CN108863353A - black ceramic material and preparation method thereof - Google Patents
black ceramic material and preparation method thereof Download PDFInfo
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- CN108863353A CN108863353A CN201810687912.9A CN201810687912A CN108863353A CN 108863353 A CN108863353 A CN 108863353A CN 201810687912 A CN201810687912 A CN 201810687912A CN 108863353 A CN108863353 A CN 108863353A
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Abstract
The invention discloses black ceramic materials and preparation method thereof.The preparation method of above-mentioned black ceramic material, includes the following steps：S1, ceramic green is made in ceramic raw material；S2, it the ceramic green is placed in dumping equipment carries out dumping, the dumping equipment is warming up to 900 DEG C -1200 DEG C with the speed of 0.1 DEG C/min-10 DEG C/min, keeps the temperature 0.5h-3h, obtains biscuit of ceramics；S3, it the biscuit of ceramics and carbonaceous material is collectively disposed in vacuum sintering furnace is sintered nigrescence, vacuum-sintering stove evacuation, and 1400 DEG C -1550 DEG C are warming up to the speed of 1 DEG C/min-10 DEG C/min, 0.5h-8h is kept the temperature, obtains blackness high (2.5 or less L value), without stain and the pure black zirconia ceramics material of color development.The preparation method of black ceramic material of the present invention, the black ceramic blackness prepared is high and pure, uniformly pure without stain, color development.
Description
Technical field
The present invention relates to technical field of ceramic material, and in particular to black ceramic material and preparation method thereof.
Background technique
Ceramic material is more and more since it has the characteristics that high tenacity, high-flexural strength, high-wearing feature, waterproof, antirust
Ground substitutes the materials such as metal, is applied to the multiple fields such as cell phone rear cover, mold.
Welcome of the ceramic material as cell phone rear cover increasingly by consumer and businessman, ceramic material is also more next in recent years
It is applied on the products such as cell phone rear cover, fingerprint piece more.Zirconium oxide, alumina ceramic material true qualities are usually white, and
Certain occasions, such as the mobile phone of black shell then need to black ceramic material, are fabricated to the ceramics of black.Current pottery
The black ceramic material that porcelain blackening is made into has many non-uniform stains, while it is rubescent or whiten etc. and to lack product easily occur
It falls into, blackness is not high and not pure enough, causes product yield low, and competitiveness is low, is difficult to meet consumer for blackness height and send out
The demand of the positive product of colour purity.
Summary of the invention
Based on this, the present invention is it is necessary to provide a kind of preparation method of black ceramic material, the black ceramic prepared
It is uniformly pure without stain, blackness height, color development, and preparation section is less, method is easy.
The present invention there is a need to provide a kind of black ceramic material.
In order to achieve the object of the present invention, the present invention uses following technical scheme：
A kind of preparation method of black ceramic material comprising following steps：
S1, ceramic raw material is prepared into slurry, and is shaped to ceramic green；
S2, the ceramic green be placed in dumping equipment carry out dumping, the dumping equipment be gradually warming up to 900 DEG C-
1200 DEG C, 0.5h-3h is kept the temperature, biscuit of ceramics is obtained；
S3, it the biscuit of ceramics and carbonaceous material is collectively disposed in vacuum sintering furnace is sintered nigrescence, the vacuum
It is sintered stove evacuation, and is gradually warming up to 1400 DEG C -1550 DEG C, 0.5h-8h is kept the temperature, obtains black ceramic material.
The preparation method of above-mentioned black ceramic material is gradually warming up to 900 DEG C -1200 after being fabricated to ceramic green
DEG C carry out dumping, relative density ceramic at this time in 60%-80%, be then gradually warming up under vacuum conditions 1400 DEG C-
1550 DEG C of nigrescence sintering, the black ceramic made black uniformly, and blackness is high and pure, and without stain, blackness is high, color development is pure
Just, appearance meets the requirements；And process is less, and preparation method is easy.
