CN108752013A - A kind of modified ceramic material and its modification method for preparing and ceramic slurry - Google Patents
A kind of modified ceramic material and its modification method for preparing and ceramic slurry Download PDFInfo
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- CN108752013A CN108752013A CN201810683794.4A CN201810683794A CN108752013A CN 108752013 A CN108752013 A CN 108752013A CN 201810683794 A CN201810683794 A CN 201810683794A CN 108752013 A CN108752013 A CN 108752013A
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62818—Refractory metal oxides
- C04B35/62823—Zirconium or hafnium oxide
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62807—Silica or silicates
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62813—Alumina or aluminates
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- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62828—Non-oxide ceramics
Abstract
The invention discloses a kind of modified ceramic material and its modification method for preparing and ceramic slurry, wherein modified ceramic material is made by the agitated reaction of the raw material including surface modifier and nano ceramic material；Wherein, nano ceramic material includes any one of nano zircite, nano aluminium oxide, nano silicon oxide and nm-class boron nitride；Surface modifier is selected from least one of phosphoric acid copolymer, silane coupling agent and C16~C20 olefin(e) acids.In the above manner, modified ceramic material scatter of the present invention is high, particle surface energy is big, and sintering temperature is relatively low, is conducive to reduce energy consumption, and after being sintered material mechanical property it is good.
Description
Technical field
The present invention relates to inorganic ceramic material process for modifying surface fields, and in particular to a kind of modified ceramic material and its changes
Property preparation method and ceramic slurry.
Background technology
Since there are ceramic material high temperature resistant, wearability and the high molecular materials such as resistant to chemical etching and metal material not to have
The advantages of, thus favor is received in Material Field, common ceramic material includes aluminium oxide, zirconium oxide, boron nitride etc..With electricity
The development of sub-industry, aeronautical and space technology, requirement of the researcher to material property is higher and higher, and ceramic slurry is to prepare high-performance
The key of ceramic component, the slurry of high dispersive low viscosity are the key that obtain high compactness ceramic part, are advantageously reduced simultaneously
Sintering energy consumption.
Moulding process traditional at present, such as tape casting, gel injection-moulding, can be molded most of simple structure ceramics zero
Part needs by mold labyrinth, and of high cost, the period is long, it is difficult to adapt to demand of the market to product.Increasing material manufacturing
It includes selectivity that technology has apparent advantage, the technology as novel manufacturing technology for processing labyrinth ceramic part
Laser sintered (Selective Laser Sintering, SLS), melt deposition modeling technology (Fused Deposition of
Ceramics, FDC) and layer separated growth technology (Laminated Object Manufacturing, LOM) etc., photocuring
Molding (Stereolithography, SLA) ceramic part has many advantages, such as that formed precision is high, simple for process.It is molded skill in SLA
In art, can the factors such as dispersibility, viscosity, uniformity and mobility of slurry determine curing molding and solidification quality.
Suitable surface modifier (dispersant) can substantially improve the dispersibility of ceramic material in the slurry, reduce slurry
Viscosity, to obtain good rheological property, be uniformly dispersed, the slurry that solid content is high and stable.Dispersant passes through three in suspension
Kind mechanism has an effect with ceramic surface and prevents to reunite mutually, is respectively：Electrostatic repulsion effect, steric hindrance effect and electrostatic
Steric hindrance.Currently, most researchers mainly study aqueous-based ceramic slurry system, therefore electrostatic repulsion effect and electrostatic steric hindrance
Two kinds of mechanism of effect are used in the dispersibility that ceramics are improved in water base zirconia slurry, but water-based slurry formed precision is not high.
In addition, existing most researchers mainly study submicron order ceramic particle, such particle surface energy is relatively low, in sintering process
Need higher energy, at the same after being sintered material mechanical property it is poor.
Invention content
In order to solve the above technical problem, the present invention provides a kind of modified ceramic material and its modification method for preparing and ceramics
Slurry, the modified ceramic material scatter is high, and particle surface energy is larger, and sintering temperature is relatively low, is conducive to reduce energy consumption, and be sintered
The mechanical property of material is good afterwards.
