CN1500857A - Aqueous cleaning liquid combination for flatted chemically machinery - Google Patents
Aqueous cleaning liquid combination for flatted chemically machinery Download PDFInfo
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- CN1500857A CN1500857A CNA021486034A CN02148603A CN1500857A CN 1500857 A CN1500857 A CN 1500857A CN A021486034 A CNA021486034 A CN A021486034A CN 02148603 A CN02148603 A CN 02148603A CN 1500857 A CN1500857 A CN 1500857A
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Abstract
The aqueous cleaning composition includes quaternary ammonium salt and/or alcohol amine in 0.1-10 wt% and non-ionic interface activator containing polyethylene glycol alcohol in the end or branch chain in 0.0001-0.2 wt% except water. It has low surface tension and thus good moistening effect, and can eliminate surface pollutant on the surface of copper chip after chemical and mechanical flattening treatment. In addition, the aqueous cleaning composition may be produced into high concentration liquid for convenient storage and transportation.
Description
Technical field
The invention relates in the semiconductor rear section processing procedure,, remove the silicon surface contaminant behind chemical-mechanical planarization in copper wiring effectively, be beneficial to the carrying out of processing procedures such as subsequent thin film deposition, little shadow with the cleaning combination that particular chemical is formed.
Background technology
In cmp (Chemical Mechanical Polishing, in process of lapping CMP), a large amount of fine ground particle and chemical assistant in the lapping liquid, and the chip of being peeled off in the process of lapping may be attached to chip surface.General chip common pollutent after grinding is metal ion, organic compound or abrasive grains etc., if no effective wash procedure is removed above-mentioned pollutent, then will influence the carrying out of successive process and the yield and the reliability of reduction assembly.Therefore, the manufacturing process for cleaning after CMP grinds has become the gordian technique whether CMP can successfully be applied to manufacture of semiconductor.
United States Patent (USP) the 6th, 044 discloses cleaning combination behind a kind of CMP for No. 851, and it contains tetralkyl ammonium fluorides (tetraalkylammonium fluoride).United States Patent (USP) the 6th, 030 also discloses cleaning combination behind a kind of CMP of fluorochemicals for No. 932.But the waste water of their halogen-containing cleaning combination is difficult for handling, and causes environmental pollution easily.
Recently the chip cleaning step is to utilize the chip cleaning machine that comprises polyvinyl alcohol (PVA) brush mostly behind the chemical-mechanical planarization, and it is directly to contact with chip surface by the PVA brush, brushes chip surface micronic dust and etched wafer surface.Then, shake cleaning with MHz ultrasound (megasonic) cleaning technique.At last, borrow pharmaceutical chemicals microetch chip surface such as acid solution and dissolve specific pollutent to remove the pollution on top layer.
Semiconductor subassembly now, towards littler live width, more the direction of high volume density develops, when the unicircuit minimum feature is reduced to below 0.25 micron, because the resistance and the caused time lag of dielectric layer stray capacitance (RC delay) of plain conductor itself, oneself becomes the main key that influences the assembly arithmetic speed.Therefore, in order to improve the arithmetic speed of assembly, the semi-conductor dealer is towards adopting than low-k material (low K dielectrics) and utilizing the copper plain conductor to replace traditional aluminum-copper alloy lead, with the conduction speed of raising unicircuit and the arithmetic speed of assembly at present.
The representative low-k material that often comes into question at present is as shown in table 1, this material surface is hydrophobicity mostly, cause the aqueous clean combination often can't effective wetting material surface, thereby can't effectively contact with the pollutent on the material surface and act on.Still need seek in the stock trick skill a kind of can be effectively moistening and the scavenging solution of cleaning low-k material surface.
