CN106588003B - The cover board and its preparation method and application of zirconia ceramics piece and preparation method thereof and induction identification mould group - Google Patents
The cover board and its preparation method and application of zirconia ceramics piece and preparation method thereof and induction identification mould group Download PDFInfo
- Publication number
- CN106588003B CN106588003B CN201611111593.4A CN201611111593A CN106588003B CN 106588003 B CN106588003 B CN 106588003B CN 201611111593 A CN201611111593 A CN 201611111593A CN 106588003 B CN106588003 B CN 106588003B
- Authority
- CN
- China
- Prior art keywords
- zirconia ceramics
- preparation
- ceramics piece
- minutes
- cover board
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/29—Producing shaped prefabricated articles from the material by profiling or strickling the material in open moulds or on moulding surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06V—IMAGE OR VIDEO RECOGNITION OR UNDERSTANDING
- G06V40/00—Recognition of biometric, human-related or animal-related patterns in image or video data
- G06V40/10—Human or animal bodies, e.g. vehicle occupants or pedestrians; Body parts, e.g. hands
- G06V40/12—Fingerprints or palmprints
- G06V40/13—Sensors therefor
- G06V40/1306—Sensors therefor non-optical, e.g. ultrasonic or capacitive sensing
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/606—Drying
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Human Computer Interaction (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Multimedia (AREA)
- Theoretical Computer Science (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to the cover boards and its preparation method and application of a kind of zirconia ceramics piece and preparation method thereof and induction identification mould group.The preparation method of the zirconia ceramics piece includes the following steps: for zirconia ceramics slurry to be cast on release film, then through drying, obtains casting belt, wherein casting belt has the bottom surface opposite with release film and the outer surface opposite with bottom surface；Blank is cut out from casting belt, the outer surface of two blank is fitted, and compression moulding, is obtained green body；By blank sintering, zirconia ceramics piece is obtained.The preparation method lower production costs and production efficiency of above-mentioned zirconia ceramics piece are higher, and obtained zirconia ceramics piece bending strength is higher.
Description
Technical field
The present invention relates to ceramic material fields, know more particularly to a kind of zirconia ceramics piece and preparation method thereof and induction
The cover board and its preparation method and application of other mould group.
Background technique
Currently, zirconia material relies on its superior mechanical property and higher dielectric constant (30~40), by increasingly
More cell phone manufacturers uses, and is proposed the mobile phone of the fingerprint recognition mould group with zirconium oxide cover board, wherein zirconia ceramics cover board
For flake, thickness is only 0.08~0.20mm.Common preparation process is that first tape casting prepares blank, then burns blank
Knot obtains the ceramic sheet that thickness is about 0.2~0.4mm, and the zirconia ceramics lid of required thickness is obtained finally by grinding and polishing
Piece.And warpage and curved edge etc. are easily occurred now after sintering with a thickness of 0.2~0.4mm blank using doctor-blade casting process preparation
As needing to correct the flatness to ensure ceramic sheet by double sintering.Although double sintering temperature is lower, double sintering
It will lead to zirconia ceramics crystal grain to grow up, reduce the bending strength of product；Secondly, double sintering can directly increase zirconium oxide
Sheet product cost reduces production efficiency.
Summary of the invention
Based on this, it is necessary to provide a kind of higher bending strength, lower production costs and the higher zirconium oxide of production efficiency
The preparation method of potsherd.
In addition, also providing the cover board and its preparation method and application of a kind of zirconia ceramics piece and induction identification mould group.
A kind of preparation method of zirconia ceramics piece, includes the following steps:
By zirconia ceramics slurry curtain coating on release film, then through drying, obtain casting belt, wherein the curtain coating belt
There are the bottom surface opposite with the release film and the outer surface opposite with the bottom surface；
Blank is cut out from the casting belt, the outer surface of blank described in two of them is fitted, and compression moulding,
Obtain green body；
By the blank sintering, zirconia ceramics piece is obtained.
It in one of the embodiments, further include the preparation step of the zirconia ceramics slurry: by Zirconium powder, molten
Agent, dispersing agent, binder and plasticizer mixing, obtain that viscosity is 1Pas~10Pas, the mass percentage of solid phase is
50%~55% zirconia ceramics slurry.
The partial size of the Zirconium powder is 0.5 micron~0.6 micron in one of the embodiments,.
Dry step after in one of the embodiments, by zirconia ceramics slurry curtain coating on the release film
Suddenly are as follows: spontaneously dry wet base of the curtain coating on the release film at room temperature 30 minutes~60 minutes, then 45 DEG C~50
It is 15 minutes~30 minutes dry at DEG C, then drying 15 minutes~30 minutes at 55 DEG C~60 DEG C, finally at 65 DEG C~70 DEG C
It is 30 minutes~60 minutes dry.
The method of compression moulding after the outer surface of two blank is fitted in one of the embodiments, is temperature
The static pressure such as water, the press temperature are 80 DEG C~90 DEG C, and pressure is 20MPa~50MPa, and the dwell time is 10 minutes~30 points
Clock.
In one of the embodiments, by blank sintering the step of are as follows: the step of by the blank sintering are as follows: by institute
Green body is stated with 0.5 DEG C/min~1 DEG C/min of heating rate from room temperature to 500 DEG C~600 DEG C, then with 2 DEG C/min~
5 DEG C/min of heating rate is warming up to 1450 DEG C~1500 DEG C, and heat preservation sintering 2 hours~4 hours, then again with 5 DEG C/minute
The rate of temperature fall of clock~10 DEG C/min is cooled to 500 DEG C~600 DEG C, last natural cooling.
