CN110078496A - The preparation method and preparation facilities of ceramic material - Google Patents
The preparation method and preparation facilities of ceramic material Download PDFInfo
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- CN110078496A CN110078496A CN201810075678.4A CN201810075678A CN110078496A CN 110078496 A CN110078496 A CN 110078496A CN 201810075678 A CN201810075678 A CN 201810075678A CN 110078496 A CN110078496 A CN 110078496A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 67
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 77
- 238000005245 sintering Methods 0.000 claims abstract description 57
- 238000004826 seaming Methods 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 25
- 238000006073 displacement reaction Methods 0.000 claims description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 5
- 239000007770 graphite material Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 238000000034 method Methods 0.000 description 29
- 239000012071 phase Substances 0.000 description 25
- 239000000919 ceramic Substances 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- 239000000523 sample Substances 0.000 description 12
- 238000003825 pressing Methods 0.000 description 10
- 238000000280 densification Methods 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 102100034013 Gamma-glutamyl phosphate reductase Human genes 0.000 description 4
- 230000008602 contraction Effects 0.000 description 4
- 210000003205 muscle Anatomy 0.000 description 4
- 101001133924 Homo sapiens Gamma-glutamyl phosphate reductase Proteins 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 210000001519 tissue Anatomy 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- 239000004927 clay Substances 0.000 description 2
- 230000005674 electromagnetic induction Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000037237 body shape Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- C04B35/48—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
- C04B35/64—Burning or sintering processes
-
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
-
- 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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
Abstract
The present invention provides a kind of preparation methods of ceramic material, in the preparation method, raw material is pressurized flash burning, and specifically, the preparation method includes the following steps: S1: raw material (4) is simultaneously loaded into mold (100) by building mold (100)；S2: the mold for being mounted with raw material is put into sintering furnace；S3: vacuumizing and heats；S4: make one in seaming chuck and push-down head closely to move relative to another, and make to act on the pressure constant pressure on raw material；S5: apply constant voltage on seaming chuck and push-down head using DC power supply, and furnace chamber temperature is made to continue to heat up with fixed rate；S6: multistage flash burning is carried out to raw material；S7: cutting DC power supply is simultaneously stopped heating furnace chamber.The present invention also provides a kind of preparation facilities of ceramic material.The preparation method and preparation facilities of ceramic material according to the present invention can reduce sintering temperature, reduce sintering time.
Description
Technical field
The present invention relates to ceramic materials preparation technology fields, and in particular, to a kind of preparation method of ceramic material, especially
Be a kind of low temperature quickly prepare zirconia ceramics pressurization auxiliary flash burning method and a kind of preparation facilities of ceramic material.
Background technique
Preparation for ceramic material, it is known to electromagnetic induction hot pressing sintering method and discharge plasma sintering process.Electromagnetism
Induction hot pressing sintering method can during heating pressurize to sample, to accelerate the diffusion process of solid phase reaction, effectively drop
Sintering temperature and low and sintering time, but the sintering temperature of this sintering process, still up to 1600 DEG C or more, sintering time needs longer
Time, reach 1-2 hours.Discharge plasma sintering process introduces electric field in sintering, using nano zirconium oxide powder as raw material,
Fine grain zirconia ceramics can be made generally at 1250-1300 DEG C in sintering temperature, but sintering time still needs to 0.5 hour or more.
Summary of the invention
It is an object of the invention at least partly overcome the deficiencies of existing technologies, a kind of preparation side of ceramic material is provided
Method can reduce sintering temperature.
The object of the invention is also to provide a kind of preparation methods of ceramic material, can reduce sintering time.
The object of the invention is also to provide a kind of preparation methods of ceramic material that preparation process is simplified.
The object of the invention is also to provide a kind of preparation facilities of ceramic material.
In order to achieve the above objectives or the first purpose, technical solution of the invention are as follows:
A kind of preparation method of ceramic material, in the preparation method, raw material is pressurized flash burning.
