CN109776090A - A kind of preparation method of 3D zirconia ceramics mobile phone backboard and the product of preparation - Google Patents
A kind of preparation method of 3D zirconia ceramics mobile phone backboard and the product of preparation Download PDFInfo
- Publication number
- CN109776090A CN109776090A CN201711129451.5A CN201711129451A CN109776090A CN 109776090 A CN109776090 A CN 109776090A CN 201711129451 A CN201711129451 A CN 201711129451A CN 109776090 A CN109776090 A CN 109776090A
- Authority
- CN
- China
- Prior art keywords
- zirconia ceramics
- sintering
- mobile phone
- cell phone
- additive
- 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.)
- Granted
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
It include: the additive of the Zirconium powder for 1) weighing 80-85 parts by weight, 15-20 parts by weight the present invention provides a kind of preparation method of 3D zirconia ceramics mobile phone backboard and its product of preparation, method；Additive includes: paraffin, polyethylene, polypropylene, vegetable oil, ethylene-vinyl acetate copolymer, oleic acid；2) weighed Zirconium powder and additive are kneaded, obtain mixing materials；3) mixing materials are injected into 3D molding die, obtain 3D zirconia ceramics cell phone back slab body；4) 3D zirconia ceramics cell phone back slab body is immersed in organic solvent and carries out degreasing, be fitted into after degreasing in draft glue discharging furnace and carry out dumping；5) it is fitted into after dumping in sintering furnace and carries out high temperature sintering；6) it is packed into after being sintered in sizing sintering smelting tool and carries out shaping sintering, obtain 3D zirconia ceramics mobile phone backboard.Using the technology of the present invention, the angularity of 3D zirconia ceramics mobile phone backboard can be reduced to 0.03mm or less.
Description
Technical field
The present invention relates to ceramic technology fields, a kind of preparation method more particularly to 3D zirconia ceramics mobile phone backboard and
Its product prepared.
Background technique
With the development of electronic technology, the electronic component in electronic equipment, such as mobile phone is more and more, therefore in mobile phone
Contact between each electronic component in portion is also increasingly closer, and the effect of mobile phone backboard (also referred to as mobile phone battery cover) is exactly to protect
Mobile phone is from from extraneous injury, therefore, mobile phone backboard plays the role of also more and more crucial in mobile phone.As cell phone back
Plate, it is desirable that its material shields less electronic signal, intensity wants high, followed by aesthetic requirement.Similarly, other electronic equipments
Backboard required there is also same.Therefore ceramic mobile phone backboard is widely used, electronic signal is shielded less by it,
Intensity is high, hardness is high, it is wear-resistant, be not easy feature dirty, in beautiful color.Zirconia ceramics mobile phone backboard can be used as electronic equipment
Backboard, especially mobile phone backboard.There are three types of mobile phone backboard is usual, 2D zirconia ceramics mobile phone backboard, 2.5D zirconia ceramics
Mobile phone backboard and 3D zirconia ceramics mobile phone backboard.2D zirconia ceramics mobile phone backboard refers to plate zirconia ceramics cell phone back
Plate；3D zirconia ceramics mobile phone backboard refers to that each crest line is polished into the plate zirconia ceramics cell phone back of circular arc chamfering
Plate；3D zirconia ceramics mobile phone backboard refers to by four zirconia ceramics facades and an integrally formed top of zirconia ceramics plate
The box-like zirconia structure of portion's opening.Four zirconia ceramics facades are used to replace the plastic package or metal hemming edge of mobile phone.
Four zirconia ceramics facades and zirconia ceramics plate surround in the cavity to be formed for accommodating circuit board of mobile phone and screen.Mesh
Before, 3D zirconia ceramics mobile phone backboard is beautiful with it, and the electricity of the 2.5D zirconia ceramics mobile phone backboard relative to metal hemming edge
Son shields small advantage and is widely used.
Currently, the preparation method of common 3D zirconia ceramics mobile phone backboard is injection molding technology, process is as follows: first
Zirconium powder and binder are kneaded after mixing to obtain colloidal sol, then by colloidal sol injection 3D molding die molding, then
Zirconia ceramics mobile phone backboard is obtained after degreasing, sintering.
However, the angularity of the 3D zirconia ceramics mobile phone backboard of prior art preparation is usually 0.5-0.6mm.Due to it
Angularity has been more than empirical value 0.1mm, cannot be directly applied on mobile phone, needs further to machine it, is eliminated
The angularity of 3D zirconia ceramics mobile phone backboard.
Summary of the invention
Big technical problem is spent in order to solve 3D zirconia ceramics cell phone back slab warping in the prior art, and due to warpage
The technical problem for causing machining allowance excessive greatly is spent, inventor conducts in-depth research this.It is unexpected in the course of the research
Discovery, using specific formula, and combine specific moulding process, degreasing process, binder removal, high-sintering process,
When sizing sintering process, the set-back of prepared 3D zirconia ceramics mobile phone backboard is obviously reduced, can be straight without machining
It scoops out and uses on mobile phone, be based on this, inventor completes the present invention.
