CN105492400B - Thermally treated ceramic substrate with ceramic coating and for coated ceramic heat treatment method - Google Patents
Thermally treated ceramic substrate with ceramic coating and for coated ceramic heat treatment method Download PDFInfo
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- CN105492400B CN105492400B CN201380010899.9A CN201380010899A CN105492400B CN 105492400 B CN105492400 B CN 105492400B CN 201380010899 A CN201380010899 A CN 201380010899A CN 105492400 B CN105492400 B CN 105492400B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 242
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 178
- 238000010438 heat treatment Methods 0.000 title claims abstract description 140
- 239000000758 substrate Substances 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims description 56
- 230000007704 transition Effects 0.000 claims description 50
- 238000012545 processing Methods 0.000 claims description 48
- 239000002245 particle Substances 0.000 claims description 43
- 230000007547 defect Effects 0.000 claims description 27
- 230000008569 process Effects 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 18
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- 229910052593 corundum Inorganic materials 0.000 claims description 15
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 15
- 230000009467 reduction Effects 0.000 claims description 11
- 239000006104 solid solution Substances 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims description 4
- 229910009474 Y2O3—ZrO2 Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 210000002381 plasma Anatomy 0.000 description 48
- 238000005516 engineering process Methods 0.000 description 18
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 14
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- 238000005229 chemical vapour deposition Methods 0.000 description 5
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 229910017083 AlN Inorganic materials 0.000 description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 238000001020 plasma etching Methods 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000013500 data storage Methods 0.000 description 2
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- 238000010894 electron beam technology Methods 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
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- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
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- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
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- 229910052905 tridymite Inorganic materials 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 2
- 229910017109 AlON Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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- 239000011324 bead Substances 0.000 description 1
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- 238000005542 laser surface treatment Methods 0.000 description 1
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- 229910003465 moissanite Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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Abstract
There is provided herein a kind of ceramic articles with ceramic substrate and ceramic coating, there is the wherein ceramic coating initial porosity to be measured with incipient crack.The ceramic articles are heated to the temperature range between about 1000 DEG C and about 1800 DEG C with about 0.1 DEG C to about 20 DEG C per minute per minute of temperature rate.The ceramic articles are heat-treated with one or more temperature in the temperature range to last of about 24 hours.Then the ceramic articles are cooled down with the temperature rate, wherein after the heat treatment, there is the porosity reduced to be measured with the crack reduced for the ceramic coating.
Description
Technical field
The specific embodiment of the present invention is typically relevant with to be heat-treated the Technology for Heating Processing of coated ceramic articles.
Background technology
In the semiconductor industry, element is manufactured by the several manufacturing process for the structure that can produce size reduction all the more.
Some manufacturing process (such as plasma etching and plasma cleaning procedure) make substrate be exposed to high-velocity plasma stream, with
Etching or cleaning substrate.Plasma is high corrosiveness, and can corrode exposed to the processing chamber housing of plasma and other
Surface.This corrosion can produce particle, and particle can often pollute processed substrate, cause component defects.
With the reduction of element physical dimension, the susceptibility of defect can be increased, and becomes for the demand of particle pollution
More attain strict.Therefore, when the physical dimension reduction of element, admissible particle pollution degree can then reduce.In order that wait from
Particle pollution caused by daughter etching and/or plasma cleaning procedure reaches minimum, and plasma can be resisted by having developed
Cell materials.The example of this kind of plasma-resistant material includes containing Al2O3、AlN、 SiC、Y2O3, quartz and ZrO2Pottery
Porcelain.However, for some applications, the plasma resistant bulk properties of these ceramic materials is inadequate.For example, using
When in the plasma etch process for the semiconductor element that threshold size is 45 nanometers or 32 nanometers, manufactured using traditional ceramics
Plasma resistant ceramic cover plate and/or nozzle manufactured by technique can produce unacceptable particle pollution degree.In addition, work as this
When class plasma resistant ceramics are normally used as ceramic coating, these coatings can produce higher particle pollution degree, and can be because
(delamination) and failure are peeled off in layering.
The content of the invention
In one embodiment, there is provided a kind of ceramic articles with ceramic substrate and ceramic coating, the ceramics apply
There is layer initial porosity to be measured with incipient crack.The ceramic articles are by with about 0.1 DEG C to about 20 DEG C per minute per minute of lifting
Warm speed is heated to the temperature range between about 1000 DEG C and about 1800 DEG C.With one or more temperature heat in the temperature range
The ceramic articles are handled to last of about 24 hours.Then the ceramic articles are cooled down with the temperature rate, wherein in Re Chu
After reason, there is the ceramic coating porosity reduced to be measured with the crack reduced.
Brief description of the drawings
In such as accompanying drawing be by illustration and it is unrestricted illustrate the present invention, identical component symbol is to represent phase in the accompanying drawings
As element.It should be noted that it is specific to be not necessarily meant to refer to identical when addressing "a" or "an" specific embodiment herein
Embodiment, this kind of narration are to represent " at least one ".
Figure 1A illustrates the example architecture of the manufacture system according to one embodiment of the invention；
Figure 1B illustrates a kind of technique for being used to be heat-treated ceramic articles according to one embodiment of the invention；
Fig. 2A is to be heat-treated according to the embodiment of the present invention before using heat treatment process ceramic coating and utilizing
The microphoto of ceramic coating surface after processing ceramic coating；
Fig. 2 B be according to the embodiment of the present invention using before heat treatment process ceramic coating and in various temperature and
Processing last ceramic coating surface after the lower ceramic coating using heat treatment process under 4,000 times of enlargement ratios other are aobvious
Micro- photo；
Fig. 2 C are using before heat treatment process ceramic coating and in various temperature according to the specific embodiment of the invention
Degree and processing last ceramic coating surface after the lower ceramic coating using heat treatment process under 20,000 times of enlargement ratios
Other microphotos；
Fig. 2 D be according to the embodiment of the present invention before ceramic coating is through processing and in ceramic coating after processing
Other microphotos under 10,000 times of enlargement ratios of ceramic coating surface；
Fig. 3 A be display according to one embodiment of the invention before heat treatment after ceramic articles side cross-sectional view
Microphoto；
Fig. 3 B be display it is according to embodiments of the present invention lower carry out being heat-treated front and rear pottery from different last in different temperatures
The microphoto of side cross-sectional view of the porcelain article under 4,000 times of enlargement ratios；
Fig. 3 C be display it is according to embodiments of the present invention before heat treatment after ceramic articles in 20,000 times of enlargement ratios
Under side cross-sectional view microphoto；
Fig. 3 D illustrate according to one embodiment of the invention before heat treatment after HPM ceramic composite coatings phase form
Compare.
