CN110386817A - Resisting plasma corrosion ceramics and preparation method - Google Patents
Resisting plasma corrosion ceramics and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of resisting plasma corrosion ceramics and preparation method, the chemical formula of the ceramics is (1-x-y) ZrO2·xCeO2·yNb2O5, wherein x=0.05-0.1, y=0.01-0.05, it can be suitable with yttrium-aluminium-garnet using the plasma etch resistance of ceramics prepared by the present invention, bending strength is better than yttrium-aluminium-garnet ceramics, and cost is far below yttrium-aluminium-garnet, may be used as the manufacture material of etching machine inside cavity part.
Description
Technical field
The present invention relates to ceramic materials preparation technology fields, and in particular to a kind of resisting plasma corrosion ceramics and preparation side
Method.
Background technique
In the production process of semiconductor devices, needs to etch microscopic pattern on a semiconductor wafer, usually be unable to do without
The sputtering and CVD device of semiconductor die on piece deposition film.Such instrument usually utilizes halogen gas, such as carbon tetrachloride
(CCl4) and boron chloride (BCl3) and fluorine carbon (such as CF4And C4F8), nitrogen fluoride (NF3) and sulfur fluoride (SF6) etc. as etching gas
Body, each is all corrosive gas.In plasma etch process, reaction gas used can generate a large amount of Cl base, F base
Therefore isoreactivity free radical is exposed to the structural elements of the above equipment in the plasma in corrosive gas, such as process chamber
Inner wall, monitor window, microwave window etc., it is necessary to have enough plasma etch resistance energy.To meet this requirement, usually adopt
Resisting plasma corrosion component is prepared with materials such as aluminium oxide ceramics, sapphire, silicon nitride ceramics and aluminium nitride ceramics.
However, resisting made of above-mentioned material (including aluminium oxide ceramics, sapphire, silicon nitride ceramics and aluminium nitride ceramics)
Plasma member can gradually corrode when being exposed to plasma in corrosive atmosphere.Therefore, the crystal grain on surface is formed
It may fall off from surface, material may react to form aluminum fluoride with fluorine, so as to cause particle contamination problems.To fall off from surface
Grain is attached on semiconductor crystal wafer, electrode and its adjacent area, so that the precision to etch process has an adverse effect.Therefore,
The reduced performance of semiconductor, reliability also reduce.CVD equipment is also exposed to the nitrogen fluorination of plasma in cleaning
In object and other fluorine base gas, therefore it is also required to corrosion resistance.
In order to provide required corrosion resistance, there has been proposed made of yttrium-aluminium-garnet (commonly referred to as YAG) ceramics
Plasma resistant product.Although the plasma etch resistance of yttrium-aluminium-garnet base ceramics can be relatively high compared with aluminium oxide,
But when needing micro etch to form micro circuit pattern, it frequently can lead to low yield.In addition, will increase cost using these materials.
Based on this, people propose demand to the high performance-price ratio material with high resisting plasma corrosion performance.
Summary of the invention
In view of this, the present invention provides a kind of resisting plasma corrosion of gas attack of resistance to halogen ceramics and preparation sides
Method.
Its technical solution is as follows: a kind of resisting plasma corrosion ceramics, key are: the chemical formula of the ceramics is (1-
x-y)ZrO2·xCeO2·yNb2O5, wherein x=0.05-0.1, y=0.01-0.05.
A kind of preparation method of resisting plasma corrosion ceramics, key are to sequentially include the following steps:
Each component is weighed in proportion, and each component is ground and dried respectively, in 1400-1500 after then mixing each component
DEG C heat preservation minimum 6 hours synthesis solid-solution materials, after which is regrind and is formed, 1550-1650 DEG C guarantor
It is 4-12 hours warm, so that the plasma resistant corrosion ceramics be made.
By adopting the above technical scheme, ZrO is chosen2It is because zirconia ceramics has preferable mechanics as main component
Performance can reduce processing cost.More importantly ZrO2Relative to cheap (the high-purity zirconia powder 20- of yttrium-aluminium-garnet
30RMB/ kilograms, and YAG powder is then up to 500-600RMB/ kilograms) production cost is low.ZrO2Content form and count with mole
Between 85%-94%.If zirconia content is lower than 85%, Mechanical Property of Ceramics is deteriorated, due to CeO2And Nb2O5Content is high, cost
Rise, economy is deteriorated；Content is higher than 95%, and plasma etch resistance can be deteriorated.In ZrO2CeO is added in ceramics2It is main to rise
Make ceramics that there is preferable mechanical property, CeO to the effect for stablizing tetragonal structure2Content is lower than 5%, tetragonal in solid solution
Type content is reduced, and mechanical property is deteriorated, and content is higher than 10%, Nb2O5It is difficult to be dissolved into ZrO2In lattice, ceramics are difficult to be sintered.
Nb2O5Effect be to improve the plasma etch resistance energy of ceramics, this is because Nb element ratio Zr element molecular weight is big,
When reacting the halide to be formed such as NbF with halogen5Compare ZrF4It is more difficult to volatilize, to have better plasma resistant rotten
Corrosion energy.Work as Nb2O5Content is lower than 1%, and the promotion of plasma resistant performance is unobvious, and content is higher than 5%, Nb2O5Be difficult to be dissolved into
ZrO2In lattice, ceramics are difficult to be sintered, while also will increase cost.
As preferred:
Each component is ground respectively, is referred to and is ground 12-36 hours in dehydrated alcohol.
Above-mentioned solid-solution material regrinding, refers to using distilled water as abrasive media, wet-milling 24-72 hours, and dry again
It is dry.
Above-mentioned molding, which refers to, is added the polyvinyl alcohol water solution that concentration is 5%, the poly- second of addition for the solid-solution material
Enol aqueous solution accounts for the 5% of the solid-solution material weight, then uses the compression moulding of 100-300Mpa pressure.
After above-mentioned solid-solution material molding, refers to and keep the temperature 8 hours at 1550-1650 DEG C.
Compared with prior art, beneficial effects of the present invention: using the resisting plasma corrosion of ceramics prepared by the present invention
Performance and yttrium-aluminium-garnet are suitable, even better than yttrium-aluminium-garnet, and bending strength is better than yttrium-aluminium-garnet ceramics, and cost is far low
In yttrium-aluminium-garnet, the manufacture material of etching machine inside cavity part may be used as.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1, a kind of preparation method of resisting plasma corrosion ceramics, with purity 99.9%ZrO2, 99.9%CeO2With
99.99%Nb2O5For starting material, by 0.9ZrO2·0.06CeO2·0.04Nb2O5Chemical ratio ingredient, in dehydrated alcohol
Grinding is dried after 12 hours, in 1500 DEG C of heat preservations, 6 hours synthesis 0.9ZrO after mixing2·0.06CeO2·0.04Nb2O5Solid solution
Then material is ground 24 hours by abrasive media rewetting of distilled water, the polyvinyl alcohol water that concentration is 5% is added in the material after drying
Solution, additional amount account for the 5% of powder total weight, then use the pressure compression moulding of 300Mpa, 1620 DEG C of heat preservations 8 in high temperature furnace
Hour, the resisting plasma corrosion ceramics that furnace cooling is.
Embodiment 2, a kind of preparation method of resisting plasma corrosion ceramics, with purity 99.9%ZrO2, 99.9%CeO2With
99.99%Nb2O5For starting material, by 0.9ZrO2·0.08CeO2·0.02Nb2O5Chemical ratio ingredient, in dehydrated alcohol
Grinding is dried after 36 hours, in minimum 6 hours synthesis 0.9ZrO of 1450 DEG C of heat preservations after mixing2·0.08CeO2·0.02Nb2O5Gu
Then solution material is ground 72 hours by abrasive media rewetting of distilled water, the polyethylene that concentration is 5% is added in the material after drying
Alcohol solution, additional amount account for the 5% of powder total weight, the pressure compression moulding of 300Mpa are then used, 1580 DEG C in high temperature furnace
Heat preservation 4 hours, the resisting plasma corrosion ceramics that furnace cooling is.
