CN101412948A - Cleaning agent for plasma etching residue - Google Patents
Cleaning agent for plasma etching residue Download PDFInfo
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- CN101412948A CN101412948A CNA2007100472657A CN200710047265A CN101412948A CN 101412948 A CN101412948 A CN 101412948A CN A2007100472657 A CNA2007100472657 A CN A2007100472657A CN 200710047265 A CN200710047265 A CN 200710047265A CN 101412948 A CN101412948 A CN 101412948A
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Abstract
The invention discloses a plasma etching remainder detergent, which contains fluoride, water and a solvent, namely N-hydroxyethylpyrrolidone. The detergent has highly-efficient cleaning capability to plasma etching remainder, has lower etching speed to low dielectric materials (such as SiO2 and PETEOS), metal materials (such as Ti, Al and Cu) and other wafer base materials as well as low defect level, has the advantages of wide operation window, safety and environmental protection, and has excellent application prospect in semiconductor wafer cleaning and other micro-electronic fields.
Description
Technical field
The present invention relates to the clean-out system in the semiconductor fabrication process, be specifically related to a kind of cleaning agent for plasma etching residue.
Background technology
In the semiconductor components and devices manufacturing processed, the coating of photoresist layer, exposure and imaging are necessary process steps to the pattern manufacturing of components and parts.Before last (promptly after coating, imaging, ion implantation and the etching at photoresist layer) of patterning carried out next processing step, the residue of photoresist layer material need thoroughly be removed.At doping step intermediate ion bombardment meeting sclerosis photoresist layer polymkeric substance, therefore make photoresist layer become and be difficult for dissolving, thereby be difficult to remove.At present, the general two-step approach (dry ashing and wet etching) of using is removed this layer photoresistance tunic in semi-conductor industry.The first step utilizes dry ashing to remove the major part of photoresist layer (PR); Second step utilized composite corrosion inhibitor wet etching/cleaning to wash remaining photoresist layer.In the cleaning process in second step, composite corrosion inhibitor can only be removed residual polymkeric substance photoresist layer and inorganics, and can not damage metal level (as aluminium lamination).
Typical scavenging solution has following several in the prior art: amine scavenging solution, semi-aqueous amido (non-azanol class) scavenging solution and fluorochemical based cleaning liquid.No matter be which kind of scavenging solution, all contain solvent.For example: US 6,828, and 289 disclosed cleaning liquid compositions comprise: acidic buffer, organic polar solvent, fluorine-containing material and water.The use of solvent mainly is in order to remove the organism part in the plasma etching residues, if the dissolving cleansing power of solvent is not enough, two kinds of situations may occur: thus 1. needs improve the cleansing power that the service temperature of cleaning improves scavenging solution; But higher service temperature tends to bring higher material unaccounted-for (MUF) and less action pane, thereby might change the characteristic dimension of semiconducter device, influences the performance of semiconducter device;
2., remain on the semi-conductor, thereby influence the cleaning performance of semi-conductor chip even by improving the way of temperature, plasma etching residues is still removed unclean.Inappropriate solvent also has other problem.A large amount of fluorine-containing scavenging solutions that use glycols as solvent are disclosed as patent documentation US 5698503.Because a large amount of ethylene glycol compounds that use, the viscosity of this scavenging solution and surface tension are all very big, influence its cleaning performance.So in the preparation process of semi-conductor industry ionic medium etching residual washing liquid, choice of Solvent is very important.
Summary of the invention
Technical problem to be solved by this invention is in order to overcome solvent in the existing cleaning agent for plasma etching residue to organism cleansing power deficiency, influence the cleaning performance of clean-out system, and the cleaning agent for plasma etching residue of the strong and safety and environmental protection of a kind of cleansing power is provided.
Cleaning agent for plasma etching residue of the present invention contains fluorochemical and water, also contains solvent N-hydroxyethyl-pyrrolidone.
Wherein, what the content of described N-hydroxyethyl-pyrrolidone was preferable is mass percent 10～80%, and better is mass percent 20～60%.