The purpose of the present invention is to provide a kind of preparation method of 3D zirconia ceramics mobile phone backboard and its product of preparation,
To realize the purpose for reducing 3D zirconia ceramics cell phone back slab warping degree.Specific technical solution is as follows:
The present invention provides a kind of preparation methods of 3D zirconia ceramics mobile phone backboard, which comprises
1) 80-85 parts by weight, specific surface area 6-10m are weighed2The Zirconium powder of/g and adding for 15-20 parts by weight
Add agent；The additive includes: the paraffin for accounting for additive gross mass 25-40%, the poly- second for accounting for additive gross mass 25-30%
Alkene, the vegetable oil for accounting for additive gross mass 5-10%, accounts for additive gross mass at the polypropylene for accounting for additive gross mass 15-20%
The ethylene-vinyl acetate copolymer of 5-10%, the oleic acid for accounting for additive gross mass 3-5%；
2) weighed Zirconium powder and additive are mixed, and 200-240 DEG C at a temperature of be kneaded 13-15h, obtain
Mixing materials；
3) mixing materials are heated to 170-190 DEG C, obtain colloidal sol, the colloidal sol is injected into 3D molding die, it is cooling
After obtain 3D zirconia ceramics cell phone back slab body；
4) the 3D zirconia ceramics cell phone back slab body is immersed in organic solvent and carries out degreasing, then will be after degreasing
3D zirconia ceramics cell phone back slab body is fitted into draft glue discharging furnace, then according to 4-10min/ DEG C of heating rate by the draft glue discharging furnace
It is warming up to 700-1000 DEG C, and keeps the temperature 60-180min and carries out dumping, is subsequently cooled to 40 DEG C or less；
5) the 3D zirconia ceramics cell phone back slab body after dumping is fitted into sintering furnace, then according to 1.5-5min/ DEG C
Heating rate the sintering furnace is warming up to 1350-1450 DEG C, and keep the temperature 60-180min carry out high temperature sintering, then cool down
To 40 DEG C or less；
6) the 3D zirconia ceramics cell phone back slab body of high temperature sintering is packed into sizing sintering smelting tool, then by the sizing
It is sintered smelting tool to be packed into sintering furnace, sintering furnace is then warming up to 1350-1450 DEG C according to 1.5-5min/ DEG C of heating rate,
And keep the temperature 60-180min and carry out shaping sintering, 40 DEG C are subsequently cooled to hereinafter, obtaining 3D zirconia ceramics mobile phone backboard.
Optionally, in a kind of specific embodiment of the invention, the Zirconium powder is the stabilization containing 3%mol
Agent and impurity content are lower than the Zirconium powder of 0.01% (wt.).
It is optionally, described that mixing materials are heated to 170-190 DEG C in a kind of specific embodiment of the invention, comprising:
Mixing materials are cooled to 40 DEG C hereinafter, mixing materials after cooling are ground into the mixing that particle diameter is 3-5mm again
Material, finally by mixed material heating to 170-190 DEG C.
Optionally, in a kind of specific embodiment of the invention, the temperature of the organic solvent of the degreasing is 60-70
DEG C, when degreasing a length of 36-48h.
Optionally, described that the colloidal sol is injected into 3D molding die in a kind of specific embodiment of the invention
Molding, comprising:
Under conditions of mold temperature is 20-70 DEG C, the colloidal sol is injected into 3D molding die and is formed.
Optionally, in a kind of specific embodiment of the invention, table that the 3D molding die is contacted with the colloidal sol
Surface roughness is less than 0.03 μm.
Optionally, in a kind of specific embodiment of the invention, the sizing sintering smelting tool is top smelting tool and lower part
Sintering smelting tool made of smelting tool is mutually fitted into, wherein smelting tool in top is mounted on the top of lower part smelting tool, and the top smelting has and institute
State lower part smelting have the shape for the cavity to be formed, size with the 3D zirconia ceramics cell phone back slab body Xiang Shi after high temperature sintering
It answers, and the weight of top smelting tool is 500-2000g.
The present invention also provides a kind of 3D zirconia ceramics mobile phone backboards prepared according to method described in any of the above embodiments.
Experiment shows using a kind of production of the preparation method preparation of 3D zirconia ceramics mobile phone backboard provided by the invention
The angularity of 3D zirconia ceramics mobile phone backboard can be reduced to 0.03mm or less by product.
Further, the angularity using the 3D zirconia ceramics mobile phone backboard of technology provided by the invention preparation is lower,
Machining processes can also be removed from, improve the production efficiency of 3D zirconia ceramics mobile phone backboard, but also oxidation can be improved
The utilization rate of zirconium powder body.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
To solve prior art problem, the embodiment of the invention provides a kind of preparation sides of 3D zirconia ceramics mobile phone backboard
Method, which comprises
1) 80-85 parts by weight, specific surface area 6-10m are weighed2The Zirconium powder of/g.15-20 parts by weight are weighed again
Additive；The additive includes: the paraffin for accounting for additive gross mass 25-40%, accounts for the poly- of additive gross mass 25-30%
Ethylene, the vegetable oil for accounting for additive gross mass 5-10%, accounts for the total matter of additive at the polypropylene for accounting for additive gross mass 15-20%
It measures the ethylene-vinyl acetate copolymer of 5-10%, account for the oleic acid of additive gross mass 3-5%.
In a kind of specific embodiment of the embodiment of the present invention, in order to improve the stabilization of 3D zirconia ceramics mobile phone backboard
Property, Zirconium powder can be with are as follows: stabilizer and impurity content containing 3%mol are lower than the Zirconium powder of 0.01% (wt.).