Embodiment 3, a kind of preparation method of resisting plasma corrosion ceramics, with purity 99.9%ZrO2, 99.9%CeO2With
99.99%Nb2O5For starting material, by 0.92ZrO2·0.06CeO2·0.02Nb2O5Chemical ratio ingredient, in dehydrated alcohol
Grinding is dried after 24 hours, in 1420 DEG C of heat preservations, 10 hours synthesis 0.92ZrO after mixing2·0.06CeO2·0.02Nb2O5Solid solution
Then body material is ground 48 hours by abrasive media rewetting of distilled water, the polyvinyl alcohol that concentration is 5% is added in the material after drying
Aqueous solution, additional amount account for the 5% of powder total weight, then use the pressure compression moulding of 100Mpa, 1560 DEG C of guarantors in high temperature furnace
Temperature 12 hours, the resisting plasma corrosion ceramics that furnace cooling is.
Embodiment 4, a kind of preparation method of resisting plasma corrosion ceramics, with purity 99.9%ZrO2, 99.9%CeO2With
99.99%Nb2O5For starting material, by 0.88ZrO2·0.09CeO2·0.03Nb2O5Chemical ratio ingredient, in dehydrated alcohol
Grinding is dried after 25 hours, in 1500 DEG C of heat preservations, 20 hours synthesis 0.88ZrO after mixing2·0.09CeO2·0.03Nb2O5Solid solution
Then body material is ground 30 hours by abrasive media rewetting of distilled water, the polyvinyl alcohol that concentration is 5% is added in the material after drying
Aqueous solution, additional amount account for the 5% of powder total weight, then use the pressure compression moulding of 200Mpa, 1580 DEG C of guarantors in high temperature furnace
Temperature 10 hours, the resisting plasma corrosion ceramics that furnace cooling is.
Embodiment 5, a kind of preparation method of resisting plasma corrosion ceramics, with purity 99.9%ZrO2, 99.9%CeO2With
99.99%Nb2O5For starting material, by 0.94ZrO2·0.05CeO2·0.01Nb2O5Chemical ratio ingredient, in dehydrated alcohol
Grinding is dried after 25 hours, in 1400 DEG C of heat preservations, 20 hours synthesis 0.94ZrO after mixing2·0.05CeO2·0.01Nb2O5Solid solution
Then body material is ground 30 hours by abrasive media rewetting of distilled water, the polyvinyl alcohol that concentration is 5% is added in the material after drying
Aqueous solution, additional amount account for the 5% of powder total weight, then use the pressure compression moulding of 300Mpa, 1650 DEG C of guarantors in high temperature furnace
Temperature 10 hours, the resisting plasma corrosion ceramics that furnace cooling is.
Embodiment 6, a kind of preparation method of resisting plasma corrosion ceramics, with purity 99.9%ZrO2, 99.9%CeO2With
99.99%Nb2O5For starting material, by 0.85ZrO2·0.1CeO2·0.05Nb2O5Chemical ratio ingredient, in dehydrated alcohol
Grinding is dried after 24 hours, in 1480 DEG C of heat preservations, 20 hours synthesis 0.85ZrO after mixing2·0.1CeO2·0.05Nb2O5Solid solution
Then body material is ground 30 hours by abrasive media rewetting of distilled water, the polyvinyl alcohol that concentration is 5% is added in the material after drying
Aqueous solution, additional amount account for the 5% of powder total weight, then use the pressure compression moulding of 1500Mpa, 1550 DEG C of guarantors in high temperature furnace
Temperature 10 hours, the resisting plasma corrosion ceramics that furnace cooling is.
Comparative example 1, using commercial high-purity YAG micro-powder (purity 99.9%), then using dehydrated alcohol as medium, with row
Planetary ball mill carries out mixing and ball-milling treatment, and the slurry after ball milling is dried for 24 hours in 80 DEG C of baking oven, the powder that will be prepared
It is fitted into graphite jig and hot pressed sintering is carried out by vacuum hotpressing stove, sintering atmosphere is Ar gas, and pressure 30MPa, sintering temperature is
1600 DEG C, soaking time 1h.
The test of resisting plasma corrosion rate is carried out to sample made from embodiment 1-4 and comparative example 1, test condition is such as
Shown in table 1:
The test condition of 1 plasma etching rate of table
Test result is as shown in table 2:
2 plasma etching rate of table
From embodiment 1-6 and comparative example 1 as can be seen that using the anti-etc. of resisting plasma corrosion ceramics prepared by the present invention
Gas ions corrosive nature and yttrium-aluminium-garnet are suitable, especially the resisting plasma corrosion ceramics of the preparation of embodiment 1, anticorrosive
Performance is obviously improved compared with yttrium-aluminium-garnet is compared to also having, and the bending strength of ceramics prepared by 6 embodiments is excellent
In yttrium-aluminium-garnet ceramics, and cost is far below yttrium-aluminium-garnet, may be used as the manufacture material of etching machine inside cavity part.
Finally, it should be noted that foregoing description is only the preferred embodiment of the present invention, the ordinary skill people of this field
Member under the inspiration of the present invention, without prejudice to the purpose of the present invention and the claims, can make multiple similar tables
Show, such transformation is fallen within the scope of protection of the present invention.
Claims (6)
1. a kind of resisting plasma corrosion ceramics, it is characterised in that: the chemical formula of the ceramics is (1-x-y) ZrO2·xCeO2·
yNb2O5, wherein x=0.05-0.1, y=0.01-0.05.
2. the preparation method of resisting plasma corrosion ceramics according to claim 1, it is characterised in that sequentially include the following steps:
Each component is weighed in proportion, each component is ground and dried respectively, is protected after then mixing each component at 1400-1500 DEG C
Warm minimum 6 hours synthesis solid-solution materials, after which is regrind and formed, in 1550-1650 DEG C of heat preservation 4-
12 hours, so that the plasma resistant corrosion ceramics be made.
3. the preparation method of resisting plasma corrosion ceramics according to claim 2, it is characterised in that: each component is ground respectively
Mill, refers to and grinds 12-36 hours in dehydrated alcohol.
4. the preparation method of the ceramics of the resisting plasma corrosion according to Claims 2 or 3, it is characterised in that: the solid solution
Material regrinding, refers to using distilled water as abrasive media, wet-milling 24-72 hours, and dry again.
5. the preparation method of resisting plasma corrosion ceramics according to claim 4, it is characterised in that: it is described molding refer to by
The polyvinyl alcohol water solution that concentration is 5% is added in the solid-solution material, and the polyvinyl alcohol water solution of addition accounts for the solid solution
Then the 5% of material weight uses the compression moulding of 100-300Mpa pressure.
6. the preparation method of resisting plasma corrosion ceramics according to claim 2, it is characterised in that: the solid-solution material
After molding, refers to and keep the temperature 8 hours at 1550-1650 DEG C.
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| US20060178010A1 (en) * | 2004-02-02 | 2006-08-10 | Toto Ltd. | Member having plasma-resistance for semiconductor manufacturing apparatus and method for producing the same |
| US20080264564A1 (en) * | 2007-04-27 | 2008-10-30 | Applied Materials, Inc. | Method of reducing the erosion rate of semiconductor processing apparatus exposed to halogen-containing plasmas |
| CN101357846A (en) * | 2007-08-02 | 2009-02-04 | 应用材料股份有限公司 | Plasma-resistant ceramics with controlled electrical resistivity |
| US20090191429A1 (en) * | 2008-01-24 | 2009-07-30 | Shin-Etsu Chemical Co., Ltd. | Ceramic sprayed member, making method, abrasive medium for use therewith |
| CN101671171A (en) * | 2008-09-12 | 2010-03-17 | 科发伦材料株式会社 | Ceramics for plasma treatment apparatus |
| JP2016056037A (en) * | 2014-09-05 | 2016-04-21 | 国立大学法人 香川大学 | Composite oxide ceramic and constituent member of semiconductor manufacturing equipment |
| CN107108374A (en) * | 2015-01-15 | 2017-08-29 | 东曹株式会社 | Translucency zirconia sintered body and its manufacture method with and application thereof |
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| Title |
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| SHIVA BEJUGAMA, AJOY KUMAR PANDEY: "Effect of Nb2O5 on sintering and mechanical properties of ceria stabilized zirconia", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Application publication date: 20191029 |