CN105563616B - The forming method of zirconia ceramic product - Google Patents
The forming method of zirconia ceramic product Download PDFInfo
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- CN105563616B CN105563616B CN201510940021.6A CN201510940021A CN105563616B CN 105563616 B CN105563616 B CN 105563616B CN 201510940021 A CN201510940021 A CN 201510940021A CN 105563616 B CN105563616 B CN 105563616B
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- C04B35/49—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 containing also titanium oxides or titanates
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- 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
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Abstract
A kind of moulding process of zirconia ceramic product includes the following steps: in proportion to weigh the Zirconium oxide powder of stabilized with yttrium oxide, surfactant, and after ethyl alcohol is added, ball milling mixing, dry, sieving obtains slurry;The slurry is mixed with binder, is kneaded, is granulated, obtain injection feeding, wherein the binder includes each component of following mass parts: polyethylene glycol: 60 parts~65 parts;The high density polyethylene (HDPE) of oxidisability: 15 parts~20 parts;Polyvinyl butyral: 15 parts~20 parts;Stearic acid: 2 parts~3 parts;It is injection moulded the feeding to obtain green body;The green body is placed in water after carrying out water degreasing, thermal debinding obtains blank;The blank is sintered, semi-finished product are obtained;The semi-finished product are machined, are polished, zirconia ceramic product is obtained.The moulding process of above-mentioned zirconia ceramic product, it can be ensured that the ceramic of acquisition has biggish intensity, is not easy to break into pieces, and consistency is higher, hole is uniform.
Description
Technical field
The present invention relates to zirconia ceramics technical fields, more particularly to a kind of forming method of zirconia ceramic product.
Background technique
As novel high-performance ceramics, zirconia ceramics have high intensity, high-fracture toughness, high rigidity and it is excellent every
The attributes such as hot property and high temperature resistance, are widely used in structural ceramics and function ceramics field.In addition, zirconium oxide does not have
It is magnetic, is non-conductive, is non-corrosive, wear-resisting, also using very wide in biomedical apparatus field and stage property, field of tool.Closely
Come, partially stabilized zirconia (TZP) can by powder metallurgy process, prepare keep away the wristwatch case of magnetic, the table part of corrosion resistant and its
Its instrument part.In addition to above-mentioned application, TZP is also widely used in decoration, life, medicine, piezoelectric ceramics, sensor ceramics
Equal fields.
The forming method of existing zirconia ceramics product mainly includes two kinds, i.e. tape casting and ceramic injection forming.
Tape casting is that ceramic powders and organic matter are mixed and made into the slurry with certain viscosity by appropriate proportion, slurry by scraper with
Certain thickness is scraped coated in dedicated base band, and the film as green tape is peeled from above after drying, solidification, then according at
The size and shape of product need to carry out the working processes such as lamination to green compact, then carry out degreasing and sintering obtains ceramics.Ceramic injection
Molding is to obtain green compact by injection molding method, in turn by being mixed with to obtain feeding by ceramic powders and organic matter
It is degreasing sintered to obtain ceramics.The major advantage of the forming method is that moulded products precision is high, and green density is uniform, green strength
Height, sintered body is had excellent performance and the consistency of product quality is good, high degree of automation, can the various complicated shapes of near-net-shape pottery
Porcelain components are suitable for large-scale production.
There is a critically important degreasing link in ceramic injection forming technology, traditional degreasing method is using heating
Mode makes organic binder volatilization or is cracked into gas discharge, i.e. thermal debinding.Since the stomata in injection molding biscuit is complete
It is filled by organic binder, belongs to pore structure of holding one's breath, the gaseous product if heating rate is too fast in thermal debinding, inside green body
It can not be discharged rapidly, air pressure increases the defects of will lead to cracking, bubbling and deformation.Therefore, thermal debinding generally requires tens hours
Time, inefficiency, and be difficult manufacture large-size ceramic product.
Currently, the ceramic mechanical strength as made from Shooting Technique is general, there is also further improved technologies to need
It asks.