In some of embodiments, the step S1 is specifically：Ceramic powder is subjected to ball milling, adds solvent, dispersion
The raw materials such as agent, adhesive, obtain ceramic slurry, carry out deaeration processing to the ceramic slurry, are then prepared by the tape casting
Ceramic green.
In some of embodiments, the step S1 is specifically：Ceramic powder is subjected to ball milling, adds solvent, dispersion
The raw materials such as agent, adhesive obtain ceramic slurry, are then granulated, by dry-pressing formed for ceramic green.
In some of embodiments, the step S1 is specifically：Ceramic powder and injection molding are subjected to mixing with sizing material, obtained
Feeding is injected, then by feeding by injection moulding, then is placed in kerosene solvent and steeps oily degreasing, degreasing preset time is made pottery
Porcelain green compact.
In some of embodiments, in the step S2：The heating rate of the dumping equipment be 0.1 DEG C/min-10 DEG C/
min。
In some of embodiments, in the step S3：The carbonaceous material is graphite load bearing board.
In some of embodiments, the step S3 is specially：The biscuit of ceramics is replaced into superposition with graphite load bearing board
Together, be placed in vacuum sintering furnace and be sintered nigrescence, the vacuum-sintering stove evacuation, and be gradually warming up to 1400 DEG C-
1550 DEG C, 0.5h-8h is kept the temperature, black ceramic material is obtained.
In some of embodiments, in the step S3, the heating rate of the vacuum sintering furnace is 1 DEG C/min-10 DEG C/
min。
In some of embodiments, between the step S1 and S2, also there is S10 step：The ceramic green is punched
At preset shape.
In some of embodiments, after the step S3, also there is S30 step：The black ceramic material is carried out
Surface treatment, the surface treatment are one such or several including polishing, polishing, cleaning, examining.
The present invention also provides a kind of black ceramic materials, are made of the preparation method of the black ceramic material.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of black ceramic material described in one embodiment of the invention；
Fig. 2 is biscuit of ceramics and graphite load bearing board in the preparation method of black ceramic material described in one embodiment of the invention
It is superimposed one of schematic diagram；
Fig. 3 is biscuit of ceramics and graphite load bearing board in the preparation method of black ceramic material described in one embodiment of the invention
It is superimposed the two of schematic diagram；
Fig. 4 is biscuit of ceramics and graphite load bearing board in the preparation method of black ceramic material described in one embodiment of the invention
It is superimposed the three of schematic diagram.
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 presently preferred embodiments of the present invention.But the invention can be realized in many different forms, however it is not limited to this paper institute
The embodiment of description.On the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more thorough
Comprehensively.
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.
Fig. 1 is please referred to, the present invention provides a kind of preparation method of black ceramic material comprising following steps：
S1, ceramic green is made in ceramic raw material；
S2, it ceramic green is placed in dumping equipment carries out dumping, dumping equipment is gradually warming up to 900 DEG C -1200 DEG C, protects
Warm 0.5h-3h, obtains biscuit of ceramics；Heating rate is preferably 0.1 DEG C/min-10 DEG C/min, and soaking time is preferably 1h-2h.
900 DEG C of -1200 DEG C of progress dumpings are gradually warming up to, ceramic relative density is in 60%-80% at this time；The suitable heating speed of selection
Degree and soaking time carry out dumping process slowly gradually, and dumping is cleaner, can reduce sintered stain.
S3, it biscuit of ceramics 10 and carbonaceous material 20 is collectively disposed in vacuum sintering furnace is sintered nigrescence, vacuum-sintering
Stove evacuation, and 1400 DEG C -1550 DEG C are gradually warming up to, 0.5h-8h is kept the temperature, black ceramic material is obtained.Vacuum sintering furnace
Heating rate is preferably 1 DEG C/min-10 DEG C/min, and soaking time is preferably 2h-5h.When selecting suitable heating rate and heat preservation
Between reaction can be sufficiently carried out so that blacking more evenly, sintered stain can be reduced, the black made pottery
Porcelain blacks uniformly, and blackness is high and pure, and without stain, appearance meets the requirements.
