CN115745607A - Infrared transparent ceramic material and preparation method thereof - Google Patents
Infrared transparent ceramic material and preparation method thereof Download PDFInfo
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- CN115745607A CN115745607A CN202211430376.7A CN202211430376A CN115745607A CN 115745607 A CN115745607 A CN 115745607A CN 202211430376 A CN202211430376 A CN 202211430376A CN 115745607 A CN115745607 A CN 115745607A
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- 239000002114 nanocomposite Substances 0.000 claims abstract description 37
- 239000011858 nanopowder Substances 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 17
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 17
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- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 9
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- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
The invention provides an infrared transparent ceramic material and a preparation method thereof, belonging to the technical field of ceramic materials and having a chemical general formula of Gd 2 O 3 ‑MgO‑RO m Wherein R = Y, sc, ca, sr, la, lu, m =1 or 1.5; the infrared transparent ceramic material is prepared from cubic phase Gd 2 O 3 And a cubic phase MgO two-phase; using a composition containing Gd 2 O 3 Nano-powder of (3), nano-powder of MgO and RO m Nano-powder of (2)Sintering the composite powder; wherein, in the nano-composite powder, gd 2 O 3 The volume ratio of the nano-powder to the MgO nano-powder is 1:5-5 m The nano powder accounts for 0.01 to 10 percent of the total molar weight of the nano composite powder. The invention realizes the high transmittance Gd of the mid-infrared broadband 2 O 3 The average transmittance of the medium infrared 3-7 mu m is more than 80 percent in the preparation of the-MgO nano complex phase ceramic.
Description
Technology neighborhood
The invention relates to an infrared transparent ceramic material and a preparation method thereof.
Background
The infrared transparent material is a material capable of transmitting infrared radiation, and is mainly used for manufacturing a window of an infrared detector, a lens and a prism of an infrared instrument and the like. Infrared transparent window materials or fairings for aircraft are required to protect the optical system from the effects of atmospheric air, moisture, dust, as well as to participate in system imaging and phase contrast correction, which requires infrared transparent materialsHas high transmittance, mechanical strength, hardness and thermal shock resistance. Gd (Gd) 2 O 3 Physicochemical properties of (C) and Y 2 O 3 Similarly, the high-temperature infrared window material belongs to heavy rare earth sesquioxide, has lower phonon energy, has longer cutoff wavelength than common optical materials (sapphire, alON, spinel and the like), has the advantages of low high-temperature infrared radiation coefficient, excellent high-temperature mechanical property and the like, and is a promising infrared window material.
The mutual solid solubility of the gadolinium oxide and the magnesium oxide is low, the growth of crystal grains in the sintering process can be effectively inhibited through the pinning effect, the size of the crystal grains is reduced, and the mechanical property of the polycrystalline ceramic is improved without influencing the transmittance of the polycrystalline ceramic.
In the process of preparing gadolinium oxide ceramic, monoclinic phase Gd is obtained by sintering 2 O 3 The ceramic, eranezhuth Wasan Awin of Indian science, utilizes the discharge plasma sintering (SPS) technology to sinter cubic phase Gd2O3 powder into monoclinic phase Gd2O3 ceramic sample, the visible waveband transmittance of the sample obtained at the sintering temperature of 1600 ℃ is 30%, and the hardness reaches 7.95GPa. Wu Na, li Xiaodong, etc. [ preparation of Gd ] at the university of northeast 2 O 3 -MgO nanocomposite optical ceramics with varied crystallographic modifications of Gd 2 O 3 constituent.Journal of the American Ceramic Society 101,4887(2018)]Research on the hot-pressing sintering temperature versus Gd 2 O 3 Gd in-MgO complex phase ceramic 2 O 3 The effect of the phase change. IR-transmissive MgO-Gd et al [ IR-transmissive MgO-Gd ] of the national university of Kupffer Broode 2 O 3 composite ceramic produced by self-propagating high-temperature synthesis and spark plasma sintering.Journal of Advanced Ceramics 10,237(2021)]Preparing powder by self-combustion method, and preparing Gd by spark plasma sintering process 2 O 3 MgO nano complex phase ceramics, which researches the influence of annealing treatment on the transmittance and hardness of samples. Both studies suggest Gd 2 O 3 the-MgO complex phase ceramic has excellent infrared transmission performance and mechanical property, and is one of candidate materials of a red light optical window in the future. But prepared in the above-mentioned several studiesGd in the ceramic of (2) 2 O 3 The phases are monoclinic phase, the powder before sintering is cubic phase, and because the monoclinic phase has higher density, phase change occurs in the sintering process, gd 2 O 3 The volume of (A) is reduced by about 10%, and monoclinic phase Gd 2 O 3 Is optically anisotropic and reduces the infrared transmittance of the material. The sintering methods in the two studies are also not suitable for preparing and generating large-size samples, and the air pre-sintering and HIP sintering post-treatment methods in the patent are suitable for preparing large-size and irregularly-shaped samples. But generally Gd 2 O 3 The sintering and compacting temperature is 1400-1600 ℃ under the pressureless condition, and exceeds Gd 2 O 3 The phase transition temperature from the cubic phase to the monoclinic phase (about 1250 ℃).