Embodiment
The specific embodiment of the present invention is relevant with a kind of technique for being used to be heat-treated ceramic articles, and with utilizing heat treatment
Handled ceramic articles are relevant.In one embodiment, there is provided a kind of ceramic articles including ceramic substrate and ceramic coating,
The ceramic coating has initial porosity, the initial key knotting strength of the ceramic substrate and incipient crack is measured.The ceramic substrate
Can be sintering ceramics, and the ceramic coating is Plasma sprayed ceramic.The ceramic articles can be, such as plasma etcher
Ceramic cover plate, nozzle or process kit.The ceramic articles are by the heating and cooling speed with about 0.1 DEG C to about 20 DEG C per minute per minute
Rate is heated to the temperature range between about 1000 DEG C and about 1800 DEG C.One or more of the ceramic articles in the temperature range
At a temperature of be heat-treated and lasted of about 24 hours.Then the ceramic articles are cooled down with the temperature rate.In heat
After processing, the ceramic coating has the crack amount of reduced surface defect, the coating porosity reduced and reduction.The ceramics
Coating also has the surface roughness reduced, and has the larger repellence of plasma in addition.In addition, in heat treatment
Afterwards, the ceramic coating has stronger interface characteristics to ceramic substrate, and this is stronger interface characteristics to provide to the larger of ceramic substrate
Bond strength.It is stronger it is interface characteristics be caused by forming transition zone between ceramic substrate and ceramic coating.
In one embodiment, heating furnace performs Technology for Heating Processing to the ceramic articles comprising ceramic substrate and ceramic coating,
Wherein there is the ceramic coating initial porosity to be measured with incipient crack.The heating furnace is with about 0.1 DEG C per minute to per minute about 20
DEG C temperature rate heat the ceramic articles, untill the ceramic articles reach assigned temperature or temperature range.This refers to
Determine temperature range and about 1800 DEG C are changed to from about 1000 DEG C, and the assigned temperature is the temperature in the specified for temperature ranges.Heating
Stove is heat-treated of about 24 hours under other assigned temperatures in the assigned temperature and/or the temperature range to the ceramic articles
Last.The heating furnace then cools down the ceramic articles with the temperature rate.After the heat treatment, the ceramic articles have drop
Low surface porosity and the crack amount of reduction.
Embodiments of the invention increase ceramic coating via the formation of transition zone and are coated with the ceramics of the ceramic coating
Bond intensity between substrate.The surface that embodiments of the invention decrease the ceramic coating on the ceramic articles through processing lacks
Fall into, reduce porosity and reduce crack amount.Embodiment also reduces the surface roughness of the ceramic coating through processing, and makes pottery
Surface particle on porcelain coating is minimized.When being used in semiconductor technology (such as the plasma etching using plasma
With plasma cleaning procedure) when, this kind of thermally treated ceramic coating has reduced high-energy bond (scission of link) number, and produces
Raw significant lower particle pollution amount.In addition, the reduction porosity of thermally treated ceramic coating oozes with reducing crack and can reduce
The processing gas amount for entering ceramic coating and being reacted with lower substrate.In addition, between ceramic coating and ceramic substrate transition zone (
Also referred herein as interface characteristics transition zone) formation can suppress to penetrate into process chemistry thing and the lower substrate of coating and react.This can
Layering is peeled off to minimize.Transition zone can improve the bond strength of ceramic coating, and can minimize stripping.Lift
For example, the cover plate through ceramics coating for etcher machine can be thermally treated with nozzle, so that in plasma etching work
Caused particle pollution and/or stripping minimize during skill.Therefore, thermally treated ceramic articles as described herein are utilized
And the semiconductor manufactured there can be the defects of relatively low to count, and the discarded rate reduced can be caused.
Term " heat treatment " used in herein is to represent to apply ceramic articles rise temperature, such as passes through heating
Stove.It is to represent that proposed nominal is all accurate in ± 10% when using term " about " in this article.
Herein, some embodiments are heat-treated using heating furnace, it should be appreciated, however, that other heat can also be used
Treatment technology carries out the heat treatment.The certain embodiments of other workable heat treatment technics include Laser Surface Treatment (
Referred to as laser heat treatment), electron beam (e-beam) surface treatment (also referred to as electron beam heat treatment), flame surface processing (also referred to as
It is heat-treated for flame) and high-temperature plasma processing.
Notice that some embodiments as described herein are used in the plasma etcher on semiconductor manufacturing simultaneously
Through ceramics coating cover plate with through ceramics coating nozzle.It will be understood, however, that this kind of plasma etcher also can be used to
Manufacture the element of MEMS (MEMS).In addition, thermally treated ceramic articles as described herein can be exposed to plasma
The other structures of body.For example, the ceramic articles can be plasma etcher, plasma cleaner, plasma drive
The ring through ceramics coating of dynamic system etc., wall portion, base portion, gas distribution plate material, spray head, substrate holder framework etc..
In addition, embodiment as described herein is on can when being used in the processing chamber housing rich in plasma process
Produce the ceramic articles of the particle pollution reduced.It should be understood, however, that ceramic articles as described herein are being used in other techniques
Processing chamber housing (such as non-plasma etch device, non-plasma cleaner, chemical vapor deposition (CVD) chamber, physics gas
Mutually deposition (PVD) chamber, chemical vapor deposition (PECVD) chamber of plasma enhancing, the physical vapor of plasma enhancing
Deposition (PEPVD) chamber, ald (PEALD) chamber etc. of plasma enhancing) in when the particle of reduction can be also provided
Pollution.
Figure 1A illustrates the example architecture of the manufacture system of the specific embodiment according to the present invention.The manufacture system 100
It can be ceramic manufacturing system.In one embodiment, the manufacture system 100 includes heating furnace 105 (for example, such as rotary kiln
(kiln) ceramic heat stove), equipment automatization layer 115 and computing device 120.In alternative embodiments, the manufacture system 100
It may include more or less components.For example, the manufacture system 100 only includes heating furnace 105, and heating furnace 105 is manual
Offline machine.
Heating furnace 105 is a kind of machine for being designed to heat such as ceramic articles.Heating furnace 105 includes heat insulation chamber
Or body of heater, control temperature can be applied to the article (such as ceramic articles) being inserted in heat insulation chamber or body of heater.Implement one
In example, the chamber is in sealing.Heating furnace 105 can include pump, and air is pumped to outside chamber, and therefore and in being produced in chamber
Vacuum.Heating furnace 105 can additionally or alternatively include gas access, by gas (for example, such as argon gas or nitrogen indifferent gas
Body) it is pumped in chamber.
