CN109761612A - A kind of low temperature high-performance silicon carbide film layer and preparation method thereof - Google Patents
A kind of low temperature high-performance silicon carbide film layer and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of low temperature high-performance silicon carbide film layers and preparation method thereof.Pass through the oxidation using silicon carbide powder in the high temperature environment, the silica that particle surface generates, silica reacts with the nanoscale alumina sol for being wrapped in silicon-carbide particle surface being added, set up mullite network structure, the intensity of granular boundary is enhanced, liquid phase is reduced using the presence of nanometer level RE oxide molecule and generates temperature, it is suppressed that the growth of mullite grains, so that the aggregate molecular particle size in film layer is uniform, film resistance is reduced.It is not necessarily to control atmosphere in silicon carbide film layer sintering process of the present invention, and adjusts the degree of oxidation of silicon carbide by the ratio of firing temperature, Aluminum sol addition.Entire preparation process is simple, and controllably, so that the firing temperature of the more existing silicon carbide film layer of firing temperature of the invention substantially reduces, firing energy consumption also substantially reduces accordingly, to greatly save the preparation cost.
Description
Technical field
The present invention relates to silicon carbide separation membrane materials, are specifically related to a kind of low temperature high-performance silicon carbide film layer and its preparation side
Method.
Background technique
Since silicon carbide separation membrane material has low contact angle, wellability is good, there is an elecrtonegativity, and it is excellent that antifouling property is good etc.
Point, therefore it has highly important application value in water treatment field, but since it is there are firing temperature height, atmosphere requirements are harsh
The problems such as, therefore the extensive use of silicon carbide separation membrane material seriously is limited, the development of water treatment field is constrained, the problem is anxious
It needs to solve.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of low temperature high-performance silicon carbide film layer and its
Preparation method.
According to an aspect of the invention, there is provided a kind of preparation method of low temperature high-performance silicon carbide film layer, including with
Lower step:
It is coated in silicon carbide, Aluminum sol, rare earth and dispersant on corresponding supporter, is burnt at 1000-1190 DEG C
It is fired at a temperature of to obtain the final product.
Further, it by silicon carbide, Aluminum sol, rare earth and dispersant, is coated on corresponding supporter,
It is fired under 1000-1190 DEG C of firing temperature, comprising:
Silicon carbide, Aluminum sol, rare earth and dispersant must disperse solution;
Dispersion solution mixes to obtain film slurry with defoaming agent;
Film slurry is coated on corresponding supporter, after dry, is fired under 1000-1190 DEG C of firing temperature.
Wherein, the solid content weight ratio of silicon carbide, the solid content of Aluminum sol, rare earth are as follows: (80-99): (15-0.1): (10-
0.1)。
Rare earth be scandium oxide, yttrium oxide, lanthana, cerium oxide, praseodymium oxide, neodymia, promethium oxide, samarium oxide, europium oxide,
The nano-powder or colloidal sol of at least one of gadolinium oxide, terbium oxide, dysprosia, holimium oxide, erbium oxide, ytterbium oxide, luteium oxide.
Dispersing agent is one of ethyl alcohol, POLYPROPYLENE GLYCOL, polyacrylic acid, Sodium Polyacrylate or a variety of.
Further, the hybrid mode for dispersing solution and defoaming agent uses stirring vacuum ultrasonic disperse.
Film slurry is immersion film-coated or spraying overlay film in the coating method of corresponding supporter.
Supporter is silicon carbide, aluminium oxide, cordierite, a kind of material supporter in mullite.
According to another aspect of the present invention, a kind of high-performance silicon carbide film layer, including mullite cubic network are provided
Structure and nanometer level RE oxide.
The high-performance silicon carbide film layer is made according to method described above.
Compared with prior art, the invention has the following advantages:
Exemplary low temperature high-performance silicon carbide film layer of the present invention and preparation method thereof, according to the accumulation principle preparation of film layer aggregate
Hole, the silica generated by the oxidation using aggregate silicon carbide powder in the high temperature environment, particle surface, oxidation reaction make
Silicon-carbide particle pattern becomes mellow and full, the resistance of film layer when further reducing filtering, and the silica of generation is the same as the packet being added
The nanoscale alumina sol for being rolled in silicon-carbide particle surface reacts, it is established that mullite network structure, the network structure is by bone
Material is connected by point with point contact, and the content of remnants silica is extremely low after reaction, easily and alkali due to the silica
Method for generation, the reduction of dioxide-containing silica substantially increase the alkaline resistance properties of low temperature high-performance silicon carbide film layer, mullite net
The foundation of network structure significantly enhances the intensity of granular boundary, and the present invention is reduced using the presence of nanometer level RE oxide molecule
Liquid phase generates temperature, it is suppressed that the growth of mullite grains reduces film layer so that the aggregate molecular particle size in film layer is uniform
Resistance.Without controlling atmosphere in silicon carbide film layer sintering process of the present invention, and by ratio that firing temperature, Aluminum sol are added come
Adjust the degree of oxidation of silicon carbide.Entire preparation process is simple, controllably, so that the more existing silicon carbide film of firing temperature of the invention
The firing temperature of layer substantially reduces, and firing energy consumption also substantially reduces accordingly, thus greatly save the preparation cost, meanwhile,
It is not necessarily to the addition of silicon source in whole preparation process, improves the alkali resistance of film layer, product prepared in accordance with the present invention, pore-size distribution
Narrow, filtering accuracy is high, is higher than similar product with the water flux under precision, film layer high mechanical strength, and acid-proof alkaline is good.Such as preparation
The aperture 100nm silicon carbide film layer, by film layer pore diameter range prepared by the above method in 100-120nm accuracy rating, flux
It can reach 800-1000m3/m2H, film layer Mohs' hardness 8-9 are boiled by the aqueous slkali of 20% sulfuric acid solution/1% respectively
After 5h, film layer Mohs' hardness is 8 after acid, film layer Mohs' hardness 8 after alkali.Continue to boil, intensity no longer becomes after alkali after the acid of film layer
Change.