Step S1 wherein specifically can be：Ceramic powder is subjected to ball milling, adds solvent, dispersing agent, adhesive etc.
Raw material obtains ceramic slurry, carries out deaeration processing to ceramic slurry, is then prepared into ceramic green by the tape casting.Ceramic powder
Body can be the ceramic materials such as zirconium oxide, aluminium oxide and its combination, be ceramic powder for example, by using yttrium stable zirconium oxide.Solvent can
To be ethyl alcohol, glycerine, acetone equal solvent；Dispersing agent can be phosphate, fish oil etc.；Adhesive is polyethylene, polyvinyl alcohol
Butyral and/or polymethyl methacrylate.
Step S1 wherein specifically can also be：Ceramic powder is subjected to ball milling, adds solvent, dispersing agent, adhesive
Equal raw materials, obtain ceramic slurry, are then granulated, by dry-pressing formed for ceramic green.The method of granulation can be spraying
It is granulated；The pressure of 60MPa-90MPa, pressure maintaining 3min-120min can be used when dry-pressing formed.Different ceramic thickness is using different
Pressure and the dwell time.
Step S1 wherein specifically can also be：Ceramic powder and injection molding are subjected to mixing with sizing material, obtain injection feeding,
Then it by feeding by injection moulding, then is placed in kerosene solvent and steeps oily degreasing, degreasing preset time degreasing obtains ceramic green
Base.Degreasing time therein is 10h-14h, preferably 12h.
In step S3：Carbonaceous material is graphite load bearing board.It is to be appreciated that the carbonaceous material is also possible to other materials
Material, is not limited to graphite.
Step S3 is specially：Biscuit of ceramics 10 is replaced with graphite load bearing board 20 and is superimposed, vacuum sintering furnace is placed in
In be sintered nigrescence, vacuum-sintering stove evacuation, and be warming up to 1400 DEG C -1550 with the speed of 1 DEG C/min-10 DEG C/min
DEG C, 0.5h-8h is kept the temperature, black ceramic material is obtained.
Between step S1 and S2, also there is S10 step：Ceramic green is punched into preset shape.Such as when ceramic material
When material prepares fingerprint piece, ceramic green is punched into disc-shaped；When ceramic material prepares ceramic rear cover, it is punched into plate.
After step S3, also there is S30 step：Black ceramic material is surface-treated, which includes beating
Grind, polish, cleaning, examine it is one such or several.After being surface-treated, black ceramic can make directly as product
With.
Referring to figure 2. to Fig. 4, the stacking method of biscuit of ceramics 10 and graphite material 20 is for example：Referring to figure 2., 1, ceramics
Biscuit 10 is placed on graphite plate 20, is then overlapped.2, referring to figure 3., several graphite plates are connected to one by graphite column
It rises, biscuit of ceramics 10 is stacked between two graphite plates 20.3, referring to figure 4., biscuit of ceramics 10 is stacked in two graphite plates 20
Between, successively it is overlapped.It is to be appreciated that being not limited to there are many stacked systems of biscuit of ceramics 10 and graphite material 20
State stacked system.
The preparation method of above-mentioned black ceramic material is gradually warming up to 900 DEG C -1200 after being fabricated to ceramic green
DEG C carry out dumping, relative density ceramic at this time in 60%-80%, be then gradually warming up under vacuum conditions 1400 DEG C-
1550 DEG C of nigrescence sintering, the black ceramic made black uniformly, and blackness is high and pure, and without stain, appearance meets the requirements；
And process is less, and preparation method is easy.
Hereinafter embodiments of the present invention will be further illustrated by several embodiments：
Embodiment one
The present invention provides a kind of preparation method of black ceramic fingerprint piece comprising following steps：Select following mass parts
Ceramic raw material：99.75 parts of yttrium stable zirconium oxide powder (yttrium oxide molar content is less than 3%), 0.25 part of nano alumina powder, second
Pure and mild isopropanol is with 2：0.8 part of 55 parts of solvent, fish oil dispersant, the polyvinylbutyral binder 10 that 1 volume ratio is made into
Part, wherein the D50 partial size of zirconia powder is 0.24um, specific surface area 10.2m2/g；Ball mill is added in above-mentioned raw materials, with 90r/
The speed of min carries out ball milling, is prepared into ceramic slurry, carries out deaeration processing to ceramic slurry, is prepared into ceramics by the tape casting
Green compact；It is in disc-shaped by ceramic green punching；Ceramic green is placed in dumping equipment, dumping equipment is adjusted, with 0.5 DEG C/min
Speed be warming up to 1000 DEG C, 1h is kept the temperature after heating, to carry out dumping, obtains biscuit of ceramics；Biscuit of ceramics and graphite plate are handed over
It for superposition, is placed in vacuum sintering furnace, to vacuum-sintering stove evacuation, adjusts temperature, be warming up to 1450 with the speed of 5 DEG C/min
DEG C, 4h is kept the temperature, ceramic green is reacted with the carbon in graphite, obtains black ceramic disk；CNC is carried out to black ceramic disk
Polishing deburring, obtains black ceramic fingerprint piece.The density for measuring black ceramic fingerprint piece is 6.08g/cm3, corresponding to Lab value is
2.00、-0.10、-0.14。
Embodiment two
The present embodiment provides a kind of preparation methods of black ceramic cell phone rear cover comprising following steps：Select following matter
Measure the ceramic raw material of part：(yttrium oxide molar content therein is 2.5% to 99.6 parts of yttrium stable zirconium oxide powder, and zirconium powder D50 partial size is
0.56um, powder specific surface area 9.7m2/g), 0.4 part of nano aluminium oxide, 0.5 part of CMC (sodium carboxymethylcellulose), PVA (poly- second
Enol) 4.5 parts, 0.5 part of PEG (polyethylene glycol)；Above-mentioned raw materials are subjected to ball milling with the speed of 70r/min, are prepared into ceramic slurry
Material, is granulated ceramic slurry, dry-pressing is carried out under the pressure of 80MPa, pressure maintaining 10min is prepared into ceramic green, then sets
Equal static pressure, pressure maintaining 5min are carried out under the pressure of 200MPa；Ceramic green is punched into preset plate body using die cutting device；
The ceramic green of plate is placed in dumping equipment, dumping equipment is adjusted, 1200 DEG C is warming up to the speed of 0.8 DEG C/min, rises
0.5h is kept the temperature after temperature, to carry out dumping, obtains biscuit of ceramics；Biscuit of ceramics is replaced into superposition with graphite plate, is placed in vacuum-sintering
In furnace, to vacuum-sintering stove evacuation, temperature is adjusted, 1500 DEG C is warming up to the speed of 10 DEG C/min, keeps the temperature 2h, biscuit of ceramics
It is reacted with the carbon in graphite, obtains black ceramic plate；CNC polishing deburring is carried out to black ceramic plate and is punched, is obtained black
Color ceramic mobile phone rear cover.Measuring sintering briquette density is 6.08g/cm3, corresponding Lab value is 2.19, -0.04, -0.09.
