CN110204327A - Colourful transparent ceramics and preparation method thereof - Google Patents
Colourful transparent ceramics and preparation method thereof Download PDFInfo
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- CN110204327A CN110204327A CN201910586785.8A CN201910586785A CN110204327A CN 110204327 A CN110204327 A CN 110204327A CN 201910586785 A CN201910586785 A CN 201910586785A CN 110204327 A CN110204327 A CN 110204327A
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Abstract
The invention discloses a kind of colourful transparent ceramics and preparation method thereof, the colourful transparent ceramic powder that will first obtain, colorant and sintering aid are sufficiently mixed using planetary ball mill technique, it is dry after the ball milling predetermined time, the broken sieving of powder after drying, pre-molding, isostatic cool pressing processing, high temperature sintering and grinding/polishing step are successively carried out again, and colourful transparent ceramics sample is prepared.Colored crystalline ceramics can be prepared in the present invention, use complex sintering aids to effectively promote the sintering process of ceramics, reduce sintering temperature, improve the translucency of crystalline ceramics, while colorant once adds and simplifies preparation process.
Description
Technical field
The present invention relates to technical field of ceramic material, more specifically to a kind of colourful transparent ceramics and its preparation side
Method.
Background technique
Colourful transparent ceramics include solid-state laser, infrared window, armo(u)red glass etc. in the application of traditional field, and this year is saturating
Gradually there is new application, such as solid-state lighting, Mobile phone screen, ornament etc. in bright ceramics.It is continuous with its application range
The increase of expansion and people to its demand increasingly requires its inexpensive, easy to operate, mass production.
Theoretically, the host material of colourful transparent ceramics must be the crystal structure of higher-symmetry first, with vertical
Square crystal structure be it is best, cubic crystal structure and hexagonal crystal can also be with to structure because they without or it is only very weak
Birefringent problem.In addition, sintered colourful transparent ceramic material must have the consistency close to 100%, stomata in other words
Rate just can guarantee sufficiently high transparency less than 0.01%, while cannot contain impurity or the second phase.Therefore, colourful transparent is made pottery
The selection range relative narrower of porcelain, and preparation process's is more demanding.Therefore, current crystalline ceramics preparation process is mainly strong
The preparation of powder is adjusted, the quality of only powder reaches certain requirement, just there is preferable sintering character, guarantees the complete cause of ceramics
Densification.Many wet chemical methods be used to prepare the powder of crystalline ceramics and colourful transparent ceramics, wherein chemical coprecipitation
It is most widely used, because comparatively process is fairly simple for chemical coprecipitation, and raw material is easy to obtain compared with other methods
, thus cost is relatively low.But since chemical coprecipitation process is related to soluble precursor (chloride or nitrate etc.),
The pollutants such as chloride ion and nitrate ion can be generated in preparation process, so that technique does not have environmental requirement.Meanwhile entire system
Standby process and cleaning process are needed using a large amount of high purity water so that complex technical process and it is very long, additionally increase and be produced into
This.
The preparation of prior art transparent ceramic powder there are aiming at the problem that, and the specific demand for colourful transparent ceramics
And purposes, the present invention greatly promotes the sintering technology of powder using multiple sintering aid technology, so that avoiding chemical method prepares powder
The process of material, while effective adding method of colorant is used, the colourful transparent ceramics of needs are prepared, colour is also made
The preparation and production of crystalline ceramics are completely compatible with traditional ceramic process, therefore are very easy to extend to industrialized production.
Summary of the invention
It is completely compatible, easy to accomplish big with traditional ceramic process that technical problem to be solved by the invention is to provide a kind of
The preparation method of the colourful transparent ceramics of batch production.