According to a preferred embodiment of the present invention, the preparation method includes the following steps:
S1: raw material is simultaneously loaded into mold by building mold, wherein the mold includes seaming chuck and push-down head, seaming chuck
It is made with push-down head of graphite material, and the side of the close raw material of seaming chuck and push-down head is respectively equipped with one layer of conductive gold
Belong to piece, two conductive metal sheets are clipped in respectively between seaming chuck and raw material and between push-down head and raw material；
S2: the mold for being mounted with raw material is put into sintering furnace, and graphite cover is wherein equipped in the furnace chamber of sintering furnace, for adding
Hot stove chamber；
S3: vacuumizing and heats: vacuumizing to furnace chamber, and by graphite cover heating furnace chamber, furnace chamber is made to be warming up to sudden strain of a muscle
Burn temperature；
S4: make one in seaming chuck and push-down head closely to move relative to another, and make to act on raw material
Pressure is constant pressure；
S5: applying constant voltage using DC power supply on seaming chuck and push-down head, and makes furnace chamber temperature with fixed speed
Rate continues to heat up；
S6: multistage flash burning is carried out to raw material；
S7: cutting DC power supply is simultaneously stopped heating furnace chamber.
According to a preferred embodiment of the present invention, described the step of carrying out multiple flash burning to raw material, includes:
S61: real-time measurement will be applied by the current strength of raw material when the trend that a moment increases occurs in electric current
The voltage added is changed into constant current mode by constant voltage mode, and wherein constant current mode includes two subpatterns；
S62: in the first initial subpattern, setting electric current value is the first current value；
S63: when the relative displacement of seaming chuck and push-down head reaches predetermined threshold or the flash burning time reaches the predetermined time,
First subpattern is changed into the second subpattern；
S64: in the second subpattern, setting electric current value is the second current value greater than the first current value, and highest is arranged
Then flash burning electrical power keeps certain time under the second subpattern,
Wherein, the first subpattern corresponds to first stage flash burning, and the second subpattern corresponds to second stage flash burning.
According to a preferred embodiment of the present invention, the raw material be through oversintering and be sieved mix Y2O3ZrO2Powder,
Wherein Y2O3Atomicity percentage composition be 3-5%, the phase structure of raw material is the mixed phase comprising tetragonal phase, contains 10-30%'s
Monoclinic phase.
According to a preferred embodiment of the present invention, the particle diameter of the powder is between 30-100nm.
According to a preferred embodiment of the present invention, one made in seaming chuck and push-down head leans on relative to another
Near-earth movement includes: fixed seaming chuck and increase push-down head；Or it fixes push-down head and declines seaming chuck.
According to a preferred embodiment of the present invention, in step s3, the vacuum degree in furnace chamber is evacuated to 10Pa hereinafter, simultaneously
And flash burning temperature is 800-900 DEG C.
According to a preferred embodiment of the present invention, in step s 4, the constant pressure is 20-100MPa.
According to a preferred embodiment of the present invention, the first current value is 2-5A, predetermined threshold 2-4mm, predetermined time
For 50-100s, the second current value is 5.5-10A, and highest flash burning electrical power is 50-100W, and the holding certain time is
Keep 20-50s.
According to another aspect of the present invention, ceramic material described in a kind of implementation any one of previous embodiment is provided
Preparation method ceramic material preparation facilities.
The preparation method and preparation facilities of ceramic material according to the present invention, sintering temperature are greatly reduced, and sintering temperature exists
1100 DEG C hereinafter, can simultaneously reduce sintering time, it is instantaneous to complete sintering.With ZrO2When for raw material, the method according to the invention and
Device can be made room temperature meta-stable tetragonal phase zirconium oxide (Y-TZP) ceramic material, density can reach the 80% of theoretical density with
On, ceramic surface is scanned the compact tissue pattern of the visible ceramic material of Electronic Speculum, by portion after overground, polishing and metal spraying
Divide ceramic block to smash and clay into power, characterized by X-ray diffraction analysis (XRD), it was demonstrated that is sintered the ceramic material of preparation
Be by based on tetragonal phase, it is identical as the XRD characterization result of powder raw material, illustrate that above-mentioned preparation method does not change the phase of powder raw material
Structure.In addition, using preparation method of the invention, do not need to carry out special green compact compression process to powder raw material, do not need for
Mold provides noble metal electrode, it is thus possible to meet continuity industrial production demand.
