CN112159228B - Preparation of Y by filling nano powder 2 O 3 Method for producing-MgO composite powder - Google Patents
Preparation of Y by filling nano powder 2 O 3 Method for producing-MgO composite powder Download PDFInfo
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Abstract
Preparation of Y by filling nano powder 2 O 3 Method for producing-MgO composite powder, Y 2 O 3 Pouring the nano powder into a ball milling tank, adding high-purity magnesium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank, and pouring the salt solution into a Y 2 O 3 Mixing the nano powder; or pouring MgO nano powder into a ball milling tank, adding high-purity yttrium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank for mixing with the MgO nano powder, carrying out ball milling, and heating and calcining the mixture of the nano powder and the salt solution to completely decompose the nitrate to form decomposed nano magnesium oxide to Y 2 O 3 Nano-filling and coating; or forming decomposed nanometer yttrium oxide to nanometer fill and coat MgO to obtain nanometer powder filled and coated Y with crystal grain size less than 150nm 2 O 3 -MgO composite powder.
Description
Technical Field
The invention belongs to the field of synthesis of nano powder, and particularly relates to a method for preparing Y by filling nano powder 2 O 3 -MgO composite powder.
Background
The infrared window/spherical cover has good mechanical, thermal, optical and other properties, plays an important role in protecting precise photoelectric components in the infrared photoelectric system and transmitting target infrared signals for the detector/sensor, and the like, and is a prerequisite condition for ensuring the infrared guidance precision. With the continuous development of supersonic aircrafts from supersonic speeds to hypersonic speeds, the infrared window/dome cover faces more and more new challenges, and provides higher and higher performance requirements for the broadband transmittance, the mechanical strength, the thermal shock resistance and the infrared low-radiation characteristic of an infrared optical material.
By self-made Y 2 O 3 Preparing Y from-MgO composite nano powder 2 O 3 And the MgO two-phase volume ratio is close to 1, the two phases of the fine-grain high-density nano multiphase ceramic are uniformly distributed, the mid-infrared transmittance can reach 83 percent, the theoretical transmittance is close, the bending strength exceeds 400MPa, the high-temperature emissivity at 300 ℃ is lower than 0.02, the near-infrared high transmittance and visible translucency can be realized under the conditions of extremely fine grain size and high density, the Vickers hardness reaches 16.6GPa, and the nano multiphase ceramic becomes a hope and an important candidate for future high-supersonic aircraft infrared window materials.
At present, there are many preparations of Y 2 O 3 The process and method for preparing-MgO composite nano powder, such as sol-gel method, sol-gel combustion method, thermal decomposition method, spray pyrolysis method, etc. can prepare Y 2 O 3 -MgO composite nanopowder. American H.Jordan et al [ Jiwen Wang, dinying Chen, eric H.Jordan, maurice Gell, journal of the American Ceramic Society,93,3535 (2010)]Preparing Y from magnesium acetate and yttrium nitrate by sol-gel method 2 O 3 -MgO composite nanopowder. CN103922742B discloses a method for preparing Y by adopting a sol-gel method 2 O 3 MgO composite nano powder and preparing infrared transparent Y by using Spark Plasma Sintering (SPS), hot isostatic pressing sintering (HIP) or hot pressing sintering (HP) 2 O 3 -method of MgO nano complex phase ceramics. However, Y prepared by these methods 2 O 3 the-MgO composite nanopowder has some disadvantages such as sol-gel method and sol-gel combustionProcess for preparing Y 2 O 3 -MgO composite nanopowder, albeit Y 2 O 3 The uniformity and the dispersibility of the MgO two phases are good, but the organic matters such as citric acid, glycol and the like adopted as a chelating agent or a combustion improver can cause serious carbon-containing group residue pollution, are difficult to completely remove through high-temperature calcination, finally cause that the residual carbon-containing groups in a sintered sample are difficult to remove, influence the thermal, optical, mechanical and other properties of the product, are unfavorable to the high-temperature properties such as the thermal shock resistance of the sample, and finally influence the prepared Y 2 O 3 The comprehensive performance of the-MgO nano complex phase ceramic product loses the practical application value. Y prepared by thermal decomposition 2 O 3 -MgO composite nanopowder, Y although not contaminated with carbon-containing groups 2 O 3 The uniformity and the dispersibility of the two phases of MgO are poor, and yttrium nitrate and magnesium nitrate are decomposed independently to form Y in different temperature regions during thermal decomposition 2 O 3 Each phase and MgO phase are respectively enriched, the sintering activity of the powder is low, higher temperature and longer time are required during sintering, agglomerated and enriched homophase substances grow, the pinning effect is weakened, the crystal grains grow abnormally, and the prepared Y 2 O 3 The comprehensive performance of the-MgO nano complex phase ceramic product is poor. The precipitation method is not easy to prepare Y on a large scale 2 O 3 -MgO composite nanopowder, and it is difficult to realize Y 2 O 3 And MgO two-phase hydroxide is uniformly precipitated at the same time, so that the uniformity of the powder is poor. The spray pyrolysis method has high requirements on equipment and higher production cost, and the prepared powder has a large amount of spherical shell-shaped or hollow spherical large-size aggregates with poor dispersibility, so that the sintering activity of the powder is seriously reduced, and the final ceramic performance is poor.