A kind of zirconia ceramics piece that the preparation method according to above-mentioned zirconia ceramics piece is prepared.
A kind of preparation method of the cover board of induction identification mould group, includes the following steps:
Above-mentioned zirconia ceramics piece is provided；
The zirconia ceramics piece is cut, grinding and buffing, obtains the cover board of the induction identification mould group.
A kind of cover board for the induction identification mould group that the preparation method for the cover board identifying mould group according to above-mentioned induction is prepared.
Application of the cover board of above-mentioned induction identification mould group in mobile phone or tablet computer.
Since tape casting is prepared into casting belt using slurry curtain coating, more or less can all make under gravity
Casting belt is greater than the solid content of the side far from release film close to the solid content of the side of release film, so that casting belt is close to release
The density of the side of film be greater than far from release film one side density, and make casting belt close to the side of release film stress with
The stress of side far from release film is unequal, so that the blank that casting belt is cut out is easy to happen warpage after being sintered and edge is curved
Bent phenomenon, and the preparation method of above-mentioned zirconia ceramics piece is by cutting out two blank from the same casting belt, and by two
(i.e. far from the one side of release film) is compressed together for the lesser outer surface of the density of a blank, to play a complementary effect,
The density for making up the existing one side far from release film of casting belt of direct tape casting itself is less than close to the side of release film
Density and bottom surface and outer surface stress problem not etc. so that the density for the green body that the above method is pressed into is more equal
It is even, the stress distribution of green body is adjusted, so that the stress on opposite two surface of green body is reached unanimity, to advantageously reduce green body
The problem of warpage during the sintering process and curved edge, the zirconia ceramics piece for obtaining sintering is more smooth, no longer need into
Row double sintering, not only reduces production cost, improves production efficiency, it is thus also avoided that tradition is cast molding double sintering and leads
The problem of ceramic crystalline grain of cause is grown up, so that the zirconia ceramics piece that the above method is prepared has better bending strength.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of the cover board of the induction identification mould group of an embodiment；
Fig. 2 is the flow chart of the preparation method of zirconia ceramics piece shown in FIG. 1.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give preferred embodiment of the invention.But the invention can be realized in many different forms, however it is not limited to herein
Described embodiment.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more saturating
It is thorough comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the listed item of pass.
As shown in Figure 1, the preparation method of the cover board of the induction identification mould group of an embodiment, the induction identify mould group for example
It can be fingerprint recognition mould group, the preparation method of the cover board of induction identification mould group includes the following steps:
Step S110: zirconia ceramics piece is provided.
Referring to Figure 2 together, wherein the preparation method of zirconia ceramics piece includes the following steps:
Step S112: by zirconia ceramics slurry curtain coating on release film, then through drying, casting belt is obtained.
Wherein, casting belt has the bottom surface opposite with release film and the outer surface opposite with bottom surface.
Wherein, the zirconia ceramics slurry in step S112 can be made by the steps to obtain: by Zirconium powder, molten
Agent, dispersing agent, binder and plasticizer mixing, obtain that viscosity is 1Pas~10Pas, the mass percentage of solid phase is
50%~55% zirconia ceramics slurry.
Specifically, the step of Zirconium powder, solvent, dispersing agent, binder and plasticizer are mixed specifically: will aoxidize
Zirconium powder body, solvent and dispersing agent ball milling mixing 3 hours~5 hours, binder is then added, plasticizer continue ball milling 5 hours~
10 hours, obtain zirconia ceramics slurry.
Wherein, binder is polyvinyl butyral (PVB)；Dispersing agent is selected from castor oil, olein, phosphoric acid
At least one of ester, herring oil and triethanolamine；Plasticizer is selected from dibutyl phthalate (DBP), polyethylene glycol
(PEG) and at least one of glycerol；Solvent is selected from least one of toluene, dimethylbenzene, ethyl alcohol and butanone.
Specifically, the mass ratio of binder and Zirconium powder is 5:100~10:100；Dispersing agent and Zirconium powder
Mass ratio is 0.5:100~2:100；The mass ratio of plasticizer and Zirconium powder is 10:100~30:100.
Wherein, the median particle diameter (D50) of Zirconium powder is 0.5 micron~0.6 micron.
Further, it in zirconia ceramics slurry, after the step of binder is added, plasticizer continues ball milling, also wraps
Addition defrother, then ball milling 0.5 hour~1 hour are included, the step of last vacuum defoamation 1 hour~2 hours.By the way that de-bubble is added
Agent reduces the stomata quantity in blank to remove the bubble in slurry.Wherein, the mass ratio of defrother and Zirconium powder is
0.1:100~0.5:100.
Wherein, defrother can be defrother commonly used in the art.In the present embodiment, defrother is n-butanol.
Wherein, by zirconia ceramics slurry curtain coating in step on release film, the rate of curtain coating is 1.5 ms/min~
2 ms/min, edge height is 300 microns~1000 microns.
