CN105732050A - Preparation technology of net size transparent ceramic part in complex shape - Google Patents
Preparation technology of net size transparent ceramic part in complex shape Download PDFInfo
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Abstract
The invention relates to a preparation technology of a net size transparent ceramic part in a complex shape. The preparation technology comprises the following steps of: (1) preparing by adopting an injection moulding method, so as to obtain a ceramic body; (2) degreasing the ceramic body by adopting a two-step degreasing method combining water extraction degreasing with thermal degreasing, so as to obtain a processed body; and (3) carrying out spark plasma sintering without directly applying pressure to the processed body by virtue of spark plasma sintering equipment, annealing, and polishing, so that the transparent ceramic part is obtained. The preparation technology of the net size transparent ceramic part in the complex shape is applicable to preparation of a transparent ceramic part with net size, high precision, high density, high uniformity, high performance and complex shape.
Description
Technical field
The present invention relates to high-performance crystalline ceramics preparing technical field, particularly to the preparation technology of a kind of dead size complicated shape crystalline ceramics part.
Background technology
Very for a long time, it is believed that pottery is opaque.But report first from the R.L.Coble of GE company of the U.S. in 1962 and be successfully prepared for translucent Al2O3Pottery (trade name is Lucalox), thus having broken the traditional view of people at one stroke, also opens new application for ceramic material.
Hereafter, other oxidic transparent pottery, such as Y2O3(yittrium oxide), MgO (magnesium oxide), BeO (beryllium oxide), CaO (calcium oxide), ThO2(thorium oxide), MgAl2O4(magnesium aluminate spinel), (Pb, La) (Zr, Ti) O (lead zirconate titanate) etc. are come out one after another.Subsequently, also can be produced out as doped yttrium aluminum garnet (such as the Nd:YAG) crystalline ceramics of a new generation's solid laser material, and studied widely and apply.In the recent decade, a collection of Non-oxide Transparent Ceramics is also developed in succession, such as AlON (A Long) crystalline ceramics, AlN (aluminium nitride) crystalline ceramics, SiAlON (Sai Long) crystalline ceramics etc..
The forming method that the many employings of current crystalline ceramics are traditional, such as dry-pressing, slip casting, isostatic pressing.Although ceramic dry-pressed efficiency is higher, but there is the phenomenon that density variation, microstructure are uneven, simultaneously not easy-formation form parts.Though the plastic special-shaped product of ceramic grout molding, but molding blank is easily generated density unevenness and component segregation, have that compact dimensions precision is low and degradation problem under product reliability.Cold isostatic compaction can obtain the molding blank of high density and high uniformity, but is difficult to the ceramic part that forming shape is complicated, and shaping efficiency is low and needs manual operation more.These traditional molding methods are not suitable for the crystalline ceramics part of preparation precision, the high-performance of complicated shape, high reliability.
Therefore, not enough for prior art, it is provided that the preparation technology of a kind of dead size complicated shape crystalline ceramics part is to overcome prior art deficiency very necessary.
Summary of the invention
It is an object of the invention to avoid the deficiencies in the prior art part to provide the preparation technology of a kind of dead size complicated shape crystalline ceramics part, this preparation technology be suitable for preparing dead size, in high precision, the crystalline ceramics part of high density, high uniformity, high-performance, complicated shape.
The above-mentioned purpose of the present invention is realized by following technological means.
The preparation technology of a kind of dead size complicated shape crystalline ceramics part is provided, comprises the steps:
(1) ceramic body is prepared with injection moulding method；
(2) adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base；
(3) in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.
Above-mentioned steps (1) prepares ceramic body with injection moulding method and specifically includes:
(1.1) ceramic powder surface modification
Using the purity high-purity nm ceramic powder be more than or equal to 99.9% as raw material, in the way of chemical precipitation, introduce trace sintering aid by magnetic stirring apparatus obtain the ceramic composite powder containing sintering aid；
Afterwards surface modifier is carried out together with ceramic composite powder ball milling pretreatment, forms the clad of one layer of several nano thickness in composite ceramic powder surface, after drying, obtain surface modification ceramic powder；
(1.2) mixing
Organic binder bond and surface modification ceramic powder are made injection suspended substance；
(1.3) injection moulding obtains needing the ceramic body of shape.