Disclosure of Invention
The invention aims to provide a method for preparing Y by filling nano powder 2 O 3 Method for preparing-MgO composite powder, overcoming existing Y 2 O 3 The preparation process of the MgO composite nano powder has the defects. The method is to mix Y 2 O 3 Pouring the nano powder into a ball milling tank, adding high-purity magnesium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, and pouring the salt solution into a ballGrinding pot and Y 2 O 3 Mixing the nano powder; or pouring MgO nano powder into a ball milling tank, adding high-purity yttrium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank for mixing with the MgO nano powder, placing the ball milling tank on a ball mill for ball milling for a plurality of hours, placing the ball milling tank into a constant-temperature oven for drying, sieving the ball milling tank by using a sieve to obtain sieving powder, and placing the sieving powder into a muffle furnace for heating and calcining to decompose nitrate into oxide; or directly placing the ball-milled mixture into a muffle furnace for heating and calcining to completely decompose the nitrate to form decomposed nano-magnesia-Y 2 O 3 Nano-filling and coating; or forming decomposed nanometer yttrium oxide to nanometer fill and coat MgO to obtain Y with grain size less than 150nm 2 O 3 -MgO composite powder. Y prepared by the method 2 O 3 -MgO composite nanopowder, Y 2 O 3 MgO two-phase powder is mutually filled and mutually coated on the nano scale, and the dispersion is uniform on the nano scale, thereby avoiding Y in other powder preparation methods 2 O 3 The problem of respective agglomeration of two phases of MgO improves the sintering activity of the powder, and the grain size of the powder is small (a)<150 nm); the preparation process has no pollution of carbon-containing groups, and has the advantages of simple calcination process, low calcination temperature, simple required equipment, short preparation period, low production cost and convenient industrial production.
The technical scheme of the invention is as follows:
will Y 2 O 3 Pouring the nano powder into a ball milling tank, adding high-purity magnesium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank, and pouring the salt solution into a Y-shaped container 2 O 3 Mixing the nano powder; or pouring MgO nano powder into a ball milling tank, adding high-purity yttrium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank for mixing with the MgO nano powder, placing the ball milling tank on a ball mill for ball milling for a plurality of hours, placing the ball milling tank into a constant-temperature oven for drying, sieving the ball milling tank by using a sieve to obtain sieving powder, and placing the sieving powder into a muffle furnace for heating and calcining to decompose nitrate into oxide; or directly placing the ball-milled mixture into a muffle furnace for heating and calcining to completely decompose the nitrate to form decomposed nano-magnesia-Y 2 O 3 Nano-filling and coating; or forming decomposed nanometer yttrium oxide to nanometer fill and coat MgO to obtain Y with grain size less than 150nm 2 O 3 -MgO composite powder.