Table 1: representative low-k material basic physical properties
| Low dielectric material | ???SiLK (notes) | Porousness SiLK film | Amorphous phase hydrogenated silicon carbide (SiC:H) |
| Dielectric coefficient | ????2.65 | ????＜2.40 | ????5.1±0.01 |
| Contact angle to water | ????73.7° | ????87.1° | ????81.2° |
| The material surface hydrophilic and hydrophobic | Hydrophobic | Hydrophobic | Hydrophobic |
Annotate: SiLK is the low-k material trade(brand)name that Dow Chemical is developed.
This case the contriver find through broad research, and the cleaning combination with some special component is applicable to PVA chip cleaning machine, can remove the pollutent on the chip surface after the chemical mechanical planarization in the copper wiring effectively.
Summary of the invention
Main purpose of the present invention is to provide a kind of aqueous clean combination that is used for the post-chemical mechanical planarization, and its main composition is non-ionic interfacial agent and the water that quarternary ammonium salt or hydramine or its mixture, end or side chain contain Volpo S 10.
The present invention relates to a kind of aqueous clean combination that is used for behind the chemical-mechanical planarization, it comprises:
(a) quarternary ammonium salt of 0.1 to 10 weight % or hydramine or its mixture;
(b) 0.0001 to 0.2 weight % end or side chain contain Volpo S 10 [(OCH
2CH
2)
nOH] non-ionic interfacial agent of (wherein n is 1 to 30 numerical value); And
(c) water.
Described composition preferably has the pH value between 7 to 14.
Said composition preferably has the pH value between 9 to 12.5.
Described quarternary ammonium salt system is preferably selected from tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide or tetrabutylammonium, or two or the mixture of multiple this quaternary ammonium compound.
This hydramine is preferably selected from thanomin, diethanolamine, trolamine, Propanolamine, Mono Methyl Ethanol Amine or methyldiethanolamine, or two or the mixture of multiple this hydramine.
Preferably, the consumption of this quarternary ammonium salt or hydramine or its mixture is 0.1 to 5 weight %.
Described should end or the side chain non-ionic interfacial agent that contains Volpo S 10 be preferably selected from non-ionic interfacial agent with following formula (I) structure:
Wherein, n is 1 to 30 numerical value; R
1, R
2, R
3And R
4Respectively be hydrogen or C
1-C
6Alkyl; And
R
5Be hydrogen or C
1-C
6Alkyl or-(OCH
2CH
2)
mOH, wherein m is 1 to 30 numerical value.
Preferably, described composition further comprises the organic acid with sequestering power.
Described organic acid is preferably selected from propanedioic acid, pentanedioic acid, hexanodioic acid, oxalic acid, citric acid, oxysuccinic acid or tartrate or above-mentioned two or the mixture of multiple acid.
Described organic acid preferable amount is 0.1 to 10 weight %.
Preferably, described composition also comprises multicomponent alcoholics compound.
Described multicomponent alcoholics compound is preferably selected from ethylene glycol, 1, ammediol, butyleneglycol, glycol ether or two or the mixture of multiple this alcohol compound.
Preferably, the consumption of multicomponent alcoholics compound is 0.1 to 5 weight %.
Preferably, described composition also comprises corrosion inhibitor.
Preferably, described corrosion inhibitor is a triazole compounds.
Preferably, described triazole compounds is benzotriazole and/or its derivative.
The consumption of described corrosion inhibitor is preferably 0.001 to 0.5 weight %.
Preferably, but the highly enriched scavenging solution of described composition simmer down to.
Preferably, described highly enriched scavenging solution comprises quarternary ammonium salt or hydramine or its mixture of (a) 15 to 40 weight %; (b) non-ionic interfacial agent of 0.001 to 2 weight %; Reach (c) water.
