CN102513314B - Method for treating pollutant of workpiece provided with yttrium oxide coating layer - Google Patents
Method for treating pollutant of workpiece provided with yttrium oxide coating layer Download PDFInfo
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- CN102513314B CN102513314B CN201110454240.5A CN201110454240A CN102513314B CN 102513314 B CN102513314 B CN 102513314B CN 201110454240 A CN201110454240 A CN 201110454240A CN 102513314 B CN102513314 B CN 102513314B
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Abstract
The invention relates to a method for treating the pollutant of a workpiece which is provided with an yttrium oxide coating layer and is used for etching plasma, which comprises the steps of: at least adopting acid solution to wipe the workpiece, and then adopting deionized water to flush the workpiece. The treatment method can be used for leading the polluted workpiece such as a spray head, a focusing ring and the like to be used again.
Description
Technical field
The present invention relates to field of semiconductor manufacture, particularly relate to a kind of processing method with the pollutant of the workpiece of yittrium oxide clad for plasma etching.
Background technology
In recent years, in field of semiconductor manufacture, plasma etching is related in a lot of processing procedure, such as, relate to the plasma etching of silicon in the formation of TSV (Through Silicon Via), relate to the plasma etching of metal in the forming process of metal interconnecting wires, in transistor, the formation of grid relates to the etching of dielectric layer.Above-mentioned processing procedure generally plasma chamber indoor carry out, be provided with various workpieces in this chamber, such as focusing ring, spray first-class.
For spray head, its matrix of existing spray head is generally aluminium, but aluminium is easily corroded under plasma ambient, causes the life-span of this spray head not long.For this problem, by covering the strong aluminium oxide (Al of one deck anti-etching energy force rate aluminium at the outer surface of this matrix in prior art
2o
3), but, due to spray head its surface meeting and etching gas in use, be generally fluoro-gas, react, generate aluminum fluoride particle, this particle aggregation gets up, and easily drops on wafer to be etched, causes polluting, thus aluminium oxide is not the tectal preferred material of spray head, is produced gradually and the silicon of excellent heat dissipation performance (pyroconductivity: 149Wm in industry by contamination-free
-1k
-1) or carborundum (pyroconductivity: 150Wm
-1k
-1) cover layer replaced.But, silicon with or carborundum easily react with etching gas, cause spray head to shorten service life, for the problems referred to above, occurred that again etch resistance can better the spray head of yittrium oxide covering.
With above-mentioned in the anti-etching object of spray head mentioned similar, other surface of the work for plasma etching is generally all coated with yittrium oxide clad.
But the present inventor finds, after the workpiece with yittrium oxide clad uses a period of time, its surface has some pollutants, and this pollutant does not process, pile up to get up easily to drop on wafer to be etched, cause polluting, final reduction wafer manufacture efficiency.
In view of this, be necessary in fact to propose a kind of pollutant processing method with the workpiece of yittrium oxide clad for plasma etching, to avoid the problems referred to above.
Summary of the invention
The object that the present invention realizes proposes a kind of pollutant processing method with the workpiece of yittrium oxide clad for plasma etching, and contaminated workpiece is used again.
For achieving the above object, the invention provides a kind of pollutant processing method with the workpiece of yittrium oxide clad for plasma etching, comprising:
At least adopt workpiece described in acid solution wiping;
Adopt workpiece described in deionized water rinsing more afterwards.
Alternatively, ultrasonic oscillation is adopted in described deionized water rinsing process.
Alternatively, high pressure de-ionized water is adopted to clean in described deionized water rinsing process.
Alternatively, adopt in high pressure de-ionized water cleaning process, in described deionized water, comprise particle.
Alternatively, described particle comprises at least one in yittrium oxide, aluminium oxide, zirconia, silica.
Alternatively, the size range of described particle is 10nm-1mm.
Alternatively, the mass concentration of described particle is less than 50%.
Alternatively, adopt in high pressure de-ionized water cleaning process, the pressure range of described deionized water is 0.5MP-50MP.
Alternatively, the pressure range of described deionized water is 1MP-30MP.
Alternatively, the pressure range of described deionized water is 2MP-20MP.
Alternatively, in described deionized water rinsing process, the temperature of deionized water is more than 50 DEG C.
Alternatively, isopropyl alcohol is added with in deionized water in described deionized water rinsing process.
Alternatively, in described deionized water rinsing process, the temperature range of deionized water is 70 DEG C-120 DEG C, and the mass concentration of described isopropyl alcohol is less than 90%.
Alternatively, the scope of the mass concentration of described isopropyl alcohol is 1%-80%.
Alternatively, the scope of the mass concentration of described isopropyl alcohol is 1%-50%.
Alternatively, described acid solution is at least one in nitric acid, HF acid, hydrochloric acid.
Alternatively, described acid solution is hydrochloric acid, and in described hydrochloric acid, HCl mass concentration is in deionized water less than 90%.
Alternatively, in described hydrochloric acid, the scope of HCl mass concentration is in deionized water 1%-15%.
Alternatively, in described hydrochloric acid, the scope of HCl mass concentration is in deionized water 3%-10%.
Alternatively, before or after adopting workpiece described in acid solution wiping, also carry out the step using workpiece described in alkaline solution wiping, described alkaline solution is KOH solution, NaOH solution, NH
4at least one in OH solution.
Alternatively, described alkaline solution is NH
4oH solution, described NH
4nH in OH solution
4oH mass concentration is in deionized water less than 50%.
Alternatively, described NH
4nH in OH solution
4the scope of OH mass concentration is in deionized water 1%-30%.
Alternatively, described NH
4nH in OH solution
4the scope of OH mass concentration is in deionized water 1%-5%.
Alternatively, spray head step described in employing deionized water rinsing is also carried out after spray head step described in the wiping of employing alkaline solution.
Alternatively, in workpiece step described in the employing deionized water rinsing also carried out after adopting workpiece step described in alkaline solution wiping, adopt in the cleaning of ultrasonic oscillation, high pressure de-ionized water, deionized water and be added with isopropyl alcohol, the temperature of deionized water be 50 DEG C with upper at least one.
Compared with prior art, the present invention has the following advantages: have the workpiece of yittrium oxide clad in use after a period of time, it can produce some pollutants, the main component of this pollutant is the compound between fluorine, yttrium, aluminium, carbon and oxygen, and other contains the pollutant of metallic element as copper, titanium etc., by using acid solution can remove the poor pollutant of most of adhesive force, after adopting deionized water rinsing afterwards, contaminated spray head can be made again to be used;
Further, for the pollutant that small part adhesive force is stronger, in use deionized water rinsing process, adopt ultrasonic oscillation or adopt high pressure de-ionized water to remove;
Further, for the pollutant that indivedual adhesive force is extremely strong, the deionized water comprising particle is adopted to clean;
Further, because the wellability of isopropyl alcohol is very strong, is added with isopropyl alcohol in deionized water in deionized water rinsing process, the wetting capacity of deionized water on pollutant surface can be strengthened, be easy to make pollutant be cleaned removal;
Further, because aluminum fluoride is dissolved in hot water, in deionized water rinsing process, increase the temperature of water, aluminum fluoride can be made to be that the pollutant of base loosens on the face contacted with yittrium oxide, be easy to make pollutant be cleaned removal;
Further, because yittrium oxide is dissolved in acid, thus when removing pollutant, for preventing the performance damaging yittrium oxide, acid concentration in deionized water needs strict control.
Accompanying drawing explanation
Fig. 1 is the SEM test result of pollutant;
Fig. 2 is the EDS test result figure in Q region in Fig. 1;
Fig. 3 is the flow chart of the processing method of the pollutant that the embodiment of the present invention provides.
Detailed description of the invention
As described in the background art, there is the workpiece of yittrium oxide clad in use after a period of time, it can produce some pollutants, the present inventor has carried out SEM test and EDS analysis of spectrum to this pollutant, respectively as shown in Figures 1 and 2, its main component is fluorine to result, yttrium is the compound of base, carries out the present invention and proposes to use acid solution to remove the poor pollutant of most of adhesive force, after adopting deionized water rinsing afterwards, contaminated workpiece can be made again to be used.
For enabling above-mentioned purpose of the present invention, feature and advantage more become apparent, and are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Owing to focusing on, principle of the present invention is described, therefore, charts not in scale.
Below for spray head, Figure 3 shows that the pollutant process flow figure with the spray head of yittrium oxide clad that the embodiment of the present invention provides.Below in conjunction with Fig. 3, introduce the implementation process of this processing method in detail.
First perform step S11, employing isopropyl alcohol (IPA) wiping has the pollutant on the spray head of yittrium oxide clad.
The composition of this pollutant is noted earlier, and being mainly fluorine-containing etching gas and yittrium oxide clad in plasma etch process, to react the fluorine, the yttrium that produce be the compound of base.
The wetting capacity of isopropyl alcohol is very strong, after isopropyl alcohol is dissolved in the deionized water of subsequent step S12, can strengthen the wetting capacity that deionized water enters the interface of pollutant and yttrium oxide layer, is easy to cleaning in subsequent step and removes this pollutant.
Then perform step S12, adopt deionized water rinsing.For strengthening pollutant removal, can 1 in this step) use Ultrasonic Cleaning, 2) also isopropyl alcohol can be added in deionized water, 3) temperature of deionized water also can control more than 50 DEG C, also can 4) adopt high pressure de-ionized water cleaning.Above-mentioned four kinds of methods can use simultaneously, also can select a use, determine according to removal effect.
For 1), the hyperacoustic concrete frequency of employing and power are determined according to removal effect.
For 2), because isopropyl alcohol is volatile, thus, in washed with de-ionized water step, not easily excessive to the addition of isopropyl alcohol, the present inventor finds, in this step, the temperature range of deionized water is 70 DEG C-120 DEG C, when described isopropyl alcohol mass concentration is in deionized water less than 90%, can not affect the function of yittrium oxide and effectively can remove pollutant, preferably, the mass concentration scope of isopropyl alcohol is 1%-80%, more preferably, the mass concentration scope of described isopropyl alcohol is 1%-50%.
For 3), because aluminum fluoride is dissolved in hot water, in deionized water rinsing process, increase the temperature of water, aluminum fluoride can be made to be that the pollutant of base loosens on the face contacted with yittrium oxide, be easy to make pollutant be cleaned removal;
For 4), when adopting high pressure de-ionized water cleaning, the present inventor finds, when pressure range is 0.5MP-50MP, obvious to pollutant removal, preferably, the pressure range of deionized water is 1MP-30MP, and more preferably, the pressure range of deionized water is 2MP-20MP, under the prerequisite removing pollutant, the degree of infringement yittrium oxide is minimum.
In addition, adopt in high pressure de-ionized water cleaning process, the pollutant that the adhesive force all cannot removed for some said methods is extremely strong, can 5 be adopted) add particle in deionized water.This particle can increase this pollutant and be stripped the probability got off.In specific implementation process, this particle can comprise one or more in yittrium oxide, aluminium oxide, zirconia or silica, and particle size range is 10nm-1mm.Can also control the content of this particle, the present inventor finds, when the mass concentration of this particle in described deionized water is less than 50%, some can be adopted 1 simultaneously)-4) pollutant removal that cannot remove of method.
Then perform step S13, adopt acid solution wiping.Acid solution in this step can be hydrochloric acid, nitric acid or HF acid, owing to being dissolved in acid as tectal yittrium oxide, even wiping, also needs to control to need strict control to the concentration of acid.Hydrochloric acid is adopted in the present embodiment, the present inventor finds, when in this hydrochloric acid, HCl mass concentration is in deionized water less than 90%, the suitable control wiping time, namely can not damage clad yittrium oxide, can pollutant be removed again, preferably, in hydrochloric acid, the mass concentration scope of HCl is 1%-15%, and more preferably, in hydrochloric acid, the mass concentration scope of HCl is 3%-10%.
Then perform step S14, adopt deionized water rinsing.This step is identical with S12 step.But can from 1)-5) select one or more schemes scheme.Perform this step, the removing function of the pollutant peeled off from yttria surfaces can be strengthened.
Perform step S15 afterwards, adopt alkaline solution wiping.Alkaline solution in this step can be KOH solution, NaOH solution or NH
4oH solution.
NH is adopted in the present embodiment
4oH solution, described NH
4nH in OH solution
4oH mass concentration is in deionized water less than 50%, the acid solution do not washed before can neutralizing, and in addition, this alkaline solution also can react with pollutant, makes pollutant dissolve in alkaline solution and be removed.Preferably, described NH
4nH in OH solution
4oH mass concentration scope is in deionized water 1%-30%.More preferably, described NH
4nH in OH solution
4oH mass concentration scope is in deionized water 1%-5%.
Then perform step S16, adopt deionized water rinsing.This step is identical with S12 step.But can from 1)-5) select one or more schemes scheme.Perform this step, the removing function of the pollutant peeled off from yttria surfaces can be strengthened.
Perform step S17 afterwards, the spray head surface through above-mentioned process is checked, judges whether pollutant removal meets the requirements, if meet instructions for use, be then disposed, if undesirable, then re-execute step S13-S17, until meet the requirements.
It should be noted that, the step S11-S17 of foregoing description, each step is finished, and can adopt the deionized water rinsing in common process, to be washed by the pollutant peeled off from yttria surfaces in this step.
Spray head described in alkaline solution wiping is adopted in S15 step in the present embodiment, also can carry out before step S13 adopts spray head described in acid solution wiping, after the acid solution wiping carried out can neutralize in the alkaline solution wiping process formerly carried out, the alkaline solution do not washed completely.
Foregoing description be the flow process of the thing that depollutes of a standard, be suitable for batch processing.In specific implementation process, can part steps be selected, but at least need to carry out acid solution removal, adopt washed with de-ionized water two steps afterwards.
Described above is the handling process of the pollutant of spray head to coated yittrium oxide, and for other in plasma etching industrial, have the workpiece of yittrium oxide clad, such as the pollutant on focusing ring surface, its handling process is identical with above-mentioned flow process.
To sum up, the present invention has the following advantages: the workpiece with yittrium oxide clad is after for plasma etching a period of time, it can produce some pollutants, the main component of this pollutant is the compound between fluorine, yttrium, aluminium, carbon and oxygen, and other contains the pollutant of metallic element as copper, titanium etc., by using acid solution can remove the poor pollutant of most of adhesive force, after adopting deionized water rinsing afterwards, contaminated spray head can be made again to be used.
For the pollutant that small part adhesive force is stronger, 1 is adopted in use deionized water rinsing process) use ultrasonic oscillation, 2) also isopropyl alcohol can be added in deionized water, the wetting capacity of isopropyl alcohol is very strong, the wetting capacity of this deionized water to spray head surface contaminant can be strengthened, thus can fast by this pollutant removal; 3) temperature of deionized water also can control more than 50 DEG C, raise the temperature of deionized water solution, the solvability of the aqueous solution to aluminum fluoride pollutant can be strengthened, make aluminum fluoride be that the pollutant of base loosens on the face contacted with yittrium oxide, be easy to make pollutant be cleaned removal; Also can 4) adopt high pressure de-ionized water cleaning, little to the Yttrium oxide thin film extent of damage, reach the ability peeling off pollutant from yttria surfaces simultaneously.
For the pollutant that indivedual adhesive force is extremely strong, adopting 5) deionized water that comprises particle cleans.
Because yittrium oxide is easily dissolved in acid solution, thus acid concentration in deionized water needs strict control, and such as, when being hydrochloric acid, HCl mass concentration is in deionized water less than 90%.
Alkaline solution also carries out deionized water rinsing step after cleaning described spray head step, in this deionized water rinsing step, can adopt above-mentioned 1)-5) step, strengthen the removing function of the pollutant peeled off from yttria surfaces.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; the Method and Technology content of above-mentioned announcement can be utilized to make possible variation and amendment to technical solution of the present invention; therefore; every content not departing from technical solution of the present invention; the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong to the protection domain of technical solution of the present invention.
Claims (16)
1. for a processing method with the pollutant of the workpiece of yittrium oxide clad for plasma etching, it is characterized in that, the main component of described pollutant is the compound between fluorine, yttrium, aluminium, carbon and oxygen, and Yi Jitong, titanium, the treating method comprises:
At least adopt workpiece described in acid solution wiping, described acid solution is hydrochloric acid, and in described hydrochloric acid, HCl mass concentration scope is in deionized water 3%-10%;
Adopt workpiece described in high pressure de-ionized water rinse more afterwards, be added with isopropyl alcohol in deionized water in described deionized water rinsing process and comprise the particle that size range is 10nm-1mm, described particle is at least one in yittrium oxide, aluminium oxide, zirconia, silica.
2. processing method according to claim 1, is characterized in that, adopts ultrasonic oscillation in described deionized water rinsing process.
3. processing method according to claim 1, is characterized in that, the mass concentration of described particle is less than 50%.
4. processing method according to claim 1, is characterized in that, adopt in high pressure de-ionized water cleaning process, the pressure range of described deionized water is 0.5MPa-50MPa.
5. processing method according to claim 4, is characterized in that, the pressure range of described deionized water is 1MPa-30MPa.
6. processing method according to claim 5, is characterized in that, the pressure range of described deionized water is 2MPa-20MPa.
7. processing method according to claim 1, is characterized in that, in described deionized water rinsing process, the mass concentration of isopropyl alcohol is less than 90%.
8. processing method according to claim 7, is characterized in that, the mass concentration scope of described isopropyl alcohol is 1%-80%.
9. processing method according to claim 8, is characterized in that, the mass concentration scope of described isopropyl alcohol is 1%-50%.
10. processing method according to claim 1, is characterized in that, before or after adopting workpiece described in acid solution wiping, also carry out the step using workpiece described in alkaline solution wiping, described alkaline solution is KOH solution, NaOH solution, NH
4at least one in OH solution.
11. processing methods according to claim 10, is characterized in that, described alkaline solution is NH
4oH solution, described NH
4nH in OH solution
4oH mass concentration is in deionized water less than 50%.
12. processing methods according to claim 11, is characterized in that, described NH
4nH in OH solution
4oH mass concentration scope is in deionized water 1%-30%.
13. processing methods according to claim 12, is characterized in that, described NH
4nH in OH solution
4oH mass concentration scope is in deionized water 1%-5%.
14. processing methods according to claim 10, is characterized in that, also carry out workpiece step described in employing deionized water rinsing after adopting workpiece step described in alkaline solution wiping.
15. processing methods according to claim 14, it is characterized in that, in workpiece step described in the employing deionized water rinsing also carried out after adopting workpiece step described in alkaline solution wiping, adopt in the cleaning of ultrasonic oscillation, high pressure de-ionized water, deionized water and be added with isopropyl alcohol, the temperature of deionized water be 50 DEG C with upper at least one.
16. processing methods according to claim 1, is characterized in that, described workpiece is spray head or focusing ring.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110454240.5A CN102513314B (en) | 2011-12-29 | 2011-12-29 | Method for treating pollutant of workpiece provided with yttrium oxide coating layer |
| TW101129591A TWI580486B (en) | 2011-12-29 | 2012-08-15 | Treatment of contaminants in workpieces with yttrium oxide coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110454240.5A CN102513314B (en) | 2011-12-29 | 2011-12-29 | Method for treating pollutant of workpiece provided with yttrium oxide coating layer |
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| CN102513314B true CN102513314B (en) | 2014-12-31 |
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| CN103628079A (en) * | 2012-08-24 | 2014-03-12 | 宁波江丰电子材料有限公司 | Cleaning method for tantalum focus rings |
| CN103903948B (en) * | 2012-12-27 | 2017-06-13 | 中微半导体设备(上海)有限公司 | Improve the focusing ring of Waffer edge etch-rate uniformity |
| CN104028503B (en) * | 2014-05-30 | 2016-06-29 | 邢台晶龙电子材料有限公司 | The cleaning method of silicon material |
| CN104312774A (en) * | 2014-09-18 | 2015-01-28 | 高建 | Cleaning liquid for parts with yttrium oxide coating and cleaning method |
| CN108144906A (en) * | 2017-12-24 | 2018-06-12 | 苏州佳亿达电器有限公司 | A kind of surface impurity removal process of LED mouldings |
| CN114496710A (en) * | 2021-12-21 | 2022-05-13 | 上海富乐德智能科技发展有限公司 | Method for cleaning yttrium oxide coating of ceramic window of semiconductor equipment |
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| CN1910059A (en) * | 2003-09-17 | 2007-02-07 | 朗姆研究公司 | Methods for cleaning a set of structures comprising yttrium oxide in a plasma processing system |
| CN101194046A (en) * | 2004-06-09 | 2008-06-04 | 兰姆研究公司 | Wet cleaning method for quartz surface of component of plasma processing chamber |
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| EP1206326A1 (en) * | 1999-06-29 | 2002-05-22 | L-Tech Corporation | Chemical film cleaning and drying |
| JP2001110801A (en) * | 1999-10-05 | 2001-04-20 | Takeshi Yao | Pattern formation method, electronic element, optical element, and circuit substrate |
| US7479304B2 (en) * | 2002-02-14 | 2009-01-20 | Applied Materials, Inc. | Gas distribution plate fabricated from a solid yttrium oxide-comprising substrate |
| US20030190870A1 (en) * | 2002-04-03 | 2003-10-09 | Applied Materials, Inc. | Cleaning ceramic surfaces |
| DE20320727U1 (en) * | 2002-12-10 | 2005-04-07 | Semitool Inc | Workpiece processing system |
| CN101219429A (en) * | 2007-01-10 | 2008-07-16 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Method for cleaning quartz parts surface in polycrystal etching cavity |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1910059A (en) * | 2003-09-17 | 2007-02-07 | 朗姆研究公司 | Methods for cleaning a set of structures comprising yttrium oxide in a plasma processing system |
| CN101194046A (en) * | 2004-06-09 | 2008-06-04 | 兰姆研究公司 | Wet cleaning method for quartz surface of component of plasma processing chamber |
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| CN102513314A (en) | 2012-06-27 |
| TW201325744A (en) | 2013-07-01 |
| TWI580486B (en) | 2017-05-01 |
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Address after: 201201 No. 188 Taihua Road, Jinqiao Export Processing Zone, Pudong New Area, Shanghai Patentee after: Medium and Micro Semiconductor Equipment (Shanghai) Co., Ltd. Address before: 201201 No. 188 Taihua Road, Jinqiao Export Processing Zone, Pudong New Area, Shanghai Patentee before: Advanced Micro-Fabrication Equipment (Shanghai) Inc. |