In order to improve the uniformity of mixing materials, paraffin can be No. 58 fully refined paraffin wax；Polyethylene can be number-average molecular weight between 10-
Polyethylene between 120000；Polypropylene can be polypropylene of the number-average molecular weight between 12-15 ten thousand；Vegetable oil can be big
Soya-bean oil, peanut oil, castor oil and sunflower oil etc..Inventor is found surprisingly that vegetable oil is added when being kneaded can be improved 3D
The success rate of zirconia ceramics cell phone back slab body disengaging 3D molding die.Inventor is further it was unexpectedly observed that when addition
When vegetable oil is soybean oil, the 3D zirconia ceramics mobile phone back plate surface after high temperature sintering will not have pollutant residual.Ethylene-
Acetate ethylene copolymer can be ethylene-vinyl acetate copolymer of the vinyl acetate content between 12-25% (wt.).Into
One step, in a kind of specific embodiment of the invention, in order to reduce the residue in vegetable oil to 3D zirconia ceramics mobile phone
The screen filtration soybean oil of 100-200 mesh can be used in the influence of backboard quality.Inventor also found, when using epigranular
When the better Zirconium powder of property, 3D zirconia ceramics cell phone back slab body can be made to shrink during the sintering process more uniform,
And then the inconsistent caused deformation of shrinking percentage for reducing the different location of 3D zirconia ceramics cell phone back slab body.
2) weighed Zirconium powder and additive are mixed, and 200-240 DEG C at a temperature of be kneaded 13-15h, obtain
Mixing materials.
3) mixing materials are heated to 170-190 DEG C, obtain colloidal sol, the colloidal sol is injected into 3D molding die, it is cooling
After obtain 3D zirconia ceramics cell phone back slab body.
It, can in order to improve the uniformity of solid particle in colloidal sol in a kind of specific embodiment of the embodiment of the present invention
Mixing materials are cooled to 40 DEG C hereinafter, the mixture that raw material after cooling is ground into particle diameter as 3-5mm again.In order to disappear
Except during injecting colloidal sol the phenomenon that colloidal sol chilling, then by mixed material heating to 170-190 DEG C obtain colloidal sol while；?
Under conditions of mold temperature is 20-70 DEG C, the colloidal sol is injected into 3D molding die and is formed.The one of the embodiment of the present invention
In kind specific embodiment, in order to further increase the surface quality of 3D zirconia ceramics cell phone back slab body, the 3D molding
The surface roughness that mold is contacted with the colloidal sol is less than 0.03 μm.Furthermore it is possible to adjust the table of 3D molding die according to demand
The surface quality of surface roughness, the smaller mold of surface roughness 3D zirconia ceramics cell phone back slab body after molding is better.
Inventor also found, the zirconia ceramics for using wolfram steel mold of the surface roughness less than 0.03 μm to make as 3D molding die
The surface quality of backboard green body is best.
It is understood that above-mentioned injection technique can use existing injection technique, colloidal sol is injected into 3D molding
In mold.
4) the 3D zirconia ceramics cell phone back slab body is immersed in organic solvent and carries out degreasing, it is organic molten to utilize
Paraffin and vegetable oil present in 3D zirconia ceramics cell phone back slab body are quickly dissolved in agent.The 3D zirconium oxide after degreasing is made pottery again
Porcelain cell phone back slab body is fitted into draft glue discharging furnace, and the draft glue discharging furnace is then warming up to 700- according to 4-10min/ DEG C of heating rate
1000 DEG C, and keep the temperature 60-180min and carry out dumping.In dumping process, high temperature while making Zirconium powder curing molding,
It can also make the remaining organic matter volatilization or cracking in 3D zirconia ceramics cell phone back slab body, and then eliminate having for remnants
Machine object, such as polyethylene, polypropylene, acetic acid and ethylene-vinyl acetate copolymer.Then again by 3D zirconia ceramics cell phone back
Plate is cooled to 40 DEG C or less.It, can be to avoid in high temperature sintering by the organic matter removal in 3D zirconia ceramics cell phone back slab body
When, organic matter gasifies at high temperature and then volume expansion, leads to 3D zirconia ceramics cell phone back plate blank cracking or deformation.
In a kind of specific embodiment of the embodiment of the present invention, for degreasing organic solvent can for common kerosene,
Aviation kerosine, temperature when degreasing are 60-70 DEG C, degreasing time 36-48h.In practical applications, in order to reduce common kerosene
In interference of the impurity to 3D zirconia ceramics cell phone back slab body skimming processes, aviation kerosine can be used and make pottery to 3D zirconium oxide
Porcelain cell phone back slab body carries out ungrease treatment, for example, can be according to submergence 3-5 branch 3D zirconia ceramics hand in every liter of aviation kerosine
The ratio of machine backboard green body using aviation kerosine carry out degreasing, certainly, when 3D zirconia ceramics cell phone back slab body volume compared with
When big, when causing aviation kerosine that can not submerge 3D zirconia ceramics cell phone back slab body, the use ratio of aviation kerosine can be increased
Example.
5) the 3D zirconia ceramics cell phone back slab body after dumping is fitted into sintering furnace, then according to 1.5-5min/ DEG C
Heating rate the sintering furnace is warming up to 1350-1450 DEG C, and keep the temperature 60-180min carry out high temperature sintering, then cool down
To 40 DEG C or less.
It should be noted that remaining in 3D zirconia ceramics hand in degreasing or dumping process in high temperature sintering process
Organic matter in machine backboard green body can gasify at high temperature, to keep the organic matter in 3D zirconia ceramics cell phone back slab body complete
It is removed entirely.
6) the 3D zirconia ceramics cell phone back slab body of high temperature sintering is packed into sizing sintering smelting tool, then by the sizing
It is sintered smelting tool to be packed into sintering furnace, sintering furnace is then warming up to 1350-1450 DEG C according to 1.5-5min/ DEG C of heating rate,
And keep the temperature 60-180min and carry out shaping sintering, 40 DEG C are subsequently cooled to hereinafter, obtaining 3D zirconia ceramics mobile phone backboard.
