CN102731111A - Novel preparation method of ceramic microspheres - Google Patents
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- CN102731111A CN102731111A CN2012102314080A CN201210231408A CN102731111A CN 102731111 A CN102731111 A CN 102731111A CN 2012102314080 A CN2012102314080 A CN 2012102314080A CN 201210231408 A CN201210231408 A CN 201210231408A CN 102731111 A CN102731111 A CN 102731111A
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Abstract
The invention provides a novel preparation method of ceramic microspheres. The method is characterized by comprising the following steps: mechanically blending or ball-milling reactant materials of the ceramic microspheres, dispersant and water to obtain uniform suspension slurry with good dispersity and carrying out deforming treatment on the obtained suspension slurry; dripping the slurry subjected to the deforming treatment by a dispersing device into hydrophobic powder with pre-etched round grooves; under the action of the surface tension, enabling the liquid drops to be shrunk to form the microspheres, wherein the powder covering the microspheres allows the microspheres to maintain good sphericity; drying and screening to obtain the precursor of the ceramic microspheres; and, calcining and sintering the blanks of the ceramic microspheres to finally obtain the ceramic microspheres. The ceramic microspheres have the characteristics of good sphericity, high strength, controllable grain size and good dispersity. The preparation method provided by the invention has the characteristics of simple process, high production efficiency and low cost, and is liable to realize the scale production.
Description
Technical field
The invention belongs to the stupalith field, relate in particular to tritium proliferating agent in the fusion reactor covering, support of the catalyst, grinding medium is with the preparation of ceramic microsphere.
Technical background
Stupalith is acknowledged as to have: advantage such as HS, high firmness and good wear resistance and erosion resistance; Have the incomparable characteristics of material such as metallic substance, organic polymer in some Application Areas, in numerous industries, bringing into play indispensable effect.Ceramic microsphere is meant that generally particle diameter is other inorganic non-metallic sintered compact of millimeter level, is spheroid or approximate spheroid, and various ways such as fine and close and porous microsphere are arranged according to request for utilization.The millimetre-sized ceramic microsphere of monodispersity has a wide range of applications at aspects such as nuclear reactor, matrix material, catalysis, separation purification, medicine.The ceramic microsphere that contains lithium can be used as a kind of solid tritium proliferating agent, have easy to use, the advantage of thermal property and satisfactory mechanical property.Ceramic microsphere also can be used as the reinforcing filler of plastics, rubber, nylon products, can make to fill evenly.Ceramic microsphere can also stress on underground oil field layer as a kind of proppant, can obviously improve oil production efficient.Ceramic microsphere with a fixed gap can also be used for Chemical Manufacture as support of the catalyst.Different Application Areass also proposes different requirement to material, density, sphere diameter and the sphericity etc. of ceramic microsphere.
About the preparation of millimeter level ceramic microsphere, existing at present several different methods.Mainly can be divided into according to its balling-up principle: (1) is through reactive force balling-up (as: granulation-rolling method, extrusion molding-rolling method, mould pressing etc.) such as mechanical force such as extruding, friction, collisions; (2) utilize principle spherical container shaping methods such as surface/interface tension force (as: method of fusion, sol-gel method, gaze at the method for forming etc.).Though these technologies can be produced the ceramic microsphere that satisfies different needs, be difficult to satisfy simultaneously performance, efficient and economic environmental protection requirement.Therefore, it is high to be necessary to seek a kind of production efficiency, the low and environment amenable novel process of preparation cost.
Summary of the invention
The present invention provide a kind of brand-new simple, economical, raw material is suitable for wide forming method; Its principle is to utilize the hydrophobicity of fluidic surface tension and outer coated composite powder body mobile with half; The preparation average particulate diameter is at the ceramic microsphere of 0.2～3mm scope; And can prepare densification or porous ceramic microsphere as required, in order to satisfy the needs of different field.