Wherein, described fluorochemical is preferable is in the salt that forms of hydrogen fluoride and/or hydrogen fluoride and alkali one or more, as HF, NH
4F, NH
4HF
2, N (CH
3)
4F or N (CH
2OH)
3HF etc.; What the content of described fluorochemical was preferable is mass percent 0.01～10%.
What wherein, the content of described water was preferable is mass percent 10～80%.
This plasma etching leftover cleaning agent also can further contain sequestrant, buffering in, corrosion inhibitor, tensio-active agent and the antifreezing agent one or more.
What wherein, the content of described sequestrant was preferable is mass percent 0～10%; What the content that described buffering is right was preferable is mass percent 0～20%. What the content of described corrosion inhibitor was preferable is mass percent 0～10%; What the content of described tensio-active agent was preferable is mass percent 0～10%; What the content of described antifreezing agent was preferable is mass percent 0～20%.
Among the present invention, described sequestrant is meant the material that contains two or more functional groups, is characterized in forming coordination or chelating with metal or metal oxide.As: contain 1 of phenolic hydroxyl group, 2-dihydroxyl phenol, pyrogallol and gallic acid etc.; The phthalic acid that contains carboxyl; Phosphonic acid based is as 1,3-(hydroxyethyl)-2,4,6-tri methylene phosphonic acid (HEDPA), Amino Trimethylene Phosphonic Acid (ATMP) or 2-phosphonic acids butane-1,2, one or more in the 4-tricarboxylic acid (PBTCA) etc.
Among the present invention, described buffering is to being meant the salt of organic acid and this organic acid and alkali formation, and as acetic acid and ammonium acetate, citric acid and ammonium citrate or lactic acid and DL-Lactic acid ammonium salt etc., that organic acid and the mol ratio of its corresponding salt are preferable is 10:1～1:10.
Among the present invention, described corrosion inhibitor can be a micromolecular inhibitor, can also be the polymer corrosion inhibitor, or both mixtures.Described small molecules corrosion inhibitor can be selected from one or more in following: phenols small molecules corrosion inhibitor, and as phenol, 1,2-dihydroxyl phenol, para hydroxybenzene phenol or pyrogallol etc.; Carboxylic-acid is as phenylformic acid, para-amino benzoic acid (PABA), phthalic acid (PA) or gallic acid (GA) etc.; Benzotriazole micromolecular corrosion inhibitor is as benzotriazole, methyl benzotriazazole or 4-carboxy benzotriazole etc.; Phosphonic acid based small molecules corrosion inhibitor, as 1,3-(hydroxyethyl)-2,4,6-tri methylene phosphonic acid (HEDPA), Amino Trimethylene Phosphonic Acid (ATMP) or 2-phosphonic acids butane-1,2,4-tricarboxylic acid (PBTCA) etc.Described polymer corrosion inhibitor is preferable is selected from hydroxyl polymer-containing and the carbonyl bearing polymer one or more.Wherein, described hydroxyl polymer-containing is preferable is the homopolymer of hydroxyl polyethers or polyvinyl alcohol or multipolymer etc.; What described carbonyl bearing polymer was preferable is ammonium salt, sylvite or the sodium salt etc. that contain carboxyl polyethers, polymaleic anhydride, polyacrylic acid, polymethyl acrylic acid, vinylformic acid and maleic acid, vinylbenzene and acrylic copolymer or above-claimed cpd.
Among the present invention, described tensio-active agent is preferable is in hydroxyl polyethers, polyvinyl alcohol (PVA), polyvinylpyrrolidone, polyoxyethylene (POE), polysiloxane (PSOA), fluoro polyvinyl alcohol, fluoro polyvinylpyrrolidone, fluoro polyoxyethylene, fluoro polysiloxane, silicate and the alkylsulfonate one or more.Wherein, be preferably the hydroxyl polyethers.
Among the present invention, described antifreezing agent is preferable is selected from polyvalent alcohol, as the ethylene glycol in the dibasic alcohol, propylene glycol; Glycerol in the trivalent alcohol; Tetramethylolmethane in the tetravalent alcohol, preferable is propylene glycol.The use of antifreezing agent can make scavenging solution of the present invention deposit under-18 ℃ condition not freeze in two months.