Detailed description of the invention
Fig. 1 is the general illustration according to the mold of the embodiment of the present invention；
Fig. 2 is flash burning power, displacement of pressing head and the temperature curve shown during the densification of Y-TZP material；
Fig. 3 is the scanning according to the Y-TZP ceramic surface of the preparation method preparation of the ceramic material of the embodiment of the present invention
Electron microscope；
Fig. 4 is the XRD curve and GSAS refine result curve of the Y-TZP ceramics of preparation；And
Fig. 5 is the XRD curve and GSAS refine result curve of raw material.
Specific embodiment
Detailed description of the present invention exemplary embodiment with reference to the accompanying drawing, wherein the same or similar label indicates phase
Same or similar element.In addition, in the following detailed description, to elaborate many concrete details to provide convenient for explaining
To the comprehensive understanding of present disclosure embodiment.It should be apparent, however, that one or more embodiments are not having the case where these details
Under can also be carried out.In other cases, well known construction and device is diagrammatically embodied to simplify attached drawing.
Designer has found when preparing ceramic material using discharge plasma sintering process to flash burning phenomenon, this method be with
The green compact of cold moudling are raw material, by being hung with the electrode wires of two end in contact of green compact, and pre-applied voltage, it can add
Sintering is completed within heat to several seconds of flash burning temperature.But this method is necessarily required with the green compact of the specific shape by cold pressing
For raw material, and green body shapes are more complicated, can not carry out continuity industrialized production；In addition, needing to utilize using this method
Noble metal electrode applies specific voltage at sample both ends, thus increases production cost.
Designer further improves common flash burning method as a result, remains the flash burning method low temperature, instantaneous
The advantages of sintering, and innovatively in conjunction with the advantages of electromagnetic induction hot pressing and sintering technique, to evade complicated green compact compacting stream
Journey and noble metal electrode problem with high costs enable the invention to become a kind of work for meeting continuity industrial production demand
Process, sintering temperature is at 1100 DEG C hereinafter, instantaneously completing the sintering of Y-TZP.
Conceived based on foregoing invention, proposes a kind of preparation method of ceramic material, in the preparation method, raw material quilt
Pressurization flash burning.The preparation method includes the following steps:
S1: raw material 4 is simultaneously loaded into mold 100 by building mold 100, wherein the mold 100 includes seaming chuck 1 under
Pressure head 2, seaming chuck 1 and push-down head 2 are made of graphite material, and the side of the close raw material of seaming chuck 1 and push-down head 2 point
Not She You one layer of conductive metal sheet 3, two conductive metal sheets 3 are clipped between seaming chuck 1 and raw material 4 respectively and 2 He of push-down head
Between raw material 4；
S2: the mold for being mounted with raw material is put into sintering furnace, and graphite cover is wherein equipped in the furnace chamber of sintering furnace, for adding
Hot stove chamber；
S3: vacuumizing and heats: vacuumizing to furnace chamber, and by graphite cover heating furnace chamber, furnace chamber is made to be warming up to sudden strain of a muscle
Burn temperature；
S4: make one in seaming chuck and push-down head closely to move relative to another, and make to act on raw material
Pressure is constant pressure；
S5: applying constant voltage using DC power supply on seaming chuck and push-down head, and makes furnace chamber temperature with fixed speed
Rate continues to heat up；
S6: multistage flash burning is carried out to raw material；
S7: cutting DC power supply is simultaneously stopped heating furnace chamber.
Further, described the step of carrying out multiple flash burning to raw material, includes:
S61: real-time measurement will be applied by the current strength of raw material when the trend that a moment increases occurs in electric current
The voltage added is changed into constant current mode by constant voltage mode, and wherein constant current mode includes two subpatterns；
S62: in the first initial subpattern, setting electric current value is the first current value；
S63: when the relative displacement of seaming chuck and push-down head reaches predetermined threshold or the flash burning time reaches the predetermined time,
First subpattern is changed into the second subpattern；
S64: in the second subpattern, setting electric current value is the second current value greater than the first current value, and highest is arranged
Then flash burning electrical power keeps certain time under the second subpattern,
Wherein, the first subpattern corresponds to first stage flash burning, and the second subpattern corresponds to second stage flash burning.
Advantageously, the raw material be through oversintering and be sieved mix Y2O3ZrO2Powder, wherein Y2O3Atomicity percentage
Content is 3-5%, and the phase structure of raw material is the mixed phase comprising tetragonal phase, the monoclinic phase containing 10-30%；Of the powder
Grain diameter is between 30-100nm.