Embodiment three
The present embodiment provides a kind of preparation methods of the rectangular cover board of black ceramic comprising following steps：Select following matter
Measure the ceramic raw material of part：99.75 parts of yttrium stable zirconium oxide powder (molar content 2.8% of yttrium oxide, zirconium powder D50 partial size 0.15um,
Powder specific surface area 10.17m2/g), 0.25 part of nano aluminium oxide, paraffin：13 parts, stearic acid：1 part, polyethylene：2.4 parts, it is poly-
Propylene：2.6 parts, DOP1 parts：Ceramic raw material is proportionally added into mixer to mixing is at ceramic injection feeding, by feeding utilization side
The injection moulding of shape die for cover plate, raw material is in 190 DEG C of molding bases.Green compact are placed in kerosene solvent and steep oily degreasing, degreasing 12h；
The ceramic green of rectangular plate after degreasing is placed in dumping equipment, dumping equipment is adjusted, with the speed liter of 0.25 DEG C/min
Temperature keeps the temperature 1.5h to 1100 DEG C after heating, to carry out dumping, obtain biscuit of ceramics；Biscuit of ceramics is replaced into superposition with graphite plate,
It is placed in vacuum sintering furnace, to vacuum-sintering stove evacuation, adjusts temperature, be warming up to 1500 DEG C with the speed of 1 DEG C/min, heat preservation
2h, biscuit of ceramics are reacted with the carbon in graphite, obtain black ceramic square plate；CNC is carried out to black ceramic square plate to beat
Mill deburring is simultaneously cleaned, and the rectangular cover board of black ceramic is obtained.Measuring sintering briquette density is 6.08g/cm3, corresponding Lab value is 2.30 ,-
0.14、-0.20。
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect 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 black ceramic material, which is characterized in that include the following steps：
S1, ceramic raw material is prepared into ceramic green；
S2, it the ceramic green is placed in dumping equipment carries out dumping, the dumping equipment is gradually warming up to 900 DEG C -1200
DEG C, 0.5h-3h is kept the temperature, biscuit of ceramics is obtained；
S3, it the biscuit of ceramics and carbonaceous material is collectively disposed in vacuum sintering furnace is sintered nigrescence, the vacuum-sintering
Stove evacuation, and 1400 DEG C -1550 DEG C are gradually warming up to, 0.5h-8h is kept the temperature, black ceramic material is obtained.
2. the preparation method of black ceramic material according to claim 1, it is characterised in that：The step S1 is specifically：
Ceramic powder is subjected to ball milling, the raw materials such as solvent, dispersing agent, adhesive is added, obtains ceramic slurry, to the ceramic slurry
Deaeration processing is carried out, ceramic green is then prepared by the tape casting.
3. the preparation method of black ceramic material according to claim 1, it is characterised in that：The step S1 is specifically：
Ceramic powder is subjected to ball milling, adds the raw materials such as solvent, dispersing agent, adhesive, ceramic slurry is obtained, is then granulated,
By dry-pressing formed for ceramic green.
4. the preparation method of black ceramic material according to claim 1, it is characterised in that：The step S1 is specifically：
Ceramic powder and injection molding are subjected to mixing with sizing material, injection feeding is obtained, then by feeding by injection moulding, then is placed in kerosene
Oily degreasing is steeped in solvent, degreasing preset time obtains ceramic green.
5. the preparation method of black ceramic material according to claim 1, it is characterised in that：In the step S2：It is described
The heating rate of dumping equipment is 0.1 DEG C/min-10 DEG C/min.
6. the preparation method of black ceramic material according to claim 1, it is characterised in that：In the step S3：It is described
Carbonaceous material is graphite load bearing board.
7. the preparation method of black ceramic material according to claim 1 or 6, it is characterised in that：The step S3 is specific
For：The biscuit of ceramics is replaced with graphite load bearing board and is superimposed, is placed in vacuum sintering furnace and is sintered nigrescence, it is described
Vacuum-sintering stove evacuation, and 1400 DEG C -1550 DEG C are gradually warming up to, 0.5h-8h is kept the temperature, black ceramic material is obtained.
8. the preparation method of black ceramic material according to claim 1 or 6, it is characterised in that：In the step S3, institute
The heating rate for stating vacuum sintering furnace is 1 DEG C/min-10 DEG C/min.
9. the preparation method of black ceramic material according to claim 1, it is characterised in that：After the step S3, also
With S30 step：The black ceramic material is surface-treated, the surface treatment includes polishing, polishing, cleaning, inspection
It tests one such or several.
10. a kind of black ceramic material, which is characterized in that by the system of the described in any item black ceramic materials of claim 1-9
Preparation Method is made.
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| CN110615685A (en) * | 2019-10-09 | 2019-12-27 | 景德镇陶瓷大学 | Black ceramic and preparation method thereof |
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