The technical solution adopted in the present invention is：A kind of modified ceramic material, by including that surface modifier and nanometer are made pottery
The agitated reaction of raw material of ceramic material is made；Wherein, the nano ceramic material includes nano zircite, nano aluminium oxide, receives
Rice any one of silica and nm-class boron nitride；It is even that the surface modifier is selected from phosphoric acid copolymer (such as BYK-111), silane
Join at least one of agent (such as KH560, KH570) and C16~C20 olefin(e) acids (such as oleic acid).
The present invention also provides a kind of modification method for preparing of modified ceramic material, include the following steps：Surface is modified
Agent is dissolved in organic solvent (such as ethyl alcohol alcohol solution), and nano ceramic material is then added, and stirs and modified Nano pottery is made
Ceramic material mixed liquor；Wherein, the surface modifier be selected from phosphoric acid copolymer (such as BYK-111), silane coupling agent (such as KH560,
At least one of KH570 etc.) and C16~C20 olefin(e) acids (such as oleic acid).In the above manner, used surface modifier point
Anchoring group (such as hydroxyl, carboxyl and phosphate group) is contained in subchain one end, and the other end is solvation segment (i.e. the one of lipophilic group
End), when anchoring group is adsorbed on nano ceramic material particle surface, since solvent of the lipophilic group in oil-based solvent is turned into
With so that the surfactant of one end adsorption particle can trail in oil-based solvent completely, form steric hindrance, to real
Now the oleophylicization of nano ceramic material particle surface is modified.
Preferably, the average grain diameter of the nano ceramic material is 40~60nm.
Preferably, the nano ceramic material is before addition by being dried, to remove in nano ceramic material
Moisture, to prevent agglomeration serious.
Preferably, the treatment temperature of the drying process be 80~100 DEG C, processing time be 12~for 24 hours.
Preferably, the stirring is carried out under 60~90 DEG C of temperature conditions.
Preferably, the modification method for preparing further includes：The modified Nano ceramic material mixed liquor is centrifuged, clearly
It washes, dry；Wherein, drying temperature is usually 110~130 DEG C, 0.5~2h of drying time, and dry under the conditions of preferably 120 DEG C
1h.Also, (such as 3 times, 4 times, 6 inferior) centrifugation, cleaning and dry can be specifically carried out repeatedly, is not modified by sorbent surface with removing
Agent prevents unabsorbed surface modifier from, since winding effect makes adjacent particle agglomeration together, causing in mixed liquor
Viscosity increases.
In addition, obtained by the above modified ceramic material or modification method for preparing by the above modified Nano ceramic material
Modified ceramic material can be applied to prepare in ceramic slurry, thus, the present invention also provides a kind of ceramic slurry, the ceramic slurry
Material includes modified ceramic material made from the modification method for preparing of the above modified ceramic material or the above modified ceramic material.
Preferably, the ceramic slurry further includes non-water solvents, and the modified ceramic slurry is scattered in non-water solvents
In, the non-water solvents is selected from least one of monofunctional monomer and polyfunctional monomer.
Preferably, the monofunctional monomer is selected from least one of isobornyl acrylate, acryloyl morpholine；It is described more
Functional monomer is selected from polyethyleneglycol diacrylate, ethoxyquin-trimethylolpropane trimethacrylate and ethoxyquin pentaerythrite
At least one of tetraacrylate.
The method have the benefit that：A kind of modified ceramic material of present invention offer and its modification method for preparing and pottery
Porcelain slurry, wherein modified ceramic material are made by the agitated reaction of the raw material including surface modifier and nano ceramic material,
Using nano ceramic material as core, the anchoring group of surface modifier and the hydroxyl on nano ceramic material surface pass through chemical bond jail
Consolidation is closed, and so that nano ceramic material particle surface is adsorbed a large amount of surface modifier and is formed steric hindrance repulsion, between particle not
Easily reunite, to form the modified Nano ceramic material of high dispersive.In addition, modified Nano ceramic particle is small, have larger
Surface energy, sintering temperature is relatively low, advantageously reduces energy consumption, reaches energy-efficient purpose, and after being sintered material mechanical property compared with
It is good.