It should be noted that sizing sintering smelting tool can be by that can be made, for example, can be in 1550 DEG C of indeformable materials
Smelting tool is sintered for molybdenum formulation type, tungsten formulation type is sintered smelting tool, graphite formulation type is sintered smelting tool etc..When that will be formed, sintering smelting tool is packed into
After in sintering furnace, when sintering furnace to be warming up to the temperature of setting according to the heating rate of setting, the temperature of sizing sintering smelting tool
It can rise with the rising of sintering furnace temperature.
In a kind of specific embodiment of the embodiment of the present invention, in order to further decrease 3D oxidation in sizing sintering process
The warpage of zircon ceramic cell phone back slab body, it is that top smelting tool and lower part smelting have burning made of mutual be fitted into that the sizing, which is sintered smelting to have,
Tie smelting tool, wherein smelting tool in top is mounted on the top of lower part smelting tool, and the top smelting tool and the lower part smelting have the cavity to be formed
Shape, size, with the shape of the finally obtained 3D zirconia ceramics mobile phone backboard that can be directly used on mobile phone, ruler
It is very little identical, and the weight of top smelting tool is 500-2000g.Since zirconia ceramics has High-Temperature Creep Performance, it is sintered in sizing
In process, the 3D zirconia ceramics cell phone back slab body after high temperature sintering softens at high temperature, and under the compressing of top smelting tool
It deforms.Since the size of top smelting tool and the mutually chimeric cavity formed of lower part smelting tool is 3D zirconia ceramics mobile phone backboard
Final size.Therefore, using above embodiment of the present invention, sticking up for 3D zirconia ceramics mobile phone backboard can be further decreased
Curvature.
The embodiment of the invention also provides a kind of 3D zirconia ceramics mobile phone backboards prepared using any of the above-described method.
The following is a clear and complete description of the technical scheme in the embodiments of the invention, wherein embodiment 1-3 is to adopt
The preparation of 3D zirconia ceramics mobile phone backboard is carried out with technical solution provided by the invention；Comparative example 1-3 is using the prior art
The technical solution of offer carries out the preparation of 3D zirconia ceramics mobile phone backboard, and detailed process and technological parameter are as follows:
Embodiment 1
1) Zirconium powder (the first uncommon element chemistry Industrial Co., Ltd, trade mark HSY-3.0B) of 80Kg is weighed.Claim
Take the additive of 20Kg；The additive includes: No. 58 fully refined paraffin wax for accounting for additive gross mass 25%, accounts for the total matter of additive
The polyethylene (China PetroChemical Corporation, trade mark 5000S) of amount 30%, the polypropylene for accounting for additive gross mass 20%
(Chiba, Japan Chemical Co., Ltd., trade mark APP-MZ), the soybean oil for accounting for additive gross mass 10%, additive gross mass is accounted for
10% ethylene-vinyl acetate copolymer (Chinese Medicine group, number xw249377885) accounts for additive gross mass 5%
Oleic acid (Chinese Medicine group, number 30138518).
2) weighed Zirconium powder and additive are mixed, and 200 DEG C at a temperature of be kneaded 13h, obtain mixing materials.
3) mixing materials are cooled to 40 DEG C hereinafter, mixing materials after cooling are ground into the mixing that particle diameter is 3mm again
Mixed material heating is finally obtained colloidal sol to 170 DEG C by material；Simultaneously under conditions of mold temperature is 20 DEG C, the colloidal sol is infused
3D tungsten steel forming die for molding is injected, 100 3D zirconia ceramics cell phone back slab bodies are obtained.In addition, 3D tungsten steel forming mould
Having the surface roughness contacted with the colloidal sol is 0.03 μm.
4) ratio of 1 liter of aviation kerosine, 100 will obtained are used according to every 5 3D zirconia ceramics cell phone back slab body
Branch 3D zirconia ceramics cell phone back slab body, which is immersed in aviation kerosine, carries out degreasing, and the temperature of aviation kerosine is 60 DEG C, is taken off
A length of 36h when rouge.The 3D zirconia ceramics cell phone back slab body after degreasing is fitted into draft glue discharging furnace again, then according to 4min/ DEG C
Heating rate the draft glue discharging furnace is warming up to 700 DEG C, and keep the temperature 60min carry out dumping, be subsequently cooled to 40 DEG C or less.
5) the 3D zirconia ceramics cell phone back slab body after dumping is fitted into sintering furnace, then according to 1.5min/ DEG C
The sintering furnace is warming up to 1350 DEG C by heating rate, and is kept the temperature 60min and carried out high temperature sintering, is subsequently cooled to 40 DEG C or less.
6) the 3D zirconia ceramics cell phone back slab body of high temperature sintering is packed into sizing sintering smelting tool, and sintering smelting of being formed
The weight of the top smelting tool of tool is 500g.Then sizing sintering smelting tool is packed into sintering furnace, then according to 1.5min/ DEG C
Sintering furnace is warming up to 1350 DEG C by heating rate, and is kept the temperature 60min and carried out shaping sintering, is subsequently cooled to 40 DEG C hereinafter, obtaining
3D zirconia ceramics mobile phone backboard.