In order to achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method of colourful transparent ceramics, it is characterised in that the following steps are included:
S1: oxide powder, colorant and sintering aid are placed in ball grinder together according to a certain ratio, while being added suitable
The deionized water or dehydrated alcohol of amount, with planetary ball mill continuous ball milling 2-12 hours at room temperature；
S2: slurry is placed in stand in baking oven after ball milling and is dried；
S3: the sample after drying is crushed, and then crosses 200-400 mesh；
S4: pre-molding, isostatic cool pressing processing, high temperature sintering are successively carried out to gained powder；
S5: sintered sinter carries out grinding and polishing treatment obtains colourful transparent ceramics.
In a preferred embodiment, oxide powder described in the step S1 is selected from Y2O3、Al2O3、
Sc2O3、Lu2O3Any one of or combination；The sintering aid is selected from MgO, ZrO2、LiF、SiO2Any one of or group
It closes.
In a preferred embodiment, colorant described in the step S1 is selected from transition metal oxide or dilute
Any one of earth elements oxide or combination.In a further preferred embodiment, the transition metal oxide choosing
From MnO2、Fe2O3, any one of CoO, NiO, CuO or combination, the rare earth oxide be selected from Nd2O3、Eu2O3、
Yb2O3、Pr2O3Any one of or combination.
In a preferred embodiment, oxide powder, colorant and sintering aid described in the step S1
Weight percent is 1:0.001-5%:0.001-5%, the weight ratio of the abrading-ball of the oxide powder and the ball mill
For 1:5-1:20.
In a preferred embodiment, stoving process condition is stood in the step S2 are as follows: stand drying 4-24
Hour, oven temperature is set as 60-90 DEG C.
In a preferred embodiment, the process conditions of the isostatic cool pressing processing in the step S4 are as follows: pressure
For 100-400MPa.
In a further preferred embodiment, the high temperature sintering step in the step S4 uses vacuum-sintering skill
Art, process conditions are as follows: vacuum degree 10-2-10-5Pa, sintering temperature are 1500-1900 DEG C, sintering time 2-24h.Alternatively,
High temperature sintering in the step S4 uses atmosphere sintering, process conditions are as follows: hydrogen atmosphere, nitrogen atmosphere, oxygen atmosphere or
Argon atmosphere, sintering temperature are 1500-1900 DEG C, sintering time 2-24h.
Another aspect of the present invention protects a kind of preparation method using the colourful transparent ceramics above-mentioned to be prepared
Colourful transparent ceramic product.
Compared with the prior art, the advantages of the present invention are as follows:
(1) colourful transparent ceramic preparation of the invention makes full use of the synergistic effect of a variety of sintering aids, to mention
The sintering process of high powder reduces sintering temperature, shortens sintering time, while guaranteeing that sintered body has very high optical property,
Disposable addition colorant simplifies preparation process more simultaneously.
(2) crystalline ceramics prepared by the present invention can reach 90% or more of theoretical optics transmitance.It is demonstrate,proved by experiment
The crystalline ceramics with a thickness of 1mm or so that is bright, being prepared using the method for the present invention, visible region straight line transmittance not
Lower than 75%.
(2) preparation process of the method for the present invention is easy to operate, low raw-material cost, is not related to chemical reaction, does not generate dirt
Water dirt, therefore large-scale industrial production easy to accomplish, colourful transparent ceramics obtained visible/near infrared/in it is infrared
Range there is very high transmitance, color multiplicity can be used in optical system, in high-intensity discharge lighting system, jewellery and dress
Ornaments design etc..
Detailed description of the invention
Fig. 1 is the preparation method flow diagram of colourful transparent ceramics of the invention.
Fig. 2 is the sample for the yttrium-aluminium-garnet base colourful transparent ceramics that the preparation method of the embodiment of the present invention 1 is prepared
Photo.
Specific embodiment
Explanation is further spread out to the present invention below with reference to more specific embodiment, it is to be noted that this hair
Bright a kind of colourful transparent ceramics and preparation method thereof are not limited to this specific form or step.For those skilled in the art
Member it will be readily appreciated that, even if the following description content does not make any adjustments or corrects, can also be directly applied for herein
Unspecified other similar compound or preparation method.
