CN107903074A - A kind of ceramic material sintering aid and preparation method thereof - Google Patents
A kind of ceramic material sintering aid and preparation method thereof Download PDFInfo
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- CN107903074A CN107903074A CN201711001742.6A CN201711001742A CN107903074A CN 107903074 A CN107903074 A CN 107903074A CN 201711001742 A CN201711001742 A CN 201711001742A CN 107903074 A CN107903074 A CN 107903074A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention discloses a kind of ceramic material sintering aid and preparation method thereof, by water soluble starch, silica, iron chloride, chitosan, the raw materials such as citric acid are made, the present invention is by magnetic nano-particle and water soluble starch, the materials such as silica combine, optimize the size distribution of product, with higher diffusion rate, because particle is tiny, diffusion length is short, so that the sintering activity of nano-particle greatly improves, it can be gathered in the gap between sintering feed and play the role of acceleration of sintering, so as to reduce integral sintered temperature, on the other hand, the present invention has extremely strong adsorptivity and very high chemism, thus easily it is combined and tends towards stability with other atoms, can effectively it be filled in the gap and surface pore of ceramic material, improve the consistency of sintering, improve ceramic sintered product quality.
Description
Technical field
The present invention relates to sintering aid technical field, more particularly to a kind of ceramic material sintering aid and preparation method thereof.
Background technology
With the development of science and technology, it is also proposed new requirement to the performance of engineering material, ceramic material is due to excellent performance
And it is used widely.Yet with sintering temperature height, it is necessary to consume the substantial amounts of energy, the requirement to Thermal Equipment is also high, together
When portion of material excessive hole in sintering cause that its matrix density is high, also needs to carry out the subsequent treatments such as carburizing after sintering
Deng performance and production cost to workpiece all have a certain impact, thus limit its use scope to a certain extent.From
Save the energy, reduction discharge capacity, the angle of environmental protection to set out, develop novel sintered auxiliary agent becomes ceramic material low-temperature sintering
Focus on research direction.
Magnetic nano-particle is as a kind of new material developed in recent years, not only with nano effect, i.e. surface
Effect, small-size effect, macro quanta tunnel effect and bulk effect, also with magnetic property, such as superparamagnetism and high magnetization
The characteristics such as rate.Its application develops into high-technology field from traditional technical field, is expanded to from simple magnetics scope
With the relevant interdisciplinary field of magnetics.Among these ferroferric oxide magnetic nano-particles have different from common material light,
The unusual performance of electricity, magnetic, thermodynamics and chemical reaction etc., can significantly reduce the sintering temperature and porosity of ceramic material.
Since the size of nano-particle is very small, there is very high surface energy, be a kind of thermodynamic unstable system, easily
Be agglomerated into larger particle, but due in solution nanoparticle surface carry many chemical bonds, can have very active chemistry
Property, ferroferric oxide magnetic nano-particles are as a kind of special nano-particle, due to magnetic dipole gravitation between particle, easily
Reunite, aggregate into offspring in the solution, be not easy to disperse, therefore compared to general nano-particle for, ferroso-ferric oxide
The surface of magnetic nano-particle is modified just very necessary.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided a kind of ceramic material sintering aid and its preparation
Method.