Above-mentioned ceramic powder is the purity yittrium oxide more than 99.9%, magnesium oxide, beryllium oxide, calcium oxide, thorium oxide, magnesium aluminate spinel, lead zirconate-titanate ceramic or is A Long pottery, aluminium nitride ceramics, Sialon ceramics；
Described sintering aid is one or more in magnesium oxide, yittrium oxide, lanthana, and the total amount of described sintering aid accounts for 0.1～1wt% of described ceramic powder total amount；
Described surface modifier is any one in stearic acid, oleic acid, ten dihydroxystearic acids, citric acid, and the total amount of surface modifier accounts for 0.1～3wt% of described ceramic composite powder total amount；
In described injection molding compound, it is 80%～90% that surface modification ceramic powder accounts for the percentage by weight of injection molding compound, and it is 10～20% that organic binder bond accounts for the percentage by weight of injection molding compound.
The preparation technology of above-mentioned dead size complicated shape crystalline ceramics part,
In the way of chemical precipitation, obtain the ceramic composite powder containing sintering aid by magnetic stirring apparatus introducing trace sintering aid specifically adopt nitrate or the chloride of metal ion, ammonia is used to regulate the pH value of slurry to 9.2～11.4 so that metal ion deposits to the surface of ceramic powder granule with the form of chemical precipitation；
Ball milling adopt aluminium oxide ceramics ball grinder, abrading-ball is high-purity transparent alumina abrading-ball, and ball-milling medium is ethanol, ceramics, ethanol, abrading-ball three mass ratio be 1:1:2, rotating speed is 80rpm～240rpm, and Ball-milling Time is 3～12h.
Preferably, above-mentioned steps (1.2) mixing employing PEG/PVB system feeding, binder system consists of:
22wt%PVB+33wt%PEG4000+33wt%PEG600+9wt%SA+2.5%DBP, the phenothiazine additionally adding 0.5wt% makes antioxidant；
First in double roll mill, add skeleton binding agent PVB, double; two roller is started after PVB presents molten state completely and double; two roll temperature rises to 170 DEG C, it is then respectively adding phenothiazine, PEG4000, PEG600 and SA, mixing altogether continuing 45min, before mixing end, 5min adds DBP to suppress to reach the purpose of plasticising.
Another is preferred, above-mentioned steps (1.2) mixing employing PEG/PMMA system feeding, and binder system consists of:
20wt%PMMA+30wt%PEG4000+35wt%PEG600+12wt%SA+2.5%DBP, the phenothiazine additionally adding 0.5wt% makes antioxidant；
First in double roll mill, add skeleton binding agent PMMA, double; two roller is started after PMMA presents molten state completely and double; two roll temperature rises to 170 DEG C, it is then respectively adding phenothiazine, PEG4000, PEG600 and SA, mixing altogether continuing 45min, before mixing end, 5min adds DBP to suppress to reach the purpose of plasticising.
Above-mentioned steps (2) adopts water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base specifically: first passes through water and extracts defat and removed by the water-soluble binder in component, removes the nonaqueous binders in base substrate again through thermal debinding.
Above-mentioned water extracts defat specifically: being placed in water-bath by ceramic body and carry out water extract defat, temperature is 40～60 DEG C, and degreasing time is 8～20h；
Described thermal debinding is specifically: the base substrate after water defat at 80～100 DEG C after air drying 12～24h, is put into and temperature rises in Muffle furnace 450～500 DEG C of insulation 2～3h obtained ripe base, and heating rate is 2～4 DEG C/min.
Above-mentioned steps (3) is specifically: ripe base is placed in graphite crucible, the graphite crucible entirety being stamped graphite cover being put in discharging plasma sintering equipment and be sintered, graphite crucible is applied pressure with fixing graphite crucible by the upper push-down head of discharging plasma sintering equipment.
In above-mentioned steps (3), the sintering temperature of discharge plasma sintering is 1300～1600 DEG C, and heating rate is 10～100 DEG C/min, and temperature retention time is 5～20min.
The preparation technology of the dead size complicated shape crystalline ceramics part of the present invention, comprises the steps: that (1) prepares ceramic body with injection moulding method；(2) adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base；(3) in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.The preparation technology of this dead size complicated shape crystalline ceramics part be suitable for preparing dead size, in high precision, the crystalline ceramics part of high density, high uniformity, high-performance, complicated shape structure.
Accompanying drawing explanation
The present invention is further illustrated to utilize accompanying drawing, but the content in accompanying drawing does not constitute any limitation of the invention.
Fig. 1 is the use view of discharging plasma sintering equipment and the graphite crucible adopted in the preparation technology of the present invention a kind of dead size complicated shape crystalline ceramics part.
Fig. 2 is the structural representation of the transparent alumina bracket prepared by the embodiment of the present invention 6.
Fig. 3 is the SEM surface topography schematic diagram of the transparent alumina bracket of Fig. 2.
In FIG, including:
Graphite crucible 100, graphite cover 200, Graphite pad 300, ripe base 400, upper push-down head 500.
Detailed description of the invention
The invention will be further described with the following Examples.
Embodiment 1.
The preparation technology of a kind of dead size complicated shape crystalline ceramics part, is undertaken by following three step.
(1) ceramic body is prepared with injection moulding method.
Step (1) prepares ceramic body with injection moulding method and specifically includes:
(1.1) ceramic powder surface modification
Using high-purity nm ceramic powder as raw material, in the way of chemical precipitation, introduce trace sintering aid by magnetic stirring apparatus obtain the ceramic composite powder containing sintering aid.High-purity nm ceramic powder refers to the purity powder body more than 99.9%.Ceramic powder is the purity yittrium oxide more than 99.9%, magnesium oxide, beryllium oxide, calcium oxide, thorium oxide, magnesium aluminate spinel, lead zirconate-titanate ceramic or is A Long pottery, aluminium nitride ceramics, Sialon ceramics.Sintering aid is one or more in magnesium oxide, yittrium oxide, lanthana, and the total amount of sintering aid accounts for 0.1～1wt% of ceramic powder total amount.
Afterwards surface modifier is carried out together with ceramic composite powder ball milling pretreatment, forms the clad of one layer of several nano thickness in composite ceramic powder surface, after drying, obtain surface modification ceramic powder.Surface modifier is any one in stearic acid, oleic acid, ten dihydroxystearic acids, citric acid, and the total amount of surface modifier accounts for 0.1～3wt% of ceramic composite powder total amount.
(1.2) mixing
Organic binder bond and surface modification ceramic powder are made injection suspended substance.In injection molding compound, it is 80%～90% that surface modification ceramic powder accounts for the percentage by weight of injection molding compound, and it is 10～20% that organic binder bond accounts for the percentage by weight of injection molding compound.Injection molding compound refers to the compound of organic binder bond and surface modification ceramic powder.
Mixing employing PEG/PVB system feeding, binder system consists of:
22wt%PVB+33wt%PEG4000+33wt%PEG600+9wt%SA+2.5%DBP, the phenothiazine additionally adding 0.5wt% makes antioxidant.
First in double roll mill, add skeleton binding agent PVB, double; two roller is started after PVB presents molten state completely and double; two roll temperature rises to 170 DEG C, it is then respectively adding phenothiazine, PEG4000, PEG600 and SA, mixing altogether continuing 45min, before mixing end, 5min adds DBP to suppress to reach the purpose of plasticising.
(1.3) injection moulding obtains needing the ceramic body of shape.On injection (mo(u)lding) machine, injection moulding obtains the ceramic body of complicated shape.According to different feeding system and need to inject difform base substrate, suitably regulate injection parameters, such as injection pressure, injection speed, barrel temperature, storing position etc., to obtain intact injection base substrate.
(2) adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, specifically: first pass through water and extract defat by the water-soluble binder elimination in component, remove the nonaqueous binders in base substrate again through thermal debinding.
Water extracts defat specifically: being placed in water-bath by ceramic body and carry out water extract defat, temperature is 40～60 DEG C, and degreasing time is 8～20h.
Thermal debinding is specifically: the base substrate after water defat at 80～100 DEG C after air drying 12～24h, is put in baking oven thermal debinding 4～6h at 80～100 DEG C and obtained ripe base.
(3) in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.
Discharging plasma sintering equipment can be realized by high strength graphite crucible in the way of not to ripe base direct weighting, the graphite crucible of high intensity refers to that the intensity of graphite crucible can bear the pressure that graphite crucible is applied by the upper push-down head of discharging plasma sintering equipment, and this pressure is usually 10MPa.As shown in Figure 1, ripe base 400 is placed in the graphite crucible 100 of high intensity, graphite crucible 100 entirety being stamped graphite cover 200 is put in discharging plasma sintering equipment and is sintered, graphite crucible 100 is applied pressure by the upper push-down head 500 of discharging plasma sintering equipment to be fixed graphite crucible and sample is not pressurizeed, and pulse current and plasma are thus realizing heat-agglomerating to the ripe base 400 as sample.Put in discharge plasma agglomerating plant by high strength graphite crucible and be sintered, it is achieved in sintering process, sample is applied pressure, eliminate the pressure destruction to precise ceramic component.
The sintering temperature of discharge plasma sintering is 1300～1600 DEG C, and heating rate is 10～100 DEG C/min, and temperature retention time is 5～20min.The ceramic member of required complicated shape is obtained after sintering.
It should be noted that discharging plasma sintering equipment carries out discharge plasma sintering in the way of not to ripe base direct weighting is not limited to the graphite crucible of the present embodiment, it is also possible to carry out otherwise.
The preparation technology of this dead size complicated shape crystalline ceramics part, by the control to each process, injection moulding is adopted to prepare the ceramic body of complicated shape, adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.Prepared crystalline ceramics part possess dead size, in high precision, the feature of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Embodiment 2.
A kind of preparation technology of dead size complicated shape crystalline ceramics part, further feature is identical with embodiment 1, it is different in that, also there is following technical characteristic: in the way of chemical precipitation, obtain the ceramic composite powder containing sintering aid by magnetic stirring apparatus introducing trace sintering aid can adopt nitrate or the chloride of metal ion, ammonia is used to regulate the pH value of slurry to 9.2～11.4 so that metal ion deposits to the surface of ceramic powder granule with the form of chemical precipitation.It is functional which has sintering aid, prepares convenient feature.
Embodiment 3.
A kind of preparation technology of dead size complicated shape crystalline ceramics part, further feature is identical with embodiment 1, it is different in that, also there is following technical characteristic: in the way of chemical precipitation, obtain the ceramic composite powder containing sintering aid by magnetic stirring apparatus introducing trace sintering aid can adopt nitrate or the chloride of magnesium ion, ammonia is used to regulate the pH value of slurry to 9.2～11.4 so that Mg2+The surface of ceramic powder granule is deposited to the form of chemical precipitation.It is functional which has sintering aid, prepares convenient feature.
Embodiment 4.
A kind of preparation technology of dead size complicated shape crystalline ceramics part, further feature is identical with embodiment 1 or 2 or 3, it is different in that, also there is following technical characteristic: ball milling adopts aluminium oxide ceramics ball grinder, abrading-ball is high-purity transparent alumina abrading-ball, and ball-milling medium is ethanol, ceramics, ethanol, abrading-ball three mass ratio be 1:1:2, rotating speed is 80rpm～240rpm, and Ball-milling Time is 3～12h.This ball-milling technology has ball milling effect, the uniform feature of powder particles, it is simple to prepare high performance crystalline ceramics part.
Embodiment 5.
A kind of preparation technology of dead size complicated shape crystalline ceramics part, further feature is identical with embodiment 1 or 2 or 3, is different in that also have following technical characteristic:
Step (1.2) mixing employing PEG/PMMA system feeding, binder system consists of:
22wt%PVB+33wt%PEG4000+33wt%PEG600+9wt%SA+2.5%DBP, the phenothiazine additionally adding 0.5wt% makes antioxidant；
First in double roll mill, add skeleton binding agent PVB, double; two roller is started after PVB presents molten state completely and double; two roll temperature rises to 170 DEG C, it is then respectively adding phenothiazine, PEG4000, PEG600 and SA, mixing altogether continuing 45min, before mixing end, 5min adds DBP to suppress to reach the purpose of plasticising.
The preparation technology of this dead size complicated shape crystalline ceramics part, by the control to each process, injection moulding is adopted to prepare the ceramic body of complicated shape, adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.Prepared crystalline ceramics part possess dead size, in high precision, the feature of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Embodiment 6.
A kind of preparation technology of dead size complicated shape crystalline ceramics part, employing mean diameter is 100nm, purity be 99.99% α-Al2O3, by MgO, Y2O3Introducing with the content of 0.5wt% as sintering aid, the SA of 1wt% introduces as surfactant.Employing ethanol is ball-milling medium, and self-control transparent alumina abrading-ball carries out ball milling, and rotating speed is 80rpm, takes out drying and obtain surface modification ceramic powder after ball milling 4h.
Adopt (1.2) method preparation PEG/PVB system feeding in inventive embodiments 1, on injection (mo(u)lding) machine, injection moulding obtains transparent alumina ceramics holding groove base substrate afterwards, Injection Molding Parameters is: the temperature from barrel to cast gate is 160-165-170-175 DEG C, and die heater temperature is 45 DEG C.
Base substrate injection moulding obtained is put in water-bath, dissolves elimination water-soluble binder, and the temperature of water is 50 DEG C, and degreasing time is 8h.Water extracts the base substrate after defat at the dry 15h of 90 DEG C of baking oven air.
Dried base substrate being put into Muffle furnace, carries out two step thermal debinding, heating rate is that 5 DEG C/min is warming up to 500 DEG C, is incubated 5h.Base substrate after thermal debinding is placed in high strength graphite crucible, have the graphite crucible of graphite cover to be placed in discharging plasma sintering equipment this to be sintered, heating rate is 100 DEG C/min, sintering temperature is 1450 DEG C, temperature retention time is 5min, then furnace cooling, obtains transparent alumina ceramics holding groove, as shown in Figure 2.
The density of the alumina ceramics holding groove prepared by the preparation method of the present invention is 3.97g/cm3, bending strength is 600 ± 35Mpa, and Vickers hardness is 19Gpa.Its SEM microstructure causes dense and uniform, and average grain size is about～200nm, without obvious pore and impurity, as shown in Figure 3.
The preparation technology of this dead size complicated shape crystalline ceramics part, by the control to each process, injection moulding is adopted to prepare the ceramic body of complicated shape, adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.Prepared crystalline ceramics part possess dead size, in high precision, the feature of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Embodiment 7.
A kind of preparation technology of dead size complicated shape crystalline ceramics part, employing mean diameter is 100nm, purity be 99.99% α-Al2O3, by MgO, Y2O3Introducing with the content of 1wt% as sintering aid, the SA of 3wt% introduces as surfactant.Employing ethanol is ball-milling medium, and self-control transparent alumina abrading-ball carries out ball milling, and rotating speed is 200rpm, takes out drying and obtain surface modification ceramic powder after ball milling 3h.
Adopt the mixed PEG/PMMA system feeding of method preparation of (1.2) in inventive embodiments 5, on injection (mo(u)lding) machine, injection moulding obtains transparent alumina ceramics holding groove base substrate afterwards, Injection Molding Parameters is: the temperature from barrel to cast gate is 158-165-172-178 DEG C, and die heater temperature is 49 DEG C.
Base substrate injection moulding obtained is put in water-bath, dissolves elimination water-soluble binder, and the temperature of water is 52 DEG C, and degreasing time is 6h.Water extracts the base substrate after defat at the dry 13h of 100 DEG C of baking oven air.
Dried base substrate being put into Muffle furnace, carries out two step thermal debinding, heating rate is that 5 DEG C/min is warming up to 500 DEG C, is incubated 5h.Base substrate after thermal debinding is placed in high strength graphite crucible, have the graphite crucible of graphite cover to be placed in discharging plasma sintering equipment this to be sintered, heating rate is 100 DEG C/min, sintering temperature is 1450 DEG C, temperature retention time is 5.6min, then furnace cooling, obtains transparent alumina ceramics holding groove.
The density of the alumina ceramics holding groove prepared by the preparation method of the present invention is 3.99g/cm3, bending strength is 610 ± 35Mpa, and Vickers hardness is 19.2Gpa.Its SEM microstructure causes dense and uniform, and average grain size is about 150～200nm, without obvious pore and impurity.
The preparation technology of this dead size complicated shape crystalline ceramics part, by the control to each process, injection moulding is adopted to prepare the ceramic body of complicated shape, adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.Prepared crystalline ceramics part possess dead size, in high precision, the feature of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Embodiment 8.
The preparation technology of a kind of dead size complicated shape crystalline ceramics part, employing mean diameter is 100nm, purity is the beryllium oxide of 99.99%, by MgO, La2O3Introducing with the content of 0.1wt% as sintering aid, the SA of 2wt% introduces as surfactant.Employing ethanol is ball-milling medium, and self-control transparent alumina abrading-ball carries out ball milling, and rotating speed is 200rpm, takes out drying and obtain surface modification ceramic powder after ball milling 3h.
Adopt (1.2) method preparation PEG/PVB system feeding in inventive embodiments 1, on injection (mo(u)lding) machine, injection moulding obtains transparent berryllia ceramics base substrate afterwards, Injection Molding Parameters is: the temperature from barrel to cast gate is 160-163-172-178 DEG C, and die heater temperature is 59 DEG C.
Base substrate injection moulding obtained is put in water-bath, dissolves elimination water-soluble binder, and the temperature of water is 60 DEG C, and degreasing time is 12h.Water extracts the base substrate after defat at the dry 15h of 90 DEG C of baking oven air.
Dried base substrate being put into Muffle furnace, carries out two step thermal debinding, heating rate is that 5 DEG C/min is warming up to 600 DEG C, is incubated 4.5h.Being placed in high strength graphite crucible by the base substrate after thermal debinding, have the graphite crucible of graphite cover to be placed in discharging plasma sintering equipment this and be sintered, heating rate is 100 DEG C/min, sintering temperature is 1450 DEG C, temperature retention time is 5min, then furnace cooling, obtains transparent berryllia ceramics.
The density of the beryllium oxide ceramics prepared by the preparation method of the present invention is 4.12g/cm3, bending strength is 620 ± 35Mpa, and Vickers hardness is 18.9Gpa.Its SEM microstructure causes dense and uniform, and average grain size is about 80～200nm, without obvious pore and impurity.
The preparation technology of this dead size complicated shape crystalline ceramics part, be suitable for preparing dead size, in high precision, the crystalline ceramics part of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Embodiment 9.
The preparation technology of a kind of dead size complicated shape crystalline ceramics part, carries out as follows.
(1) ceramic body is prepared with injection moulding method.
Step (1) prepares ceramic body with injection moulding method and specifically includes:
(1.1) ceramic powder surface modification
Using the yittrium oxide nano-ceramic powder of purity 99.9% as raw material, in the way of chemical precipitation, obtain the ceramic composite powder containing sintering aid by the magnesium oxide of magnetic stirring apparatus introducing 0.5wt% as knot auxiliary agent.Specifically adopt the chloride of magnesium, use ammonia to regulate the pH value of slurry to 9.2～11.4 so that Mg2+The surface of ceramic powder granule is deposited to the form of chemical precipitation.
Afterwards surface modifier is carried out together with ceramic composite powder ball milling pretreatment, forms the clad of one layer of several nano thickness in composite ceramic powder surface, after drying, obtain surface modification ceramic powder.Surface modifier is oleic acid, and the total amount of surface modifier accounts for the 0.8wt% of ceramic composite powder total amount.
(1.2) mixing
Organic binder bond and surface modification ceramic powder are made injection suspended substance.In injection molding compound, it is 85% that surface modification ceramic powder accounts for the percentage by weight of injection molding compound, and it is 15% that organic binder bond accounts for the percentage by weight of injection molding compound.Mixing employing PEG/PVB system feeding.
(1.3) injection moulding obtains needing the ceramic body of shape.On injection (mo(u)lding) machine, injection moulding obtains the ceramic body of complicated shape.Regulate injection parameters, such as injection pressure, injection speed, barrel temperature, storing position etc., obtain intact injection base substrate.
(2) adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, specifically: first pass through water and extract defat by the water-soluble binder elimination in component, remove the nonaqueous binders in base substrate again through thermal debinding.
Water extracts defat specifically: being placed in water-bath by ceramic body and carry out water extract defat, temperature is 60 DEG C, and degreasing time is 15h.
Thermal debinding is specifically: the base substrate after water defat at 90 DEG C after air drying 20h, is put in baking oven thermal debinding 4h at 100 DEG C and obtained ripe base.
(3) in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.
Discharging plasma sintering equipment can be realized by high strength graphite crucible in the way of not to ripe base direct weighting, and the sintering temperature of discharge plasma sintering is 1500 DEG C, and heating rate is 40 DEG C/min, and temperature retention time is 10min.The ceramic member of required complicated shape is obtained after sintering.
The preparation technology of this dead size complicated shape crystalline ceramics part, by the control to each process, injection moulding is adopted to prepare the ceramic body of complicated shape, adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.Prepared crystalline ceramics part possess dead size, in high precision, the feature of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Embodiment 11.
The preparation technology of a kind of dead size complicated shape crystalline ceramics part, carries out as follows.
(1) ceramic body is prepared with injection moulding method.
Step (1) prepares ceramic body with injection moulding method and specifically includes:
(1.1) ceramic powder surface modification
Using the thorium oxide nano-ceramic powder of purity 99.9% as raw material, in the way of chemical precipitation, obtain the ceramic composite powder containing sintering aid by the lanthana of magnetic stirring apparatus introducing 0.3wt% as knot auxiliary agent.
Afterwards surface modifier is carried out together with ceramic composite powder ball milling pretreatment, forms the clad of one layer of several nano thickness in composite ceramic powder surface, after drying, obtain surface modification ceramic powder.Surface modifier is oleic acid, and the total amount of surface modifier accounts for the 0.6wt% of ceramic composite powder total amount.
(1.2) mixing
Organic binder bond and surface modification ceramic powder are made injection suspended substance.In injection molding compound, it is 90% that surface modification ceramic powder accounts for the percentage by weight of injection molding compound, and it is 16% that organic binder bond accounts for the percentage by weight of injection molding compound.Mixing employing PEG/PMMA system feeding.
(1.3) injection moulding obtains needing the ceramic body of shape.On injection (mo(u)lding) machine, injection moulding obtains the ceramic body of complicated shape.Regulate injection parameters, such as injection pressure, injection speed, barrel temperature, storing position etc., obtain intact injection base substrate.
(2) adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, specifically: first pass through water and extract defat by the water-soluble binder elimination in component, remove the nonaqueous binders in base substrate again through thermal debinding.
Water extracts defat specifically: being placed in water-bath by ceramic body and carry out water extract defat, temperature is 80 DEG C, and degreasing time is 10h.
Thermal debinding is specifically: the base substrate after water defat at 100 DEG C after air drying 20h, is put in baking oven thermal debinding 6h at 70 DEG C and obtained ripe base.
(3) in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.
Discharging plasma sintering equipment can be realized by high strength graphite crucible in the way of not to ripe base direct weighting, and the sintering temperature of discharge plasma sintering is 1580 DEG C, and heating rate is 60 DEG C/min, and temperature retention time is 12min.The ceramic member of required complicated shape is obtained after sintering.
The preparation technology of this dead size complicated shape crystalline ceramics part, by the control to each process, injection moulding is adopted to prepare the ceramic body of complicated shape, adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base, in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.Prepared crystalline ceramics part possess dead size, in high precision, the feature of high density, high uniformity, and functional, solve a difficult problem for the crystalline ceramics part preparing complicated shape.
Finally should be noted that; above example is only in order to illustrate technical scheme but not limiting the scope of the invention; although the present invention being explained in detail with reference to preferred embodiment; it will be understood by those within the art that; technical scheme can be modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention.
Claims (10)
1. the preparation technology of a dead size complicated shape crystalline ceramics part, it is characterised in that comprise the steps:
(1) ceramic body is prepared with injection moulding method；
(2) adopt water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base；
(3) in the way of not to ripe base direct weighting, carry out discharge plasma sintering by discharging plasma sintering equipment, after annealed polishing, obtain crystalline ceramics part.
2. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 1, it is characterised in that described step (1) prepares ceramic body with injection moulding method and specifically includes:
(1.1) ceramic powder surface modification
Using the purity high-purity nm ceramic powder be more than or equal to 99.9% as raw material, in the way of chemical precipitation, introduce trace sintering aid by magnetic stirring apparatus obtain the ceramic composite powder containing sintering aid；
Afterwards surface modifier is carried out together with ceramic composite powder ball milling pretreatment, forms the clad of one layer of several nano thickness in composite ceramic powder surface, after drying, obtain surface modification ceramic powder；
(1.2) mixing
Organic binder bond and surface modification ceramic powder are made injection suspended substance；
(1.3) injection moulding obtains needing the ceramic body of shape.
3. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 2, it is characterised in that:
Described ceramic powder is the purity yittrium oxide more than 99.9%, magnesium oxide, beryllium oxide, calcium oxide, thorium oxide, magnesium aluminate spinel, lead zirconate-titanate ceramic or is A Long pottery, aluminium nitride ceramics, Sialon ceramics；
Described sintering aid is one or more in magnesium oxide, yittrium oxide, lanthana, and the total amount of described sintering aid accounts for 0.1～1wt% of described ceramic powder total amount；
Described surface modifier is any one in stearic acid, oleic acid, ten dihydroxystearic acids, citric acid, and the total amount of surface modifier accounts for 0.1～3wt% of described ceramic composite powder total amount；
In described injection molding compound, it is 80%～90% that surface modification ceramic powder accounts for the percentage by weight of injection molding compound, and it is 10～20% that organic binder bond accounts for the percentage by weight of injection molding compound.
4. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 3, it is characterised in that:
In the way of chemical precipitation, obtain the ceramic composite powder containing sintering aid by magnetic stirring apparatus introducing trace sintering aid specifically adopt nitrate or the chloride of metal ion, ammonia is used to regulate the pH value of slurry to 9.2～11.4 so that metal ion deposits to the surface of ceramic powder granule with the form of chemical precipitation；
Ball milling adopt aluminium oxide ceramics ball grinder, abrading-ball is high-purity transparent alumina abrading-ball, and ball-milling medium is ethanol, ceramics, ethanol, abrading-ball three mass ratio be 1:1:2, rotating speed is 80rpm～240rpm, and Ball-milling Time is 3～12h.
5. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 2, it is characterised in that:
Described step (1.2) mixing employing PEG/PVB system feeding, binder system consists of:
22wt%PVB+33wt%PEG4000+33wt%PEG600+9wt%SA+2.5%DBP, the phenothiazine additionally adding 0.5wt% makes antioxidant；
First in double roll mill, add skeleton binding agent PVB, double; two roller is started after PVB presents molten state completely and double; two roll temperature rises to 170 DEG C, it is then respectively adding phenothiazine, PEG4000, PEG600 and SA, mixing altogether continuing 45min, before mixing end, 5min adds DBP to suppress to reach the purpose of plasticising.
6. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 2, it is characterised in that:
Described step (1.2) mixing employing PEG/PMMA system feeding, binder system consists of:
20wt%PMMA+30wt%PEG4000+35wt%PEG600+12wt%SA+2.5%DBP, the phenothiazine additionally adding 0.5wt% makes antioxidant；
First in double roll mill, add skeleton binding agent PMMA, double; two roller is started after PMMA presents molten state completely and double; two roll temperature rises to 170 DEG C, it is then respectively adding phenothiazine, PEG4000, PEG600 and SA, mixing altogether continuing 45min, before mixing end, 5min adds DBP to suppress to reach the purpose of plasticising.
7. the preparation technology of the dead size complicated shape crystalline ceramics part according to claim 1 to 6 any one, it is characterised in that:
Described step (2) adopts water to extract defat in conjunction with two step defat methods of thermal debinding, ceramic body to be carried out defat and obtain ripe base specifically: first passes through water and extracts defat and removed by the water-soluble binder in component, removes the nonaqueous binders in base substrate again through thermal debinding.
8. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 7, it is characterised in that:
Described water extracts defat specifically: being placed in water-bath by ceramic body and carry out water extract defat, temperature is 40～60 DEG C, and degreasing time is 8～20h；
Described thermal debinding is specifically: the base substrate after water defat at 80～100 DEG C after air drying 12～24h, is put into and temperature rises in Muffle furnace 450～500 DEG C of insulation 2～3h obtained ripe base, and heating rate is 2～4 DEG C/min.
9. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 1, it is characterised in that:
Described step (3) is specifically: ripe base is placed in graphite crucible, the graphite crucible entirety being stamped graphite cover being put in discharging plasma sintering equipment and be sintered, graphite crucible is applied pressure with fixing graphite crucible by the upper push-down head of discharging plasma sintering equipment.
10. the preparation technology of dead size complicated shape crystalline ceramics part according to claim 5, it is characterised in that:
In described step (3), the sintering temperature of discharge plasma sintering is 1300～1600 DEG C, and heating rate is 10～100 DEG C/min, and temperature retention time is 5～20min.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412148A (en) * | 2002-12-06 | 2003-04-23 | 王国梁 | Transparent alumina ceramic product and its production method |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569731A (en) * | 2004-04-23 | 2005-01-26 | 清华大学 | Li-Si-O-based high dielectric constant ceramic materials and method for synthesizing same |
| CN1709823A (en) * | 2005-06-21 | 2005-12-21 | 清华大学深圳研究生院 | Method for preparing transparent MgAlON ceramic and transparent MgAlON ceramic |
| CN101643360B (en) * | 2009-09-02 | 2012-05-16 | 清华大学 | Method for manufacturing dentate special-shaped ceramic components by injection molding |
| CN101691086A (en) * | 2009-10-29 | 2010-04-07 | 哈尔滨工业大学 | Powder micro injection molding method for ceramic substrate of printing head |
| CN102515720A (en) * | 2011-12-08 | 2012-06-27 | 西安交通大学 | Preparation method of transparent alumina ceramic |
| CN103833373A (en) * | 2014-01-02 | 2014-06-04 | 佛山市东方智柏纳米材料科技有限公司 | Environment-friendly production method for nanometer ultrafine ceramic |
-
2016
- 2016-01-13 CN CN201610025595.5A patent/CN105732050A/en active Pending
- 2016-01-31 WO PCT/CN2016/073023 patent/WO2017120990A1/en active Application Filing
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412148A (en) * | 2002-12-06 | 2003-04-23 | 王国梁 | Transparent alumina ceramic product and its production method |
Non-Patent Citations (2)
| Title |
|---|
| 刘伟: "透明氧化铝陶瓷成型与烧结工艺的基础研究", 《中国博士学位论文全文数据库 工程科技I辑（月刊）》 * |
| 谢志鹏 等: "高技术陶瓷精密注射成型的研究与应用进展", 《人工晶体学报》 * |
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