Summary of the invention
Based on this, in view of the above-mentioned problems, it is necessary to provide a kind of moulding process of zirconia ceramic product, the pottery that makes
Ceramic products have preferable mechanical performance, and biggish intensity is not easy to break into pieces, and consistency is higher.
A kind of moulding process of zirconia ceramic product, includes the following steps:
The Zirconium oxide powder of stabilized with yttrium oxide, surfactant are weighed in proportion, after ethyl alcohol is added, ball milling mixing is done
Dry, sieving, obtains slurry;
The slurry is mixed with binder, is kneaded, is granulated, obtain injection feeding, wherein the binder includes such as
The each component of lower mass parts: polyethylene glycol: 60 parts~65 parts;The high density polyethylene (HDPE) of oxidisability: 15 parts~20 parts;Polyvinyl alcohol
Butyral: 15 parts~20 parts;Stearic acid: 2 parts~3 parts;
It is injection moulded the feeding to obtain green body;
The green body is placed in water after carrying out water degreasing, thermal debinding obtains blank;
The blank is sintered, semi-finished product are obtained;
The semi-finished product are machined, are polished, zirconia ceramic product is obtained.
The binder includes each component of following mass parts: polyethylene glycol in one of the embodiments: 61 parts~63
Part;The high density polyethylene (HDPE) of oxidisability: 16 parts~18 parts;Polyvinyl butyral: 17 parts~18 parts;Stearic acid: 2 parts~3 parts.
Polyvinyl butyral is reacted by polyvinyl acetate, polyvinyl alcohol and butyraldehyde and is given birth in one of the embodiments,
At hydroxy radical content is 18%~20%, and acetate groups content is 1~25%.
The molecular weight of the polyvinyl alcohol is 2000~4000 in one of the embodiments,.
The partial size of the Zirconium oxide powder of the stabilized with yttrium oxide is 10~150nm in one of the embodiments,.
In one of the embodiments, in the Zirconium oxide powder of the stabilized with yttrium oxide, the molar percentage of yttrium oxide is
2.8%~3.2%.
The surfactant is titanate, stearic acid, phosphate or silane in one of the embodiments,.
The moulding process of above-mentioned zirconia ceramic product, it can be ensured that the ceramic of acquisition has biggish intensity, no
It easily breaks into pieces, and consistency is higher, hole is uniform, and preparation process is simple, easy to operate, and degreasing time is shorter, can be processed after molding
At arbitrary shape and size, it is suitble to extensive, complicated shape product.
Detailed description of the invention
Fig. 1 is the flow diagram of the moulding process of zirconia ceramic product in one embodiment of the invention.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
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
Any and all combinations of relevant listed item.
Referring to Fig. 1, its flow diagram for the moulding process of zirconia ceramic product in one embodiment of the invention.
The moulding process of zirconia ceramic product, includes the following steps:
S110, the Zirconium oxide powder of stabilized with yttrium oxide, surfactant are weighed in proportion, be added ethyl alcohol, after, ball milling is mixed
It closes, dry, sieving obtains slurry.
Effect based on the dispersing agent that ethyl alcohol has especially has fabulous profit to the Zirconium powder of stabilized with yttrium oxide
Wet effect can equably disperse the Zirconium oxide powder of stabilized with yttrium oxide, to reduce the Zirconium oxide powder hair of stabilized with yttrium oxide
Raw the phenomenon that reuniting.In addition, surfactant is added by the Zirconium oxide powder in stabilized with yttrium oxide, it is steady yttrium oxide can be increased
The compatibility of fixed Zirconium oxide powder and ethyl alcohol plays the role of reducing viscosity.Further, surfactant be titanate,
Stearic acid, phosphate or silane.For example, the mass ratio of the surfactant and the Zirconium oxide powder of the stabilized with yttrium oxide is
1~5:100, it is preferred that the mass ratio of the Zirconium oxide powder of the surfactant and the stabilized with yttrium oxide is 2~3:100,
In this way, the viscosity of system can be effectively reduced, increase mobility, the Zirconium oxide powder of stabilized with yttrium oxide is avoided to occur reuniting now
As, but also postorder skimming processes can be conducive to, it avoids excessively increasing postorder degreasing difficulty due to surfactant.