Description of the drawings
It is required in being described below to embodiment to make for the clearer technical solution illustrated in the embodiment of the present invention
Attached drawing briefly describes.
Fig. 1 is the Hydrolytic Mechanism figure of the surface modifier silane coupling agent KH560 employed in the embodiment of the present invention 3；
Fig. 2 is that the viscosity of different zirconia ceramics slurries in rheological experiment in the embodiment of the present invention 4 adds with surface modifier
The change curve of dosage.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
Before modified, by original nano zirconium oxide powder, 100 DEG C of dryings are for 24 hours in vacuum drying chamber first.It is measured with graduated cylinder
100mL absolute ethyl alcohols are added in 7 150mL beakers (number 1,2,3,4,5,6 and 7), are weighed respectively with electronic balance
0.05g, 0.25g, 0.5g, 1g, 1.5g, 2.5g, 4g surface modifier BYK-111 are added dropwise in above-mentioned 7 beakers, room temperature
Lower magnetic agitation 1h is gradually separately added into 60 DEG C of nano zirconium oxide powder after 50g is dried into beaker later to being completely dissolved
Magnetic agitation 4h makes surface modifier BYK-111 fully absorb nano zirconium oxide powder particle surface.Modified mixed liquor
It is added in 50mL centrifuge tubes, 8000rpm centrifuges 10min, outwells supernatant, later by modified 120 DEG C of drying 1h of powder, allows
Powder is changed into chemical absorbing with surface modifier from Physical Absorption.Powder is distributed to 100mL absolute ethyl alcohols again after drying
In solution, ultrasonic disperse 1h, again centrifugal drying repeat the above process 3 times and remove no absorbed surface modifier BYK-
111, finally for 24 hours by the 90 DEG C of dryings of powder being modified, it is sieved for use with 80 mesh screens after mechanical lapping.
Embodiment 2
Before modified, by original nano zirconium oxide powder, 100 DEG C of dryings are for 24 hours in vacuum drying chamber first.It is measured with graduated cylinder
100mL absolute ethyl alcohols are added in 7 150mL beakers (number 1,2,3,4,5,6 and 7), are weighed respectively with electronic balance
0.05g, 0.25g, 0.5g, 1g, 1.5g, 2.5g, 4g surface modifier oleic acid (OA) are added dropwise in above-mentioned 7 beakers, often
The lower magnetic agitation 1h of temperature is gradually separately added into the nano zirconium oxide powder 60 after 50g is dried into beaker later to being completely dissolved
DEG C magnetic agitation 4h makes surface modifier OA fully absorb nano zirconium oxide powder particle surface.Modified mixed liquor is added
Into 50mL centrifuge tubes, 8000rpm centrifuges 10min, outwells supernatant, later by 120 DEG C of drying 1h of modified powder, allows powder
It is changed into chemical absorbing from Physical Absorption with surface modifier.Powder is distributed to 100mL ethanol solutions again after drying
In, ultrasonic disperse 1h, again centrifugal drying repeat the above process 3 times and remove no absorbed surface modifier OA, finally will
90 DEG C of dryings of the powder being modified for 24 hours, are sieved for use after mechanical lapping with 80 mesh screens.
Embodiment 3
Before modification, by original nano zirconium oxide powder, 100 DEG C of dryings are for 24 hours in vacuum drying chamber first.Also, surface
Modifying agent silane coupling agent KH560 is hydrolyzed, and Fig. 1 show silane coupling agent KH560 Hydrolytic Mechanism figures.It is measured respectively with graduated cylinder
It takes 95mL absolute ethyl alcohols and 5mL deionized waters to be configured to hydrolyzate, adjusts hydrolyzate pH value to 4~5 with glacial acetic acid, be added to 7
In a 150mL beakers (number 1,2,3,4,5,6 and 7), weighed respectively with electronic balance 0.05g, 0.25g, 0.5g, 1g, 1.5g,
2.5g, 4g surface modifier KH560 are added dropwise in above-mentioned 7 beakers, and magnetic agitation 4h is to complete hydrolysis under room temperature, later
60 DEG C of magnetic agitation 12h of 50g nano zirconium oxide powders are gradually separately added into beaker makes surface modifier KH560 fully absorb
To nano zirconium oxide powder particle surface.Modified mixed liquor is added in 50mL centrifuge tubes, and 8000rpm centrifuges 10min,
Fall supernatant, later by modified 120 DEG C of drying 1h of powder, powder is allowed to be changed into chemical suction from Physical Absorption with surface modifier
It receives.Powder is distributed in 100mL ethanol solutions again after drying, ultrasonic disperse 1h, centrifugal drying repeats above-mentioned again
3 no absorbed silane coupling agent KH560 of removing of process finally for 24 hours by the 90 DEG C of dryings of powder being modified are sieved with 80 mesh
Net sieving is for use.
Embodiment 4
The modified effect of processing, inventor couple are modified to assess above example 1-3 to nano zirconium oxide powder
The modified Nano zirconium oxide (as experimental group) of the modified gained of above example 1-3 and non-modified processing it is nano oxidized
Zirconium powder body (as a control group) has carried out rheological experiment.It is specific as follows：
Non-water solvents is configured first.Specifically, 32mLACMO (acryloyl morpholine) is measured respectively and 48mLPEGDA is (poly-
Glycol diacrylate) uniformly mixing, it is made into 80mL non-water solvents；And 22 parts are configured by the above process.
Gained after using different content and different surfaces modifying agent to be modified processing in above example 1-3 is weighed respectively
Modified Nano zirconium oxide (density 6g/cm3) 36g and non-modified processing nano zirconium oxide powder (density 6g/
cm3) 36g, it is distributed to respectively in 80mL or more non-water solvents, it is 7vol% zirconia ceramics slurries to form volume fraction, altogether
22 samples.The viscosity number and record of 22 samples of rotary viscosity measuring are then used, test condition is room temperature, rotating speed 50rmp.
The nano zirconium oxide powder of non-modified processing is scattered in the zirconium oxide formed in non-water base mixed solution in control group after testing
Ceramic slurry viscosity is 189mPa.s；The viscosity of zirconia ceramics slurry exists with corresponding modified Nano zirconium oxide in experimental group
Relation curve in modified preparation process between surface modifier dosage is specifically as shown in Figure 2.Wherein, curve A indicates embodiment 1
It is modified each modified Nano Zirconium powder of gained using surface modifier BYK-111, is scattered in shape in non-water solvents
At zirconia ceramics slurry；Curve B indicates that embodiment 2 is modified gained using surface modifier silane coupling agent KH560
Modified Nano Zirconium powder, be scattered in the zirconia ceramics slurry formed in non-water solvents；Curve C indicates embodiment 3
It is modified the modified Nano Zirconium powder of gained using surface modifier oleic acid, is scattered in the oxygen formed in non-water solvents
Change zircon ceramic slurry.
As shown in Figure 2, three kinds of surface modifiers used by embodiment 1-3 are glued to reducing nanometer zirconium oxide ceramic slurry
Degree improves dispersibility with good effect；Also, with the increase of surface modifier additive amount, the viscosity of ceramic slurry by
Gradually tend towards stability.In addition, compared with the nano zirconium oxide powder of the non-modified processing of control group, the present invention implements 1-3 and uses table
After face modifying agent is modified processing to nano zirconium oxide powder, the modified Nano zirconium oxide of gained is dispersed in non-water base mixed liquor
The zirconia ceramics slurry viscosity of middle formation is substantially reduced, and dispersibility significantly improves.Wherein, non-water solvents can also be used individually
Monofunctional monomer (such as isobornyl acrylate) or esters of acrylic acid polyfunctional monomer (such as ethoxyquin-trimethylolpropane tris third
Olefin(e) acid ester and ethoxyquin pentaerythritol tetraacrylate etc.).
