CN105236941B - A kind of aluminum oxide anti-electrostatic ceramic material and preparation method thereof - Google Patents
A kind of aluminum oxide anti-electrostatic ceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of ceramic material and preparation method, the ceramic material has the electrostatic dissipation characteristic of electrostatic charge safe-discharge.A kind of aluminum oxide anti-electrostatic ceramic material, the ceramic material include following constituent：Aluminum oxide, the conductive phase of nanometer second and 3Y zirconium oxides, for the present invention as a result of above-mentioned technical scheme, obtained anti-electrostatic ceramic material has the characteristics of excellent antistatic performance, wear-resisting, corrosion-resistant, high tenacity, high compactness；Meanwhile the present invention also provides the preparation method of the cheap aluminum oxide anti-electrostatic ceramic material of a kind of preparation technology simple, not aging, cost.
Description
Technical field
The present invention relates to a kind of ceramic material and preparation method, the ceramic material has the electrostatic of electrostatic charge safe-discharge
Dissipation characteristic.
Background technology
Electrostatic, it is a kind of electric charge to remain static.It is formed when accumulation is on some object or surface
Electrostatic, and electric charge is divided into two kinds of positive charge and negative electrical charge, that is to say, that electrostatic phenomenon is also classified into two kinds of i.e. positive electrostatic and negative electrostatic.
Positive electrostatic is formed when positive charge is gathered on some object, is formed bearing when negative electrical charge is gathered on some object
Electrostatic, but either positive electrostatic still bears electrostatic, when static electrification object contacts zero potential object（It is grounded object）Or there is electricity with it
Electric charge transfer can all occur during the object of potential difference, being exactly that we are daily sees spark static discharge phenomenon.
In the current growing electronics industry epoch, various microelectronics, the application of photoelectron original paper are very extensive, and quiet
Discharge of electricity can destroy electronic original part, the electrical property for changing semiconductor components and devices, destroy electronic system, cause whole equipment failure
Or failure；At the same time, electrostatic spark is produced when electrostatic charge discharges, equipment of Flammable and Explosive Materials of easily igniting, causes considerable risk
And economic loss；In addition, electrostatic easily sucks foul into clean environment, such as dust, foreign particles, easily make can not be mutual
The product of contact sticks together, and these can all cause great loss.Electrostatic is as a kind of universal physical phenomenon, closely during the last ten years
Along with the rapid development of integrated circuit and the extensive use of high polymer material, active force, electric discharge and the induction of electrostatic are drawn
The harm risen is extremely serious, U.S.'s statistics, American Electronic industry department every year because electrostatic hazard cause damage it is up to 10,000,000,000 beautiful
Member, the loss caused by electrostatic is 2,000,000,000 pounds to Britain's electronic product every year, many in the defective work of JEOL's component
Harm in 45% is because caused by static discharge (ESD).
Because electrostatic hazard is very huge, therefore cause the great attention of people.Prepare at present many anti-quiet
The material of electricity, the apparatus for designing many electrostatic discharge dissipatives, for preventing the generation of static discharge phenomenon.It is quiet for preventing
The static dissipative material of electricity should be semi-insulated, and its volume resistance range is 104To 1011Ω-cm, when such a material by
During friction, electrostatic charge caused by its surface can spread and leak faster.Particularly, when the specific insulation of material is 106
To 108Ω-cm, the electrostatic of material surface can at utmost prevent static discharge with more slow speed slowly sustained release
Destruction to product.Antistatic material most widely used at present, is mostly by adding the conductions such as carbon black, metal powder in the plastic
Powder is made, and being evenly distributed on plastics inner using conductive powder body forms conductive network, reduces the resistivity of plastics in itself, so as to
Reach the purpose of electrostatic dissipation.It is reason and ceramic material has the advantages that good wearability, corrosion-resistant, high temperature resistant, rigidity are good
The antistatic material thought.Being presently used for the special cermacis of structural member mainly has aluminium oxide ceramics, zirconia ceramics, silicon nitride pottery
Porcelain, silicon carbide ceramics etc..Wherein, aluminium oxide ceramics has cheap, easy preparation, excellent mechanical property and high abrasion
Property, will not the special benefits such as low temperature aging, therefore can be as excellent anti-electrostatic ceramic material matrix.It is most at present anti-
Electrostatic ceramic material, using zirconia ceramics as matrix material, as patent CN200480013963.X provide it is a kind of shallow
Color static discharge ceramics, by adding resistance adjustment agent in zirconia ceramics matrix, and with hip treatment sintered body
Method, the static discharge ceramics of densification are obtained；Patent CN201010101876.7 provides a kind of ZrO2-ZnO-SnO systems
Anti-static ceramic, and introduce SiO2, SiC, Si powder etc. reduce sintering temperature, improve compactness.Patent
CN200710071983.8 proposes to mix TiC conductive phases in ZrO2, and by vacuum-sintering, obtains the anti-quiet of resistivity satisfaction
Electric material.
