and the solid concentration of silicon carbide declines in suspension
The reason of, but even if viscosity declines, as pH=12, viscosity is still higher.
Fig. 4 is the volume of distribution and pH value of silicon carbide solid phase in the silicon carbide slurry that step (1) obtains in above-described embodiment 1
Relationship, show as pH=2, volume of distribution is relatively low, this is because most of depositing SiC is in bottom；With the increasing of pH value
Add, dispersibility of the silicon carbide in suspension improves, and distribution space volume gradually increases；As pH=10, silicon carbide solid phase
Distribution space volume it is maximum, reach 100ml, illustrating silicon carbide powder particle, dispersibility and stability is most in aqueous based systems
It is good；When continuing growing gradual pH value, the distribution space volume of silicon carbide solid phase declines, but as pH=12, the distribution
Spatial volume is still higher.
Embodiment 2：
In the present embodiment, the preparation method of silicon carbide ceramics powder is as follows：
(1) silicon carbide powder is scattered in distilled water, silicon carbide powder quality is 1 with distilled water mass ratio:1, then
Sucrose ester surfactants solution is added, sucrose ester quality is made to account for the 5% of silicon carbide quality, 10% respectively, 15%, 20%,
25%, 30%, 5h is mixed under conditions of 750r/min, obtains six groups of silicon carbide slurries；
For sucrose ester as dispersant, ethyl alcohol, as solvent, is by sucrose ester with acetone in the surfactant solution
It is dissolved at a temperature of 60~80 DEG C, ethyl alcohol and acetone then is added and prepares to obtain；
Then, the pH value that silicon carbide slurry is adjusted with ammonium hydroxide and hydrochloric acid, it is 10 to obtain pH, under conditions of 300r/min after
Continuous stirring 1h, adjusts the pH value of silicon carbide slurry, to ensure that pH value is constant again after stirring；Silicon carbide slurry is stood later
Material, observes the distribution space of wherein silicon carbide solid phase, and sample the suspension on top after stablizing, can by measuring its viscosity
Obtain the solid concentration information of wherein silicon carbide；
(2) it takes out silicon carbide slurry to stand for 24 hours, is finally putting into drying in 50 DEG C of constant temperature drying boxes and for 24 hours, obtains silicon carbide pottery
Ceramic powder.
Fig. 5 is that the viscosity of suspension section in the silicon carbide slurry that step (1) obtains in above-described embodiment 2 contains with dispersant
The relationship of amount.Fig. 6 be in the silicon carbide slurry that step (1) obtains in above-described embodiment 2 volume of distribution of silicon carbide solid phase with point
The relationship of powder content.From show that sucrose ester adds content to the viscosity of suspension section and silicon carbide solid phase in Fig. 3 and Fig. 4
Volume of distribution has large effect.When dispersant is 5%, the viscosity of suspension section and the distribution body of silicon carbide solid phase
Product is all minimum；When dispersant increases, the viscosity of dispersant suspension section and the volume of distribution of silicon carbide solid phase totally become
Gesture is constantly increased with the increase of dispersant；When dispersant reaches 25%, the distribution body of silicon carbide solid phase
Product reaches maximum；When dispersant continues growing, the viscosity of suspension section continues growing, and the distribution body of silicon carbide solid phase
Product no longer changes, this is because there are a critical values for the absorption on sucrose ester and silicon-carbide particle surface, when sucrose ester content reaches
When to 25%, silicon-carbide particle can be thoroughly dispersed in water system system suspension at this time, and steric hindrance function and effect are best.When
When the content of sucrose ester continues growing, an oversaturated state can be reached, inherently had when sucrose ester is soluble in water certain
Viscosity, content increase can cause slurry viscosity to continue to increase, and particle occurs to reunite and flocculation, mobility are deteriorated.Therefore, when point
When powder content is 25%, slurry dispersibility and stability reach best.
Embodiment 3：
(1) essentially identical with the step (1) in embodiment 1, except that sucrose ester quality accounts for silicon carbide quality
5%, the pH value that silicon carbide slurry is adjusted with ammonium hydroxide and hydrochloric acid is 10；
(2) identical as step (2) in embodiment 1.
