CN113245279A - Method for cleaning ceramic parts - Google Patents
Method for cleaning ceramic parts Download PDFInfo
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- CN113245279A CN113245279A CN202110553437.8A CN202110553437A CN113245279A CN 113245279 A CN113245279 A CN 113245279A CN 202110553437 A CN202110553437 A CN 202110553437A CN 113245279 A CN113245279 A CN 113245279A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 228
- 238000004140 cleaning Methods 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 112
- 239000002245 particle Substances 0.000 claims abstract description 70
- 239000000243 solution Substances 0.000 claims abstract description 55
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 46
- 239000003929 acidic solution Substances 0.000 claims abstract description 36
- 239000000126 substance Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 68
- 238000002791 soaking Methods 0.000 claims description 42
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 239000012670 alkaline solution Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 7
- 239000004065 semiconductor Substances 0.000 claims description 7
- 239000002086 nanomaterial Substances 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000010408 sweeping Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 21
- 230000000694 effects Effects 0.000 description 10
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005237 degreasing agent Methods 0.000 description 1
- 239000013527 degreasing agent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- JVJQPDTXIALXOG-UHFFFAOYSA-N nitryl fluoride Chemical compound [O-][N+](F)=O JVJQPDTXIALXOG-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B08B1/143—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
Abstract
The embodiment of the invention provides a method for cleaning a ceramic part, which comprises the following steps: a first cleaning process, wherein particles on the ceramic piece are dissolved by adopting a chemical solution; in the second cleaning process, specified acidic solution is adopted to soften and corrode particles on the ceramic piece and eliminate a damaged layer on the ceramic piece; and in the third cleaning process, the ceramic piece is cleaned in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece. The ceramic part cleaning method provided by the embodiment of the invention can effectively remove suspended particles and a damaged layer on the ceramic part, thereby solving the problem that the number of ceramic particles exceeds the standard and improving the yield of chips.
Description
Technical Field
The invention relates to the field of semiconductor manufacturing, in particular to a method for cleaning a ceramic part.
Background
The integrated circuit is used as the foundation and the core of the information industry and is a global strategic industry which is related to national economy and social development. Because the dimensions of the trench and the line width in the integrated circuit are very small, tiny particles can cause great damage to the process result of a wafer (such as a silicon wafer), and the particle pollution problem seriously restricts the extension of the field of the integrated circuit to lower technical nodes. The particle control capability is also an important index for measuring the equipment stability and the process stability in the integrated circuit process, and especially the requirement for particle control in the current advanced process is higher and higher, which provides a greater challenge for the integrated circuit equipment.
The alumina ceramic is prepared from alumina (Al)2O3) The ceramic material as the main body is the most stable substance in oxide, and has the advantages of high temperature resistance, corrosion resistance, wear resistance, high mechanical strength, high hardness, high electrical insulation, low dielectric loss and the like, so that the alumina ceramic material is increasingly applied to semiconductor equipment. However, such materials inevitably produce some powdery particles on the surface during the molding process of granulation, sintering, machining, etc., and these particles, once dropped on the wafer during the semiconductor manufacturing process, may affect the process results, such as conduction of different wires, disconnection of the same wire, formation of voids, causing greater energy consumption and heat generation, etc. These particles, if not removed, can severely affect process results and chip yield.
In order to remove particles on the ceramic part, the ceramic part needs to be cleaned, but the existing ceramic part cleaning method is difficult to clean the ceramic part, and a damaged layer and suspended particles on the ceramic part still exist, so that the requirement on the number of the particles cannot be met.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art, and provides a ceramic part cleaning method which can effectively remove suspended particles and a damaged layer on a ceramic part, so that the problem that the number of ceramic particles exceeds the standard can be solved, and the yield of chips can be improved.
In order to achieve the purpose of the invention, the ceramic piece cleaning method comprises the following steps:
a first cleaning process, wherein particles on the ceramic piece are dissolved by adopting a chemical solution;
a second cleaning process, wherein specified acidic solution is adopted to soften and corrode particles on the ceramic piece and eliminate a damaged layer on the ceramic piece;
and in the third cleaning process, the ceramic piece is cleaned in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece.
Optionally, the specified acidic solution includes a fluoronitric acid solution, and the fluoronitric acid solution is formed by mixing a hydrofluoric acid solution, a nitric acid solution and pure water.