Specific embodiment
In order to be better understood by technical solution of the present invention, the present invention is made into one below with reference to specification specific embodiment
Walk explanation.
Embodiment one
The low temperature high-performance silicon carbide film layer preparation process of the present embodiment are as follows:
S1, by 80:15:5 in proportion weigh silicon carbide (0.05-200 microns), Aluminum sol solid content and rare-earth oxidation
Scandium nano powder is added in dispersing agent ethyl alcohol, is placed on mixing in device being stirred to obtain and is dispersed solution;
S2, defoaming agent will be added in dispersion solution, and will be put into film slurry preparation facilities and is stirred vacuum ultrasonic and disperses to obtain film
Slurry.
S3, film slurry is coated on silicon carbide supporter by means such as immersion film-coated, spraying overlay films, solidification is dried
Afterwards, it is burnt at 1100 DEG C up to silicon carbide film layer.
Embodiment two
The low temperature high-performance silicon carbide film layer preparation process of the present embodiment are as follows:
S1, by 99:0.9:0.1 in proportion weigh silicon carbide (0.05-200 microns), Aluminum sol solid content and rare earth
The solid content of yttrium oxide colloidal sol is added in dispersing agent POLYPROPYLENE GLYCOL, is placed on mixing in device being stirred to obtain and is dispersed solution;
S2, defoaming agent will be added in dispersion solution, and will be put into film slurry preparation facilities and is stirred vacuum ultrasonic and disperses to obtain film
Slurry.
S3, film slurry is coated in alumina support by means such as immersion film-coated, spraying overlay films, solidification is dried
Afterwards, it is burnt at 1190 DEG C up to silicon carbide film layer.
Embodiment three
The low temperature high-performance silicon carbide film layer preparation process of the present embodiment are as follows:
S1, by 89.9:0.1:10 in proportion weigh silicon carbide (0.05-200 microns), Aluminum sol solid content and rare earth
Lanthana is added to dispersion with cerium oxide mixing nano-powder (lanthana is 1:1 with the weight ratio of cerium oxide mixing nano-powder)
Agent polyacrylic acid, Sodium Polyacrylate mixed liquor (polyacrylic acid, Sodium Polyacrylate volume ratio be 1:1) in, be placed on mixing in device
It is stirred to obtain dispersion solution;
S2, defoaming agent will be added in dispersion solution, and will be put into film slurry preparation facilities and is stirred vacuum ultrasonic and disperses to obtain film
Slurry.
S3, film slurry is coated on cordierite supporter by means such as immersion film-coated, spraying overlay films, solidification is dried
Afterwards, it is burnt at 1000 DEG C up to silicon carbide film layer.
Example IV
The low temperature high-performance silicon carbide film layer preparation process of the present embodiment are as follows:
S1, by 90:7:3 in proportion weigh silicon carbide (0.05-200 microns), Aluminum sol solid content and rare-earth oxidation
Praseodymium, neodymia, promethium oxide, samarium oxide, europium oxide collosol intermixture solid content (praseodymium oxide, neodymia, cerium oxide, samarium oxide,
The weight ratio of europium oxide colloidal sol is 1:1:1:1:1) it is added in dispersing agent polyacrylic acid, it is placed on mixing and is stirred score in device
Dissipate solution;
S2, defoaming agent will be added in dispersion solution, and will be put into film slurry preparation facilities and is stirred vacuum ultrasonic and disperses to obtain film
Slurry.
S3, film slurry is coated on mullite supporter by means such as immersion film-coated, spraying overlay films, solidification is dried
Afterwards, it is burnt at 1000-1190 DEG C up to silicon carbide film layer.
Embodiment five
The low temperature high-performance silicon carbide film layer preparation process of the present embodiment are as follows:
S1, silicon carbide (0.05 micron), the solid content of Aluminum sol and the rare-earth oxidation gadolinium for weighing 80:15:10 in proportion
Nano-powder is added in dispersing agent Sodium Polyacrylate, is placed on mixing in device being stirred to obtain and is dispersed solution;
S2, defoaming agent will be added in dispersion solution, and will be put into film slurry preparation facilities and is stirred vacuum ultrasonic and disperses to obtain film
Slurry.
S3, film slurry is coated in the supporter (branch of various shape various material by means such as immersion film-coated, spraying overlay films
Support body, such as silicon carbide, aluminium oxide, cordierite, mullite) on, after solidification is dried, it is burnt at 1000-1200 DEG C to obtain the final product
Silicon carbide film layer.
Embodiment six
The low temperature high-performance silicon carbide film layer preparation process of the present embodiment are as follows:
S1, silicon carbide (100 microns), the solid content of Aluminum sol and the rare-earth oxidation terbium for weighing 99:0.1:10 in proportion
Nano-powder is added in dispersing agent ethyl alcohol, is placed on mixing in device being stirred to obtain and is dispersed solution;
S2, defoaming agent will be added in dispersion solution, and will be put into film slurry preparation facilities and is stirred vacuum ultrasonic and disperses to obtain film
Slurry.
S3, film slurry is coated in the supporter (branch of various shape various material by means such as immersion film-coated, spraying overlay films
Support body, such as silicon carbide, aluminium oxide, cordierite, mullite) on, after solidification is dried, it is burnt at 1000 DEG C up to silicon carbide
Film layer.
Embodiment seven
The feature that the present embodiment is the same as example 1 repeats no more, and the present embodiment feature different from embodiment one exists
In:
Rare earth is the mixture of dysprosia, holimium oxide, erbium oxide nano-powder, dysprosia, holimium oxide, erbium oxide nano powder
The weight ratio of body is 1:2:2.
Embodiment eight
The present embodiment feature identical with embodiment three repeats no more, and the present embodiment feature different from embodiment three exists
In:
Rare earth be ytterbium oxide, luteium oxide colloidal sol mixture, ytterbium oxide, luteium oxide colloidal sol weight ratio be 1:2.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Claims (10)
1. a kind of preparation method of low temperature high-performance silicon carbide film layer, characterized in that the following steps are included:
Silicon carbide, Aluminum sol, rare earth and dispersant are coated on corresponding supporter, in 1000-1190 DEG C of firing temperature
It is fired under degree to obtain the final product.
2. the preparation method of high-performance silicon carbide film layer according to claim 1, characterized in that by silicon carbide, Aluminum sol,
Rare earth and dispersant are coated on corresponding supporter, fire under 1000-1190 DEG C of firing temperature, comprising:
Silicon carbide, Aluminum sol, rare earth and dispersant must disperse solution;
Dispersion solution mixes to obtain film slurry with defoaming agent;
Film slurry is coated on corresponding supporter, after dry, is fired under 1000-1190 DEG C of firing temperature.
3. the preparation method of low temperature high-performance silicon carbide film layer according to claim 2, characterized in that silicon carbide, aluminium are molten
The solid content weight ratio of the solid content of glue, rare earth are as follows: (80-99): (15-0.1): (10-0.1).
4. the preparation method of low temperature high-performance silicon carbide film layer according to claim 2 or 3, characterized in that rare earth is oxygen
Change scandium, yttrium oxide, lanthana, cerium oxide, praseodymium oxide, neodymia, promethium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, oxygen
Change the nano-powder or colloidal sol of at least one of dysprosium, holimium oxide, erbium oxide, ytterbium oxide, luteium oxide.
5. the preparation method of low temperature high-performance silicon carbide film layer according to claim 4, characterized in that dispersing agent is second
One of alcohol, POLYPROPYLENE GLYCOL, polyacrylic acid, Sodium Polyacrylate are a variety of.
6. the preparation method of low temperature high-performance silicon carbide film layer according to claim 4, characterized in that disperse solution and disappear
The hybrid mode of infusion uses stirring vacuum ultrasonic disperse.
7. the preparation method of low temperature high-performance silicon carbide film layer according to claim 6, characterized in that film is starched corresponding
The coating method of supporter is immersion film-coated or spraying overlay film.
8. the preparation method of low temperature high-performance silicon carbide film layer according to claim 6, characterized in that supporter is carbonization
Silicon, aluminium oxide, cordierite, a kind of material supporter in mullite.
9. a kind of low temperature high-performance silicon carbide film layer, characterized in that including mullite dimensional network structure and nano-scale rare earth oxygen
Compound.
10. low temperature high-performance silicon carbide film layer according to claim 9, characterized in that -8 any institute according to claim 1
Method is stated to be made.
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CN112226661A (en) * | 2020-10-16 | 2021-01-15 | 内蒙金属材料研究所 | Ablation-resistant molybdenum alloy and preparation method thereof |
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CN113800942A (en) * | 2021-10-22 | 2021-12-17 | 滁州学院 | Silicon carbide molecular sieve membrane support and application thereof on molecular sieve membrane |
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Application publication date: 20190517 |