Wherein, the mold is the mold of Bidirectional-pressure, and the graphite is high strength graphite, conductive metal sheet conduct
Electrode, with a thickness of 0.5mm-1mm, electric conductivity is good, and chemical property is highly stable, under extreme conditions, does not occur with raw material
Chemical reaction.One made in seaming chuck and push-down head relative to another closely movement include: fixed seaming chuck simultaneously
Increase push-down head；Or it fixes push-down head and declines seaming chuck.Alternatively, seaming chuck and push-down head can be not fixed,
It is mobile simultaneously.However, being fixed using a pressure head, being advantageous by the way of another movable press head, this is because keeping permanent
Under the conditions of fixed contact pressure, the moving displacement of single pressure head is exactly the densification process of raw material, is conducive to monitor densification mistake
Journey.
In step s3, the vacuum degree in furnace chamber is evacuated to 10Pa hereinafter, and flash burning temperature be 800-900 DEG C, these
Parameter is for by mixing Y2O3ZrO2It is particularly advantageous that powder, which obtains zirconia ceramics,.In step s 4, the constant pressure
For 20-100MPa.In step s 5, constant voltage 50-100V, fixed rate are 10-20 DEG C/h.In step S61-S64,
First current value is 2-5A, predetermined threshold 2-4mm, predetermined time 50-100s, and the second current value is 5.5-10A, and highest is dodged
Burning electrical power is 50-100W, and the holding certain time is to keep 20-50s.
According to another aspect of the present invention, ceramic material described in a kind of implementation any one of previous embodiment is provided
Preparation method ceramic material preparation facilities.
The preparation method and preparation facilities of ceramic material according to the present invention, sintering temperature are greatly reduced, and sintering temperature exists
1100 DEG C hereinafter, can simultaneously reduce sintering time, it is instantaneous to complete sintering.With ZrO2When for raw material, the method according to the invention and
Device can be made room temperature meta-stable tetragonal phase zirconium oxide (Y-TZP) ceramic material, density can reach the 80% of theoretical density with
On, ceramic surface is scanned the compact tissue pattern of the visible ceramic material of Electronic Speculum, by portion after overground, polishing and metal spraying
Divide ceramic block to smash and clay into power, characterized by X-ray diffraction analysis (XRD), it was demonstrated that is sintered the ceramic material of preparation
Be by based on tetragonal phase, it is identical as the XRD characterization result of powder raw material, illustrate that above-mentioned preparation method does not change the phase of powder raw material
Structure.In addition, using preparation method of the invention, do not need to carry out special green compact compression process to powder raw material, do not need for
Mold provides noble metal electrode, it is thus possible to meet continuity industrial production demand.
Embodiment:
It is said referring to mold used in preparation method and preparation facilities of the Fig. 1 to ceramic material of the invention
Bright, Fig. 1 shows the general illustration of mold, as shown in Figure 1, mold 100 includes seaming chuck 1 and push-down head 2,1 He of seaming chuck
Push-down head 2 is made of graphite material, and the side of the close raw material of seaming chuck 1 and push-down head 2 is respectively equipped with one layer of conduction
Sheet metal 3, two conductive metal sheets 3 are clipped in respectively between seaming chuck 1 and raw material 4 and between push-down head 2 and raw material 4.
Illustrate the preparation method of ceramic material of the invention for preparing zirconia ceramics below.During the preparation process,
With through oversintering and be sieved mix Y2O3ZrO2Powder is raw material, wherein Y2O3Atomicity percentage composition be 3-5%, by X
X ray diffraction analysis x (XRD) characterization, the phase structure of raw material be based on tetragonal phase mixed phase (containing about 20% monoclinic phase,
XRD curve and GSAS fitting result are referring to Fig. 5), particle diameters are between 30-100nm, using following processing step system
Standby zirconia ceramics:
(1) suitable powder raw material is loaded in the mold (see Fig. 1) of Bidirectional-pressure, wherein upper and lower two pressure heads of mold
It is high strength graphite, pads one layer of conductive metal sheet between two pressure heads and powder raw material respectively；
(2) mold is put into sintering furnace first, vacuum degree in furnace chamber is evacuated to 10Pa hereinafter, then by furnace chamber
The heating of graphite cover, is rapidly heated to 800-900 DEG C of flash burning temperature；Fixed seaming chuck, rises push-down head, carries out Bidirectional-pressure,
The constant pressure acted on raw material is set as 20-100MPa；
(3) after temperature is stablized, the constant DC voltage of 50-100V is added at upper and lower pressure head both ends, and make in-furnace temperature
Continue to heat up with 10-20 DEG C/h rate；
(4) real-time measurement is by the current strength of raw material, when electric current trend that a moment straight line increases occurs (see figure
2), added DC voltage is changed into constant current controlling mode by constant voltage mode, different according to the electric current of setting, is divided into two stages sudden strain of a muscle
It burns.First stage flash burning setting electric current is 2-5A, when movable press head displacement reaches 2-4mm or the flash burning time reaches 50-100s
Shi Zidong jumps to second stage flash burning, and second stage flash burning setting electric current is 5-10A, and highest flash burning electrical power 50- is arranged
100W automatically cuts off DC power supply after being kept for the 20-50s time, while being automatically stopped heating furnace chamber.In above-mentioned two stages flash burning mistake
Cheng Zhong, pressure head also correspond to generation instantaneous flash burning displacement twice.
