CN108408754A - A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying - Google Patents
A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying Download PDFInfo
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- CN108408754A CN108408754A CN201810109902.7A CN201810109902A CN108408754A CN 108408754 A CN108408754 A CN 108408754A CN 201810109902 A CN201810109902 A CN 201810109902A CN 108408754 A CN108408754 A CN 108408754A
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- yttrium oxide
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- color
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention belongs to the technical field of hot based on yttrium oxide, more particularly to a kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method used for hot spraying for being granulated yttrium oxide.I.e. by slurry granularity D50 after controlling depolymerization at 1.3 μm~1.4 μm, the yttria coating for making finally to spray gained is white.Avoid spraying after coating be pink colour in the case of, influence corrosion-resistant, high temperature resistance and service life.
Description
Technical field
The invention belongs to the technical field of hot based on yttrium oxide, more particularly to one kind being conducive to color after control spraying
Resistant to plasma corrode it is used for hot spraying be granulated yttrium oxide preparation method.
Background technology
Yttrium oxide has high-melting-point, phase stability and low heat expansion, is to prepare high-performance electronic ceramics, the corruption of anti-plasma
Lose the important source material of spray coating powder.And yttrium oxide also shows that its superior performance in the application of Aeronautics and Astronautics, ceramic field, it is main
It is used to manufacture microwave magnetic material and military project important materials, also serves as optical glass, ceramic material additive, large screen
TV phosphor of high brightness and other kinescope coatings.It is additionally operable to the strong heat-resisting alloy of manufacture high temperature, aircraft nozzle etc.；In recent years
Come, yttrium oxide powder is also more applied in electronics industry, semicon industry, it is particularly possible to anti-as semiconductor etching machine
Only plasma etching, ray corrosion sprayed on material.
The higher yttrium oxide of purity is white shape, but but deposits the case where being converted into pink colour after spray coating in many cases,
Influence the corrosion-resistant of coating, high temperature resistance and service life.But the specific of pink colour is rendered as after causing yttrium oxide to be sprayed-on
Reason can not but define always, and applicant attempted the particle diameter distribution by controlling yttria particles before, but had tested very
Mostly different particle size distribution ranges, is but still shown as pink colour after spraying；It is that calcination lacks in the process that applicant also suspected before
Oxygen and the lattice defect for causing yttrium oxide, coating is pink after eventually leading to spraying, therefore has been carried out sternly to calcination technique
The control of lattice is also attempted to have carried out multiple improvement experiment to calcination operation link, finally can not still solve this technical problem.
Invention content
The present invention first, it is realized that " after spraying yttria coating present in pink colour " this reason appears in depolymehzation process,
Slurry granularity D50 has a major impact coating color of the yttrium oxide after granulation through spraying gained after depolymerization, slurry grain after depolymerization
D50 is spent at 1.3 μm~1.4 μm, and the yttria coating of final spraying gained is white, and the concrete operations of this programme are：
(1) yttrium oxide powder and dispersant are sufficiently mixed and are configured to slurry,
Purity >=99.99%, the grain size of yttrium oxide powder are 2~3 μm, when yttrium oxide powder is with dispersant, the two
Weight ratio be 1:2,
(2) slurry obtained in step (1) is subjected to depolymerization reduction, the D50 of yttrium oxide is 1.1 in slurry after control depolymerization
μm~1.5 μm,
Preferably, the D50 of yttrium oxide is 1.3 μm~1.4 μm in slurry after control depolymerization,
Depolymerization reduction is carried out in depolymerizer specifically, slurry is injected, control rotating speed is 500~1600r/min, when depolymerization
Between be 30min~120min, after obtained depolymerization in slurry yttrium oxide D50 be 1.1 μm~1.5 μm, and after depolymerization gained
Particle finally constitute the granulation yttrium oxide in subsequent step (5),
And rotating speed is 900r/min, the depolymerization time is 60min, and the D50 of yttrium oxide is 1.3 in slurry after obtained depolymerization
μm~1.4 μm；
(3) surface-active activator is added in the slurry after being restored to step (2) depolymerization and is sufficiently stirred,
Surface-active activator is the combination of one or more of malic acid, tartaric acid, acetic acid and oxalic acid；
(4) yttrium oxide ball-type powder is made in the mixed slurry obtained in step (3),
It is specific to be prepared by mist projection granulating using the puffing ball equipment processed of heat；
(5) the yttrium oxide ball-type powder obtained in step (4) is subjected to consolidation processing, obtains resistant to plasma corrosion
Granulation yttrium oxide used for hot spraying,
Preferably, consolidation processing carries out under atmospheric environment, it is ensured that sufficient oxygen supply avoids anoxic
There is the generation of spot or the insufficient phenomenon of calcination in particle surface caused by calcination,
Consolidation processing be divided into preheating, in mild three heating periods of high temperature, preferably, preheating temperature is 800
DEG C, soaking time 1h；Medium temperature temperature is 1200 DEG C, soaking time 1.5h；High-temperature temperature is 1750 DEG C, high temperature hold time
For 5h.
Description of the drawings
Fig. 1 is embodiment 1 (b) and the granulation yttrium oxide prepared by comparative example 1 (a), is obtained after progress thermal spraying
The color contrast figure of resistant to plasma corrosion resistant coating, in contrast, the color of a are deep.
Fig. 2 is embodiment 2 (b) and the granulation yttrium oxide prepared by comparative example 2 (a), is obtained after progress thermal spraying
The color contrast figure of resistant to plasma corrosion resistant coating, in contrast, the color of a are deep.
Fig. 3 is embodiment 3 (b) and the granulation yttrium oxide prepared by comparative example 3 (a), is obtained after progress thermal spraying
The color contrast figure of resistant to plasma corrosion resistant coating, in contrast, the color of a are deep.
Specific implementation mode
Embodiment 1
(1) by purity >=99.99%, the yttrium oxide powder that grain size is 2~3 μm and deionized water according to 1:2 mass ratio
Mixing, and be sufficiently stirred and be configured to slurry；
(2) slurry obtained in step (1) is injected and carries out depolymerization reduction in depolymerizer, depolymerizer rotating speed is 900r/
Min, depolymerization time are 60min, and the D50 of yttrium oxide is 1.3 μm in slurry after depolymerization, and particle size range is 0.5~5 μm；
(3) apple acid crystal is added in the slurry after being restored to step (2) depolymerization and is thoroughly mixed, apple acid crystal
Mass ratio with yttrium oxide powder in step (1) is 1:100；
(4) yttrium oxide is made by mist projection granulating using the puffing ball equipment processed of heat in the mixed slurry obtained in step (3)
Ball-type powder；
(5) the yttrium oxide ball-type powder that will be obtained in step (4), prior to 800 DEG C at isothermal holding 1h, at 1200 DEG C
Isothermal holding 1.5h, finally the isothermal holding 5h at 1750 DEG C, obtains resistant to plasma and corrodes granulation yttrium oxide used for hot spraying, this is made
Granule yttria particle size range is 10~70 μm；D50 is 36 μm, apparent density 2.3g/cm3, resistance to broken intensity is 30Mpa,
Thermal spraying is carried out to granulation yttrium oxide manufactured in the present embodiment and obtains resistant to plasma corrosion resistant coating, coating color is white
Color.
Embodiment 2
(1) by purity >=99.99%, the yttrium oxide powder that grain size is 2~3 μm and ethyl alcohol according to 1:2 mass ratio mixing,
And it is sufficiently stirred and is configured to slurry；
(2) slurry obtained in step (1) is injected and carries out depolymerization reduction in depolymerizer, depolymerizer rotating speed is 1500r/
Min, depolymerization time are 100min, and the D50 of yttrium oxide is 1.1 μm in slurry after depolymerization, and particle size range is 0.3~4 μm；
(3) winestone acid crystal is added in the slurry after being restored to step (2) depolymerization and is thoroughly mixed, winestone acid crystal
Mass ratio with yttrium oxide powder in step (1) is 1:85；
(4) yttrium oxide is made by mist projection granulating using the puffing ball equipment processed of heat in the mixed slurry obtained in step (3)
Ball-type powder；
(5) the yttrium oxide ball-type powder that will be obtained in step (4), prior to 800 DEG C at isothermal holding 1h, at 1200 DEG C
Isothermal holding 1.5h, finally the isothermal holding 5h at 1750 DEG C, obtains resistant to plasma and corrodes granulation yttrium oxide used for hot spraying, this is made
Granule yttria particle size range is 10~70 μm；D50 is 36 μm, apparent density 2.17g/cm3, resistance to broken intensity is 31Mpa,
Thermal spraying is carried out to granulation yttrium oxide manufactured in the present embodiment and obtains resistant to plasma corrosion resistant coating, coating color is white
Color.
Embodiment 3
(1) by purity >=99.99%, the yttrium oxide powder that grain size is 2~3 μm and propyl alcohol according to 1:2 mass ratio mixing,
And it is sufficiently stirred and is configured to slurry；
(2) slurry obtained in step (1) is injected and carries out depolymerization reduction in depolymerizer, depolymerizer rotating speed is 600r/
Min, depolymerization time are 45min, and the D50 of yttrium oxide is 1.5 μm in slurry after depolymerization, and particle size range is 0.7~6 μm；
(3) oxalic acid crystal is added in the slurry after being restored to step (2) depolymerization and is thoroughly mixed, oxalic acid crystal and step
Suddenly the mass ratio of yttrium oxide powder is 1 in (1):80；
(4) yttrium oxide is made by mist projection granulating using the puffing ball equipment processed of heat in the mixed slurry obtained in step (3)
Ball-type powder；
(5) the yttrium oxide ball-type powder that will be obtained in step (4), prior to 800 DEG C at isothermal holding 1h, at 1200 DEG C
Isothermal holding 1.5h, finally the isothermal holding 5h at 1750 DEG C, obtains resistant to plasma and corrodes granulation yttrium oxide used for hot spraying, this is made
Granule yttria particle size range is 10~70 μm；D50 is 36 μm, apparent density 2.24g/cm3, resistance to broken intensity is 32Mpa,
Thermal spraying is carried out to granulation yttrium oxide manufactured in the present embodiment and obtains resistant to plasma corrosion resistant coating, coating color is white
Color.
Comparative example 1
(1) with embodiment 1；
(2) slurry obtained in step (1) is injected and carries out depolymerization reduction in depolymerizer, aoxidized in slurry after control depolymerization
The D50 of yttrium is 1.0 μm, and particle size range is 0.3~4 μm；
(3) with embodiment 1；
(4) with embodiment 1；
(5) the yttrium oxide ball-type powder obtained in step (4) is kept the temperature respectively at 800 DEG C, 1200 DEG C, 1750 DEG C
Processing, obtain resistant to plasma corrosion granulation yttrium oxide used for hot spraying makes the granulation oxygen by the control to each stage soaking time
It is 10~70 μm to change yttrium particle size range；D50 is 36 μm.
Thermal spraying is carried out to granulation yttrium oxide prepared by this comparative example and obtains resistant to plasma corrosion resistant coating, coating color
For pink.
Comparative example 2
(1) with embodiment 2；
(2) slurry obtained in step (1) is injected and carries out depolymerization reduction in depolymerizer, aoxidized in slurry after control depolymerization
The D50 of yttrium is 1.0 μm, and particle size range is 0.3~4 μm；
(3) with embodiment 2；
(4) with embodiment 2；
(5) the yttrium oxide ball-type powder obtained in step (4) is kept the temperature respectively at 800 DEG C, 1200 DEG C, 1750 DEG C
Processing, obtain resistant to plasma corrosion granulation yttrium oxide used for hot spraying makes the granulation oxygen by the control to each stage soaking time
It is 10~70 μm to change yttrium particle size range；D50 is 36 μm.
Thermal spraying is carried out to granulation yttrium oxide prepared by this comparative example and obtains resistant to plasma corrosion resistant coating, coating color
For pink.
Comparative example 3
(1) with embodiment 3；
(2) slurry obtained in step (1) is injected and carries out depolymerization reduction in depolymerizer, aoxidized in slurry after control depolymerization
The D50 of yttrium is 1.6 μm, and particle size range is 0.7~6 μm；
(3) with embodiment 3；
(4) with embodiment 3；
(5) the yttrium oxide ball-type powder obtained in step (4) is kept the temperature respectively at 800 DEG C, 1200 DEG C, 1750 DEG C
Processing, obtain resistant to plasma corrosion granulation yttrium oxide used for hot spraying makes the granulation oxygen by the control to each stage soaking time
It is 10~70 μm to change yttrium particle size range；D50 is 36 μm.
Thermal spraying is carried out to granulation yttrium oxide prepared by this comparative example and obtains resistant to plasma corrosion resistant coating, coating color
For pink.
Claims (9)
1. a kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method used for hot spraying for being granulated yttrium oxide, special
Sign is：The preparation method is,
(1) yttrium oxide powder and dispersant are sufficiently mixed and are configured to slurry；
(2) slurry obtained in step (1) is subjected to depolymerization reduction, control after depolymerization the D50 of yttrium oxide in slurry be 1.1 μm~
1.5μm；
(3) surface-active activator is added in the slurry after being restored to step (2) depolymerization and is sufficiently stirred；
(4) yttrium oxide ball-type powder is made in the mixed slurry obtained in step (3)；
(5) the yttrium oxide ball-type powder obtained in step (4) is subjected to consolidation processing, obtains resistant to plasma corrosion thermal jet
It applies with granulation yttrium oxide.
2. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：Purity >=99.99% of yttrium oxide powder described in step (1).
3. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：In step (1), when yttrium oxide powder is with dispersant, the weight ratio of the two is 1:2.
4. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：In step (2), will slurry inject depolymerizer in carry out depolymerization reduction, control rotating speed be 500~
1600r/min, depolymerization time are 30min~120min, and the D50 of yttrium oxide is 1.1 μm~1.5 in slurry after obtained depolymerization
μm。
5. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：In step (2), the D50 of yttrium oxide is 1.3 μm~1.4 μm in slurry after control depolymerization.
6. the resistant to plasma as claimed in claim 5 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：In step (2), slurry is injected and carries out depolymerization reduction in depolymerizer, control rotating speed is 900r/
Min, depolymerization time are 60min.
7. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：Surface-active activator described in step (3) is in malic acid, tartaric acid, acetic acid and oxalic acid
One or more of combinations.
8. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：In step (5), consolidation processing carries out under atmospheric environment.
9. the resistant to plasma as described in claim 1 for being conducive to color after control sprays corrodes granulation yttrium oxide used for hot spraying
Preparation method, it is characterised in that：In step (5), consolidation processing be divided into preheating, in mildly three heating periods of high temperature,
Preheating temperature is 800 DEG C, soaking time 1h；Medium temperature temperature is 1200 DEG C, soaking time 1.5h；High-temperature temperature is 1750
DEG C, high temperature hold time 5h.
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| CN201810109902.7A CN108408754B (en) | 2018-02-05 | 2018-02-05 | A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying |
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| CN201810109902.7A CN108408754B (en) | 2018-02-05 | 2018-02-05 | A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158009A (en) * | 2019-06-24 | 2019-08-23 | 江苏立达高科特种材料有限公司 | The preparation method of yttrium oxide hot spraying powder |
| CN113912103A (en) * | 2021-11-02 | 2022-01-11 | 常州市卓群纳米新材料有限公司 | Preparation method of corrosion-resistant yttrium oxide capable of controlling spraying color |
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| CN113912103A (en) * | 2021-11-02 | 2022-01-11 | 常州市卓群纳米新材料有限公司 | Preparation method of corrosion-resistant yttrium oxide capable of controlling spraying color |
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