Embodiment 2
1) Zirconium powder (the first uncommon element chemistry Industrial Co., Ltd, trade mark HSY-3W) of 82Kg is weighed.It weighs
The additive of 18Kg；The additive includes: No. 58 fully refined paraffin wax for accounting for additive gross mass 35%, accounts for additive gross mass
25% polyethylene (China PetroChemical Corporation, trade mark 5000S), the polypropylene (day for accounting for additive gross mass 15%
This Chiba Chemical Co., Ltd., trade mark SUNATAC-L), the soybean oil that accounts for additive gross mass 10%, account for additive gross mass
10% ethylene-vinyl acetate copolymer (Chinese Medicine group, number xw249377886) accounts for additive gross mass 5%
Oleic acid (Chinese Medicine group, number 30138518).
2) weighed Zirconium powder and additive are mixed, and 220 DEG C at a temperature of be kneaded 14h, obtain mixing materials.
3) mixing materials are cooled to 40 DEG C hereinafter, compound powder after cooling is broken into the mixing that particle diameter is 4mm again
Mixed material heating is finally obtained colloidal sol to 180 DEG C by material；Simultaneously under conditions of mold temperature is 50 DEG C, the colloidal sol is infused
3D tungsten steel forming die for molding is injected, 100 3D zirconia ceramics cell phone back slab bodies are obtained.In addition, 3D tungsten steel forming mould
Having the surface roughness contacted with the colloidal sol is 0.03 μm.
4) ratio of 1 liter of aviation kerosine, 100 will obtained are used according to every 5 3D zirconia ceramics cell phone back slab body
Branch 3D zirconia ceramics cell phone back slab body, which is immersed in aviation kerosine, carries out degreasing, and the temperature of aviation kerosine is 65 DEG C, is taken off
The rouge time is 42h.The 3D zirconia ceramics cell phone back slab body after degreasing is fitted into draft glue discharging furnace again, then according to 7min/ DEG C
Heating rate the draft glue discharging furnace is warming up to 850 DEG C, and keep the temperature 120min carry out dumping, be subsequently cooled to 40 DEG C or less.
5) the 3D zirconia ceramics cell phone back slab body after dumping is fitted into sintering furnace, then according to 3min/ DEG C of liter
The sintering furnace is warming up to 1400 DEG C by warm rate, and is kept the temperature 120min and carried out high temperature sintering, is subsequently cooled to 40 DEG C or less.
6) the 3D zirconia ceramics cell phone back slab body of high temperature sintering is packed into sizing sintering smelting tool, and sintering smelting of being formed
The weight of the top smelting tool of tool is 1000g.Then sizing sintering smelting tool is packed into sintering furnace, then according to 3min/ DEG C
Sintering furnace is warming up to 1400 DEG C by heating rate, and is kept the temperature 120min and carried out shaping sintering, is subsequently cooled to 40 DEG C hereinafter, obtaining
3D zirconia ceramics mobile phone backboard.
Embodiment 3
1) Zirconium powder (the first uncommon element chemistry Industrial Co., Ltd, trade mark HSY-2.6) of 85Kg is weighed.It weighs
The additive of 15Kg；The additive includes: No. 58 fully refined paraffin wax for accounting for additive gross mass 40%, accounts for additive gross mass
30% polyethylene (China PetroChemical Corporation, trade mark 5000S), the polypropylene (day for accounting for additive gross mass 17%
This Chiba Chemical Co., Ltd., trade mark SUNATAC-LX), the soybean oil that accounts for additive gross mass 5%, account for additive gross mass
5% ethylene-vinyl acetate copolymer (Chinese Medicine group, number xw249377887) accounts for additive gross mass 3%
Oleic acid (Chinese Medicine group, number 30138518).
2) weighed Zirconium powder and additive are mixed, and 240 DEG C at a temperature of be kneaded 15h, obtain mixing materials.
3) mixing materials are cooled to 40 DEG C hereinafter, mixing materials after cooling are ground into the mixing that particle diameter is 5mm again
Mixed material heating is finally obtained colloidal sol to 190 DEG C by material；Simultaneously under conditions of mold temperature is 70 DEG C, the colloidal sol is infused
3D tungsten steel forming die for molding is injected, 100 3D zirconia ceramics cell phone back slab bodies are obtained.In addition, 3D tungsten steel forming mould
Having the surface roughness contacted with the colloidal sol is 0.01 μm.
4) ratio of 1 liter of aviation kerosine, 100 will obtained are used according to every 5 3D zirconia ceramics cell phone back slab body
Branch 3D zirconia ceramics cell phone back slab body, which is immersed in aviation kerosine, carries out degreasing, and the temperature of aviation kerosine is 70 DEG C, is taken off
A length of 48h when rouge.The 3D zirconia ceramics cell phone back slab body after degreasing is fitted into draft glue discharging furnace again, then according to 10min/ DEG C
Heating rate the draft glue discharging furnace is warming up to 1000 DEG C, and keep the temperature 180min carry out dumping, be subsequently cooled to 40 DEG C or less.
5) the 3D zirconia ceramics cell phone back slab body after dumping is fitted into sintering furnace, then according to 5min/ DEG C of liter
The sintering furnace is warming up to 1450 DEG C by warm rate, and is kept the temperature 180min and carried out high temperature sintering, is subsequently cooled to 40 DEG C or less.
6) the 3D zirconia ceramics cell phone back slab body of high temperature sintering is packed into sizing sintering smelting tool, and sintering smelting of being formed
The weight of the top smelting tool of tool is 2000g.Then sizing sintering smelting tool is packed into sintering furnace, then according to 5min/ DEG C
Sintering furnace is warming up to 1450 DEG C by heating rate, and is kept the temperature 180min and carried out shaping sintering, is subsequently cooled to 40 DEG C hereinafter, obtaining
3D zirconia ceramics mobile phone backboard.