The powder coated legal system is equipped with ceramic microsphere, specifically may further comprise the steps:
(1) pulp preparation: dispersion agent is dissolved in the water, add ceramic powder then, obtain stable slurry, froth breaking degasification again behind stirring or the ball milling;
(2) microballoon moulding: the above-mentioned slurry that makes is splashed into diverting device in the hydrophobic powder that is carved with circular groove in advance, and the slurry drop is shrunk to sphere by powder coated and under surface tension effects;
(3) drying and screening: will be transferred to together with powder by the slurry drop of powder wrapped and carry out drying in the baking oven, and obtain the microballoon presoma that the surface speckles with small quantities of powder after sieving;
(4) calcining: the microballoon presoma in (3) is calcined in oxidizing atmosphere, and the powder voloxidation at high temperature on surface is fallen, and it is pure to obtain composition, has the green microspheres of certain intensity;
(5) sintering: take corresponding system to carry out sintering according to the character of ceramic powder, obtain the ceramic microsphere of size and porosity.
Further, in the technique scheme, in the slurry that said step (1) obtains, the solid content of ceramic powder is 35%-55%; Dispersant dosage is 0.2～2% of a ceramic powder.
Further, in the technique scheme, ceramic powder is for be not higher than 500 ℃ inorganic salt, oxide compound, nitride and composition thereof etc. with water generates chemical reaction and fusing point, like Li in the said step (1)
2TiO
3, Li
2ZrO
3, LiAlO
2, LiTaO
3, Li
4SiO
4, ZrO
2, Al
2O
3, Si
3N
4, tourmalinite, trichroite, or add carbon black as pore former.
Further, in the technique scheme, in the said step (2), hydrophobic powder is Graphite Powder 99 or carbon dust 1～2 kind, and diameter of particle is 1～500 μ m.The selection of diameter of particle is by the microsphere diameter size decision of need preparation, and microsphere diameter is big more, the also corresponding increase of the particle diameter of available Graphite Powder 99 or carbon dust.
Further, in the technique scheme, in the said step (2), the bottom of circular groove is a semisphere, and diameter equates that with the slurry drop degree of depth of groove is 0.5～2 times of diameter.
Further, in the technique scheme, in the said step (2), the preparation method of groove has the plate of spherical protuberances or cylinder light pressure on smooth Graphite Powder 99 or carbon dust to form with the surface.
Further, in the technique scheme, in the said step (3), microballoon is dry together with graphite or carbon dust, and temperature is a room temperature to 110 ℃, and temperature rise rate is 0.1～5 ℃ of a per minute, soaking time 0.5～100 hour.For preventing that the dry too fast microballoon presoma that causes from shrinking inhomogeneous or cracking, can take temperature-gradient method.
Further, in the technique scheme, in the said step (3), the isolating method of microballoon and Graphite Powder 99 or carbon dust is for sieving, and the width of sieve aperture should be less than diameter of micro ball, and Graphite Powder 99 or carbon dust after sieving are reusable.Sieve and adopt mesh to be slightly less than the metallic screen of microballoon.
Further, in the technique scheme, said step (4) calcination atmosphere is an oxidizing atmosphere, and temperature is 500～1000 ℃, and temperature rise rate is 0.5～10 ℃ of a per minute, is incubated 0～10 hour.Like graphite or carbon on the surface or infiltrate inside and do not influence use and also can in inertia or reducing atmosphere, calcine.Graphite Powder 99 of being selected for use or carbon dust particle diameter are big more, the then corresponding rising of calcining temperature.
Principle of the present invention is: utilize the hydrophobicity of graphite or carbon dust and fluid under surface tension, to be shrunk to the spheric principle; Graphite Powder 99 or carbon dust are coated on slurry drop surface; Play parcel and isolate the effect of slurry drop and picking-up, keep original sphere behind the slurry droplet drying.Just can be after sieving with microballoon presoma and unnecessary powder separation, the graphite on microballoon idiosome surface or carbon dust just can obtain the ceramic microsphere of different purposes 500～1000 ℃ of voloxidation behind the knot that reburns.
The invention has the advantages that:
(1) method of employing powder coated has been simplified composition of raw materials, has improved the stability of technology, and is simultaneously easy to operate, need not complex apparatus and can realize producing, and is beneficial to practicability and promotes.