The document CN 109369183A proposes a Y 2 O 3 -MgO complex phase ceramic as substrate material and doped with Gd 2 O 3 The obtained ceramic material has the transmittance of about 81 percent at 2-6.5 mu m and the hardness of about 11.1GPa, and Gd is used as the Gd for the preparation method of the novel infrared transparent material 2 O 3 -MgO complex phase ceramic as substrate doped with Y 2 O 3 、Sc 2 O 3 、CaO、SrO、Lu 2 O 3 Equal rare earth oxide, effectively increases Gd 2 O 3 Stable cubic Gd phase may be obtained at the phase transition temperature from cubic to monoclinic phase 2 O 3 The MgO complex phase ceramic has higher mid-infrared transmittance and mechanical property.
Disclosure of Invention
The invention aims to provide an infrared transparent ceramic material and a preparation method thereof, which firstly adopts the method of air pre-sintering and Hot Isostatic Pressing (HIP) sintering to prepare cubic phase Gd 2 O 3 -MgO complex phase ceramic, infrared transparent Gd obtained by the process of the invention 2 O 3 -MgO-RO m The nano multiphase ceramic has a cubic phase, the density is close to a theoretical value, the crystal grains are small and uniform, the transmittance of 3-6 mu m of middle infrared is more than 81%, and the Vickers hardness exceeds 10GPa. The invention adopts the sol-gel method to prepare the nano multiphase powder, has low raw material cost and high efficiencySimple process and is convenient for large-scale industrial production.
The technical scheme of the invention is realized as follows:
the invention provides an infrared transparent ceramic material with a chemical general formula of Gd 2 O 3 -MgO-RO m Wherein R = Y, sc, ca, sr, la, lu, m =1 or 1.5;
the infrared transparent ceramic material is prepared from cubic phase Gd 2 O 3 And a cubic phase MgO two-phase;
the infrared transparent ceramic material is prepared by adopting a material containing Gd 2 O 3 Nano-powder of (3), nano-powder of MgO and RO m The nano composite powder is formed by sintering the nano composite powder;
wherein, in the nano-composite powder, gd 2 O 3 The volume ratio of the nano-powder to the MgO nano-powder is 1:5-5 m The nano powder accounts for 0.01 to 10 percent of the total molar weight of the nano composite powder.
As a further improvement of the invention, the infrared transmittance of the infrared transparent ceramic material is 70-83%.
The invention further provides a preparation method of the infrared transparent ceramic material, which comprises the following steps:
(1) Preparing nano composite powder by using gadolinium oxide, magnesium salt, R salt, concentrated nitric acid and an organic additive as raw materials by a sol-gel method; r = Y, sc, ca, sr, la, lu;
(2) Carrying out dry pressing molding treatment on the nano composite powder obtained in the step (1) to obtain a molded biscuit;
(3) Air presintering and hot isostatic pressing sintering are carried out on the formed biscuit, and a nano complex phase sintered body is obtained;
(4) And annealing and machining the nano complex phase sintered body to obtain the infrared complex phase ceramic.
