CN113955763A - Ytterbium silicate spheroidized powder and plasma in-situ synthesis preparation method thereof - Google Patents
Ytterbium silicate spheroidized powder and plasma in-situ synthesis preparation method thereof Download PDFInfo
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- CN113955763A CN113955763A CN202111469975.5A CN202111469975A CN113955763A CN 113955763 A CN113955763 A CN 113955763A CN 202111469975 A CN202111469975 A CN 202111469975A CN 113955763 A CN113955763 A CN 113955763A
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The invention discloses a method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis, which comprises the following steps: mixing ytterbium oxide, silicon dioxide powder, a binder, a dispersant and water, and performing ball milling to prepare slurry; drying and granulating the slurry, and screening to obtain mixed powder; and (3) carrying out plasma high-temperature spheroidizing on the mixed powder, and synthesizing in situ to prepare the ytterbium silicate spheroidized powder. The synthesized ytterbium silicate spheroidized powder is spherical and has better fluidity.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to ytterbium silicate spheroidized powder and a plasma in-situ synthesis preparation method thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Environmental Barrier Coating (EBC) for advanced high thrust weight ratio engine hot end components C/C, C/SiC and SiCfThe performance improvement and the service life extension of the/SiC composite material have important significance. Typical types of environmental barrier coating materials include mullite/zirconia systems, barium strontium aluminosilicate systems, rare earth silicate systems, and the like. In which the ytterbium silicate system (consisting of Yb)2SiO5And Yb2Si2O7) The excellent chemical stability and the good matching property with the thermal expansion coefficient of the base material are particularly interesting, and the method is also an important development direction of a new generation of environmental barrier coating materials.
Plasma thermal spraying is a common method for preparing environmental barrier coatings. In the plasma spraying process, one of the important parameters influencing the coating organization structure and the deposition efficiency of the environmental barrier is the powder feeding amount, and the powder feeding amount has a larger relationship with the appearance of the powder. Therefore, the development and production of ytterbium silicate powder with high roundness and sphericity and uniform component become a focus of attention.
The method for synthesizing ytterbium silicate powder includes solid-phase reaction method and solid-liquid reaction method (YInyu Fan et al. effects of differential signaling on the synthesis of gamma-Y2Si2O7powders[J]Ceramics International, 42 (2016): 14813-14817), sol-gel method (Cen Zhao et al synthesis and catalysis of β -Yb)2Si2O7powders[J]Ceramics International,39(2013):5805-5811), and the like, and also have reports related to the preparation of ytterbium silicate nanopowder. However, these synthesized powders cannot be directly used for plasma spraying, and require spheroidizing.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an ytterbium silicate spheroidized powder and a plasma in-situ synthesis preparation method thereof. The shape of the ytterbium silicate spheroidized powder synthesized in situ by plasma is spherical and has better fluidity.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the plasma in-situ synthesis preparation method of the ytterbium silicate spheroidized powder comprises the following steps:
mixing ytterbium oxide, silicon dioxide powder, a binder, a dispersant and water, and performing ball milling to prepare slurry;
drying and granulating the slurry, and screening to obtain mixed powder;
and carrying out plasma high-temperature spheroidization on the mixed powder, and preparing the ytterbium silicate spheroidized powder in situ.
In some embodiments, the binder is selected from one or a combination of polyvinyl alcohol, hydroxymethyl cellulose, dextrin or starch.
Further, the binder is polyvinyl alcohol.
In some embodiments, the dispersant is selected from CE64 or/and PC 67.
In some embodiments, the mass ratio of ytterbium oxide, silica powder, binder, dispersant and water is 1000:198-396:1.8-2.2:0.8-1.1: 620-660.
In some embodiments, the particle size of the sieved particles is 80-150 mesh. The powder in the particle size range can obtain particles with good spheroidizing effect more easily, and the poor powder flowability and gun blockage are easily caused when the particle size is too small.
In some embodiments, the temperature of the high temperature spheronization is 5000-.
In some embodiments, the plasma gas is nitrogen.
In a second aspect, the invention provides ytterbium silicate spheroidized powder, which is synthesized and prepared by the preparation method.
The beneficial effects of the invention are as follows:
the main crystal phase of the spheroidized ytterbium silicate powder synthesized in situ by plasma is Yb2Si2O7Or Yb2SiO5。
The ytterbium silicate spheroidized powder synthesized in situ by the plasma has the advantages of simple process, high yield and cost saving because the ytterbium silicate crystal phase is synthesized in situ in the preparation process.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is an X-ray diffraction pattern of ytterbium silicate spheroidized powder prepared in example 1 of the present invention;
fig. 2 is an optical microscope photograph of the ytterbium silicate spheroidized powder prepared in example 2 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
The method for in-situ synthesis of ytterbium silicate spheroidized powder by using plasma specifically comprises the following steps:
1) putting 1000 parts of ytterbium oxide powder, 396 parts of silicon dioxide powder, 1 part of CE64 and 2 parts of polyvinyl alcohol into a ball mill, adding 650 parts of deionized water, and carrying out ball milling for 4 hours to obtain mixed slurry;
2) and (3) performing spray granulation on the mixed slurry in a spray drying tower, screening, and drying powder with the granularity of 80-150 meshes at 100 ℃ for plasma spheroidization. And continuously adding the undersize powder and the oversize powder into the ball mill for use.
3) And (3) feeding the dried powder with the granularity of 80-150 meshes into a feeding machine of plasma spheroidizing equipment for plasma spheroidizing. The plasma gas is nitrogen, and the plasma spheroidization temperature is 7000 ℃.
The roundness and sphericity of the ytterbium silicate spheroidized powder particles are high, the fluidity is 18.00g/s, the repose angle is 45 degrees, and the yield is 76 percent. The main crystal phase being Yb2Si2O7The X-ray diffraction pattern is shown in FIG. 1.
Example 2
As in example 1, except that: the weight portion of the silicon dioxide powder is 198 portions.
The yield of ytterbium silicate spheroidized powder is 78%, and the main crystal phase is Yb2SiO5As shown in fig. 2.
Example 3
As in example 1, except that: the weight portion of the silicon dioxide powder is 264 portions.
The main crystal phase of the ytterbium silicate spheroidized powder is Yb2SiO5And Yb2Si2O7The yield of the mixture was 80%.
Comparative example 1
1) Mixing 1000 parts of ytterbium oxide powder, 396 parts of silicon dioxide powder and 14 parts of lithium fluoride in a high-speed mixer for 20min, putting into an alumina crucible, putting into a muffle furnace, raising the temperature to 1450 ℃ at the speed of 3 ℃/min, preserving the temperature for 2h, and cooling along with the furnace. Crushing to obtain ytterbium silicate powder.
2) Adding 1000 parts of synthesized ytterbium silicate powder into 700 parts of deionized water, putting 1 part of polyvinyl alcohol into a ball mill, and carrying out ball milling and mixing for 2 hours to obtain mixed slurry;
3) and (3) performing spray granulation on the mixed slurry in a spray drying tower, screening, and drying powder with the granularity of 80-150 meshes at 100 ℃ for plasma spheroidization.
4) And (3) sending the granulation powder of 80-150 meshes into plasma spheroidizing equipment, and carrying out high-temperature spheroidizing treatment at 7000 ℃ to obtain plasma spheroidized ytterbium silicate powder.
The process has the disadvantages that ytterbium silicate powder is firstly synthesized, and then granulation, spheroidization and secondary high-temperature treatment are carried out, so that the process is complicated, the energy consumption is high, the raw material loss in the preparation process is large, the product yield is lower than 30%, and the cost is high.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The plasma in-situ synthesis preparation method of the ytterbium silicate spheroidized powder is characterized by comprising the following steps of: the method comprises the following steps:
mixing ytterbium oxide, silicon dioxide powder, a binder, a dispersant and water, and performing ball milling to prepare slurry;
drying and granulating the slurry, and screening to obtain mixed powder;
and carrying out plasma high-temperature spheroidization on the mixed powder, and preparing the ytterbium silicate spheroidized powder in situ.
2. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 1, wherein the method comprises the following steps: the binder is selected from one or the combination of polyvinyl alcohol, hydroxymethyl cellulose, dextrin or starch.
3. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 2, wherein the method comprises the following steps: the binder is polyvinyl alcohol.
4. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 1, wherein the method comprises the following steps: the dispersing agent is selected from CE64 or/and PC 67.
5. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 1, wherein the method comprises the following steps: the mass ratio of ytterbium oxide, silicon dioxide powder, binder, dispersant and water is 1000:198-396:1.8-2.2:0.8-1.1: 620-660.
6. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 1, wherein the method comprises the following steps: the particle size of the sieved particles is 80-150 meshes.
7. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 1, wherein the method comprises the following steps: the temperature of high-temperature spheroidization is 5000-8000 ℃.
8. The method for preparing ytterbium silicate spheroidized powder by plasma in-situ synthesis according to claim 1, wherein the method comprises the following steps: the plasma gas is nitrogen.
9. The ytterbium silicate spheroidized powder is characterized in that: is synthesized by the preparation method of any one of claims 1 to 8.
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Citations (5)
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|---|---|---|---|---|
| JP2006037238A (en) * | 2001-03-08 | 2006-02-09 | Shin Etsu Chem Co Ltd | Method for producing spherical particle for thermal spraying |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN109837496A (en) * | 2017-11-27 | 2019-06-04 | 深圳航发复合材料有限公司 | A kind of preparation method of ytterbium silicate plasma spraying powder |
| CN111410201A (en) * | 2020-03-06 | 2020-07-14 | 哈尔滨工业大学 | Preparation method of nano-structure ytterbium silicate feed suitable for plasma spraying |
| CN112662982A (en) * | 2019-10-15 | 2021-04-16 | 哈尔滨工业大学 | Nano-structure Yb suitable for plasma spraying2Si2O7Preparation method of spherical feed |
-
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- 2021-12-03 CN CN202111469975.5A patent/CN113955763A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006037238A (en) * | 2001-03-08 | 2006-02-09 | Shin Etsu Chem Co Ltd | Method for producing spherical particle for thermal spraying |
| CN105036146A (en) * | 2015-08-28 | 2015-11-11 | 北京理工大学 | Method for preparing spherical nanometer zirconium silicate powder |
| CN109837496A (en) * | 2017-11-27 | 2019-06-04 | 深圳航发复合材料有限公司 | A kind of preparation method of ytterbium silicate plasma spraying powder |
| CN112662982A (en) * | 2019-10-15 | 2021-04-16 | 哈尔滨工业大学 | Nano-structure Yb suitable for plasma spraying2Si2O7Preparation method of spherical feed |
| CN111410201A (en) * | 2020-03-06 | 2020-07-14 | 哈尔滨工业大学 | Preparation method of nano-structure ytterbium silicate feed suitable for plasma spraying |
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| 王海军: "热喷涂材料及应用", 国防工业出版社 * |
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