Y-TZP ceramic material made from preparation method according to above-described embodiment, density can reach theoretical density
80% or more, but the present invention can be according to raw material and properties of product requirement, on the basis of two-stage flash burning program
Superposition forms more multistage flash burning.For example, constant current mode includes three subpatterns, the step that multiple flash burning is carried out to raw material
Suddenly further include: after step S64, the second subpattern is changed into third subpattern, in third subpattern, setting electric current value
It for the third current value greater than the second current value, is then kept under third subpattern a period of time, third subpattern corresponding the
Three stage flash burnings.
It should be noted that above-mentioned preparation method is also referred to as pressurizeed, auxiliary flash burning prepares tetragonal zirconia ceramics material
Sintering method, in the method, powder raw material are loaded in the Bidirectional pressurizing mould of special designing, this makes sintering of the invention
Method does not need to carry out special green compact compression process to powder raw material.Used sintering furnace is that special graphite heating is sintered
Furnace, while pressure and voltage can be applied on the pressure head of mold, because without providing noble metal electrode for mold.In the reality
It applies in example, fixed seaming chuck, push-down head liftable, under the conditions of the contact pressure kept constant, the moving displacement of push-down head is just
It is the densification process of specimen material.It in step (2), is rapidly heated to 800-900 DEG C, and keeps constant pressure 20-
100MPa, temperature and constant pressure value here is determined by the property of powder raw material, other being prepared using the present invention
It can be modified according to material properties when material.As furnace chamber is with 10-20 DEG C/h of heating rate heating, powder raw material (sample material
Material) conductivity non-linear increase trend is presented as the temperature rises, voltage remains unchanged at this time, and electric current can gradually increase
Greatly.In step (3), graphite pressure head both ends add 50-100V constant DC voltage, however it should be noted that according to
Inner section product, the amount of filled sample and the difference of properties of samples of mold, setting voltage can be different.In step (4), when
When electric current moment ramps, added DC voltage is changed into constant current controlling mode by constant voltage mode, passes through setting electricity here
Upper limit value is flowed to realize constant current controlling.
After constant voltage mode is transformed into constant current mode in step (4), since the resistance of raw material is anxious under the conditions of flash burning
Reduce sharply it is small, so voltage can moment reduce, meet Ohm's law.In addition, no according to the current value (the maximum current upper limit) of setting
Together, two stages flash burning can be divided into, here the number in flash burning stage be can be required according to powder raw material property and properties of sample and
Change.In step (4), the first stage flash burning setting electric current upper limit is 2-5A, current value here will with feedstock property and
Mold inner section product is consistent, and generally passes through the current density 10-100mA/mm of sample2.When movable press head displacement reaches 2-
Automatically second stage is jumped to when 4mm, the first trigger value that displacement of pressing head jumps automatically as the flash burning stage here, it sets
Definite value is determined by the property and additional axial compressive force of sample.Jump to automatically when the flash burning time reaching 50-100s
Two-stage flash burning, the second trigger value that the flash burning time jumps automatically as the flash burning stage here, its setting value is by sample
Property and additional axial compressive force determined.
In step (4), two trigger values that the flash burning stage jumps automatically are set, meet any one during flash burning
Trigger value can result in flash burning and jump to next stage automatically.The second stage flash burning setting electric current upper limit is 5-10A, is kept
DC power supply is automatically cut off after the 20-50s time, while furnace chamber is automatically stopped heating, when current upper limit value and holding here
Between have to be consistent with properties of samples and mold inner section product, generally by the current density 70-150mA/mm of sample2。
It is 50-100W that highest flash burning electrical power, which is arranged, in second stage flash burning, flash burning electrical power here be equal to two sections of sample added by direct current
The product of voltage and the electric current by sample.During above-mentioned two stages flash burning, pressure head also corresponds to generation instantaneous sudden strain of a muscle twice
Burn displacement, illustrate sample densification be sintered along with the process that electric current moment increases and moment generation.
Fig. 2 is flash burning power, displacement of pressing head and the temperature curve shown during the densification of Y-TZP material, wherein
Flash burning power (flash burning electrical power) is indicated that shrinking displacement (displacement of pressing head) is indicated that sintering temperature is by justifying by triangle point by side's point
Point indicates, as seen from the figure, during the densification of Y-TZP material, shrinks displacement there are three phases, i.e. rank is shunk in cold pressing
Section, flash burning contraction phase first stage and second stage flash burning contraction phase, respectively corresponded in figure cold pressing shrink displacement,
The contraction displacement of the contraction displacement and second stage flash burning of first stage flash burning.In addition, from Figure 2 it can be seen that raw material sintering from
Start within 830 seconds, until 970 seconds terminate, sintering time is 140 seconds, and first stage sintering temperature is 960 DEG C, second stage sintering temperature
Degree is 1100 DEG C, and sintering temperature is greatly reduced.It can be seen that sintering temperature and sintering time are greatly reduced.
By measurement, the density for being sintered the ceramic material of preparation reaches 80% of theoretical density or more.Fig. 3 is according to this
The scanning electron microscope (SEM) photograph of the Y-TZP ceramic surface of the preparation method preparation of the ceramic material of the embodiment of invention, as shown in figure 3, pottery
Porcelain surface is scanned the compact tissue pattern of the visible ceramic material of Electronic Speculum after overground, polishing and metal spraying.
Fig. 4 gives the XRD curve and GSAS software refine result curve of the Y-TZP ceramics of preparation, will part ceramics
Block is smashed and is clayed into power, by XRD characterization, it was demonstrated that the ceramic material for being sintered preparation is also by based on tetragonal phase, containing about
20% monoclinic phase, it is identical as XRD characterization result (referring to the Fig. 5) of powder raw material, illustrate that above-mentioned preparation method does not change powder
The phase structure of raw material.
The present invention assists flash burning using additional axial compressive force using the charging mold of the Bidirectional-pressure of a special designing,
So that powder raw material is needed not move through cold pressing base, densification sintering can be completed moment.
Of the invention is technically characterized by comprising the steps as follows:
(1) sintering mold uses the design of Bidirectional-pressure conductive charges mold, the contact surface of graphite pressure head and specimen material
The conductive metal sheet of a piece of 0.5-1mm is padded, does not need to carry out special cold pressing treatment to dusty material before sintering.
(2) in flash burning sintering process, specimen material both ends add the constant axial pressure of 20-100MPa.
(3) in flash burning sintering process, by monitor push-down head moving displacement can in situ study specimen material it is closely knit
Change process.
(4) it in flash burning sintering process, according to the sintering of different materials needs that flash burning twice or more than twice can be set
Stage.The constant current controlling of power supply is realized by two different current upper limit values of setting, and the flash burning that two stages occur is burnt
Knot.
(5) in sintering process, gradient it is stepped up flash burning electric current, first stage flash burning setting electric current upper limit 2-5A,
Two-stage flash burning setting electric current upper limit 5-10A.
(6) two trigger values are arranged in the end of flash burning first stage: 1, being jumped automatically using displacement of pressing head as the flash burning stage
The first trigger value, when movable press head displacement reach 2-4mm when jump to second stage automatically；2, using the flash burning time as flash burning
The second trigger value that stage jumps automatically, jumps to second stage when the flash burning time reaching 50-100s automatically.During flash burning
Meet any one trigger value, can flash burning be caused to jump to second stage automatically.
