CN114409394B - Preparation method of large-size YAG transparent ceramic sheet - Google Patents
Preparation method of large-size YAG transparent ceramic sheet Download PDFInfo
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- CN114409394B CN114409394B CN202210048586.3A CN202210048586A CN114409394B CN 114409394 B CN114409394 B CN 114409394B CN 202210048586 A CN202210048586 A CN 202210048586A CN 114409394 B CN114409394 B CN 114409394B
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Abstract
A preparation method of a large-size YAG transparent ceramic sheet comprises the following steps: will Y 2 O 3 Powder and Al 2 O 3 Placing the powder, polyetherimide and sintering aid in a ball milling tank, and calcining after ball milling, drying and sieving to obtain YAG powder for water-based tape casting; mixing polyacrylic acid, ammonium hydroxide and deionized water to prepare a premixed solution; adding YAG powder into the premixed liquid for primary ball milling, adding a plasticizer, a binder and polypropylene glycol, performing secondary ball milling to prepare water-based YAG ceramic slurry, carrying out tape casting after removing bubbles, demoulding after drying to obtain a casting film, and carrying out cutting lamination, cold isostatic pressing and warm isostatic pressing on the casting film to obtain a biscuit; calcining the biscuit at 900-1100 ℃ for 10-15 h in air atmosphere, then placing the biscuit in a vacuum furnace for sintering, and annealing in a muffle furnace to obtain the YAG transparent ceramic sheet. The method effectively improves the defects that the large-size ceramic sheet is easy to deform and crack when being dried.
Description
Technical Field
The invention relates to the technical field of transparent ceramic preparation, in particular to a preparation method of a large-size YAG transparent ceramic sheet.
Background
The transparent ceramic is a polycrystalline material with light transmission prepared by adopting a ceramic process. In 1959, the ceramic was first proposed to have light transmissivity by the American general electric company, and then translucent Al was first prepared by the Coble doctor of the GE company in 1962 2 O 3 The ceramic opens up a new application field of ceramic materials. Through years of research and development, transparent ceramics become a variety of important functional ceramics, which are mainly divided into two categories, namely oxide transparent ceramics and non-oxide transparent ceramics, among the oxide transparent ceramics, YAG transparent ceramics have the advantages of highly symmetrical crystal structure, good thermodynamic and optical properties, wide light-transmitting wave band, stable physicochemical properties and the like, and are widely researched and applied in the fields of solid laser gain media, window materials, white light LEDs and the like.
In recent years, with the continuous expansion of the application field of YAG transparent ceramics, the dry pressing technique has been difficult to meet the application requirements of transparent ceramics in size and shape, such as high power laser gain media, large-sized optical devices, and the like. The tape casting is a ceramic colloidal forming technology, which is characterized in that slurry with good fluidity is injected into a tape casting machine, then the slurry is formed by a scraper, long chains of the slurry are mutually wound to form a three-dimensional network, and a biscuit is formed after demoulding and drying. The technology has great advantages in the aspect of preparing large-size and ultrathin ceramic parts. Compared with other ceramic forming technologies, tape casting has the advantages of simple process, low equipment cost and uniform formed biscuit.
Since the invention of tape casting, a plurality of solvent systems have been formed at present, the traditional organic tape casting system has the advantages of fast drying, no crack, uniform prepared biscuit and the like, but the organic tape casting system has certain toxicity and is not beneficial to human health. The water-based tape casting system is a clean, environment-friendly and nontoxic system, but the system has the defects of high organic matter content in the formula, easiness in cracking during drying, high viscosity of a bonding system, inconvenience in preparing slurry with high solid content and the like, so that the prepared large-size ceramic sheet biscuit is easy to deform after vacuum sintering and is not favorable for subsequent polishing and industrial application.
Disclosure of Invention
The invention aims to provide a preparation method of a large-size YAG transparent ceramic sheet, which can enable a biscuit to generate YAM (Y) in a glue discharging stage 4 Al 2 O 9 ) The newly formed YAM phase contributes to Al 2 O 3 And Y 2 O 3 Stronger combination is formed among the ceramic powders, and the defects of easy deformation, easy crack generation during drying and the like of large-size ceramic sheets can be effectively improved.
In order to realize the purpose, the invention adopts the technical scheme that: a preparation method of a large-size YAG transparent ceramic sheet comprises the following steps:
(1) According to Y 3 Al 5 O 12 Stoichiometric ratio of Y 2 O 3 Powder and Al 2 O 3 The powder is used as ceramic powder, absolute ethyl alcohol is used as a ball milling medium, accurately weighed ceramic powder, dispersant polyetherimide and sintering aid are placed in a ball milling tank, and the ceramic powder, the dispersant polyetherimide and the sintering aid are sequentially subjected to ball milling, drying and sieving and then placed in a muffle furnace to be calcined to obtain YAG powder for water-based tape casting;
(2) Mixing polyacrylic acid serving as a dispersant, ammonium hydroxide serving as a pH regulator and deionized water to prepare a premixed solution;
(3) Adding the YAG powder prepared in the step (1) into the premixed liquid prepared in the step (2) for primary ball milling, then sequentially adding a plasticizer, a binder and defoaming agent polypropylene glycol, and then performing secondary ball milling to prepare water-based YAG ceramic slurry with the solid content of 45-55 wt%;
(4) Defoaming the water-based YAG ceramic slurry obtained in the step (3) by adopting a planetary vacuum defoaming machine, pouring the defoamed ceramic slurry into a trough of a casting machine for casting molding, drying for 20-24 h at room temperature, curing the slurry, demolding to obtain a casting film, and cutting and laminating the casting film, and carrying out cold isostatic pressing and warm isostatic pressing to obtain a biscuit with the thickness of 5-8 mm;
(5) And (3) carrying out glue discharging treatment on the biscuit obtained in the step (4) in a muffle furnace, calcining the biscuit at 900-1100 ℃ for 10-15 h in an air atmosphere, then sintering the biscuit in a vacuum furnace after glue discharging, and finally annealing the biscuit in the muffle furnace to obtain the YAG transparent ceramic.
Preferably, in the step (1), the addition amount of the dispersant polyetherimide is 0.1-0.5% of the total mass of the ceramic powder; the sintering aid is magnesium oxide and ethyl orthosilicate in a mass ratio of 1: (1-5), the addition amount of the sintering aid is 0.1-0.5% of the total mass of the ceramic powder.
Preferably, in the step (2), the addition amount of the polyacrylic acid is 0.4-1.0% of the total mass of the ceramic powder; the addition amount of the pH regulator is 0.8-1.6% of the total mass of the ceramic powder.
Preferably, in the step (3), the plasticizer is one or two of polyethylene glycol and glycerol, and the addition amount of the plasticizer is 2.0-6.0% of the total mass of the ceramic powder; the adhesive is polyvinyl alcohol, and the addition amount of the adhesive is 3.0-6.0% of the total mass of the ceramic powder; the addition amount of the defoaming agent polypropylene glycol is 1.0-1.6% of the total mass of the ceramic powder.
Preferably, in the step (3), the ball milling is carried out for 8-12 h for the first time; and performing secondary ball milling for 12-18 hours.
Preferably, in the step (4), the casting base tape in the casting machine is cellophane, the humidity is 40 to 60% RH, the casting film is cut into a square with a side length of 5 to 8cm, the time of cold isostatic pressing is 5 to 8min, and the pressure is 200 to 300MPa; the time of the warm isostatic pressing is 10-20 min, the temperature is 70-80 ℃, and the pressure is 40-60 MPa.
Preferably, in the step (4), the vacuum pressure of the vacuum defoaming machine is 0.2-1.0 KPa, and the defoaming time is 1-2 min.
Preferably, in the step (5), the vacuum sintering temperature is 1650-1870 ℃, and the vacuum degree in a vacuum furnace chamber is kept at 10 -3 ～10 -4 Pa, the sintering time is 15-20 h; the annealing temperature is 1200-1600 ℃, and the annealing time is 10-20 h.
Compared with the prior art, the invention has the following advantages:
(1) The ceramic sheet is prepared by water-based tape casting, and the process is green and environment-friendly; in addition, the polypropylene glycol used in the invention not only serves as a defoaming agent, but also serves as a nonionic surfactant to be adsorbed on the surface of the ceramic powder, so that the surface tension of water is effectively reduced, the contact angle between the water-based slurry and the high-polarity tape casting base band is reduced to about 10 degrees, the addition amount of organic matters such as a binder and the like is effectively reduced, the viscosity of the slurry is reduced, and the biscuit is molded to obtain a uniform and soft biscuit;
(2) In the invention, the biscuit is degummed for 10 to 15 hours at 900 to 1000 ℃, so that YAM phase is generated in the degummed stage, and the newly formed YAM phase is beneficial to Al 2 O 3 And Y 2 O 3 Stronger combination is formed among the ceramic powder bodies, and the defects that a large-size ceramic sheet is easy to deform and crack when being dried are effectively overcome.
Drawings
FIG. 1 is a photograph of a cast film prepared according to example one of the present invention;
FIG. 2 is a graph of the optical transmittance and the physical property of a YAG transparent ceramic sheet prepared in accordance with one embodiment of the present invention;
FIG. 3 is a XRD analysis chart of the biscuit prepared by the first embodiment of the invention after the glue is discharged;
FIG. 4 is a comparison of the 3D profile scan of a ceramic (a) prepared according to example one of the present invention and a ceramic (b) without a sintering pretreatment.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Example one
A preparation method of a large-size YAG transparent ceramic sheet comprises the following steps:
(1) According to Y 3 Al 5 O 12 Stoichiometric ratio of Y 2 O 3 Powder and Al 2 O 3 The powder was used as a ceramic powder 60g in total, and the ceramic powder, 0.06g of polyetherimide (ceramic powder total mass: 0.1%), 0.06g of magnesium oxide and normal alumina were weighed accurately with anhydrous ethanol as a ball milling mediumPutting ethyl silicate (the total mass of the ceramic powder is 0.1%) into a ball milling tank, wherein the mass ratio of magnesium oxide to ethyl orthosilicate is 1:1, sequentially performing ball milling, drying and 200-mesh sieving, and then placing the powder in a muffle furnace for calcining to obtain YAG powder for water-based tape casting;
(2) 0.24g of dispersant polyacrylic acid (0.4 percent of the total mass of the ceramic powder), 0.48g of pH regulator ammonium hydroxide (0.8 percent of the total mass of the ceramic powder) and deionized water are mixed to prepare a premixed solution;
(3) Adding the YAG powder prepared in the step (1) into the premixed liquid prepared in the step (2) for ball milling for 8 hours, sequentially adding 1.2g of polyethylene glycol and 1.2g of glycerol (each is added with 2.0 percent of the total mass of the ceramic powder), 1.8g of polyvinyl alcohol (3.0 percent of the total mass of the ceramic powder), 0.6g of defoaming agent polypropylene glycol (1.0 percent of the total mass of the ceramic powder) and ball milling for 12 hours to prepare water-based YAG ceramic slurry with the solid content of 50 wt%;
(4) Removing bubbles from the water-based YAG ceramic slurry obtained in the step (3) for 2min under the vacuum pressure of 0.2KPa by adopting a planetary vacuum bubble removing machine; pouring the ceramic slurry after bubble removal into a casting machine trough, carrying out casting molding on a glass paper casting base band, drying at the room temperature of 40RH for 20h, solidifying the slurry, demolding to obtain a casting film, cutting the casting film into square rear laminations with the side length of 5-8 cm, carrying out cold isostatic pressing at 200MPa for 5min, and carrying out warm isostatic pressing at 70 ℃ and 40MPa for 10min to obtain a biscuit with the thickness of 5 mm;
(5) Carrying out degumming treatment on the biscuit obtained in the step (4) in a muffle furnace, calcining for 10h at 1000 ℃ in air atmosphere, and finally placing the biscuit at 1780 ℃ and a vacuum degree of 10 -3 Sintering for 15h in a vacuum furnace, and finally annealing for 10h in a muffle furnace at 1200 ℃ to obtain the YAG transparent ceramic sheet.
As shown in FIG. 1, which is a real image of the trimmed casting film prepared in step (4) of this example, it can be seen that the casting film is uniform, soft and flexible.
As shown in FIG. 2, which is a graph showing the optical transmittance and the physical property of the YAG transparent ceramic flake prepared in this example, it can be seen that the ceramic flake has a transmittance as high as 83% and has excellent light transmittance.
As shown in FIG. 3, which is an XRD analysis chart of the biscuit after high-temperature degumming obtained in step (5) of this example, YAM phase appears in the biscuit after degumming.
As shown in FIG. 4, which is a 3D contour scan of the YAG transparent ceramic flake prepared in this example, it can be seen that the transparent ceramic flake has almost no deformation.
Example two
A preparation method of a large-size YAG transparent ceramic sheet comprises the following steps:
(1) According to Y 3 Al 5 O 12 Stoichiometric ratio of Y 2 O 3 Powder and Al 2 O 3 Taking 60g of powder as ceramic powder, taking absolute ethyl alcohol as a ball milling medium, and putting accurately weighed ceramic powder, 0.18g of polyetherimide (the total mass of the ceramic powder is 0.3%), 0.18g of magnesium oxide and tetraethoxysilane (the total mass of the ceramic powder is 0.3%) into a ball milling tank, wherein the mass ratio of the magnesium oxide to the tetraethoxysilane is 1:3, sequentially performing ball milling, drying and 200-mesh sieving, and then placing in a muffle furnace for calcining to obtain YAG powder for water-based tape casting;
(2) 0.36g of dispersant polyacrylic acid (0.6 percent of the total mass of the ceramic powder), 0.72g of pH regulator ammonium hydroxide (1.2 percent of the total mass of the ceramic powder) and deionized water are mixed to prepare a premixed solution;
(3) Adding the YAG powder prepared in the step (1) into the premixed liquid prepared in the step (2) for ball milling for 10 hours, sequentially adding 2.4g of polyethylene glycol (the total mass of the ceramic powder is 4.0%), 2.4g of polyvinyl alcohol (the total mass of the ceramic powder is 4.0%) and 0.72g of defoaming agent polypropylene glycol (the total mass of the ceramic powder is 1.2%) for ball milling for 15 hours, and preparing water-based YAG ceramic slurry with the solid content of 45 wt%;
(4) Defoaming the water-based YAG ceramic slurry obtained in the step (3) for 1.5min by adopting a planetary vacuum defoaming machine under the vacuum pressure of 0.7 KPa; pouring the ceramic slurry after bubble removal into a casting machine trough, carrying out casting molding on a glass paper casting base band, drying at the room temperature of 50RH for 22h, solidifying the slurry, demolding to obtain a casting film, cutting the casting film into square rear laminations with the side length of 5-8 cm, carrying out cold isostatic pressing at 250MPa for 6min, and carrying out warm isostatic pressing at 75 ℃ and 50MPa for 15min to obtain biscuit with the thickness of 6 mm;
(5) Carrying out glue discharging treatment on the biscuit obtained in the step (4) in a muffle furnace, calcining for 12h at 900 ℃ in air atmosphere, and finally placing the biscuit at 1650 ℃ and 10 degrees of vacuum -3 Sintering for 18h in a vacuum furnace, and finally, placing in a muffle furnace at 1400 ℃ for annealing for 15h to obtain the YAG transparent ceramic sheet.
The cut casting film prepared by the embodiment is uniform, soft and flexible, the prepared transparent ceramic sheet is almost free of deformation, and the transmittance of the transparent ceramic sheet can reach 83.4%.
EXAMPLE III
A preparation method of a large-size YAG transparent ceramic sheet comprises the following steps:
(1) According to Y 3 Al 5 O 12 Stoichiometric ratio of Y 2 O 3 Powder and Al 2 O 3 Taking 60g of powder as ceramic powder, taking absolute ethyl alcohol as a ball milling medium, and putting accurately weighed ceramic powder, 0.3g of polyetherimide (the total mass of the ceramic powder is 0.5%), 0.3g of magnesium oxide and tetraethoxysilane (the total mass of the ceramic powder is 0.5%) into a ball milling tank, wherein the mass ratio of the magnesium oxide to the tetraethoxysilane is 1:5, sequentially performing ball milling, drying and 200-mesh sieving, and then placing the powder in a muffle furnace for calcining to obtain YAG powder for water-based tape casting;
(2) 0.6g of dispersant polyacrylic acid (1.0 percent of the total mass of the ceramic powder), 0.96g of pH regulator ammonium hydroxide (1.6 percent of the total mass of the ceramic powder) and deionized water are mixed to prepare a premixed solution;
(3) Adding the YAG powder prepared in the step (1) into the premixed liquid prepared in the step (2), ball-milling for 12 hours, sequentially adding 3.6g of glycerol (6.0 percent of the total mass of the ceramic powder), 3.6g of polyvinyl alcohol (6.0 percent of the total mass of the ceramic powder) and 0.96g of defoaming agent polypropylene glycol (1.6 percent of the total mass of the ceramic powder), and ball-milling for 18 hours to prepare water-based YAG ceramic slurry with the solid content of 55 wt%;
(4) Defoaming the water-based YAG ceramic slurry obtained in the step (3) for 1min under the vacuum pressure of 1.0KPa by adopting a planetary vacuum defoaming machine; pouring the ceramic slurry after bubble removal into a casting machine trough, carrying out casting molding on a glass paper casting base band, drying at the room temperature of 60RH for 24h, solidifying the slurry, demolding to obtain a casting film, cutting the casting film into square rear laminations with the side length of 5-8 cm, carrying out cold isostatic pressing at 300MPa for 8min, and carrying out warm isostatic pressing at 80 ℃ and 60MPa for 20min to obtain a biscuit with the thickness of 8 mm;
(5) Carrying out degumming treatment on the biscuit obtained in the step (4) in a muffle furnace, calcining for 15h at 1100 ℃ in air atmosphere, and finally placing the biscuit at 1870 ℃ and a vacuum degree of 10 -4 Sintering for 20h in a vacuum furnace, and finally, annealing for 20h in a muffle furnace at 1600 ℃ to obtain the YAG transparent ceramic sheet.
The cut casting film prepared by the embodiment is uniform, soft and tough, the prepared transparent ceramic sheet is almost free from deformation, and the transmittance of the transparent ceramic sheet can reach 82.8%.
Claims (8)
1. A preparation method of a large-size YAG transparent ceramic sheet is characterized by comprising the following steps:
(1) According to Y 3 Al 5 O 12 Stoichiometric ratio of Y 2 O 3 Powder and Al 2 O 3 The powder is used as ceramic powder, absolute ethyl alcohol is used as a ball milling medium, accurately weighed ceramic powder, dispersant polyetherimide and sintering aid are placed in a ball milling tank, and the ceramic powder, the dispersant polyetherimide and the sintering aid are sequentially subjected to ball milling, drying and sieving and then placed in a muffle furnace to be calcined to obtain YAG powder for water-based tape casting;
(2) Mixing polyacrylic acid serving as a dispersant, ammonium hydroxide serving as a pH regulator and deionized water to prepare a premixed solution;
(3) Adding the YAG powder prepared in the step (1) into the premixed liquid prepared in the step (2) for primary ball milling, then sequentially adding a plasticizer, a binder and defoaming agent polypropylene glycol, and then performing secondary ball milling to prepare water-based YAG ceramic slurry with the solid content of 45-55 wt%;
(4) Defoaming the water-based YAG ceramic slurry obtained in the step (3) by adopting a planetary vacuum defoaming machine, pouring the defoamed ceramic slurry into a trough of a casting machine for casting molding, drying for 20-24 h at room temperature, curing the slurry, demolding to obtain a casting film, and cutting and laminating the casting film, and carrying out cold isostatic pressing and warm isostatic pressing to obtain a biscuit with the thickness of 5-8 mm;
(5) And (5) carrying out glue discharging treatment on the biscuit obtained in the step (4) in a muffle furnace, calcining at 1000-1100 ℃ for glue discharging for 10-15 h in an air atmosphere, generating a YAM phase in the biscuit at the glue discharging stage, sintering the biscuit after glue discharging in a vacuum furnace, and finally annealing in the muffle furnace to obtain the YAG transparent ceramic sheet.
2. The preparation method of the YAG transparent ceramic sheet with large size as claimed in claim 1, wherein in the step (1), the addition amount of the dispersant polyetherimide is 0.1-0.5% of the total mass of the ceramic powder; the sintering aid is magnesium oxide and ethyl orthosilicate in a mass ratio of 1: (1-5), the addition amount of the sintering aid is 0.1-0.5% of the total mass of the ceramic powder.
3. The method for preparing a large-size YAG transparent ceramic sheet according to claim 1 or 2, wherein in the step (2), the addition amount of the polyacrylic acid is 0.4-1.0% of the total mass of the ceramic powder; the addition amount of the pH regulator is 0.8-1.6% of the total mass of the ceramic powder.
4. The preparation method of YAG transparent ceramic sheet with large size as claimed in claim 1 or 2, wherein in step (3), the plasticizer is one or two of polyethylene glycol and glycerol, and the addition amount is 2.0-6.0% of the total mass of the ceramic powder; the adhesive is polyvinyl alcohol, and the addition amount of the adhesive is 3.0-6.0% of the total mass of the ceramic powder; the addition amount of the defoaming agent polypropylene glycol is 1.0-1.6% of the total mass of the ceramic powder.
5. The preparation method of the YAG transparent ceramic sheet with the large size as claimed in claim 1, wherein in the step (3), the ball milling is carried out for the first time for 8 to 12 hours; and performing secondary ball milling for 12 to 18h.
6. The method for preparing YAG transparent ceramic flakes of large size according to claim 1, wherein in step (4), the casting base band in said casting machine is cellophane, the humidity is 40-60% RH, the casting film is cut into squares of 5-8 cm side length, the time of cold isostatic pressing is 5-8 min, and the pressure is 200-300 MPa; the time of the warm isostatic pressing is 10-20 min, the temperature is 70-80 ℃, and the pressure is 40-60 MPa.
7. The preparation method of YAG transparent ceramic sheet with large size as claimed in claim 1, wherein in step (4), the vacuum pressure of the vacuum defoaming machine is 0.2-1.0 KPa, and the defoaming time is 1-2 min.
8. The method for preparing YAG transparent ceramic flakes with large size according to claim 1, wherein in step (5), the vacuum sintering temperature is 1650-1870 ℃, and the vacuum degree in the vacuum furnace chamber is kept at 10 -3 ～10 -4 Pa, the sintering time is 15-20 h; the annealing temperature is 1200-1600 ℃, and the annealing time is 10-20 h.
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