Wherein, the drying steps after by zirconia ceramics slurry curtain coating on release film are as follows: will be cast on release film
Wet base spontaneously dry 30 minutes~60 minutes at room temperature, it is then 15 minutes~30 minutes dry at 45 DEG C~50 DEG C, then
It is 15 minutes~30 minutes dry at 55 DEG C~60 DEG C, it is finally 30 minutes~60 minutes dry at 65 DEG C~70 DEG C.
Step S114: cutting out blank from casting belt, the outer surface of two blank is fitted, and compression moulding, is obtained
To green body.
Wherein, the thickness of the green body is equal to the thickness for the casting belt that traditional direct tape casting obtains.
It wherein, further include the release film removed on casting belt before the step of blank is cut out from casting belt.
Wherein, the method for the compression moulding after the outer surface of two blank being fitted is the static pressure such as warm water, press temperature
It is 80 DEG C~90 DEG C, pressure is 20MPa~50MPa, and the dwell time is 10 minutes~30 minutes.
Step S116: by blank sintering, zirconia ceramics piece is obtained.
Wherein, by blank sintering the step of are as follows: by green body with 0.5 DEG C/min~1 DEG C/min of heating rate from room temperature
500 DEG C~600 DEG C are warming up to, then is warming up to 1450 DEG C~1500 DEG C with 2 DEG C/min~5 DEG C/min of heating rate, and protect
Temperature sintering 2 hours~4 hours, is then cooled to 500 DEG C~600 DEG C again with 5 DEG C/min~10 DEG C/min of rate of temperature fall, most
Natural cooling afterwards.
Wherein, the zirconia ceramics piece being sintered with a thickness of 0.2 millimeter~0.4 millimeter.
Since tape casting is prepared into casting belt using slurry curtain coating, more or less can all make under gravity
Casting belt is greater than the solid content of the side far from release film close to the solid content of the side of release film, so that casting belt is close to release
The density of the side of film be greater than far from release film one side density, and make casting belt close to the side of release film stress with
The stress of side far from release film is unequal, so that the blank that casting belt is cut out is easy to happen warpage after being sintered and edge is curved
Bent phenomenon, and the preparation method of above-mentioned zirconia ceramics piece is by cutting out two blank from the same casting belt, and by two
(i.e. far from the one side of release film) is compressed together for the lesser outer surface of the density of a blank, to play a complementary effect,
The density for making up the existing one side far from release film of casting belt of direct tape casting itself is less than close to the side of release film
Density and bottom surface and outer surface stress problem not etc. so that the density for the green body that the above method is pressed into is more equal
It is even, the stress distribution of green body is adjusted, so that the stress on opposite two surface of green body is reached unanimity, to advantageously reduce green body
The problem of warpage during the sintering process and curved edge, the zirconia ceramics piece for obtaining sintering is more smooth, no longer need into
Row double sintering, not only reduces production cost, improves production efficiency, it is thus also avoided that tradition is cast molding double sintering and leads
The problem of ceramic crystalline grain of cause is grown up, so that the zirconia ceramics piece that the above method is prepared has better bending strength.
Step S120: zirconia ceramics piece being cut, grinding and buffing, obtains the cover board of induction identification mould group.
Wherein, method zirconia ceramics piece cut is laser cutting, in order to cut out zirconia ceramics body piece
It is cut into required shape.
Wherein, grinding and buffing is and to obtain the thin of required thickness in order to which the zirconia ceramics after cutting is flat and smooth
The cover board of the induction identification mould group of piece.Wherein, cover plate with a thickness of 0.08 millimeter~0.2 millimeter.
Due to the cover board of above-mentioned induction identification mould group be cut using above-mentioned zirconia ceramics piece, grinding and buffing it
It obtains afterwards, therefore, the cover board of above-mentioned induction identification mould group has preferable bending strength.
The zirconia ceramics piece of one embodiment is prepared, due to this by the preparation method of above-mentioned zirconia ceramics piece
Zirconia ceramics piece is prepared using the preparation method of above-mentioned zirconia ceramics piece, so that the zirconia ceramics piece is with smaller
Crystal grain and biggish bending strength, and it is more smooth.
The cover board of the induction identification mould group of one embodiment, is prepared by the preparation method of the cover board of above-mentioned induction identification mould group
It obtains, so that the cover board of induction identification mould group has preferable bending strength.
And the cover board of induction identification mould group can be applied in mobile phone or tablet computer.
The following are specific embodiment parts:
Embodiment 1
The preparation process of the cover board of the induction identification mould group of the present embodiment is as follows:
(1) by Zirconium powder, solvent and dispersing agent ball milling mixing 4 hours, binder is then added, plasticizer continues ball
Mill 8 hours is subsequently added into defrother, then ball milling 1 hour, and last vacuum defoamation 1 hour, obtaining viscosity is 8.3Pas, solid phase
The zirconia ceramics slurry that mass percentage is 55%.Wherein, the median particle diameter of Zirconium powder is 0.5 micron~0.6 micro-
Rice, wherein binder is polyvinyl butyral；Dispersing agent is castor oil；Plasticizer is dibutyl phthalate；Solvent is
Ethyl alcohol, defrother are n-butanol；The mass ratio of binder and Zirconium powder is 5:100；The matter of dispersing agent and Zirconium powder
Amount is than being 2:100；The mass ratio of plasticizer and Zirconium powder is 20:100；The mass ratio of solvent and Zirconium powder is
The mass ratio of 73.8:100, defrother and Zirconium powder is 0.3:100.