Compared with prior art, the present composition has following beneficial effect:
1. cleaning combination surface tension of the present invention is low, especially has good wettability effect to being hydrophobic material (as the dielectric material of low-k) on the chip, this good wettability makes scavenging solution can effectively contact and act on chip, so can promote cleaning performance;
2. cleaning combination of the present invention do not contain can to various materials on copper, dielectric materials and the wafer cause heavy corrosion as chemical substances such as hydrofluoric acid, hydrochloric acid, sulfuric acid and ammoniacal liquor; And
3. the not halogen-containing and phenyl ring of cleaning combination of the present invention, its metal content is less than 1ppm, so its waste is very little to the influence of environment simultaneously.
Description of drawings
Fig. 1: the water (A) and the present composition (B) are to the wetting effect comparison diagram of low-k material.
Embodiment
The invention relates to a kind of aqueous clean combination that is used for the post-chemical mechanical planarization, it comprises quarternary ammonium salt or hydramine or its mixture of 0.1 to 10 weight %; 0.0001 contain [(OCH to 0.2 weight % end or side chain
2CH
2)
nOH] the Volpo S 10 non-ionic interfacial agent and the water of functional group.
But cleaning combination mat of the present invention adds alkali, and is as KOH, to adjust the pH value between 7 to 14, preferable between 9 to 12.5.
Quarternary ammonium salt used in the present invention there is no particular restriction, and it is a personage institute well known of haveing the knack of this technology.The quarternary ammonium salt that can be used among the present invention for example can be selected from tetramethyl ammonium hydroxide (TMAH, tetramethyl ammonium hydroxide), tetraethyl ammonium hydroxide (TEAH, tetraethyl ammonium hydroxide), tetrapropylammonium hydroxide (TPAH, tetraproplyammonium hydroxide) or tetrabutylammonium (TBAH, or two or the mixture of multiple this quarternary ammonium salt tetrabutyl ammonium hydroxide).
Hydramine used in the present invention there is no particular restriction, and it is also for haveing the knack of the personage institute well known of this technology.United States Patent (USP) the 6th, 194 has disclosed the hydramine kind that can be used in the CMP cleaning combination of back for No. 366, and the content of this patent is incorporated herein for referencial use now.Therefore, can be used for hydramine among the present invention and for example can be selected from thanomin (ethanolamine), diethanolamine (Diethanolamine), trolamine (triethanolamine), Propanolamine (3-amino-1-propanol), Mono Methyl Ethanol Amine (methylethanolamine), and methyldiethanolamine (methyldiethanolamine), or two or the mixture of multiple this hydramine.
Quarternary ammonium salt used in the present invention or hydramine or its mixture, its consumption are 0.1 to 10 weight %, preferred 0.1 to 5 weight %.
End used in the present invention or side chain contain [(OCH
2CH
2)
nOH] non-ionic interfacial agent of Volpo S 10, preferred tool is with following formula (I) structure person:
Wherein, n is 1 to 30 numerical value; R
1, R
2, R
3And R
4Respectively be hydrogen or C
1-C
6Alkyl; And R
5Be hydrogen or C
1-C
6Alkyl or-(OCH
2CH
2)
mOH, wherein m is 1 to 30 numerical value.Can be used for non-ionic interfacial agent among the present invention can be commerce can the person of buying, the Surfynol series interfacial agent that it for example can be AirProducts is produced.According to a preferred embodiment of the present invention, formula used in the present invention (I) non-ionic interfacial agent can be wherein R
2And R
3It is methyl; R
1And R
4It is isobutyl-; And R
5Be-(OCH
2CH
2)
mOH person.In the cleaning combination of the present invention, the content of this non-ionic interfacial agent is 0.0001 to 0.2 weight %, preferred 0.0001 to 0.1 weight %.
Cleaning combination of the present invention can optionally comprise the additive in those who familiarize themselves with the technology the known cleaning combination that can be used for the post-chemical mechanical planarization, this additive for example comprises the organic acid that metal is possessed sequestering power, and preferable organic acid system is selected from propanedioic acid, pentanedioic acid, hexanodioic acid, oxalic acid, citric acid, oxysuccinic acid or tartrate or above-mentioned two or the mixture of multiple acid.When existing, this organic acid content is 0.1 to 15 weight %, preferred 0.1 to 10 weight %.Other additive that optionally uses for example comprises multicomponent alcoholics compound and corrosion inhibitor.Preferable multicomponent alcoholics compound system is selected from ethylene glycol, 1, ammediol, butyleneglycol or glycol ether (diethylene glycol), or two or the mixture of multiple this alcohols, when existing, the consumption of this multicomponent alcoholics compound is counted 0.01 to 5 weight % with composition total weight.Preferable corrosion inhibitor is a triazole compounds, be more preferred from benzotriazole (benzotriazole, BTA) and/or its derivative, in the time of in being present in cleaning combination of the present invention, the consumption of this corrosion inhibitor is counted 0.001 to 0.5 weight % with composition total weight.
Cleaning combination of the present invention can become highly enriched liquid through concentrating, the cost that therefore can effectively reduce the freight, and improve storage stability.Composition after concentrating is decided on degree of enrichment, and the concentration of its quarternary ammonium salt or hydramine or its mixture can be 15 to 40 weight %, and the concentration of interfacial agent can be 0.001 to 2 weight %.
Following examples will the present invention is further illustrated, but be not in order to limiting the scope of the invention, and modification and change that any personage who is familiar with this skill can reach are easily all included in scope of the present invention.
Embodiment
Example 1-7
Various interfacial agent wettability effect tests:
Get commercially available dibasic alcohol, cationic, anionic, non-ionic interfacial agent, make an addition in the deionized water, relatively its surface tension and the contact angle of SiLK and silicon carbide (SiC, Silicon carbide) with the amount of 500ppm.The gained result is as shown in table 2 below.
Table 2
| Instance number | Interfacial agent | The source | The interfacial agent kind | Surface tension (dyne/centimetre) | Solution is to SiLK material contact angle | Solution is to the silicon carbide material contact angle |
| ????1 | Deionized water | ????74.0 | ??82.8° | ??75.7° | ||
| ????2 | The 500ppm aqueous glycol solution | Dibasic alcohol | ????73.5 | ??79.7° | ??80.9° | |
| ????3 | The 500ppm PEG200 aqueous solution | Poly-dihydric alcohol | ????74.1 | ??79.6° | ??76.1° | |
| ????4 | The 500ppm KC-143 aqueous solution | Show outstanding | Cationic | ????61.9 | ??68.7° | ??72.4° |
| ????5 | 500ppm ammonium lauryl sulfate (C 12H 25OSO 3(NH 4) aqueous solution | Anionic | ????50.7 | ??81.5° | ??74.7° | |
| ????6 | 500ppm surfynol 440 aqueous solution | ?AIR ?Products | Non-ionic type | ????35.4 | ??40.5° | ??52.9° |
| ????7 | 500ppm surfynol 336 aqueous solution | ?AIR ?Products | Non-ionic type | ????28.8 | ??37.4° | ??48.8° |
(a) by the data of example in the table 22,3 as can be known, dibasic alcohol and poly-dihydric alcohol can't effectively reduce surface tension and moistening SiLK and silicon carbide;
Can find out by example 4,5 that (b) cationic and anionic interfacial agent (KC-143 and ammonium lauryl sulfate) can reduce surface tension but can't complete moistening SiLK and silicon carbide; And
Can find out by embodiment 6,7 that (c) non-ionic interfacial agent (surfynol 440 and surfynol 336) can effectively reduce surface tension and moistening SiLK and silicon carbide.
(d) as shown in Figure 1, water and 5% thanomin+500ppm surfynol 336 aqueous solution are poured on the SiLK surface, can find out that the latter can moistening fully its surface.
Example 8-15
The preparation of aqueous clean combination:
The quarternary ammonium salt of different sorts as shown in table 3, ratio or hydramine and interfacial agent added in the entry evenly stir, optionally add the pH value that KOH adjusts the gained scavenging solution.
The assessment of cleaning performance:
(1) get commercially available copper wiring lapping liquid ETERPOL-U6 and mix with 9: 1 with hydrogen peroxide, other adds the cupric nitrate of 72ppm, with the preparation contaminating fluid.
(2) just the surface chip that is coated with low-k material SiLK or silicon carbide was dipped in the contaminating fluid after 12 minutes, immersed in the deionized water 2 to 3 seconds again, took out afterwards.
(3) will pollute chip places cleaning machine (On track) collocation cleaning combination to clean.
(4) measure instrument (KLA-2138) with surface imperfection and measure surperficial granule number.
(5) calculating removes rate, wherein removes the rate=preceding granule number of (granule number one cleans the back granule number before the cleaning)/cleaning * 100%.
Gained the results are shown in the table 3.
Table 3 scavenging solution is formed and cleaning performance
| Instance number | Scavenging solution is formed | The pH value | The silicon carbide residual particulates removes rate | SiLK remained on surface particulate removes rate |
| ????8 | The 5 weight % tetramethyl ammonium hydroxide aqueous solution | ????13.6 | ????35％ | ????38％ |
| ????9 | The 5 weight % thanomin aqueous solution | ????12.3 | ????26％ | ????28％ |
| ????10 | The 5 weight % tetramethyl ammonium hydroxide aqueous solution+500ppm surfynol 440 | ????13.6 | ????77％ | ????78％ |
| ????11 | 5 weight % thanomins+500ppm surfynol 440 aqueous solution | ????12.3 | ????72％ | ????73％ |
| ????12 | 5 weight % diethanolamine+500ppm surfynol 440 aqueous solution | ????11.7 | ????68％ | ????71％ |
| ????13 | 5 weight % diethanolamine+500ppm surfynol 336 aqueous solution | ????11.9 | ????70％ | ????74％ |
| ????14 | 5 weight % thanomins+500ppm surfynol 336 aqueous solution are adjusted the pH value with 1N KOH | ????13.0 | ????72％ | ????79％ |
| ????15 | 5 weight % thanomins+500ppm surfynol 336 aqueous solution are with 1N HNO 3Adjust the pH value | ????8.0 | ????71％ | ????70％ |
| ????16 | 5 weight % thanomins+0.5 weight % oxalic acid 500ppm surfynol, 440 aqueous solution, | ????11.2 | ????77％ | ????82％ |
I) as can be known, example 8 and 9 lists there is no obvious cleaning performance with quarternary ammonium salt or hydramine by data shown in the table 3.
Ii) the interpolation interfacial agent can be compared and cleaning performance can be promoted by example 8 and 10 and 9 and 11.
Iii) can find out different sorts quarternary ammonium salt or hydramine and interfacial agent blended cleaning performance by example 10 to 13
Iv) can find out cleaning performance under the different pH values by example 11,14 and 15.
V) interpolation oxalic acid can be compared and cleaning performance can be promoted slightly by example 11 and 16.
Below what is claimed is in order to define Reasonable Protection scope of the present invention.But should be appreciated that those skilled in the art also should belong to the rational protection domain of the present invention based on the attainable all conspicuous improvement of announcement of the present invention.
Claims (19)
1. aqueous clean combination that is used for behind the chemical-mechanical planarization, it comprises:
(a) quarternary ammonium salt of 0.1 to 10 weight % or hydramine or its mixture;
(b) 0.0001 to 0.2 weight % end or side chain contain Volpo S 10 [(OCH
2CH
2)
nOH] non-ionic interfacial agent of (wherein n is 1 to 30 numerical value); And
(c) water.
2. composition as claimed in claim 1, wherein said composition has the pH value between 7 to 14.
3. composition as claimed in claim 1, wherein said composition has the pH value between 9 to 12.5.
4. composition as claimed in claim 1, wherein this quarternary ammonium salt system is selected from tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide or tetrabutylammonium, or two or the mixture of multiple this quaternary ammonium compound.
5. composition as claimed in claim 1, wherein this hydramine is selected from thanomin, diethanolamine, trolamine, Propanolamine, Mono Methyl Ethanol Amine or methyldiethanolamine, or two or the mixture of multiple this hydramine.
6. composition as claimed in claim 1, wherein the consumption of this quarternary ammonium salt or hydramine or its mixture is 0.1 to 5 weight %.
7. composition as claimed in claim 1, wherein should end or the side chain non-ionic interfacial agent that contains Volpo S 10 be the non-ionic interfacial agent that is selected from following formula (I) structure:
Wherein, n is 1 to 30 numerical value; R
1, R
2, R
3And R
4Respectively be hydrogen or C
1-C
6Alkyl; And
R
5Be hydrogen or C
1-C
6Alkyl or-(OCH
2CH
2)
mOH, wherein m is 1 to 30 numerical value.
8. composition as claimed in claim 1 further comprises the organic acid with sequestering power.
9. composition as claimed in claim 8, wherein this organic acid is selected from propanedioic acid, pentanedioic acid, hexanodioic acid, oxalic acid, citric acid, oxysuccinic acid or tartrate or above-mentioned two or the mixture of multiple acid.
10. composition as claimed in claim 8, wherein this organic acid consumption is 0.1 to 10 weight %.
11. composition as claimed in claim 1 comprises multicomponent alcoholics compound in addition.
12. composition as claimed in claim 11, wherein said multicomponent alcoholics compound is selected from ethylene glycol, 1, ammediol, butyleneglycol, glycol ether or two or the mixture of multiple this alcohol compound.
13. composition as claimed in claim 11, wherein the consumption of this multicomponent alcoholics compound is 0.1 to 5 weight %.
14. composition as claimed in claim 1 comprises corrosion inhibitor in addition.
15. composition as claimed in claim 14, wherein this corrosion inhibitor is a triazole compounds.
16. composition as claimed in claim 15, wherein this triazole compounds is benzotriazole and/or its derivative.
17. composition as claimed in claim 14, wherein the consumption of this corrosion inhibitor is 0.001 to 0.5 weight %.
18. as each described composition in the claim 1 to 17, but the highly enriched scavenging solution of its simmer down to.
19. as the composition of 18 of claims the, wherein this highly enriched scavenging solution comprises quarternary ammonium salt or hydramine or its mixture of (a) 15 to 40 weight %; (b) non-ionic interfacial agent of 0.001 to 2 weight %; Reach (c) water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021486034A CN1500857A (en) | 2002-11-12 | 2002-11-12 | Aqueous cleaning liquid combination for flatted chemically machinery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021486034A CN1500857A (en) | 2002-11-12 | 2002-11-12 | Aqueous cleaning liquid combination for flatted chemically machinery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1500857A true CN1500857A (en) | 2004-06-02 |
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ID=34233221
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA021486034A Pending CN1500857A (en) | 2002-11-12 | 2002-11-12 | Aqueous cleaning liquid combination for flatted chemically machinery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012009941A1 (en) * | 2010-07-21 | 2012-01-26 | 河北工业大学 | Cleaning method of multi-layered copper wiring of super-large-scale integrated circuit after chemical-mechanical-polishing |
| CN101041794B (en) * | 2006-03-24 | 2012-02-22 | 达兴材料股份有限公司 | Cleaning fluid composition and usage thereof |
-
2002
- 2002-11-12 CN CNA021486034A patent/CN1500857A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041794B (en) * | 2006-03-24 | 2012-02-22 | 达兴材料股份有限公司 | Cleaning fluid composition and usage thereof |
| WO2012009941A1 (en) * | 2010-07-21 | 2012-01-26 | 河北工业大学 | Cleaning method of multi-layered copper wiring of super-large-scale integrated circuit after chemical-mechanical-polishing |
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