The antistatic material defect of plastics is apparent：1st, material itself is easy to aging, wearability, corrosion resistance, poor rigidity,
It is easily deformed；2nd, the carbon black that is added in plastics, metal powder etc. easily come off after friction, produce conductive dust, polluted product and ring
Border, electronic component short circuit is caused to be scrapped when serious.
The anti-electrostatic ceramic material preparation method disclosed at present, mostly it is by adding second in zirconia ceramics matrix
The method of phase, i.e. conductive phase, the resistivity of ceramic material is set to be reduced to 104To 1011Ω-cm, so as to reach the mesh of electrostatic dissipation
's.But the defects of current technology is present is also apparent：Such as patent CN200480013963.X, it is necessary to the side for passing through high temperature insostatic pressing (HIP)
Formula obtains that compactness is good, and the qualified anti-static ceramic sintered body of resistivity, cost is very high, is not suitable for large-scale industry metaplasia
Production；Patent CN201010101876.7 is sintered using conventional air atmosphere, but in order to improve the compactness of material, is introduced
The glass phases such as SiO2, the fragility of ceramics is considerably increased, reduces the mechanical properties such as intensity, hardness, toughness；Patent
CN200710071983.8 introduces TiC conductive materials in zirconia ceramics matrix, because TiC is easily aoxidized in atmosphere, because
This must be sintered in vacuum atmosphere, and this not only adds cost, is unfavorable for large-scale production.Also, zirconia ceramics is deposited
It is with high costs although this defect can be made up by various technological means in the inherent shortcoming of low temperature aging, and simultaneously
Can not perfectly solve problem of aging.
Because current anti-electrostatic ceramic material is using the side that the conductive phase of micron order second is introduced in ceramic matrix
Prepared by method, the second phase content that formation conductive network needs is more, and the second phase has part volatilization under high temperature, it is therefore desirable to
More conductive phase is added in ceramic matrix raw material（In general ratio is 20% --- 50% mass fraction）It can be only achieved required
The specific insulation wanted, because second meets a large amount of liquid phases are formed in ceramic post sintering, a large amount of glass are formed after the cooling of these liquid phases
Glass phase, the mechanical property of glass phase itself is very poor, and this greatly reduces the performance of ceramic body in itself.
The content of the invention
The present invention is exactly to solve above technical problem and propose, it is therefore an objective to it is excellent, resistance to provide a kind of antistatic performance
Mill, corrosion-resistant, high tenacity, the anti-electrostatic ceramic material of high compactness；Meanwhile also provide a kind of preparation technology simple, not aging,
The preparation method of the cheap aluminum oxide anti-electrostatic ceramic material of cost.
In order to realize first above-mentioned purpose, present invention employs following technical scheme：
A kind of aluminum oxide anti-electrostatic ceramic material, the ceramic material include following constituent by mass percentage：
Aluminum oxide 70t%-90wt%；
The second conductive phase 10wt%-20wt% of nanometer；
3Y- zirconium oxides 5%-12%.
Preferably, the ceramic material includes following constituent by mass percentage：
Aluminum oxide 70t%-85wt%；
The second conductive phase 10wt%-20wt% of nanometer；
3Y- zirconium oxides 5%-10%.