Heating furnace 105 is the hand with the temperature controller manually set by technical staff during the processing of ceramic articles
Dynamic heating furnace.Heating furnace 105 can also be offline machine, and offline machine can be programmed with technical recipe.The technical recipe
Heating rate, rate of temperature fall, process time, temperature, pressure, gas flow etc. can be controlled.Either, heating furnace 105 can be
Automate heating furnace on line, heating furnace is automated on line can be via equipment automatization layer 115 and from such as PC, servomechanism
The computing device 120 of machine etc. receives technical recipe.The equipment automatization layer 115 make heating furnace 105 and computing device 120, with
Other manufacture machines and measuring tool and/or other devices interconnect.
Equipment automatization layer 115 can include network (such as LAN (LAN)), router, gateway, server, data storage
Storage etc..Heating furnace 105 can via semiconductor equipment communication standard/general device pattern (SECS/GEM) interface, via ether
Net interface and/or be connected to equipment automatization layer 115 via other interfaces.In one embodiment, the equipment automatization layer
115 can make process data (such as the data of heating furnace 105 collected by during process operation) be stored in data storage (not
Show) in.In alternative embodiments, the computing device 120 is connected directly to heating furnace 105.
In one embodiment, heating furnace 105 includes programmable controller, and programmable controller can be loaded, stored with performing
Technical recipe.Temperature setting, gas and/or the vacuum of the Controlled by Programmable Controller Technology for Heating Processing are set, the time sets etc..
Controlled by Programmable Controller chamber is heated, and temperature is declined and is risen, and multi-step heat treatment can be made to be enter as single work
Skill etc..The programmable controller can include main storage, and (such as read-only storage (ROM), flash memory, dynamic random are deposited
Access to memory (DRAM), static RAM (SRAM) etc.), and/or second-level storage is (for example, such as disc driver
Data memory device).Main storage and/or second-level storage can store the finger for performing Technology for Heating Processing as described herein
Order.
The programmable controller can also include coupling (such as via bus) and be held to main storage and/or second-level storage
The processing unit of row instruction.The processing unit can be general processing unit, such as microprocessor, CPU etc..At this
Reason device is alternatively special processor, such as application specific integrated circuit (ASIC), field programmable gate array (FPGA), data signal
Processor (DSP), network processing unit etc..In one embodiment, the programmable processor is programmable logic controller
(PLC)。
In one embodiment, heating furnace 105 is programmed, to perform heating furnace 105 will be made to can be used on hot described in Figure 1B
Handling process is come the formula that is heat-treated to ceramic articles.
Figure 1B is flow chart, this flowchart illustrates according to one embodiment of the invention be used for be heat-treated ceramic articles
Technique 150.In the square 155 of technique 150, there is provided ceramic articles (such as providing to heating furnace or rotary kiln).It is specific one
In embodiment, the ceramic articles are automatically loaded into heating furnace by loader.The ceramic articles include ceramic substrate, the ceramics
Substrate is at least having been coated with ceramic coating on a surface.In one embodiment, the ceramic articles be plasma etcher or
Ceramic cover plate, ceramic nozzle or other processing chamber housing elements of plasma cleaner.The ceramic articles can have predominantly yttrium
The ceramic coating of oxide.Ceramics using predominantly yttrium oxide are because yttrium oxide has preferable plasma resistant bulk properties
Event.The ceramic articles can also have a ceramic substrate, and the ceramic substrate has a good mechanical property, for example, high flexural strength with
For the repellence of the rupture caused by high temperature and/or thermal stress.
Before ceramic coating is applied, ceramic substrate can be first processed.In addition, ceramic coating can be coated with the ceramic base
It is processed again after plate.The example of processing includes surface grinding, polishing, drilling, friction, cutting, bead sandblasting or to add
Other processing that work instrument is carried out.In one embodiment, after ceramic coating is formed above ceramic substrate, the pottery
Porcelain coating is polished.This can produce substantial amounts of particle, and particle can stay in crack, hole or the other surfaces defect of ceramic coating
In.
Ceramic substrate is formed by ceramic bulk material, such as Y2O3、Y4Al2O9、Al2O3、Y3Al5O12(YAG), quartz, SiC,
Si3N4、AlN、ZrO2Deng.For example, the ceramic substrate can be hereinafter with regard to any one ceramics illustrated by ceramic coating
Sintered form bulk.Substrate is alternatively ceramic complexes, such as Al2O3- YAG ceramic complexes or SiC-Si3N4's
Ceramic complexes.It (or is yttrium oxide or Y that the ceramic substrate, which is alternatively including the yittrium oxide containing solid solution,2O3) ceramics
Compound.For example, ceramic substrate can be high performance material (High Performance Material, HPM), the high property
Energy material is by compound Y4Al2O9(YAM) with solid solution Y2-xZrxO3(Y2O3-ZrO2Solid solution) formed.Pay attention to,
Pure yittrium oxide and the yittrium oxide containing solid solution can be mixed with ZrO2、Al2O3、SiO2、B2O3、Er2O3、 Nd2O3、Nb2O5、
CeO2、Sm2O3、Yb2O3Or one or more in other oxides.
Similar to ceramic substrate, ceramic coating is by Y2O3(yittrium oxide), Y4Al2O9(YAM)、Al2O3(aluminum oxide), Y3Al5O12
(YAG), quartz, YAlO3(YAP), SiC (carborundum), Si3N4(silicon nitride), AlN (aluminium nitride), ZrO2(zirconium dioxide),
AlON (aluminum oxynitride), TiO2(titanium dioxide), TiC (titanium carbide), ZrC (zirconium carbide), TiN (titanium nitride), TiCN (carbonitrides
Titanium), with Y2O3Stabilized ZrO2Etc. (YSZ) formed.Ceramic substrate is also similarly to, ceramic coating can be pure yittrium oxide
Or the yittrium oxide containing solid solution, pure yittrium oxide or yittrium oxide containing solid solution can be mixed with ZrO2、Al2O3、
SiO2、B2O3、Er2O3、Nd2O3、Nb2O5、CeO2、Sm2O3、Yb2O3Or one or more in other oxides.In one embodiment,
Ceramic coating is HPM compounds.However, the ceramic coating can be by the spraying on ceramic substrate or ceramic coating of growing up and shape
Into, and the ceramic substrate is formed by sintering process.
In one embodiment, the ceramic coating is containing utilizing plasma spray technology or plasma spray technology to sink
Ceramic yittrium oxide of the product on ceramic substrate.Plasma spray technology fusible material (such as ceramic powders), and by the material of fusing
Material is sprayed on ceramic substrate.Thermal Sperayed Ceramic Coatings can have about 20 microns to about several millimeters of thickness.
In one embodiment, the ceramic coating is through on plasma spray coating to ceramic substrate.Either, it is possible to use other
Plasma spray technology, such as detonation flame spraying, electric arc spraying, high-velocity oxy-fuel (HVOF) spraying, flame-spraying, warm spraying and cold spray
Apply.In addition, it is possible to use other coating processes form ceramic coating, such as gas glue deposition, plating, physical vapour deposition (PVD)
(PVD), ion assisted deposition (IAD) and chemical vapor deposition (CVD).Pay attention to, ceramic coating process can be produced with such as hole
Hole, crack and the not exclusively small empty ceramic coating such as bond region, the ceramic coating have the ceramics for differing markedly from bulk
The architectural characteristic of material (such as ceramic substrate).
In one embodiment, the ceramic coating is by Y2O3Made by powder.Either, the ceramic coating can be by Y2O3
Powder, ZrO2Powder and Al2O3HPM ceramic complexes made by the mixture of powder.In one embodiment, HPM ceramics
Compound contains 77% Y2O3, 15% ZrO2And 8% Al2O3.In another embodiment, the HPM ceramic complexes contain
There is 63% Y2O3, 23% ZrO2And 14% Al2O3.In another embodiment, the HPM ceramic complexes contain
55% Y2O3, 20% ZrO2And 25% Al2O3.Relative percentage is alternatively molar ratio.For example, the HPM makes pottery
Y of the porcelain containing 77 moles of %2O3, 15 moles of % ZrO2And 8 moles of % Al2O3.Other distribution of these ceramic powders
It can also be used for HPM materials.
The ceramic coating initially has weakly caking intensity (e.g., from about 3 MPas (MPa)), and this can make ceramic coating with the time
(such as due to ceramic articles are used in into the result rich in plasma process) and be layered or from ceramic substrate peel off come off.This
Outside, there is ceramic coating initial porosity to be measured with incipient crack.These holes can make processing gas and cleaning chemistry thing with crack
Matter is penetrated into ceramic coating and reacted with the ceramic substrate of lower section during processing.This kind of reaction can produce below ceramic coating
Gas, aqueous vapor or different materials, and bubble is produced below ceramic coating.These bubbles can further make ceramic coating and ceramics
Substrate separates.This separation can produce larger amount of particle pollution to the material (such as wafer through processing) through processing.In addition,
Even if not peeling off, bubble, crack and hole (and other surface defects) itself also can be to producing particle through handling substrate
Pollution.
In one example, the hole in ceramic coating, crack, cavity with other surfaces defect can include fracture (or
It is open) key, (or open) key of such fracture is high-energy position.These surface defects can particle entrapment.For example,
Particle can form weak scission of link (broken bonds) at surface defect with ceramic articles.During corona treatment, etc.
Gas ions can destroy these weak scission of links, and the particle of part is removed from ceramic coating.Ceramic particle is then deposited on through processing
Substrate on.In addition, plasma can destroy bond of the ceramic articles at defect address, at hole, at crack etc., this
Act can corrode ceramic coating, and produce other particles.
At square 160, the ceramic thing is heated with about 0.1 DEG C to about 20 DEG C per minute per minute of temperature rate
Product.The ceramic articles are fragility, and can be ruptured when under changing exposed to excessive temperatures.Therefore, it need to use enough slow and be enough to keep away
Exempt from the temperature rate of ceramic articles rupture.It is expectable for it is some ceramics for, the temperature rate more than 20 DEG C per minute
It is and feasible.Therefore, in some specific embodiments, the lifting that will not cause to rupture and more than 20 DEG C per minute can be used
Warm speed.
The temperature change that ceramic articles rupture can be made depending on the composition of ceramic articles.For example, can be with every point
The temperature rate that 10 DEG C or higher of clock heats Al2O3Without rupturing.If however, faster to be risen than about 5 DEG C per minute
Rate of temperature fall heats Y2O3, Y2O3It can then rupture.In one embodiment, to Y2O3Make with the ceramic coating of HPM ceramic complexes
With about 0.1 to 5 DEG C per minute of temperature rate.In a further embodiment, for by Y2O3With HPM ceramic complexes institute
Manufactured ceramic coating uses about 5 DEG C per minute of temperature rate.In general, ceramic articles are in environment temperature or connect
Start under nearly environment temperature, and predetermined temperature is slowly heated to temperature rate.
The ceramic articles are heated to untill reaching assigned temperature or temperature range.The assigned temperature is between about
1000 DEG C to about 1800 DEG C of scope.The used assigned temperature is thick according to the composition of ceramic articles or the specified target of transition zone
Depending on degree.In one embodiment, for aluminum oxide substrate and HPM ceramic coatings or yttrium oxide (Y2O3) ceramic coating
Ceramic articles use 1400 DEG C to 1500 DEG C of temperature.
The quilt at a temperature of square 165, one or more of the ceramic articles under the assigned temperature or in the temperature range
Heat and lasted up to 24 hours.Used specified last can be according to the composition of ceramic articles and the needs of ceramic articles
Depending on performance characteristics.For example, this specify last can be according to the target temperature of the transition zone depending on.
As described above, the particle that the ceramic coating has substantial amounts of surface defect and stayed in these surface defects.
Heat treatment can reduce or eliminate these defects and/or particle.Specifically, heat treatment can make particle melt and/or make on surface
A part of ceramic coating fusing at curve regions.The particle of fusing can flow together with the ceramic coating at surface defect areas
It is dynamic.The particle of fusing then be it is redeposited on ceramic coating, and with the ceramic coating shape at these surface defect areas
Into non-scission of link.Caused non-scission of link can than previously making the stronger many of scission of link that particle is combined with ceramic coating, therefore, wait from
In daughter etch process, particle can become less likely to remove from ceramic coating, and defect area also becomes to be less affected by abrasion.
In addition, ceramic coating is typically measured with relatively high porosity and relatively high crack.Heat treatment can make hole with
Crack reduces and/or is removed.Hole and crack can be based on above-mentioned ceramic coating identical fusing with it is redeposited and reduce or
Disappear.For example, the ceramic coating at hole or crack can melt and then redeposited, filling and/or healing hole or
Crack.
In one embodiment, the ceramic coating can form transition with the ceramic substrate in Technology for Heating Processing present invention
Layer.When ceramic coating and ceramic substrate in the material to being reacted during heat exposure by that can form, i.e., it can form transition zone.Citing
For, if ceramic substrate is Al2O3And ceramic coating is HPM ceramic complexes, then the ceramic coating and the ceramic substrate will be
It is heat-treated present invention and forms YAG transition zones.In another example, if ceramic substrate is Al2O3And ceramic coating is Y2O3,
Then the ceramic coating can during heating treatment react with the ceramic substrate and form YAG transition zones.Other ceramic coating materials
Combination with ceramic substrate material will form other transition zones.
Especially, the transition zone is non-reacted with non-pore layer.Therefore, after using thermally treated ceramic articles
During continuous processing, processing gas can penetrate into ceramic coating, but not penetrate into transition zone.Therefore, the transition zone can avoid handling gas
Body reacts with ceramic substrate.This can minimize or be avoided bubble, and can improve the stripping performance of ceramic coating and cohere strong
Spend (bond intensity).
Although transition zone has various favourable effects, if transition zone becomes blocked up, transition zone can become problematic.
Some transition zones are by with the coefficient of expansion different from ceramic coating and/or ceramic substrate.Therefore, if transition zone compares threshold thickness
(e.g., from about 5 microns) are thicker, then the transition zone can produce crack in subsequent treatment in ceramic coating.For example, HPM makes pottery
Porcelain compound and aluminum oxide have a roughly equal coefficient of expansion, but YAG transition zones then have and are different from HPM Ceramic Composites
The coefficient of expansion of thing and aluminum oxide.Therefore, when YAG transition zones are thicker than about 5 microns (μm), the expansion and contraction of YAG transition zones
Ceramic coating can be ruptured.
Transition zone is grown up with the speed relevant with temperature and time.When temperature and heat treatment last increase, transition zone
Thickness can also increase.Therefore, for be heat-treated the temperature (or multiple temperature) of ceramic articles with last should be chosen it is not thick to be formed
In about 5 microns of transition zone.In one embodiment, temperature is chosen can make about 0.1 micron to about 5 microns of mistake with lasting
Layer is crossed to be formed.In one embodiment, transition zone has the minimum for being enough to avoid gas during processing with ceramic substrate reaction
Thickness (e.g., from about 0.1 micron).In one embodiment, the transition zone has 1 micron to 2 microns of target thickness.
Heat treatment also can increase the grain size of ceramic coating.When temperature and heat treatment last increase, ceramic coating
Grain size can also increase.The increase of grain size causes less crystal boundary.Crystal boundary then than ceramics crystal grain be easier by
Plasma is denuded.Therefore, the increase of grain size can make ceramic coating less be also easy to produce particle pollution in subsequent treatment.Cause
This, can select heat treatment temperature with lasting according to the target grain size of ceramic coating.
For aluminium oxide ceramic substrate and HPM or yttrium coating, 1500 DEG C are carried out, is heat-treated and lasts about
The heat treatment of 3 hours to 6 hours.In one embodiment, the heat treatment of the ceramic coating of yittrium oxide or HPM ceramic complexes lasts
It is about 4 hours.
In one embodiment, the ceramic articles are maintained single temperature in heat treatment history.Either, in the heat treatment phase
Between, the ceramic articles are heated and/or multiple different temperatures for being cooled in the temperature range.For example, the ceramic articles
It is heat-treated 4 hours, is then heat-treated 2 hours at a temperature of 1700 DEG C, then in 1000 DEG C of temperature at a temperature of 1500 DEG C
Lower heat treatment 3 hours in addition of degree.Notice that the ceramic articles are with the temperature rate when using multiple different heat treatment temperatures
Heated and/or cooled down, to be changed between heat treatment temperature.
At square 170, ceramic articles are cooled down with temperature rate.In one embodiment, ceramic articles with
Cooled down with the temperature rate identical temperature rate of heating ceramic article.In another embodiment, can be used not
With temperature rate heat the ceramic articles.On through handling the particle pollution of substrate, plasma resistant abrasion, glutinous
On knotting strength, porosity, the quantity in crack and size and stripper-resistance, the ceramics of caused thermally treated ceramic articles
Coating all has the performance promoted.In addition, caused thermally treated ceramic articles have in ceramic coating and ceramic substrate
Between transition zone.Therefore, ceramic cover plate, ceramic nozzle, process kit and other ceramic inter-process chamber combination profits
It is heat-treated with technique 150, to promote the yield of the product of manufacture.In addition, the ceramic articles that technique 150 is applied have
The replacement frequency of reduction, and the equipment downtime can be reduced.
Notice that technique 150 can be implemented as the system of ceramic articles after ceramic coating is formed on ceramic substrate
Make a part for technique.In addition, technique 150 can be periodically carried out to the ceramic articles through using, to cure or repair these
Ceramic articles.For example, ceramic articles are heat-treated using technique 150 before the use, then per the several months once, one
Year once, it is heat-treated again twice or with other some frequency utilization techniques 150 within 1 year.The frequency for performing technique 150 can be according to
Depending on plasma etching and/or the plasma cleaning formula used according to ceramic articles.For example, if ceramic articles frequency
Numerously exposed to especially severe plasma environment, then the ceramic articles are heat-treated with upper frequency.
Ceramic coating can be made to denude and/or corrode with the time exposed to plasma.For example, plasma can make
Scission of link is betided at the surface of ceramic coating, can produce the ceramic particle that can pollute the substrate through processing, can cause to apply in ceramics
The defects of at layer surface, ceramic coating can be made from ceramic substrate stripping etc..Therefore, when ceramic articles aging, may produce
More particle pollutions.Technology for Heating Processing 150 can be carried out to the ceramic articles of this aging, to reply because of aggressive plasmas
Damaged caused by body environment.In addition to newly formed ceramic articles, heat treatment or the ceramic articles reparation used
Defect and reduction particle.Therefore, technique 150 can be performed to the ceramic articles used, to extend the service life of ceramic articles.
Notice that Technology for Heating Processing 150 also can be used to dry type in addition to repairing surface defect and minimizeing particle
Clean ceramic articles.Polymer can be made to be formed on the surface of ceramic articles exposed to plasma environment.These polymer meetings
Particle pollution is produced on substrate during subsequent treatment.Periodically wet type cleaning process would generally be performed and remove ceramic thing
Polymer on product.In one embodiment, Technology for Heating Processing 150 is performed to substitute wet type cleaning process.The meeting of Technology for Heating Processing 150
Make the polymer of coating ceramic article polymer can be made to be changed into gas with air or other gas reactions, this reaction in hot environment
State, and leave the surface of ceramic articles.Therefore, Technology for Heating Processing 150 can be used to clean ceramic articles and to repair ceramics
The surface of article.It is to be noted that the temperature of subsequent heat treatment technique and/or last can be with the temperature for initial Technology for Heating Processing
And/or last difference.
Fig. 2A illustrate it is according to embodiments of the present invention using heat treatment come before handling ceramic coating and using heat
Handle to handle the microphoto 202-216 of the ceramic coating after ceramic articles.It is shown in microphoto 202-216
Ceramic coating be with Y4Al2O9With Y2-xZrxO3HPM ceramic complexes.
Microphoto 202 shows the example of ceramic articles before the heat treatment.Microphoto 204 is shown in microphoto
The zoomed-in view in the region 208 shown in 202.Region 208 is relatively free of surface defects.Microphoto 204 illustrates ceramic coating
Grain size.Microphoto 206 is shown in the zoomed-in view in the region 210 in microphoto 202.Region 210 illustrates to make pottery
The surface defect and surface particle of porcelain coating.
Microphoto 212 shows the example shown in microphoto 202 after the heat treatment.As illustrated, surface defect
Amount is reduced because of heat treatment.Microphoto 214 shows the zoomed-in view in the region 218 shown in microphoto 212.Area
Domain 218 is relatively free of surface defects and surface particle.Microphoto 214 illustrates the grain size of ceramic coating than micro- photograph
Grain size shown in piece 204 is bigger.Microphoto 216 shows that the amplification in region 220 shown in microphoto 212 regards
Figure.Region 220 illustrates the surface defect of ceramic coating.However, surface defect shown in microphoto 216 is than micro- photograph
Surface defect shown in piece 206 is less serious, and surface particle has also substantially been removed.
Fig. 2 B are shown in use according to embodiments of the present invention and are heat-treated to exist before handling ceramic coating and
Different temperatures and processing, which last, lower handles other micro- photographs of the ceramic coating surface after the ceramic coating using being heat-treated
Piece 222-234 (enlargement ratio is 4000 times).Microphoto 222 shows the example of ceramic coating before the heat treatment.It is micro-
Photo 224 is shown in the example for carrying out the ceramic coating after being heat-treated at a temperature of 1300 DEG C 4 hours.Microphoto 226 is aobvious
Show the example that the ceramic coating after heat treatment in 4 hours is carried out at a temperature of 1400 DEG C.Microphoto 228 is shown in 1500 DEG C
At a temperature of carry out 4 hours heat treatment after ceramic coating example.Microphoto 234 enters at a temperature of being shown in 1600 DEG C
The example of ceramic coating after row heat treatment in 4 hours.As illustrated, under fixed heat treatment time, the increase meeting of temperature
The size and quantity for making crack are reduced.In addition, the increase of temperature can reduce the size of hole and quantity (thus reduces hole
Rate).
Microphoto 230 illustrates the example of the ceramic coating after heat treatment in 24 hours is carried out at temperature is 1300 DEG C.
Microphoto 232 illustrates the example of the ceramic coating after heat treatment in 24 hours is carried out at temperature is 1400 DEG C.As illustrated,
Ceramic coating, which is heat-treated, substantially can't further reduce porosity or crack amount up to more than 4 hours.Therefore, it is real one
Apply in example, heat treatment lasts substantially 4 hours.
Fig. 2 C are shown in use according to embodiments of the present invention and are heat-treated to exist before handling ceramic coating and
Different temperatures and processing, which last, lower handles other micro- photographs of the ceramic coating surface after the ceramic coating using being heat-treated
Piece 236-248 (enlargement ratio is 20000 times).Microphoto 236 shows ceramic coating before the heat treatment.Microphoto
238 are shown in temperature to carry out the ceramic coating after being heat-treated at 1300 DEG C 4 hours.Microphoto 240 is shown in temperature
The ceramic coating after heat treatment in 4 hours is carried out at 1400 DEG C.It is that progress 4 is small at 1500 DEG C that microphoto 242, which is shown in temperature,
When heat treatment after ceramic coating.It is that the pottery after heat treatment in 4 hours is carried out at 1600 DEG C that microphoto 248, which is shown in temperature,
Porcelain coating.Grain size shown in microphoto 248 is more than the grain size shown in microphoto 242, microphoto 242
Shown in grain size be more than microphoto 240 shown in grain size, the rest may be inferred.Therefore, the increasing of heat treatment temperature
Add the increase for the grain size that can cause ceramic coating.
It is that the ceramic coating after heat treatment in 24 hours is carried out at 1300 DEG C that microphoto 244, which is shown in temperature,.Micro- photograph
It is that the ceramic coating after heat treatment in 24 hours is carried out at 1400 DEG C that piece 246, which is shown in temperature,.Therefore, it is heat-treated the increase lasted
Also the grain size of ceramic coating can be made increase.Before the heat treatment, the grain size of ceramic coating is initially nano-scale, and
Finally grown into because of heat treatment more than nano-scale.The temperature of heat treatment and/or last based on target grain size and be subject to
Selection.Increase processing, which lasts, can cause uneven grain size, as shown in microphoto 244 and 246.
Fig. 2 D show and have been processed according to embodiments of the present invention before ceramic coating is processed and in the ceramic coating
Other microphotos 250-256 of ceramic coating surface afterwards (enlargement ratio is 10000 times).Microphoto 250 and 254 is aobvious
Show before the heat treatment, ceramic coating includes substantial amounts of ceramic particle.Microphoto 252 and 256 show after the heat treatment,
Ceramic particle has reduced or eliminated.In one embodiment, surface particle count can be reduced of about 93%.
Fig. 3 A illustrate microphoto 302-304, and microphoto 302-304 is shown to exist according to one embodiment of the invention
The front and rear ceramic articles side cross-sectional view of heat treatment.Microphoto 302 shows that the ceramic articles include ceramic substrate 314 and at this
The ceramic coating 310 of the top of ceramic substrate 314.Described ceramic substrate 314 is aluminum oxide, and described ceramic coating 310 is
HPM ceramic complexes.
Microphoto 304 shows ceramic substrate 314 and ceramic coating 310 and has been formed over ceramic coating 310 and pottery
Transition zone 312 between porcelain substrate 314.The transition zone has about 1 micron to 2 microns of thickness.
The element collection of illustrative plates 308 of transition zone is also show simultaneously.Element collection of illustrative plates 308 is according to energy dispersion X-ray spectrometer
(EDX) elementary analysis of transition zone 312 is provided.Element collection of illustrative plates 308 shows that transition zone 312 is made up of carbon, oxygen, aluminium and yttrium.
Element collection of illustrative plates 308 more shows carbon, 46% oxygen, 23% aluminium of the Elements Atom concentration substantially 18% in transition zone 312
And 13% yttrium.Therefore, show that transition zone 312 is Y3Al5O12(YAG).Transition zone can significantly enhance ceramic coating to ceramics
The bond strength of substrate.
Fig. 3 B illustrate display it is according to embodiments of the present invention before and after being heat-treated under different temperatures and difference are lasted
Ceramic articles 4,000 times of enlargement ratio side cross-sectional views microphoto.Microphoto 320 shows, before the heat treatment,
There is interface between ceramic coating 310 and ceramic substrate 314.Microphoto 322, which is shown at 1300 DEG C, to be carried out at 4 hours heat
The interface between ceramic coating 310 and ceramic substrate 314 after reason.Microphoto 324 is shown at 1400 DEG C and carried out 4 hours
The interface between ceramic coating 310 and ceramic substrate 314 after heat treatment.Microphoto 326 is shown at 1500 DEG C and carried out
The interface between ceramic coating 310 and ceramic substrate 314 after heat treatment in 4 hours.Microphoto 332 is shown at 1600 DEG C
Carry out the interface between the ceramic coating 310 and ceramic substrate 314 after being heat-treated 4 hours.Microphoto 328 is shown in 1300
Carry out the interface between the ceramic coating 310 and ceramic substrate 314 after being heat-treated at DEG C 24 hours.Microphoto 330 is shown
Carry out the interface between the ceramic coating 310 and ceramic substrate 314 after being heat-treated at 1300 DEG C 24 hours.
As shown in microphoto 326,330 and 332, pottery is formed at during the heat treatment of transition zone 312 under certain conditions
Between porcelain coating 310 and ceramic substrate 314.Heat treatment temperature be 1300 DEG C at, no matter be heat-treated last how long, all do not had
Layer is crossed to be formed.In the case where heat treatment temperature is 1400 DEG C, after handling 4 hours and transition zone can not be detected, but can locate
Reason detects transition zone 312 after 24 hours.In the case where heat treatment temperature is 1500 DEG C and 1600 DEG C, it is afterwards within 4 hours in processing
It may detect that transition zone.
Being shown in increased treatment temperature and being lasted with increased processing lower can form thicker transition zone.For transition thickness
For degree, temperature ratio, which lasts, has bigger influence.As illustrated, it is lasted for 4 hours, caused by the heat treatment of 1500 DEG C of temperature
The thickness ratio of transition zone 312 is lasted for 24 hours, the thickness of transition zone 312 is slightly thicker caused by the heat treatment of 1400 DEG C of temperature
A bit.
Fig. 3 C illustrate display according to the specific embodiment of the invention before heat treatment after 20,000 times of ceramic articles
The microphoto 350-356 of enlargement ratio side cross-sectional view.The display of microphoto 350 and 354 applies in ceramics before the heat treatment
Interface between layer 310 and ceramic substrate 314.Before the heat treatment, shown between ceramic substrate 314 and ceramic coating 310
There is gap 370 to exist.These gaps can cause ceramic coating 310 to be layered later from ceramic substrate 314.Microphoto 352 and 356
Display transition zone 312 is formed at the interface between ceramic coating 310 and ceramic substrate 314 during heat treatment.It is in addition, micro-
Photo 352 shows that gap 370 existing before the heat treatment eliminates or reduced because of the result of heat treatment with 356.This can drop
The possibility of low layering, and the cohering or be bonded intensity to ceramic substrate 314 of ceramic coating 310 can be lifted.
Fig. 3 D illustrate according to one embodiment of the invention before heat treatment after HPM ceramic composite coatings phase form
Compare.As illustrated, the phase composition of heat treatment and unobvious change ceramic coating or ceramic substrate.
The surface morphology of ceramic coating can be represented with surface roughness parameter and/or surface evenness parameter.Surface type
Porosity, crack and/or the parameter in cavity can also be used in state.Represent porosity measurement parameter can include hole count and/or
Average pore size.Similarly, the measurement parameter for representing cavity and/or crack includes average hole/Size of Crack and/or sky
Hole/crack counts.
The measurement parameter for representing particle counting counts (LPC) as adhesive tape peel test particle counting and liquid particle.Adhesive tape
Test by by adhesive tape be attached on ceramic coating then tearing-off adhesive tape and calculate stick the number of particles on adhesive tape to enter
OK.Ceramic articles by being placed in water-bath (such as deionization (DI) water-bath) and sound wave shock being carried out to water-bath, then by LPC
Such as laser counter can be used and carried out to count disengaging into the number of particles in solution.
Bond strength by applying a power (such as with MPa to measure) to ceramic coating, until ceramic coating is from ceramic base
Determined untill plate is peeled off.In one embodiment, the bond strength of ceramic coating is 4MPa degree before the heat treatment, and
It is then 12MPa degree after heat treatment.Therefore, after the heat treatment, ceramic coating can compare the bond strength of ceramic substrate
Bond strength before the heat treatment is substantially strong three times.
Bond strength, porosity, crack and the particle counting value of ceramic coating can be lifted because of heat treatment.In addition, crystal grain
Size can increase because of heat treatment, and hardness can reduce because of heat treatment.Empirically evidence displays that, the cover plate through ceramics coating
Caused particle pollution is reduced because of heat treatment during plasma etch process with the nozzle through ceramics coating.Empirically
Evidence displays that, because of the result of heat treatment, can reduce stripping of the ceramic coating from ceramic substrate.In addition, the surface of ceramic coating
Roughness also reduces because of heat treatment.
Pay attention to for being up to about 1200 DEG C of heat treatment, the interaction between particle and ceramic coating surface be by
Van der Waals (van der Waals) power is dominated, according to following formula：
Wherein F is power, and A is area, and H is distance.As heat treatment temperature from room temperature increases to about 500 DEG C, Van der Waals
Power can weaken, and thermal expansion can cause distance H increase.When heat treatment temperature increases to about 1200 DEG C from about 500 DEG C, Van der Waals
Power at least can strengthen because of distance H reduction.The reduction of this distance is absorbed because of substrate table caused by particle and/or deformation.
At a temperature of between about 1200 DEG C with 1800 DEG C, liquid can be formed between particle and ceramic coating surface
Film.Between about 1200 DEG C and 1500 DEG C, fluid film can be thin liquid film, and between about 1500 DEG C and 1800 DEG C, should
Liquid film can be thick liquid film.At a temperature of being up to about 1800 DEG C, the interaction between particle and ceramic coating surface
Dominated by capillary force by being interacted between liquid, according to following formula：
F=4 π γ Rcos θ (formula 2)
Wherein F is power, and γ is fluid-air surface tension, interface equivalent redius of the R between particle and substrate surface,
And θ is contact angle.At these tem-peratures, Particle diffusion is into liquid, and can grow up again on corresponding crystal grain.This can make particle
Removed from substrate surface, even as the same after ceramic articles have cooled down.
For HPM ceramic complexes and yttrium oxide, 1800 DEG C are sintering temperature.Therefore, at substantially 1800 DEG C
Or at a temperature of greater than about 1800 DEG C, liquid phase is formed in the ceramic coating between powder.These powder can be molten into liquid,
And grow into larger-sized crystal grain.Atom can diffuse to low energy crystal grain from high-energy grains, untill reaching balance.
Therefore, in one embodiment, it is heat-treated at a temperature of below about 1800 DEG C.
Preceding description proposes various details (such as example of specific system, component, method etc.), to provide to this hair
Bright several embodiments it is well-understood.However, it will be obvious to a person skilled in the art that also can be real under without these details
Apply at least some of embodiment of the present invention.In other examples, known component or method do not explain detailedly or only with
Simple block diagram form is presented, and to avoid being not required to strategic point obscures the present invention.Therefore, the detail proposed is only to illustrate,
Specific embodiment can change with these illustration details, and be regarded as falling within scope of the invention.
In this manual, it is to represent mutually to speak on somebody's behalf with the embodiment when addressing " one embodiment " or " embodiment "
A bright special characteristic, structure or characteristic is contained at least one embodiment.Therefore, when various pieces appearance in this specification
When term " in one embodiment " or " in one embodiment ", i.e. it is not necessary to all referring to same embodiment.
In addition, term "or" be represent inclusive "or" and non-exclusive "or".
Though the operation of method described herein illustrates that the order of operation of each method can be adjusted with particular order
It is whole so that some operations can be performed with a reverse order, or some operations at least partly can be held simultaneously with other operations
OK.In another specific embodiment, the instruction of different operating or secondary operation can be periodicity and/or alternate form.
It should be understood that described above is only to illustrate and unrestricted be used.After studying carefully and understanding described above, this area skill
Art personnel can substantially learn other more specific embodiments.Therefore, scope of the invention should refer to as attached claim and these
The full scope of equivalent described in claim and determine.
Claims (8)
1. a kind of method for handling ceramic articles, comprise the following steps：
Hot-spraying technique is performed with including Al2O3Ceramic substrate on form ceramic coating, the ceramic coating includes Y2O3-
ZrO2Solid solution and Y4Al2O9, wherein there is the ceramic coating initial porosity to be measured with incipient crack；
With 0.1 DEG C to 20 DEG C per minute per minute of temperature rate, the ceramic articles are heated between 1000 DEG C and 1800
Temperature range between DEG C, the ceramic articles include the ceramic substrate and the ceramic coating；
The ceramic articles are heat-treated with one or more temperature in the temperature range to last up to 24 hours, with described in reduction
The porosity of ceramic coating is measured with crack, wherein be heat-treated below the sintering temperature of the ceramic coating ceramic articles from
And the sintering of the ceramic coating is prevented, and wherein described heat treatment makes to include the Y2O3-ZrO2Solid solution and
Y4Al2O9The ceramic coating and include Al2O3Ceramic substrate reaction so as in the ceramic substrate and the ceramics
Transition zone is formed between coating, the transition zone includes Y3Al5O12；And
The ceramic articles are cooled down with the temperature rate after the heat treatment.
2. the method as described in claim 1, cohered by force with initial wherein there is the ceramic coating primary to count in addition
Degree, and wherein after the heat treatment, the ceramic coating has the particle counting reduced and increased bond strength.
3. the method as described in claim 1, wherein described last is chosen so that the transition zone has with the temperature range
There is 1 micron to 2 microns of thickness.
4. the method as described in claim 1, further comprising the steps of：
After the ceramic articles have been used to plasma etch process, Repeat-heating, heat treatment and cooling, to reduce
State increased surface defect density caused by plasma etch process.
5. method as claimed in claim 4, wherein the plasma etch process makes polymer be formed at the ceramic thing
On product, and the heat treatment is wherein repeated in the presence of oxygen by making the polymer be reacted with oxygen to become gas and dry type
Clean the ceramic articles.
6. the method as described in claim 1, wherein methods described are in vacuum, the presence of air, the presence of argon gas or nitrogen
Carried out in the presence of at least under one.
7. the method as described in claim 1, wherein the ceramic articles are the processing chamber housing components of plasma etcher.
8. the method as described in claim 1, wherein the heat treatment increases the grain size of the ceramic coating, and wherein
Described last passes through selection to reach target grain size with the temperature range.
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| CN201710692398.3A CN107382376B (en) | 2012-02-22 | 2013-02-20 | Ceramic article |
| CN201810096333.7A CN108249957B (en) | 2012-02-22 | 2013-02-20 | Method for dry cleaning ceramic articles |
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| US201261602020P | 2012-02-22 | 2012-02-22 | |
| US61/602,020 | 2012-02-22 | ||
| US201261619854P | 2012-04-03 | 2012-04-03 | |
| US61/619,854 | 2012-04-03 | ||
| US13/745,589 | 2013-01-18 | ||
| US13/745,589 US9212099B2 (en) | 2012-02-22 | 2013-01-18 | Heat treated ceramic substrate having ceramic coating and heat treatment for coated ceramics |
| PCT/US2013/026963 WO2013126466A1 (en) | 2012-02-22 | 2013-02-20 | Heat treated ceramic substrate having ceramic coating and heat treatment for coated ceramics |
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| CN201810096333.7A Division CN108249957B (en) | 2012-02-22 | 2013-02-20 | Method for dry cleaning ceramic articles |
| CN201710692398.3A Division CN107382376B (en) | 2012-02-22 | 2013-02-20 | Ceramic article |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101293771A (en) * | 2007-04-27 | 2008-10-29 | 应用材料股份有限公司 | Apparatus and method which reduce the erosion rate of surfaces exposed to halogen-containing plasmas |
| CN101589455A (en) * | 2007-01-11 | 2009-11-25 | 朗姆研究公司 | Extending lifetime of yttrium oxide as a plasma chamber material |
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101589455A (en) * | 2007-01-11 | 2009-11-25 | 朗姆研究公司 | Extending lifetime of yttrium oxide as a plasma chamber material |
| CN101293771A (en) * | 2007-04-27 | 2008-10-29 | 应用材料股份有限公司 | Apparatus and method which reduce the erosion rate of surfaces exposed to halogen-containing plasmas |
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