Further, the smaller slurry more evenly of partial size in order to obtain, for example, the ball milling using planetary ball mill into
Row wet ball grinding technique, for another example, Ball-milling Time are 0.5~4h, and rotational speed of ball-mill is 180~220r/min, in this way, can make to aoxidize
Occur adequately to contact and rub between zircon ceramic powder particle and mill ball, so as to obtain the smaller slurry more evenly of partial size
Material.
Further, in order to increase the bond properties of slurry Yu subsequent binder, for example, being also added into mechanical milling process
Starch continues ball milling after starch is added, and Ball-milling Time is 5~30min, and rotational speed of ball-mill is 80~180r/min, in this way, can increase
Add the affinity of pulp surface and binder, to improve the adhesive strength of slurry and binder, avoids in subsequent injection work
The defects of slurry separates with binder and ceramic is caused cracking, deformation occur and be bubbled in skill.
Further, partial size is smaller and the more uniform slurry of partial size in order to obtain, for example, the oxidation of the stabilized with yttrium oxide
The partial size of zirconium powder is 10~150nm, the partial size of the Zirconium powder by controlling stabilized with yttrium oxide, so as to obtained after ball milling
Slurry partial size is smaller, and partial size is more uniform.It should be noted that the Zirconium oxide powder of stabilized with yttrium oxide can pass through in the present embodiment
Existing coprecipitation or organic gel method obtain, and details are not described herein for preparation process.
Further, it in order to reduce the moisture in the slurry after ball milling, avoids due to moisture cladding powder, in mixing process
Middle moisture can sharply gasify, and cause to generate bubble in feeding, for example, the particulate matter after ball milling is put in a drying box drying, do
Dry temperature is 60~80 DEG C, and the dry time is that 6~12h is avoided with removing the moisture in slurry due to moisture coated composite powder
End, moisture can sharply gasify in mixing process, cause to generate bubble in feeding.Further, dry temperature is 60 DEG C, is done
The dry time is 10h, and the fusing of surfactant is caused when to avoid drying, causes adhesion and the powder surface level of coverage of powder
Change.Preferably, the solid content of slurry is 48%~52% after drying, so that slurry has lower viscosity, avoids slurry
Reunion.
Further, in order to reduce subsequent sintering temperature, the consistency of ceramic is improved, for example, the institute after ball milling
The average grain diameter for stating slurry is 0.5~0.8 micron, it is preferred that the average grain diameter of the slurry after ball milling is 0.4~0.5 micro-
Rice, in this way, the slurry surface with higher after ball milling can be enable, so that the pelletizing sintering with higher after being granulated
Activity, and then subsequent sintering temperature is reduced, while the consistency of obtained ceramic also can be improved.
Further, in order to improve the uniformity of slurry particle diameter distribution, for example, passing through the particulate matter after drying 200
It is sieved under purpose sieve, the minus mesh of collection is slurry, in this way, the uniformity of slurry can be improved, is conducive to subsequent work
Sequence.
It is appreciated that the yttrium oxide in yttrium oxide-stabilized zirconium oxide powder can make Phase Transformation of Zirconia stable state or metastable
State, the features such as making it have good heat-resisting, corrosion-resistant, toughening.Yttrium oxide can in wide temperature range stable cubic or
Tetragonal phase zirconium oxide has good effect to the stabilization of material property.In the present embodiment, the zirconium oxide of the stabilized with yttrium oxide
In powder, the molar percentage of yttrium oxide is 2.8%~3.2%, to improve the performance of ceramic.