As a further improvement of the invention, the specific steps of the step (1) are as follows:
a) Preparing a solution containing gadolinium salt, magnesium salt, R salt, concentrated nitric acid and an organic additive;
b) Putting the solution prepared in the step a) into an oven, heating to 100-250 ℃, and preserving heat for 0.5-6h to obtain xerogel;
c) Putting the xerogel prepared in the step b) into a muffle furnace, heating to 600-1000 ℃, preserving heat for 1-8h, and then naturally cooling to obtain the nano composite powder.
As a further improvement of the invention, the gadolinium salt is at least one of gadolinium nitrate, gadolinium acetate, gadolinium sulfate and gadolinium chloride, the magnesium salt is at least one of magnesium nitrate, magnesium acetate, magnesium sulfate and magnesium chloride, and the R salt is R (NO) 3 ) 2m 、R(Ac) 2m 、R(SO 4 ) 2m 、RCl 2m M =1 or 1.5, the organic additive is at least one of citric acid, glycol, glucose, glycine and urea, and the concentration of the concentrated nitric acid is 50-70%.
As a further improvement of the invention, in the step b), the oven is preheated first and then the initial solution is put into the oven, wherein the preheating temperature is 50-200 ℃; in step c), heating at a heating rate of 1-5 ℃/min; the heating is staged heating comprising: keeping the temperature for 0-4h at 150-250 ℃, keeping the temperature for 0-12h when heating to 400-500 ℃, and keeping the temperature for 0.5-8h when heating to 600-1000 ℃.
As a further improvement of the invention, the nano composite powder prepared in the step (1) is subjected to ball milling, drying and sieving to form spherical particle powder with the particle size of 50-1000nm, and then sintering is carried out.
As a further improvement of the invention, the ball milling medium is at least one of absolute ethyl alcohol, acetone, glycerol and isopropanol, the ball milling speed is 50-300r/min, and the ball milling time is 1-48h; the drying is carried out in an oven at 50-90 ℃ for 0.5-24h; and the sieving is to sieve a 25-200 mesh sieve and granulate.
As a further improvement of the invention, the process parameters of the air pre-burning in the step (3) are as follows: the heating rate is 1-20 ℃/min, the heat preservation temperature is 800-1400 ℃, and the heat preservation time is 0.5-3h; the sintering process parameters of the hot isostatic pressing are as follows: the heating rate is 2-200 ℃/min, the heat preservation temperature is 800-1400 ℃, the heat preservation time is 0.5-5h, and the pressure maintaining pressure is 50-300MPa.
As a further improvement of the invention, the annealing temperature in the step (4) is 900-1400 ℃, and the holding time is 0.5-24h.
The preparation method of the infrared transparent ceramic material comprises the following specific steps:
the first stage is as follows: sol-gel process for preparing composite nano powder
Step 1.1) gadolinium oxide is dissolved in nitric acid solution, and mixed with magnesium nitrate hexahydrate and R (NO) 3 ) 2m Mixing the solution prepared by dissolving in deionized water, and fully mixing on a magnetic stirrer;
step 1.2) dissolving an organic additive in deionized water to prepare a solution, wherein the organic additive is citric acid, ethylene glycol, glucose, fructose, glycine, urea, propylene glycol and the like;
step 1.3) mixing the solutions obtained in step 1.1) and step 1.2), magnetically stirring and heating to obtain viscous gel;
step 1.4) putting the gel obtained in the step 1.3) into an oven for heating, wherein the temperature of the oven is 150-250 ℃, and the heating time is 0.5-6h, so as to obtain a yellow brown xerogel;
step 1.5) putting the xerogel obtained in the step 1.4) into an oxygen furnace for high-temperature calcination at the temperature of 600-900 ℃ for 0.5-6h to obtain Gd 2 O 3 -MgO-RO m Compounding nanometer powder;
step 1.6) Gd described in step 1.5) 2 O 3 -MgO-RO m After ball milling and sieving treatment, the composite nano powder is calcined for 1-6h at 500-800 ℃ to obtain the high-activity composite nano powder.
And a second stage: preparation of complex phase ceramics
Step 2.1) pressing the high-activity composite nano powder in the step 1.6) into a biscuit by using a mold;
and 2.2) pre-burning the biscuit in the step 2.1) in a muffle furnace in the air atmosphere, wherein the sintering temperature is 1300-1500 ℃, the heating rate is 1-50 ℃/min, the heat is preserved for 0.5-12h, and the compact ceramic blank is obtained after natural cooling.
Step 2.3) carrying out hot isostatic pressing sintering (HIP) on the ceramic blank in the step 2.2) by adopting a hot isostatic pressing sintering furnace, wherein the sintering temperature is 1250-1450 ℃, the heat preservation time is 0.5-4h, and the pressurizing pressure of argon atmosphere is 50-300MPa to obtain a compact ceramic sample;
step 2.4) annealing the ceramic sample obtained in the step 2.3) in a muffle furnace at the temperature of 800-1200 ℃ for 5-30h;
and 2.5) carrying out double-sided mirror polishing on the annealing treatment sample obtained in the step 2.4) to obtain an infrared transparent complex-phase ceramic product.
In step 1.1), gadolinium oxide, magnesium nitrate hexahydrate and R (NO) 3 ) 2m The purity of (A) is not less than 99%.
In step 1.3), the heating temperature of the magnetic stirrer is 50 to 300 ℃.
The ball milling and sieving in the step 1.6) are carried out, specifically, a zirconia ball milling tank and a ball mill are adopted, the diameter of the ball mill is 1-5mm, the mass ratio of powder to the ball mill is 1:2-1, absolute ethyl alcohol is selected as a ball milling medium, the ratio of the powder to the absolute ethyl alcohol is 1:1-1:5, the ball milling time is 12-60h, the ball mill is dried in an oven at 60-100 ℃ for 5-20h, and the ball mill is sieved by a 100-350 mesh sieve.
The die in the step 2.1) is a stainless steel die with the diameter phi of 10mm, the diameter phi of 20mm, the diameter phi of 40mm, the diameter phi of 80mm or the diameter phi of 100 mm.
The density of the ceramic body in the step 2.2) is more than 95 percent and less than 99 percent.
The density of the ceramic sample in the step 2.3) is more than 99% and less than 100%.
The invention selects a sol-gel method to prepare Gd 2 O 3 the-MgO nano multiphase powder selects organic matters which have good complexing performance with metal ions, are easy to form a space network structure and have high heat release during combustion reaction as additives, thus ensuring that Gd in the powder 2 O 3 And the uniformity of the two-phase distribution of MgO ensures that the powder has better crystallinity, avoids the growth and agglomeration of crystal grains caused by further calcination, and realizes the densification of the complex phase ceramic by adopting hot isostatic pressing sintering after effectively controlling the size of the crystal grains to be in submicron or nanometer scale.
The invention has the following beneficial effects: the invention is toRO m Solid solution into Gd 2 O 3 Can raise phase-change temp. and inhibit its phase-change process to obtain cubic phase Gd 2 O 3 -MgO complex phase ceramics. The cubic phase Gd is prepared by adopting the method of air pre-sintering and Hot Isostatic Pressing (HIP) sintering 2 O 3 -MgO-RO m Complex phase ceramic, infrared transparent Gd obtained by the method of the invention 2 O 3 -MgO-RO m The nano complex phase ceramic has a cubic phase, the density of the nano complex phase ceramic is close to a theoretical value, the crystal grains are small and uniform, the nano complex phase ceramic has excellent optical performance in a middle infrared band, and the Vickers hardness exceeds 10GPa. The invention adopts the sol-gel method to prepare the nano complex phase powder, has low raw material cost and simple process, and is convenient for large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a transmission electron micrograph of the nanocomposite powder prepared in example 1;
FIG. 2 is an XRD pattern of the nanocomposite powder prepared in example 1;
FIG. 3 is an XRD pattern of the infrared nanocomposite ceramic prepared in example 1;
FIG. 4 is an infrared transmittance of the infrared nano-composite ceramic prepared in example 1;
FIG. 5 is a scanning electron microscope image of the infrared nano-composite ceramic prepared in example 1;
FIG. 6 is a graph of Vickers hardness of infrared transparent ceramic materials prepared in examples 1-4.
