CN111253153A - Method for preparing toughened large-size ultrathin YAG transparent ceramic biscuit based on Isodam gel system - Google Patents
Method for preparing toughened large-size ultrathin YAG transparent ceramic biscuit based on Isodam gel system Download PDFInfo
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Abstract
The invention discloses a method for preparing a toughened large-size ultrathin YAG transparent ceramic biscuit based on an Isodam gel system, which comprises the following steps: respectively weigh Y2O3Powder of Al2O3The powder is used as ceramic powder; mixing and ball-milling ceramic powder, a sintering aid, a dispersing agent A, a grinding ball and absolute ethyl alcohol according to a certain proportion to obtain mixed slurry; drying, sieving and calcining the mixed slurry to obtain raw material powder formed by gel injection molding; mixing deionized water, an Isodam 104 solution, a dispersant B, a plasticizer, grinding balls and the raw material powder according to a certain proportion, and performing ball milling to adjust the pH value of the system to 10-12 to prepare ceramic slurry; vacuum defoaming, pouring the defoamed slurry into a mould by pressure injection, naturally gelling and solidifying at room temperature, drying and removing gelAnd obtaining the YAG ceramic biscuit. The preparation process is simple and environment-friendly, and the prepared ultrathin ceramic biscuit is good in flatness, not easy to crack and easy to demould.
Description
Technical Field
The invention belongs to the field of advanced ceramics, relates to a preparation method of large-size ultrathin transparent ceramics, and particularly relates to a method for preparing a toughened large-size ultrathin YAG transparent ceramic biscuit based on an Isobam gel system.
Background
YAG transparent ceramics have the inherent characteristics of high temperature resistance, corrosion resistance, high insulation, high strength and the like of ceramics, also have the optical performance of glass, and have wide application prospects in the fields of illumination display technology, optical technology, special instrument manufacturing, wireless electronics, information detection, high-temperature technology, military industry and the like. Particularly in the display field, the material can be used for various visible light and infrared light transmission windows and display panels of various devices, and YAG is used as a matrix material to prepare a new generation of fluorescent material. The large-size ultrathin YAG (base) ceramic can be used for designing side-light type LED backlight sources and replacing ultrathin glass in the original touch screen industry. Therefore, the large-size ultrathin YAG transparent ceramic with high optical quality has wide application prospect.
The traditional dry pressing molding is easy to have the defects of unevenness, cracking, deformation and the like under the conditions of large size and extreme thinness; the optical quality of YAG ceramics is certainly influenced by more organic matters in injection molding; the tape casting requires an expensive tape casting machine, and the organic tape casting causes harm to human bodies and environmental pollution due to the fact that the used additive contains certain toxicity.
Gel casting is a near-net-size forming process developed after slip casting and tape casting, and is successfully developed and developed by national laboratories of oak ridge in the United states. The process is characterized in that: the ceramic powder is dispersed in an organic monomer solution, and the organic monomer is subjected to in-situ polymerization reaction under the action of an initiator to form a network structure to wrap the ceramic powder therein, so as to form a hard blank. The gel casting molding has the advantages of high biscuit strength, no need of complex and expensive equipment and the like, and is the first choice for preparing large-size ultrathin YAG ceramics. Particularly, the Isobam gel system can be used as a gelling agent and a dispersing agent because the used Isobam is an alternating copolymer of isobutene and maleic anhydride, and has no toxicity and green color and obvious advantages.
However, for the molding requirements of large-size ultra-thin pieces, the Isobam gel system faces the following molding difficulties: (1) the thickness of the slice is less than or equal to 0.5mm, and the tension of water can prevent the slurry from being injected into the mould; (2) the blank sheet is difficult to demould after being formed and has insufficient toughness; (3) the flatness of the green sheet still needs to be further improved.
Disclosure of Invention
The invention aims to provide a method for preparing a toughened large-size ultrathin YAG transparent ceramic biscuit based on an Isobam gel system, which has the advantages of simple and environment-friendly process, obvious toughness of the prepared ceramic biscuit, and good compactness and uniformity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing a toughened large-size ultrathin YAG transparent ceramic biscuit based on an Isodam gel system comprises the following specific steps:
step one, according to a chemical formula Y3Al5O12The stoichiometric ratio of each element in (A) is measured by weighing Y2O3Powder of Al2O3The powder is used as ceramic powder; mixing and ball-milling the weighed ceramic powder, sintering aid, dispersant A, grinding balls and absolute ethyl alcohol according to a certain proportion to obtain mixed slurry; drying the mixed slurry, sieving the dried mixed slurry by a 200-mesh sieve, and then placing the sieved powder into a muffle furnace for calcining to obtain raw material powder formed by gel injection molding;
mixing and ball-milling deionized water, an Isodam 104 solution, a dispersant B, a plasticizer, grinding balls and the raw material powder according to a certain proportion, and adjusting the pH value of the system to 10-12 by using a pH regulator to prepare YAG ceramic slurry with the solid content of 70-80 wt.%;
step three, placing the YAG ceramic slurry obtained in the step two under a vacuum condition of 1-2 torr for degassing for 2-5 min; pouring the YAG slurry subjected to vacuum defoaming into a mold by adopting a pressure injection method, naturally gelling and curing for 12-24 h at room temperature, wherein the mold is a glass plate combined mold with the flatness of less than or equal to 0.001mm, and a precisely processed ultrathin filler strip is clamped between an upper glass plate and a lower glass plate to control the thickness of a ceramic blank;
and step four, slowly taking out the ceramic biscuit after the gel curing from the mold, and sequentially carrying out drying treatment and glue discharging treatment to obtain the YAG ceramic biscuit.
Preferably, in the first step, the sintering aid is magnesium oxide (MgO) and Tetraethoxysilane (TEOS), the addition amount of the sintering aid is 0.1 to 0.5 wt% of the total mass of the raw material powder, the dispersant a is Polyetherimide (PEI), the addition amount of the dispersant a is 0.1 to 0.8 wt% of the total mass of the raw material powder, and the grinding ball is high-purity Al2O3And the total mass ratio of the grinding balls to the raw material powder is 1-3: 1.
Preferably, in the first step, the drying temperature is 50-60 ℃, and the drying time is 24-48 h; the specific process of the calcination is as follows: and heating to 700-900 ℃ from room temperature, keeping the temperature for 6-8 h at the heating rate of 2-3 ℃/min, and then cooling to 100 ℃ from room temperature at the cooling rate of 1-3 ℃/min.
Preferably, in the second step, the addition amount of the Isobam104 solution is 2.5-5 wt.% of the total mass of the raw material powder; the dispersing agent B is one of ammonium citrate, polyacrylic acid and polyethylene glycol, and the adding amount of the dispersing agent B is 0.2-0.5 wt% of the total mass of the raw material powder; the plasticizer is glycerol or ethylene glycol, and the adding amount of the plasticizer is 1-5 wt% of the total mass of the raw material powder; the pH regulator is ammonia water or tetramethyl ammonium hydroxide.
Preferably, in the fourth step, the drying specifically comprises the following steps: preserving heat for 24-72 h at the temperature of 25-35 ℃; then heating to 55-80 ℃, and preserving heat for 24-72 h; the rubber discharging method comprises the following specific steps: raising the temperature to 400-500 ℃ at the speed of 0.5-2 ℃/min at room temperature, preserving the heat for 4-8 h, raising the temperature to 800-900 ℃ at the speed of 0.5-2 ℃/min, and preserving the heat for 4-8 h.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention overcomes the problem that the casting is difficult to realize due to the extremely thin thickness caused by the tension of water in the prior art, and controls the thickness of the ceramic blank by using the precisely processed ultrathin filler strip, thereby not only controlling the flatness, but also ensuring the thickness.
2. According to the method for preparing the toughened large-size ultrathin YAG transparent ceramic blank by using the Isobam gel system, provided by the invention, the Isobam ceramic slurry containing the plasticizer is injected into a glass plate assembling die, and the addition of the plasticizer ensures that the ultrathin part is not easy to crack in the drying process and easy to demould, so that the method is simple and efficient.
Drawings
FIG. 1 is a diagram of an example in which no plasticizer is added, and extensive cracking occurs during demolding after Isobam gelation.
FIG. 2 is a physical diagram of a toughened ceramic biscuit with plasticizer added in example 1 of the present invention.
FIG. 3 is a diagram of an ultrathin large-sized ceramic biscuit in example 3 of the present invention after the addition of a plasticizer and after complete drying.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
The raw material powders used in the following examples were all high-purity (not less than 99.99%) powders. The glass plate assembling die used in the following examples comprises an upper glass plate and a lower glass plate with flatness less than or equal to 0.001mm, and a precisely machined ultrathin filler strip is clamped between the two glass plates to control the thickness of a ceramic body.
Example 1:
(1) according to Y3Al5O12Stoichiometric ratios of the molecular formulae separately weigh nanoscale Y2O371.324g powder, Al2O353.676g of powder, putting the oxide raw material powder into a high-purity alumina ceramic ball-milling tank, adding 375g of high-purity alumina grinding balls, and adding a sintering aid MgO and TEOS, a dispersant PEI and absolute ethyl alcohol to prepare slurry; ball-milling for 15h on a planetary ball mill at the rotating speed of 160r/min(ii) a Drying the obtained mixed slurry A at 60 ℃ for 24h, sieving the dried mixed slurry A by a 100-mesh sieve for 3 times, calcining the sieved powder in a muffle furnace, wherein the calcining process is to heat the mixed slurry A to 700 ℃ from room temperature, the heating rate is 2 ℃/min, keeping the temperature for 6h, and then naturally cooling the mixed slurry A to room temperature to obtain the powder which is the raw powder for gel casting. Then adding deionized water, an Isobam104 solution, a dispersant ammonium citrate, high-purity alumina grinding balls and 1.5g of a glycerol plasticizer into a ball-milling tank, finally adding the raw material powder, adjusting the pH value to 10 by using tetramethylammonium hydroxide, primarily stirring for 10min, and then carrying out ball-milling mixing, wherein the ball-milling rotation speed is 250r/min, and the ball-milling time is 60min, so as to obtain mixed slurry B with the solid content of 80 wt.%; namely the slurry used for gel casting; the prepared slurry has good fluidity and high solid content.
(2) Carrying out defoaming treatment on the gel slurry obtained in the step (1), wherein the conditions are as follows: degassing for 2min under a vacuum environment of 1 torr; then pouring the YAG slurry into a glass plate assembling die by adopting an injector method, and naturally gelling and curing for 12h at room temperature.
(3) Slowly taking out the ceramic biscuit after complete gelation from the mould, putting the ceramic biscuit into an oven, and preserving heat for 24 hours at 25 ℃; then the temperature is raised to 55 ℃ and the temperature is preserved for 24 h. And (3) after drying, removing the glue, heating to 400 ℃ at the speed of 0.5 ℃/min at room temperature, preserving heat for 4h, heating to 800 ℃ at the speed of 0.5 ℃/min, preserving heat for 4h, and effectively removing organic matters.
FIG. 2 is a physical representation of a toughened ceramic greenbody of example 1 with the addition of a plasticizer. The gel biscuit is perfect in appearance, uniform in whole, free of cracks or fractures and provided with certain strength and toughness. FIG. 1 is a schematic representation of a comparative example which was prepared in the same manner as in example 1, except that no plasticizer was added, and extensive cracking during demolding was observed after Isobam gel had formed.
Example 2:
(1) according to Y3Al5O12Stoichiometric ratios of the molecular formulae separately weigh nanoscale Y2O371.324g powder, Al2O353.676g of powder, putting the oxide raw material powder into a high-purity alumina ceramic ball milling tank, adding 125g of high-purity alumina grinding balls, and addingAdding sintering aids MgO and TEOS, a dispersant PEI and absolute ethyl alcohol to prepare slurry; ball-milling for 24 hours on a planetary ball mill at the rotating speed of 120 r/min; drying the obtained mixed slurry A at 50 ℃ for 48h, sieving the dried mixed slurry A by a 100-mesh sieve for 3 times, calcining the sieved powder in a muffle furnace, wherein the calcining process is to heat the mixed slurry A to 900 ℃ from room temperature, the heating rate is 3 ℃/min, keeping the temperature for 8h, and then naturally cooling the mixed slurry A to 100 ℃ to obtain the powder which is the raw powder for gel casting. Then adding deionized water, an Isobam104 solution, a dispersant which is polyethylene glycol, high-purity alumina grinding balls and a plasticizer which is a mixture of 6g of ethylene glycol and 0.25g of glycerol into a ball-milling tank, finally adding the raw material powder, adjusting the pH value to 12 by using tetramethylammonium hydroxide, carrying out ball-milling mixing after preliminary stirring for 30min, wherein the ball-milling rotation speed is 350r/min, and the ball-milling time is 20min, so as to obtain mixed slurry B with the solid content of 75 wt.%; namely the slurry used for gel casting; the prepared slurry has good fluidity and high solid content.
(2) Carrying out defoaming treatment on the gel slurry obtained in the step (1), wherein the conditions are as follows: degassing for 5min under a vacuum environment of 2 torr; then pouring the YAG slurry into a glass plate combined mould by adopting an air compressor assisted method, and naturally gelling and curing for 24h at room temperature.
(3) Slowly taking out the ceramic biscuit after complete gelation from the mould, putting the ceramic biscuit into a drying oven after complete gelation, and keeping the temperature for 72 hours at 35 ℃; then the temperature is increased to 80 ℃ and the temperature is preserved for 72 h. And (3) after drying, removing the glue, heating to 500 ℃ at the room temperature at the speed of 2 ℃/min, preserving the heat for 8h, heating to 900 ℃ at the speed of 2 ℃/min, preserving the heat for 8h, and effectively removing organic matters. The obtained YAG ceramic biscuit without defects has certain strength and toughness.
Example 3:
(1) according to Y3Al5O12Stoichiometric ratios of the molecular formulae separately weigh nanoscale Y2O371.324g powder, Al2O353.676g of powder, putting the oxide raw material powder into a high-purity alumina ceramic ball milling tank, adding 250g of high-purity alumina grinding balls, and adding a sintering aid MgO and TEOS, a dispersant PEI and absolute ethyl alcohol to prepare slurry; ball-milling for 20 hours on a planetary ball mill at the rotating speed of 150 r/min; to obtainDrying the mixed slurry A at 55 ℃ for 36h, sieving the dried mixed slurry A by a 200-mesh sieve for 3 times, calcining the sieved powder in a muffle furnace, wherein the calcining process is to heat the mixed slurry A to 800 ℃ from room temperature, the heating rate is 2 ℃/min, keeping the temperature for 7h, and then naturally cooling the calcined mixed slurry A to 50 ℃ to obtain the powder which is the raw powder for gel casting. Then adding deionized water, an Isobam104 solution, a dispersant ammonium polyacrylate, high-purity alumina grinding balls and 5g of plasticizer ethylene glycol into a ball-milling tank, finally adding the raw material powder, adjusting the pH value to 11 by using ammonia water, primarily stirring for 20min, and then carrying out ball-milling mixing, wherein the ball-milling rotation speed is 350r/min, and the ball-milling time is 40min, so as to obtain mixed slurry B with the solid content of 70 wt.%; namely the slurry used for gel casting; the prepared slurry has good fluidity and low viscosity.
(2) Carrying out defoaming treatment on the gel slurry obtained in the step (1), wherein the conditions are as follows: degassing for 3min under a vacuum environment of 1.5 torr; YAG slurry was then cast into a glass plate assembly mold using a pilot injection method and allowed to gel cure naturally for 18 hours at room temperature.
(3) Slowly taking out the ceramic biscuit after complete gelation from the glass plate assembly mold, putting the ceramic biscuit into a drying oven after complete gelation, and keeping the temperature for 48 hours at 30 ℃; then the temperature is raised to 70 ℃ and the temperature is preserved for 48 hours. And (3) after drying, removing the glue, heating to 450 ℃ at the room temperature at the speed of 1 ℃/min, preserving the heat for 6h, heating to 850 ℃ at the speed of 1 ℃/min, preserving the heat for 6h, and effectively removing organic matters. The shape of the gel biscuit is intact and the gel biscuit is tough.
FIG. 3 is a diagram of an ultrathin large-sized ceramic biscuit in example 3 of the present invention after the addition of a plasticizer and after complete drying. It can be seen that the thickness of the biscuit is only 0.50mm, and the biscuit has large size, perfect appearance, uniform whole, no crack or fracture, and certain strength and toughness.
Claims (5)
1. A method for preparing a toughened large-size ultrathin YAG transparent ceramic biscuit based on an Isodam gel system is characterized by comprising the following specific steps:
step one, according to a chemical formula Y3Al5O12The stoichiometric ratio of each element in (A) is measured by weighing Y2O3Powder of Al2O3The powder is used as ceramic powder; mixing and ball-milling the weighed ceramic powder, sintering aid, dispersant A, grinding balls and absolute ethyl alcohol according to a certain proportion to obtain mixed slurry; drying the mixed slurry, sieving the dried mixed slurry by a 200-mesh sieve, and then placing the sieved powder into a muffle furnace for calcining to obtain raw material powder formed by gel injection molding;
mixing and ball-milling deionized water, an Isodam 104 solution, a dispersant B, a plasticizer, grinding balls and the raw material powder according to a certain proportion, and adjusting the pH value of the system to 10-12 by using a pH regulator to prepare YAG ceramic slurry with the solid content of 70-80 wt.%;
step three, placing the YAG ceramic slurry obtained in the step two under a vacuum condition of 1-2 torr for degassing for 2-5 min; pouring the YAG slurry subjected to vacuum defoaming into a mold by adopting a pressure injection method, naturally gelling and curing for 12-24 h at room temperature, wherein the mold is a glass plate combined mold with the flatness of less than or equal to 0.001mm, and a precisely processed ultrathin filler strip is clamped between an upper glass plate and a lower glass plate to control the thickness of a ceramic blank;
and step four, slowly taking out the ceramic biscuit after the gel curing from the mold, and sequentially carrying out drying treatment and glue discharging treatment to obtain the YAG ceramic biscuit.
2. The method for preparing a toughened large-size ultrathin YAG transparent ceramic biscuit based on an Isobam gel system according to claim 1, wherein the sintering aids are magnesium oxide and tetraethoxysilane, the addition amount of the sintering aids is 0.1-0.5 wt% of the total mass of the raw material powder, the dispersing agent A is polyetherimide, the addition amount of the dispersing agent A is 0.1-0.8 wt% of the total mass of the raw material powder, and the grinding balls are high-purity Al2O3And the total mass ratio of the grinding balls to the raw material powder is 1-3: 1.
3. The method for preparing the toughened large-size ultrathin YAG transparent ceramic biscuit based on the Isobam gel system according to claim 1, wherein in the first step, the drying temperature is 50-60 ℃, and the drying time is 24-48 h; the specific process of the calcination is as follows: and heating to 700-900 ℃ from room temperature, keeping the temperature for 6-8 h at the heating rate of 2-3 ℃/min, and then cooling to 100 ℃ from room temperature at the cooling rate of 1-3 ℃/min.
4. The method for preparing the toughened large-size ultrathin YAG transparent ceramic biscuit based on the Isobam gel system as claimed in claim 1, wherein in the second step, the addition amount of the Isobam104 solution is 2.5-5 wt.% of the total mass of the raw material powder; the dispersing agent B is one of ammonium citrate, polyacrylic acid and polyethylene glycol, and the adding amount of the dispersing agent B is 0.2-0.5 wt% of the total mass of the raw material powder; the plasticizer is glycerol or ethylene glycol, and the adding amount of the plasticizer is 1-5 wt% of the total mass of the raw material powder; the pH regulator is ammonia water or tetramethyl ammonium hydroxide.
5. The method for preparing the toughened large-size ultrathin YAG transparent ceramic biscuit based on the Isobam gel system as claimed in claim 1, wherein in the fourth step, the drying comprises the following specific steps: preserving heat for 24-72 h at the temperature of 25-35 ℃; then heating to 55-80 ℃, and preserving heat for 24-72 h; the rubber discharging method comprises the following specific steps: raising the temperature to 400-500 ℃ at the speed of 0.5-2 ℃/min at room temperature, preserving the heat for 4-8 h, raising the temperature to 800-900 ℃ at the speed of 0.5-2 ℃/min, and preserving the heat for 4-8 h.
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