S102, the slurry is mixed with binder, is kneaded, is granulated, obtains the feeding for injection;
For example, the binder includes polyethylene glycol, the high density polyethylene (HDPE) of oxidisability, polyvinyl butyral and tristearin
Acid.Polyethylene glycol is water-soluble, and dissolution and diffusion rate are all very fast under certain water temperature, in the at a temperature of viscosity of mixing and injection
It is lower.Polyvinyl butyral is not soluble in water, and swelling action does not occur, and in the removing of main binder Aqueous Solutions of Polyethylene Glycol, rises
Skeleton function keeps the intensity of green body.The high density polyethylene (HDPE) of oxidisability and the compatibility of polyethylene glycol are than general polyethylene
It is much better, it is able to maintain blank strength and dimensional stability in the hot water, and the high density polyethylene (HDPE) of oxidisability has low viscosity
Property, the viscosity caused by polyvinyl butyral increased a buffer function.Stearic acid can increase slurry with it is organic
The compatibility of body plays the role of reducing viscosity.But also can serve as a connection between organism and powder particle, it prevents
Two-phase laminated flow guarantees the uniform of mixing, and plays lubrication between powder particle, between powder particle and injection mold and make
With to reach smooth injection molding effect.For example, the binder includes each component of following mass parts: polyethylene glycol:
60 parts~65 parts;The high density polyethylene (HDPE) of oxidisability: 15 parts~20 parts;Polyvinyl butyral: 15 parts~20 parts;Stearic acid: 2
Part~3 parts.
Further, in order to improve the consistency and intensity of ceramic, for example, the binder includes following mass parts
Each component: polyethylene glycol: 61 parts~63 parts;The high density polyethylene (HDPE) of oxidisability: 16 parts~18 parts;Polyvinyl butyral:
17 parts~18 parts;Stearic acid: 2 parts~3 parts.When the content of polyvinyl alcohol is less, the mobility of pelletizing is poor, and injection is relatively tired
Difficulty, and it is easy the defects of causing crackle in green body, so that the bulk density and intensity of ceramic obtained are smaller;And poly- second
Glycol content is more, and the mobility of feeding is preferable, but after polyethylene glycol removing, plays the polyvinyl butyral content of skeleton function
Less, framework compound does not play the role of due, and polymer molecular chain sliding causes the movement of powder granule, occurs one
Fixed fault of construction, so that the bulk density and intensity of ceramic obtained are smaller.By adjusting each component in binder
The bulk density of ceramic can be improved in ratio, makes it have higher consistency and intensity.
Further, polyvinyl butyral is terpolymer, is reacted by polyvinyl acetate, polyvinyl alcohol and butyraldehyde
It generates, hydroxy radical content is 18%~20%, and acetate groups content is 0~25%, and fusing point is higher, after guaranteeing polyethylene glycol removing
The structural strength of green body.
In the present embodiment, the molecular weight of the polyvinyl alcohol is 2000~4000, soluble easily in water, and viscosity is lower, and
And the intensity of green body can be enhanced, guarantee fast demoulding after injection.
It is appreciated that pelletizing must have good mobility, thus need in order to guarantee going on smoothly for injection technique
Improve the content of binder in feeding;However due to injection-molded product sintering after dimensional contraction it is very big, for prevent deformation and
Dimensional accuracy is controlled, and the useful load of pelletizing ceramic powders must be improved.Preferably, the matter of the slurry and the binder
Amount is than being 3~5:1.It is furthermore preferred that the mass ratio of the slurry and the binder is 4:1, in this way, slurry can be equal with binder
Even mixing, after binder removes completely, the zirconia particles in green body can be tightly packed, and the fault of construction of formation is less,
To improve the intensity and toughness of ceramic.
In order to make Zirconium oxide powder and binder is sufficiently mixed uniformly so that after mixing particle mobility, guarantee to inject
Technique is gone on smoothly, for example, being kneaded under conditions of on double roller shearing kneading machine in 150~200 DEG C, mixing time is
0.5~3h.Further, the temperature of mixing is 160~180 DEG C, and mixing time is 2~3h.In this way, slurry and bonding can be made
Agent is sufficiently mixed uniformly so that mixing after particle mobility, guarantee going on smoothly for injection technique.
In the present embodiment, it after the cooling drying of product will be kneaded, cuts and is granulated in pelletizer, obtain injection feeding.
For example, the partial size of the feeding after being granulated is 1~2mm.In order to be sufficiently mixed Zirconium oxide powder and binder uniformly, for example, institute
State mixing action and granulation operations circulation three times.After being kneaded, it is granulated, then be kneaded, be granulated, be kneaded again, be granulated, so that oxygen
Change zirconium powder to be sufficiently mixed with binder, to guarantee going on smoothly for injection technique.
Further, in order to avoid oxygenolysis occurs in mixing process in binder, for example, being also added into binder
The antioxidant that mass parts are 0.5~1 part, this way it is possible to avoid oxygenolysis occurs in mixing process in binder, to improve
The intensity of green body.
S103, it is injection moulded the feeding to obtain green body.
For example, injection feeding is placed in injection (mo(u)lding) machine heating transformation in toughness melt, in certain temperature and
It injects in metal die at a high speed, is cooled and solidified as the green body of required shape, demoulding under pressure.
It will affect the complete of mold filling process since injection pressure is too small, cause to short, increase injection pressure and be conducive to mold filling
Flow process, but may be that green body generates biggish residual stress, cause fracture or overlap, therefore, in order to reduce injection
Defect, for example, injection pressure is 20~200MPa.For another example, injection pressure is 60~160MPa.For another example, injection pressure be 100~
120MPa, in this way, both mold filling can be made complete, and can be to avoid occurring being broken in injection process or overlap.
Further, injection temperature is 130~170 DEG C, it is furthermore preferred that injection temperature is 150~160 DEG C.In this way, can be with
Keep mold filling complete, the volatilization of organic matter in feeding can also be avoided and form stomata in green body, improve the consistency of green compact.
Further, in order to improve the quality of injection, for example, mould temperature is 40~60 DEG C in injection process, pressure maintaining is 80~
100MPa, dwell time are 10~20s, in this way, being conducive to the consistency of green body after raising injection, improve the quality of green body.It is excellent
Choosing, after obtaining green body, also execution step: some time is stood in hyperbaric environment, for example, in 20~40MPa stand 1~
5 minutes.Preferably, the slow discharge in injection molding pressure maintaining environment, so that it is down to 20MPa after 1~5 minute hereinafter,
Such as in pressure maintaining environment, pressure maintaining is 80~100MPa, and the dwell time is 10~20s;For example, being released by 0.2MPa/3 seconds speed
Pressure;Preferably, when being down to 20MPa or less, by 0.1MPa/3 seconds speed discharges;In this way, being conducive to green body after raising injection
Consistency, to effectively increase the quality of green body.
Further, the feeding is injection moulded after obtaining green body, further includes that dyeing detection is carried out to the green body.Example
Such as, after the green body being placed in color different from impregnating 3~4h under conditions of temperature is 30 DEG C in the ink of green body color, fishing
Out, it is placed in clear water and cleans, whether observation green body is colored, if the face of the surface color of the blank and the blank itself
The ratio that the identical area of color accounts for the gross area is more than 90%, then illustrates that the blank inside solid is uniform, the ceramics finally obtained
Product it is up-to-standard.If green body color is entirely different with intrinsic colour, show existing defects inside green body, then it can be by it
Give up, saves subsequent procedure of processing, save the cost.
S104, by the green body be placed in water carry out water degreasing after, thermal debinding obtains blank.
1~5h of water degreasing is carried out for example, the green body is placed in the deionized water that temperature is 40~60 DEG C, then 50
Under conditions of~80 DEG C after drying, thermal debinding.
It is appreciated that water temperature is higher, the solution rate of polyethylene glycol is faster, that is, water degreasing efficiency is higher, still, works as water
When temperature is more than certain temperature, the swelling rate for easily leading to polyethylene glycol is too fast and causes body defect, therefore, de- in order to improve water
Rouge efficiency, while body defect is avoided, water degreasing is carried out for example, green body is placed in the deionized water that temperature is 45~50 DEG C.
In this way, water degreasing efficiency both can be improved, while green body can also be avoided defect occur and influence the consistency of ceramic.Again
Such as, water degreasing time can also avoid the too long shadow of degreasing time in this way, the polyethylene glycol of larger proportion can be removed for 3~4h
Ring production efficiency.One preferable example is that the temperature of water degreasing is 50 DEG C, and the time of water degreasing is 4h, in this way, polyethylene glycol
Removal efficiency can reach 75%.
In order to improve water degreasing efficiency, for example, using stirring operation, stirring can accelerate the stream of water in water skimming processes
Dynamic speed, allows fresh water to reach the stomata network formed inside the surface and green body of green body, accelerates poly- second two
The course of dissolution of alcohol.For another example, the water skimming processes are carried out using ultrasonic wave.For another example, the power of ultrasonic wave is 1~2KW, this
Sample can accelerate the efficiency of water degreasing, also can avoid body defect.
Further, it in order to avoid generating stomata in thermal degreasing process, for example, green body is dried after water degreasing, does
Dry temperature is 80~100 DEG C, and drying time is 2~4 hours, to remove the moisture of billet surface and inside, is avoided subsequent
In thermal degreasing process, the Quick-gasifying of moisture causes green body to generate stomata, influences the consistency of ceramic.
Further, in order to remove remaining organic matter in green body, while the consistency of green body is improved, for example, by green body
It is placed in high temperature furnace, under normal temperature state, is warming up to 600 DEG C with the heating rate of 5~10 DEG C/min and keeps the temperature 1~3 hour, with
Remaining organic matter in green body is sloughed, while improving the consistency of green body.Preferably, under normal temperature state, with 3~5 DEG C of liter
Warm rate is warming up to 200 DEG C, then is warming up to 400 DEG C with 0.5~2 DEG C of heating rate and keeps the temperature 1h, then with 1~2 DEG C of heating
Rate rises to 600 DEG C, and keeps the temperature 1h, to remove remaining organic matter in green body, while also can avoid the too fast shadow of organic matter volatilization
Ring consistency.
Since water degreasing is stripped of most polyethylene glycol from green body, via outer and inner shape inside green body
At continuous air vent channel, the high density polyethylene (HDPE) of binder polyvinyl butyral not soluble in water and oxidisability is support
Green body, these ducts also become the path that they heat green body of escaping when removing later.Accordingly, with respect to traditional degreasers
Skill, degreasing time can be greatly reduced by carrying out thermal debinding again after water degreasing, improve production efficiency.
S105, the blank is sintered, obtains semi-finished product.
For example, the temperature of the sintering is 1300~1800 DEG C.For another example, the temperature of the sintering is 1450~1650 DEG C.
For another example, the time of the sintering is 10~16h.When sintering temperature is lower, ceramics are unable to densified sintering product, and the porosity is larger, intensity
It is lower with toughness;When sintering temperature is higher, a degree of burn-off phenomenon, abnormal grain growth, so as to cause pottery may cause
The porosity of porcelain increases, and bending strength and fracture toughness reduce.
Although it is appreciated that the step of have passed through water degreasing and thermal debinding, it is also possible to having there are some in blank green body
Machine binder, disposably heat up it is excessively high be easy to be allowed to gasify suddenly generate stomata.In addition, due to by water degreasing and thermal debinding
It after step, is inevitable in blank with hole, consequence caused in this way is in sintering step, and there are one for these holes
A process for being expanded into contraction, last product with respect to blank for, in volume can exist 20% or more variation, therefore, such as
Fruit sintering temperature, temperature-rise period are improper, these holes can generate many not noticeable crackles, cause product strength to decline, together
When cause hole uneven, therefore low density in order to improve the quality of ceramic, reduces internal flaw, for example, will give birth to
Base is placed in high temperature furnace and is heated to 600 DEG C with the heating rate of 3 DEG C/min, and keeps 1h at 600 DEG C, then with 10 DEG C/min
Heating rate be heated to 1450~1500 DEG C, 2~4h of isothermal sintering cools to room temperature with the furnace after sintering.It is appreciated that burning
When junction temperature is lower than 600 DEG C, the burn off process of the exclusion of moisture and binder mainly in green body, with mentioning for sintering temperature
The shrinking percentage of height, green body gradually increases, but increased rate is slower, when sintering temperature reaches 1200 DEG C or more, green body shrinking percentage
Increase suddenly, green body inner air vent excludes rapidly, reaches densification.Preferably, in order to further increase the consistency of blank, example
Such as, green compact are placed in high temperature furnace and are heated to 800 DEG C with the heating rate of 3 DEG C/min, and keep 1h viscous to remove at 800 DEG C
Agent and dispersing agent are tied, is then heated to 1200 DEG C with the heating rate of 10 DEG C/min, then with the heating rate liter of 3~5 DEG C/min
For temperature to 1500,2~4h of isothermal sintering cools to room temperature with the furnace after sintering, so that the intracorporal stomata of base sufficiently excludes, makes
Blank consistency is higher.One preferable example is under normal temperature state, to be warming up to the heating rate of 1.0~1.5 DEG C/min
100 DEG C, kept for 100 DEG C 0.5 hour;Then 450 DEG C are warming up to the heating rate of 0.8~1.2 DEG C/min, are kept for 450 DEG C 0.5
Hour;Then 800 DEG C are warming up to the heating rate of 1.1~1.5 DEG C/min, are kept for 800 DEG C 0.5 hour;Then with 0.8~
The heating rate of 1.2 DEG C/min is warming up to 1000 DEG C, is kept for 1000 DEG C 0.5 hour;Then with the heating of 1.0~1.5 DEG C/min
Rate is warming up to 1200 DEG C, is kept for 1200 DEG C 0.5 hour;Then 1450 are warming up to the heating rate of 1.0~1.5 DEG C/min
DEG C, kept for 1450 DEG C 4 hours;Then 1000 DEG C are being cooled to the rate of temperature fall of 1.5~2.0 DEG C/min;Last natural cooling
The defects of to room temperature, being sintered by way of gradually heating up, stomata, crackle being generated to avoid product uneven heating.
S106, the semi-finished product are machined, are polished, obtaining zirconia ceramic product.
Specifically, semi-finished product are roughly ground by Carborundum wheel, are refined, and the semi-finished product after polishing are placed in sand mill
In be processed by shot blasting, make ceramic have mirror finish effect, improve the apparent effect of ceramic.It needs to illustrate
It is that other processing can also be carried out to semi-finished product according to specific needs, for example, sandblasting etc..
It should be noted that the ceramic that the present invention is prepared may include the shell of mobile phone, tablet computer etc.
Part perhaps mechanical parts such as the automobile parts such as spark plug, valve, piston, nozzle or gear, cutter, sealing element etc..
The moulding process of above-mentioned zirconia ceramic product, it can be ensured that the ceramic of acquisition has biggish intensity, no
It easily breaks into pieces, and consistency is higher, hole is uniform.Ceramic bulk density produced by the present invention is greater than 2.8g/cm3, 3 points curved
Qu Qiangdu is greater than 300MPa.
In addition, the moulding process of above-mentioned zirconia ceramic product, preparation process is simple, easy to operate, and degreasing time is shorter, at
It can be processed into arbitrary shape and size after type, be suitble to extensive, complicated shape product.
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 (6)
1. a kind of moulding process of zirconia ceramic product, which comprises the steps of:
The Zirconium oxide powder of stabilized with yttrium oxide, surfactant are weighed in proportion, after ethyl alcohol is added, ball milling mixing, dry, mistake
Sieve, obtains slurry;The mass ratio of the Zirconium oxide powder of the surfactant and the stabilized with yttrium oxide is (2~3): 100;?
It is also added into starch in mechanical milling process, continues ball milling after starch is added, Ball-milling Time is 5min~30min, and rotational speed of ball-mill is
80r/min~180r/min;The partial size of the Zirconium oxide powder of the stabilized with yttrium oxide is 10nm~150nm;By after ball milling
Grain object puts in a drying box drying, and dry temperature is 60 DEG C~80 DEG C, and the dry time is 6h~12h, slurry after drying
Solid content is 48%~52%, and the average grain diameter of the slurry after ball milling is 0.4~0.5 micron;
The slurry is mixed with binder, is kneaded, is granulated, obtain injection feeding, wherein the binder includes following matter
Measure each component of part: polyethylene glycol: 60 parts~65 parts;The high density polyethylene (HDPE) of oxidisability: 15 parts~20 parts;Polyvinyl alcohol contracting fourth
Aldehyde: 15 parts~20 parts;Stearic acid: 2 parts~3 parts;The mass ratio of the slurry and the binder is 3~5:1;It is sheared in double roller
It is kneaded under conditions of 150 DEG C~200 DEG C on kneading machine, mixing time is 0.5h~3h;
It is injection moulded the feeding to obtain green body;Wherein, injection pressure is 100MPa~120MPa, and injection temperature is 150 DEG C
~160 DEG C;In injection process, mould temperature is 40 DEG C~60 DEG C, and pressure maintaining is 80MPa~100MPa, and the dwell time is 10s~20s;
The green body is placed in water after carrying out water degreasing, thermal debinding obtains blank;Wherein, green body is placed in temperature is 50 DEG C
Deionized water in carry out water degreasing, time of water degreasing is 4h;In water skimming processes, using stirring operation;It is right after water degreasing
Green body is dried, and dry temperature is 80~100 DEG C, and drying time is 2~4 hours;Green body is placed in high temperature furnace, from normal
Under temperature state, 200 DEG C are warming up to 3~5 DEG C of heating rate, then be warming up to 400 DEG C with 0.5~2 DEG C of heating rate and protect
Warm 1h, then 600 DEG C are risen to 1~2 DEG C of heating rate, and keep the temperature 1h, to remove remaining organic matter in green body;
The blank is sintered, semi-finished product are obtained;Wherein, blank is placed in high temperature furnace, under normal temperature state, with 1.0
The heating rate of~1.5 DEG C/min is warming up to 100 DEG C, keeps at 100 DEG C 0.5 hour;Then with the liter of 0.8~1.2 DEG C/min
Warm rate is warming up to 450 DEG C, keeps at 450 DEG C 0.5 hour;Then 800 are warming up to the heating rate of 1.1~1.5 DEG C/min
DEG C, it keeps at 800 DEG C 0.5 hour;Then 1000 DEG C are warming up to the heating rate of 0.8~1.2 DEG C/min, kept at 1000 DEG C
0.5 hour;Then 1200 DEG C are warming up to the heating rate of 1.0~1.5 DEG C/min, kept at 1200 DEG C 0.5 hour;Then
1450 DEG C are warming up to the heating rate of 1.0~1.5 DEG C/min, is kept at 1450 DEG C 4 hours;Then with 1.5~2.0 DEG C/
The rate of temperature fall of min is cooled to 1000 DEG C;Last cooled to room temperature;
The semi-finished product are machined, are polished, zirconia ceramic product is obtained.
2. the moulding process of zirconia ceramic product according to claim 1, which is characterized in that the binder includes such as
The each component of lower mass parts: polyethylene glycol: 61 parts~63 parts;The high density polyethylene (HDPE) of oxidisability: 16 parts~18 parts;Polyvinyl alcohol
Butyral: 17 parts~18 parts;Stearic acid: 2 parts~3 parts.
3. the moulding process of zirconia ceramic product according to claim 1, which is characterized in that polyvinyl butyral by
Polyvinyl acetate, polyvinyl alcohol and butyraldehyde reaction generate, hydroxy radical content be 18%~20%, acetate groups content be 1~
25%.
4. the moulding process of zirconia ceramic product according to claim 1, which is characterized in that point of the polyvinyl alcohol
Son amount is 2000~4000.
5. the moulding process of zirconia ceramic product according to claim 1, which is characterized in that the stabilized with yttrium oxide
In Zirconium oxide powder, the molar percentage of yttrium oxide is 2.8%~3.2%.
6. the moulding process of zirconia ceramic product according to claim 1, which is characterized in that the surfactant is
Titanate, stearic acid, phosphate or silane.
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