Comparative example 1
1) according to paraffin: polypropylene: polyethylene: oleic acid=50:15:20:6 ratio, 160 DEG C at a temperature of by paraffin
Then polypropylene and polyethylene is added in heating and melting, keeping temperature is 160 DEG C, and stirring is completely disappeared to solid, is then added
Oleic acid stir mixing 40min, cooling and solidifying are broken to obtain the adhesive particle material that partial size is 2mm.According still further to zirconium oxide: bonding
Agent particulate material=85:15 ratio weighs zirconia ceramics and adhesive particle material, is uniformly mixed, obtains mixture.
2) by mixture 180 DEG C at a temperature of, be kneaded 5h.Then again in the item that temperature is 190 DEG C, pressure is 70MPa
Mixture is injected into mold under part, obtains 3D zirconia ceramics cell phone back slab body.
3) 3D zirconia ceramics cell phone back slab body is immersed in 20 DEG C of organic solvent, with the speed liter of 0.5 DEG C/min
For temperature to 50 DEG C, heat preservation 7h carries out degreasing.
4) the 3D zirconia ceramics cell phone back slab body after degreasing is fitted into heat-treatment furnace, with 1.5 in oxidizing atmosphere
DEG C/speed of min rises to 900 DEG C, heat preservation 5.2h is heat-treated, and is then cooled to 40 DEG C or less with the speed of 2 DEG C/min.
5) the 3D zirconia ceramics cell phone back slab body after heat treatment is fitted into sintering furnace, 1450 DEG C at a temperature of,
It keeps the temperature 6h and carries out high temperature sintering, obtain 3D zirconia ceramics mobile phone backboard.
Comparative example 2
1) according to paraffin: polypropylene: polyethylene: oleic acid=45:17:18:8 ratio, 135 DEG C at a temperature of by paraffin
Then polypropylene and polyethylene is added in heating and melting, keeping temperature is 160 DEG C, and stirring is completely disappeared to solid, is then added
Oleic acid stir mixing 55min, cooling and solidifying are broken to obtain the adhesive particle material that partial size is 5mm.According still further to zirconium oxide: bonding
Agent particulate material=88:12 ratio weighs zirconia ceramics and adhesive particle material, is uniformly mixed, obtains mixture.
2) by mixture 210 DEG C at a temperature of, be kneaded 4h.Then again in the item that temperature is 198 DEG C, pressure is 64MPa
Mixture is injected into mold under part, obtains 3D zirconia ceramics cell phone back slab body.
3) 3D zirconia ceramics cell phone back slab body is immersed in 150 DEG C of organic solvent, with the speed liter of 0.3 DEG C/min
For temperature to 48 DEG C, heat preservation 7.5h carries out degreasing.
4) the 3D zirconia ceramics cell phone back slab body after degreasing is fitted into heat-treatment furnace, in oxidizing atmosphere with 2 DEG C/
The speed of min rises to 980 DEG C, and heat preservation 5h is heat-treated, and is then cooled to 40 DEG C or less with the speed of 3 DEG C/min.
5) the 3D zirconia ceramics cell phone back slab body after heat treatment is fitted into sintering furnace, 1500 DEG C at a temperature of,
It keeps the temperature 5.5h and carries out high temperature sintering, obtain 3D zirconia ceramics mobile phone backboard.
Comparative example 3
1) according to paraffin: polypropylene: polyethylene: oleic acid=58:12:24:5.5 ratio, 190 DEG C at a temperature of by stone
Then polypropylene and polyethylene is added in wax heating and melting, keeping temperature is 160 DEG C, and stirring to solid completely disappears, then plus
Enter oleic acid stir mixing 40min, cools and solidifies, it is broken to obtain the adhesive particle material that partial size is 10mm.According still further to zirconium oxide: viscous
Knot agent particulate material=83:17 ratio weighs zirconia ceramics and adhesive particle material, is uniformly mixed, obtains mixture.
2) by mixture 160 DEG C at a temperature of, be kneaded 7.5h.Then again temperature is 185 DEG C, pressure is 78MPa's
Under the conditions of mixture is injected into mold, obtain 3D zirconia ceramics cell phone back slab body.
3) 3D zirconia ceramics cell phone back slab body is immersed in 25 DEG C of organic solvent, with the speed liter of 0.8 DEG C/min
For temperature to 55 DEG C, heat preservation 6.5h carries out degreasing.
4) the 3D zirconia ceramics cell phone back slab body after degreasing is fitted into heat-treatment furnace, in oxidizing atmosphere with 1 DEG C/
The speed of min rises to 830 DEG C, and heat preservation 5.8h is heat-treated, and is then cooled to 40 DEG C or less with the speed of 1.5 DEG C/min.
5) the 3D zirconia ceramics cell phone back slab body after heat treatment is fitted into sintering furnace, 1520 DEG C at a temperature of,
It keeps the temperature 5h and carries out high temperature sintering, obtain 3D zirconia ceramics mobile phone backboard.
10 are randomly choosed respectively from 3D zirconia ceramics mobile phone backboard prepared by embodiment 1-3 and comparative example 1-3
3D zirconia ceramics mobile phone backboard measures each 3D zirconia ceramics cell phone back according to method as defined in GB/T 31352-2014
The angularity of plate, the results are shown in Table 1.Table 1 is 3D zirconia ceramics cell phone back prepared by embodiment 1-3 and comparative example 1-3
The angularity measurement result of plate.