(2) casting machine is used to be cast zirconia ceramics slurry on release film with 1.8 ms/min of rate, wherein knife
Open height is 500 microns；Then wet base of the curtain coating on release film is spontaneously dried 45 minutes at room temperature, then at 48 DEG C
Lower drying 20 minutes, then drying 20 minutes at 58 DEG C, it is finally 45 minutes dry at 68 DEG C, obtain casting belt, wherein curtain coating
Band has the bottom surface opposite with release film and the outer surface opposite with bottom surface.
(3) release film is removed, and cuts out two blank from casting belt, the outer surface of two blank is fitted,
It is suppressed 20 minutes under 85 DEG C and 30MPa of pressure using warm water isostatic pressing machine, obtains green body.
(4) by green body with 0.8 DEG C/min of heating rate from room temperature to 600 DEG C, then with 3 DEG C/min of heating speed
Rate is warming up to 1480 DEG C, and heat preservation sintering 3 hours, is then cooled to 600 DEG C again with 8 DEG C/min of rate of temperature fall, last natural
It is cooling, obtain the zirconia ceramics piece with a thickness of 0.38 millimeter.
(5) zirconia ceramics piece is cut into required size, and grinding and buffing is incuded to a thickness of 0.08 millimeter
Identify the cover board of mould group.
The zirconia ceramics piece of the present embodiment is laser-cut into the circular sample that diameter is 2 feet, sample is placed
On marble measuring table, the flatness of the zirconia ceramics piece of the present embodiment is then measured using feeler gauge, obtains this implementation
The flatness of the zirconia ceramics piece of example is shown in Table 1.
The bending strength of the cover board of the induction identification mould group of the present embodiment is tested with the following method:
The cover board (15 × 6 × 0.08mm) of the induction identification mould group of the present embodiment is placed on universal testing machine special fixture
On, design parameter is as follows: compression bar diameter is φ 2.5mm, span 6mm, pushes speed 0.5mm/min, is pushed until ceramic segment
It splits, records breaking load F, and calculate bending strength according to the following formula: σ=3FL/ (2bd2), wherein σ bending strength in formula,
Units MPa；F maximum load, unit N；L span, unit mm；B specimen width, unit mm；D sample thickness, unit mm obtain this
The bending strength of the cover board of the induction identification mould group of embodiment is shown in Table 1.
The crystallite dimension of the zirconia ceramics piece of the present embodiment is tested with the following method:
Firstly, mirror effect is ground and is polished to sample；Then heat erosion is carried out, sample is put into Muffle furnace,
300 DEG C/h is warming up to heat erosion temperature, keeps the temperature furnace cooling after 10~30min, sintering temperature of this heat erosion temperature than ceramics
Spend low 300~400 DEG C.After heat erosion, obtains size of microcrystal and analyze sample.
Then, Electronic Speculum observation is scanned to sample after heat erosion, arbitrarily chooses 2~3 positions and amplifies 10000 times of bats
Stereoscan photograph is taken the photograph, describes the circle of area (A) on photo, by following formula by the number of die n in justifyingcWith the crystalline substance of circumference
Grain number niFind out the number of die N of per unit areaG, formula are as follows: NG=(nc+1/2ni) /(A/100002)。
Wherein, 1/NGFor area shared by 1 crystal grain.Thus equivalent circle diameter (D) is calculated as flat using following formula
Equal diameter, formula are as follows: D=2/ (π NG)1/2。
The crystallite dimension for obtaining the zirconia ceramics piece of the present embodiment is shown in Table 1.
Embodiment 2
The preparation process of the cover board of the induction identification mould group of the present embodiment is as follows:
(1) by Zirconium powder, solvent and dispersing agent ball milling mixing 3 hours, binder is then added, plasticizer continues ball
Mill 10 hours, is subsequently added into defrother, then ball milling 0.5 hour, and last vacuum defoamation 2 hours obtains viscosity and is 7.5Pas, consolidates
The zirconia ceramics slurry that phase mass percentage is 51.9%.Wherein, the median particle diameter of Zirconium powder be 0.5 micron~
0.6 micron, wherein binder is polyvinyl butyral；Dispersing agent is olein；Plasticizer is phthalic acid two
Butyl ester；Solvent is dimethylbenzene, and defrother is n-butanol；The mass ratio of binder and Zirconium powder is 10:100；Dispersing agent with
The mass ratio of Zirconium powder is 0.5:100；The mass ratio of plasticizer and Zirconium powder is 25:100；Solvent and zirconia powder
The mass ratio of body is 79.6:100, and the mass ratio of defrother and Zirconium powder is 0.5:100.
(2) casting machine is used to be cast zirconia ceramics slurry on release film with 1.5 ms/min of rate, wherein knife
Open height is 380 microns；Then wet base of the curtain coating on release film is spontaneously dried 30 minutes at room temperature, then at 45 DEG C
Lower drying 30 minutes, then drying 15 minutes at 60 DEG C, it is finally 60 minutes dry at 65 DEG C, obtain casting belt, wherein curtain coating
Band has the bottom surface opposite with release film and the outer surface opposite with bottom surface.
(3) release film is removed, and cuts out two blank from casting belt, the outer surface of two blank is fitted,
It is suppressed 30 minutes under 80 DEG C and 20MPa of pressure using warm water isostatic pressing machine, obtains green body.