(2) Graphite Powder 99 or the carbon dust after sieving can use repeatedly, consumes seldom at every turn, so promptly reduced cost, reduced environmental pollution again.
(3) presoma inside does not contain caking agent, and Graphite Powder 99 or carbon dust only are bonded at the idiosome surface, thus when calcining internal stress little, can realize being rapidly heated, need not independent decarburization program, calcining and sintering can once be accomplished.
(4) forming step is few, and production efficiency is high, can be easy to realize with batching, moulding, drying and the bead step of sieving integrated, thereby realize industrial production in enormous quantities.
Embodiment
Embodiment 1: the tritium proliferating agent is with the preparation of lithium titanate ceramic microsphere
With Li
2TiO
3Powder and water are raw material, and Triammonium citrate is as dispersion agent, and isooctyl alcohol is a skimmer.Select the Graphite Powder 99 of the about 20 μ m of median size for use, the ceramic microsphere of preparation particle diameter 0.8mm, undertaken by following step:
(1) with Li
2TiO
3Powder, water and Triammonium citrate mix, the slurry of configuration solid content 45%, and the Triammonium citrate quality is Li
2TiO
30.4% of powder quality; With mixed solution on planet mill with 300 commentaries on classics/PM ball millings 4 hours, add the isooctyl alcohol of powder quality 0.1%, restir vacuumizes 5min; Obtain the uniform sizing material of good dispersivity;
(2) Graphite Powder 99 is spread out strickling, extrude diameter 1mm on the surface, the hemispherical groove of dark 2mm splashes into slurry and to be carved with on the groove Graphite Powder 99 through diverting device;
(3) slurry drop and Graphite Powder 99 are transferred to baking oven together, 50 ℃ of dryings were warming up to 110 ℃ of dryings 1 hour again after 4 hours, obtain the microballoon presoma after sieving;
(4) the microballoon presoma that the surface is speckled with Graphite Powder 99 is put into muffle furnace, is heated to 600 ℃ with the temperature rise rate of 5 ℃ of per minutes, is incubated furnace cooling after 4 hours, obtains the green microspheres of certain intensity;
(5) green microspheres is transferred in the high temperature resistance furnace, is heated to 1150 ℃ of insulations 2 hours, obtain the Li of the about 0.8mm of diameter behind the furnace cooling with 5 ℃ of temperature rise rates of per minute
2TiO
3Microballoon.
Embodiment 2: the tritium proliferating agent is with the preparation of lithium niobate ceramic microsphere
With γ-LiAlO
2Powder and water are raw material, and ammonium polyacrylate is as dispersion agent, and lipid acid is skimmer.Select the carbon dust of the about 50 μ m of median size for use, the ceramic microsphere of preparation particle diameter 1mm, undertaken by following step:
(1) with γ-LiAlO
2Powder, water and ammonium polyacrylate mix, the slurry of configuration solid content 50%, and the Triammonium citrate quality is γ-LiAlO
20.4% of powder quality; With mixed solution continuously stirring 2 hours, add the lipid acid of powder quality 0.1% then, restir vacuumizes 10min; Obtain the uniform sizing material of good dispersivity;
(2) carbon dust is spread out strickling, extrude diameter 1.3 mm on the surface, the hemispherical groove of dark 2mm splashes into slurry and to be carved with on the groove carbon dust through diverting device;
(3) slurry drop and carbon dust are transferred to baking oven together, 60 ℃ of dryings were warming up to 110 ℃ of dryings 2 hours again after 2 hours, obtain the microballoon presoma after sieving;
(4) the microballoon presoma that the surface is speckled with carbon dust is put into muffle furnace, is heated to 500 ℃ with the temperature rise rate of 2 ℃ of per minutes, is incubated furnace cooling after 5 hours, obtains the green microspheres of certain intensity;
(5) green microspheres is transferred in the high temperature resistance furnace, is heated to 1250 ℃ of insulations 1 hour, obtain γ-LiAlO of the about 1mm of diameter behind the furnace cooling with 2 ℃ of temperature rise rates of per minute
2Microballoon.
Embodiment 3: the tritium proliferating agent is with the preparation of positive lithium silicate ceramic microsphere
With Li
4SiO
4Powder and water are raw material, and Triammonium citrate is as dispersion agent, and lipid acid is skimmer.Select for use the carbon dust of median size 50 μ m and the Graphite Powder 99 of 20 μ m to mix, the Li of preparation particle diameter 1mm by mass ratio 1:1
4SiO
4Ceramic microsphere, undertaken by following step:
(1) with Li
4SiO
4Powder, water and Triammonium citrate mix, the slurry of configuration solid content 55%, and the Triammonium citrate quality is Li
4SiO
40.5% of powder quality; With mixed solution on planet mill with 300 commentaries on classics/PM ball millings 8 hours, add the lipid acid of powder quality 0.1%, restir vacuumizes 5min; Obtain the uniform sizing material of good dispersivity;
(2) mixture with graphite and carbon dust spreads out strickling, extrudes diameter 1.3 mm on the surface, and the hemispherical groove of dark 2mm splashes into slurry and to be carved with on the groove powder through diverting device;
(3) slurry drop and mixed powder are transferred to baking oven together, 50 ℃ of dryings were warming up to 110 ℃ of dryings 2 hours again after 4 hours, obtain the microballoon presoma after sieving;
(4) the microballoon presoma that the surface is speckled with powder is put into muffle furnace, is heated to 700 ℃ with the temperature rise rate of 2 ℃ of per minutes, is incubated furnace cooling after 2 hours, obtains the green microspheres of certain intensity;
(5) green microspheres is transferred in the high temperature resistance furnace, is heated to 1050 ℃ of insulations 2 hours, obtain the Li of the about 1mm of diameter behind the furnace cooling with 2 ℃ of temperature rise rates of per minute
4SiO
4Microballoon.
Embodiment 4: the preparation of wear-resisting zirconia ceramic microsphere
With ZrO
2Powder and water are raw material, and Triammonium citrate is a dispersion agent, and dimethyl silicone oil is a skimmer.Select the Graphite Powder 99 of median size 100 μ m for use, the ceramic microsphere of preparation particle diameter 2mm, concrete steps are following:
(1) with ZrO
2Powder, water and Triammonium citrate mix, the slurry of configuration solid content 50%, and the Triammonium citrate quality is ZrO
20.3% of powder quality; With mixed solution on planet mill with 300 commentaries on classics/PM ball millings 4 hours, add the methyl-silicone oil of powder quality 0.2%, restir vacuumized 10 minutes; Obtain the uniform sizing material of good dispersivity;
(2) Graphite Powder 99 is spread out strickling, extrude diameter 2.5mm on the surface, the hemispherical groove of dark 3mm splashes into slurry and to be carved with on the groove Graphite Powder 99 through diverting device;
(3) slurry drop and Graphite Powder 99 are transferred to baking oven together, 40 ℃ of dryings were warming up to 110 ℃ of dryings 1 hour again after 8 hours, and sieving obtains the microballoon idiosome;
(4) the microballoon presoma that the surface is speckled with Graphite Powder 99 is put into muffle furnace, is heated to 900 ℃ with the temperature rise rate of 2 ℃ of per minutes, is incubated furnace cooling after 3 hours, obtains the green microspheres of certain intensity.
(5) green microspheres is transferred in the high temperature resistance furnace, is heated to 1600 ℃ of insulations 2 hours, obtain the ZrO of the about 2mm of diameter behind the furnace cooling with 4 ℃ of temperature rise rates of per minute
2Bead.