As shown in Figure 1, the preparation method of colourful transparent ceramics of the invention, comprising the following steps:
S1: oxide powder, colorant and sintering aid are placed in ball grinder together according to a certain ratio, while being added suitable
The deionized water or dehydrated alcohol of amount, with planetary ball mill continuous ball milling 2-12 hours at room temperature；
Wherein, oxide powder can be Y2O3、Al2O3、Sc2O3、Lu2O3Any one of combination, preferably combination of two
Or three kinds or more of composition, the composition can be the composition of two oxides, can also be and contain the two oxides
The compound of ingredient, such as yttrium-aluminium-garnet (Y3Al5O12) powder, itself just contains Y2O3And Al2O3Two oxides ingredient,
This similar composite oxides powder also should be within protection scope of the present invention.
Wherein, sintering aid is selected from MgO, ZrO2、LiF、SiO2Any one of or combination, preferably MgO, ZrO2、LiF、
SiO2Middle in combination of any two or more, for example including but be not limited to SiO2With LiF, MgO and LiF, MgO and ZrO2、
SiO2, LiF and ZrO2Etc., it will be appreciated by the skilled person that it should all be within protection scope of the present invention described in this field.This
Invention makes full use of the synergistic effect of a variety of sintering aids, to improve the sintering process of powder, reduces sintering temperature, shortens and burn
The time is tied, while guaranteeing that sintered body has very high optical property.
Wherein, colorant is selected from any one of transition metal oxide or rare earth oxide or combination, Ke Yigen
It is selected according to required color, by disposably adding colorant the preparation process of colourful transparent ceramics is more simplified,
With traditional ceramic process is completely compatible, mass production easy to accomplish.The transition metal oxide is selected from MnO2、
Fe2O3, any one of CoO, NiO, CuO or combination, the rare earth oxide be selected from Nd2O3、Eu2O3、Yb2O3、
Pr2O3Any one of or combination, it is described combination can be two kinds or more transition metal oxide combination, can be two
The combination of kind or the above rare earth oxide, the group being also possible between transition metal oxide and rare earth oxide
It closes.
Wherein, oxide powder, colorant and sintering aid weight percent are 1:0.001-5%:0.001-5%, excellent
Be selected as 1:0.1-4%, more preferably 1:0.5-2%, when colorant is two kinds and combination of the above object, proportion can it is identical or
It is slightly different, so that the total weight percent of colorant is in aforementioned range.The oxide powder and the ball milling
The weight ratio of the abrading-ball of machine is 1:5-1:20, preferably 1:8-1:15, more preferably 1:10-1:12, the abrading-ball of the ball mill
For conventional abrading-ball, such as aluminium oxide abrading-ball etc..
Wherein, suitable deionized water or dehydrated alcohol are added simultaneously during mixing and ball milling, dosage with by powder and
Subject to abrading-ball just floods, with planetary ball mill continuous ball milling 2-12 hours at room temperature, it can also use commonly used in the art
Other ball grinding techniques, or Ball-milling Time is appropriately extended, it will be understood by those skilled in the art that also should be in protection of the invention
Within the scope of.
S2: the slurry that S1 step ball milling obtains is placed in stand in baking oven and is dried, stands stoving process condition are as follows: stand and dry
4-24 hours dry, oven temperature is set as 60-90 DEG C.
S3: the sample after the drying of S2 step is crushed, 200-400 mesh is then crossed.
Wherein, it is crushed and sieves and realized using the prior art of this field routine, phase can be used according to degree of agglomeration
The breaking method answered, such as squeeze, grind etc..Meanwhile screening is the powder of required granularity in order to obtain, is added so as to subsequent
Work molding and required consistency and the porosity etc..
S4: pre-molding, isostatic cool pressing processing, high temperature sintering are successively carried out to powder obtained by S3 step.