Optionally, the ratio of the hydrofluoric acid solution to the nitric acid solution to pure water with the resistivity of 18M omega cm is 1:1: 1; wherein the content of the first and second substances,
the hydrofluoric acid solution contains hydrofluoric acid in a mass fraction range of 5% or more and 15% or less; the nitric acid solution contains nitric acid with a mass fraction of 25% or more and 35% or less.
Optionally, the second washing process is performed at least 4 times before the third washing process is performed.
Optionally, the second cleaning process specifically includes the following steps:
s21, washing the ceramic piece by using the specified acidic solution;
s22, soaking the ceramic piece washed by the specified acidic solution in the specified acidic solution;
s23, washing the soaked ceramic piece by pure water;
s24, wiping the ceramic piece which is washed by pure water by using a grinding tool made of a nano material;
s25, soaking the wiped ceramic piece in deionized water, and carrying out ultrasonic cleaning;
and S26, washing the ceramic piece subjected to ultrasonic cleaning by using pure water.
Optionally, in step S21, the ceramic piece is washed with the specified acidic solution at least 3 times; in step S22, the ceramic piece washed with the specified acidic solution is soaked in the specified acidic solution for a soaking time ranging from 10min to 20 min; in the step S23, the ceramic piece after soaking is washed with pure water for 3 to 5 times; in the step S24, the ceramic piece rinsed with pure water is wiped for 3 to 5 times with a polishing tool made of a nano material; in step S25, the range of the cleaning time for the ultrasonic cleaning is 15min or more and 30min or less; in the step S26, the time for rinsing the ceramic piece after the ultrasonic cleaning with pure water is 15min or more and 60min or less.
Optionally, the first cleaning process specifically includes the following steps:
s11, wiping the ceramic piece by using a dust-free cloth stained with an isopropyl alcohol solution;
s12, soaking the wiped ceramic piece in alkaline solution, and carrying out ultrasonic cleaning;
s13, washing the ceramic piece subjected to ultrasonic cleaning by using pure water;
s14, soaking the washed ceramic piece in an acid solution;
s15, washing the ceramic piece soaked in the acidic solution by pure water;
and S16, soaking the washed ceramic piece in an alkaline solution.
Optionally, the purity of the isopropyl acetone solution is 99.7%; the alkaline solution is a KOH solution with the concentration percentage of more than or equal to 15 percent and less than or equal to 20 percent, and the temperature of the alkaline solution is more than or equal to 75 ℃ and less than or equal to 85 ℃; in step S12, the ultrasonic cleaning is performed for a time period of 1h or more and 3h or less; in the step S13, the ceramic piece after ultrasonic cleaning is washed 3 to 5 times with pure water; in the step S14, the ceramic piece after being washed is soaked in the acidic solution for a soaking time ranging from 5min to 10 min; in the step S15, the ceramic piece soaked in the acidic solution is washed with pure water for 3 to 5 times; in step S16, the ceramic piece after washing is soaked in the alkaline solution for a soaking time that is 1h or more and 3h or less.
Optionally, the third cleaning process specifically includes the following steps:
s31, washing the ceramic piece by pure water;
s32, soaking the washed ceramic piece in deionized water, and carrying out ultrasonic cleaning;
s33, soaking the ceramic piece subjected to ultrasonic cleaning in deionized water, always introducing new deionized water into the cleaning tank in the soaking process, and discharging the deionized water in the cleaning tank in an overflow mode;
and S34, blowing the soaked ceramic piece, and baking the ceramic piece after blowing.
Optionally, in step S31, the range of the rinsing time is greater than or equal to 45min and less than or equal to 60 min; in step S32, the ultrasonic cleaning is performed for a time period of 30min or more and 60min or less; in the step S33, the soaking time is greater than or equal to 30min and less than or equal to 60 min; in the step S33, the temperature of the deionized water is maintained within a range of 32 ℃ or more and 42 ℃ or less; in the step S34, the adopted purge gas includes nitrogen, and the purity of the nitrogen is 99.999%; the range of an included angle between the sweeping direction of the nitrogen and the surface of the ceramic piece is more than or equal to 30 ℃ and less than or equal to 45 ℃.
Optionally, the ceramic piece comprises a ceramic process kit for a semiconductor device.
The invention has the following beneficial effects:
according to the ceramic part cleaning method provided by the embodiment of the invention, cleaning is divided into three cleaning processes, wherein a first cleaning process adopts a chemical solution to dissolve particles on the ceramic part, and the process can effectively clean particles on blind holes, folds and non-welding seams with larger sizes on the surface of the ceramic part; the second cleaning process adopts a specified acidic solution to soften and corrode particles on the ceramic piece and eliminate a damaged layer on the ceramic piece, and because the existence of the damaged layer is one of important sources for generating the particles, compared with the prior art, the particles can be effectively removed from the source, so that the particle quantity can be greatly reduced; the third cleaning process adopts the ultrasonic cleaning mode to clean the ceramic parts to get rid of the residual granule and solution (acid or alkaline solution) on the ceramic parts, thereby can wash the ceramic parts comprehensively, finally can effectively improve the cleaning effect, solve the problem that ceramic granule quantity exceeds standard, improve the chip yield.
Drawings
FIG. 1 is a block flow diagram of a method for cleaning a ceramic part according to an embodiment of the present invention;
FIG. 2 is a block flow diagram of a second cleaning process employed by an embodiment of the present invention;
FIG. 3 is a block flow diagram of a first cleaning process employed by an embodiment of the present invention;
FIG. 4 is a block flow diagram of a third cleaning process employed by embodiments of the present invention;
FIG. 5 is a comparative graph of damage layers on a ceramic part obtained by a prior art ceramic part cleaning method and a ceramic part cleaning method according to an embodiment of the present invention, respectively;
fig. 6 is a graph showing a comparison of suspended particles on a ceramic article obtained by a ceramic article cleaning method according to the prior art and a ceramic article cleaning method according to an embodiment of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following describes the ceramic piece cleaning method provided by the embodiment of the present invention in detail with reference to the accompanying drawings.
The embodiment of the invention provides a method for cleaning a ceramic part, which can be applied to cleaning the ceramic parts of a process kit, a ceramic cover, a ceramic layer of an electrostatic chuck and the like of a process chamber in semiconductor equipment.
Specifically, referring to fig. 1, the method for cleaning the ceramic member includes:
a first cleaning process S1 of dissolving particles on the ceramic piece with a chemical solution;
the first cleaning process can effectively clean particles on the surface of the ceramic part, and particularly clean particles on blind holes, folds and non-welding gaps with large sizes on the surface of the ceramic part.
A second cleaning process S2 of softening and etching the particles on the ceramic member and removing the damaged layer on the ceramic member with a prescribed acidic solution;
since the existence of the damage layer is one of the important sources of particle generation, compared with the prior art, the particles can be effectively removed at the source, thereby greatly reducing the number of particles.
The third cleaning process S3 is to clean the ceramic part by ultrasonic cleaning to remove the residual particles and solution on the ceramic part.
The ultrasonic cleaning is to clean particles on the ceramic member by water waves generated by ultrasonic oscillation. The third cleaning process S3 can clean the ceramic pieces comprehensively, and can effectively improve the cleaning effect finally.
Specifically, in the second cleaning process S2, the predetermined acidic solution includes a nitric fluoride solution mixed with a hydrofluoric acid solution, a nitric acid solution, and pure water, and is capable of softening particles on the ceramic material and removing a damaged layer on the ceramic material. Of course, in practical application, any other acidic solution that can perform the same function may be used.
In order to enhance the softening and eliminating effects on the damaged layer on the ceramic piece, optionally, the ratio of the hydrofluoric acid solution to the nitric acid solution to the pure water with the resistivity of 18M omega cm is 1:1: 1; wherein the hydrofluoric acid solution contains hydrofluoric acid with a mass fraction range of more than or equal to 5% and less than or equal to 15%; the nitric acid solution contains nitric acid in a mass fraction of 25% or more and 35% or less.
In order to enhance the above softening and removal of the damage layer on the ceramic member, optionally, the above-mentioned second cleaning process S2 is performed at least 4 times before the third cleaning process S3 is performed.
A detailed description will be given of a specific embodiment of the above-described second cleaning process S2. Specifically, as shown in fig. 2, the second cleaning process S2 specifically includes the following steps:
s21, washing the ceramic piece by adopting the specified acidic solution;
optionally, in step S21, the ceramic piece is rinsed at least 3 times with the specified acidic solution.
S22, soaking the ceramic piece washed by the specified acidic solution in the specified acidic solution;
optionally, in step S22, the ceramic piece washed with the specified acidic solution is soaked in the specified acidic solution for a soaking time that is greater than or equal to 10min and less than or equal to 20 min.
S23, washing the soaked ceramic piece by pure water;
optionally, in step S23, the soaked ceramic member is washed 3 to 5 times with pure water.
S24, wiping the ceramic piece washed by pure water by using a polishing tool made of a nano material;
optionally, in step S24, the ceramic member that has been washed with pure water is wiped for 3 to 5 times by using a polishing tool made of a nano material.
S25, soaking the wiped ceramic piece in deionized water, and carrying out ultrasonic cleaning;
optionally, in step S25, the range of the cleaning time for performing the ultrasonic cleaning is 15min or more and 30min or less.
And S26, washing the ceramic piece subjected to ultrasonic cleaning by using pure water.
Optionally, in step S26, the time for rinsing the ceramic piece after ultrasonic cleaning with pure water is greater than or equal to 15min and less than or equal to 60 min.
A detailed description will be given of a specific embodiment of the above-described first cleaning process S1. Specifically, as shown in fig. 3, the first cleaning process S1 specifically includes the following steps:
s11, wiping the ceramic piece by using a dust-free cloth stained with an isopropyl alcohol (IPA) solution;
the above step S11 may conduct electricity to the ceramic piece to neutralize the charged ceramic particles on the ceramic piece.
Optionally, the purity of the above-mentioned isopropyl alcohol solution is 99.7%.
It should be noted that if the surface of the dust-free cloth is stained, the dust-free cloth needs to be cleaned again to avoid damaging the texture and smooth surface of the ceramic piece surface.
S12, soaking the wiped ceramic piece in alkaline solution, and carrying out ultrasonic cleaning;
the alkaline solution can dissolve particles on the ceramic piece, and the particles can be effectively removed by combining ultrasonic cleaning.
In order to effectively dissolve particles on the ceramic piece and improve the cleaning effect, optionally, the alkaline solution is, for example, a KOH solution with a concentration percentage ranging from 15% to 20%, and the temperature of the alkaline solution ranges from 75 ° to 85 °; in step S12, the ultrasonic cleaning time is set in the range of 1h or more and 3h or less, which can not only effectively dissolve the particles on the ceramic piece, but also prevent the sealing surface and the hole edge of the ceramic piece from being damaged and affecting the sealing performance of the part due to the excessively long soaking time of the ceramic piece in the alkaline solution.
In practical application, a concentration detector can be used to detect the concentration value of the KOH solution, and replace or supplement the solution according to the detected concentration value, so as to reach the target concentration value.
S13, washing the ceramic piece subjected to ultrasonic cleaning by using pure water;
optionally, in step S13, the ceramic member after ultrasonic cleaning is washed 3 to 5 times with pure water.
S14, soaking the washed ceramic piece in an acid solution;
the step S14 can neutralize the alkaline solution remaining on the ceramic part to reduce the corrosion of the alkaline solution to the ceramic part and avoid the damage of the alkaline solution to the sealing surface and the hole edge of the ceramic part.
Optionally, in step S14, the ceramic piece after being washed is soaked in the acidic solution for a soaking time that is greater than or equal to 5min and less than or equal to 10 min.
Optionally, the acidic solution is hydrochloric acid or a fluoronitric acid solution, wherein the fluoronitric acid solution has a better dissolving effect with an alkaline solution (for example, KOH solution).
In addition, the step S14 may not use ultrasonic cleaning.
S15, washing the ceramic piece soaked in the acid solution by pure water;
and S16, soaking the washed ceramic piece in an alkaline solution.
The above step S16 may further dissolve the particles on the ceramic piece.
Optionally, in step S16, the soaking time of the ceramic part after washing in the alkaline solution is set to be greater than or equal to 1 hour and less than or equal to 3 hours, and the soaking time is set in the above range, so that the particles on the ceramic part can be effectively dissolved, and the sealing surface and the hole edge of the ceramic part can be prevented from being damaged due to too long soaking time of the ceramic part in the alkaline solution, which affects the sealing performance of the part.
A detailed description will be given below of a specific embodiment of the above-described third cleaning process S3. Specifically, as shown in fig. 4, the third cleaning process S3 specifically includes the following steps:
s31, washing the ceramic piece by pure water;
optionally, in step S31, the range of the rinsing time is greater than or equal to 45min and less than or equal to 60 min;
s32, soaking the washed ceramic piece in deionized water, and carrying out ultrasonic cleaning;
the step S32 can be used for comprehensively cleaning the ceramic piece, and the cleaning effect of ultrasonic cleaning by using deionized water is most obvious, so that after the ultrasonic cleaning step is completed, the cleaning effect of the ceramic piece can be ensured to meet the process requirement. Also, the removal of the damaged layer and the suspended particles has been achieved using the previous first and second cleaning processes S1 and S2, so that it is possible to make up for the shortage that the ultrasonic cleaning cannot completely remove the damaged layer and the suspended particles.
Optionally, in step S32, the ultrasonic cleaning is performed for a time period of 30min or more and 60min or less.
Optionally, the deionized water has a resistivity of 4M Ω · cm or more.
S33, soaking the ceramic piece subjected to ultrasonic cleaning in deionized water, always introducing new deionized water into the cleaning tank in the soaking process, and discharging the deionized water in the cleaning tank in an overflow mode;
in the step S33, new deionized water is always introduced into the cleaning tank during the soaking process, and the deionized water in the cleaning tank is discharged in an overflow manner, so that the deionized water can be in a circulating flow state, and the cleaning effect can be further improved.
Optionally, in step S33, the temperature of the deionized water is maintained within a range of 32 ℃ or higher and 42 ℃ or lower.
And S34, blowing the soaked ceramic piece, and baking the ceramic piece after blowing.
Optionally, the purge gas used in step S34 includes nitrogen, and the purity of the nitrogen is 99.999%; the included angle between the purging direction of the nitrogen and the surface of the ceramic piece is more than or equal to 30 ℃ and less than or equal to 45 ℃ so as to prevent the particles from falling on the surface of the ceramic piece again.
Optionally, firstly, completely purging the ceramic piece by using dry nitrogen; then purging the purification furnace (or oven) with dry nitrogen gas to dry the inside thereof; finally, the ceramic piece is put into a purging purification furnace (or an oven) for baking.
Next, a comparative experiment will be performed on the ceramic parts obtained by the ceramic part cleaning method in the prior art and the ceramic part cleaning method provided in the embodiment of the present invention. Specifically, the ceramic part cleaning method in the prior art comprises the following steps: firstly, soaking the ceramic piece in an alkaline degreasing agent for 50-80 min, and then putting the ceramic piece into deionized water for rinsing (spraying pressurized deionized water on all parts of the surface of the ceramic piece); and then, immersing the ceramic piece in an acid solution for 5min-10min, taking out the ceramic piece from the solution, immersing the ceramic piece in deionized water again for rinsing, immersing the ceramic piece in deionized water with the resistivity of more than or equal to 4M omega cm and normal temperature for ultrasonic cleaning for 10min-15min, immersing the ceramic piece in deionized water with the resistivity of more than or equal to 8M omega cm for hot water immersion cleaning, finally, blowing the ceramic piece with nitrogen, and drying the ceramic piece to finish the whole cleaning process.
The ceramic piece cleaning method provided by the embodiment of the invention comprises the three cleaning processes S1-S3, wherein the first cleaning process S1 comprises the steps S11-S16; the second cleaning process S2 includes the above-described steps S21-S26; the third cleaning process S3 includes the above-described steps S31-S34.
Fig. 5 is a comparative diagram of damaged layers on a ceramic part obtained by a ceramic part cleaning method in the prior art and a ceramic part cleaning method provided in an embodiment of the present invention, respectively. In the ceramic member obtained by the cleaning method of the prior art in combination with the experimental data and shown in fig. 5, the surface layer still has a machining damage layer, as shown in (a) of fig. 5, the thickness of the damage layer is 10 μm to 30 μm, and the existence of the damage layer is one of the important sources of particle generation. In contrast, as can be seen from fig. 5 (b), the damaged layer on the ceramic part obtained by the ceramic part cleaning method provided by the embodiment of the present invention is significantly removed, so that particles of the ceramic part are prevented from continuously falling off during the use of the ceramic part on the equipment.
Fig. 6 is a graph showing a comparison of suspended particles on a ceramic article obtained by a ceramic article cleaning method according to the prior art and a ceramic article cleaning method according to an embodiment of the present invention. In the ceramic member obtained by the cleaning method of the prior art according to the experimental data and shown in fig. 6, suspended particles of 0.2 μm to 1 μm still exist on the ceramic surface, as shown in fig. 6 (a), and black areasThe white dots on the surface are suspended particles. In addition, the ceramic part obtained by the ceramic part cleaning method in the prior art has the particle number per unit area of more than or equal to 500ea which falls on the wafer in the process and is far higher than the particle index (the particle number per unit area)<2ea), and further, the measured value obtained by measuring the liquid particle count (i.e., LPC) on the ceramic piece was 75856PA/cm2. In contrast, as can be seen from the graph (b) in fig. 6, the white dots on the black area in the graph are significantly reduced, and thus it can be seen that the ceramic article obtained by the ceramic article cleaning method provided by the embodiment of the present invention has significantly reduced suspended particles, and the number of particles per unit area of the ceramic article falling on the wafer during the process is lower than the particle index (the number of particles per unit area of the ceramic article is lower than the particle index)<2ea), and a detection value of measuring LPC acquisition thereof is 729PA/cm2Much smaller than the above-mentioned LPC detection values of the prior art.
The ceramic article in the embodiment of the present invention includes, for example, a ceramic process kit for a semiconductor apparatus. The ceramic process kit can be parts such as a lining, a medium window, a nozzle, a sieve tube, a main medium cylinder and an auxiliary medium cylinder of a three-dimensional induction coil, an observation window protection cylinder and the like which are made of ceramic materials. By improving the cleaning effect of the parts, the problem that the quantity of ceramic particles exceeds the standard can be effectively solved, and the yield of chips is improved.
In summary, the cleaning method for the ceramic part provided by the embodiment of the invention divides the cleaning into three cleaning processes, wherein the first cleaning process adopts a chemical solution to dissolve particles on the ceramic part, and the process can effectively clean particles on the blind holes, folds and non-welding gaps with larger sizes on the surface of the ceramic part; the second cleaning process adopts a specified acidic solution to soften and corrode particles on the ceramic piece and eliminate a damaged layer on the ceramic piece, and because the existence of the damaged layer is one of important sources for generating the particles, compared with the prior art, the particles can be effectively removed from the source, so that the particle quantity can be greatly reduced; the third cleaning process adopts the ultrasonic cleaning mode to clean the ceramic parts to get rid of the residual granule and solution (acid or alkaline solution) on the ceramic parts, thereby can wash the ceramic parts comprehensively, finally can effectively improve the cleaning effect, solve the problem that ceramic granule quantity exceeds standard, improve the chip yield.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (11)
1. A method of cleaning a ceramic part, comprising:
a first cleaning process, wherein particles on the ceramic piece are dissolved by adopting a chemical solution;
a second cleaning process, wherein specified acidic solution is adopted to soften and corrode particles on the ceramic piece and eliminate a damaged layer on the ceramic piece;
and in the third cleaning process, the ceramic piece is cleaned in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece.
2. The ceramic piece cleaning method according to claim 1, wherein the specified acidic solution includes a fluoronitric acid solution mixed by a hydrofluoric acid solution, a nitric acid solution, and pure water.
3. The ceramic piece cleaning method according to claim 2, wherein the ratio of the hydrofluoric acid solution to the nitric acid solution to pure water having a resistivity of 18M Ω -cm is 1:1: 1; wherein the content of the first and second substances,
the hydrofluoric acid solution contains hydrofluoric acid in a mass fraction range of 5% or more and 15% or less; the nitric acid solution contains nitric acid with a mass fraction of 25% or more and 35% or less.
4. A method for cleaning ceramic parts according to any one of claims 1-3, characterized in that the second cleaning process is performed at least 4 times before the third cleaning process is performed.
5. A method for cleaning ceramic parts according to any one of claims 1-3, characterized in that the second cleaning process comprises the following steps:
s21, washing the ceramic piece by using the specified acidic solution;
s22, soaking the ceramic piece washed by the specified acidic solution in the specified acidic solution;
s23, washing the soaked ceramic piece by pure water;
s24, wiping the ceramic piece which is washed by pure water by using a grinding tool made of a nano material;
s25, soaking the wiped ceramic piece in deionized water, and carrying out ultrasonic cleaning;
and S26, washing the ceramic piece subjected to ultrasonic cleaning by using pure water.
6. The ceramic part cleaning method according to claim 5, wherein in the step S21, the ceramic part is washed at least 3 times with the specified acidic solution; in step S22, the ceramic piece washed with the specified acidic solution is soaked in the specified acidic solution for a soaking time ranging from 10min to 20 min; in the step S23, the ceramic piece after soaking is washed with pure water for 3 to 5 times; in the step S24, the ceramic piece rinsed with pure water is wiped for 3 to 5 times with a polishing tool made of a nano material; in step S25, the range of the cleaning time for the ultrasonic cleaning is 15min or more and 30min or less; in the step S26, the time for rinsing the ceramic piece after the ultrasonic cleaning with pure water is 15min or more and 60min or less.
7. The ceramic piece cleaning method according to claim 1, wherein the first cleaning process specifically comprises the steps of:
s11, wiping the ceramic piece by using a dust-free cloth stained with an isopropyl alcohol solution;
s12, soaking the wiped ceramic piece in alkaline solution, and carrying out ultrasonic cleaning;
s13, washing the ceramic piece subjected to ultrasonic cleaning by using pure water;
s14, soaking the washed ceramic piece in an acid solution;
s15, washing the ceramic piece soaked in the acidic solution by pure water;
and S16, soaking the washed ceramic piece in an alkaline solution.
8. The ceramic part cleaning method according to claim 7, wherein the purity of the isopropyl alcohol solution is 99.7%; the alkaline solution is a KOH solution with the concentration percentage of more than or equal to 15 percent and less than or equal to 20 percent, and the temperature of the alkaline solution is more than or equal to 75 ℃ and less than or equal to 85 ℃; in step S12, the ultrasonic cleaning is performed for a time period of 1h or more and 3h or less; in the step S13, the ceramic piece after ultrasonic cleaning is washed 3 to 5 times with pure water; in the step S14, the ceramic piece after being washed is soaked in the acidic solution for a soaking time ranging from 5min to 10 min; in the step S15, the ceramic piece soaked in the acidic solution is washed with pure water for 3 to 5 times; in step S16, the ceramic piece after washing is soaked in the alkaline solution for a soaking time that is 1h or more and 3h or less.
9. The ceramic piece cleaning method according to claim 1, wherein the third cleaning process specifically comprises the steps of:
s31, washing the ceramic piece by pure water;
s32, soaking the washed ceramic piece in deionized water, and carrying out ultrasonic cleaning;
s33, soaking the ceramic piece subjected to ultrasonic cleaning in deionized water, always introducing new deionized water into the cleaning tank in the soaking process, and discharging the deionized water in the cleaning tank in an overflow mode;
and S34, blowing the soaked ceramic piece, and baking the ceramic piece after blowing.
10. The ceramic piece cleaning method according to claim 9, wherein in the step S31, the rinsing time is in a range of 45min or more and 60min or less; in step S32, the ultrasonic cleaning is performed for a time period of 30min or more and 60min or less; in the step S33, the soaking time is greater than or equal to 30min and less than or equal to 60 min; in the step S33, the temperature of the deionized water is maintained within a range of 32 ℃ or more and 42 ℃ or less; in the step S34, the adopted purge gas includes nitrogen, and the purity of the nitrogen is 99.999%; the range of an included angle between the sweeping direction of the nitrogen and the surface of the ceramic piece is more than or equal to 30 ℃ and less than or equal to 45 ℃.
11. A method for cleaning ceramic parts according to any one of claims 1-10, wherein the ceramic parts comprise ceramic process kits for semiconductor equipment.
Priority Applications (3)
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| CN202110553437.8A CN113245279A (en) | 2021-05-20 | 2021-05-20 | Method for cleaning ceramic parts |
| PCT/CN2022/092423 WO2022242539A1 (en) | 2021-05-20 | 2022-05-12 | Ceramic piece cleaning method |
| TW111117910A TWI828146B (en) | 2021-05-20 | 2022-05-12 | Cleaning method for ceramic parts |
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| CN202110553437.8A CN113245279A (en) | 2021-05-20 | 2021-05-20 | Method for cleaning ceramic parts |
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| CN (1) | CN113245279A (en) |
| TW (1) | TWI828146B (en) |
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| WO2022242539A1 (en) * | 2021-05-20 | 2022-11-24 | 北京北方华创微电子装备有限公司 | Ceramic piece cleaning method |
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Also Published As
| Publication number | Publication date |
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| TWI828146B (en) | 2024-01-01 |
| WO2022242539A1 (en) | 2022-11-24 |
| TW202245924A (en) | 2022-12-01 |
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