Embodiment 5: the preparation of porous cordierite ceramic microballoon
With trichroite 2Mg2Al
2O
35SiO
2, water is raw material, Triammonium citrate is a dispersion agent, lipid acid is skimmer, the carbon black of particle diameter 20 μ m is done pore former.Select the carbon dust of median size 100 μ m for use, the ceramic foam microballoon of preparation particle diameter 3mm, concrete steps are following:
(1) cordierite powder, carbon black, water and Triammonium citrate are mixed, the slurry of configuration solid content 40%, the mass ratio of trichroite and carbon black is 7:3, the Triammonium citrate quality is 0.4% of trichroite and a carbon black total mass powder quality; With mixed solution on planet mill with 300 commentaries on classics/PM ball millings 2 hours, add the lipid acid of powder quality 0.2% then, restir obtains the uniform sizing material of good dispersivity after 10 minutes;
(2) carbon dust is spread out strickling, extrude diameter 4mm on the surface, the hemispherical groove of dark 6mm splashes into slurry and to be carved with on the groove Graphite Powder 99 through diverting device;
(3) slurry drop and carbon dust are transferred to baking oven together, 70 ℃ of dryings are after 10 hours, and sieving obtains the microballoon presoma;
(4) the microballoon presoma that the surface is speckled with carbon dust is put into muffle furnace, is heated to 800 ℃ with the temperature rise rate of 4 ℃ of per minutes, is incubated furnace cooling after 4 hours, obtains the green microspheres of certain intensity.
(5) green microspheres is transferred in the high temperature resistance furnace, is heated to 1200 ℃ of insulations 2 hours, obtain the porous cordierite ceramic bead of the about 3mm of diameter behind the furnace cooling with per 5 ℃ of temperature rise rates.
Embodiment 6: the preparation of porous alumina microballoon
With Al
2O
3, water is raw material, Triammonium citrate is a dispersion agent, lipid acid is skimmer, the carbon black of particle diameter 20 μ m is done pore former.Select the Graphite Powder 99 of median size 200 μ m for use, the ceramic foam microballoon of preparation particle diameter 3mm, concrete steps are following:
(1) with Al
2O
3Powder, carbon black, water and Triammonium citrate mix, the slurry of configuration solid content 40%, Al
2O
3With the mass ratio of carbon dust be 7:3, the ammonium citrate quality is 0.4% of aluminum oxide and a carbon black total mass powder quality; With mixed solution continuously stirring 4 hours, add the lipid acid restir 10min of powder quality 0.1% then, obtain the uniform sizing material of good dispersivity;
(2) Graphite Powder 99 is spread out strickling, extrude diameter 4mm on the surface, the hemispherical groove of dark 6mm splashes into slurry and to be carved with on the groove Graphite Powder 99 through diverting device;
(3) microballoon drop and Graphite Powder 99 are transferred to baking oven together, 60 ℃ of dryings are after 10 hours, and 110 ℃ of dryings are 2 hours again, and sieving obtains the microballoon presoma;
(4) the microballoon presoma that the surface is speckled with Graphite Powder 99 is put into muffle furnace, is heated to 1000 ℃ with the temperature rise rate of 4 ℃ of per minutes, is incubated furnace cooling after 1 hour, obtains the green microspheres of certain intensity.
(5) green microspheres is transferred in the high temperature resistance furnace, is heated to 1600 ℃ of insulations 2 hours, obtain the porous Al of the about 3mm of diameter behind the furnace cooling with per 5 ℃ of temperature rise rates
2O
3Ceramic bead.
Claims (9)
1. the novel preparation method of a ceramic microsphere is characterized in that, process step is:
(1) pulp preparation: dispersion agent is dissolved in the water, add ceramic powder then, obtain stable slurry, froth breaking degasification again behind stirring or the ball milling;
(2) microballoon moulding: the above-mentioned slurry that makes is splashed into diverting device in the hydrophobic powder that is carved with circular groove in advance, and the slurry drop is shrunk to sphere by powder coated and under surface tension effects;
(3) drying and screening: will be transferred to together with powder by the slurry drop of powder wrapped and carry out drying in the baking oven, and obtain the microballoon presoma that the surface speckles with small quantities of powder after sieving;
(4) calcining: the microballoon presoma in (3) is calcined in oxidizing atmosphere, and the powder voloxidation at high temperature on surface is fallen, and it is pure to obtain composition, has the green microspheres of certain intensity;
(5) sintering: take corresponding system to carry out sintering according to the character of ceramic powder, obtain the ceramic microsphere of size and porosity.
2. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1, it is characterized in that: in the slurry that said step (1) obtains, the solid content of ceramic powder is 35%-55%; Dispersant dosage is 0.2～2% of a ceramic powder.
3. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1; It is characterized in that: in the said step (1); Ceramic powder is for being higher than inorganic salt, oxide compound, nitride of 500 ℃ and composition thereof with water generates chemical reaction and fusing point, or adds carbon black as pore former.
4. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1, it is characterized in that: in the said step (2), hydrophobic powder is Graphite Powder 99 or carbon dust 1～2 kind, and diameter of particle is 1-500 μ m.
5. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1, it is characterized in that: in the said step (2), the bottom of circular groove is a semisphere, diameter and slurry drop equal diameters semisphere, the degree of depth is 0.5～2 times of a diameter.
6. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1 is characterized in that: in the said step (2), the preparation method of groove has the plate of spherical protuberances or cylinder light pressure on smooth powder to form with the surface.
7. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1; It is characterized in that: in the said step (3), microballoon is dry together with graphite or carbon dust, and temperature is a room temperature to 110 ℃; Temperature rise rate is 0.1～5 ℃ of a per minute, soaking time 0.5～100 hour.
8. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1; It is characterized in that: in the said step (3); The isolating method of microballoon and Graphite Powder 99 or carbon dust is for sieving, and the width of sieve aperture should be less than diameter of micro ball, and Graphite Powder 99 or carbon dust after sieving are reusable.
9. the novel preparation method of a kind of ceramic microsphere as claimed in claim 1, it is characterized in that: said step (4) calcination atmosphere is an oxidizing atmosphere, and temperature is 500～1000 ℃, temperature rise rate is 0.5～10 ℃ of a per minute, is incubated 0.5～10 hour.
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| CN103387395A (en) * | 2013-07-25 | 2013-11-13 | 天津城建大学 | Hollow ceramic microsphere and preparation method of hollow ceramic microsphere |
| CN103708419A (en) * | 2013-12-27 | 2014-04-09 | 北京科技大学 | Method for preparing of high-activity LiH microspheres through wet process |
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| CN104387043A (en) * | 2014-10-27 | 2015-03-04 | 北京科技大学 | Preparation method of lithium-silicate-based gradient ceramic microspheres |
| CN105801108B (en) * | 2016-03-11 | 2018-09-14 | 北京科技大学 | A kind of preparation method of three-dimensional open-framework lithium matrix body tritium increment agent material |
| CN105801108A (en) * | 2016-03-11 | 2016-07-27 | 北京科技大学 | Preparation method of three-dimensional open-framework structure lithium base block tritium value-added agent material |
| CN106966716A (en) * | 2017-03-14 | 2017-07-21 | 清华大学 | The preparation method of high-voltage gradient ZnO voltage-sensitive ceramic microballoons |
| CN107140953B (en) * | 2017-04-18 | 2019-11-22 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN107325320A (en) * | 2017-07-21 | 2017-11-07 | 中国工程物理研究院激光聚变研究中心 | The method for avoiding polystyrene type tiny balloon drying process from ftractureing |
| CN107325320B (en) * | 2017-07-21 | 2020-03-24 | 中国工程物理研究院激光聚变研究中心 | Method for preventing polystyrene hollow microsphere from cracking in drying process |
| CN108554370A (en) * | 2018-03-30 | 2018-09-21 | 华中科技大学 | A kind of spherical lithium base CO2The preparation method and equipment of adsorbent |
| CN108554370B (en) * | 2018-03-30 | 2020-07-10 | 华中科技大学 | Spherical lithium-based CO2Method and equipment for preparing adsorbent |
| CN108911735A (en) * | 2018-05-24 | 2018-11-30 | 四川大学 | A kind of high sphericity tritium multiplication agent nanostructure metatitanic acid lithium ceramic bead and preparation method thereof |
| CN108911735B (en) * | 2018-05-24 | 2020-11-03 | 四川大学 | High-sphericity tritium breeder nano-structure lithium titanate ceramic pellet and preparation method thereof |
| CN113045318A (en) * | 2021-05-11 | 2021-06-29 | 西北工业大学 | Submicron carbide ceramic hollow microsphere and preparation method thereof |
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