(4) by green body with 0.5 DEG C/min of heating rate from room temperature to 500 DEG C, then with 2 DEG C/min of heating speed
Rate is warming up to 1450 DEG C, and heat preservation sintering 4 hours, is then cooled to 500 DEG C again with 10 DEG C/min of rate of temperature fall, finally certainly
It is so cooling, obtain the zirconia ceramics piece with a thickness of 0.3 millimeter.
(5) zirconia ceramics piece is cut into required size, and grinding and buffing is incuded to a thickness of 0.08 millimeter
Identify the cover board of mould group.
It tests to obtain the flatness and crystal grain of the zirconia ceramics piece of the present embodiment using the identical test method of embodiment 1
Size, and induction identify that the bending strength of the cover board of mould group is shown in Table 1.
Embodiment 3
The preparation process of the cover board of the induction identification mould group of the present embodiment is as follows:
(1) by Zirconium powder, solvent and dispersing agent ball milling mixing 5 hours, binder is then added, plasticizer continues ball
Mill 5 hours is subsequently added into defrother, then ball milling 1 hour, and last vacuum defoamation 1.5 hours, obtaining viscosity is 7Pas, solid phase
The zirconia ceramics slurry that mass percentage is 51.9%.Wherein, the partial size of Zirconium powder is 0.5 micron~0.6 micron,
Wherein, binder is polyvinyl butyral；Dispersing agent is phosphate；Plasticizer is polyethylene glycol；Solvent is dimethylbenzene, de-bubble
Agent is n-butanol；The mass ratio of binder and Zirconium powder is 8:100；The mass ratio of dispersing agent and Zirconium powder is 1:
100；The mass ratio of plasticizer and Zirconium powder is 30:100；The mass ratio of solvent and Zirconium powder is 81.2:100, is removed
The mass ratio of infusion and Zirconium powder is 0.1:100.
(2) casting machine is used to be cast zirconia ceramics slurry on release film with 2 ms/min of rate, wherein the edge of a knife
Height is 380 microns；Then wet base of the curtain coating on release film is spontaneously dried 60 minutes at room temperature, then at 50 DEG C
It is 15 minutes dry, then drying 30 minutes at 55 DEG C, it is finally 30 minutes dry at 70 DEG C, obtain casting belt, wherein casting belt
With the bottom surface opposite with release film and the outer surface opposite with bottom surface.
(3) release film is removed, and cuts out two blank from casting belt, the outer surface of two blank is fitted,
It is suppressed 10 minutes under 90 DEG C and 50MPa of pressure using warm water isostatic pressing machine, obtains green body.
(4) by green body with 1 DEG C/min of heating rate from room temperature to 600 DEG C, then with 5 DEG C/min of heating rate
1500 DEG C, and heat preservation sintering 2 hours are warming up to, are then cooled to 600 DEG C again with 5 DEG C/min of rate of temperature fall, it is last naturally cold
But, the zirconia ceramics piece with a thickness of 0.29 millimeter is obtained.
(5) zirconia ceramics piece is cut into required size, and grinding and buffing is incuded to a thickness of 0.2 millimeter
Identify the cover board of mould group.
It tests to obtain the flatness and crystal grain of the zirconia ceramics piece of the present embodiment using the identical test method of embodiment 1
Size, and induction identify that the bending strength of the cover board of mould group is shown in Table 1.
Embodiment 4
The preparation process of the cover board of the induction identification mould group of the present embodiment is as follows:
(1) by Zirconium powder, solvent and dispersing agent ball milling mixing 4.5 hours, binder is then added, plasticizer continues
Ball milling 7 hours, it is subsequently added into defrother, then ball milling 1 hour, last vacuum defoamation 1 hour obtains viscosity and is 5.2Pas, consolidates
The zirconia ceramics slurry that phase mass percentage is 50.9%.Wherein, the median particle diameter of Zirconium powder be 0.5 micron~
0.6 micron, wherein binder is polyvinyl butyral；Dispersing agent is herring oil；Plasticizer is polyethylene glycol (PEG)；Solvent
For toluene, defrother is n-butanol；The mass ratio of binder and Zirconium powder is 10:100；Dispersing agent and Zirconium powder
Mass ratio is 1:100；The mass ratio of plasticizer and Zirconium powder is 10:100；The mass ratio of solvent and Zirconium powder is
The mass ratio of 84.6:100, defrother and Zirconium powder is 0.4:100.
(2) casting machine is used to be cast zirconia ceramics slurry on release film with 1.9 ms/min of rate, wherein knife
Open height is 300 microns；Then wet base of the curtain coating on release film is spontaneously dried 40 minutes at room temperature, then at 47 DEG C
Lower drying 22 minutes, then drying 20 minutes at 56 DEG C, it is finally 35 minutes dry at 69 DEG C, obtain casting belt, wherein curtain coating
Band has the bottom surface opposite with release film and the outer surface opposite with bottom surface.
(3) release film is removed, and cuts out two blank from casting belt, the outer surface of two blank is fitted,
It is suppressed 15 minutes under 82 DEG C and 40MPa of pressure using warm water isostatic pressing machine, obtains green body.
(4) by green body with 0.6 DEG C/min of heating rate from room temperature to 520 DEG C, then with 4 DEG C/min of heating speed
Rate is warming up to 1500 DEG C, and heat preservation sintering 3 hours, is then cooled to 520 DEG C again with 6 DEG C/min of rate of temperature fall, last natural
It is cooling, obtain the zirconia ceramics piece with a thickness of 0.21 millimeter.
(5) zirconia ceramics piece is cut into required size, and grinding and buffing is incuded to a thickness of 0.1 millimeter
Identify the cover board of mould group.
It tests to obtain the flatness and crystal grain of the zirconia ceramics piece of the present embodiment using the identical test method of embodiment 1
Size, and induction identify that the bending strength of the cover board of mould group is shown in Table 1.
Embodiment 5
The preparation process of the cover board of the induction identification mould group of the present embodiment is as follows:
(1) by Zirconium powder, solvent and dispersing agent ball milling mixing 4 hours, binder is then added, plasticizer continues ball
Mill 8 hours is subsequently added into defrother, then ball milling 1 hour, and last vacuum defoamation 1 hour, obtaining viscosity is 3Pas, solid phase matter
Measure the zirconia ceramics slurry that percentage composition is 55%.Wherein, the median particle diameter of Zirconium powder is 0.5 micron~0.6 micron,
Wherein, binder is polyvinyl butyral；Dispersing agent is triethylamine and castor oil；Plasticizer be dibutyl phthalate and
Glycerol；Solvent is butanone, and defrother is n-butanol；The mass ratio of binder and Zirconium powder is 5:100；Dispersing agent and oxidation
The mass ratio of zirconium powder body is 2:100；The mass ratio of plasticizer and Zirconium powder is 20:100；The matter of solvent and Zirconium powder
Ratio is measured as 73.8:100, the mass ratio of defrother and Zirconium powder is 0.3:100.
(2) casting machine is used to be cast zirconia ceramics slurry on release film with 1.8 ms/min of rate, wherein knife
Open height is 500 microns；Then wet base of the curtain coating on release film is spontaneously dried 45 minutes at room temperature, then at 48 DEG C
Lower drying 20 minutes, then it is 20 minutes dry at 58 DEG C, it is finally 45 minutes dry at 68 DEG C, obtain casting belt, wherein curtain coating belt
There are the bottom surface opposite with release film and the outer surface opposite with bottom surface.
(3) release film is removed, and cuts out two blank from casting belt, the outer surface of two blank is fitted,
It is suppressed 20 minutes under 85 DEG C and 30MPa of pressure using warm water isostatic pressing machine, obtains green body.
(4) by green body with 0.8 DEG C/min of heating rate from room temperature to 600 DEG C, then with 3 DEG C/min of heating speed
Rate is warming up to 1480 DEG C, and heat preservation sintering 3 hours, is then cooled to 600 DEG C again with 8 DEG C/min of rate of temperature fall, last natural
It is cooling, obtain the zirconia ceramics piece with a thickness of 0.3 millimeter.
(5) zirconia ceramics piece is cut into required size, and grinding and buffing is incuded to a thickness of 0.08 millimeter
Identify the cover board of mould group.
It tests to obtain the flatness and crystal grain of the zirconia ceramics piece of the present embodiment using the identical test method of embodiment 1
Size, and induction identify that the bending strength of the cover board of mould group is shown in Table 1.
Comparative example 1
The preparation process of the cover board of the induction identification mould group of comparative example 1 is as follows:
(1) by Zirconium powder, solvent and dispersing agent ball milling mixing 4 hours, binder is then added, plasticizer continues ball
Mill 8 hours is subsequently added into defrother, then ball milling 1 hour, and last vacuum defoamation 1 hour, obtaining viscosity is 8.3Pas, solid phase
The zirconia ceramics slurry that mass percentage is 55%.Wherein, the median particle diameter of Zirconium powder is 0.5 micron~0.6 micro-
Rice, wherein binder is polyvinyl butyral；Dispersing agent is castor oil；Plasticizer is dibutyl phthalate；Solvent is
Ethyl alcohol, defrother are n-butanol；The mass ratio of binder and Zirconium powder is 5:100；The matter of dispersing agent and Zirconium powder
Amount is than being 2:100；The mass ratio of plasticizer and Zirconium powder is 20:100；The mass ratio of solvent and Zirconium powder is
The mass ratio of 73.8:100, defrother and Zirconium powder is 0.3:100.
(2) casting machine is used to be cast zirconia ceramics slurry on release film with 1.8 ms/min of rate, wherein knife
Open height is 1000 microns；Then wet base of the curtain coating on release film is spontaneously dried 60 minutes at room temperature, then at 48 DEG C
Lower drying 40 minutes, then it is 30 minutes dry at 58 DEG C, it is finally 30 minutes dry at 68 DEG C.
(3) release film is removed, and cuts out green body from casting belt.
(4) by green body with 0.8 DEG C/min of heating rate from room temperature to 600 DEG C, then with 3 DEG C/min of heating speed
Rate is warming up to 1480 DEG C, and heat preservation sintering 3 hours, is then cooled to 600 DEG C again with 8 DEG C/min of rate of temperature fall, last natural
It is cooling, obtain the sintered sheets of first sintering.
(5) phenomena such as generally having warpage and curved edge due to the sintered sheets after first sintering, needing will for the first time
The sintered sheets of sintering carry out second and are sintered: applying 5g/cm2Under conditions of pressure, 1430 DEG C heat preservation sintering 2 hours, into
Second of sintering of row, obtains the zirconia ceramics piece that final thickness is 0.37 millimeter.
(5) zirconia ceramics piece is cut into required size, and grinding and buffing is incuded to a thickness of 0.08 millimeter
Identify the cover board of mould group.
It tests to obtain the flatness and crystal grain of the zirconia ceramics piece of comparative example 1 using the identical test method of embodiment 1
Size, and induction identify that the bending strength of the cover board of mould group is shown in Table 1.
Table 1 is the flatness and crystallite dimension of the zirconia ceramics piece of Examples 1 to 5 and comparative example 1, and induction identification
The bending strength of the cover board of mould group.
Table 1
From table 1 it follows that the flatness of the zirconia ceramics piece of Examples 1 to 5 is only at most 0.04mm, at least may be used
Up to 0.02mm, and the flatness of the zirconia ceramics piece of comparative example 1 is up to 0.06mm, the significantly larger than oxidation of Examples 1 to 5
The flatness of zircon ceramic piece, it is clear that the zirconia ceramics piece of the method preparation of Examples 1 to 5 is more smooth.
It can also be seen that the bending strength of the cover board of the induction identification mould group of Examples 1 to 5 is at least from table 1
950MPa reaches as high as 1100MPa, the significantly larger than bending strength of the cover board of the induction identification mould group of comparative example 1, it is clear that real
The cover board for applying the induction identification mould group of the method preparation of example 1~5 has higher bending strength.
And it can also be seen that the crystallite dimension of the zirconia ceramics piece of Examples 1 to 5 is at most only 0.8 micro- from table 1
Rice, and the crystallite dimension of the zirconia ceramics piece of comparative example 1 is 1.3 microns, the significantly larger than zirconia ceramics of Examples 1 to 5
The crystallite dimension of piece, this is because the zirconia ceramics piece of Examples 1 to 5 has smaller crystallite dimension.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of zirconia ceramics piece, which comprises the steps of:
By zirconia ceramics slurry curtain coating on release film, then through drying, obtain casting belt, wherein the casting belt have with
The opposite bottom surface of the release film and the outer surface opposite with the bottom surface；
Blank is cut out from the casting belt, the outer surface of two blank is fitted, and compression moulding, obtains base
Body；
By the blank sintering, obtain zirconia ceramics piece, wherein the zirconia ceramics piece with a thickness of 0.2 millimeter~0.4
Millimeter.
2. the preparation method of zirconia ceramics piece according to claim 1, which is characterized in that further include the zirconium oxide pottery
The preparation step of porcelain slurry: Zirconium powder, solvent, dispersing agent, binder and plasticizer are mixed, and obtaining viscosity is 1Pas
~10Pas, solid phase mass percentage be 50%~55% the zirconia ceramics slurry.
3. the preparation method of zirconia ceramics piece according to claim 2, which is characterized in that the grain of the Zirconium powder
Diameter is 0.5 micron~0.6 micron.
4. the preparation method of zirconia ceramics piece according to claim 1, which is characterized in that starch the zirconia ceramics
Stream prolong on the release film after drying steps are as follows: wet base of the curtain coating on the release film is done naturally at room temperature
It is dry 30 minutes~60 minutes, then 15 minutes~30 minutes dry at 45 DEG C~50 DEG C, then dry 15 at 55 DEG C~60 DEG C
Minute~30 minutes, it is finally 30 minutes~60 minutes dry at 65 DEG C~70 DEG C.
5. the preparation method of zirconia ceramics piece according to claim 1, which is characterized in that by the outer of two blank
The method of compression moulding after surface fits is the static pressure such as warm water, and the press temperature is 80 DEG C~90 DEG C, pressure 20MPa
~50MPa, dwell time are 10 minutes~30 minutes.
6. the preparation method of zirconia ceramics piece according to claim 1, which is characterized in that by the step of the blank sintering
Suddenly are as follows: by the green body with 0.5 DEG C/min~1 DEG C/min of heating rate from room temperature to 500 DEG C~600 DEG C, then with 2
DEG C/min~5 DEG C/min of heating rate is warming up to 1450 DEG C~1500 DEG C, and heat preservation sintering 2 hours~4 hours, then again
500 DEG C~600 DEG C are cooled to 5 DEG C/min~10 DEG C/min of rate of temperature fall, last natural cooling.
7. the oxidation that a kind of preparation method of zirconia ceramics piece described in any one according to claim 1~6 is prepared
Zircon ceramic piece.
8. a kind of preparation method of the cover board of induction identification mould group, which comprises the steps of:
Zirconia ceramics piece as claimed in claim 7 is provided；
The zirconia ceramics piece is cut, grinding and buffing, obtains the cover board of the induction identification mould group.
9. a kind of induction identification mould that the preparation method of the cover board of induction identification mould group according to claim 8 is prepared
The cover board of group.