Scavenging solution of the present invention is simply mixed and can be used by mentioned component.This scavenging solution is applicable to the batch immersion type, use in multiple cleaning instrument such as the rotary or rotary treater of monolithic and the cleaning way in batches.And scavenging solution of the present invention can use in bigger temperature range, generally can use in ℃ scope of room temperature～50.
Agents useful for same of the present invention and raw material are all commercially available to be got.
Positive progressive effect of the present invention is: it is solvent that plasma etching residual washing liquid of the present invention has adopted the N-hydroxyethyl-pyrrolidone, and it has the dissolving cleansing power of plasma etching residues efficiently, and Environmental Safety.Plasma etching residual washing liquid article on plasma etch residue of the present invention has cleansing power efficiently, to hanging down dielectric material (as SiO
2And PETEOS) and metallic substance wafer substrates such as (as Ti, Al and Cu) lower etch-rate is arranged, low defect level, and action pane is wide, safety and environmental protection has a good application prospect at microelectronics such as semiconductor wafer cleanings.
Description of drawings
Fig. 1 is for there being the electronic scanning Electronic Speculum figure of figure metal wafer before cleaning.
Fig. 2 is the electronic scanning Electronic Speculum figure that the figure metal wafer is arranged after adopting dipropylene glycol methyl ether (DPME) for contrast clean-out system 1 cleaning of solvent.
Fig. 3 is the electronic scanning Electronic Speculum figure that the figure metal wafer is arranged after adopting methyl-sulphoxide (DMSO) for contrast clean-out system 2 cleanings of solvent.
Fig. 4 is the electronic scanning Electronic Speculum figure that the figure metal wafer is arranged after adopting N-Methyl pyrrolidone (NMP) for contrast clean-out system 3 cleanings of solvent.
Fig. 5 is the electronic scanning Electronic Speculum figure that the figure metal wafer is arranged after adopting N-hydroxyethyl-pyrrolidone (HEP) for clean-out system of the present invention 1 cleaning of solvent.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.Among the following embodiment, per-cent is mass percent.
Embodiment 1
1%HF, 19%N-hydroxyethyl-pyrrolidone and 80% water.
Embodiment 2
10%NH
4F, 10%N-hydroxyethyl-pyrrolidone, 0.01%2-phosphonic acids butane-1,2,4-tricarboxylic acid and 79.99% water.
Embodiment 3
5%NH
4HF
2, the 40%N-hydroxyethyl-pyrrolidone, 20% acetic acid/ammonium acetate cushions (mol ratio 8:1) and 35% water.
Embodiment 4
3%N (CH
3)
4F, 50%N-hydroxyethyl-pyrrolidone, 10% hydroxyl gather ethyl ether (molecular weight 1000) and 37% water.
Embodiment 5
0.01%N (CH
3)
4F, 80%N-hydroxyethyl-pyrrolidone, 0.98% para hydroxybenzene phenol, 0.01% polymethyl acrylic acid and 19% water.
Embodiment 6
3%N (CH
3)
4F, 67%N-hydroxyethyl-pyrrolidone, 20% ethylene glycol and 10% water.
Embodiment 7
1%N (CH
2OH)
3HF, the 77.7998%N-hydroxyethyl-pyrrolidone, 1% lactic acid/DL-Lactic acid ammonium salt cushions (mol ratio 10:1), 0.0001% polyacrylic acid, 0.1% ammonium silicate, 0.1%1,2-dihydroxyl phenol, 0.0001% propylene glycol and 20% water.
Embodiment 8
1%HF, 63%N-hydroxyethyl-pyrrolidone, 10% citric acid/citric acid tetramethyl-ammonium cushion (mol ratio 6:1), 0.1% polyvinyl alcohol (molecular weight 2000), 0.1% polymaleic anhydride (molecular weight 400), 1% glycerol, 1% phenylformic acid and 23.8% water.
Embodiment 9
5% fluoridizes tetramethyl-ammonium, 2%HF, the 50%N-hydroxyethyl-pyrrolidone, 15% citric acid/citric acid Tetrylammonium cushions (mol ratio 5:1), 0.05% polyvinylpyrrolidone (molecular weight 3000), 0.01% polymethyl acrylic acid (molecular weight 800), 2% tetramethylolmethane, 0.01% Amino Trimethylene Phosphonic Acid and 25.93% water.
Embodiment 10
0.01% fluoridizes tetraethyl ammonium, 60%N-hydroxyethyl-pyrrolidone, 5% citric acid/Tripotassium Citrate cushion (mol ratio 4:1), 5% polyoxyethylene (molecular weight 1000), 0.01% vinylformic acid and maleic acid (molecular weight 1500), 0.01% polyvinyl alcohol and acrylic copolymer (molecular weight 800), 4.99% ethylene glycol, 1% tetramethylolmethane, 0.02%1,3-(hydroxyethyl)-2,4,6-tri methylene phosphonic acid and 23.96% water.
Embodiment 11
1% Neutral ammonium fluoride, the 70%N-hydroxyethyl-pyrrolidone, 3% citric acid/Tripotassium Citrate cushions (mol ratio 2:1), 1% pyrogallol, 0.01% polysiloxane (molecular weight 800), 0.01% vinylbenzene and acrylic copolymer (molecular weight 1000), 0.01%2-phosphonic acids butane-1,2,4-tricarboxylic acid, 2% tetramethylolmethane and 22.97% water.
Embodiment 12
5% fluoridizes tetraethyl ammonium, the 30%N-hydroxyethyl-pyrrolidone, 5% citric acid/Tripotassium Citrate cushions (mol ratio 1:10), 0.01% fluoro polyvinyl alcohol (molecular weight 600), 0.01% polyacrylic acid potassium (molecular weight 800), 5% methyl benzotriazazole, 5% ethylene glycol, poly-ethyl ether of 5% hydroxyl and 44.98% water.
Embodiment 13
7% fluoridizes tetraethyl ammonium, the 50%N-hydroxyethyl-pyrrolidone, 10% citric acid/citric acid Tetrylammonium cushions (mol ratio 1:8), 0.01% fluoro polyvinylpyrrolidone (molecular weight 1500), 0.01% sodium polyacrylate (molecular weight 900), 1.98%4-carboxy benzotriazole, 1% tetramethylolmethane and 30% water.
Embodiment 14
10% fluoridizes tetraethyl ammonium, the 34.97%N-hydroxyethyl-pyrrolidone, 15% citric acid/citric acid Tetrylammonium cushions (mol ratio 1:6), 0.01% fluoro polyoxyethylene (molecular weight 800), 0.01% ammonium polyacrylate (molecular weight 600), 0.01% polyvinyl alcohol (molecular weight 800), 5% benzotriazole, 5% ethylene glycol and 30% water.
30% water.
Embodiment 15
4% Neutral ammonium fluoride, 20%N-hydroxyethyl-pyrrolidone, 15% acetic acid/ammonium acetate cushion (mol ratio 1:4), 0.01% fluoro polysiloxane (molecular weight 1000), 1% hydroxyl gathers ethyl ether (molecular weight 800), 5% gallic acid, 5% ethylene glycol and 49.99% water.
Embodiment 16
6% Neutral ammonium fluoride, 32.98%N-hydroxyethyl-pyrrolidone, 15% acetic acid/ammonium acetate cushion (mol ratio 1:2), 0.01% sodium laurylsulfonate, 0.01% contains the poly-ethyl ether (molecular weight 1000) of carboxyl, 1% glycerol, 5% phthalic acid and 40% water.
Embodiment 17
1% Neutral ammonium fluoride, 59%N-hydroxyethyl-pyrrolidone, 20% water, 10% 1,2-dihydroxyl phenol and 10% benzotriazole.
Effect embodiment
Press each component of table 1 prescription uniform mixing, preparation contrast clean-out system 1～3 and clean-out system 1.
Table 1 contrast clean-out system 1～3 and clean-out system 1 and base material erosion rate thereof
*The erosion rate value is the data of twice test.
The rate of metal corrosion testing method of solution:
(1) utilize Napson four-point probe instrument to test the resistance initial value (Rs1) of the blank silicon chip of 4*4cm aluminium;
(2) the blank silicon chip of this 4*4cm aluminium is immersed in advance in the solution of constant temperature to 35 ℃ 30 minutes;
(3) take out the blank silicon chip of this 4*4cm aluminium, use washed with de-ionized water, high pure nitrogen dries up, and utilizes the resistance value (Rs2) of the blank silicon chip of Napson four-point probe instrument test 4*4cm aluminium again;
(4) repeated for the second and the 3rd step and test once, resistance value is designated as Rs3;
(5) above-mentioned resistance value and soak time are input to suitable procedure and can calculate its erosion rate.
The nonmetal erosion rate testing method of solution:
(1) utilize the Nanospec6100 thickness tester to test the thickness (T1) of 4*4cm PETEOS silicon chip;
(2) this 4*4cmPETEOS silicon chip is immersed in advance in the solution of constant temperature to 35 ℃ 30 minutes;
(3) take out this 4*4cmPETEOS silicon chip, use washed with de-ionized water, high pure nitrogen dries up, and utilizes the thickness (T2) of Nanospec6100 thickness tester test 4*4cmPETEOS silicon chip again;
(4) the second and the 3rd step of repetition tests a thickness again and is designated as T3;
(5) above-mentioned one-tenth-value thickness 1/10 and soak time are input to suitable procedure and can calculate its erosion rate.
As can be seen from Table 1: select different solvents for use, even under the same condition of other components, the corrosion speed of its metallic aluminium and nonmetal PETEOS also is not quite similar.When wherein DPME was solvent, its erosion rate was greater than standard that industry requires (2A/min).In semi-conductor industry, scavenging solution is applicable to the batch immersion type, in batches in multiple cleaning instrument such as the rotary or rotary treater of monolithic and the cleaning way; The wafer type of cleaning has metal wire (pattern metal wafer) and passage (pattern via wafer) etc.The present invention has selected for use figure metal wafer (pattern metal wafer) to carry out immersion type and has cleaned (conclusion of the present invention is not limited thereto for example) when comparing cleansing power.(select for use with a kind of figure metal silicon chip (Fig. 1) arranged there being figure metal wafer (patternmetal wafer) plasma etching residues to clean with the clean-out system in the table 1, same cleaning step), its cleaning performance characterizes by the electronic scanning Electronic Speculum, sees Fig. 2～5, sums up and sees Table 2.
The effect that table 2 contrast clean-out system 1～3 and 1 pair of clean-out system have figure metal silicon chip (pattern metal wafer) plasma etching residues to clean
Claims (12)
1. a cleaning agent for plasma etching residue contains fluorochemical and water, it is characterized in that: it also contains solvent N-hydroxyethyl-pyrrolidone.
2. clean-out system as claimed in claim 1 is characterized in that: the content of described N-hydroxyethyl-pyrrolidone is mass percent 10～80%.
3. clean-out system as claimed in claim 2 is characterized in that: the content of described N-hydroxyethyl-pyrrolidone is mass percent 20～60%.
4. clean-out system as claimed in claim 1 is characterized in that: the content of described fluorochemical is mass percent 0.01～10%.
5. clean-out system as claimed in claim 1 is characterized in that: described fluorochemical is HF, NH
4F, NH
4HF
2, N (CH
3)
4F and N (CH
2OH)
3Among the HF one or more.
6. clean-out system as claimed in claim 1 is characterized in that: the content of described water is mass percent 10～80%.
7. clean-out system as claimed in claim 1 is characterized in that: described cleaning agent for plasma etching residue also contains sequestrant, buffering in, corrosion inhibitor, tensio-active agent and the antifreezing agent one or more.
8. clean-out system as claimed in claim 7 is characterized in that: the content of described sequestrant is mass percent 0～10%; The content that described buffering is right is mass percent 0～20%; The content of described corrosion inhibitor is mass percent 0～10%; The content of described tensio-active agent is mass percent 0～10%; The content of described antifreezing agent is mass percent 0～20%.
9. clean-out system as claimed in claim 7, it is characterized in that: described sequestrant is 1,2-dihydroxyl phenol, pyrogallol, gallic acid, phthalic acid, 1,3-(hydroxyethyl)-2,4,6-tri methylene phosphonic acid, Amino Trimethylene Phosphonic Acid and 2-phosphonic acids butane-1,2, one or more in the 4-tricarboxylic acid; Described buffering is to being the salt that organic acid and this organic acid and alkali form; Described corrosion inhibitor is micromolecular inhibitor and/or polymer corrosion inhibitor; Described tensio-active agent is one or more in hydroxyl polyethers, polyvinyl alcohol, polyvinylpyrrolidone, polyoxyethylene, polysiloxane, fluoro polyvinyl alcohol, fluoro polyvinylpyrrolidone, fluoro polyoxyethylene, fluoro polysiloxane, silicate and the alkylsulfonate; Described antifreezing agent is a polyvalent alcohol.
10. clean-out system as claimed in claim 9 is characterized in that: the salt that described organic acid and this organic acid and alkali form is acetic acid and ammonium acetate, citric acid and ammonium citrate, perhaps lactic acid and DL-Lactic acid ammonium salt; Described small molecules corrosion inhibitor is selected from one or more in phenols, carboxylic-acid, benzotriazole, the phosphonic acid based small molecules corrosion inhibitor; Described polymer corrosion inhibitor is selected from hydroxyl polymer-containing and/or carbonyl bearing polymer; Described polyvalent alcohol is one or more in ethylene glycol, propylene glycol, glycerol and the tetramethylolmethane.
11. clean-out system as claimed in claim 10 is characterized in that: described phenols small molecules corrosion inhibitor is a phenol, 1, one or more in 2-dihydroxyl phenol, para hydroxybenzene phenol and the pyrogallol; Described carboxylic-acid small molecules corrosion inhibitor is one or more in phenylformic acid, para-amino benzoic acid, phthalic acid and the gallic acid; Described benzotriazole micromolecular corrosion inhibitor is one or more in benzotriazole, methyl benzotriazazole and the 4-carboxy benzotriazole; Described phosphonic acid based small molecules corrosion inhibitor is 1,3-(hydroxyethyl)-2,4,6-tri methylene phosphonic acid, Amino Trimethylene Phosphonic Acid and 2-phosphonic acids butane-1,2, one or more in the 4-tricarboxylic acid; Described hydroxyl polymer-containing is one or more in hydroxyl polyethers, polyvinyl alcohol homopolymer and the polyvinyl alcohol copolymer; Described carbonyl bearing polymer is one or more in ammonium salt, sylvite and the sodium salt that contains carboxyl polyethers, polymaleic anhydride, polyacrylic acid, polymethyl acrylic acid, vinylformic acid and maleic acid, vinylbenzene and acrylic copolymer, above-claimed cpd.
12. clean-out system as claimed in claim 9 is characterized in that: the mol ratio of the salt that described organic acid and this organic acid and alkali form is 10:1～1:10.
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| WO2014071688A1 (en) * | 2012-11-12 | 2014-05-15 | 安集微电子科技(上海)有限公司 | Rinse solution for removal of photoresist etching residues |
| WO2014071689A1 (en) * | 2012-11-12 | 2014-05-15 | 安集微电子科技(上海)有限公司 | Cleaning solution for removing photoresist residue |
| CN107109134A (en) * | 2014-12-22 | 2017-08-29 | 巴斯夫欧洲公司 | Chemically-mechanicapolish polish purposes of (CMP) composition in base material of the polishing comprising cobalt and/or cobalt alloy |
| CN107109134B (en) * | 2014-12-22 | 2021-04-13 | 巴斯夫欧洲公司 | Use of Chemical Mechanical Polishing (CMP) compositions for polishing substrates comprising cobalt and/or cobalt alloys |
| CN106011881A (en) * | 2016-06-30 | 2016-10-12 | 无锡伊佩克科技有限公司 | Water-based steel brightening and rust removing agent and preparation method thereof |
| CN108255027A (en) * | 2016-12-28 | 2018-07-06 | 安集微电子（上海）有限公司 | A kind of photoresist cleaning solution |
| CN108255027B (en) * | 2016-12-28 | 2024-04-12 | 安集微电子（上海）有限公司 | Photoresist cleaning solution |
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