Processing is modified to nano zirconium oxide powder using surface modifier in above example 1-3, with nano oxygen
Change zirconium powder body is that core, the anchoring group of surface modifier and the hydroxyl on nano zircite surface are strong bonded by chemical bond,
Make a large amount of surface modifier of nano zircite particle adsorption and form steric hindrance repulsion, is not easy to reunite between particle, from
And form the modified Nano zirconium oxide of high dispersive；In addition, modified Nano zirconia particles have larger surface energy, sintering temperature
It is relatively low, advantageously reduce energy consumption, reach energy-efficient purpose, and after being sintered material mechanical property it is preferable.Due to such as nano oxidized
The surface of the nano ceramic materials such as aluminium, nano silicon oxide and nm-class boron nitride also has a large amount of hydroxyl, has hydrophilic well
Property, therefore deducibility：Similarly, the above surface modifier can also be used to nano aluminium oxide, nano silicon oxide and nm-class boron nitride
Equal nano ceramic materials are modified processing, form modified ceramic material, and be similarly formed by modified Nano ceramic material
Particle is small, has larger surface energy, and sintering temperature is relatively low, advantageously reduces energy consumption, reaches energy-efficient purpose, and material after sintering
The mechanical property of material is preferable.
Although specifically showing and describing the present invention in conjunction with preferred embodiment, those skilled in the art should be bright
In vain, it is not departing from the spirit and scope of the present invention defined by described claims, it in the form and details can be right
The present invention makes a variety of changes, and is protection scope of the present invention.
Claims (10)
1. a kind of modified ceramic material, which is characterized in that the modified ceramic material is by including surface modifier and nano ceramics
The agitated reaction of raw material of material is made；Wherein, the nano ceramic material includes nano zircite, nano aluminium oxide, nanometer
Any one of silica and nm-class boron nitride；The surface modifier be selected from phosphoric acid copolymer, silane coupling agent and C16~
At least one of C20 olefin(e) acids.
2. a kind of modification method for preparing of modified ceramic material, which is characterized in that include the following steps：
Surface modifier is dissolved in organic solvent, nano ceramic material is then added, is stirred, modified Nano ceramics material is made
Expect mixed liquor；Wherein, the nano ceramic material includes any in nano zircite, nano aluminium oxide and nano silicon oxide
Kind；The surface modifier is selected from least one of phosphoric acid copolymer, silane coupling agent and C16~C20 olefin(e) acids.
3. the modification method for preparing of modified ceramic material according to claim 2, which is characterized in that the surface is modified
Agent：The mass ratio of the nano ceramic material is 0.1wt%~10wt%.
4. the modification method for preparing of modified ceramic material according to claim 2, which is characterized in that the nano ceramics material
Material is before addition by being dried.
5. the modification method for preparing of modified ceramic material according to claim 4, which is characterized in that the drying process
Treatment temperature be 80~100 DEG C, processing time be 12~for 24 hours.
6. the modification method for preparing of modified ceramic material according to claim 2, which is characterized in that the stirring is 60
It is carried out under~90 DEG C of temperature conditions.
7. the modification method for preparing of the modified ceramic material according to any one of claim 2-6, which is characterized in that also wrap
It includes：The modified Nano ceramic material mixed liquor is centrifuged, cleaned, is dried.
8. a kind of ceramic slurry, which is characterized in that the ceramic slurry includes modified ceramic material described in claim 1, or
Ceramic slurry described in person includes modified ceramic material made from the modification method for preparing of modified ceramic material described in claim 2-7
Material.
9. ceramic slurry according to claim 8, which is characterized in that the ceramic slurry further includes non-water solvents, institute
It states modified ceramic slurry to be scattered in non-water solvents, the non-water solvents is in monofunctional monomer and polyfunctional monomer
It is at least one.
10. ceramic slurry according to claim 9, which is characterized in that the monofunctional monomer is selected from isobomyl acrylate
At least one of ester, acryloyl morpholine；The polyfunctional monomer is selected from polyethyleneglycol diacrylate ,-three hydroxyl first of ethoxyquin
At least one of base propane triacrylate and ethoxyquin pentaerythritol tetraacrylate.
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| CN111170747A (en) * | 2020-02-12 | 2020-05-19 | 深圳市光韵达增材制造研究院 | Ceramic powder and modification method thereof |
| CN112358761A (en) * | 2020-10-20 | 2021-02-12 | 广东环境保护工程职业学院 | Modified nano ceramic slurry, water-based paint, and preparation method and application thereof |
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