Embodiment 4：
(1) essentially identical with the step (1) in embodiment 1, except that sucrose ester quality accounts for silicon carbide quality
10%, the pH value that silicon carbide slurry is adjusted with ammonium hydroxide and hydrochloric acid is 10；
(2) identical as step (2) in embodiment 1.
Embodiment 5：
(1) essentially identical with the step (1) in embodiment 1, except that sucrose ester quality accounts for silicon carbide quality
20%, the pH value that silicon carbide slurry is adjusted with ammonium hydroxide and hydrochloric acid is 10；
(2) identical as step (2) in embodiment 1.
Embodiment 6：
The present embodiment is substantially the same manner as Example 3, the difference is that before step (1), is carried out such as to silicon carbide powder
Lower processing：
Silicon carbide powder is scattered in 5% hydrochloric acid solution, is made into the suspension that solid volume fraction is 20% respectively,
It is stood after 1h is mixed under conditions of 750r/min, removes supernatant liquid after suspension layering, then to gained suspension
Centrifugation and distilled water cleaning are carried out, until suspension pH value in neutral range, is finally putting into drying in 100 DEG C of constant temperature drying boxes
12h obtains silicon carbide powder.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method improving silicon carbide powder dispersion stabilization in water system, it is characterized in that：Silicon carbide powder is scattered in
In water system, it is made into the slurry that solid volume fraction is 10%-50%, sucrose ester surfactants solution is added, makes sucrose ester matter
Amount accounts for the 5%-30% of silicon carbide quality, is mixed evenly, obtains mixed liquor, and adjust the pH value of the mixed liquor 8~
Between 12；
In the sucrose ester surfactants solution, sucrose ester is solute, and ethyl alcohol is solvent.
2. the method for improving silicon carbide powder dispersion stabilization in water system as described in claim 1, it is characterized in that：Described
The mean particle size range of silicon carbide powder is 7.5 μm~102.5 μm.
3. the method for improving silicon carbide powder dispersion stabilization in water system as described in claim 1, it is characterized in that：Sucrose ester
Quality accounts for the 15%-25% of silicon carbide quality, preferably 25%.
4. the method for improving silicon carbide powder dispersion stabilization in water system as described in claim 1, it is characterized in that：Adjusting should
The pH value of mixed liquor is 9~10.
5. the method for improving silicon carbide powder dispersion stabilization in water system as described in claim 1, it is characterized in that：Described
Sucrose ester surfactants solution is to dissolve sucrose ester at a temperature of 60~80 DEG C, and ethyl alcohol then is added and prepares to obtain.
6. the method for improving silicon carbide powder dispersion stabilization in water system as claimed in claim 4, it is characterized in that：Described
Further include acetone in sucrose ester surfactants solution.
7. the method for improving silicon carbide powder dispersion stabilization in water system as described in claim 1, it is characterized in that：Utilize alkali
Adjust the pH value of the mixed solution；The alkali is one kind in sodium hydroxide solution and ammonium hydroxide；As further preferred, hydrogen
A concentration of the 5%~10% of sodium hydroxide solution, a concentration of the 5%~10% of ammonia spirit.
8. the method for improving silicon carbide powder dispersion stabilization in water system as described in claim 1, it is characterized in that：Silicon carbide
Powder is scattered in before water system, first starts the cleaning processing silicon carbide powder.
9. the method for improving silicon carbide powder dispersion stabilization in water system as claimed in claim 8, it is characterized in that：Silicon carbide
The cleaning treatment process of powder is：Silicon carbide powder is scattered in the hydrochloric acid solution of 2%-10%, is mixed evenly rear quiet
It sets, supernatant liquid is removed after slurry layering, centrifugation then is carried out to gained slurry and distilled water cleans, until pH value is in neutrality
It in range, is finally dried, obtains silicon carbide powder.
10. a kind of preparation method of the sic powder of polymolecularity utilizes any claim institute in such as claim 1 to 9
The method stated improves silicon carbide powder dispersion stabilization in water system, is then stood, is dried, obtains the carbonization of polymolecularity
Silica flour material.
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| CN111463113A (en) * | 2020-05-25 | 2020-07-28 | 哈尔滨晶创科技有限公司 | Processing method for protecting silicon carbide surface in semi-insulating SiC ion doping annealing process |
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