Flash burning electrical power upper limit 50-100w was arranged in (7) second flash burning stages.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can be changed these embodiments without departing from the principles and spirit of the present invention.Applicable model of the invention
It encloses and is defined by the appended claims and the equivalents thereof.
Reference signs list:
100 molds
1 seaming chuck
2 push-down heads
3 conductive metal sheets
4 raw materials
Claims (10)
1. a kind of preparation method of ceramic material, which is characterized in that in the preparation method, raw material is pressurized flash burning.
2. the preparation method of ceramic material according to claim 1, which is characterized in that the preparation method includes following step
It is rapid:
S1: raw material (4) is simultaneously loaded into mold (100) by building mold (100), wherein the mold (100) includes seaming chuck
(1) it is made with push-down head (2), seaming chuck (1) and push-down head (2) of graphite material, and seaming chuck (1) and push-down head (2)
The side of close raw material be respectively equipped with one layer of conductive metal sheet (3), two conductive metal sheets (3) are clipped in seaming chuck (1) respectively
Between raw material (4) and between push-down head (2) and raw material (4)；
S2: the mold for being mounted with raw material is put into sintering furnace, and graphite cover is wherein equipped in the furnace chamber of sintering furnace, is used for heating furnace
Chamber；
S3: vacuumizing and heats: vacuumizing to furnace chamber, and by graphite cover heating furnace chamber, furnace chamber is made to be warming up to flash burning temperature
Degree；
S4: make one in seaming chuck and push-down head closely to move relative to another, and make to act on the pressure on raw material
For constant pressure；
S5: applying constant voltage using DC power supply on seaming chuck and push-down head, and make furnace chamber temperature with fixed rate after
Temperature of continuing rising；
S6: multistage flash burning is carried out to raw material；
S7: cutting DC power supply is simultaneously stopped heating furnace chamber.
3. the preparation method of ceramic material according to claim 2, which is characterized in that described to carry out multiple flash burning to raw material
The step of include:
S61: real-time measurement is by the current strength of raw material, when the trend that a moment increases occurs in electric current, by what is applied
Voltage is changed into constant current mode by constant voltage mode, and wherein constant current mode includes two subpatterns；
S62: in the first initial subpattern, setting electric current value is the first current value；
S63: when the relative displacement of seaming chuck and push-down head reaches predetermined threshold or the flash burning time reaches the predetermined time, by
One subpattern is changed into the second subpattern；
S64: in the second subpattern, setting electric current value is the second current value greater than the first current value, and highest flash burning is arranged
Then electrical power keeps certain time under the second subpattern,
Wherein, the first subpattern corresponds to first stage flash burning, and the second subpattern corresponds to second stage flash burning.
4. the preparation method of ceramic material according to claim 3, which is characterized in that the raw material is through oversintering and mistake
Sieve mixes Y2O3ZrO2Powder, wherein Y2O3Atomicity percentage composition be 3-5%, the phase structure of raw material includes tetragonal phase
Mixed phase, the monoclinic phase containing 10-30%.
5. the preparation method of ceramic material according to claim 4, which is characterized in that the particle diameter of the powder exists
Between 30-100nm.
6. the preparation method of ceramic material according to claim 2, which is characterized in that described to make in seaming chuck and push-down head
One relative to another, closely movement includes: fixed seaming chuck and increase push-down head；Or it fixes push-down head and makes
Seaming chuck decline.
7. the preparation method of ceramic material according to claim 2, which is characterized in that in step s3, will be in furnace chamber
Vacuum degree is evacuated to 10Pa hereinafter, and flash burning temperature is 800-900 DEG C.
8. the preparation method of ceramic material according to claim 2, which is characterized in that in step s 4, the constant pressure
It is by force 20-100MPa.
9. the preparation method of ceramic material according to claim 3, which is characterized in that the first current value is 2-5A, is made a reservation for
Threshold value is 2-4mm, and predetermined time 50-100s, the second current value is 5.5-10A, and highest flash burning electrical power is 50-100W, and
And the holding certain time is to keep 20-50s.
10. a kind of preparation dress of the ceramic material for the preparation method for implementing ceramic material described in any one of any one of claims 1 to 99
It sets.
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| CN112683062B (en) * | 2020-12-08 | 2022-09-02 | 国网江西省电力有限公司电力科学研究院 | Ultrafast sintering method and device for ceramic material |
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Application publication date: 20190802 |