Wherein, three pre-molding, isostatic cool pressing processing, high temperature sintering techniques can use this field conventional technique
Or equipment is realized；Such as the powder after sieving is needed to add in the process suitable polyvinyl alcohol water solution and is made using dry-pressing formed
Ensure molding effect for adhesive；The pressure that molding uses need to be adjusted correspondingly according to the composition and property of powder, to protect
Demonstrate,prove the not no defect because caused by pressure is improper in microstructure in formed body；Because such defect is once being formed by nothing
Method is eliminated in subsequent sintering process；Guarantee it is dry-pressing formed after green body relative density be 50-55% within the scope of.
Wherein, the process conditions of isostatic cool pressing processing are pressure 100-400MPa, preferably 150-300MPa, more preferable 200-
250MPa, so that the relative density of sample is within the scope of 60-65% after processing.
Wherein, high temperature sintering step can use vacuum sintering technique, can also use atmosphere sintering.It is burnt when using vacuum
When knot technology, process conditions are as follows: vacuum degree 10-2~10-5Pa, sintering temperature are 1500-1900 DEG C, sintering time 2-
24h；When using atmosphere sintering technology, process conditions are as follows: hydrogen atmosphere, nitrogen atmosphere, oxygen atmosphere or argon atmosphere, sintering
Temperature is 1500-1900 DEG C, sintering time 2-24h.Suitable control heating and rate of temperature fall during the sintering process, do not have
Special requirement.
S5: step S4 sintered sinter carries out grinding and polishing treatment obtains colourful transparent ceramics of the invention.
The preparation method for the colourful transparent ceramics that present invention will be further explained by specific examples below.
Embodiment 1
S1: to the yttrium-aluminium-garnet (Y of 10kg3Al5O12) 0.5kg transition metal oxide CoO is added in powder is used as
Toner, the SiO of the LiF and 0.05kg of 0.05kg2As sintering aid, the mixture arrived is placed in nylon ball grinder, simultaneously
It is put into aluminium oxide abrading-ball and deionized water；So that the weight ratio of aforementioned powders mixture and aluminium oxide abrading-ball is 1:20, it is added
Amount of deionized water be just powder and abrading-ball are flooded；Powder ball milling is carried out using planetary ball mill, the revolving speed of ball mill is
200 revs/min, Ball-milling Time 12h.
S2: after ball milling, ball milling slurry is transferred in size glassware appropriate, and be placed into drying box
In be dried, drying temperature be 90 DEG C, drying time 2h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 52%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 240MPa；Sample after processing
The relative density of product is 63%.
Normal high-temperature vacuum sintering, the process conditions of vacuum-sintering are carried out to isostatic cool pressing treated green body are as follows: true
Reciprocal of duty cycle 10-3Pa, sintering temperature are 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet base blue-tinted transparent ceramics.
Fig. 2 gives the yttrium-aluminium-garnet base colourful transparent ceramics sample image that the preparation method of embodiment 1 obtains, part
Sample does not have ground and polishing treatment.As shown in Fig. 2, sample all has penetrating texture.Similarly, following further embodiments system
The colourful transparent ceramics sample that Preparation Method obtains also possesses similar appearance, and it is quite high to illustrate that technology of preparing of the invention has
Reliability can be realized mass production.
Embodiment 2
S1: to 1kg yttrium-aluminium-garnet (Y3Al5O12) 0.01kg transition metal oxide CoO and 0.01kg is added in powder
Rare earth oxide Nd2O3, the MgO of the LiF and 0.01kg of 0.01kg are as sintering aid, by the mixture arrived merging Buddhist nun
Imperial ball grinder, while being put into aluminium oxide abrading-ball and deionized water；So that the weight ratio of powders mixture and aluminium oxide abrading-ball is 1:
15, the amount of deionized water being added is just to flood powder and abrading-ball；Powder ball milling, ball mill are carried out using planetary ball mill
Revolving speed be 180 revs/min, Ball-milling Time 10h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature is 90 DEG C, time 4h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 54%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 220MPa；Sample after processing
The relative density of product is 64%.
High-temperature vacuum sintering, high-temperature vacuum sintering process conditions are as follows: vacuum degree are carried out to isostatic cool pressing treated green body
10-5Pa, sintering temperature are 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet base blue-tinted transparent ceramics.
Embodiment 3
S1:: to 1kg yttrium-aluminium-garnet (Y3Al5O12) be added in powder 0.01kg transition metal oxide CoO and
The ZrO2 of the MgO and 0.005kg of 0.005kg transition metal oxide NiO, 0.01kg are as sintering aid, the mixing that will be arrived
Object is placed in nylon ball grinder, while being put into aluminium oxide abrading-ball and deionized water；So that the weight of powders mixture and aluminium oxide abrading-ball
For amount than being 1:10, the amount of deionized water being added is just to flood powder and abrading-ball；Powder ball is carried out using planetary ball mill
Mill, the revolving speed of ball mill are 150 revs/min, Ball-milling Time 8h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature is 85 DEG C, time 6h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 54%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 200MPa；Sample after processing
The relative density of product is 63%.
High-temperature vacuum sintering, the process conditions of high-temperature vacuum sintering are as follows: vacuum are carried out to isostatic cool pressing treated green body
Degree 10-5Pa, sintering temperature are 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet base blue-tinted transparent ceramics.
Embodiment 4
S1: to 1kgY2O3And Al2O3Mixed powder (Y2O3:Al2O3=3:5) in be added 0.003kg rare earth oxide
Yb2O3, the SiO of the LiF and 0.0016kg of 0.0021kg2As sintering aid, the mixture arrived is placed in nylon ball grinder,
It is put into aluminium oxide abrading-ball and deionized water simultaneously；So that the weight ratio of powders mixture and aluminium oxide abrading-ball is 1:8, it is added
Amount of deionized water is just to flood powder and abrading-ball；Using planetary ball mill and powder ball milling is carried out, the revolving speed of ball mill is 120
Rev/min, Ball-milling Time 8h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature is 65 DEG C, time 23h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 54%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 180MPa；Sample after processing
The relative density of product is 64%.
High-temperature vacuum sintering, the process conditions of high-temperature vacuum sintering are as follows: vacuum are carried out to isostatic cool pressing treated green body
Degree 10-5Pa, sintering temperature are 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet base green transparent ceramics.
Embodiment 5
S1: to 1kgY2O3And Al2O3Mixed powder (Y2O3:Al2O3=3:5) in be added 0.008kg rare earth oxide
Nd2O3With the Eu of 0.005kg2O3, the MgO of the LiF and 0.016kg of 0.018kg as sintering aid, by mixture set
Enter nylon ball grinder, while being put into aluminium oxide abrading-ball and deionized water；So that the weight ratio of powders mixture and aluminium oxide abrading-ball
For 1:12, the amount of deionized water being added is just to flood powder and abrading-ball；Using planetary ball mill and carry out powder ball milling, ball
The revolving speed of grinding machine is 60 revs/min, Ball-milling Time 4h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature is 60 DEG C, and the time is for 24 hours.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 53%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 160MPa；Sample after processing
The relative density of product is 63%.
High-temperature vacuum sintering, process conditions are as follows: vacuum degree 10 are carried out to isostatic cool pressing treated green body-3Pa, sintering temperature
Degree is 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet base green transparent ceramics.
Embodiment 6
S1: to the Y of 1kg2O3And Al2O3Mixed powder (Y2O3:Al2O3=3:5) in be added 0.013kg rare-earth oxidation
Object Nd2O3With the Pr of 0.05kg2O3, the ZrO of the MgO and 0.021kg of 0.012kg2As sintering aid, by mixture set
Enter nylon ball grinder, while being put into aluminium oxide abrading-ball and deionized water；So that the weight ratio of powders mixture and aluminium oxide abrading-ball
For 1:5, the amount of deionized water being added is just to flood powder and abrading-ball；Using planetary ball mill and carry out powder ball milling, ball
The revolving speed of grinding machine is 100 revs/min, Ball-milling Time 8h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature are as follows: 70 DEG C, time 18h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 52%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 200MPa；Sample after processing
The relative density of product is 62%.
High-temperature vacuum sintering, process conditions are as follows: vacuum degree 10 are carried out to isostatic cool pressing treated green body-2Pa, sintering temperature
Degree is 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet base green transparent ceramics.
Embodiment 7
S1: to the Sc of 1kg2O3And Lu2O3Powder (Sc2O3: Lu2O3=4:6) in be added 0.028kg rare earth oxide
Nd2O3With the Yb of 0.015kg2O3, the SiO of the LiF and 0.0017kg of 0.0021kg2As sintering aid, the mixture that will be arrived
It is placed in nylon ball grinder, while being put into aluminium oxide abrading-ball and deionized water；So that the weight of powders mixture and aluminium oxide abrading-ball
Than for 1:12, the amount of deionized water being added is just to flood powder and abrading-ball；Using planetary ball mill and powder ball milling is carried out,
The revolving speed of ball mill is 95 revs/min, Ball-milling Time 8h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature are as follows: 75 DEG C, time 20h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 55%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 190MPa；Sample after processing
The relative density of product is 64%.
High-temperature vacuum sintering, process conditions are as follows: vacuum degree 10 are carried out to isostatic cool pressing treated green body-4Pa, sintering temperature
Degree is 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet original washing powder red, transparent ceramics.
Embodiment 8
S1: to the Sc of 1kg2O3And Lu2O3Powder (Sc2O3: Lu2O3=7:3) in be added 0.05kg rare earth oxide
Eu2O3, the MgO of the LiF (0.001-2.5%) and 0.0023kg of 0.002kg are as sintering aid, by the mixture arrived merging
Nylon ball grinder, while being put into aluminium oxide abrading-ball and deionized water；So that the weight ratio of powders mixture and aluminium oxide abrading-ball is
1:15, the amount of deionized water being added are just to flood powder and abrading-ball；Using planetary ball mill and carry out powder ball milling, ball milling
The revolving speed of machine is 120 revs/min, Ball-milling Time 8h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature are as follows: 80 DEG C, time 10h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: powder after sieving using dry-pressing formed, it is dry-pressing formed after green body relative density be 54%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 200MPa；Sample after processing
The relative density of product is 63%.
High-temperature vacuum sintering is carried out to isostatic cool pressing treated green body, process conditions are vacuum degree 10-4Pa, sintering temperature
It is 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet original washing powder red, transparent ceramics.
Embodiment 9
S1: to the Sc of 1kg2O3And Lu2O3Powder (Sc2O3: Lu2O3=3:5) in be added 0.035kg rare earth oxide
Nd2O3, the ZrO of the MgO and 0.007kg of 0.015kg2As sintering aid, the mixture arrived is placed in nylon ball grinder, together
When be put into aluminium oxide abrading-ball and deionized water；So that the weight ratio of powders mixture and aluminium oxide abrading-ball is 1:18, it is added
Amount of deionized water is just to flood powder and abrading-ball；Using planetary ball mill and powder ball milling is carried out, the revolving speed of ball mill is 160
Rev/min, Ball-milling Time 8h.
S2: after ball milling, ball milling slurry is transferred in size glass culture dish appropriate, and be placed into drying
It is dried in case, drying temperature is 75 DEG C, time 18h.
S3: the powder after dry needs to be crushed there are caking phenomenon；Corresponding breaking method is used according to degree of agglomeration；
Broken powder is after 200-400 mesh.
S4: the powder after sieving use it is dry-pressing formed after green body relative density for 54%.
Isostatic cool pressing processing is carried out to dry-pressing formed green body, the pressure of cold isostatic compaction is 190MPa；Sample after processing
The relative density of product is 63%.
High-temperature vacuum sintering, process conditions are as follows: vacuum degree 10 are carried out to isostatic cool pressing treated green body-3Pa, sintering temperature
Degree is 1760 DEG C, sintering time 13h.
S5: the sinter obtained after high temperature pressure-free sintering is machined again, that is, includes grinding and polishing, finally obtains
Obtain yttrium-aluminium-garnet original washing powder red, transparent ceramics.
Although the detailed description and description of the specific embodiments of the present invention are given above, it should be noted that
We can carry out various equivalent changes and modification to above embodiment according to the concept of the present invention, and generated function is made
It, should all be within protection scope of the present invention when with the spirit still covered without departing from specification and attached drawing.
Claims (10)
1. a kind of preparation method of colourful transparent ceramics, it is characterised in that the following steps are included:
S1: oxide powder, colorant and sintering aid are placed in ball grinder together according to a certain ratio, while being added suitable
Deionized water or dehydrated alcohol, with planetary ball mill continuous ball milling 2-12 hours at room temperature；
S2: slurry is placed in stand in baking oven after ball milling and is dried；
S3: the sample after drying is crushed, and then crosses 200-400 mesh；
S4: pre-molding, isostatic cool pressing processing, high temperature sintering are successively carried out to gained powder；
S5: sintered sinter carries out grinding and polishing treatment obtains colourful transparent ceramics.
2. the preparation method of colourful transparent ceramics according to claim 1, it is characterised in that described in the step S1
Oxide powder is selected from Y2O3、Al2O3、Sc2O3、Lu2O3Any one of or combination；The sintering aid is selected from MgO, ZrO2、
LiF、SiO2Any one of or combination.
3. the preparation method of colourful transparent ceramics according to claim 1, it is characterised in that described in the step S1
Colorant be selected from any one of transition metal oxide or rare earth oxide or combination.
4. the preparation method of colourful transparent ceramics according to claim 3, it is characterised in that the transiting metal oxidation
Object is selected from MnO2、Fe2O3, any one of CoO, NiO, CuO or combination, the rare earth oxide be selected from Nd2O3、
Eu2O3、Yb2O3、Pr2O3Any one of or combination.
5. the preparation method of colourful transparent ceramics according to claim 1-4, it is characterised in that the step S1
Described in oxide powder, colorant and sintering aid weight percent be 1:0.001-5%:0.001-5%, the oxygen
The weight ratio of the abrading-ball of compound powder and the ball mill is 1:5-1:20.
6. the preparation method of colourful transparent ceramics according to claim 1, it is characterised in that stood in the step S2
Stoving process condition are as follows: stand drying 4-24 hours, oven temperature is set as 60-90 DEG C.
7. the preparation method of colourful transparent ceramics according to claim 1, it is characterised in that cold in the step S4
The process conditions of isostatic pressing are as follows: pressure 100-400MPa.
8. the preparation method of colourful transparent ceramics according to claim 1 or claim 7, it is characterised in that in the step S4
High temperature sintering step uses vacuum sintering technique, process conditions are as follows: vacuum degree 10-2-10-5Pa, sintering temperature 1500-
1900 DEG C, sintering time 2-24h.
9. the preparation method of colourful transparent ceramics according to claim 1 or claim 7, it is characterised in that in the step S4
High temperature sintering uses atmosphere sintering, process conditions are as follows: hydrogen atmosphere, nitrogen atmosphere, oxygen atmosphere or argon atmosphere, sintering temperature
It is 1500-1900 DEG C, sintering time 2-24h.
10. the colourful transparent ceramics of the preparation method preparation of -9 described in any item colourful transparent ceramics according to claim 1.
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| CN113213902A (en) * | 2021-05-27 | 2021-08-06 | 阿特麦哲(东莞)新材料科技有限公司 | Color porous ceramic atomizing core and preparation method thereof |
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| CN117069482A (en) * | 2023-08-15 | 2023-11-17 | 湖南省新化县恒生电子陶瓷有限责任公司 | Alumina ceramic for new energy automobile fuse and preparation method thereof |
| CN117069482B (en) * | 2023-08-15 | 2024-02-02 | 湖南省新化县恒生电子陶瓷有限责任公司 | Alumina ceramic for new energy automobile fuse and preparation method thereof |
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Application publication date: 20190906 |