Preferably, aluminum oxide uses the oxide of high activity aluminium powder of granularity prepared by coprecipitation for 100nm -500nm.
The sintering temperature of this alumina powder is low, easily densification, and obtained sintered body crystal grain is tiny, uniform, and mechanical property is good.But
It is that aluminium oxide ceramics is used alone to have too high resistivity（10 under normal temperature12More than）, thus material surface electrostatic can not be reduced
Accumulation, can not slowly safe electric discharge.Therefore it is this kind of, it is necessary to add conducting or semiconducting material in alumina substrate
After material sintering, the conductive network of contact or half contact is formed in aluminium oxide ceramics matrix, so that the resistance of whole material
Rate drops to 106-108Ω-m。
The anti-electrostatic ceramic material matrix of the present invention uses the aluminium oxide ceramics of toughness reinforcing.Because adopted relative to most of inventions
Zirconia ceramics matrix, not only hardness is higher for aluminium oxide ceramics, more resistant to abrasion, and is not in low temperature aging defect.
It is well known that low temperature aging defect, the application field and reliability and stability of zirconia ceramics are greatly reduced.But and oxidation
Zircon ceramic is compared, and the toughness and bending strength of aluminium oxide ceramics are poor, it is therefore desirable to carries out toughness reinforcing to it using zirconium oxide.Part
For stable zirconium oxide when receiving external force effect, the t of part metastable phase, which meets, occurs the transformation for arriving m phases：Tetragonal（T phases）→
Monoclinic phase（M phases）Belong to martensitic traoformation, 3%-5% volumetric expansion will be produced.When Crack Extension enters the area containing t-ZrO2
During domain, in the presence of crack tip stress field, in crack tip forming process area, t → m phases occur for the t-ZrO2 in process area
Transformation, absorb energy in addition to producing the new plane of disruption and absorbing energy, the Volumetric expansion also when phase transformation.Simultaneously because
The volumetric expansion of t → m Phase-change particles in process area and compression is generated to crackle, hinder Crack Extension.So as to improve
The intensity and toughness of alumina matrix material.
Because the aluminum oxide anti-electrostatic ceramic material of preparation is using the cheap air atmosphere sintering processing of cost, therefore, one
A little conducting or semiconducting carbide（Such as SiC, TiC, B4C, ZrC, TaC）, nitride（Such as TiN, ZrN, TaN, AlN）、
Boride（Such as TiB2, ZrB2, LaB6）Although can also play a part of reducing matrix material resistivity, this kind of material is in sky
When gas atmosphere high temperature sinters, meeting oxidation Decomposition forms volatilization gas, and this, which is not only resulted in, produces hole inside ceramic sintered bodies,
And final sintered body bulk resistor is easily set to rise to 1011More than, do not reach the requirement of antistatic material.
In view of cost and factor, the second conductive phase of landing low-resistivity effect, the described conductive phase of nanometer second is adopted
Mixed with the one or more in single oxide or the oxide of doping；Preferably, described single oxide uses
CuO、Cu2O、V2O5、NiO、MnO、MnO2、CoO、Co2O3、Co3O4、Fe2O3、FeO、Fe3O4And Cr2O3In one or more mix
Close；The oxide of described doping uses ZnO, SnO2、TiO2With the one or more mixing in ITO.Most preferred nanometer second
Conductive phase uses CoO, Fe2O3Or TiO2.This kind of material is readily available, and the property with conductor or semiconductor, is added to oxidation
After in zirconium base body, the resistivity of zirconia material in itself can be significantly reduced.Meanwhile the invention is conductive by more than
Material is introduced into ceramic matrix in the form of nano-powder, and because the specific surface area of nano-powder is huge, granularity is tiny, by nanometer
After the conductive phase of level is evenly spread in matrix material, relative to the micron-sized powder of other invention use, it is easier to which formation connects
The conductive network for touching or partly contacting.In this case, the specific insulation of material is reached the standard of antistatic material, add
The amount of the second conductive phase can be greatly reduced.Simultaneously as the second conductive phase of addition is nano-scale particle, it is therefore desirable to
Firing temperature also than relatively low, which reduces the volatilization under conductive phase material high temperature, remain conductive phase thing to greatest extent
Matter.
In order to realize second above-mentioned purpose, present invention employs following technical scheme：
A kind of method for preparing a kind of described aluminum oxide anti-electrostatic ceramic material, this method comprise the following steps：
Step 1：By AlCl3Solution, ZrOCl2Solution, Y（NO3）3Solution is mixed after weighing, stirred by formula
It is set uniformly to mix；
Step 2：Ammoniacal liquor is slowly added dropwise into well mixed solution with peristaltic pump, while solution is slowly stirred,
Until solution pH value is 9-10, mixed precipitation is generated；Precipitation is rinsed repeatedly with water, until Cl is not present in colloidal sol-Untill；Then
With centrifugal dehydrator, unnecessary water is removed, has obtained the mixed gel of aluminium hydroxide, zirconium hydroxide, yttrium hydroxide；
Step 3：Obtained mixed gel and the second conductive phase of load weighted nanometer material are added into suitable quantity of water, are added to
Ball milling mixing is carried out in planetary ball mill；
Step 4：The slurry filtration that ball milling is obtained is come out, and being pumped into spray tower with wriggling is spray-dried；
Step 5：Pre-burning is carried out to the powder being spray-dried, makes aluminium hydroxide dehydration, is finally changed into Alpha's oxidation
Aluminium, and complete stabilization of the yittrium oxide to zirconium oxide；
Step 6：Shape and chi by pre- burned toughened zirconium oxide anti-static ceramic powder sieving aftershaping for needs
It is very little；
Step 7：The green compact of forming are put into air furnace and are sintered, low-temperature zone needs slowly heating during sintering, burns
Junction temperature scope is 1500 DEG C -1600 DEG C；
Step 8：The aluminum oxide anti-static ceramic sintered is machined as needed, polished, obtain size,
The qualified anti-static ceramic finished product of shape, surface quality.
Preferably, described AlCl3Solution, ZrOCl2Solution, Y（NO3）3The concentration of solution is 0.4mol/L-
0.6mol/L。
Preferably, the quality of described water is 0.3-0.5 times of mixed gel and nanometer the second conductive phase material mass；
Rotational speed of ball-mill is set as 300-500r/ points, 5-10 hours ball milling mixing time.
It is spray-dried preferably, being pumped into spray tower using wriggling；Inlet temperature is set as 200-250 DEG C, is gone out
Material mouth temperature is 90-130 DEG C, atomizer rotating speed 15-30Hz, wriggling revolution speed 10-25Hz.
Preferably, calcined temperature is 1000-1200 DEG C, soaking time 1-4 hours, heating rate is 2-8 DEG C.
Preferably, it was in the past 0.5-2 DEG C/minute that heating rate, which is 750 degrees Celsius,；4-5 DEG C/minute after 750 DEG C, until rising
To maximum sintering temperature；Maximum sintering temperature may range from 1500 DEG C -1600 DEG C, be incubated 2-4 hours.
For the present invention as a result of above-mentioned technical scheme, obtained anti-electrostatic ceramic material has antistatic performance excellent
The characteristics of good, wear-resisting, corrosion-resistant, high tenacity, high compactness；Meanwhile also to provide a kind of preparation technology simple, not old by the present invention
Change, the preparation method for the aluminum oxide anti-electrostatic ceramic material that cost is cheap.
Embodiment
Embodiment 1
A kind of antistatic aluminium oxide ceramics includes the component of following mass fraction：
Step 1：By 0.4mol/L AlCl3Solution, ZrOCl2Solution, Y（NO3）3Solution is changed by the mass ratio in table
Calculate and mixed for mol ratio and weighing, stirred 1 hour with 300r/ points of rotating speeds, it is uniformly mixed.
Step 2：Ammoniacal liquor is slowly added dropwise into well mixed solution with peristaltic pump, while solution is slowly stirred,
Mixing speed is 30r/ points, until solution pH value is 9, generates mixed precipitation.Precipitation is rinsed repeatedly with water, until molten with AgNO3
Liquid is examined in colloidal sol in the absence of untill Cl-.Then centrifugal dehydrator is used, with 4000r/ points of rotating speed, unnecessary water is removed, obtains
Aluminium hydroxide, zirconium hydroxide, the mixed gel of yttrium hydroxide.
Step 3：Obtained mixed gel and nano-sized iron oxide are added in planetary ball mill and carry out ball milling mixing, is added
Suitable quantity of water, the quality of water are（Mixed gel+conductive phase）0.3 times of gross mass.Rotational speed of ball-mill is set as 300r/ points, and ball milling mixes
Close 5 hours time.
Step 4：The slurry filtration that ball milling obtains is come out, and being pumped into spray tower with wriggling is spray-dried.Set charging aperture
Temperature is 200 DEG C, and discharging opening temperature is 90 DEG C, atomizer rotating speed 15Hz, wriggling revolution speed 10Hz.
Step 5：Pre-burning is carried out to the powder being spray-dried, makes aluminium hydroxide dehydration, is finally changed into Alpha's oxidation
Aluminium, and complete stabilization of the yittrium oxide to zirconium oxide.Calcined temperature be 1200 DEG C, soaking time 2 hours, heating rate be 2 DEG C/
Point.
Step 6：Dry pressing die set will be put into after pre- burned aluminum oxide anti-static ceramic powder sieving, be pressed into needs
Shape and size.
Step 7：The green compact of forming are put into air furnace and are sintered.Heating rate is 2 before being 700 degrees Celsius
DEG C/minute；5 DEG C/minute after 700 DEG C, until being raised to maximum sintering temperature.1600 DEG C of maximum sintering temperature, and it is incubated 4 hours.
Step 8：The aluminum oxide anti-static ceramic for sintering toughness reinforcing is machined as needed, polished, obtains chi
The qualified anti-static ceramic finished product of very little, shape, surface quality.
Embodiment 2
A kind of antistatic aluminium oxide ceramics includes the component of following mass fraction：
Step 1：By 0.5mol/L AlCl3Solution, ZrOCl2Solution, Y（NO3）3Solution is changed by the mass ratio in table
Calculate and mixed for mol ratio and weighing, stirred 2 hours with 400r/ points of rotating speeds, it is uniformly mixed.
Step 2：Ammoniacal liquor is slowly added dropwise into well mixed solution with peristaltic pump, while solution is slowly stirred,
Mixing speed is 20r/ points, until solution pH value is 10, generates mixed precipitation.Precipitation is rinsed repeatedly with water, until molten with AgNO3
Liquid is examined in colloidal sol in the absence of untill Cl-.Then centrifugal dehydrator is used, with 3000r/ points of rotating speed, unnecessary water is removed, obtains
Aluminium hydroxide, zirconium hydroxide, the mixed gel of yttrium hydroxide.
Step 3：Obtained mixed gel and nano-sized iron oxide are added in planetary ball mill and carry out ball milling mixing, is added
Suitable quantity of water, the quality of water are（Mixed gel+conductive phase）0.4 times of gross mass.Rotational speed of ball-mill is set as 400r/ points, and ball milling mixes
Close 8 hours time.
Step 4：The slurry filtration that ball milling obtains is come out, and being pumped into spray tower with wriggling is spray-dried.Set charging aperture
Temperature is 220 DEG C, and discharging opening temperature is 110 DEG C, atomizer rotating speed 20Hz, wriggling revolution speed 20Hz.
Step 5：Pre-burning is carried out to the powder being spray-dried, makes aluminium hydroxide dehydration, is finally changed into Alpha's oxidation
Aluminium, and complete stabilization of the yittrium oxide to zirconium oxide.Calcined temperature be 1100 DEG C, soaking time 3 hours, heating rate be 3 DEG C/
Point.
Step 6：Isostatic tooling, isostatic pressing will be put into after pre- burned aluminum oxide anti-static ceramic powder sieving
For the shape and size of needs.
Step 7：The green compact of forming are put into air furnace and are sintered.Heating rate is 700 degrees Celsius
0.5 DEG C/minute；4 DEG C/minute after 700 DEG C, until being raised to maximum sintering temperature.1550 DEG C of maximum sintering temperature, and it is incubated 3 hours.
Step 8：The aluminum oxide anti-static ceramic for sintering toughness reinforcing is machined as needed, polished, obtains chi
The qualified anti-static ceramic finished product of very little, shape, surface quality.
Embodiment 3
A kind of antistatic aluminium oxide ceramics includes the component of following mass fraction：
Step 1：By 0.5mol/L AlCl3Solution, ZrOCl2Solution, Y（NO3）3Solution is changed by the mass ratio in table
Calculate and mixed for mol ratio and weighing, stirred 3 hours with 500r/ points of rotating speeds, it is uniformly mixed.
Step 2：Ammoniacal liquor is slowly added dropwise into well mixed solution with peristaltic pump, while solution is slowly stirred,
Mixing speed is 40r/ points, until solution pH value is 10, generates mixed precipitation.Precipitation is rinsed repeatedly with water, until molten with AgNO3
Liquid is examined in colloidal sol in the absence of untill Cl-.Then centrifugal dehydrator is used, with 3500r/ points of rotating speed, unnecessary water is removed, obtains
Aluminium hydroxide, zirconium hydroxide, the mixed gel of yttrium hydroxide.
Step 3：Obtained mixed gel and nano-sized iron oxide are added in planetary ball mill and carry out ball milling mixing, is added
Suitable quantity of water, the quality of water are（Mixed gel+conductive phase）0.5 times of gross mass.Rotational speed of ball-mill is set as 500r/ points, and ball milling mixes
Close 10 hours time.
Step 4：The slurry filtration that ball milling obtains is come out, and being pumped into spray tower with wriggling is spray-dried.Set charging aperture
Temperature is 250 DEG C, and discharging opening temperature is 130 DEG C, atomizer rotating speed 30Hz, wriggling revolution speed 25Hz.
Step 5：Pre-burning is carried out to the powder being spray-dried, makes aluminium hydroxide dehydration, is finally changed into Alpha's oxidation
Aluminium, and complete stabilization of the yittrium oxide to zirconium oxide.Calcined temperature be 1000 DEG C, soaking time 4 hours, heating rate be 8 DEG C/
Point.
Step 6：It will be noted after pre- burned aluminum oxide anti-static ceramic powder sieving and after paraffin, polyethylene, EVA mixings
Shaping is penetrated, obtains injecting green compact.
Step 7：The green compact of forming are put into air furnace and are sintered.Heating rate is 700 degrees Celsius
0.5 DEG C/minute；4 DEG C/minute after 700 DEG C, until being raised to maximum sintering temperature.1500 DEG C of maximum sintering temperature, and it is incubated 2 hours.
Step 8：The aluminum oxide anti-static ceramic for sintering toughness reinforcing is machined as needed, polished, obtains chi
The qualified anti-static ceramic finished product of very little, shape, surface quality.
Comparative example：
| Aluminum oxide | 80% |
| Micron ferric oxide | 20% |
Step 1：Aluminum oxide and micron ferric oxide are weighed respectively by mass ratio in table, are then added in ball mill, are entered
Row physical mixed.Wherein, expect：Ball：Water=1:2:0.6, Ball-milling Time 30 hours.
Step 2：The PVA of powder gross mass 2% is weighed, is then made into 20% PVA solution, is added to the good slurry of ball milling
In, stir.
Step 3：The slurry for having added PVA is transferred in the material-storage jar with agitating paddle, mist projection granulating is then carried out, obtains
Spheroidal powder.
Step 4：Obtained spherical powder is put into dry pressing die set and is molded.
Step 5：The green compact of forming are put into air furnace and are sintered, 2 DEG C/minute of programming rate, until highest sinters
1400 DEG C of temperature, then it is incubated 2 hours.
Step 6：The blank sintered is processed, the shape and size needed.
Test case
Resistivity measurement uses volume resistance tester, test temperature：25 DEG C, testing humidity：50%；
Density measurement uses accurate density balance, test temperature：25℃；
Bending strength uses bending strength test instrument, and method of testing is three-point bending resistance strength testing method；
Hardness test uses Vickers hardness instrument.
。
Claims (11)
1. a kind of aluminum oxide anti-electrostatic ceramic material, it is characterised in that the ceramic material includes following group by mass percentage
Into composition：
Aluminum oxide 70wt%-90wt%；The second conductive phase 10wt%-20wt% of nanometer；3Y- zirconium oxides 5%-12%；
The preparation method of above-mentioned ceramic material comprises the following steps：
Step 1：By AlCl3Solution, ZrOCl2Solution, Y（NO3）3Solution is mixed, stirring makes its equal by formula after weighing
Even mixing；
Step 2：Ammoniacal liquor is slowly added dropwise into well mixed solution with peristaltic pump, while solution is slowly stirred, until
Solution ph is 9-10, generates mixed precipitation；Precipitation is rinsed repeatedly with water, until Cl is not present in colloidal sol-Untill；Then with from
Heart dewaterer, unnecessary water is removed, obtained the mixed gel of aluminium hydroxide, zirconium hydroxide, yttrium hydroxide；
Step 3：Obtained mixed gel and the second conductive phase of load weighted nanometer material are added into suitable quantity of water, are added to planet
Ball milling mixing is carried out in ball mill；
Step 4：The slurry filtration that ball milling is obtained is come out, and being pumped into spray tower with wriggling is spray-dried；
Step 5：Pre-burning is carried out to the powder being spray-dried, makes aluminium hydroxide dehydration, is finally changed into Alpha's aluminum oxide,
And complete stabilization of the yittrium oxide to zirconium oxide；
Step 6：Shape and size by pre- burned toughened aluminum oxide anti-static ceramic powder sieving aftershaping for needs；
Step 7：The green compact of forming are put into air furnace and are sintered, low-temperature zone needs slowly heating, sintering temperature during sintering
It is 1500 DEG C -1600 DEG C to spend scope；
Step 8：The aluminum oxide anti-static ceramic sintered is machined as needed, polished, obtain size, shape,
The qualified anti-static ceramic finished product of surface quality.
2. a kind of aluminum oxide anti-electrostatic ceramic material according to claim 1, it is characterised in that the ceramic material presses quality
Percentages include following constituent：Aluminum oxide 70wt%-85wt%；The second conductive phase 10wt%-20wt% of nanometer； 3Y-
Zirconium oxide 5%-10%.
3. a kind of aluminum oxide anti-electrostatic ceramic material according to claim 1 or 2, it is characterised in that aluminum oxide is using coprecipitated
Granularity prepared by shallow lake method is 100nm -500nm oxide of high activity aluminium powder.
A kind of 4. aluminum oxide anti-electrostatic ceramic material according to claim 1 or 2, it is characterised in that the conductive phase of nanometer second
Mixed using the one or more in single oxide or the oxide of doping.
A kind of 5. aluminum oxide anti-electrostatic ceramic material according to claim 4, it is characterised in that described single oxide
Using CuO, Cu2O、V2O5、NiO、MnO、MnO2、CoO、Co2O3、Co3O4、Fe2O3、FeO、Fe3O4And Cr2O3In one kind or more
Kind mixing；The oxide of described doping uses ZnO, SnO2、TiO2With the one or more mixing in ITO.
6. a kind of aluminum oxide anti-electrostatic ceramic material according to claim 4, it is characterised in that the conductive phase of nanometer second is adopted
With CoO, Fe2O3Or TiO2。
A kind of 7. method for preparing a kind of aluminum oxide anti-electrostatic ceramic material described in claim 1 or 2, it is characterised in that the party
Method comprises the following steps：
Step 1：By AlCl3Solution, ZrOCl2Solution, Y（NO3）3Solution is mixed, stirring makes its equal by formula after weighing
Even mixing；
Step 2：Ammoniacal liquor is slowly added dropwise into well mixed solution with peristaltic pump, while solution is slowly stirred, until
Solution ph is 9-10, generates mixed precipitation；Precipitation is rinsed repeatedly with water, until Cl is not present in colloidal sol-Untill；Then with from
Heart dewaterer, unnecessary water is removed, obtained the mixed gel of aluminium hydroxide, zirconium hydroxide, yttrium hydroxide；
Step 3：Obtained mixed gel and the second conductive phase of load weighted nanometer material are added into suitable quantity of water, are added to planet
Ball milling mixing is carried out in ball mill；
Step 4：The slurry filtration that ball milling is obtained is come out, and being pumped into spray tower with wriggling is spray-dried；
Step 5：Pre-burning is carried out to the powder being spray-dried, makes aluminium hydroxide dehydration, is finally changed into Alpha's aluminum oxide,
And complete stabilization of the yittrium oxide to zirconium oxide；
Step 6：Shape and size by pre- burned toughened aluminum oxide anti-static ceramic powder sieving aftershaping for needs；
Step 7：The green compact of forming are put into air furnace and are sintered, low-temperature zone needs slowly heating, sintering temperature during sintering
It is 1500 DEG C -1600 DEG C to spend scope；
Step 8：The aluminum oxide anti-static ceramic sintered is machined as needed, polished, obtain size, shape,
The qualified anti-static ceramic finished product of surface quality.
8. preparation method according to claim 7, it is characterised in that the quality of water is that mixed gel and nanometer second are conductive
0.3-0.5 times of phase material mass；Rotational speed of ball-mill is set as 300-500r/ points, 5-10 hours ball milling mixing time.
9. preparation method according to claim 7, it is characterised in that spray tower is pumped into using wriggling and is spray-dried；If
Inlet temperature is determined for 200-250 DEG C, and discharging opening temperature is 90-130 DEG C, atomizer rotating speed 15-30Hz, wriggling revolution speed
10-25Hz。
10. preparation method according to claim 7, it is characterised in that calcined temperature is 1000-1200 DEG C, soaking time 1-
4 hours, heating rate was 2-8 DEG C.
11. preparation method according to claim 7, it is characterised in that it was in the past 0.5-2 that heating rate, which is 750 degrees Celsius,
DEG C/minute；4-5 DEG C/minute after 750 DEG C, until being raised to maximum sintering temperature；Maximum sintering temperature scope is 1500 DEG C -1600 DEG C,
It is incubated 2-4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510606526.9A CN105236941B (en) | 2015-09-22 | 2015-09-22 | A kind of aluminum oxide anti-electrostatic ceramic material and preparation method thereof |
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| CN107473741A (en) * | 2017-09-21 | 2017-12-15 | 深圳市商德先进陶瓷股份有限公司 | Anti-static ceramic and preparation method thereof |
| CN107759205B (en) * | 2017-11-07 | 2020-09-01 | 江西新景象陶瓷有限公司 | Anti-static ceramic and preparation method thereof |
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| CN110015887A (en) * | 2019-04-01 | 2019-07-16 | 中国有色桂林矿产地质研究院有限公司 | A kind of titanium nitride reinforcement Zirconia reinforced alumina ceramic powder and preparation method thereof |
| CN112500152B (en) * | 2020-12-15 | 2022-09-09 | 无锡特科精细陶瓷有限公司 | Preparation method of anti-static ceramic |
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| CN113698182B (en) * | 2021-08-05 | 2023-05-26 | 杭州大和江东新材料科技有限公司 | Antistatic alumina ceramic material and preparation method thereof |
| CN114262209B (en) * | 2021-12-23 | 2023-07-07 | 佛山欧神诺陶瓷有限公司 | Light antistatic ceramic tile and preparation method thereof |
| CN115340367B (en) * | 2022-08-17 | 2023-05-12 | 湖南圣瓷科技有限公司 | Alumina ceramic and preparation method and application thereof |
| CN115448742B (en) * | 2022-08-29 | 2024-03-29 | 湖南圣瓷科技有限公司 | Alumina antistatic ceramic and preparation method thereof |
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