The present invention is achieved by the following technical solutions：
A kind of ceramic material sintering aid, is prepared by the following method：
（1）Water soluble starch is added to the water, is warming up to 80-90 DEG C, gelatinization adds titanium dioxide thereto after 50-60 minutes
The mass ratio of silicon, wherein water soluble starch and silica is (2-2.5):1, be stirred continuously to being uniformly mixed, after the completion of it is dry
Cross 50-60 mesh sieves；
（2）Step 1 resulting material is sent into high temperature furnace, is warming up to 750-850 DEG C, postcooling, will to room temperature when sintering 4-5 is small
Gained sintered product is sent into decarbonizing furnace, and it is spare that 80-100 mesh sieves are crossed when insulation decarburization 2-3 is small at 500-550 DEG C, after taking-up；
（3）Iron chloride is pressed into solid-to-liquid ratio 1：（28-32）G/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then thereto
Anhydrous sodium acetate and polyethylene glycol are added, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1：（2.5-2.7）：
（0.7-0.8）, 50-55 DEG C is warming up to, is stirred continuously to uniform mixed liquor is formed, ultrasonic disperse is uniformly sent into reaction kettle afterwards,
Be warming up to 200-220 DEG C, when reaction 5-6 is small after takes out and is cooled to room temperature, and with ethanol and clear water alternately cleaning removing impurity, by
Obtained solid is dried, and obtains Superparamagnetic Fe3O4 nanoparticles；
（4）Step 3 gained ferriferrous oxide nano-particle is dispersed in 20-25% ethanol solutions, then adds shell thereto
Glycan and citric acid, mixed liquor is transferred in blender, and connection nitrogen protection, is warming up to 35-40 DEG C and with 800-1000 revs/min
Stirring 30-40 minutes, products therefrom ethanol and clear water are alternately cleaned, until pH is 7, be re-fed into drying box after stirring
In dried, it is spare that chitosan-citric acid duplex surface modification magnetic ferroferric oxide nano-particles are obtained after grinding；
（5）By step 2 resulting material and step 4 gained nano-particle in mass ratio（1-1.5）：1 is mixed to join in oleic acid, rises
Temperature is to when insulation standing 8-10 is small after 68-72 DEG C, and filtering afterwards, which is taken out, simultaneously dries, up to sintering aid of the present invention.
The carbon content of water soluble starch is 50-55% in the step 1.
Front row is sintered in high temperature furnace in the step 2 and remove furnace air, and it is 3-4 to be passed through ratio：1 ammonia and hydrogen
Mixed gas is as reaction atmosphere.
Ultrasound condition is to be ultrasonically treated 10-12 minutes under 35-38kHz in the step 3.
Ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are in the step 4（5-6）：（1-1.2）：
（2-2.5）.
It is an advantage of the invention that：
The present invention carries out surface modification by preparing ferriferrous oxide nano-particle, and with chitosan and citric acid are compound to it,
The electronegative polar end of citric acid has been utilized respectively by Coulomb force and ferroso-ferric oxide institute is positively charged attracts each other and shell
Functional group in glycan forms chemical bonds with its surface, so as to locally be coated to ferroso-ferric oxide particle surface, improves
Its inoxidizability and dispersion stabilization in use, then it is combined with materials such as water soluble starch, silica, optimize
The size distribution of product, with higher diffusion rate, because particle is tiny, diffusion length is short so that nano-particle
Sintering activity greatly improve, can be gathered in the gap between sintering feed and play the role of acceleration of sintering, so as to reduce whole
Body sintering temperature, on the other hand, the present invention have extremely strong adsorptivity and a very high chemism, thus easily with other atoms
It is combined and tends towards stability, can effectively be filled in the gap and surface pore of ceramic material, improves the consistency of sintering,
Improve ceramic sintered product quality.
Embodiment
A kind of ceramic material sintering aid, is prepared by the following method：
（1）The water soluble starch that carbon content is 50% is added to the water, is warming up to 80 DEG C, gelatinization adds thereto after 50 minutes
The mass ratio of silica, wherein water soluble starch and silica is 2.4:1, be stirred continuously to be uniformly mixed, after the completion of do
Dry 50 mesh sieve of mistake；
（2）Step 1 resulting material is sent into high temperature furnace, furnace air is removed at sintering front row, and is passed through ratio as 3：1 ammonia and
Hydrogen gas mixture is warming up to 750 DEG C, postcooling is to room temperature when sintering 4 is small, by gained sintered product afterwards as reaction atmosphere
It is sent into decarbonizing furnace, it is spare that 80 mesh sieves is crossed when insulation decarburization 2 is small at 500 DEG C, after taking-up；
（3）Iron chloride is pressed into solid-to-liquid ratio 1：30g/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then add nothing thereto
Water sodium acetate and polyethylene glycol, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1：2.7：0.7, it is warming up to 50
DEG C, it is stirred continuously to uniform mixed liquor is formed, is ultrasonically treated under 35kHz 10 minutes and is sent into after being uniformly dispersed in reaction kettle, risen
Temperature to 200 DEG C, when reaction 5 is small after takes out and is cooled to room temperature, and removing impurity is alternately cleaned with ethanol and clear water, by obtained solid
It is dry, obtain Superparamagnetic Fe3O4 nanoparticles；
（4）Step 3 gained ferriferrous oxide nano-particle is dispersed in 20% ethanol solution, then adds shell thereto and gathers
Sugar and citric acid, wherein ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are 5.5：1：2.2, mixed liquor is turned
Enter in blender, connection nitrogen protection, is warming up to 35 DEG C and is stirred 30 minutes with 800 revs/min, by products therefrom after stirring
Alternately cleaned with ethanol and clear water, until pH is 7, is re-fed into drying box and is dried, chitosan citrate is obtained after grinding
Duplex surface modification magnetic ferroferric oxide nano-particles are spare；
（5）By step 2 resulting material and step 4 gained nano-particle in mass ratio 1.2：1 is mixed to join in oleic acid, is warming up to
When insulation standing 8 is small after 68 DEG C, filtering afterwards, which is taken out, simultaneously dries, up to sintering aid of the present invention.
Claims (5)
1. a kind of ceramic material sintering aid, it is characterised in that be prepared by the following method：
（1）Water soluble starch is added to the water, is warming up to 80-90 DEG C, gelatinization adds titanium dioxide thereto after 50-60 minutes
The mass ratio of silicon, wherein water soluble starch and silica is (2-2.5):1, be stirred continuously to being uniformly mixed, after the completion of it is dry
Cross 50-60 mesh sieves；
（2）Step 1 resulting material is sent into high temperature furnace, is warming up to 750-850 DEG C, postcooling, will to room temperature when sintering 4-5 is small
Gained sintered product is sent into decarbonizing furnace, and it is spare that 80-100 mesh sieves are crossed when insulation decarburization 2-3 is small at 500-550 DEG C, after taking-up；
（3）Iron chloride is pressed into solid-to-liquid ratio 1：（28-32）G/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then thereto
Anhydrous sodium acetate and polyethylene glycol are added, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1：（2.5-2.7）：
（0.7-0.8）, 50-55 DEG C is warming up to, is stirred continuously to uniform mixed liquor is formed, ultrasonic disperse is uniformly sent into reaction kettle afterwards,
Be warming up to 200-220 DEG C, when reaction 5-6 is small after takes out and is cooled to room temperature, and with ethanol and clear water alternately cleaning removing impurity, by
Obtained solid is dried, and obtains Superparamagnetic Fe3O4 nanoparticles；
（4）Step 3 gained ferriferrous oxide nano-particle is dispersed in 20-25% ethanol solutions, then adds shell thereto
Glycan and citric acid, mixed liquor is transferred in blender, and connection nitrogen protection, is warming up to 35-40 DEG C and with 800-1000 revs/min
Stirring 30-40 minutes, products therefrom ethanol and clear water are alternately cleaned, until pH is 7, be re-fed into drying box after stirring
In dried, it is spare that chitosan-citric acid duplex surface modification magnetic ferroferric oxide nano-particles are obtained after grinding；
（5）By step 2 resulting material and step 4 gained nano-particle in mass ratio（1-1.5）：1 is mixed to join in oleic acid, rises
Temperature is to when insulation standing 8-10 is small after 68-72 DEG C, and filtering afterwards, which is taken out, simultaneously dries, up to sintering aid of the present invention.
2. the preparation method of ceramic material sintering aid according to claim 1, it is characterised in that water in the step 1
The carbon content of soluble starch is 50-55%.
3. the preparation method of ceramic material sintering aid according to claim 1, it is characterised in that in the step 2
Front row is sintered in high temperature furnace and removes furnace air, and it is 3-4 to be passed through ratio：1 ammonia and hydrogen gas mixture is as reaction atmosphere.
4. the preparation method of ceramic material sintering aid according to claim 1, it is characterised in that surpass in the step 3
Sound condition is to be ultrasonically treated 10-12 minutes under 35-38kHz.
5. the preparation method of ceramic material sintering aid according to claim 1, it is characterised in that four in the step 4
Fe 3 O nano-particle, chitosan, the mass ratio of citric acid are（5-6）：（1-1.2）：（2-2.5）.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108752015A (en) * | 2018-06-12 | 2018-11-06 | 佛山市华强协兴陶瓷有限公司 | A kind of ceramic material sintering aid and preparation method thereof |
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| CN104910445A (en) * | 2015-06-09 | 2015-09-16 | 天津大学 | Chitosan-coated ferroferric oxide magnetic nano composite particle and preparation method thereof |
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