FIG. 7 is an XRD pattern of the nanocomposite powder prepared in example 5;
FIG. 8 is an XRD pattern of the infrared nanocomposite ceramic prepared in example 5;
FIG. 9 is an infrared transmittance of the infrared nano-composite ceramic prepared in example 5;
FIG. 10 is a scanning electron micrograph of the infrared nanocomposite ceramic prepared according to example 5;
detailed description of the preferred embodiment
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
EXAMPLES 1, 2, 3, 4 raw material content tables
Example 1
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with a quantity of Mg (NO) 3 ) 2 Solution and Y (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Y (NO) 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Y (NO) 3 ) 3 Respectively adding citric acid monohydrate and ethylene glycol into the nitrate mixed solution by 10 percent of the total amount, stirring and heating the mixture on magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5 hours after the solution becomes thick, putting the prepared dried gel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at the speed of 1 ℃/min, preserving the heat for 4 hours, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring into a mould, and dry-pressing to form the powder with the thickness of 40mmA square piece of 60mm is multiplied, and then cold isostatic pressing treatment of 210MPa is carried out to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace in the air atmosphere, keeping the temperature for 2h at 1350 ℃, cooling to obtain a pre-sintered complex-phase ceramic body, placing the pre-sintered body in a hot isostatic pressing furnace in the argon atmosphere, pressurizing to 200MPa, keeping the temperature for 1.5h at 1350 ℃, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic. FIG. 1 is Gd prepared in example 1 2 O 3 SEM image of-MgO nanopowder, FIG. 2 is Gd prepared in example 1 2 O 3 XRD pattern of-MgO nano powder, FIG. 3 is Gd prepared in example 1 2 O 3 XRD pattern of the MgO nano complex phase ceramic, it can be seen that the prepared ceramic sample is cubic gadolinium oxide and cubic magnesium oxide phase, and no other complex phase exists. FIG. 4 is Gd prepared in example 1 2 O 3 -infrared transmittance of the MgO nano-composite ceramic, the transmittance within the range of 3-6 μm being over 80%; FIG. 5 is Gd prepared in example 1 2 O 3 The scanning electron microscope image of the MgO nano complex phase ceramic shows that the grain size distribution in the complex phase ceramic is uniform, and the grain size is about 190 nm.
Example 2
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with a quantity of Mg (NO) 3 ) 2 Solution and Y (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Y (NO 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Y (NO) 3 ) 3 Respectively adding citric acid monohydrate and ethylene glycol into the nitrate mixed solution with the total amount of 15 percent, stirring and heating the mixture on magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5 hours after the solution becomes thick, putting the prepared dried gel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at the speed of 1 ℃/min, preserving the heat for 4 hours, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Using absolute ethyl alcohol asBall milling the ball milling medium, putting the ball milling medium into an oven for drying after ball milling for 48 hours, sieving the ball milling medium by using a 200-mesh sieve, putting the obtained powder into a muffle furnace, heating the powder at 600 ℃ for 5 hours to obtain the high-activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small round pieces by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace at 1350 ℃ for 2h under the air atmosphere, cooling to obtain a pre-sintered complex phase ceramic biscuit, placing the pre-sintered biscuit in a hot isostatic pressing furnace at argon atmosphere, pressurizing to 200MPa, keeping the temperature at 1350 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 3
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with a quantity of Mg (NO) 3 ) 2 Solution and Y (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Y (NO 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Y (NO) 3 ) 3 Respectively adding citric acid monohydrate and ethylene glycol into the nitrate mixed solution with the total amount of 20 percent, stirring and heating the mixture on magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5 hours after the solution becomes thick, putting the prepared dried gel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at the speed of 1 ℃/min, preserving the heat for 4 hours, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Will be provided withPlacing the ceramic biscuit in a muffle furnace at 1350 ℃ for 2h under the air atmosphere, cooling to obtain a pre-sintered complex phase ceramic biscuit, placing the pre-sintered biscuit in a hot isostatic pressing furnace at argon atmosphere, pressurizing to 200MPa, keeping the temperature at 1350 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 4
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with a quantity of Mg (NO) 3 ) 2 Solution and Y (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Y (NO 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Y (NO) 3 ) 3 30 percent of the total amount of the Gd nitrate mixed solution is respectively added with citric acid monohydrate and ethylene glycol, the mixture is stirred and heated on magnetic stirring, the solution is put into a 200 ℃ oven for heat preservation for 5h after becoming thick, the prepared dried gel is put into a 200 ℃ muffle furnace, oxygen is introduced, the temperature is raised to 800 ℃ at 1 ℃/min, the temperature is preserved for 4h, and then the temperature is naturally reduced to obtain the Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into 40mm × 60mm square pieces, and then carrying out cold isostatic pressing treatment at 210MPa to obtain ceramic biscuit. Placing the ceramic biscuit in a muffle furnace at 1350 ℃ for 2h under the air atmosphere, cooling to obtain a pre-sintered complex phase ceramic biscuit, placing the pre-sintered biscuit in a hot isostatic pressing furnace at argon atmosphere, pressurizing to 200MPa, keeping the temperature at 1350 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano multiphase ceramicAnd (4) porcelain.
FIG. 6 is a graph of the Vickers hardness of the infrared transparent ceramic materials prepared in examples 1-5, with the hardness averaging 10.0GPa.
Example 5
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with a quantity of Mg (NO) 3 ) 2 Solution and Sc (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Sc (NO 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Sc (NO) 3 ) 3 Adding glycine accounting for 10 percent of the total amount into the nitrate mixed solution, stirring and heating the mixed solution by magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5 hours after the solution becomes thick, putting the prepared xerogel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at the temperature of 1 ℃/min, preserving the heat for 4 hours, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace under the air atmosphere for heat preservation at 1350 ℃ for 2h, cooling to obtain a pre-sintered complex phase ceramic biscuit, placing the pre-sintered biscuit in a hot isostatic pressing furnace under the argon atmosphere for pressurizing to 200MPa, preserving heat at 1250 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 6
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with a quantity of Mg (NO) 3 ) 2 Solution and Lu (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Lu (NO) 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Lu (NO) 3 ) 3 Adding glycine 10% of the total amount into the nitrate mixed solution, stirring and heating the mixed solution by magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5h after the solution becomes thick, putting the prepared xerogel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at 1 ℃/min, preserving the heat for 4h, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small round pieces by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace under the air atmosphere for heat preservation at 1350 ℃ for 2h, cooling to obtain a pre-sintered complex phase ceramic biscuit, placing the pre-sintered biscuit in a hot isostatic pressing furnace under the argon atmosphere for pressurizing to 200MPa, preserving heat at 1250 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 7
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with an amount of Mg (NO) 3 ) 2 Solution and Lu (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Lu (NO) 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Lu (NO) 3 ) 3 Adding glycine 20% of the total amount into the nitrate mixed solution, stirring and heating on magnetic stirring, placing the solution into a 200 ℃ oven for heat preservation for 5h after the solution becomes thick, and placing the obtained productPutting the dried gel into a muffle furnace preheated to 200 ℃, introducing oxygen, heating to 800 ℃ at the speed of 1 ℃/min, preserving the temperature for 4h, and then naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace in an air atmosphere, keeping the sintering temperature at 1300-1350 ℃ for 2h, cooling to obtain a pre-sintered complex phase ceramic blank, placing the pre-sintered blank in a hot isostatic pressing furnace in an argon atmosphere, pressurizing to 200MPa in the argon atmosphere, keeping the temperature at 1250 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 8
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with an amount of Mg (NO) 3 ) 2 Solution and La (NO) 3 ) 3 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,La (NO 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And La (NO) 3 ) 3 Adding glycine 10% of the total amount into the nitrate mixed solution, stirring and heating the mixed solution by magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5h after the solution becomes thick, putting the prepared xerogel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at 1 ℃/min, preserving the heat for 4h, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace in the air atmosphere at 1300-1400 ℃ for 2h, cooling to obtain a pre-sintered complex phase ceramic biscuit, placing the pre-sintered biscuit in a hot isostatic pressing furnace in the argon atmosphere to be pressurized to 200MPa, keeping the temperature at 1250 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 9
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with an amount of Mg (NO) 3 ) 2 Solution and Ca (NO) 3 ) 2 Mixing the solutions to ensure the final Gd 2 O 3 And MgO in a volume ratio of 1,Lu (NO) 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Ca (NO) 3 ) 2 Adding glycine 10% of the total amount into the nitrate mixed solution, stirring and heating the mixed solution by magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5h after the solution becomes thick, putting the prepared xerogel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at 1 ℃/min, preserving the heat for 4h, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small round pieces by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace in air atmosphere, keeping the sintering temperature at 1300-1400 ℃, preserving the heat for 2h, cooling to obtain a pre-sintered complex-phase ceramic blank, placing the pre-sintered complex-phase ceramic blank in a hot isostatic pressing furnacePressurizing to 200MPa in argon atmosphere, preserving heat for 1.5h at 1250 ℃, cooling to obtain a ceramic sample, annealing the sample for 20h at 1000 ℃, and finally performing double-sided high-precision mirror polishing to obtain infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
Example 10
Weighing a certain amount of Gd 2 O 3 Dissolving in nitric acid solution until just dissolving to prepare Gd (NO) 3 ) 3 Solution with an amount of Mg (NO) 3 ) 2 Solution and Sr (NO) 3 ) 2 Mixing the solutions to ensure the final Gd 2 O 3 And MgO at a volume ratio of 1,Lu (NO) 3 ) 3 Molar amount of Gd (NO) 3 ) 3 And Sr (NO) 3 ) 2 Adding glycine accounting for 10 percent of the total amount into the nitrate mixed solution, stirring and heating the mixed solution by magnetic stirring, putting the solution into a 200 ℃ oven for heat preservation for 5 hours after the solution becomes thick, putting the prepared xerogel into a 200 ℃ muffle furnace, introducing oxygen, heating to 800 ℃ at the temperature of 1 ℃/min, preserving the heat for 4 hours, and naturally cooling to obtain Gd 2 O 3 -MgO nano complex phase powder. Ball milling with anhydrous ethanol as ball milling medium for 48 hr, drying in oven, sieving with 200 mesh sieve, heating at 600 deg.C in muffle furnace for 5 hr to obtain high activity Gd 2 O 3 -MgO composite nanopowder. Weighing 3g of powder, pouring the powder into a mould, and dry-pressing the powder into small wafers by using an oil press; weighing 20g of powder, pouring the powder into a mould, dry-pressing the powder into a square sheet with the thickness of 40mm multiplied by 60mm, and then carrying out cold isostatic pressing treatment at 210MPa to obtain a ceramic biscuit. Placing the ceramic biscuit in a muffle furnace in an air atmosphere, keeping the sintering temperature at 1300-1400 ℃, keeping the temperature for 2h, cooling to obtain a pre-sintered complex phase ceramic blank, placing the pre-sintered blank in a hot isostatic pressing furnace in an argon atmosphere, pressurizing to 200MPa in the argon atmosphere, keeping the temperature at 1250 ℃ for 1.5h, cooling to obtain a ceramic sample, annealing the sample at 1000 ℃ for 20h, and finally performing double-sided high-precision mirror polishing to obtain the infrared transparent Gd 2 O 3 -MgO nano-composite ceramic.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (9)
1. The infrared transparent ceramic material is characterized in that the chemical general formula of the infrared transparent ceramic material is Gd 2 O 3 -MgO-RO m Wherein R = Y, sc, ca, sr, la, lu, m =1 or 1.5;
the infrared transparent ceramic material is prepared from cubic phase Gd 2 O 3 And a cubic phase MgO two-phase;
the infrared transparent ceramic material is prepared by adopting a material containing Gd 2 O 3 Nano-powder of (3), nano-powder of MgO and RO m The nano composite powder is formed by sintering the nano composite powder;
wherein, in the nano-composite powder, gd 2 O 3 The volume ratio of the nano-powder to the MgO nano-powder is 1:5-5 m The nano powder accounts for 0.01 to 10 percent of the total molar weight of the nano composite powder.
2. A method for preparing the infrared complex phase ceramic according to claim 1, characterized in that the method comprises the following steps:
(1) Preparing nano composite powder by using gadolinium oxide, magnesium salt, R salt, concentrated nitric acid and an organic additive as raw materials by adopting a sol-gel method;
(2) Carrying out dry pressing molding treatment on the nano composite powder obtained in the step (1) to obtain a molded biscuit;
(3) Air presintering and hot isostatic pressing sintering are carried out on the formed biscuit, and a nano complex phase sintered body is obtained;
(4) And annealing the nano complex phase sintered body to obtain the infrared complex phase ceramic.
3. The preparation method according to claim 2, wherein the specific steps of step (1) are as follows:
a) Preparing a solution containing gadolinium salt, magnesium salt, R salt, concentrated nitric acid and an organic additive;
b) Putting the solution prepared in the step a) into an oven, heating to 100-250 ℃, and preserving heat for 0.5-6h to obtain xerogel;
c) Putting the xerogel prepared in the step b) into a muffle furnace, heating to 600-1000 ℃, preserving heat for 1-8h, and then naturally cooling to obtain the nano composite powder.
4. The method according to claim 2 or 3, wherein the gadolinium salt is at least one of gadolinium nitrate, gadolinium acetate, gadolinium sulfate and gadolinium chloride, the magnesium salt is at least one of magnesium nitrate, magnesium acetate, magnesium sulfate and magnesium chloride, and the R salt is R (NO) 3 ) 2m 、R(Ac) 2m 、R(SO 4 ) 2m 、RCl 2m M =1 or 1.5, the organic additive is at least one of citric acid, glycol, glucose, glycine and urea, and the concentration of the concentrated nitric acid is 50-70%.
5. A method as claimed in claim 3, characterized in that, in step b), the oven is preheated and then the starting solution is placed, the preheating temperature being 50-200 ℃; in step c), heating is carried out at a ramp rate of 1-5 ℃/minute, comprising: keeping the temperature for 0-4 hours at 150-250 ℃, keeping the temperature for 0-12 hours when the temperature is raised to 400-500 ℃, and then keeping the temperature for 0.5-8 hours when the temperature is raised to 600-1000 ℃.
6. The preparation method according to claim 2, wherein the composite powder prepared in step (1) is subjected to ball milling, drying, sieving to form spherical particle powder with a particle size of 50-1000nm, and then sintering.
7. The preparation method of claim 6, wherein the ball milling medium is at least one of absolute ethyl alcohol, acetone, glycerol and isopropanol, the ball milling speed is 50-300r/min, and the ball milling time is 1-48h; the drying is carried out in an oven at 50-90 ℃ for 0.5-24h; and the sieving is to sieve a 25-200 mesh sieve and granulate.
8. The method for preparing a ceramic tile according to claim 2, wherein the process parameters of the air pre-burning in the step (3) are as follows: the heating rate is 1-20 ℃/min, the heat preservation temperature is 800-1400 ℃, and the heat preservation time is 0.5-3h; the sintering process parameters of the hot isostatic pressing are as follows: the heating rate is 2-200 ℃/min, the heat preservation temperature is 800-1400 ℃, the heat preservation time is 0.5-5h, and the pressure maintaining pressure is 50-300MPa.
9. The method according to claim 2, wherein the annealing temperature in the step (4) is 900 to 1400 ℃, and the holding time is 0.5 to 24 hours.
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| CN116283289B (en) * | 2023-02-28 | 2024-02-02 | 四川大学 | High-transparency Gd 2 O 3 Preparation method of transparent ceramic material |
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