CN113754436A - Preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic - Google Patents

Preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic Download PDF

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CN113754436A
CN113754436A CN202111187964.8A CN202111187964A CN113754436A CN 113754436 A CN113754436 A CN 113754436A CN 202111187964 A CN202111187964 A CN 202111187964A CN 113754436 A CN113754436 A CN 113754436A
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sesquioxide
laser
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王俊
李晴
马杰
张长华
周刊
卜祥晒
刘鹏
王莹
章健
唐定远
沈德元
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Jiangsu Normal University
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Abstract

The invention discloses a preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic, which is prepared by mixing Y2O3And a Cr-containing dopant of the formula (Cr)xY1‑x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y2O3Powder; mixing Cr with Y2O3Molding the powder to obtain a blank; sintering the green body in a vacuum environment of 1200-1600 ℃ for 0.5-50h, hot isostatic pressing in an inert gas of 1200-1600 ℃ for 0.5-8h, finally annealing in an atmosphere of 1100-1500 ℃ in air, oxygen or reducing atmosphere for 0.5-30h, and finely polishing the two surfaces to obtain Cr, Y2O3Is transparentThe ceramic material takes a proper amount of Cr as a doping agent, so that the sintering temperature of pure sesquioxide ceramic can be reduced, and simultaneously, the prepared ceramic material can be ensured to have nano-scale grain size and laser-level transparency, and has excellent mechanical properties and infrared transmittance.

Description

Preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic
Technical Field
The invention relates to a preparation method of a nanocrystalline laser-grade sesquioxide transparent ceramic, belonging to the technical field of sesquioxide transparent ceramics.
Background
Compared with common YAG materials, sesquioxide materials (such as Y)2O3、Sc2O3And Lu2O3) Has lower phonon energy, lower thermal expansion coefficient and higher thermal conductivity, and has great development potential in the field of high-power solid laser. However, the melting point of sesquioxide is as high as 2400 ℃ or higher, and the transformation point is lower than the melting point, so that the technique of growing a single crystal thereof is extremely complicated. Furthermore, the size of the single crystal is limited by the equipment required and the mechanical properties are low, making it difficult to meet different applications. By adopting the ceramic preparation process, the sesquioxide transparent ceramic can be sintered at a temperature far lower than the melting point of the material, and the large-size, large-scale and low-cost preparation can be realized more easily. Meanwhile, the sesquioxide ceramic also has the characteristics of wide light transmission range, high mechanical strength, high refractoriness and high dielectric constant, and can be used for manufacturing infrared windows, infrared fairings and high temperatureThe material such as the lens, the microwave substrate and the like has great application prospect in the civil and military fields.
For a high-power laser system, the good mechanical property can enable the material to bear more thermal stress, so that the damage of the material is avoided as much as possible, and the power scaling and amplification are facilitated; in addition to the basic requirement that the material has high infrared transmittance, the biggest challenge is to further improve the bending resistance. By means of the Hall-Petrc formula (sigma ∞ 1/d)1/2) It is known that the grain size d is inversely proportional to the strength σ of the ceramic, i.e., the smaller the grain size, the higher the strength of the ceramic. In addition, according to the report of h.yagi et al, since the crystal grains in the polycrystalline ceramic material are randomly oriented, a smaller crystal grain size may contribute to the elimination of internal stress of the ceramic.
Therefore, to improve the mechanical properties of the sesquioxide ceramic, it is critical that the ceramic has a small grain size while ensuring high optical quality. Dopants are typically added to the matrix material to lower the sintering temperature or to suppress grain boundary mobility, thereby reducing the grain size. In 2015, L.Zhang et al expressed ZrO2 and La2O3Y is prepared from Cr as sintering assistant by vacuum sintering2O3Transparent ceramics, which are found to be advantageous for reducing the grain size by incorporating a suitable amount of Cr, are considered as a potential laser material with good mechanical properties. However, the Cr prepared is Y2O3The grain size of the ceramic is large (with a doping concentration of 0-0.7 at.% Cr, the grain size corresponds to 8.3-4.3 μm), and no Cr-doped sesquioxide ceramic has been found to achieve densification at low temperatures. The crystal material doped with Cr or co-doped with other rare earth ions (such as Yb3+, Nd3+, and the like) is often used as a saturable absorber or a laser gain medium, and can improve the flash lamp pumping efficiency of the laser crystal material. Therefore, the further research on the Cr-doped sesquioxide transparent ceramic material has very important significance.
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 provides a preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic, so as to solve the problem that the Cr, Y and the like prepared in the prior art are Y2O3The grain size of the ceramic is large.
In order to solve the technical problems, the invention is realized by adopting the following technical scheme:
a preparation method of nanocrystalline laser-grade sesquioxide transparent ceramics comprises the following steps: step A, adding Y2O3And a Cr-containing dopant of the formula (Cr)xY1-x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y2O3Powder;
step B, mixing Cr and Y2O3Molding the powder to obtain a blank;
step C, sintering the blank in a vacuum environment at 1200-1600 ℃ for 0.5-50h, sintering the blank in an inert gas at 1200-1600 ℃ for 0.5-8h in a hot isostatic manner, finally annealing the blank in an atmosphere of air, oxygen or reducing at 1100-1500 ℃ for 0.5-30h, and finely polishing the two surfaces to obtain Cr, Y2O3A transparent ceramic.
As a preferred embodiment of the present invention, step a includes:
weighing Y2O3And a doping agent containing Cr is placed in a ball mill, and absolute ethyl alcohol is added to obtain mixed slurry;
adding grinding balls into the mixed slurry, and finishing ball milling treatment on the slurry through a ball mill;
placing the mixed slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding and screening the dried material to obtain a screened material;
placing the obtained sieved material in a muffle furnace for carrying outCalcining to obtain Cr, Y2O3And (3) powder.
As a preferable technical scheme of the invention, the Cr-containing dopant is Cr2O3、CrCl3、Cr(NO3)3、Cr2(SO4)3One kind of (1).
As a preferable technical scheme of the invention, the absolute ethyl alcohol and Y2O3The volume ratio of the mixed powder to the mixed powder containing the Cr doping agent is 1:2-5: 2;
and/or the rotating speed of the ball mill is 100-250rpm, and the ball milling time is 3-48 h;
and/or the drying temperature of the mixed slurry is 40-120 ℃, and the drying time is 12-48 h;
and/or the calcining temperature of the sieving material is 600-1200 ℃, and the calcining time is 3-10 h.
As a preferred embodiment of the present invention, the step B includes: mixing Cr with Y2O3Dry pressing the powder to form; to the Cr: Y after dry pressing2O3And 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 molding is 5-20 Mpa;
and/or the pressure of the cold isostatic pressing is 100-200 MPa.
As a preferable technical scheme of the invention, the vacuum degree of the vacuum environment is less than or equal to 10-3Pa。
In a preferred embodiment of the present invention, the pressure of the hot isostatic pressing sintering is 50 to 200 MPa.
In a preferred embodiment of the present invention, the inert gas used for hot isostatic pressing sintering is argon or/and nitrogen;
and/or the oxidizing atmosphere for annealing is oxygen, and the reducing atmosphere is hydrogen or/and argon.
A nanocrystalline laser-grade sesquioxide transparent ceramic is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a proper amount of Cr is used as a dopant, so that the sintering temperature of pure sesquioxide ceramic can be reduced, and simultaneously, the prepared ceramic material can be ensured to have nano-scale grain size and laser-level transparency, and has excellent mechanical properties and infrared transmittance.
Drawings
FIG. 1 shows Cr: Y provided in examples 1 to 4 of the present invention2O3XRD of transparent ceramics.
FIG. 2 shows Cr: Y provided in examples 1 to 2 of the present invention2O3SEM after transparent ceramic hot isostatic pressing sintering.
FIG. 3 shows Cr: Y provided in example 12 of the present invention2O3And (3) a statistical graph of the grain size of the transparent ceramic after hot isostatic pressing sintering.
FIG. 4 shows Cr: Y provided in example 1 of the present invention2O3Infrared spectroscopy of transparent ceramics.
FIG. 5 is a process flow diagram of the present invention.
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.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
As shown in figures 1 to 3, a method for preparing a nanocrystalline laser-grade sesquioxide transparent ceramic comprises the steps of A, mixing commercial high-purity Y2O3And a Cr-containing dopant as a raw material according to the chemical formula (Cr)xY1-x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y2O3Powder;
the step A comprises the following steps:
weighing Y2O3And a doping agent containing Cr is placed in a ball mill, and absolute ethyl alcohol is added to obtain mixed slurry; absolute ethanol with Y2O3The volume ratio of the mixed powder to the mixed powder containing the Cr doping agent is 1:2-5: 2;
the Cr-containing dopant is preferably Cr2O3、CrCl3、Cr(NO3)3、Cr2(SO4)3One of them, also other Cr-containing dopants, can be determined according to the actual requirements.
Adding grinding balls into the mixed slurry, and finishing ball milling treatment on the slurry through a ball mill; the rotation speed of the ball mill is 100 and 250rpm, and the ball milling time is 3-48 h; the diameter of the powder particles after ball milling is 50-200 nm.
Placing the mixed slurry subjected to ball milling treatment in an oven for drying to obtain a dried material; the drying temperature of the mixed slurry is 40-120 ℃, and the drying time is 12-48 h.
Grinding and screening the dried material to obtain a screened material; the screening precision is between 80 and 300 meshes.
Placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Cr, Y2O3Powder; the calcining temperature of the screened material is 600-1200 ℃, and the calcining time is 3-10 h.
Step B, mixing Cr and Y2O3Molding the powder to obtain a blank;
Cr:Y2O3the powder is molded and processed as follows: dry pressing to form and dry pressing to form Cr, Y2O3And carrying out cold isostatic pressing on the powder to obtain a biscuit.
The pressure of dry pressing is 5-20MPa, and the pressure of cold isostatic pressing is 100-200 MPa.
Step C, sintering the biscuit in a vacuum environment at 1200-1600 ℃ for 0.5-50h, wherein the vacuum degree of the vacuum environment is less than or equal to 10-3Pa;
Hot isostatic pressing sintering is carried out in an inert gas at 1200-1600 ℃ for 0.5-8h, the pressure of the hot isostatic pressing sintering is 50-200MPa, and the inert gas used for the hot isostatic pressing sintering is argon or/and nitrogen;
finally annealing for 0.5-30h in 1100-1500 ℃ air, oxygen or reducing atmosphere, wherein the oxidizing atmosphere for annealing is oxygen, and the reducing atmosphere is hydrogen or/and argon;
fine polishing on both sides to obtain Cr, Y2O3A transparent ceramic.
A nanocrystalline laser-grade sesquioxide transparent ceramic is prepared by the preparation method.
With Cr to Y2O3Ceramics are exemplified:
example one
(1) As commercial high purity Y2O3And Cr2O3Is used as raw material and has a chemical formula of 0.1 at.% Cr: Y2O3100g of Y are weighed2O3Powder and 0.067g Cr2O3Adding a proper amount of absolute ethyl alcohol into the powder, and putting the mixture into a ball mill with the rotating speed of 140rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5h to obtain Cr, Y2O3And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed at a pressure of 200 MPa.
(3) And (3) placing the blank body in a vacuum environment at 1260 ℃ for sintering for 7h, then performing hot isostatic pressing sintering in an argon atmosphere at 1240 ℃ for 3h, and finally performing oxygen annealing in a tube furnace at 1100 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y2O3A transparent ceramic.
Example two
(1) As commercial high purity Y2O3And Cr2O3Is used as raw material and has a chemical formula of 0.1 at.% Cr: Y2O3100g of Y are weighed2O3Powder and 0.067g Cr2O3Adding a proper amount of absolute ethyl alcohol into the powder, and putting the mixture into a ball mill with the rotating speed of 140rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5h to obtain Cr, Y2O3And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed at a pressure of 200 MPa.
(3) And (3) placing the blank body in a vacuum environment at 1260 ℃ for sintering for 7h, then performing hot isostatic pressing sintering in an argon atmosphere at 1240 ℃ for 3h, and finally performing hydrogen annealing in a tube furnace at 1100 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y2O3A transparent ceramic.
EXAMPLE III
(1) As commercial high purity Y2O3And Cr2O3Is used as raw material and has a chemical formula of 0.1 at.% Cr: Y2O3100g of Y are weighed2O3Powder and 0.067g Cr2O3Adding a proper amount of absolute ethyl alcohol into the powder, and putting the mixture into a ball mill with the rotating speed of 140rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5h to obtain Cr, Y2O3And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed at a pressure of 200 MPa.
(3) And (3) placing the blank body in a vacuum environment at 1330 ℃ for sintering for 7h, then performing hot isostatic pressing sintering in an argon atmosphere at 1300 ℃ for 3h, and finally performing oxygen annealing in a tube furnace at 1200 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y2O3A transparent ceramic.
Example four
(1) As commercial high purity Y2O3And Cr2O3Is used as raw material and has a chemical formula of 0.1 at.% Cr: Y2O3100g of Y are weighed2O3Powder and 0.067g Cr2O3Adding a proper amount of absolute ethyl alcohol into the powder, and putting the mixture into a ball mill with the rotating speed of 140rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5h to obtain Cr, Y2O3And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed at a pressure of 200 MPa.
(3) And (3) placing the blank body in a vacuum environment at 1330 ℃ for sintering for 7h, then performing hot isostatic pressing sintering in an argon atmosphere at 1300 ℃ for 3h, and finally performing hydrogen annealing in a tube furnace at 1200 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y2O3A transparent ceramic.
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 preparation method of nanocrystalline laser-grade sesquioxide transparent ceramics is characterized by comprising the following steps:
step A, adding Y2O3And a Cr-containing dopant of the formula (Cr)xY1-x)2O3Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y2O3Powder;
step B, mixing Cr and Y2O3Molding the powder to obtain a blank;
step C, sintering the blank in a vacuum environment at 1200-1600 ℃ for 0.5-50h, then sintering the blank in an inert gas at 1200-1600 ℃ for 0.5-8h in a hot isostatic manner, and finally annealing the blank in an atmosphere of 1100-1500 ℃ air, oxygen or reducing gasFire for 0.5-30h, and finely polishing two sides to obtain Cr, Y2O3A transparent ceramic.
2. The method of claim 1, wherein step a comprises:
weighing Y2O3And a doping agent containing Cr is placed in a ball mill, and absolute ethyl alcohol is added to obtain mixed slurry;
adding grinding balls into the mixed slurry, and finishing ball milling treatment on the slurry through a ball mill;
placing the mixed slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding and screening the dried material to obtain a screened material;
placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Cr, Y2O3And (3) powder.
3. The method of claim 2, wherein the Cr-containing dopant is Cr2O3、CrCl3、Cr(NO3)3、Cr2(SO4)3One kind of (1).
4. The method of claim 2, wherein the absolute ethyl alcohol and Y are selected from the group consisting of2O3The volume ratio of the mixed powder to the mixed powder containing the Cr doping agent is 1:2-5: 2;
and/or the rotating speed of the ball mill is 100-250rpm, and the ball milling time is 3-48 h;
and/or the drying temperature of the mixed slurry is 40-120 ℃, and the drying time is 12-48 h;
and/or the calcining temperature of the sieving material is 600-1200 ℃, and the calcining time is 3-10 h.
5. The method of claim 1, wherein step B comprises: mixing Cr with Y2O3Dry pressing the powder to form; to the Cr: Y after dry pressing2O3And carrying out cold isostatic pressing on the powder to obtain a biscuit.
6. The method for preparing the nanocrystalline laser-grade sesquioxide transparent ceramic according to claim 5, wherein the pressure of the dry pressing is 5-20 Mpa;
and/or the pressure of the cold isostatic pressing is 100-200 MPa.
7. The method for preparing a nanocrystal laser grade sesquioxide transparent ceramic according to claim 1, wherein the vacuum degree of the vacuum environment is less than or equal to 10-3Pa。
8. The method of claim 1, wherein the hot isostatic pressing sintering is performed at a pressure of 50-200 MPa.
9. The method of claim 1, wherein the inert gas used for hot isostatic pressing sintering is argon or/and nitrogen;
and/or the oxidizing atmosphere for annealing is oxygen, and the reducing atmosphere is hydrogen or/and argon.
10. A nanocrystalline laser grade sesquioxide transparent ceramic, characterized by being prepared by the preparation method of any one of claims 1 to 9.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115893991A (en) * 2022-10-21 2023-04-04 江苏师范大学 High-transparency Al 2 O 3 Method for producing polycrystalline ceramic

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