CN113773081A - Transparent ceramic and preparation method thereof - Google Patents
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Abstract
The invention discloses a transparent ceramic, which comprises a component Y2O3And an Er-containing dopant of the formula (Er)xY1‑x)2O3Weighing and mixing, wherein x is more than or equal to 0.0005 and less than or equal to 0.005, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Er, Y2O3Powder; adding Er to Y2O3Molding the powder to obtain a blank; sintering the biscuit in a vacuum environment at the temperature of 1400-1800 ℃ for 0.5-50h, sintering the biscuit in an inert gas at the temperature of 1400-1800 ℃ for 0.5-8h by hot isostatic pressing, finally annealing the biscuit in an air or oxygen atmosphere at the temperature of 600-1300 ℃ for 0.5-30h, and polishing the two surfaces to obtain Er, Y2O3Is transparentA ceramic; the invention adopts a mode of combining vacuum sintering and hot isostatic pressing treatment, and can prepare Er: Y with high optical quality on the premise of not additionally adding a sintering aid2O3Transparent ceramics, excited by suitable pump source, can use Er3+Of ions4I13/2→4I15/2The energy level transition can realize the output of 1.6 μm laser which can be safely absorbed by human eyes without generating the pump light darkening effect.
Description
Technical Field
The invention relates to transparent ceramic and a preparation method thereof, belonging to the technical field of transparent ceramic.
Background
With Y2O3The typical sesquioxide material has the advantages of low phonon energy, low thermal expansion coefficient, high thermal conductivity, high laser damage threshold and the like, and is one of ideal solid laser gain media. However, due to the extremely high melting point of the sesquioxide material: (>2400 deg.C), it is difficult to realize large-size single crystal preparation of high optical quality. By adopting a ceramic forming process, a large-size blank body is easy to prepare, and the transparency of the sesquioxide ceramic can be realized at a sintering temperature (1400 ℃ plus 1800 ℃) far lower than the melting point of the material by combining the regulation and control of a sintering system. In addition, compared with a single crystal material, the sesquioxide ceramic has higher mechanical strength and shorter preparation period, and is more suitable for mass production. The sesquioxide matrix is doped with a proper amount of active ions, and high optical quality equivalent to that of a sesquioxide single crystal is realized, so that high-power and high-efficiency laser output is expected to be realized.
For solid state laser systems, in addition to the host material, the choice of the active ion to be doped plays a crucial role in achieving stable and wavelength-specific laser operation. Wherein, Er3+Ions have rich energy level structures and wide absorption ranges, 970/976/980nm Laser Diodes (LD) or 1535nm fiber lasers can be generally selected as pumping sources, and Er is utilized3+:4I13/2→4I15/2Energy level transition ofNow a laser output with a center wavelength of about 1.6 μm.
Current pair Y2O3The sintering of transparent ceramics, whether vacuum sintering or atmosphere sintering, is usually doped with a certain amount of sintering aids to lower the sintering temperature of the ceramics or to suppress abnormal grain growth. However, the additional addition of sintering aids inevitably leads to a loss of material thermal conductivity on the one hand, exacerbating the thermal effect problem of the laser system. On the other hand, the addition of the sintering aid usually introduces point defects into the material lattice to form color centers, which easily causes the pump light darkening effect, resulting in the reduction of laser efficiency. Therefore, in addition to high optical quality and high thermal conductivity, the laser ceramic should also consider how to minimize the introduction of impurity defects.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a solid laser gain medium, so as to solve the problem that Y is produced by adding a sintering aid in the prior art2O3Transparent ceramics can cause the loss of the thermal conductivity of materials, and the technical problems of the thermal effect of a laser system and the darkening effect of pump light are aggravated.
In order to solve the technical problems, the invention is realized by adopting the following technical scheme:
a method for preparing a transparent ceramic, comprising:
step A, adding Y2O3And an Er-containing dopant of the formula (Er)xY1-x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0005 and less than or equal to 0.005, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Er, Y2O3Powder;
step B, adding Er to Y2O3Molding the powder to obtain a blank;
step C, sintering the biscuit in a vacuum environment at the temperature of 1400-1800 ℃ for 0.5-50h, then sintering the biscuit in an inert gas at the temperature of 1400-1800 ℃ for 0.5-8h in a hot isostatic manner, finally annealing the biscuit in an air or oxygen atmosphere at the temperature of 600-1300 ℃ for 0.5-30h, and polishing the two surfaces to obtain Er, Y2O3A transparent ceramic.
As a preferred embodiment of the present invention, step a includes:
weighing the high-purity Y2O3And Er-containing doping agent are placed in a ball mill, and absolute ethyl alcohol is added to obtain slurry with the powder content of 10-30 Vol%;
adding grinding balls into the slurry, and finishing ball milling treatment on the slurry through a ball mill;
placing the slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding the dried material, and screening to obtain a screened material with a particle diameter of less than 104 μm;
placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Er: Y2O3And (3) powder.
As a preferred technical scheme of the invention, the rotation speed of the ball milling treatment is 100-250rpm, and the ball milling time is 3-48 h;
and/or the mass ratio of the grinding balls to the mixed powder is 3:1-8: 1;
and/or the calcination temperature is 400-1100 ℃, and the calcination time is 3-10 h.
As a preferable technical scheme of the invention, the Er-containing dopant is Er2O3、ErCl3、Er(NO3)3、Er2(SO4)3One kind of (1).
As a preferred embodiment of the present invention, step B includes: adding Er to Y2O3Dry pressing the powder to obtain dry pressed Er: Y2O3And carrying out cold isostatic pressing on the powder to obtain a biscuit.
As a preferred technical scheme of the invention, the pressure of the dry pressing forming is 0.5-20 MPa;
and/or the pressure of the cold isostatic pressing is 100-200 MPa.
In a preferred embodiment of the present invention, the pressure of the hot isostatic pressing sintering is 50 to 200MPa, and the inert gas used for the hot isostatic pressing sintering includes argon and nitrogen.
As a preferable technical scheme of the invention, the vacuum degree of the vacuum environment is less than or equal to 10-3Pa。
The transparent ceramic is prepared by the preparation method.
The transparent ceramic is applied to a fixed laser medium of a laser;
further, the fixed laser gain medium is used for a 1.6 μm eye-safe laser.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts a mode of combining vacuum sintering and hot isostatic pressing treatment, and can prepare Er: Y with high optical quality on the premise of not additionally adding a sintering aid2O3Transparent ceramics, excited by suitable pump source, can use Er3+Of ions4I13/2→4I15/2And energy level transition is carried out, so that 1.6-micron laser output which can be safely absorbed by human eyes is realized under the condition of not generating a pump light darkening effect.
Drawings
FIG. 1 is a plot of the amount of Er: Y provided in example 1 of the present invention based on 0.25 at.% Er2O3A schematic diagram of a transparent ceramic solid-state laser device;
FIG. 2 is a 0.25 at.% Er: Y sintered in an oxygen atmosphere as provided in example 1 of the present invention2O3The transmission spectrum of the transparent ceramic;
FIG. 3 is a 0.25 at.% Er: Y sintered in an oxygen atmosphere as provided in example 1 of the present invention2O3A photograph of a sample of transparent ceramic;
FIG. 4 is a 0.25 at.% Er: Y provided by example 1 of the present invention2O3Laser spectrum of transparent ceramics.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
As shown in fig. 1 to 4, a method for preparing a transparent ceramic, comprising:
step A, adding Y2O3And an Er-containing dopant of the formula (Er)xY1-x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0005 and less than or equal to 0.005, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Er, Y2O3Powder;
when Er3+When the ion concentration is higher than 0.5 at.%, a significant upconversion phenomenon occurs, which is not favorable for the generation of 1.6 μm laser. Thus, the best case is according to the formula (Er)xY1-x)2O3(x is more than or equal to 0.0005 and less than or equal to 0.005) the raw materials are weighed.
Preparing Er and Y in step A2O3The powder comprises the following steps:
weighing the high-purity Y2O3And Er-containing doping agent are placed in a ball mill, and absolute ethyl alcohol is added to obtain slurry with the powder content of 10-30 Vol%;
adding grinding balls into the slurry, and finishing ball milling treatment on the slurry through a ball mill;
placing the slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding the dried material, and screening to obtain a screened material with a particle diameter of less than 104 μm;
placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Er: Y2O3And (3) powder.
The grinding balls added into the slurry are preferably high-purity zirconia balls, and the mass ratio of the grinding balls to the mixed powder is 3:1-8: 1.
The rotation speed of the ball milling treatment is 100 and 250rpm, the ball milling time is 3-48h, and the ball milling time is 3-48 h.
And (3) treating the slurry after ball milling treatment by using an oven, wherein the temperature of the oven is preferably 40-120 ℃, and the drying time is about 12-48h, so as to ensure that a dried material can be obtained finally.
It is noted that the calcining temperature of the muffle furnace to the sieved material is 400-1100 ℃, and the calcining time is 3-10 h.
Step B, adding Er to Y2O3Molding the powder to obtain a blank;
the biscuit can also be prepared by gel casting, slip casting, tape casting, extrusion molding and other molding modes, and can be prepared according to the actual selection of corresponding processes.
The preparation of the embryo comprises: and carrying out dry pressing on the Er: Y2O3 powder, and carrying out cold isostatic pressing on the dry pressed Er: Y2O3 powder to obtain a biscuit.
The pressure of dry pressing is 0.5-20MPa, which is unidirectional pressing.
The pressure of the cold isostatic pressing is 100-200MPa, and the compactness can be further improved in the process.
Step C, sintering the biscuit in a vacuum environment at the temperature of 1400-1800 ℃ for 0.5-50h, then sintering the biscuit in an inert gas at the temperature of 1400-1800 ℃ for 0.5-8h in a hot isostatic manner, finally annealing the biscuit in an air or oxygen atmosphere at the temperature of 600-1300 ℃ for 0.5-30h, and polishing the two surfaces to obtain Er, Y2O3A transparent ceramic.
Wherein the vacuum degree of the vacuum environment is less than or equal to 10-3Pa, the pressure of the hot isostatic pressing sintering is 50-200MPa, and the inert gases used for the hot isostatic pressing sintering comprise argon and nitrogen.
It is noted that the Er-containing dopant is one of Er2O3, ErCl3, Er (NO3)3, and Er2(SO4) 3.
A transparent ceramic is prepared by a preparation method.
Er:Y2O3The application of the transparent ceramic in a fixed laser medium of a laser; further, the fixed laser gain medium is used for a 1.6 μm eye-safe laser.
Example one
Selecting commercial high purityDegree Y2O3And Er2O3The powder is used as raw material. According to the formula (Er)0.0025Y0.9975)2O3The raw material was weighed, wherein the amount of yttrium oxide was 80 g. And adding 100mL of absolute ethyl alcohol and 500g of zirconia grinding balls, and then carrying out ball milling treatment, wherein the rotating speed of the ball mill is 140rpm, and the ball milling time is 10 h. Mixing the materials uniformly, drying in a 50 deg.C oven for about 48 hr, grinding, sieving, and calcining in a muffle furnace at 800 deg.C for 3 hr to obtain Er: Y2O3And (3) powder.
Adding Er to Y2O3The powder is firstly pressed unidirectionally under the pressure of 5MPa, and in order to further improve the density, the biscuit is subjected to cold isostatic pressing under the pressure of 200MPa to obtain Er, Y2O3A ceramic biscuit.
Firstly sintering the biscuit for 5h in 1500 ℃ flowing oxygen atmosphere, and then carrying out hot isostatic pressing sintering in 196MPa argon atmosphere, wherein the sintering temperature is 1450 ℃, and the sintering time is 3 h. Finally, the ceramic is annealed in air in a muffle furnace at 1200 ℃ for 10h to realize the transparent Er: Y2O3And (3) preparing the ceramic.
Compared with the prior art, the invention has at least the following beneficial effects:
in order to keep the high thermal conductivity of the material to the maximum extent, the method of combining vacuum sintering (or oxygen atmosphere sintering) with hot isostatic pressing treatment is adopted, and Er: Y with high optical quality can be prepared on the premise of not adding a sintering aid additionally2O3A transparent ceramic. On the premise of ensuring no obvious abnormal growth of crystal grains, the oxygen sintering has a wider sintering temperature range, and compared with vacuum sintering, the maximum sintering temperature of a sample can be increased by 10-50 ℃. Er: Y sintered in two ways2O3After the ceramic is sintered by hot isostatic pressing, a compact and nonporous microstructure can be formed, and excellent transparency and optical uniformity are shown after annealing. Under the excitation of a proper pump source, Er is utilized3+Of ions4I13/2→4I15/2Energy level transition, can realize 1.6 μm laser output capable of being safely absorbed by human eye, and does not generatePump light darkening effect. Er prepared by the invention Y2O3The transparent ceramic can be used as an ideal laser gain medium in the fields of laser radar, laser ranging, atmospheric detection and the like.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for preparing a transparent ceramic, comprising:
step A, adding Y2O3And an Er-containing dopant of the formula (Er)xY1-x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0005 and less than or equal to 0.005, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Er, Y2O3Powder;
step B, adding Er to Y2O3Molding the powder to obtain a blank;
step C, sintering the biscuit in a vacuum environment at the temperature of 1400-1800 ℃ for 0.5-50h, then sintering the biscuit in an inert gas at the temperature of 1400-1800 ℃ for 0.5-8h in a hot isostatic manner, finally annealing the biscuit in an air or oxygen atmosphere at the temperature of 600-1300 ℃ for 0.5-30h, and polishing the two surfaces to obtain Er, Y2O3A transparent ceramic.
2. The method for preparing a transparent ceramic according to claim 1, wherein the step a comprises:
weighing the high-purity Y2O3And Er-containing doping agent are placed in a ball mill, and absolute ethyl alcohol is added to obtain slurry with the powder content of 10-30 Vol%;
adding grinding balls into the slurry, and finishing ball milling treatment on the slurry through a ball mill;
placing the slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding the dried material, and screening to obtain a screened material with a particle diameter of less than 104 μm;
placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Er: Y2O3And (3) powder.
3. The method as claimed in claim 2, wherein the rotation speed of the ball milling process is 100-250rpm, and the ball milling time is 3-48 h;
and/or the mass ratio of the grinding balls to the mixed powder is 3:1-8: 1;
and/or the calcination temperature is 400-1100 ℃, and the calcination time is 3-10 h.
4. The method of claim 1, wherein the Er-containing dopant is Er2O3、ErCl3、Er(NO3)3、Er2(SO4)3One kind of (1).
5. The method according to claim 1, wherein the step B comprises: adding Er to Y2O3Dry pressing the powder to obtain dry pressed Er: Y2O3And carrying out cold isostatic pressing on the powder to obtain a biscuit.
6. The method for preparing a transparent ceramic according to claim 5, wherein the pressure of the dry press molding is 0.5 to 20 MPa;
and/or the pressure of the cold isostatic pressing is 100-200 MPa.
7. The method of claim 1, wherein the hot isostatic pressing sintering is performed at a pressure of 50-200MPa, and the inert gas used for the hot isostatic pressing sintering comprises argon and nitrogen.
8. A transparent ceramic according to claim 1The preparation method is characterized in that the vacuum degree of the vacuum environment is less than or equal to 10-3Pa。
9. A transparent ceramic produced by the production method according to any one of claims 1 to 8.
10. Use of the transparent ceramic of claim 9 in a fixed lasing medium for a laser;
further, the fixed laser gain medium is used for a 1.6 μm eye-safe laser.
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| CN114685166A (en) * | 2022-05-05 | 2022-07-01 | 闽都创新实验室 | Scintillation ceramic and preparation method and application thereof |
| CN115353389A (en) * | 2022-09-26 | 2022-11-18 | 江苏师范大学 | Ho ion doped sesquioxide transparent ceramic and preparation method thereof |
| CN116332647A (en) * | 2023-02-14 | 2023-06-27 | 沪硅精密陶瓷科技(苏州)有限公司 | Plasma resistant rare earth oxide solid solution ceramics and method for manufacturing same |
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| CN115353389B (en) * | 2022-09-26 | 2023-09-05 | 江苏师范大学 | Ho ion doped sesquioxide transparent ceramic and preparation method thereof |
| CN116332647A (en) * | 2023-02-14 | 2023-06-27 | 沪硅精密陶瓷科技(苏州)有限公司 | Plasma resistant rare earth oxide solid solution ceramics and method for manufacturing same |
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