Table 1
As it can be seen from table 1 the angularity maximum value of the 3D zirconia ceramics mobile phone backboard of 1-3 of embodiment of the present invention preparation
0.028mm, minimum value 0.011mm, average value 0.019mm.The 3D zirconia ceramics mobile phone backboard of comparative example 1-3 preparation
Angularity maximum value 2.627mm, minimum value 0.468mm, average value 1.517mm.As it can be seen that the 3D of preparation of the embodiment of the present invention
The angularity of zirconia ceramics mobile phone backboard has obtained greatly than the angularity of the 3D zirconia ceramics backboard of prior art preparation
Reduction, reached 0.03mm or less.
Since the hardness of zirconia ceramics is larger, machining difficulty is high, is to the method that zirconium oxide is machined out at present
Surplus is removed using grinding technics.The unit time processing capacity of grinding technics is small, therefore carries out machine to zirconia ceramics backboard and add
Work needs to expend a large amount of working hour and rapidoprint.And apply the angularity of 3D zirconia ceramics mobile phone backboard prepared by the present invention
It is lower, machining processes can be removed from, saved machining period, to improve production efficiency, while also saving processing material
Material.In addition, due to not needing removal surplus, carrying out 3D zirconia ceramics mobile phone backboard process using the present invention can be with
The utilization rate for improving Zirconium powder further decreases the production cost of 3D zirconia ceramics mobile phone backboard, improves product market
Competitiveness.
It should be noted that the terms "include", "comprise" or its any other variant are intended to the packet of nonexcludability
Contain, so that the process, method, article or equipment for including a series of elements not only includes those elements, but also including
Other elements that are not explicitly listed, or further include for elements inherent to such a process, method, article, or device.
In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that including the element
Process, method, article or equipment in there is also other identical elements.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (8)
1. a kind of preparation method of 3D zirconia ceramics mobile phone backboard, which is characterized in that the described method includes:
1) 80-85 parts by weight, specific surface area 6-10m are weighed2The Zirconium powder of/g and the additive of 15-20 parts by weight；
The additive includes: the paraffin for accounting for additive gross mass 25-40%, the polyethylene for accounting for additive gross mass 25-30%, Zhan Tian
Add the polypropylene of agent gross mass 15-20%, the vegetable oil for accounting for additive gross mass 5-10%, account for additive gross mass 5-10%'s
Ethylene-vinyl acetate copolymer, the oleic acid for accounting for additive gross mass 3-5%；
2) weighed Zirconium powder and additive are mixed, and 200-240 DEG C at a temperature of be kneaded 13-15h, be kneaded
Material；
3) mixing materials are heated to 170-190 DEG C, obtain colloidal sol, the colloidal sol is injected into 3D molding die, obtained after cooling
To 3D zirconia ceramics cell phone back slab body；
4) the 3D zirconia ceramics cell phone back slab body is immersed in organic solvent and carries out degreasing, then by the 3D oxygen after degreasing
Change zircon ceramic cell phone back slab body to be fitted into draft glue discharging furnace, then the draft glue discharging furnace heats up according to 4-10min/ DEG C of heating rate
It to 700-1000 DEG C, and keeps the temperature 60-180min and carries out dumping, be subsequently cooled to 40 DEG C or less；
5) the 3D zirconia ceramics cell phone back slab body after dumping is fitted into sintering furnace, then according to 1.5-5min/ DEG C of liter
The sintering furnace is warming up to 1350-1450 DEG C by warm rate, and is kept the temperature 60-180min and carried out high temperature sintering, is subsequently cooled to 40
DEG C or less；
6) the 3D zirconia ceramics cell phone back slab body of high temperature sintering is packed into sizing sintering smelting tool, is then sintered the sizing
Smelting tool is packed into sintering furnace, sintering furnace is then warming up to 1350-1450 DEG C according to 1.5-5min/ DEG C of heating rate, and protect
Warm 60-180min carries out shaping sintering, is subsequently cooled to 40 DEG C hereinafter, obtaining 3D zirconia ceramics mobile phone backboard.
2. the method according to claim 1, wherein the Zirconium powder be the stabilizer containing 3%mol,
And impurity content is lower than the Zirconium powder of 0.01% (wt.).
3. the method according to claim 1, wherein described be heated to 170-190 DEG C for mixing materials, comprising:
Mixing materials are cooled to 40 DEG C hereinafter, mixing materials after cooling are ground into the mixture that particle diameter is 3-5mm again, most
Afterwards by mixed material heating to 170-190 DEG C.
4. being taken off the method according to claim 1, wherein the temperature of the organic solvent of the degreasing is 60-70 DEG C
The rouge time is 36-48h.
5. the method according to claim 1, wherein it is described by the colloidal sol be injected into 3D molding die at
Type, comprising:
Under conditions of mold temperature is 20-70 DEG C, the colloidal sol is injected into 3D molding die and is formed.
6. the method according to claim 1, wherein the surface that the 3D molding die is contacted with the colloidal sol is thick
Rugosity is less than 0.03 μm.
7. the method according to claim 1, wherein sizing sintering smelting tool is that top smelting tool and lower part smelting have
Sintering smelting tool made of being mutually fitted into, and the weight of top smelting tool is 500-2000g.
8. the 3D zirconia ceramics mobile phone backboard of method preparation according to claim 1-7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711129451.5A CN109776090B (en) | 2017-11-15 | 2017-11-15 | Preparation method of 3D zirconia ceramic mobile phone backboard and prepared product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711129451.5A CN109776090B (en) | 2017-11-15 | 2017-11-15 | Preparation method of 3D zirconia ceramic mobile phone backboard and prepared product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109776090A true CN109776090A (en) | 2019-05-21 |
| CN109776090B CN109776090B (en) | 2021-09-10 |
Family
ID=66494914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711129451.5A Active CN109776090B (en) | 2017-11-15 | 2017-11-15 | Preparation method of 3D zirconia ceramic mobile phone backboard and prepared product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109776090B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002074714A1 (en) * | 2001-03-21 | 2002-09-26 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Dense ceramic body, in particular for dental application |
| CN1519406A (en) * | 2003-01-24 | 2004-08-11 | 中国科学院上海硅酸盐研究所 | Method for manufacturing injection molding zirconia products |
| CN101066874A (en) * | 2007-06-08 | 2007-11-07 | 湖南正阳精密陶瓷有限公司 | Zirconia injection molding process and organic carrier for zirconia powder |
| CN101618568A (en) * | 2009-02-27 | 2010-01-06 | 清华大学 | Preparation method of superfine ceramic powder injection molding mixture |
| CN102010199A (en) * | 2010-11-19 | 2011-04-13 | 湖南正阳精密陶瓷有限公司 | Production method of zirconia ceramic bushing |
| CN103113102A (en) * | 2013-03-15 | 2013-05-22 | 湖南正阳精密陶瓷有限公司 | Zirconia ceramic insert core and preparation method thereof |
| CN105666890A (en) * | 2016-02-04 | 2016-06-15 | 叶志杰 | Die-interior mark special shape/hook face forming method and device |
-
2017
- 2017-11-15 CN CN201711129451.5A patent/CN109776090B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002074714A1 (en) * | 2001-03-21 | 2002-09-26 | Saint-Gobain Centre De Recherches Et D'etudes Europeen | Dense ceramic body, in particular for dental application |
| CN1519406A (en) * | 2003-01-24 | 2004-08-11 | 中国科学院上海硅酸盐研究所 | Method for manufacturing injection molding zirconia products |
| CN101066874A (en) * | 2007-06-08 | 2007-11-07 | 湖南正阳精密陶瓷有限公司 | Zirconia injection molding process and organic carrier for zirconia powder |
| CN101618568A (en) * | 2009-02-27 | 2010-01-06 | 清华大学 | Preparation method of superfine ceramic powder injection molding mixture |
| CN102010199A (en) * | 2010-11-19 | 2011-04-13 | 湖南正阳精密陶瓷有限公司 | Production method of zirconia ceramic bushing |
| CN103113102A (en) * | 2013-03-15 | 2013-05-22 | 湖南正阳精密陶瓷有限公司 | Zirconia ceramic insert core and preparation method thereof |
| CN105666890A (en) * | 2016-02-04 | 2016-06-15 | 叶志杰 | Die-interior mark special shape/hook face forming method and device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109776090B (en) | 2021-09-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104907567B (en) | A kind of method for preparing high-density complicated shape cemented carbide parts and cutter | |
| CN103240412B (en) | Method for preparing powder super-alloy by near net shape | |
| US20180312674A1 (en) | Binder for injection moulding compositions | |
| CN103304227B (en) | Alumina-based ceramic core for directional solidification and preparation method thereof | |
| CN106118588B (en) | Method for the injection molding binder of titanium alloy powder and injection moulding titanium alloy component | |
| CN103981436A (en) | Metal powder injection molded high-strength martensite aged steel and preparation method thereof | |
| CN105481364B (en) | The preparation method of ceramic watchcase | |
| CN105732014A (en) | Silicon-based ceramic core preparation method | |
| CN109467419A (en) | A kind of graphene enhancing alumina based ceramic core and preparation method thereof | |
| CN106756148B (en) | The method that a kind of foundry alloy method of low oxygen content prepares MIM418 alloys | |
| CN105130438A (en) | Method for preparing boron carbide ceramic composite material based on reaction sintering | |
| CN105732007B (en) | A kind of calcium oxide-based ceramic-mould fast preparation method for complex parts manufacture | |
| KR100888766B1 (en) | Process for producing silica glass product | |
| CN104440601A (en) | Diamond grinding wheel for high-speed four-edge grinding and manufacturing method thereof | |
| CN107755697A (en) | Ormolu product and its increasing material manufacturing forming method | |
| CN108191409A (en) | It is a kind of for aqueous-based ceramic slurry of free extrusion molding and preparation method and application | |
| CN109293349A (en) | A kind of silica base graphene ceramic core and preparation method thereof | |
| CN108424124A (en) | Magnesium oxide-based crucible of a kind of magnesia crystal whisker fabricated in situ spinelle enhancing and preparation method thereof | |
| CN105622109A (en) | Preparation method of silicon nitride ceramic ball and silicon nitride ceramic ball | |
| CN102924087B (en) | Method for preparing cubic born nitride-silicon carbide composite ceramic material and product thereof | |
| CN104496503A (en) | Rapid-repair refractory material and preparation and use methods thereof | |
| CN101293280A (en) | Method for producing molybdenum alloy gas vane with powder injection forming | |
| CN101695808B (en) | Preparation method of high-performance pored ceramic blade | |
| CN108546093A (en) | Short fine magnesium oxide-based crucible of enhancing of a kind of aluminium oxide and preparation method thereof | |
| CN109776090A (en) | A kind of preparation method of 3D zirconia ceramics mobile phone backboard and the product of preparation |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |