CN107140953B - A kind of method that quick extrusion prepares ceramic microsphere - Google Patents
A kind of method that quick extrusion prepares ceramic microsphere Download PDFInfo
- Publication number
- CN107140953B CN107140953B CN201710252125.7A CN201710252125A CN107140953B CN 107140953 B CN107140953 B CN 107140953B CN 201710252125 A CN201710252125 A CN 201710252125A CN 107140953 B CN107140953 B CN 107140953B
- Authority
- CN
- China
- Prior art keywords
- slurry
- ceramic
- ceramic microsphere
- microsphere
- extrusion molding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/20—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein the material is extruded
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
- C04B2235/3203—Lithium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/94—Products characterised by their shape
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to ceramic microspheres to manufacture correlative technology field, and disclose a kind of method that quick extrusion prepares ceramic microsphere, comprising: be uniformly mixed ceramic powder, binder, dispersing agent, defoaming agent and deionized water and form required slurry；The technological parameter of ceramic microsphere to be processed is set according to demand；Slurry is transferred in the size barrel of extrusion molding equipment, and slurry is quickly squeezed out using preset technological parameter, it is formed by drop to be fallen into the container molding containing curing agent solution dropwise, and to form spherical green body via the collective effect of curing agent and surface tension to shrink；Spherical green body is collected, and is dried and required ceramic microsphere product is made after calcination process.Through the invention, do not need any mold in entire manufacturing process, processing is quickly, controllability is strong, high production efficiency, it is low in cost the features such as, be therefore particularly suitable for the high-volume large-scale production of ceramic microsphere.
Description
Technical field
The invention belongs to ceramic microspheres to manufacture correlative technology field, quickly squeeze out preparation ceramics more particularly, to a kind of
The method of microballoon.
Background technique
Ceramic material has many advantages, such as that hardness is high, wearability is good, corrosion resistance is good, good insulating, machinery, material, chemical industry,
The fields such as electric power, military affairs are widely used.It is the other inorganic non-metallic sintering of grade that ceramic microsphere, which generally refers to partial size,
Body is in spherical or approximate sphericity.Ceramic microsphere nuclear reactor, composite material, catalysis, in terms of have it is extensive
Using.For example, the ceramic microsphere containing lithium can be used as a kind of solid tritium multiplication agent, there is easy to use, hot property and mechanical performance
Good advantage.
The method for preparing ceramic microsphere at present mainly has the precipitation method, polymerization-inducing colloidal aggregation method, sol-gel method, gas
Flow polishing, granulation-rolling method, extrusion forming-rolling method etc..Specifically, for example CN104140259A discloses one kind
Quickly preparation LiTiO3The method that tritium is proliferated bead, it is rapid-result fastly using SLS using epoxy resin, stearic acid or nylon as binder
Shape ceramic bead and hot isostatic pressing densify LiTiO3Bead, manufactured bead have many advantages, such as high sphericity, high-compactness；But
Be this method preparation cost it is high, and the high requirements on the equipment.For another example, CN105330288A, which is disclosed, a kind of prepares zirconium oxide microballoons
Method, with ZrOCl2·8H2O is initial feed, acrylamide is organic monomer, poly amic acid is dispersing agent, Ammonium Persulfate 98.5
Ceramic slurry is prepared for initiator and deionized water, slurry is distributed in methyl-silicone oil and is solidified into spherical shape, through dry and sintering
It can be made into the zirconia ceramics microballoon of 0.5~2mm diameter afterwards, microballoon spherical shape is good, high mechanical properties；But the production of this method is imitated
Rate is not high, and especially acrylamide has toxicity, has accordingly influenced practice.For another example, CN101857442A discloses one
The preparation method of kind lithium-based ceramic microsphere will be made mixing slurry after the mixing of binder, water and ceramic powder, and carry out water-bath and add
Colloidal sol is made after heat, slurry is added dropwise to dispersal device and forms microballoon with the medium of water mutual exclusion, by microballoon washing, it is dry and
Lithium-based ceramic microsphere is made in sintering；However, further investigations have shown that, the production efficiency of this method is not high, it is difficult to realize large quantities of
Amount production.
On the whole, all kinds of preparation processes in the prior art often require mold, deposit to production cost and efficiency
It is adversely affecting；Furthermore some key indexes such as size tunable, in terms of need further to be improved.Correspondingly,
This field needs to find more perfect solution, to meet growing quality and technique requirement.
Summary of the invention
For the above insufficient or Improvement requirement of the prior art, the present invention provides a kind of quick extrusions to prepare ceramic microsphere
Method accordingly research and propose and abundant benefit wherein by being designed to as the crucial pulp components for participating in object and proportion
Ceramic microsphere is formed with the principle of slurry droplet ejection rapid shaping to process；Additionally the important process of subsequent technique is joined
Number carry out targeted designs, accordingly can preferably with slurry curing and surface tension of liquid effect come obtain size tunable and
The better ceramic microsphere of ball-type degree, and do not need any mold in entire technical process, exist simultaneously high efficiency, high quality,
It is at low cost, non-toxic and convenient for manipulation the advantages that, be therefore particularly suitable for large-scale production application occasion.
To achieve the above object, it is proposed, according to the invention, provide a kind of method that quick extrusion prepares ceramic microsphere, feature
It is, this method includes the following steps:
(i) ceramic powder, binder, dispersing agent, defoaming agent and deionized water are uniformly mixed and form slurry, and each group
The mass percent setting divided is as follows: ceramic powder 60%~80%, binder 0.5%~1%, dispersant 0.8%
~1.5%, antifoam content is 0.3%~0.6%, remaining is deionized water；
(ii) technological parameter of ceramic microsphere to be processed is set according to demand, including microsphere diameter size parameter, is extruded into
Type path etc.；
(iii) slurry formed according to step (i) is transferred in the size barrel of extrusion molding equipment, and uses step
(ii) technological parameter set by quickly squeezes out slurry, be formed by drop fallen into dropwise to containing curing agent solution at
In type container, and spherical green body is formed to shrink via the collective effect of curing agent and surface tension；
(iv) collection step (iii) is formed by spherical green body, and be dried and calcination process after be made it is required
Ceramic microsphere product.
As it is further preferred that the ceramic powder is preferably one of following substance or it is mixed in step (i)
Close object: Al2O3、SiO2、ZrO2、Li2TiO3、Li2SiO4；The binder is preferably PVA-1788, PVA-2088 or PVA-
2488；The dispersing agent is preferably the mixture of acetic acid, propionic acid or both；The defoaming agent be preferably organic silicon defoamer or
Fatty acid.
As it is further preferred that the mass percent of each component further preferably set it is as follows: ceramic powder 75%, glue
Agent 0.8% is tied, dispersant 1.5%, antifoam content 0.5%, remaining is deionized water.
As it is further preferred that the extrusion molding path is preferably designed to surround in same in step (ii)
Mandrel, and former and later two are formed by drop and are not on same position.
As it is further preferred that in step (iii), it is preferred to use curing agent be boric acid or borax, solution be it is sweet
Oil solution, and curing agent preferable amount is the 5%~15% of glycerite quality.As it is further preferred that in step
(iii) in, it is preferred to use nozzle quickly squeezes out the slurry, and the jet diameters of the nozzle are 0.5mm~1.5mm.
As it is further preferred that the quantity of the nozzle is preferably several in step (iii), and this multiple spray
Liquid level distance between mouth and the curing agent solution remains unchanged.
As it is further preferred that in step (iii), for the droplet retracts to be formed to the process of spherical green body,
Its technological parameter preferred design is as follows: inlet pressure is 10psi~30psi, slurry pressure is 0.01psi~0.03psi, squeezes
The time is 0.03s~0.08s out.
As it is further preferred that the condition of the drying process is preferably as follows in step (iv): drying temperature 40
DEG C~60 DEG C, drying time be 1h~4h；The condition of the calcination process is preferably as follows: maturing temperature be 600 DEG C~1500 DEG C,
Soaking time is 2h~6h.
As it is further preferred that the sphericity of made ceramic microsphere product is 1.02 or so, partial size can basis
The diameter of the nozzle and change.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit:
1, it is proposed using the quick extrusion theory of slurry by pionerring research come processing ceramic microballoon, while to slurry
Component and charge ratio exclusively carry out design, measurement shows that the use of mold can not only be avoided, while in the subsequent process can
The effect of curing agent and surface tension of liquid is enough preferably quoted to improve molding effect, accordingly compared with the prior art in product
It is significantly increased in terms of quality and efficiency；
2, present invention is alternatively directed to such as microballoon forming path, nozzle syringe needle of the important technical parameter in quick shaping process is big
Small, slurry, which finds time etc., carries out research and contrast test, accordingly can be further assured that and quickly prepares size tunable and spherical shape
The ceramic microsphere spent；
3, the material system that the present invention uses has the advantages that at low cost and avirulent, is provided simultaneously with and does not need any mould
Tool, processing is quickly, controllability is strong, high production efficiency, it is low in cost the features such as, be therefore particularly suitable for the high-volume of ceramic microsphere
Large-scale production.
Detailed description of the invention
Fig. 1 is the process flow diagram that ceramic microsphere is prepared according to quick extrusion constructed by the present invention；
Fig. 2 is the process schematic that the quick extrusion molding of slurry of the invention is shown as demonstration；
In all the appended drawings, identical appended drawing reference is used to denote the same element or structure, in which:
1- computer；2- size barrel；3- extrusion molding controller；4- nozzle；5-XY axis direction transmission parts；The axis side 6-Z
To transmission parts；7- device for storing liquid.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Fig. 1 is the process flow diagram that ceramic microsphere is prepared according to quick extrusion constructed by the present invention.Institute as shown in figure 1
Show, which mainly includes following scheme step:
Firstly, as one of key improvements of the invention, to the formula of size for executing subsequent quick extrusion molding into
It has gone and has studied and design.Specifically, shape can be uniformly mixed for ceramic powder, binder, dispersing agent, defoaming agent and deionized water
At slurry, and the mass percent setting of each component is as follows: ceramic powder 60%~80%, binder 0.5%~1%, point
Powder content is 0.8%~1.5%, and antifoam content is 0.3%~0.6%, remaining is deionized water.
Then, the technological parameter of ceramic microsphere to be processed is set according to demand, including microsphere diameter size parameter, is extruded into
Type path etc.；These technological parameters for example can store as STL format, and be stored in computer to call；
Then, the slurry configured is transferred in the size barrel of extrusion molding equipment, and uses preset technological parameter
Slurry quickly is squeezed out, drop is formed by and is fallen into dropwise into the container molding containing curing agent solution, and via solidification
The collective effect of agent and surface tension to form spherical green body to shrink；In the process, all kinds of existing extrusions appropriate can be used
Molding equipment, and preferably it configures nozzle to execute the concrete operations quickly squeezed out, the diameter of the nozzle head is to be, for example,
0.5mm~1.5mm, quantity can be one or more.
Finally, collecting spherical green body, and it is dried and required ceramic microsphere product is made after calcination process.
More specifically, as shown in Figure 2, the production system for preparing ceramic microsphere for quick extrusion according to the present invention is main
Including computer 1, size barrel 2, extrusion molding controller 3, nozzle 4, XY axis direction transmission parts 5, Z-direction transmission parts 6
With device for storing liquid 7 etc..Wherein computer 1 is used as central processing system, for inputting, storing and call quick shaping process to join
Number, and be for example connected via USB with quick extrusion molding apparatus signal.The lower part of the quick extrusion molding apparatus is device for storing liquid
7, transmission parts of the top equipped with size barrel 2 and for the size barrel to be executed to tri- axis free movement of XYZ, and the slurry
The lower part of bucket 2 is used to execute the concrete operations for quickly squeezing out drop equipped with nozzle 4.At work, 3 base of extrusion molding controller
The technological parameter provided by computer 1 manipulates each associated components specifically to realize preparation process, and as described above sufficiently
With the collective effect of slurry extrusion theory and curing agent and surface tension, and then obtain size tunable and sphericity
Good ceramic microsphere.
The course of work of test macro according to the invention is explained further below in conjunction with specific embodiment.
Embodiment 1: the preparation of aluminium oxide ceramics microballoon
(1) by Al2O3Powder, PVA-2088, acetic acid, organic silicon defoamer and deionized water are uniformly mixed and form slurry；Its
Middle Al2O3The content of powder is that 75%, PVA-2088 content is 1%, acetic acid content 1.5%, and organic silicon defoamer content is
0.6%, remaining is deionized water.
(2) size parameter of ceramic microsphere is set in computer and extrusion molding path, the size of ceramic microsphere is
1.2mm extrusion molding path need around a central axis and should be avoided two drops same position and guarantee nozzle with it is sweet
The liquid level of oil solution saves as STL format apart from constant.
(3) slurry in step (1) is transferred in the size barrel of the quick extrusion molding equipment of slurry, and by step (2)
The forming parameter of middle STL format imports in the control system of the quick extrusion molding equipment of slurry, the quick extrusion molding equipment of slurry
Nozzle syringe needle size be 1.2mm, nozzle number be 1.
(4) ceramic slurry extrusion is carried out using the quick extrusion molding equipment of slurry, and along certain path by drop rapidly
It is added dropwise in the glycerite containing 15% boric acid, slurry is shrunk to spherical shape under the action of curing agent and surface tension；Slurry
The technological parameter of quick extrusion molding equipment shaped ceramic green microspheres is as follows: inlet pressure 30psi, slurry pressure are
0.03psi, it finds time as 0.08s.
(5) ceramic microsphere is made in ceramic microsphere green body after drying and roasting, and drying temperature is 60 DEG C, drying time is
1h, maturing temperature is 1500 DEG C, heat preservation is 2h.
The sphericity of manufactured aluminium oxide ceramics microballoon is 1.03, and partial size is 1.2 ± 0.01mm.
Embodiment 2: the preparation of silicon oxide ceramics microballoon
(1) by SiO2Powder, PVA-2088, acetic acid, fatty acid and deionized water are uniformly mixed and form slurry；Wherein SiO2
The content of powder is that 70%, PVA-2088 content is 0.8%, and propionic acid content 1.2%, content of fatty acid 0.3%, remaining is
Deionized water.
(2) size parameter of ceramic microsphere is set in computer and extrusion molding path, the size of ceramic microsphere is
1mm, extrusion molding path need around a central axis and two drops should be avoided in same position and guarantee nozzle and glycerol
The liquid level of solution saves as STL format apart from constant.
(3) slurry in step (1) is transferred in the size barrel of the quick extrusion molding equipment of slurry, and by step (2)
The forming parameter of middle STL format imports in the control system of the quick extrusion molding equipment of slurry, the quick extrusion molding equipment of slurry
Nozzle syringe needle size be 1mm, nozzle number be 10.
(4) ceramic slurry extrusion is carried out using the quick extrusion molding equipment of slurry, and along certain path by drop rapidly
It is added dropwise in the glycerite containing 10% borax, slurry is shrunk to spherical shape under the action of curing agent and surface tension；；Slurry
The technological parameter of quick extrusion molding equipment shaped ceramic green microspheres is as follows: inlet pressure 20psi, slurry pressure are
0.02psi, it finds time as 0.05s.
(5) ceramic microsphere is made in ceramic microsphere green body after drying and roasting, and drying temperature is 50 DEG C, drying time is
2h, maturing temperature is 1200 DEG C, heat preservation is 3h.
The sphericity of manufactured silicon oxide ceramics microballoon is 1.02, and partial size is 1 ± 0.01mm.
Embodiment 3: the preparation of zirconia ceramics microballoon
(1) by ZrO2Powder, PVA-2488, acetic acid, fatty acid and deionized water are uniformly mixed and form slurry；Wherein ZrO2
The content of powder is that 80%, PVA-2488 content is 1%, acetic acid content 1.5%, content of fatty acid 0.6%, remaining is to go
Ionized water.
(2) size parameter of ceramic microsphere is set in computer and extrusion molding path, the size of ceramic microsphere is
1.5mm, extrusion molding path need around a central axis and should be avoided two drops same position and guarantee nozzle with it is sweet
The liquid level of oil solution saves as STL format apart from constant.
(3) slurry in step (1) is transferred in the size barrel of the quick extrusion molding equipment of slurry, and by step (2)
The forming parameter of middle STL format imports in the control system of the quick extrusion molding equipment of slurry, the quick extrusion molding equipment of slurry
Nozzle syringe needle size be 1.5mm, nozzle number be 2.
(4) ceramic slurry extrusion is carried out using the quick extrusion molding equipment of slurry, and along certain path by drop rapidly
It is added dropwise in the glycerite containing 15% borax, slurry is shrunk to spherical shape under the action of curing agent and surface tension；；Slurry
The technological parameter of quick extrusion molding equipment shaped ceramic green microspheres is as follows: inlet pressure 30psi, slurry pressure are
0.03psi, it finds time as 0.08s.
(5) ceramic microsphere is made in ceramic microsphere green body after drying and roasting, and drying temperature is 60 DEG C, drying time is
4h, maturing temperature is 1500 DEG C, heat preservation is 6h.
The sphericity of manufactured zirconia ceramics microballoon is 1.03, and partial size is 1.5 ± 0.02mm.
Embodiment 4: the preparation of metatitanic acid lithium ceramic microphere
(1) by Li2TiO3Powder, PVA-1788, propionic acid, organic silicon defoamer and deionized water are uniformly mixed and form slurry；
Wherein Li2TiO3The content of powder is that 60%, PVA-1788 content is 0.5%, and acetic acid content 0.8%, organic silicon defoamer contains
Amount is 0.3%, remaining is deionized water.
(2) size parameter of ceramic microsphere is set in computer and extrusion molding path, the size of ceramic microsphere is
0.5mm, extrusion molding path need around a central axis and should be avoided two drops same position and guarantee nozzle with it is sweet
The liquid level of oil solution saves as STL format apart from constant.
(3) slurry in step (1) is transferred in the size barrel of the quick extrusion molding equipment of slurry, and by step (2)
The forming parameter of middle STL format imports in the control system of the quick extrusion molding equipment of slurry, the quick extrusion molding equipment of slurry
Nozzle syringe needle size be 0.5mm, nozzle number be 3.
(4) ceramic slurry extrusion is carried out using the quick extrusion molding equipment of slurry, and along certain path by drop rapidly
It is added dropwise in the glycerite containing 5% boric acid, slurry is shrunk to spherical shape under the action of curing agent and surface tension；；Slurry
The technological parameter of quick extrusion molding equipment shaped ceramic green microspheres is as follows: inlet pressure 10psi, slurry pressure are
0.01psi, it finds time as 0.03s.
(5) ceramic microsphere is made in ceramic microsphere green body after drying and roasting, and drying temperature is 40 DEG C, drying time is
3h, maturing temperature is 600 DEG C, heat preservation is 6h.
The sphericity of manufactured metatitanic acid lithium ceramic microphere is 1.02, and partial size is 0.5 ± 0.01mm.
Embodiment 5: the preparation of silicic acid lithium ceramic microphere
(1) by Li2SiO4Powder, PVA-1788, acetic acid, fatty acid and deionized water are uniformly mixed and form slurry；Wherein
Li2SiO4The content of powder is that 65%, PVA-1788 content is 0.6%, acetic acid content 1%, content of fatty acid 0.4%,
Remaining is deionized water.
(2) size parameter of ceramic microsphere is set in computer and extrusion molding path, the size of ceramic microsphere is
0.8mm, extrusion molding path need around a central axis and should be avoided two drops same position and guarantee nozzle with it is sweet
The liquid level of oil solution saves as STL format apart from constant.
(3) slurry in step (1) is transferred in the size barrel of the quick extrusion molding equipment of slurry, and by step (2)
The forming parameter of middle STL format imports in the control system of the quick extrusion molding equipment of slurry, the quick extrusion molding equipment of slurry
Nozzle syringe needle size be 0.8mm, nozzle number be 20.
(4) ceramic slurry extrusion is carried out using the quick extrusion molding equipment of slurry, and along certain path by drop rapidly
It is added dropwise in the glycerite containing 5% borax, slurry is shrunk to spherical shape under the action of curing agent and surface tension；；Slurry
The technological parameter of quick extrusion molding equipment shaped ceramic green microspheres is as follows: inlet pressure 12psi, slurry pressure are
0.01psi, it finds time as 0.04s.
(5) ceramic microsphere is made in ceramic microsphere green body after drying and roasting, and drying temperature is 40 DEG C, drying time is
4h, maturing temperature is 800 DEG C, heat preservation is 6h.
The sphericity of manufactured silicic acid lithium ceramic microphere is 1.02, and partial size is 0.8 ± 0.02mm.
To sum up, through the invention constructed process mainly consider to be utilized slurry droplet ejection Quick-forming,
The principles such as the effect of curing agent and surface tension carry out researching and designing to as the crucial component for participating in object slurry and proportion, together
When the important technical parameter in microballoon fast shaping technology is improved, can quickly prepare size tunable and good sphericity
Ceramic microsphere, this method have the characteristics that simple process, high production efficiency, it is low in cost, do not need mold, it is thus possible to realize
The mass production of ceramic microsphere.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (4)
1. a kind of method that quick extrusion prepares ceramic microsphere, which is characterized in that this method includes the following steps:
(i) ceramic powder, binder, dispersing agent, defoaming agent and deionized water are uniformly mixed and form slurry, and each component
Mass percent setting is as follows: ceramic powder 60%~80%, binder 0.5%~1%, dispersant for 0.8%~
1.5%, antifoam content is 0.3%~0.6%, remaining is deionized water；Wherein, the ceramic powder is in following substance
Or mixtures thereof one kind: Al2O3、SiO2、ZrO2、Li2TiO3、Li2SiO4；The binder be PVA-1788, PVA-2088 or
PVA-2488；The dispersing agent is the mixture of acetic acid, propionic acid or both；The defoaming agent is organic silicon defoamer or fat
Acid
(ii) technological parameter of ceramic microsphere to be processed, including microsphere diameter size parameter, extrusion molding road are set according to demand
Diameter；Wherein the microsphere diameter size parameter is 0.5mm~1.5mm, and the extrusion molding path is designed to surround in same
Mandrel, and former and later two are formed by drop and are not on same position；
(iii) slurry formed according to step (i) is transferred in the size barrel of extrusion molding equipment, and uses step (ii) institute
The technological parameter of setting quickly squeezes out slurry using nozzle, is formed by drop and is fallen into dropwise to containing curing agent solution
In container molding, and spherical green body is formed to shrink via the collective effect of curing agent and surface tension；In the process, for
The droplet retracts are formed to the process of spherical green body, process parameters design is as follows: inlet pressure be 10psi~30psi,
Slurry pressure is 0.01psi~0.03psi, finds time as 0.03s~0.08s；The curing agent be boric acid or borax, it is molten
Liquid is glycerite, and hardener dose is the 5%~15% of glycerite quality；
(iv) collection step (iii) is formed by spherical green body, and is dried and required ceramics are made after calcination process
Microspheres product.
2. a kind of method that quick extrusion prepares ceramic microsphere as described in claim 1, which is characterized in that in step (i),
The mass percent of each component further sets as follows: ceramic powder 75%, binder 0.8%, dispersant 1.5%,
Antifoam content is 0.5%, remaining is deionized water.
3. a kind of method that quick extrusion prepares ceramic microsphere as claimed in claim 1 or 2, which is characterized in that in step
(iv) in, the condition of the drying process is as follows: drying temperature is 40 DEG C~60 DEG C, drying time is 1h~4h；The roasting
The condition of processing is as follows: maturing temperature is 600 DEG C~1500 DEG C, soaking time is 2h~6h.
4. a kind of method that quick extrusion prepares ceramic microsphere as claimed in claim 3, which is characterized in that made ceramics
The sphericity of microspheres product is 1.02, and partial size can change according to the diameter of the nozzle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710252125.7A CN107140953B (en) | 2017-04-18 | 2017-04-18 | A kind of method that quick extrusion prepares ceramic microsphere |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710252125.7A CN107140953B (en) | 2017-04-18 | 2017-04-18 | A kind of method that quick extrusion prepares ceramic microsphere |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107140953A CN107140953A (en) | 2017-09-08 |
| CN107140953B true CN107140953B (en) | 2019-11-22 |
Family
ID=59774602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710252125.7A Active CN107140953B (en) | 2017-04-18 | 2017-04-18 | A kind of method that quick extrusion prepares ceramic microsphere |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107140953B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109129820A (en) * | 2018-09-29 | 2019-01-04 | 南昌大学 | A kind of pneumatic printing prepares ceramic microsphere device and method |
| CN109454752B (en) * | 2018-10-31 | 2020-07-14 | 华中科技大学 | Method and device for preparing ceramic microspheres |
| CN110835263A (en) * | 2019-10-31 | 2020-02-25 | 中国船舶重工集团公司第七二五研究所 | Method for preparing zirconia ceramic microspheres |
| CN111302791A (en) * | 2020-02-24 | 2020-06-19 | 东莞市永笃纳米科技有限公司 | Zirconia micro-bead and preparation method thereof |
| CN112274696A (en) * | 2020-10-30 | 2021-01-29 | 陶合体科技(苏州)有限责任公司 | Bone filling material with long-acting antibacterial function and application and preparation method thereof |
| CN112295020B (en) * | 2020-10-30 | 2023-10-27 | 陶合体科技(苏州)有限责任公司 | Preparation method of calcium phosphate porous pellets coated with calcium sulfate salt on surface |
| CN114394836B (en) * | 2022-02-28 | 2022-09-23 | 南京航空航天大学 | Method for preparing nanocrystalline silicon carbide ceramic by SLS based on phase-transition microspheres |
| CN117735960A (en) * | 2023-12-21 | 2024-03-22 | 任红波 | Production device and production method for automatic titration of alumina grinding media |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04200735A (en) * | 1990-11-30 | 1992-07-21 | Shinagawa Refract Co Ltd | Production of ceramic sphere |
| JPH0891823A (en) * | 1994-09-28 | 1996-04-09 | Suzuki Yushi Kogyo Kk | Production of inorganic uniform fine sphere |
| KR970007550B1 (en) * | 1994-07-19 | 1997-05-10 | 한국기계연구원 | Producing method and equipment of a ceramic ball |
| JP2004284943A (en) * | 2003-03-04 | 2004-10-14 | Taimei Chemicals Co Ltd | Method of producing ceramic microsphere, ceramic microsphere, and alumina microsphere |
| CN1241876C (en) * | 2002-07-17 | 2006-02-15 | 圣戈班西普磨介(邯郸)有限公司 | Ceramic bead preparing process and apparatus |
| CN101342520A (en) * | 2007-07-10 | 2009-01-14 | 研能科技股份有限公司 | Fine liquid drop spray structure |
| CN101510450A (en) * | 2009-03-31 | 2009-08-19 | 北京科技大学 | Method for preparing ceramic tritium proliferation agent in fusion stack cladding |
| CN100551654C (en) * | 2006-10-16 | 2009-10-21 | 清华大学 | A kind of method of preparing ceramic microball by injection-condensation and device thereof |
| CN101857442A (en) * | 2010-05-28 | 2010-10-13 | 北京科技大学 | Preparation method of lithium-based ceramic microsphere |
| CN102731111A (en) * | 2012-07-05 | 2012-10-17 | 北京科技大学 | Novel preparation method of ceramic microspheres |
| CN104140259A (en) * | 2014-07-30 | 2014-11-12 | 华中科技大学 | Method for quickly manufacturing Li2TiO3 tritium breeding small balls |
| CN104387061A (en) * | 2014-11-06 | 2015-03-04 | 上海交通大学 | Method for preparing ceramic hollow microspheres by using peristaltic pump assisted coaxial micro-fluidic system |
| CN104446479A (en) * | 2014-11-06 | 2015-03-25 | 中国核动力研究设计院 | Method of preparing ceramic grade uranium dioxide ball |
| CN105330288A (en) * | 2015-09-29 | 2016-02-17 | 洛阳暖盈电子技术有限公司 | Preparation method of zirconia microspheres |
| CN105367054A (en) * | 2015-11-30 | 2016-03-02 | 东莞信柏结构陶瓷有限公司 | Preparation method for gel-casting system-based zirconium dioxide ball-milling medium |
| CN106431396A (en) * | 2016-08-31 | 2017-02-22 | 赣州科盈结构陶瓷有限公司 | Ceramic blank preparation method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE0101852D0 (en) * | 2001-05-23 | 2001-05-23 | Svenska Rymdaktiebolaget | Method of preparing granules |
| BRPI0513173A (en) * | 2004-07-09 | 2008-04-29 | Carbo Ceramics Inc | method for producing solid ceramic particles using a spray drying process |
-
2017
- 2017-04-18 CN CN201710252125.7A patent/CN107140953B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04200735A (en) * | 1990-11-30 | 1992-07-21 | Shinagawa Refract Co Ltd | Production of ceramic sphere |
| KR970007550B1 (en) * | 1994-07-19 | 1997-05-10 | 한국기계연구원 | Producing method and equipment of a ceramic ball |
| JPH0891823A (en) * | 1994-09-28 | 1996-04-09 | Suzuki Yushi Kogyo Kk | Production of inorganic uniform fine sphere |
| CN1241876C (en) * | 2002-07-17 | 2006-02-15 | 圣戈班西普磨介(邯郸)有限公司 | Ceramic bead preparing process and apparatus |
| JP2004284943A (en) * | 2003-03-04 | 2004-10-14 | Taimei Chemicals Co Ltd | Method of producing ceramic microsphere, ceramic microsphere, and alumina microsphere |
| CN100551654C (en) * | 2006-10-16 | 2009-10-21 | 清华大学 | A kind of method of preparing ceramic microball by injection-condensation and device thereof |
| CN101342520A (en) * | 2007-07-10 | 2009-01-14 | 研能科技股份有限公司 | Fine liquid drop spray structure |
| CN101510450A (en) * | 2009-03-31 | 2009-08-19 | 北京科技大学 | Method for preparing ceramic tritium proliferation agent in fusion stack cladding |
| CN101857442A (en) * | 2010-05-28 | 2010-10-13 | 北京科技大学 | Preparation method of lithium-based ceramic microsphere |
| CN102731111A (en) * | 2012-07-05 | 2012-10-17 | 北京科技大学 | Novel preparation method of ceramic microspheres |
| CN104140259A (en) * | 2014-07-30 | 2014-11-12 | 华中科技大学 | Method for quickly manufacturing Li2TiO3 tritium breeding small balls |
| CN104387061A (en) * | 2014-11-06 | 2015-03-04 | 上海交通大学 | Method for preparing ceramic hollow microspheres by using peristaltic pump assisted coaxial micro-fluidic system |
| CN104446479A (en) * | 2014-11-06 | 2015-03-25 | 中国核动力研究设计院 | Method of preparing ceramic grade uranium dioxide ball |
| CN105330288A (en) * | 2015-09-29 | 2016-02-17 | 洛阳暖盈电子技术有限公司 | Preparation method of zirconia microspheres |
| CN105367054A (en) * | 2015-11-30 | 2016-03-02 | 东莞信柏结构陶瓷有限公司 | Preparation method for gel-casting system-based zirconium dioxide ball-milling medium |
| CN106431396A (en) * | 2016-08-31 | 2017-02-22 | 赣州科盈结构陶瓷有限公司 | Ceramic blank preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107140953A (en) | 2017-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107140953B (en) | A kind of method that quick extrusion prepares ceramic microsphere | |
| CN106242507B (en) | Clay mud for directly-formed 3D ceramic printing and preparation method and application thereof | |
| CN107030853B (en) | A kind of desktop grade ceramic 3D printing forming method | |
| CN110229011A (en) | A kind of orientated short fiber reinforced metal or ceramic matric composite 3D printing method | |
| CN102898134B (en) | Method for preparing zirconium dioxide ceramic microspheres with microfluid device | |
| CN110835263A (en) | Method for preparing zirconia ceramic microspheres | |
| CN106927820A (en) | High-purity high-strength high-ductility zirconia composite ceramics structural member and preparation method thereof | |
| CN102731111A (en) | Novel preparation method of ceramic microspheres | |
| CN108751975A (en) | Preparation method of tritium-proliferated ceramic pellets in fusion reactor solid blanket | |
| CN107266077A (en) | A kind of ultra-fine zirconium carbide ceramics fiber and preparation method thereof | |
| CN108191409A (en) | It is a kind of for aqueous-based ceramic slurry of free extrusion molding and preparation method and application | |
| CN108558408A (en) | A kind of preparation method of integrated microchannels plate | |
| CN109454752A (en) | A kind of ceramic microsphere preparation method and its device | |
| CN108456456A (en) | The zirconium oxide colloid ink of 3D direct writes | |
| CN110668813A (en) | Preparation method of nano zirconia granulated powder | |
| CN103964874B (en) | Zirconium mullite sagger | |
| CN109020549A (en) | A kind of direct write type 3D printer SiC ink and its preparation method and application | |
| CN108858681A (en) | Mass prepares the equipment of bead biscuit and the preparation method of tritium multiplication agent nanostructure metatitanic acid lithium ceramic bead | |
| Zhao et al. | 3D printing of ZrO2 ceramic using nano-zirconia suspension as a binder | |
| CN106977199A (en) | High-purity ultra-toughness zirconia composite ceramics gear and preparation method thereof | |
| CN204772890U (en) | Forming device is spouted to declining of super microballon body of pottery | |
| CN105801012A (en) | Slurry | |
| CN104451222B (en) | A kind of preparation method of nanograined W-Cu composite block material | |
| CN206981747U (en) | A kind of powder metallurgy die with cooling system | |
| CN211429538U (en) | Heating wire |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |