CN108409323A - A kind of production method of ecru zirconia ceramics - Google Patents
A kind of production method of ecru zirconia ceramics Download PDFInfo
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Abstract
The present invention relates to a kind of production methods of ecru zirconia ceramics, first, colorant and zirconium oxide are taken to be put into the abundant mix grinding of ball mill, obtain formula grain and draw；Again formula grain is drawn to be put into 110 DEG C~150 DEG C of mixer and be puddled, auxiliary material is added when puddling rotation and is kneaded, mixing materials body is obtained；Mixing materials body is cooled to 28 DEG C from mixer taking-up；Mixing materials body after cooling is put into crusher and is crushed, feeding is obtained；Feeding is put into vacuum drier again to dry, it is spare that the feeding after drying can be used directly or be put into storage in vacuum drying storage bin；Feeding after drying is molded by injection molding machine to obtain the molding element embryo of required shape；The plain embryo of molding is subjected to degreasing successively and sintering obtains mature embryo；Mature embryo is polished to obtain final ceramic product.The production method of above-mentioned ecru zirconia ceramics has the function of the advantages of high temperature resistance, be uniformly dispersed, toner is inhibited to decompose volatilization.
Description
Technical field
The present invention relates to a kind of manufacturing method of ceramic, especially a kind of production method of ecru zirconia ceramics.
Background technology
Zirconia ceramics since with good toughness, be otherwise known as Ceramo-steel, is widely applied on structural member, and its
The unique metal gloss having, which makes it again, becomes the favorite of appearance member.Other metal oxides are added in zirconium oxide to be made
It generates colored decorative effect, especially black and uses widely, such as watchcase, ornaments.Existing black zirconia color
Material is most of to use aluminium oxide, iron oxide, the oxides such as nickel oxide, generates black spinel to dye, at low cost, is easy system
It is standby.
But the degree of blackness of the black pigment of existing zirconia ceramics is low, and colorant is ball milling mixing (solid phase method)
It prepares, uneven color easy tos produce aberration；In addition, other ecru zirconia ceramics are coloured by coloring solution,
Toner easily decomposes volatilization, the zirconia ceramics after coloring, and the unstable easy decomposition volatilization of color keeps entire zirconia ceramics eclipsed.
Invention content
In view of above-mentioned condition, it is necessary to which a kind of ecru for having high temperature resistance, being uniformly dispersed, toner being inhibited to decompose volatilization is provided
The production method of zirconia ceramics.
In order to solve the above technical problems, providing a kind of production method of ecru zirconia ceramics, include the following steps：
S1, it takes colorant and zirconium oxide particle or powder to be put into the abundant mix grinding of ball mill, obtains formula grain and draw；
S2, again formula grain is drawn to be put into mixer and is puddled, auxiliary material is added when puddling rotation and is kneaded, is kneaded
Expect body；
S3, mixing materials body is taken out into cooling from mixer；
S4, it the mixing materials body after cooling is put into crusher is crushed, obtain feeding；
S5, it feeding is put into vacuum drier again dries, it is dry that the feeding after drying can be used directly or be put into vacuum
Storage is spare in dry storage bin；
S6, the feeding after drying is molded by injection molding machine to obtain the molding element embryo of required shape；
S7, the plain embryo of molding is subjected to degreasing and sintering obtains mature embryo successively；
S8, mature embryo is polished to obtain final ceramic product；
Wherein, it is described formula grain draw be put into mixer mix mixing temperature be 110 DEG C~150 DEG C, the mixing materials body
It is cooled after being taken out from mixer to the break process in progress step S4 after 28 DEG C；
The auxiliary material includes wax, zirconium powder and plastics, and according to mass percent meter, the mixing materials body includes：82%~
90% zirconium oxide particle, powder and zirconium powder, 5%~15% colorant, remaining is wax, the filling plastic of equivalent；
The colorant by mass percentage, includes 20%~80% nano-cerium oxide, 10%~20% nano oxygen
Change aluminium.
In the production method of aforementioned present invention ecru zirconia ceramics, in step sl, the colorant passes through 100 mesh
After sieving 12 times the abundant mix grinding of ball mill is put into togerther with the zirconium oxide particle or powder.
In the production method of aforementioned present invention ecru zirconia ceramics, in step sl, the colorant and zirconium oxide
The time that particle or powder are put into the abundant mix grinding of ball mill is 12 hours.
In the production method of aforementioned present invention ecru zirconia ceramics, in step S4, mixing materials body is put into broken
It is crushed in machine, obtains the feeding of a diameter of 1mm-2mm.
In the production method of aforementioned present invention ecru zirconia ceramics, in the step s 7, it is molded plain embryo and is placed in dumping
In stove degreasing is carried out in the environment of 400 DEG C~700 DEG C.
In the production method of aforementioned present invention ecru zirconia ceramics, in the step s 7, by the molding element after degreasing
Embryo is placed in sintering furnace, passes sequentially through the first heating phase, the first soak, the second temperature raising period, the second soak, third heating
Phase, third soak and the first catathermal sintering form mature embryo, and specific sintering temperature, time parameter include as follows：
S71, the first heating phase：In 2 hours, sintering in-furnace temperature is risen to 500 DEG C from room temperature；
S72, the first soak：It is constant at 500 DEG C that in-furnace temperature will be sintered, keep the temperature 10 hours；
S73, the second temperature raising period：In 5 hours, sintering in-furnace temperature is risen to 1100 DEG C from 500 DEG C；
S74, the second soak：It is constant at 1100 DEG C that in-furnace temperature will be sintered, keep the temperature 3 hours；
S75, third temperature raising period：In 5 hours, sintering in-furnace temperature is risen to 1320 DEG C from 1100 DEG C；
S76, third soak：It is constant at 1320 DEG C that in-furnace temperature will be sintered, keep the temperature 2 hours；
S77, the first cooldown period：In 12 hours, sintering in-furnace temperature is down to 50 DEG C from 1300 DEG C.
In the production method of above-mentioned ecru zirconia ceramics, zirconium oxide color ceramics be using high-purity mangesium oxide zirconium body with
Toner is allocated and then is obtained after not being in the mood for ball mill ball milling formula grain and draws in proportion, and formula grain is then introduced row heating mixing,
Mixing materials body is obtained after other auxiliary material auxiliary agents are added in heating internal mixing pass and are kneaded a few hours, then breaks mixing materials body
It is broken to obtain feeding, it suppresses to obtain using molding die and is molded plain embryo, finally pass through degreasing, mature embryo is made in sintering, it will be ripe
Embryo obtains finished product by post-processing polishing, the ecru zirconia ceramics of making can be widely applied to medical instrument, machinery,
A variety of industries such as military project, intelligence wearing, material have the effects that wear-resisting, high temperature resistant, anticorrosion, antistatic, impermeable non-
Metal material.
Description of the drawings
Fig. 1 is the production method flow diagram of ecru zirconia ceramics of the present invention.
Fig. 2 be ecru zirconia ceramics of the present invention production method in step S7 sintering temperatures-time parameter curve graph.
Fig. 3 is a finished figure of ecru zirconia ceramics of the present invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The production method of ecru zirconia ceramics of the present invention is further elaborated.It should be appreciated that described herein specific
Embodiment only to explain the present invention, is not intended to limit the present invention.
Fig. 1 is referred to, a kind of production method of ecru zirconia ceramics of the embodiment of the present invention includes the following steps：
S1, prepare batch mixing first, take colorant and zirconium oxide particle or powder to be put into the abundant mix grinding of ball mill, be formulated
Grain draws；
S2, again formula grain is drawn to be put into mixer and is puddled, auxiliary material is added when puddling rotation and is kneaded, is kneaded
Expect body；
S3, mixing materials body is taken out into cooling from mixer；
The S4 and then mixing materials body after cooling is put into crusher is crushed, and obtains feeding；
S5, it feeding is put into vacuum drier again dries, it is dry that the feeding after drying can be used directly or be put into vacuum
Storage is spare in dry storage bin；
S6, the feeding after drying is molded to obtain the molding element embryo of required shape by injection molding machine, injection molding machine injection molding uses
The each withdrawal amount of drying feeding should be finished in 2 hours, avoid long-time ingress of air and make moist；
S7 and then the plain embryo of molding is subjected to degreasing and sintering obtains mature embryo successively；
S8, mature embryo is polished to obtain final ceramic product, as shown in Figure 3；
In above-mentioned steps, it is described formula grain draw be put into mixer mix mixing temperature be 110 DEG C~150 DEG C, it is described
Mixing materials body is cooled after being taken out from mixer to the break process in progress step S4 after 28 DEG C.
In the production method of ecru zirconia ceramics of the present invention, formula grain, which draws to be put into mixer, to be puddled, and is being puddled
Auxiliary material is added when rotation to be kneaded, after being kneaded a few hours, takes out and is granulated, wherein auxiliary material includes wax, zirconium powder and plastics, is pressed
According to mass percent meter, mixing materials body in step s 2 includes：82%~90% zirconium oxide particle, powder and zirconium powder, 2%
~15% colorant, remaining is wax, the filling plastic of equivalent, and the mixing materials body obtained by the method has high temperature resistance, dispersion
Uniformly, toner is inhibited to decompose the effect of volatilization.
In the production method of ecru zirconia ceramics of the present invention, the colorant include nickel oxide, zinc oxide and
Titanium oxide, by mass percentage, including 20%~80% nano-cerium oxide, 10%~20% nano aluminium oxide.
In the production method of ecru zirconia ceramics of the present invention, in step S1, when preparing colorant, colorant is led to first
Sieve with 100 mesh sieve and be put into togerther the abundant mix grinding of ball mill with zirconium oxide particle or powder after sieve 12 times, colorant and zirconium oxide particle or
The time that powder is put into the abundant mix grinding of ball mill is 12 hours.
In step S4, mixing materials body is put into crusher and is crushed, obtains the feeding of a diameter of 1mm-2mm.
In the step s 7, the plain embryo of molding is placed in draft glue discharging furnace carries out degreasing in the environment of 400 DEG C~700 DEG C.
Embodiment one
In the production method of present embodiment, the formula grain in step S1 draws, and by mass percentage, includes 82% oxygen
Change zirconium particle, 5% colorant, 7.5% wax and 7.5% plastics, is put into togerther in mixer and puddles, be kneaded, obtained
Mixing materials body；
Embodiment two
In the production method of present embodiment, the formula grain in step S1 draws, and by mass percentage, includes 85% oxygen
Change zirconium particle, 7% colorant, 4% wax and 4% plastics, is put into togerther in mixer and puddles, be kneaded, is kneaded
Expect body；
Embodiment three
In the production method of present embodiment, the formula grain in step S1 draws, and by mass percentage, includes 90% oxygen
Change zirconium particle, 5% colorant, 2.5% wax and 2.5% plastics, is put into togerther in mixer and puddles, be kneaded, obtained
Mixing materials body；
Example IV
In the production method of present embodiment, in the colorant in step S1, by mass percentage, include 20% nanometer
Cerium oxide, 10% nano aluminium oxide.
Embodiment five
Embodiment five
In the production method of present embodiment, in the colorant in step S1, by mass percentage, include 50% nanometer
Cerium oxide, 15% nano aluminium oxide.
Embodiment six
In the production method of present embodiment, in the colorant in step S1, by mass percentage, include 80% nanometer
Cerium oxide, 20% nano aluminium oxide.
As shown in Fig. 2, in the step s 7, the molding element embryo after degreasing being placed in sintering furnace, the first heating is passed sequentially through
Phase, the first soak, the second temperature raising period, the second soak, third temperature raising period, third soak and the first catathermal sintering shape
At mature embryo, specific sintering temperature, time parameter include as follows：
S71, the first heating phase：In 2 hours, sintering in-furnace temperature is risen to 500 DEG C from room temperature；
S72, the first soak：It is constant at 500 DEG C that in-furnace temperature will be sintered, keep the temperature 10 hours；
S73, the second temperature raising period：In 5 hours, sintering in-furnace temperature is risen to 1100 DEG C from 500 DEG C；
S74, the second soak：It is constant at 1100 DEG C that in-furnace temperature will be sintered, keep the temperature 3 hours；
S75, third temperature raising period：In 5 hours, sintering in-furnace temperature is risen to 1320 DEG C from 1100 DEG C；
S76, third soak：It is constant at 1320 DEG C that in-furnace temperature will be sintered, keep the temperature 2 hours；
S77, the first cooldown period：In 12 hours, sintering in-furnace temperature is down to 50 DEG C from 1300 DEG C.
Zirconium oxide color ceramics are to be allocated in proportion and then using high-purity mangesium oxide zirconium body and toner through not being in the mood for ball mill ball
Formula grain is obtained after mill to draw, and formula grain is then introduced into row heating mixing, other auxiliary material auxiliary agents are added in heating internal mixing pass
Mixing materials body is obtained after being kneaded a few hours, then is crushed mixing materials body to obtain feeding, be suppressed using molding die
To the plain embryo of molding, finally pass through degreasing, the obtained mature embryo of sintering, mature embryo is obtained into finished product by post-processing polishing, is made
The ecru zirconia ceramics of work can be widely applied to a variety of industries such as medical instrument, machinery, military project, intelligence wearing, material
Have the effects that wear-resisting, high temperature resistant, anticorrosion, antistatic, impermeable non-metallic material.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as be without departing from technical solution of the present invention content, it is right according to the technical essence of the invention
Any simple modification, equivalent change and modification made by above example, in the range of still falling within technical solution of the present invention.
Claims (6)
1. a kind of production method of ecru zirconia ceramics, which is characterized in that include the following steps：
S1, it takes colorant and zirconium oxide particle or powder to be put into the abundant mix grinding of ball mill, obtains formula grain and draw；
S2, again formula grain is drawn to be put into mixer and is puddled, auxiliary material is added when puddling rotation and is kneaded, mixing materials are obtained
Body；
S3, mixing materials body is taken out into cooling from mixer；
S4, it the mixing materials body after cooling is put into crusher is crushed, obtain feeding；
S5, it feeding is put into vacuum drier again dries, the feeding after drying can be used directly or be put into vacuum drying
Storage is spare in storage bin；
S6, the feeding after drying is molded by injection molding machine to obtain the molding element embryo of required shape；
S7, the plain embryo of molding is subjected to degreasing and sintering obtains mature embryo successively；
S8, mature embryo is polished to obtain final ceramic product；
Wherein, the formula grain draws that be put into the temperature that mixing is mixed in mixer be 110 DEG C~150 DEG C, and the mixing materials body is from close
Mill is cooled after taking out to the break process in progress step S4 after 28 DEG C；
The auxiliary material includes wax, zirconium powder and plastics, and according to mass percent meter, the mixing materials body includes：82%~90%
Zirconium oxide particle, powder and zirconium powder, 2%~15% colorant, remaining be equivalent wax, filling plastic；
The colorant by mass percentage, includes 20%~80% nano-cerium oxide, 10%~20% nano aluminium oxide.
2. the production method of ecru zirconia ceramics as claimed in claim 3, it is characterised in that：In step sl, described
Colorant is logical to be sieved with 100 mesh sieve and is put into togerther the abundant mix grinding of ball mill with the zirconium oxide particle or powder after sieve 12 times.
3. the production method of ecru zirconia ceramics as described in claim 1, it is characterised in that：In step sl, described
The time that colorant is put into the abundant mix grinding of ball mill with zirconium oxide particle or powder is 12 hours.
4. the production method of ecru zirconia ceramics as described in claim 1, it is characterised in that：In step S4, it will be kneaded
Material body, which is put into crusher, to be crushed, and the feeding of a diameter of 1mm-2mm is obtained.
5. the production method of ecru zirconia ceramics as described in claim 1, it is characterised in that：In the step s 7, it is molded
Plain embryo is placed in draft glue discharging furnace carries out degreasing in the environment of 400 DEG C~700 DEG C.
6. the production method of ecru zirconia ceramics as described in claim 1, it is characterised in that：In the step s 7, it will take off
Molding element embryo after fat is placed in sintering furnace, passes sequentially through the first heating phase, the first soak, the second temperature raising period, the second heat preservation
Phase, third temperature raising period, third soak and the first catathermal sintering form mature embryo, specific sintering temperature, time parameter packet
It includes as follows：
S71, the first heating phase：In 2 hours, sintering in-furnace temperature is risen to 500 DEG C from room temperature；
S72, the first soak：It is constant at 500 DEG C that in-furnace temperature will be sintered, keep the temperature 10 hours；
S73, the second temperature raising period：In 5 hours, sintering in-furnace temperature is risen to 1100 DEG C from 500 DEG C；
S74, the second soak：It is constant at 1100 DEG C that in-furnace temperature will be sintered, keep the temperature 3 hours；
S75, third temperature raising period：In 5 hours, sintering in-furnace temperature is risen to 1320 DEG C from 1100 DEG C；
S76, third soak：It is constant at 1320 DEG C that in-furnace temperature will be sintered, keep the temperature 2 hours；
S77, the first cooldown period：In 12 hours, sintering in-furnace temperature is down to 50 DEG C from 1300 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704784A (en) * | 2019-03-04 | 2019-05-03 | 河北恒博新材料科技股份有限公司 | A kind of ceramic microsphere preparation method |
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