The preparation method comprises two stages, and comprises the following specific steps:
the first stage is as follows: mixing and ball-milling the nano powder and a nitrate solution:
step 1.1) weighing appropriate amount of nano Y 2 O 3 Or MgO powder is poured into the ball milling tank respectively;
step 1.2) weighing Y 2 O 3 Or weighing a certain amount of high-purity magnesium nitrate hexahydrate or yttrium nitrate hexahydrate according to the mass ratio of the MgO powder, and respectively adding absolute ethyl alcohol to completely dissolve the magnesium nitrate hexahydrate or the yttrium nitrate hexahydrate in a beaker to obtain a nitrate solution;
step 1.3) pouring the magnesium nitrate solution obtained in the step 1.2) into a ball milling tank and Y 2 O 3 Mixing the powder; or pouring yttrium nitrate solution into a ball milling tank to be mixed with MgO powder, and placing the mixture on a ball mill for ball milling for several hours to obtain mixture slurry;
and a second stage: heating, calcining and decomposing the obtained mixture slurry completely to form the Y filled and coated with the nano powder 2 O 3 -MgO composite powder:
step 2.1) putting the mixture slurry obtained in the step 1.3) into a constant-temperature oven for drying, sieving by using a sieve to obtain sieve powder, and putting the sieve powder into a muffle furnace for heating and calcining to decompose nitrate into oxide; or directly placing the mixture slurry after ball milling into a muffle furnace for heating and calcining to completely decompose the nitrate, thus obtaining the Y filled and coated with the nano powder 2 O 3 -MgO composite powder.
The nano powder in the step 1.1) is commercial Y 2 O 3 Or MgO powder with grain size less than 100nm.
The high-purity magnesium nitrate hexahydrate or yttrium nitrate hexahydrate in the step 1.2) is a commercial raw material, and the purity is not lower than 99%.
The proportion in the step 1.2) is as follows: weighing Y 2 O 3 Quality of (1)The mass ratio of the amount of MgO to the amount of MgO obtained after the magnesium nitrate hexahydrate is completely decomposed by heating is 1:9 to 9: 1; weighing the mass of MgO and Y obtained after yttrium nitrate hexahydrate is completely decomposed by heating 2 O 3 The mass ratio of (1): 9 to 9: 1.
The ball milling time in the step 1.3) is 2-72h.
The heating calcination temperature in the step 2.1) is 500-1000 ℃, and the calcination time is 1-10h.
The temperature of the constant temperature oven in the step 2.1) is 50-200 ℃.
The mesh number of the mesh sieve in the step 2.1) is 50-300 meshes.
The composite nano powder in the step 2.1) has the powder grain size less than 150nm.
Compared with the prior art, the invention has the technical effects that:
y prepared by nano-filling 2 O 3 -MgO composite nanopowder, Y 2 O 3 MgO two-phase powder is mutually filled and mutually coated on the nano scale, and the dispersion is uniform on the nano scale, thereby avoiding Y in other powder preparation methods 2 O 3 MgO two phases are respectively agglomerated and dispersed unevenly, the sintering activity of the powder is improved, and the grain size of the powder is small (<150 nm); the preparation process has no pollution of introduced carbon-containing radical, simple calcining process, low calcining temperature, simple apparatus, short preparation period, low production cost and easy industrial production.
Drawings
FIG. 1 shows Y prepared in example 1 2 O 3 TEM morphology of-MgO composite nanopowder.
FIG. 2 shows Y obtained in example 5 2 O 3 TEM morphology of-MgO composite nanopowder.
FIG. 3 shows Y obtained in example 7 2 O 3 SEM topography of-MgO composite nanopowder.
FIG. 4 shows Y obtained in example 12 2 O 3 SEM topography of-MgO composite nanopowder.
Detailed Description
The invention is further illustrated by the following description of examples and the accompanying drawings, which are given solely for the purpose of illustration and are not intended to limit the scope of the invention.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The preparation parameters and conditions of the composite nanopowders used in examples 1-6 are specifically shown in the following table 1:
table 1: process parameter conditions for examples 1 to 6
Examples 1 to 3
Examples 1-3Y was measured according to the process parameters of Table 1 2 O 3 Pouring the nano powder into a ball milling tank, adding the weighed high-purity magnesium nitrate hexahydrate into absolute ethyl alcohol for dissolving, pouring the obtained salt solution into the ball milling tank and Y 2 O 3 Mixing nano-powder, placing a ball milling tank on a ball mill for ball milling for several hours, placing the ball milling tank on a constant-temperature oven for drying, sieving the powder by using a sieve to obtain sieved powder, placing the sieved powder into a muffle furnace for heating and calcining to completely decompose nitrate into oxide to form decomposed nano-magnesium oxide Y 2 O 3 To obtain a nanopowder filled and coated Y 2 O 3 -MgO composite powder. The specific steps are similar to the steps described above and are mainly realized by adjusting various parameter conditions.
Examples 4 to 6
Examples 4 to 6 were prepared by weighing MgO nano-powder according to the process parameters of Table 1, pouring the MgO nano-powder into a ball mill pot, adding the weighed high-purity yttrium nitrate hexahydrate into absolute ethanol to dissolve the obtained salt solution, pouring the salt solution into the ball mill pot to mix with the MgO nano-powder, placing the ball mill pot on a ball mill to ball-mill for several hours, placing the ball mill pot on a constant temperature oven to dry, sieving the dried ball pot with a sieve to obtain sieved powder, placing the sieved powder in a muffle furnace to heat and calcine the powder to completely decompose nitrate into oxide, thereby forming decomposed nano-powderNanometer filling and coating of MgO by using yttrium oxide to obtain Y filled and coated with nanometer powder 2 O 3 -MgO composite powder. The specific steps are similar to the steps described above and are mainly realized by adjusting various parameter conditions.
The conditions of the parameters for preparing the composite nanopowders used in examples 7-12 are specifically shown in the following Table 2:
table 2: process parameter conditions for examples 7 to 12
Examples 7 to 9
Examples 7-9 weighing Y according to the process parameters of Table 2 2 O 3 Pouring the nano powder into a ball milling tank, adding the weighed high-purity magnesium nitrate hexahydrate into absolute ethyl alcohol for dissolving, pouring the obtained salt solution into the ball milling tank and Y 2 O 3 Mixing the nano-powder, placing the ball milling tank on a ball mill for ball milling for several hours, directly placing the mixture slurry after ball milling in a muffle furnace for heating and calcining to completely decompose nitrate to form decomposed nano-magnesia pair Y 2 O 3 To obtain a nanopowder filled and coated Y 2 O 3 -MgO composite nanopowder. The specific steps are similar to the steps described above and are mainly realized by adjusting various parameter conditions.
Examples 10 to 12
Examples 10 to 12 were carried out by weighing MgO nanopowder according to the process parameters of table 2, pouring the MgO nanopowder into a ball mill pot, adding the weighed high purity yttrium nitrate hexahydrate into anhydrous ethanol to dissolve the obtained salt solution, pouring the salt solution into the ball mill pot to mix with the MgO nanopowder, placing the ball mill pot on a ball mill to ball mill for several hours, directly placing the ball milled mixture slurry into a muffle furnace to heat and calcine the mixture slurry to completely decompose nitrate, forming decomposed nano yttrium oxide to nano-fill and coat MgO, and obtaining Y filled and coated with nanopowder 2 O 3 -MgO composite nanopowder. The specific steps are similar to the steps described above and are mainly realized by adjusting various parameter conditions.
In summary, the present invention provides Y prepared by any of the above methods 2 O 3 -MgO composite nanopowder, Y 2 O 3 MgO two-phase powder is mutually filled and mutually coated on the nano scale, and the dispersion is uniform on the nano scale, thereby avoiding Y in other powder preparation methods 2 O 3 MgO two phases agglomerate and disperse unevenly, the nano composite powder synthesized under the above parameters is very fine, the two phases are distributed evenly and stably, and the powder grain size is fine: (<150 nm) and has higher sintering activity. The method for preparing the nano composite powder has the advantages of simple operation, no pollution of carbon-containing groups introduced in the preparation process, simple calcination process, low calcination temperature, no need of precise instruments, short preparation period, easy large-yield preparation, low production cost and easy realization of industrial production. And the method with lower cost can be easily used for synthesizing other oxide powder or oxide composite powder materials.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the present invention in any way, so that any person skilled in the art can make modifications or changes in the technical content disclosed above. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (4)
1. Preparation of Y by filling nano powder 2 O 3 A method for producing the MgO composite powder, characterized in that Y is added 2 O 3 Pouring the nano powder into a ball milling tank, adding high-purity magnesium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank, and pouring the salt solution into a Y-shaped container 2 O 3 Mixing the nano powder; or pouring MgO nano powder into a ball milling tank, adding high-purity yttrium nitrate hexahydrate into absolute ethyl alcohol for dissolving to obtain a salt solution, pouring the salt solution into the ball milling tank to mix with the MgO nano powder, placing the ball milling tank on a ball mill for ball milling for a plurality of hours, placing the ball milling tank into a constant-temperature oven for drying, sieving by a sieve to obtain sieving powder, placing the sieving powder into a muffle furnace for heating and calcining to obtain the sieving powderDecomposing the nitrate to oxide; or directly placing the ball-milled mixture into a muffle furnace for heating and calcining to completely decompose the nitrate to form decomposed nano-magnesia-Y 2 O 3 Nano-filling and coating; or forming decomposed nanometer yttrium oxide to nanometer fill and coat MgO to obtain Y with grain size less than 150nm 2 O 3 -MgO composite powder, comprising in particular two stages, the steps of:
the first stage is as follows: mixing and ball-milling the nano powder and a nitrate solution:
step 1.1) weighing proper amount of nano Y 2 O 3 Or MgO powder is poured into the ball milling tank respectively;
step 1.2) weighing Y 2 O 3 Or weighing a certain amount of high-purity magnesium nitrate hexahydrate or yttrium nitrate hexahydrate according to the mass ratio of the MgO powder, and respectively adding absolute ethyl alcohol to completely dissolve the magnesium nitrate hexahydrate or the yttrium nitrate hexahydrate in a beaker to obtain a nitrate solution;
the proportions are as follows: weighing Y 2 O 3 The mass ratio of the magnesium nitrate hexahydrate to the MgO obtained after complete thermal decomposition of magnesium nitrate hexahydrate is 1:9 to 9: 1; weighing the mass of MgO and Y obtained after yttrium nitrate hexahydrate is completely decomposed by heating 2 O 3 The mass ratio of (1): 9 to 9: 1;
step 1.3) pouring the magnesium nitrate solution obtained in the step 1.2) into a ball milling tank and Y 2 O 3 Mixing the powder; or pouring yttrium nitrate solution into a ball milling tank to be mixed with MgO powder, and placing the mixture on a ball mill for ball milling for several hours to obtain mixture slurry;
the high-purity magnesium nitrate hexahydrate or yttrium nitrate hexahydrate is a commercial raw material, and the purity is not lower than 99%;
and a second stage: heating, calcining and decomposing the obtained mixture slurry completely to form the Y filled and coated with the nano powder 2 O 3 -MgO composite powder:
putting the mixture slurry obtained in the step 1.3) into a constant-temperature oven for drying, sieving by using a sieve to obtain sieve powder, putting the sieve powder into a muffle furnace for heating and calcining at the temperature of 500-1000 ℃ for 1-10h to decompose nitrate into oxide;
or directly placing the mixture slurry obtained in the step 1.3) into a muffle furnace for heating and calcining to completely decompose the nitrate, namely preparing the Y filled with the nano powder 2 O 3 -MgO composite powder having a grain size of less than 150nm.
2. The method for preparing Y by filling nano powder according to claim 1 2 O 3 The method for preparing the MgO composite powder is characterized in that the ball milling time in the step 1.3) is 2-72h.
3. The method for preparing Y by filling nano powder according to claim 1 2 O 3 The method for preparing the MgO composite powder is characterized in that the temperature of the constant-temperature oven in the second stage is 50-200 ℃.
4. The nano-powder filling preparation Y of claim 1 2 O 3 The method for preparing the MgO composite powder is characterized in that the mesh number of the mesh sieve in the second stage is 50-300 meshes.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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