CN103074562B - A kind of Y improving performance2o3the preparation method of resistant to corrosion ceramic coating - Google Patents
A kind of Y improving performance2o3the preparation method of resistant to corrosion ceramic coating Download PDFInfo
- Publication number
- CN103074562B CN103074562B CN201110328241.5A CN201110328241A CN103074562B CN 103074562 B CN103074562 B CN 103074562B CN 201110328241 A CN201110328241 A CN 201110328241A CN 103074562 B CN103074562 B CN 103074562B
- Authority
- CN
- China
- Prior art keywords
- plasma
- resistant
- preparation
- coating
- ceramic coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to atmospheric plasma spraying technology field, be specifically related to a kind of Y improving performance2O3The preparation method of resistant to corrosion ceramic coating.Described preparation method, comprises the steps: step (1), selects the purity Y more than 99.95%2O3Powder；Step (2), carries out pretreatment to the substrate surface being sprayed-on；Step (3), selects Ar and H2Gas is ionized gas, carries out plasma spraying by plasma-spraying device at described substrate surface, prepares Y2O3Coating；Step (4), will spray Y2O3The base material of coating is placed in plasma oxygen processing equipment, carries out plasma oxygen process.Use Y prepared by the present invention2O3Coating is pure white, uniform color, variegated speckle no longer occurs, and has the etch resistant performance of excellence.
Description
Technical field
The present invention relates to atmospheric plasma spraying technology field, be specifically related to a kind of Y improving performance2O3Resistant to corrosion pottery
The preparation method of coating.
Background technology
Currently, low temperature plasma fine machining method has become a key technology of material micro-nano processing, and it is micro-
The basis of the technologies of preparing such as electronics, photoelectron, micromechanics, micro-optic, particularly in super large-scale integration manufacturing process,
The operation having nearly 1/3rd is by mean of what plasma process completed, such as plasma foil deposition, plasma etching
And removing of photoresist by plasma etc..Wherein plasma etching is one of technological process of most critical, is to realize ultra-large integrated electricity
Micropicture during road produces with high fidelity transfers to the irreplaceable technique silicon chip from Lithographic template.
During plasma dry etch process, exist substantial amounts of there is severe corrosive living radical (as
Cl*,Cl2*, F*, CF* etc.), the inner surface in they meeting article on plasma etching technics chambeies produces corrosiveness, causes pollution, shadow
Ring etching effect, and etching technics chamber can be made to lose efficacy.The plasma etching equipment of the nineties in early days, at smaller power and list
In the case of one plasma-generating source, aluminum substrate layer adds Al2O3Coating just can meet plasma to etching technics chamber
Etch damage.Enter into 300mm equipment, along with plasma power is increasing, the plasma damage to etching technics cavity wall
Hinder the most increasing so that the process in etching is susceptible to series of problems: produce granule；Technique cavity wall disbonding, leads
Cause plasma directly to have an effect with aluminum substrate；Al2O3The life-span of parts is limited by more power.So needing to seek
Look for a kind of new approach that etching technics inner cavity surface is modified, meet the needs of etching technics.
Research shows, Y2O3Coating has good protective effect to etching technics chamber.With Al2O3Compare, Y2O3Chemistry
Character is highly stable, has the resistant to plasma etching performance of excellence, and and product YF of CF system gas generation3Vapour pressure
Low, it is difficult to disperse as granule.With Y2O3Powder, as sprayed on material, utilizes air plasma spraying method, in etching technics chamber
Inner surface prepares the Y of single structure2O3Coating, it is possible to effectively solve above-mentioned Al2O3The various problems that coating is faced.
Air plasma spraying is to use N2、Ar、H2And He etc. is as ion-gas, produces plasma high temperature and high speed through ionization and penetrates
Stream, by input material fusing or the melted method being ejected into working surface formation coating.Plasma-arc extreme temperatures therein,
Enough melt and include Y2O3At interior all of high-melting-point ceramic powders；Melted powder kinetic energy in jet is big, after substrate contact
Can be sufficiently spread out, stacking, be effectively improved anchoring strength of coating, reduce porosity.Prepare high-performance, high-quality ceramic coating
Key technology.
In plasma spray coating process, the final performance of coating can be had by gaseous environment to be affected significantly.The choosing of gas
Select principle and mainly consider practicality and economy.Concrete requirement is: (1) stable performance, does not occur harmful with sprayed on material
Reaction；(2) heat content is high, is suitable for refractory material, but should too high and ablation nozzle；(3) should select with electrode or nozzle not
There is the gas of chemical action；(4) with low cost, supply is convenient.Plasma spraying commonly uses gas mainly N2,Ar,H2And He
Deng.
N2Being diatomic gas, therefore the heat enthalpy value of plasma flame flow is higher, beneficially the heating of powder and fusing, have again relatively
High ionization potential (15.8V), therefore the utilization ratio of heat is high.Wide material sources simultaneously, low price, is therefore plasma spray
The most frequently used working gas in painting.Its shortcoming is easy under high temperature and powdered reaction, and protected effect is poor.Ar is monatomic gas
Body, directly absorbs heat in the ionization that heats up and ionizes, heat up quickly, do not react with any powder simultaneously, protective value
Good.But its arc voltage is relatively low, and heat conductivity is little, is seldom used alone, and expensive, originate less.He is also monatomic gas
Body, ionization voltage 24.5V, heat enthalpy value is high, and viscosity is high, and a certain amount of He can effectively stablize electric arc.H2Ionization potential is low, tool
There is the highest heat conductivity, contribute to powder smelting.Metal material is had the strongest reproducibility, is possible to prevent oxidation.Additionally,
Ar counts a small amount of H2, voltage and the power of plasma arcs can be effectively improved.
If using Ar/He as ionized gas, spraying effect is preferable, and coating performance is preferable.In view of He is expensive, examine
Consider to economic and practical, actual Y2O3Plasma spray coating process uses Ar/H2As ionized gas to reduce cost, but so
Often result in Y2O3There is uneven black splotch in local in coating, thus affects coating performance.This is due to H2In spraying
During with Y2O3Powder there occurs reduction reaction so that the Y of anaerobic condition2O3Powder presents black.Accordingly, it would be desirable to be aided with
Some new technological measures, to solve the problems referred to above.
Summary of the invention
It is an object of the invention to provide a kind of Y improving performance2O3The preparation method of resistant to corrosion ceramic coating, can wait
Ion etch process inner cavity surface prepares the Y of excellent performance2O3Coating.
In order to achieve the above object, the technical solution used in the present invention is:
A kind of Y improving performance2O3The preparation method of resistant to corrosion ceramic coating, comprises the steps:
Step (1), selects the purity Y more than 99.95%2O3Powder；
Step (2), carries out pretreatment to the substrate surface being sprayed-on；
Step (3), selects Ar and H2Gas is ionized gas, is entered at described substrate surface by plasma-spraying device
Row plasma spraying, prepares Y2O3Coating；
Step (4), will spray Y2O3The base material of coating is placed in plasma oxygen processing equipment, carries out plasma oxygen process.
Y in such scheme, in described step (1)2O3The granularity of powder is 5～50 μm.
In such scheme, described step carries out pretreatment to the substrate surface being sprayed-on in (2), specifically includes following step
Rapid: the substrate surface being sprayed-on to be carried out blasting treatment, and cleans with acetone.
In such scheme, the sand-blast material that described blasting treatment uses is white fused alumina, and sand size is 50～100 μm.
In such scheme, in described step (3), the flow of Ar gas is 40～90L/min, H2The flow of gas be 5～
20L/min。
In such scheme, the arc voltage of described step (3) plasma spraying equipment is 40～50V, arc current
Being 800～900A, powder feed rate is 15～100g/min, and spray distance is 80～135mm, and powder feeding angle is 50 ° ~ 90 °.
In such scheme, in described step (3) during plasma spraying, use air blowing method or recirculated water
Cooling method cool down described in the base material that is sprayed-on, the flow cooling down gas in described air blowing method is 100～2000L/
Min, the flow cooling down water in described recirculated water cooling method is 10～500L/min.
In such scheme, in described step (4), the running parameter of plasma oxygen processing equipment is: plasma oxygen processing equipment
The operating air pressure of chamber is 1Pa ~ 100Pa, and operating power is 50W ~ 500W, and the temperature of chamber substrate is 50 DEG C ~ 200 DEG C, etc.
Ion-oxygen oxidization time is 30min ~ 2h, and the flow of plasma oxygen is 50-300 mL/min.
In such scheme, in described step (4), the operating power of plasma oxygen processing equipment chamber is 100W ~ 150W, chamber
The temperature of room substrate is 50 DEG C ~ 100 DEG C, and plasma oxygen oxidization time is 30min ~ 1h, and the flow of plasma oxygen is 80-150
mL/min。
Compared with prior art, what the technical solution used in the present invention produced has the beneficial effect that:
Use Y prepared by the present invention2O3Coating is pure white, and uniform color variegated speckle no longer occurs, and has
Excellent etch resistant performance.
Accompanying drawing explanation
The Y that Fig. 1 provides for the embodiment of the present invention2O3The flow chart of the preparation method of resistant to corrosion ceramic coating.
Detailed description of the invention
With embodiment, technical solution of the present invention is described in detail below in conjunction with the accompanying drawings.
As it is shown in figure 1, the embodiment of the present invention provides a kind of Y improving performance2O3The preparation method of resistant to corrosion ceramic coating,
Specifically include following steps:
(1) Y is selected2O3Powder, particle size range is 5～50 μm, and powder should have single Emission in Cubic structure；Powder former
Beginning particle diameter is 40～60nm, and after secondary granulation, particle diameter is for for 5～50 μm, and the bulky grain powder after pelletize is the ball of loose structure
Shape, is the hollow micron bead being assembled into by the little granule of nanometer, has splendid mobility；
(2) the etching technics cavity wall needing the aluminium base being sprayed-on being carried out blasting treatment, sand-blast material is white fused alumina,
Particle size range is 50～100 μm, and cleans with acetone；
(3) using Sluzer Metco 9MC plasma spraying equipment to carry out plasma spraying, spray gun type is 9MB；?
Ar and H2Spraying under gaseous environment, the flow of Ar gas is 40～90L/min, H2The flow of gas is 5～20L/min；Deng
The arc voltage of plasma spray equipment is 40 ~ 50V, and arc current is 800～900A, and powder feed rate is 15～100g/min, spray
Being coated with distance is 80～135mm, powder feeding angle 50 °～90 °；In spraying process, use air blowing method or recirculated water cooling
Method cools down the base material being sprayed-on, and the flow of the cooling gas of air blowing method is 100～2000L/min, recirculated water cooling
The flow of the cooling water of method is 10～500L/min.
(4) base material after spraying is carried out plasma oxygen process: utilize relevant device, such as etching machine, ion implantation apparatus etc.,
Material is placed under plasma oxygen environment.As a example by RIE etching machine, technological parameter is as follows: in etching machine chamber, operating air pressure is
1Pa ~ 100Pa, operating power be 50W ~ 500W, preferably operating power be 100W ~ 150W be easily caused because power is excessive
The generation of plasma etching effect so that coating morphology is destroyed；In chamber, substrate temperature controls at 50 DEG C ~ 200 DEG C,
Preferably temperature is 50 DEG C ~ 100 DEG C, because temperature is too high is easily caused coating and matrix stripping；Plasma oxygen oxidization time is
30min ~ 2h, preferably oxidization time are 30min ~ 1h, and the time is obviously enhanced after being easily caused etching effect for a long time, makes painting break on the contrary
Fall into and increase；Plasma oxygen flow is that 50-300 mL/min, preferably flow are at 80-150 about mL/min.
The present invention is directed to Y2O3In the atmospheric plasma spraying method of coating, the Y prepared for spray gas with Ar/H22O3
Variegated speckle problem present in coating, proposes to utilize plasma oxygen processing method, allows material be under plasma oxygen atmosphere and make
Y2O3Anoxic Phase aoxidizes.Plasma is the 4th state of material, the gas i.e. ionized, and it presents the labile state highly excited.
Plasma is combined into by ion, electronics and unionized neutral particle collection, overall in neutral state of matter.Utilize additional
Electric field or high-frequency induction electric field make gaseous conduction be gas discharge, and gas discharge is the important means producing plasma.Utilize
Glow discharge produces plasma and has been widely used in various industrial occasions.Plasma chemistry activity is the highest, it is easy to reaction, suitable
Process in low-temperature surface.Plasma rich in active group react at coating surface so that holiday disappears, thus improves
The etch resistant performance of coating, obtains, at etching technics inner cavity surface, the Y that performance is the most excellent2O3Coating.The present invention is used to prepare
Y2O3Coating is pure white, uniform color, variegated speckle no longer occurs, and has the etch resistant performance of excellence.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (8)
1. the Y improving performance2O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that comprise the steps:
Step (1), selects the purity Y more than 99.95%2O3Powder；
Step (2), carries out pretreatment to the substrate surface being sprayed-on；
Step (3), selects Ar and H2Gas is ionized gas, is carried out at described substrate surface by plasma-spraying device
Plasma spray, prepares Y2O3Coating；
Step (4), will spray Y2O3The base material of coating is placed in plasma oxygen processing equipment, carries out plasma oxygen process；
In described step (4), the running parameter of plasma oxygen processing equipment is: the operating air pressure of plasma oxygen processing equipment chamber
For 1Pa～100Pa, operating power is 50W～500W, and the temperature of chamber substrate is 50 DEG C～200 DEG C, plasma oxygen oxidization time
For 30min～2h, the flow of plasma oxygen is 50-300mL/min.
2. the Y improving performance as claimed in claim 12O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
Y in step (1)2O3The granularity of powder is 5～50 μm.
3. the Y improving performance as claimed in claim 12O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
Step carries out pretreatment to the substrate surface being sprayed-on in (2), specifically includes following steps: carry out the substrate surface being sprayed-on
Blasting treatment, and clean with acetone.
4. the Y improving performance as claimed in claim 32O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
The sand-blast material that blasting treatment uses is white fused alumina, and sand size is 50～100 μm.
5. the Y improving performance as claimed in claim 12O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
In step (3), the flow of Ar gas is 40～90L/min, H2The flow of gas is 5～20L/min.
6. the Y improving performance as claimed in claim 12O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
The arc voltage of step (3) plasma spraying equipment is 40～50V, and arc current is 800～900A, and powder feed rate is 15
～100g/min, spray distance is 80～135mm, and powder feeding angle is 50 °～90 °.
7. the Y improving performance as claimed in claim 12O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
In step (3) during plasma spraying, use air blowing method or recirculated water cooling method cool down described in be sprayed-on
Base material, the flow cooling down gas in described air blowing method is 100～2000L/min, cold in described recirculated water cooling method
But the flow of water is 10～500L/min.
8. the Y improving performance as claimed in claim 12O3The preparation method of resistant to corrosion ceramic coating, it is characterised in that described
In step (4), the operating power of plasma oxygen processing equipment chamber is 100W～150W, and the temperature of chamber substrate is 50 DEG C～100
DEG C, plasma oxygen oxidization time is 30min, and the flow of plasma oxygen is 80-150mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110328241.5A CN103074562B (en) | 2011-10-26 | A kind of Y improving performance2o3the preparation method of resistant to corrosion ceramic coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110328241.5A CN103074562B (en) | 2011-10-26 | A kind of Y improving performance2o3the preparation method of resistant to corrosion ceramic coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103074562A CN103074562A (en) | 2013-05-01 |
| CN103074562B true CN103074562B (en) | 2016-12-14 |
Family
ID=
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1156130A1 (en) * | 1999-12-10 | 2001-11-21 | Tocalo Co. Ltd. | Plasma processing container internal member and production method therefor |
| WO2007013184A1 (en) * | 2005-07-29 | 2007-02-01 | Tocalo Co., Ltd. | Y2o3 thermal sprayed film coated member and process for producing the same |
| 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 |
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1156130A1 (en) * | 1999-12-10 | 2001-11-21 | Tocalo Co. Ltd. | Plasma processing container internal member and production method therefor |
| WO2007013184A1 (en) * | 2005-07-29 | 2007-02-01 | Tocalo Co., Ltd. | Y2o3 thermal sprayed film coated member and process for producing the same |
| 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 (2)
| Title |
|---|
| （Characterization of plasma-sprayed Y2O3 coating and investigation of its visual aspect change;Hyun-Kwang Seok 等;《Surface & Coatings Technology》;20110225;第205卷(第11期);第3341-3346页 * |
| 等离子喷涂氧化钇涂层的组织结构;刘邦武 等;《金属热处理》;20101031;第35卷(第10期);第16-18页 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103194715B (en) | Method for preparing amorphous Y3Al5O12 coating through atmospheric plasma spraying technology | |
| JP2009001891A (en) | Nozzle for cold spray, and cold spray device using nozzle for cold spray | |
| CN106048502B (en) | Nanometer YAG coating, preparation method and application | |
| CN103074566A (en) | Method for preparing Y3O3 coating by using supersonic plasma spraying technology | |
| CN103074563B (en) | A kind of Y2O3The improved method of resistant to corrosion ceramic coating | |
| CN102296263B (en) | Modification treatment method for inner surface of plasma etching process chamber | |
| CN110396002A (en) | A kind of preparation method of the high-temperature oxidation resistant non-oxidized substance of resistance to ablation base dense coating | |
| CN103194714B (en) | A kind of method of Plasma Spray Boron Carbide Coating | |
| US20100034979A1 (en) | Thermal spraying method and device | |
| CN114481003A (en) | Hot cathode spray gun, nano plasma spraying device and method | |
| CN103132007B (en) | A kind of low-voltage plasma spraying technology prepares Y 2o 3the method of ceramic coating | |
| CN110004393A (en) | A kind of supersonic flame spraying technology preparation Y2O3The method of ceramic coating | |
| CN103074562B (en) | A kind of Y improving performance2o3the preparation method of resistant to corrosion ceramic coating | |
| CN103132002B (en) | Preparation method of black yttrium oxide (Y2O3) ceramic coating | |
| CN103132003B (en) | Black Y in a kind of semiconductor devices 2o 3ceramic coating manufacture method | |
| CN103132001B (en) | Improvement method for preparing Y2O3 ceramic coating | |
| CN112647037A (en) | Four-cathode plasma spraying spray gun device | |
| CN103074568A (en) | Preparation method of Y2O3 erosion-resistant ceramic coating | |
| CN103540889A (en) | Method for preparing boron carbide coating through low-pressure plasma spraying technology | |
| CN105624602B (en) | A kind of Y applied to aluminium base base material3Al5O12The preparation method of coating | |
| CN103074562A (en) | Preparation method of performance-improved Y2O3 erosion-resistant ceramic coating | |
| CN103074564A (en) | Method for preparing Y3O3 coating by using vacuum plasma spraying technology | |
| CN103074567A (en) | Method for preparing Y3O3 coating by using water-stable plasma spraying technology | |
| CN104711503A (en) | Boron carbide gradient coating used in quartz substrate and preparation method thereof | |
| CN114059024A (en) | Spray gun for plasma physical vapor deposition and thermal barrier coating preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201215 Address after: 510000 601, building a, 136 Kaiyuan Avenue, Huangpu District, Guangzhou City, Guangdong Province Patentee after: AoXin integrated circuit technology (Guangdong) Co.,Ltd. Address before: 100029 Beijing city Chaoyang District Beitucheng West Road No. 3 Patentee before: Institute of Microelectronics, Chinese Academy of Sciences |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20220425 Address after: 510000 room 710, Jianshe building, No. 348, Kaifa Avenue, Huangpu District, Guangzhou, Guangdong Patentee after: Ruili flat core Microelectronics (Guangzhou) Co.,Ltd. Address before: 510000 601, building a, 136 Kaiyuan Avenue, Huangpu District, Guangzhou City, Guangdong Province Patentee before: AoXin integrated circuit technology (Guangdong) Co.,Ltd. |