CN106048502A - Nano YAG coating layer, and preparation method and application of nano YAG coating layer - Google Patents
Nano YAG coating layer, and preparation method and application of nano YAG coating layer Download PDFInfo
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- CN106048502A CN106048502A CN201610397863.6A CN201610397863A CN106048502A CN 106048502 A CN106048502 A CN 106048502A CN 201610397863 A CN201610397863 A CN 201610397863A CN 106048502 A CN106048502 A CN 106048502A
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Abstract
The invention discloses a nano YAG coating layer, and a preparation method and an application of the nano YAG coating layer. The preparation method comprises the steps that suspending liquid containing Al2O3 particles and Y2O3 particles that are evenly dispersed is provided; and the suspending liquid is sprayed on a matrix by a plasma spraying technology, and a Y3Al5O12 coating layer, namely the nano YAG coating layer, is formed. The nano YAG coating layer is high in density and excellent in plasma erosion resistance, and is applicable to various matrixes. The preparation method of the nano YAG coating layer requires no pelleting link, and is simple and easy to operate and high in production efficiency; the usage amount of high-cost Y2O3 can be reduced without degrading the plasma erosion resistance of the nano YAG coating layer; the production cost is low; and the preparation method is suitable for large-scale implementation.
Description
Technical field
The present invention relates to a kind of ceramic coating, particularly to a kind of nanometer YAG coating, its preparation method and application, described
YAG coating can resist plasma erosion, and has high-compactness.
Background technology
Along with the development of electronics industry, dry etch process serves the most important effect.Add in all of dry method
In work technology, plasma etching technology is most widely used, and is also the technology that micro-nano working ability is the strongest.In recent years,
The utilization of electronics industry large scale semiconductor equipment so that the power of plasma etching is the most increasing, cause etchant gas (as
CF4, SF6, O2, Cl2, Ar) and the plasma damage increase to etching technics cavity wall.Prior art uses anodised aluminium
Or aluminum oxide coating layer can not meet high-power under the conditions of protective effect to etching technics cavity wall, make plasma directly with
The problems such as aluminum substrate is had an effect, and produces particle contamination, technique cavity wall disbonding.It is, thus, sought for a kind of new coating,
To meet the requirement of high-power etching technics.
In plasma etch process, there is chemically active plasma and be typically by chlorine or carbon fluorine gas discharge
Producing, they contain electronics and ion and substantial amounts of living radical, and these materials corrode chamber when etching apparatus internal chamber wall
Wall.Accordingly, it would be desirable to deposit one layer of protective coating on inwall, to prevent in use aggressive ion and ion pair cavity wall
Infringement.The nineties in 20th century is industrial generally with anodic alumina films or Al2O3Coating protects etching apparatus cavity inner wall,
Being used for stoping the plasma etch damage to etching technics cavity wall, but plasma etching equipment power is less, plasma is sent out
Source of students is single.In recent years, along with the development of industrial technology, in order to improve the etching efficiency of large-sized silicon wafers, reduce production cost,
Increase the power of plasma generator, cause plasma gas more serious to the erosion of etching apparatus internal chamber wall.High-strength
Degree plasma erosion can produce substantial amounts of little granule, pollutes etching apparatus and sample surfaces, the frequency of the maintenance that increases manufacturing facilities
And the small particles of pollution sample of erosion remaining years, thus reduce the qualification rate of product, seeing Fig. 1 is product during plasma etching
The photo of raw little granule institute contaminated samples.
Simultaneously as equipment size is relatively big, and interior wall construction is mostly irregular shape, and prior art is typically with sintering
Block materials, it is adaptable to small-size equipment.In large scale field, typically use plasma spraying technology, but conventional plasma sprays
Coating consistency prepared by painting technology is relatively low, in the face of the large scale of current industrial circle, and high power plasma etching equipment,
It is difficult to meet requirement.Other thin film or coat preparing technology, preparation efficiency is all difficult to meet heavy industrialization demand.Existing
High-purity Y that in technology, development of novel goes out2O3, although its plasma resistant erosion performance is preferable, but high-purity compact Y2O3Coating preparation and
Its difficulty, and high-purity Y2O3Price is the highest, and large-scale commercial use cost is high.Therefore, current semi-conductor industry is badly in need of a kind of high-quality
The plasma resistant erosion material of amount stops high powered plasma to etch the erosion for etching apparatus, thus improves production efficiency
And conforming product rate, reduce production cost.
Conventional coatings has encountered bottleneck in terms of promoting coating physical property and mechanical property, and existing spraying method is very
The difficult microstructure improving coating.Due to the development of nanotechnology, sight has been turned to nano coating by people.Nano coating refers to
Be that the crystallite dimension in coating is generally less than 100nm, this coating has more more preferable microstructure than conventional coatings, thus more
Be conducive to improving the properties of coating.Traditional agglomerate type powder preparing nano coating by plasma spraying, although raw material is for receiving
Rice flour end, due to features such as powder size is little, quality is little, poor fluidities, is not suitable for directly as spraying raw material, it is necessary to through overspray
Mist is dried and sintering densification balling-up, makes quality Conglobation type micron powder slightly larger, good fluidity and just can carry out plasma spray
It is coated with preparation coating.The operation that experience is so complicated, not only the loss of material is relatively big, and be sintered densification balling-up and etc.
During plasma spray, owing to temperature is higher, nanocrystal has the trend grown up, and even can exceed nanometer critical dimensions.Therefore,
Even if raw material is preferable nanometer powder, experiencing such process, obtained coating structure differs and is set to nano crystal structure,
The nanostructured performance ultimately resulting in coating vanishes, and affects nano coating physical property and mechanical property.
Summary of the invention
Present invention is primarily targeted at a kind of nanometer YAG coating of offer, its preparation method and application, to overcome existing skill
Deficiency in art.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes:
Embodiments provide the preparation method of a kind of nanometer YAG coating, comprising:
There is provided containing homodisperse Al2O3Granule and Y2O3The suspension of granule；
Described suspension is sprayed to be formed on matrix Y with plasma spray coating process3Al5O12Coating, the most described nanometer YAG
Coating.
Further, described preparation method includes: directly inputs in plasma flame by described suspension, sprays to afterwards
On matrix, form described nanometer YAG coating.
The embodiment of the present invention additionally provides the nanometer YAG coating prepared by any one method aforementioned.
The embodiment of the present invention additionally provides the purposes of any one nanometer YAG coating aforementioned.
Compared with prior art, the invention have the advantages that
(1) the nanometer YAG coating consistency provided is high, and plasma resistant erosion performance is excellent, and being suitable to should on various matrixes
With；
(2) preparation method of the nanometer YAG coating provided is without links such as pelletizes, and technique is simple, and production efficiency is high, and
Expensive Y can be reduced on the premise of not reducing coating plasma resistant erosion performance2O3Consumption, production cost is low.
Accompanying drawing explanation
Fig. 1 is the photo of the little granule institute contaminated samples produced during plasma etching in prior art；
Fig. 2 is the XRD figure spectrum of the coating using plasma spraying to be formed in the present invention one exemplary embodiments；
Fig. 3 is that the cross section microstructure of the coating using plasma spraying to be formed in the present invention one exemplary embodiments is shone
Sheet；
Fig. 4 a-Fig. 4 b is that the coating using plasma spraying to be formed in the present invention one exemplary embodiments is at erosion power
Stereoscan photograph before and after corroding during 400W.
Detailed description of the invention
In view of deficiency of the prior art, inventor, through studying for a long period of time and putting into practice in a large number, is proposed the present invention's
Technical scheme.This technical scheme, its implementation process and principle etc. will be further explained as follows.
The preparation method of a kind of nanometer YAG coating that the embodiment of the present invention provides includes:
There is provided containing homodisperse Al2O3Granule and Y2O3The suspension of granule；
Described suspension is sprayed on matrix with plasma spray coating process, forms Y3Al5O12Coating, the most described nanometer
YAG coating.
More preferred, described Al2O3Granule, Y2O3The particle diameter of granule is 5～100 nanometers, and purity is more than 99.5%.
More preferred, described Al2O3The consumption of granule is described Al2O3Granule and Y2O3The total consumption of granule
More than 62.5mol%.
More preferred, described suspension comprises 5～30wt%Al2O3Granule and Y2O3Granule solid thing.
More preferred, described suspension comprises anionic dispersing agents, such as DOLAPIX PC 75 or DOLAPIX PC
64, but it is not limited to this.
More preferred, the solvent used in described suspension includes deionized water, ethanol etc., and is not limited to this.
More preferred, the pH value of described suspension is 4～6.9.
In some embodiments, described preparation method includes: directly input in plasma flame by described suspension,
Spray to afterwards on matrix, form described nanometer YAG coating.
More preferred, the process conditions used in described plasma spray coating process include: playing arc gas is argon, flow
Being 28～60L/min, auxiliary gas is H2, flow is 3～30L/min, and suspension transfer rate is 5～40ml/min, atomization gas
Using argon, flow is 6～32L/min.
Further, in described plasma spray coating process, the suspension time of staying in plasma torch is by plasma
The control of flame speed, it is preferred that in suspension the gait of march of the powder particle of solvent remaining after evaporation control 150～
400m/s。
Wherein, the temperature of described plasma flame is typically more than 10000～15000 DEG C.
Wherein, described plasma flame is usually the plasma formed after Ar gas ionizes under high frequency voltage.
Further, the present invention should meet following requirement in order to forming the gas of plasma: (1) stable performance, no
With sprayed on material generation adverse reaction；(2) heat content is high, is suitable for refractory material, but should too high and ablation nozzle；(3) should
Chemical action is there is not with electrode or nozzle；(4) with low cost, supply is convenient.
The plasma used in the aforementioned preparation process of the present invention preferably employs atmosphere plasma and (derives from N2、Ar、
H2And He etc.), i.e. using air plasma spraying, it uses gas to produce plasma high temperature and high speed jet through ionization, will input
Melt material or the melted working surface that is ejected into form coating.Plasma-arc extreme temperatures therein, enough melts and includes
Al2O3, Y2O3At interior all of high-melting-point ceramic powders.
More preferred, the spray distance used in described plasma spray coating process is 40～100mm.
In some embodiments, described substrate is selected from metallic substrates.
In some embodiments, described preparation method includes: after substrate surface carries out sandblasting, cleaning process, then
Described nanometer YAG coating is formed in the spraying of described substrate surface.
By by Al in the aforementioned preparation process of the present invention2O3、Y2O3Well disperse in a liquid Deng nano-particle, so
After stable suspension is sent into plasma flame center as plasma spraying feeding, both improved nanometer powder spraying such as
The problem of mobility, and this process is carried out in plasma flame stream, and the time of experience is extremely short, the nanocrystal in powder
Have little time to grow up and be deposited upon on matrix, therefore can form nano-structured coating, coating consistency is greatly improved, enhances
The plasma resistant erosion performance of coating.
And, the aforementioned preparation process of the present invention is directly synthesized Al by the method for suspending liquid plasma spraying2O3/
Y2O3Composite oxide coating, it is to avoid the pelletize link of conventional plasma spraying, before not reducing coating plasma erosion performance
Put and reduce expensive Y2O3Consumption, improves production efficiency, reduces production cost.
In the aforementioned preparation process of the present invention, nanometer Al2O3And Y2O3Powder is according to following reaction in plasma torch
Synthesize Y3Al5O12Coating:
2Y2O3+Al2O3→Y4Al2O9；(900-1000℃)
Y4Al2O9+Al2O3→3YAlO3；(1100-1250℃)
4YAlO3+Al2O3→Y3Al5O12；(1400-1600℃)
The embodiment of the present invention additionally provides the nanometer YAG coating prepared by any one method aforementioned.
Further, described nanometer YAG coating is mainly by Y3Al5O12Nanocrystal assembles formation, described nanocrystal
A size of 20-80nm.Additionally, described nanometer YAG coating also can comprise unreacted Al completely2O3、Y2O3、Y4Al2O9And YAlO3
Composite oxides etc., but main with Y3Al5O12, i.e. YAG is main.
Further, the thickness of described nanometer YAG coating is more than 0.3 μm, and porosity is less than 10%, Vickers hardness
HV0.2>700。
The embodiment of the present invention additionally provides a kind of device, and it comprises: matrix, and be formed at described matrix surface, as
Any one nanometer YAG coating described in before.
Below in conjunction with embodiment and accompanying drawing, the technology of the present invention is further explained.
Embodiment 1
(1) preparation of suspension
Selecting grain size is 5-100 nanometer, the purity Al more than 99.5%2O3And Y2O3Powder, according to Al2O3: Y2O3For
After the ratio of 5:3 weighs, adding pH value=4～the deionized water of 6.9, and be stirred continuously, control suspension concentration is 5-
30wt.%, adds appropriate anionic dispersing agents afterwards, adds the 0.5-3wt% that concentration is suspension solids content, and ultrasonic
Dispersion 10-120min, obtains the Al of stable uniform2O3/Y2O3Suspension.
(2) preparation of coating
First metallic substrates is carried out before spraying blasting treatment (such as by SiC or Al2O3Sand carries out sandblasting, spray
Fineness of sand is 50～100 μm), then clean substrate surface with ethanol or acetone, standby after drying.By the suspension of stable uniform
It is transported in Ar plasma torch by peristaltic pump pipeline, then sprays to prepare on metallic matrix Y3Al5O12Coating.Wherein spray
During to play arc gas be argon, flow is 28～60L/min, and auxiliary gas is H2, flow is 3-30L/min, suspension conveying speed
Rate is 5～40ml/min, and atomization gas uses argon, and atomization air flow is 6-32L/min, and spray distance is 40-100mm.
The porosity of a kind of typical coating sample prepared by the present embodiment is less than 10%, vickers hardness hv 0.2 > 700, its
XRD figure is composed as in figure 2 it is shown, pattern see Fig. 3, and the pattern before and after corroding when corroding power and being 400W see Fig. 4 a-figure
4b。
Additionally, inventor also to the present embodiment prepare other coating sample carried out standard testing, its result with
The test result of this typical coating is basically identical.
Should be appreciated that above-described embodiment is only technology design and the feature of the explanation present invention, its object is to allow and be familiar with this
The personage of item technology will appreciate that present disclosure and implements according to this, can not limit the scope of the invention with this.All
The equivalence change made according to spirit of the invention or modification, all should contain within protection scope of the present invention.
Claims (10)
1. the preparation method of a nanometer YAG coating, it is characterised in that including:
There is provided containing homodisperse Al2O3Granule and Y2O3The suspension of granule；
Described suspension is sprayed to be formed on matrix Y with plasma spray coating process3Al5O12Coating, the most described nanometer YAG coating.
Preparation method the most according to claim 1, it is characterised in that:
Described Al2O3Granule or Y2O3The particle diameter of granule is 5～100 nanometers, and purity is more than 99.5%；
And/or, described Al2O3The consumption of granule is described Al2O3Granule and Y2O3More than the 62.5mol% of the total consumption of granule；
And/or, described suspension comprises 5～30wt%Al2O3Granule and Y2O3Granule solid thing.
Preparation method the most according to claim 1, it is characterised in that: described suspension comprises anionic dispersing agents；With/
Or, the solvent used in described suspension includes water and/or ethanol；And/or, the pH value of described suspension is 4～6.9；With/
Or, in described suspension, the content of anionic dispersing agents is described suspension the 0.5～3wt% of solids content.
Preparation method the most according to claim 1, it is characterised in that including: described suspension is inputted plasma continuously
In flame, spray to afterwards on matrix, form described nanometer YAG coating.
Preparation method the most according to claim 1, it is characterised in that the technique bar used in described plasma spray coating process
Part includes: playing arc gas is argon, and flow is 28-60L/min, and auxiliary gas is H2, flow is 3-30L/min, suspension conveying speed
Rate is 5～40ml/min, and atomization gas uses argon, and flow is 6～32L/min；And/or, in described plasma spray coating process
The spray distance used is 40～100mm；And/or, in described plasma spray coating process, suspension is steamed in plasma torch
The gait of march sending out powder particle remaining after removing solvent is 150-400m/s.
Preparation method the most according to claim 1, it is characterised in that including: substrate surface carries out sandblasting, cleaning processes
After, then form described nanometer YAG coating in the spraying of described substrate surface；And/or, described substrate is selected from metallic substrates.
7. the nanometer YAG coating prepared by method according to any one of claim 1-6.
Nanometer YAG coating the most according to claim 7, it is characterised in that: described nanometer YAG coating is mainly by Y3Al5O12Receive
Formation assembled by rice crystal grain, and the size of described nanocrystal is 20～100nm.
Nanometer YAG coating the most according to claim 7, it is characterised in that: the thickness of described nanometer YAG coating is in 0.3 μm
Above, porosity is less than 10%, vickers hardness hv 0.2 > 700.
10. a device, it is characterised in that comprise: matrix, and be formed at described matrix surface, as in claim 7-9
Nanometer YAG coating described in any one.
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Cited By (6)
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| CN110218965A (en) * | 2019-05-28 | 2019-09-10 | 沈阳富创精密设备有限公司 | A kind of preparation method of advanced ceramics layer |
| CN110331362A (en) * | 2019-08-21 | 2019-10-15 | 重庆臻宝实业有限公司 | The composite coating and preparation method of resisting plasma corrosion |
| CN110629216A (en) * | 2019-09-11 | 2019-12-31 | 武汉市赟巨科技有限公司 | Preparation method of steel plate heat radiation prevention coating |
| CN111763900A (en) * | 2020-06-12 | 2020-10-13 | 嘉兴市爵拓科技有限公司 | Mixture for hot work die coating and preparation method of hot work die coated with nano coating |
| CN112063956A (en) * | 2020-08-10 | 2020-12-11 | 暨南大学 | Suspension plasma spraying high-purity Y2O3Erosion-resistant coating and preparation method and application thereof |
| CN113584421A (en) * | 2021-08-05 | 2021-11-02 | 重庆臻宝实业有限公司 | Method for enhancing bonding strength of yttrium oxide coating and substrate surface |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110629216B (en) * | 2019-09-11 | 2022-04-26 | 武汉市赟巨科技有限公司 | Preparation method of steel plate heat radiation prevention coating |
| CN111763900A (en) * | 2020-06-12 | 2020-10-13 | 嘉兴市爵拓科技有限公司 | Mixture for hot work die coating and preparation method of hot work die coated with nano coating |
| CN112063956A (en) * | 2020-08-10 | 2020-12-11 | 暨南大学 | Suspension plasma spraying high-purity Y2O3Erosion-resistant coating and preparation method and application thereof |
| CN113584421A (en) * | 2021-08-05 | 2021-11-02 | 重庆臻宝实业有限公司 | Method for enhancing bonding strength of yttrium oxide coating and substrate surface |
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