CN103074568A - Preparation method of Y2O3 erosion-resistant ceramic coating - Google Patents
Preparation method of Y2O3 erosion-resistant ceramic coating Download PDFInfo
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- CN103074568A CN103074568A CN2011103285396A CN201110328539A CN103074568A CN 103074568 A CN103074568 A CN 103074568A CN 2011103285396 A CN2011103285396 A CN 2011103285396A CN 201110328539 A CN201110328539 A CN 201110328539A CN 103074568 A CN103074568 A CN 103074568A
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Abstract
The invention relates to the technical field of atmospheric plasma spraying, and specifically relates to a preparation method of an Y2O3 erosion-resistant ceramic coating. The preparation method comprises the steps that: step (1), Y2O3 powder with purity higher than 99.95% is selected; step (2), the surface of a substrate requiring spraying is pretreated; and step (3) Ar and He gases are selected as ion gases, and plasma spraying is carried out upon the surface of the substrate by using a plasma spraying device, such that an Y2O3 coating is prepared. With the method provided by the invention, the prepared Y2O3 coating has a pure white color, uniform color, no noise or speckle, and excellent etching-resistance.
Description
Technical field
The present invention relates to the atmospheric plasma spraying technology field, be specifically related to a kind of Y
2O
3The preparation method of the ceramic coating of anti-the erosion.
Background technology
At present, the low-temperature plasma fine machining method is the gordian technique of material micro-nano processing, it is the basis of the technologies of preparing such as microelectronics, photoelectron, micromechanics, micro-optic, particularly in the super large-scale integration manufacturing process, there is nearly 1/3rd operation to finish by means of plasma process, such as plasma foil deposition, plasma etching and removing of photoresist by plasma etc.Wherein plasma etching is one of technical process of most critical, is to realize that the Micropicture of super large-scale integration in producing with high fidelity transfer to irreplaceable technique on the silicon chip from Lithographic template.
In etching process since exist a large amount of living radicals with severe corrosive (such as Cl*, Cl
2*, F*, CF* etc.), the internal surface in their article on plasma etching technics chambeies also can produce corrosive nature, causes pollution, affects etching effect, and is lost efficacy in the etching technics chamber.The plasma etching equipment of the early stage nineties is in the situation that smaller power and single plasma-generating source add Al at the aluminum substrate layer
2O
3Coating just can satisfy plasma body to the etch damage in etching technics chamber.Enter into 300mm equipment, along with plasma power is increasing, plasma body is also increasing to the damage of etching technics chamber wall, so that in the process of etching following problem occurs easily: (1) particle; (2) process cavity wall disbonding causes plasma body directly and aluminum substrate is had an effect; (3) Al
2O
3The life-span of component is subject to more high-power restriction.So need to seek a kind of new approach the etching technics inner cavity surface is carried out modification, satisfy the needs of etching technics.
Studies show that Y
2O
3Coating has good provide protection to the etching technics chamber.With Al
2O
3Compare Y
2O
3Chemical property highly stable, have excellent anti-plasma etching performance, and and CF be the reaction product YF that gas generates
3Steam forces down, and is difficult to disperse as particle.With Y
2O
3Powder utilizes the air plasma spraying method as spray material, prepares the Y of single structure at the etching technics inner cavity surface
2O
3Coating can effectively solve above-mentioned Al
2O
3The variety of issue that coating faces.
Air plasma spraying is to use N
2, Ar, H
2And He etc. produces plasma high temperature and high speed jet as ion-gas through ionization, and input material fusing or melting are ejected into the method that working-surface forms coating.Plasma arc extreme temperatures wherein, enough thawing comprises Y
2O
3At interior all high-melting-point ceramic powder; Melted powder kinetic energy in the jet is large, with can fully launch behind the substrate contact, stacked, the Effective Raise anchoring strength of coating reduces porosity.It is the gordian technique of preparation high-performance, high quality ceramic coating.
In the plasma spray coating process, atmosphere surrounding can have on the final performance of coating significantly impact.The selection principle of gas mainly is to consider practicality and economy.Concrete requirement is: (1) stable performance, not with spray material generation adverse reaction; (2) heat content is high, is suitable for refractory material, but does not answer too high and the ablation nozzle; (3) should selection and electrode or nozzle the gas of chemical action does not occur; (4) with low cost, supply is convenient.Plasma spraying gas commonly used mainly contains N
2, Ar, H
2With He etc.
N
2Be diatomic gas, therefore the heat enthalpy value of plasma flame flow is higher, be conducive to the heating and melting of powder, higher ionization potential (15.8V) is arranged again, so the utilising efficiency of heat is high.The while wide material sources, therefore low price is the most frequently used working gas in the plasma spraying.Its shortcoming is easy under the high temperature and powdered reaction, and the protection effect is relatively poor.Ar is monoatomic gas, directly absorbs heat in the ionization that heats up and ionizes, and heats up very fast, does not react with any powder simultaneously, and protective value is good.But its arc voltage is lower, and thermal conductivity is little, use seldom separately, and expensive, originate less.He also is monoatomic gas, ionization voltage 24.5V, and heat enthalpy value is high, and viscosity is high, and a certain amount of He is stable arc effectively.H
2Ionization potential is low, has the highest thermal conductivity, helps powder smelting.Metallic substance there is very strong reductibility, can prevents oxidation.In addition, in Ar, count a small amount of H
2, voltage and the power of energy Effective Raise plasma arcs.
Y in reality
2O
3In the plasma spray coating process, if adopt wide material sources, traditional Ar/H
2As ionized gas, often can cause Y
2O
3Inhomogeneous black splotch appears in coating in the part.This is because H
2Reduction characteristic, in spraying process with Y
2O
3Reduction reaction has occured in powder, and the Y of anoxic condition
2O
3Powder can present black.
Summary of the invention
The object of the present invention is to provide a kind of Y
2O
3The preparation method of the ceramic coating of anti-the erosion can prepare at the plasma etching industrial inner cavity surface Y of excellent performance
2O
3Coating.
In order to achieve the above object, the technical solution used in the present invention is:
A kind of Y
2O
3The preparation method of the ceramic coating of anti-the erosion comprises the steps:
Step (1) selects purity greater than 99.95% Y
2O
3Powder;
Step (2) is carried out pre-treatment to the substrate surface that is sprayed;
Step (3), selecting Ar and He gas is ionized gas, carries out plasma spraying by plasma-spraying device at described substrate surface, prepares Y
2O
3Coating.
In the such scheme, the Y in the described step (1)
2O
3The granularity of powder is 5～50 μ m.
In the such scheme, in the described step (2) substrate surface that is sprayed is carried out pre-treatment, specifically comprise the steps: the substrate surface that is sprayed is carried out sandblasting, and clean with acetone.
In the such scheme, the sand-blast material that described sandblasting is adopted is white fused alumina, and sand size is 50～100 μ m.
In the such scheme, the flow of Ar gas is 40～90L/min in the described step (3), and the flow of He gas is 2～10L/min.
In the such scheme, the arc voltage of described step (3) applying plasma spraying equipment is 40～50V, and flame current is 800～900A, and powder feed rate is 15～100g/min, and spray distance is 80～135mm, and the powder feeding angle is 50
~ 90
In the such scheme, in the process of described step (3) ionic medium spraying, adopt air blowing method or recirculated water cooling method to cool off the described base material that is sprayed, the flow of cooling gas is 100～2000L/min in the described air blowing method, and the flow of water coolant is 10～500L/min in the described recirculated water cooling method.
Compare with the prior art scheme, the beneficial effect that the technical solution used in the present invention produces is as follows:
Use the Y of the present invention's preparation
2O
3Coating is pure white, and color and luster is even, variegated spot no longer occurs, and has excellent etch resistance energy.
Description of drawings
Fig. 1 is the Y that has the Emission in Cubic structure in the embodiment of the invention
2O
3The XRD figure spectrum of powder;
Fig. 2 is Y in the embodiment of the invention
2O
3The scanning electron microscope shape appearance figure of powder;
Fig. 3 is the Y that has the Emission in Cubic structure in the embodiment of the invention
2O
3The XRD figure spectrum of coating;
Fig. 4 is Y in the embodiment of the invention
2O
3The scanning electron microscope shape appearance figure of coating;
Fig. 5 is Y in the embodiment of the invention
2O
3The Cross Section Morphology figure of coating;
Fig. 6 is at Ar and H in the embodiment of the invention
2The Y for preparing under the condition
2O
3The coatingsurface photo;
Fig. 7 is the Y for preparing under Ar and He condition in the embodiment of the invention
2O
3The coatingsurface photo.
Embodiment
Below in conjunction with drawings and Examples technical solution of the present invention is described in detail.
The embodiment of the invention provides a kind of Y
2O
3The preparation method of the ceramic coating of anti-the erosion specifically comprises the steps:
(1) selects Y
2O
3Powder, size range are 5～50 μ m, and powder should have single Emission in Cubic structure, Y
2O
3The XRD figure spectrum of powder as shown in Figure 1; The initial size of powder is 40～60nm, and particle diameter is for being 5～50 μ m behind the secondary granulation, and as shown in Figure 2, the macrobead powder after the granulation is the sphere of vesicular structure, is the hollow micron bead that is assembled into by the nanometer small-particle, has splendid flowability;
The etching technics cavity wall of the aluminium base that (2) needs is sprayed carries out sandblasting, and sand-blast material is white fused alumina, and size range is 50～100 μ m, and cleans with acetone;
(3) adopt Sluzer Metco 9MC plasma spraying equipment to carry out plasma spraying, the spray gun type is 9MB; Spray under Ar and He atmosphere surrounding, the flow of Ar gas is that the flow of 40～90L/min, He gas is 2～10L/min; The arc voltage of plasma spraying equipment is 40 ~ 50V, and flame current is 800～900A, and powder feed rate is 15～100g/min, and spray distance is 80～135mm, powder feeding angle 50
～90
In spraying process, adopt air blowing method or recirculated water cooling method to cool off the base material that is sprayed, the flow of the cooling gas of air blowing method is 100～2000L/min, the flow of the water coolant of recirculated water cooling method is 10～500L/min.
The phase of powder and coating forms utilizes X ' pert PHILIPS X-ray diffractometer to measure and analyze.Fig. 3 is prepared Y
2O
3The XRD figure spectrum of coating can find out that coating presents single Emission in Cubic structure, and is useful to the anti-plasma etching of coating.Prepared coating pattern is observed with Cambridge S-360 type scanning electronic microscope, Fig. 4 is the surface topography of coating, can find out from photo, its surface mainly presents spherical, macrobead is arranged, also have small-particle, regional area to present the fused junction crystalline state, coatingsurface does not have crackle, is combined closely with aluminum substrate.Coating porosity is measured by metallographic method, and Fig. 5 is the metallograph that is coated with layer cross section, and visible coating is combined with base material and is mechanical chimerism, helps to improve the bonding force between coating and the base material.
If at Ar and H
2Prepare Y under the condition
2O
3Coating, Ar flow are 40～90L/min, H
2Flow is 5～20L/min, and other processing parameters of plasma spraying equipment are same as described above, the Y of preparation gained
2O
3The coatingsurface photo presents the black splotch of uneven distribution as shown in Figure 6.Use the method for the invention, the Y that under Ar and He environment, prepares
2O
3The coatingsurface photo as shown in Figure 7, the surface be white, color and luster is even, black splotch do not occur.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. Y
2O
3The preparation method of the ceramic coating of anti-the erosion is characterized in that, comprises the steps:
Step (1) selects purity greater than 99.95% Y
2O
3Powder;
Step (2) is carried out pre-treatment to the substrate surface that is sprayed;
Step (3), selecting Ar and He gas is ionized gas, carries out plasma spraying by plasma-spraying device at described substrate surface, prepares Y
2O
3Coating.
2. Y as claimed in claim 1
2O
3The preparation method of the ceramic coating of anti-the erosion is characterized in that, the Y in the described step (1)
2O
3The granularity of powder is 5～50 μ m.
3. Y as claimed in claim 1
2O
3The preparation method of the ceramic coating of anti-the erosion is characterized in that, in the described step (2) substrate surface that is sprayed is carried out pre-treatment, specifically comprises the steps: the substrate surface that is sprayed is carried out sandblasting, and cleans with acetone.
4. Y as claimed in claim 1
2O
3The preparation method of the ceramic coating of anti-the erosion is characterized in that, the sand-blast material that described sandblasting is adopted is white fused alumina, and sand size is 50～100 μ m.
5. Y as claimed in claim 1
2O
3The preparation method of the ceramic coating of anti-the erosion is characterized in that, the flow of Ar gas is 40～90L/min in the described step (3), and the flow of He gas is 2～10L/min.
6. Y as claimed in claim 1
2O
3The preparation method of the ceramic coating of anti-the erosion is characterized in that, the arc voltage of described step (3) applying plasma spraying equipment is 40～50V, flame current is 800～900A, powder feed rate is 15～100g/min, and spray distance is 80～135mm, and the powder feeding angle is 50
~ 90
7. Y as claimed in claim 1
2O
3The preparation method of the ceramic coating of anti-the erosion, it is characterized in that, in the process of described step (3) ionic medium spraying, adopt air blowing method or recirculated water cooling method to cool off the described base material that is sprayed, the flow of cooling gas is 100～2000L/min in the described air blowing method, and the flow of water coolant is 10～500L/min in the described recirculated water cooling method.
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|---|---|---|---|
| CN2011103285396A CN103074568A (en) | 2011-10-26 | 2011-10-26 | Preparation method of Y2O3 erosion-resistant ceramic coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103285396A CN103074568A (en) | 2011-10-26 | 2011-10-26 | Preparation method of Y2O3 erosion-resistant ceramic coating |
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| CN103074568A true CN103074568A (en) | 2013-05-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609888A (en) * | 2018-11-29 | 2019-04-12 | 沈阳富创精密设备有限公司 | A kind of plasma spray coating yttria coating preparation method for preventing boundary from falling off |
| WO2022228308A1 (en) * | 2021-04-26 | 2022-11-03 | 洛阳理工学院 | Method for preparing low-exudation electro-fused zirconia-corundum brick with added yttrium oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5277936A (en) * | 1987-11-19 | 1994-01-11 | United Technologies Corporation | Oxide containing MCrAlY-type overlay coatings |
| TW200925323A (en) * | 2007-12-06 | 2009-06-16 | Tocalo Co Ltd | Method of forming black yttrium oxide sprayed coating and member provided with black yttrium oxide sprayed coating |
-
2011
- 2011-10-26 CN CN2011103285396A patent/CN103074568A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5277936A (en) * | 1987-11-19 | 1994-01-11 | United Technologies Corporation | Oxide containing MCrAlY-type overlay coatings |
| TW200925323A (en) * | 2007-12-06 | 2009-06-16 | Tocalo Co Ltd | Method of forming black yttrium oxide sprayed coating and member provided with black yttrium oxide sprayed coating |
Non-Patent Citations (1)
| Title |
|---|
| 刘邦武等: "等离子喷涂氧化钇涂层的组织结构", 《金属热处理》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609888A (en) * | 2018-11-29 | 2019-04-12 | 沈阳富创精密设备有限公司 | A kind of plasma spray coating yttria coating preparation method for preventing boundary from falling off |
| WO2022228308A1 (en) * | 2021-04-26 | 2022-11-03 | 洛阳理工学院 | Method for preparing low-exudation electro-fused zirconia-corundum brick with added yttrium oxide |
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Application publication date: 20130501 |
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