10. application of the cover board of induction identification mould group as claimed in claim 9 in mobile phone or tablet computer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611111593.4A CN106588003B (en) | 2016-12-06 | 2016-12-06 | The cover board and its preparation method and application of zirconia ceramics piece and preparation method thereof and induction identification mould group |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611111593.4A CN106588003B (en) | 2016-12-06 | 2016-12-06 | The cover board and its preparation method and application of zirconia ceramics piece and preparation method thereof and induction identification mould group |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106588003A CN106588003A (en) | 2017-04-26 |
| CN106588003B true CN106588003B (en) | 2019-06-28 |
Family
ID=58596274
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611111593.4A Active CN106588003B (en) | 2016-12-06 | 2016-12-06 | The cover board and its preparation method and application of zirconia ceramics piece and preparation method thereof and induction identification mould group |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106588003B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975909B (en) * | 2017-06-02 | 2021-04-06 | 东莞华晶粉末冶金有限公司 | Annealing method of zirconia ceramic blank and preparation method of zirconia ceramic |
| CN109020540B (en) * | 2017-06-08 | 2021-04-30 | 中国科学院宁波材料技术与工程研究所 | Sintering method of dense oxide ceramic body |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104446457A (en) * | 2014-11-18 | 2015-03-25 | 潮州三环（集团）股份有限公司 | Modified zirconium oxide ceramic material and application thereof |
| CN104844198A (en) * | 2014-02-18 | 2015-08-19 | 清华大学 | Hand-held terminal product appearance ceramic thin type member and production method thereof |
| CN104892007A (en) * | 2015-05-06 | 2015-09-09 | 广东风华高新科技股份有限公司 | Ceramic substrate preparation method |
| CN105459516A (en) * | 2014-08-28 | 2016-04-06 | 比亚迪股份有限公司 | Ceramic substrate and preparation method thereof, and power module |
| CN205692182U (en) * | 2016-05-26 | 2016-11-16 | 郑州中瓷科技有限公司 | A kind of zirconia ceramics fingerprint recognition cover plate |
-
2016
- 2016-12-06 CN CN201611111593.4A patent/CN106588003B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104844198A (en) * | 2014-02-18 | 2015-08-19 | 清华大学 | Hand-held terminal product appearance ceramic thin type member and production method thereof |
| CN105459516A (en) * | 2014-08-28 | 2016-04-06 | 比亚迪股份有限公司 | Ceramic substrate and preparation method thereof, and power module |
| CN104446457A (en) * | 2014-11-18 | 2015-03-25 | 潮州三环（集团）股份有限公司 | Modified zirconium oxide ceramic material and application thereof |
| CN104892007A (en) * | 2015-05-06 | 2015-09-09 | 广东风华高新科技股份有限公司 | Ceramic substrate preparation method |
| CN205692182U (en) * | 2016-05-26 | 2016-11-16 | 郑州中瓷科技有限公司 | A kind of zirconia ceramics fingerprint recognition cover plate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106588003A (en) | 2017-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110304920B (en) | Zirconia ceramic, preparation method thereof, shell and electronic equipment | |
| CN108640678B (en) | Black zirconia ceramic material, preparation method of black zirconia ceramic and product | |
| CN104844198B (en) | Hand-held terminal product appearance ceramic thin type member and production method thereof | |
| JP5661278B2 (en) | Method for producing refractory metal molded body | |
| JP6636515B2 (en) | Transparent spinel article and tape forming method for producing the same | |
| CN100519475C (en) | Method of preparing zirconium oxide ceramic by curtain coating method and product obtained by using the method | |
| CN106588003B (en) | The cover board and its preparation method and application of zirconia ceramics piece and preparation method thereof and induction identification mould group | |
| JPS6259564A (en) | Molding aid for ceramics, molded body obtained using the same and production of ceramic product | |
| CN110655401A (en) | Zirconia ceramic material, zirconia ceramic structural member and preparation method thereof | |
| CN110330358A (en) | A kind of porous alumina ceramic plate and preparation method thereof | |
| CN104844224A (en) | Non-aqueous tape casting method for preparing laminar composite transparent ceramic | |
| CN108218422A (en) | Wear-resistant ceramic tape casting slurry and its application process | |
| CN106778553B (en) | Cover plate of induction identification module and preparation method and application thereof | |
| Nunn et al. | Tensile strength of dried gelcast green bodies | |
| KR101630826B1 (en) | manufacturing method of high strength ceramic sheet for firing electronic ceramic and high strength ceramic sheet manufactured by the same | |
| CN111499377A (en) | Piezoelectric ceramic and preparation method thereof | |
| KR101950411B1 (en) | The Diamond polisher abrasive for dental prosthesis and manufacturing method thereof | |
| KR101436468B1 (en) | High strength Aluminum Nitride ceramics and the method of low temperature sintering thereof | |
| CN110759731B (en) | Mobile phone rear cover and preparation method thereof | |
| CN101266854A (en) | A method for making ZnO base voltage sensitive resistor | |
| CN106348751B (en) | Preparation method of fingerprint identification module ceramic cover plate | |
| CN109796197A (en) | The preparation method of one type mono-crystalline structures alumina transparent ceramic | |
| CN115611639B (en) | Silicon wafer casting slurry and silicon wafer forming method | |
| CN115650759B (en) | Porous alumina ceramic sheet applied to gas sensor packaging and preparation method thereof | |
| CN106631035A (en) | Composite ceramic and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 518000, Shenzhen, Guangdong province Baoan District manhole street new two community Nanling Road, No. 21, B building on the first floor, two floor Applicant after: Shenzhen City, Germany and advanced ceramics Limited by Share Ltd Address before: 518000, Shenzhen, Guangdong province Baoan District manhole street new two community Nanling Road, No. 21, B building on the first floor, two floor Applicant before: Shenzhen Shangde Advanced Ceramic Co., Ltd. |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |