Cleaning compositions for microelectronics substrates

ES 2 335 786 T3

DESCRIPTION

Cleaning compositions for microelectronic substrates.

Field of the invention

This invention relates to cleaning and extraction compositions for microelectronic substrates, and particularly for cleaning metal-containing residues from aluminum-containing microelectronic components, without causing excessive corrosion of the aluminum. The invention also relates to the cleaning of pathways that pierce the metallic layers of microelectronic components, such as layers of titanium or titanium nitride, while being compatible with adjacent aluminum structures, that is, causing little or no metallic corrosion in microelectronic components. The invention further relates to such cleaning compositions, which can also clean subsequent ash residues from other pathways and other metal pipes, as well as clean or remove ashless photoresistors from microelectronic substrates. An additional aspect of this invention is a process for cleaning or removing photoresistors and residues of microelectronic components containing aluminum, without causing excessive corrosion of the aluminum.

Background of the invention

During the manufacture of microelectronic devices, photoresistors are used to transfer images from a microelectronic substrate to create a desired circuit layer. Many of these microelectronic devices are metallized with aluminum. As adhesion promoters and diffusion barriers, metals can also be used in the microelectronic substrate, such as titanium, titanium nitride, tungsten and the like.

Many alkaline microelectronic extraction and cleaning compositions have been proposed for the separation of crosslinked and hardened photoresistors and other residues from such microelectronic substrates, such as residues from a chemical attack. However, a problem with such extraction and cleaning compositions is the potential for metallic corrosion to occur as a result of the use of such cleaning compositions. Such corrosion leads to hairs, pitting, and nicks in metal pipes, due, at least in part, to the reaction of the metals in the device substrates with the alkaline extractors used. Such an alkaline microelectronic extraction and cleaning composition is disclosed in US Patent No. 5,308,745. Although the extraction and cleaning compositions of that patent have been used commercially to extract hardened, cross-linked photoresistors from substrates, it has been discovered that attempts to clean microelectronic substrates that have an aluminum metallization and contain metal residues from layers such as layers of titanium, titanium nitride, tungsten and the like, with the cleaning composition of this patent, It has led to significant corrosion of the aluminum or insufficient cleaning of metal residues. Therefore, there is a limitation in the use of the cleaning compositions of that patent in cleaning pathways that pierce adjacent layers of titanium, titanium nitride, tungsten, and the like.

Therefore, there is a need for microelectronic extraction and cleaning compositions that can effectively separate such metal residues, and do so without significant corrosion of the aluminum resulting from the extraction and cleaning composition. There is also a need for extraction and cleaning compositions which, in addition to cleaning these metallic residues, also effectively clean subsequent ash residues from other pathways and other metallic pipes, as well as for cleaning the substrate of photoresistor residues that do not they have ashes.

Brief summary of the invention

In accordance with this invention, extraction and cleaning compositions are provided for cleaning microelectronic substrates, the composition comprising: at least one organic extraction solvent; at least one nucleophilic alkanolamine; at least one weak acid that does not contain nitrogen, in an amount sufficient to neutralize from about 3% to about 75%, preferably from about 19% to about 75%, by weight of the nucleophilic alkanolamine, such that the extraction composition has a Aqueous pH of from about 9.6 to about 10.9, said weak acid having a pK value in aqueous solution of 2.0 or greater and an equivalent weight of less than 140; at least one metal removal compound selected from the group consisting of diethylene glycol and diethylene glycol amine, and water; and methods for cleaning microelectronic substrates with these compositions.

The extraction and cleaning composition of this invention for cleaning microelectronic substrates consists of:

a) at least one organic extraction solvent, comprising a solvent from the group consisting of 2-pyrrolidinone, 1-methyl-2-pyrrolidinone, 1-ethyl-2-pyrrolidinone, 1-propyl-2-pyrrolidinone, 1-hydroxyethyl- 2-pyrrolidinone, 1-hydroxypropyl-2-pyrrolidinone, diethylene glycol monoalkyl ethers of the formula HO-CH₂-O-CH₂-CH₂OR, where R is an alkyl radical of 1 to 4 carbon atoms, dialkyl sulfones of the formula R¹ -S (O) (O) R², where R¹ and R² they are alkyl groups of 1 to 4 carbon atoms, dimethyl sulfoxide (DMSO), sulfolane, methyl sulfolane, alkyl sulfolanes, dimethylacetamide and dimethylformamide;

b) at least one nucleophilic alkanolamine;

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c) at least one weak acid that does not contain nitrogen, in an amount sufficient to neutralize from about 3% to about 75%, preferably from about 19% to about 75%, by weight of the nucleophilic alkanolamine, such that the extraction composition has an aqueous pH of from about 9.6 to about 10.9, said weak acid having a pK value in aqueous solution of 2.0 or greater and an equivalent weight of less than 140;

d) at least one metal separating compound selected from the group consisting of diethylene glycol and diethylene glycol amine;

e) water, and optionally one or more components selected from the group consisting of metal complexing / corrosion resistant compounds, other corrosion inhibitors and surfactants.

The method of cleaning microelectronic substrates according to this invention comprises a method of cleaning microelectronic substrates without producing substantial metallic corrosion, the substrate containing at least one of a photoresist polymer material, etching residues and metallic residues, the method comprising placing the substrate in contact with a cleaning composition for a time sufficient to clean the substrate, wherein the cleaning composition consists of:

a) at least one organic extraction solvent, comprising a solvent from the group consisting of 2-pyrrolidinone, 1-methyl-2-pyrrolidinone, 1-ethyl-2-pyrrolidinone, 1-propyl-2-pyrrolidinone, 1-hydroxyethyl -2-pyrrolidinone, 1-hydroxypropyl-2-pyrrolidinone, diethylene glycol monoalkyl ethers of the formula HO-CH₂-O-CH₂CH₂-OR, where R is an alkyl radical of 1 to 4 carbon atoms, dialkyl sulfones of the formula R¹S (O) (O) -R², where R¹ and R² they are alkyl groups of 1 to 4 carbon atoms, dimethyl sulfoxide (DMSO), sulfolane, methyl sulfolane, alkyl sulfolanes, dimethylacetamide and dimethylformamide;

b) at least one nucleophilic alkanolamine;

c) at least one weak acid that does not contain nitrogen, in an amount sufficient to neutralize from about 3% to about 75%, preferably from about 19% to about 75%, by weight of the nucleophilic alkanolamine, such that the extraction composition has an aqueous pH of from about 9.6 to about 10.9, said weak acid having a pK value in aqueous solution of 2.0 or greater and an equivalent weight of less than 140;

d) at least one metal separating compound selected from the group consisting of diethylene glycol and diethylene glycol amine;

e) water, and optionally one or more components selected from the group consisting of metal complexing / corrosion resistant compounds, other corrosion inhibitors and surfactants. The microelectronic substrate cleaning method according to this invention is particularly useful for cleaning substrates comprising aluminum-metallized substrates having vias and containing metallic residues of at least one of layers of titanium and / or titanium nitride.

Detailed Description of the Invention and Preferred Embodiments

This invention provides extraction and cleaning compositions for cleaning microelectronic substrates, the composition comprising: at least one organic extraction solvent; at least one nucleophilic alkanolamine; at least one weak acid that does not contain nitrogen, in an amount sufficient to neutralize from about 3% to about 75%, preferably from about 19% to about 75%, by weight of the nucleophilic alkanolamine, such that the extraction composition has a Aqueous pH of from about 9.6 to about 10.9, said weak acid having a pK value in aqueous solution of 2.0 or greater and an equivalent weight of less than 140; at least one metal removal compound selected from the group consisting of diethylene glycol and diethylene glycol amine, and water; and methods for cleaning microelectronic substrates with these compositions.

The extraction and cleaning composition of this invention to clean microelectronic substrates, consists of:

a) at least one organic extraction solvent, comprising a solvent from the group consisting of 2-pyrrolidinone, 1-methyl-2-pyrrolidinone, 1-ethyl-2-pyrrolidinone, 1-propyl-2-pyrrolidinone, 1-hydroxyethyl- 2-pyrrolidinone, 1-hydroxypropyl-2-pyrrolidinone, diethylene glycol monoalkyl ethers of the formula HO-CH₂-O-CH₂-CH₂OR, where R is an alkyl radical of 1 to 4 carbon atoms, dialkyl sulfones of the formula R¹-S (O) (O) R², where R¹ and R² they are alkyl groups of 1 to 4 carbon atoms, dimethyl sulfoxide (DMSO), sulfolane, methyl sulfolane, alkyl sulfolanes, dimethylacetamide and dimethylformamide;

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b) at least one nucleophilic alkanolamine;

c) at least one weak acid that does not contain nitrogen, in an amount sufficient to neutralize from about 3% to about 75%, preferably from about 19% to about 75%, by weight of the nucleophilic alkanolamine, such that the extraction composition has an aqueous pH of from about 9.6 to about 10.9, said weak acid having a pK value in aqueous solution of 2.0 or greater and an equivalent weight of less than 140;

d) at least one metal separating compound selected from the group consisting of diethylene glycol and diethylene glycol amine;

e) water, and optionally one or more components selected from the group consisting of metal complexing / corrosion resistant compounds, other corrosion inhibitors and surfactants.

Generally, the at least one organic extraction solvent is present in the composition in an amount of about 20 to about 80% by weight, preferably in an amount of about 30 to about 75% by weight, and more preferably in an amount of about 40 to about 60% by weight. Preferably the solvent is N-methylpyrrolidinone.

Generally, the at least one nucleophilic alkanolamine component of the compositions of the invention is present in the compositions in an amount of from about 1 to about 50% by weight, preferably from about 10 to about 45% by weight, and more preferably from about 20 to about 30% by weight. Among the alkanolamine components that can be used, mention may be made of monoethanolamine, 1-amino-2-propanol, 2- (2-aminoethoxy) ethanol, 2-aminoethanol and 2- (2-aminoethylamino) ethanol. More important than the actual pK value of alkanolamine is its nucleophilicity which should be high. Most preferably, the nucleophilic alkanolamine is monoethanolamine or 1-amino-2-propanol.

Generally, the nitrogen-free weak acid component of the composition of this invention is present in the composition in an amount of from about 0.5 to about 10% by weight, preferably from about 1 to about 8% by weight, and more. preferably from about 2 to about 6% by weight. Weak non-nitrogen containing acids that can be employed in this invention include organic acids, such as carboxylic acids or phenols, as well as inorganic acid salts such as carbonic acid or hydrofluoric acid. By weak acids we mean acids having a strength, expressed as the "pK" value of the dissociation constant in aqueous solution, of at least 2.0 or greater, preferably 2.5 or greater. Weak acids of pK> 2.0 and preferably have an equivalent weight of less than about 140 are particularly useful. As examples of such weak nitrogen-free acids useful in this invention, there may be mentioned, for example, carboxylic acids, such as acetic acid, phthalic acid, phenoxyacetic acid and the like; organic acids, such as 2-mercaptobenzoic acid, 2-mercaptoethanol, and the like; phenols generally having a pK in the range of 9 to 10, such as phenol, catechol, 1,3,5-trihydroxybenzene, pyrogallol, resorcinol, 4-tert-butylcatechol, and the like; and inorganic acids, such as carbonic acid, hydrofluoric acid, and the like. The amount of weak acid employed in the extraction compositions of this invention is the amount necessary to neutralize from about 3% to about 75%, preferably from about 19% to about 75%, by weight of the alkanolamine present in the extraction composition. , thereby resulting in an aqueous rinse pH for said extractor compositions of from about 9.6 to about 10.9. Most preferably the weak acid is catechol.

The at least one component for the separation of metals is diethylene glycol or diethylene glycol amine, or their mixtures. Generally, this component is present in the composition in an amount of from about 0.5 to about 40% by weight, preferably from about 1 to about 20% by weight, and more preferably from about 5 to about 15% by weight. Preferably this component is diethylene glycol.

The cleaning and extraction compositions of this invention are aqueous alkaline compositions, and the water is generally present in an amount of from about 0.5 to about 50% by weight, preferably from about 1 to about 35% by weight, and more preferably from about 5 to about 20% by weight.

The compositions of this invention may also optionally contain one or more components selected from the group consisting of metal complexing / corrosion resistant compounds, other corrosion inhibitors and surfactants.

No organic or inorganic chelating or metal complexing agents / corrosion inhibitors are required, but may optionally be included in the compositions of this invention, but offer substantial benefits, such as for example improved product stability, when used. incorporated into the aqueous cleaning compositions of this invention. Examples of chelating or complexing agents include,

ES 2 335 786 T3 but not limited to, trans-1,2-cyclohexanediamine tetraacetic acid (CyDTA), ethylenediaminetetraacetic acid (EDTA), stannates, pyrophosphates, derivatives of alkylidene diphosphonic acid (e.g. ethane-1- hydroxy1,1-diphosphonate), phosphonates containing ethylenediamine, diethylenetriamine or triethylenetetramino functional moieties [e.g. ethylenediamine tetra (methylene phosphonic) acid (EDTMP), diethylenetriamine penta (methylene phosphonic acid), triethylenetetramino penta (methylene phosphonic acid)]. The chelating agent is present in the composition in an amount of from 0 to about 5% by weight, preferably from about 0.1 to about 2% by weight, based on the weight of the composition.

The aqueous cleaning compositions of this invention may also optionally contain other corrosion inhibitors and similar non-corrosive components used in microelectronic cleaning compositions. The compounds can include resorcinol, gallic acid, propyl-gallate, pyrogallol, hydroquinone, benzotriazole, and benzotriazole derivatives, and polyfunctional carboxylic acids, such as citric acid, tartaric acid, gluconic acid, sugar acid, glyceric acid, oxalic acid, acid Phthalic, Maleic Acid, Mandelic Acid, Malonic Acid, Lactic Acid, and Salicylic Acid. These other corrosion inhibitors may be present in any suitable amount, generally in an amount from about 0 to about 5% by weight, preferably from about 0.1 to about 3% by weight, and more preferably from about 0.2 to about 2% by weight.

The compositions of the present invention may also optionally contain any suitable water soluble amphoteric cationic or anionic surfactant. The addition of a surfactant reduces the surface tension of the formulation and improves the wetting of the surface to be cleaned and therefore improves the cleaning action of the composition. The surfactant can also be added to reduce aluminum corrosion rates, if an inhibition of aluminum corrosion is also desired. Amphoteric surfactants useful in the compositions of the present invention include betaines and sulfobetaines, such as the alkyl betaines, amidoalkyl betaines, alkyl sulfobetaines, and amidoalkyl sulfobetaines; aminocarboxylic acid derivatives, such as amphoglycinates, amphopropionates, amphodiglycinates and amphodipropionates; imino acids, such as alkoxyalkyl or alkoxyaryl imino acids; amine oxides, such as alkylamine oxides and alkylamido-alkylamine oxides; fluoroalkyl sulfonates and fluorinated alkyl amphoteric; and their mixtures. Preferably, amphoteric surfactants are cocoamidopropyl-betaine, cocoamidopropyl-dimethyl-betaine, cocoamidopropyl-hydroxy-sultaine, capryloampho-dipropionate, cocoamidodipropionate, cocoamphopropionate, cocoamphohydroxyethylpropionate, cocodecyloxypropyliminopropyl oxide-cocodecyloxypropyl oxide, and cocodecyloxypropyl oxidepropyl oxide, and cocoamidopropyl oxidepropyl-diphionepropyl oxide fluorinated. Nonionic surfactants useful in the compositions of the present invention include acetylenic diols, ethoxylated acetylenic diols, fluorinated alkyl alkoxylates, fluorinated alkyl esters, fluorinated polyoxyethylene alkanols, aliphatic acid esters of polyhydric alcohols, polyoxyethylene monoalkyl ethers, polyoxyethylene monoalkyl ethers. diols, siloxane surfactants, and alkylene glycol monoalkyl ethers. Preferably, the nonionic surfactants are acetylenic diols or ethoxylated acetylenic diols. Anionic surfactants useful in the compositions of the present invention include carboxylates, N-acylsarcosinates, sulfonates, sulfates, and mono- and diesters of orthophosphoric acid, such as decyl phosphate. Preferably, the anionic surfactants are metal-free surfactants. Cationic surfactants useful in the compositions of the present invention include amino ethoxylates, dialkyldimethylammonium salts, dialkylmorpholino salts, alkylbenzyldimethylammonium salts, alkyltrimethylammonium salts, and alkylpyridinium salts. Preferably, the cationic surfactants are non-halogen surfactants. Examples of especially suitable surfactants include, but are not limited to, 3,5-dimethyl-1-hexyn-3-ol (Surfynol-61), 2,4,7,9-tetramethyl-5-decino-4, Ethoxylated 7-diol (Surfynol-465), polytetrafluoroethylene-ketoxypropyl-betaine (Zonyl FSK), Zonyl FSH, Triton X-100, ie octylphenoxypolyethoxyethanol, and the like. Generally, the surfactant is present in an amount of 0 to about 5% by weight, preferably 0.001 to about 3 by weight, based on the weight of the composition.

Examples of cleaning compositions of this invention include, but are not limited to, the compositions set forth in the following Tables 1, 2, 3, and 4. In Tables 1, 2, 3, and 4, as well as in the following Tables 5 to 9, the abbreviations used are the following:

NMP = N-methylpyrrolidinone

DMSO = dimethyl sulfoxide

DMAC = dimethylacetamide

DMF = dimethylformamide

DEG = diethylene glycol

DEGA = diethylene glycolamine

CAT = catechol

MEA = monoethanolamine

AMP = 1-amino-2-propanol

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TABLE 1

Compositions / Parts by weight

<td>Components (edit)</td><td></td><td></td><td> 3</td><td> 4</td><td></td>

<td>NMP</td><td> 46</td><td> 26</td><td> 26</td><td> 26</td><td> 26</td>

<td>DMSO</td><td></td><td></td><td></td><td></td><td></td>

<td>DMAC</td><td></td><td></td><td></td><td></td><td></td>

<td>MEA</td><td> 23</td><td> 20</td><td> 20</td><td> 10</td><td> 10</td>

<td>AMP</td><td></td><td></td><td></td><td></td><td></td>

<td>SDR</td><td> 11</td><td> 8</td><td></td><td></td><td></td>

<td>DEGA</td><td></td><td></td><td> 8</td><td> 2</td><td> 8</td>

<td>CAT</td><td> 5</td><td> 1</td><td> 1</td><td> 1</td><td> 5</td>

<td>WATER</td><td> 15</td><td> 4</td><td> 4</td><td> 4</td><td> 4</td>

TABLE 2

Compositions / Parts by weight

<td>Components (edit)</td><td></td><td></td><td></td><td> 9</td><td> 10</td>

<td>NMP</td><td> 26</td><td> 26</td><td> 26</td><td> 26</td><td> 26</td>

<td>DMSO</td><td></td><td></td><td></td><td></td><td></td>

<td>DMAC</td><td></td><td></td><td></td><td></td><td></td>

<td>MEA</td><td> 20</td><td> 20</td><td> 15</td><td> 15</td><td> 15</td>

<td>AMP</td><td></td><td></td><td></td><td></td><td></td>

<td>SDR</td><td></td><td></td><td></td><td></td><td> 5</td>

<td>DEGA</td><td> 2</td><td> 8</td><td> 5</td><td> 5</td><td></td>

<td>CAT</td><td> 5</td><td> 5</td><td> 3</td><td> 1</td><td> 3</td>

<td>WATER</td><td> 4</td><td> 10</td><td> 7</td><td> 7</td><td> 4</td>

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TABLE 3

Compositions / Parts by weight

<td>Components (edit)</td><td> 11</td><td> 12</td><td> 13</td><td> 14</td><td> 15</td>

<td>NMP</td><td> 46</td><td> 46</td><td> 54</td><td> 46</td><td></td>

<td>DMSO</td><td></td><td></td><td></td><td></td><td></td>

<td>DMAC</td><td></td><td></td><td></td><td></td><td> 46</td>

<td>MEA</td><td> 21</td><td> 25</td><td> 21</td><td></td><td></td>

<td>AMP</td><td></td><td></td><td></td><td> 23</td><td> 23</td>

<td>SDR</td><td> 13</td><td> 9</td><td></td><td> 11</td><td> 11</td>

<td>DEGA</td><td></td><td></td><td> 9</td><td></td><td></td>

<td>CAT</td><td> 7</td><td> 3</td><td> 3</td><td> 5</td><td> 5</td>

<td>WATER</td><td> 13</td><td> 17</td><td> 13</td><td> 15</td><td> 15</td>

TABLE 4

Compositions / Parts by weight

<img file="ES2335786T3_D0001.tif" />

Cleaning Examples 1 through 11 below demonstrate the outstanding performance of cleaning and non-corrosion properties of the compositions of this invention, compared to similar compositions with other polyhydroxy compounds in place of DEG and DEGA. Various cleaning compositions were prepared by mixing 26 g of NMP, 20 g of monoethanolamine, 1 g of catechol, 4 g of deionized water and 8 g of a cleaning compound from the following substances: diethylene glycol (DEG), diethylene glycol amine (DEGA ), triethylene glycol, tetraethylene glycol, ethylene glycol, propylene glycol, N-methylethanolamine, 2- (2-aminoethylamino) ethanol, 2-butene-1,4-diol and 2- (2-methoxyethoxy) ethanol. Some samples of discs modeled with Al technology with "perforated" pathway structures (pathways of chemical attack through Si and TiN in an Al layer) were placed in these solutions, heated at 85 ° C for 20 minutes, then from which they were separated, rinsed in deionized water for two minutes, and blown dry with dry nitrogen. For comparison, the same discs were cleaned in a commercially available extraction composition of US Pat. 5,308,745 (containing NMP, sulfolane, MEA, catechol, and deionized water). The clean discs were then evaluated for ash residue separation (0 = no separation, at 10 = 100% separation) and aluminum corrosion (0 = no corrosion, at 10 = corrosion), as observed below in Table 5.

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TABLE 5

<td>IslOflI Example</td><td>Cleaning compound</td><td>Aluminum corrosion</td><td>Ash residue separation</td>

<td> 1</td><td>diethylene glycol</td><td> 0</td><td> 10</td>

<td> 2</td><td>diethylene glycollamine</td><td> 1</td><td> 8</td>

<td> 3</td><td>tetraethylene glycol</td><td> 0</td><td> 5</td>

<td> 4</td><td>2-butene-1,4-diol</td><td> 0</td><td> 5</td>

<td> 5</td><td>ethylene glycol</td><td> 0</td><td> 4</td>

<td> 6</td><td>propylene glycol</td><td> 0</td><td> 4</td>

<td> 7</td><td>N, N-dimethylethanolamine</td><td> 1</td><td> 4</td>

<td> 8</td><td>2- (2-aminoethylamino) ethanol</td><td> 2</td><td> 2</td>

<td> 9</td><td>2- (2-methoxyethoxy) ethanol</td><td> 0</td><td> 2</td>

<td> 10</td><td>triethylene glycol</td><td> 0</td><td> 1</td>

<td> 11</td><td>Commercial product of the US Patent 5,308,745</td><td> 0</td><td> 1</td>

Only DEG and DEGA provided both excellent debris separation and aluminum corrosion inhibition. Examples 12 to 29 below exemplify the utility of the cleaning compositions of this invention under a variety of cleaning conditions, time and temperature, and with various formulations.

Examples 12 to 16

Various cleaning compositions were prepared by mixing 1-methyl-2-pyrrolidinone (NMP), monoethanolamine (MEA), diethylene glycol (DEGA) catechol (CAT) and deionized water, in the amounts shown below. The same type of Al technology patterned disc samples with "perforated" path structures as used in Examples 1 to 11 were placed in these solutions, heated at 85 ° C for 20 minutes, after which they were separated, They were rinsed in deionized water for two minutes and blown dry with dry nitrogen. The clean discs were then evaluated for ash residue separation (0 = no separation, at 10 = 100% separation) and aluminum corrosion (0 = no corrosion, at 10 = corrosion), as observed in Table 6.

TABLE 6

<td>Example No.</td><td>NMP</td><td>MEA</td><td>DEGA</td><td>Catechol</td><td>H₂OR</td><td>Aluminum corrosion</td><td>Ash residue separation</td>

<td> 12</td><td> 26</td><td> 10</td><td> 2</td><td> 1</td><td> 4</td><td> 0</td><td> 10</td>

<td> 13</td><td> 26</td><td> 10</td><td> 8</td><td> 5</td><td> 4</td><td> 0</td><td> 8</td>

<td> 14</td><td> 26</td><td> 20</td><td> 2</td><td> 5</td><td> 4</td><td> 0</td><td> 10</td>

<td> 15</td><td> 26</td><td> 20</td><td> 8</td><td> 5</td><td> 10</td><td> 2</td><td> 10</td>

<td> 16</td><td> 26</td><td> 15</td><td> 5</td><td> 3</td><td> 7</td><td> 1</td><td> 10</td>

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Examples 17 to 22

Various cleaning compositions were prepared by mixing 26 g of NMP, 15 g of monoethanolamine (MEA), 5 g of either diethylene glycol (DEGA) or diethylene glycol (DEG), 3 g of catechol (CAT) and 7 g of deionized water. The same type of Al technology patterned disc samples with "perforated" path structures as used in the previous examples were placed in these solutions, heated at the temperatures indicated below for 20 minutes, after which they were separated, They were rinsed in deionized water for two minutes and blown dry with dry nitrogen. The clean discs were then evaluated for ash residue separation (0 = no separation, at 10 = 100% separation) and aluminum corrosion (0 = no corrosion, at 10 = corrosion), as observed in Table 7.

TABLE 7

<td>Example No.</td><td>Solution content</td><td>Temperature lllllllll</td><td>Aluminum corrosion</td><td>Ash residue separation</td>

<td> 17</td><td>DEGA</td><td> 65</td><td> 0</td><td> 3</td>

<td> 18</td><td>DEGA</td><td> 75</td><td> 0</td><td> 6</td>

<td> 19</td><td>DEGA</td><td> 85</td><td> 1</td><td> 9</td>

<td> 20</td><td>SDR</td><td> 65</td><td> 0</td><td> 6</td>

<td> 21</td><td>SDR</td><td> 75</td><td> 0</td><td> 8</td>

<td> 22</td><td>SDR</td><td> 85</td><td> 0</td><td> 10</td>

Examples 23 to 25

Various cleaning compositions were prepared by mixing 1-methyl-2-pyrrolidinone (NMP), monoethanolamine (MEA), diethylene glycol (DEG), catechol (CAT), and deionized water in the amounts shown below. The same type of Al technology patterned disc samples with "perforated" path structures as used in the previous examples were placed in these solutions, heated at 65 ° C for 20 minutes, after which they were separated, rinsed in deionized water for two minutes and blown dry with dry nitrogen. The clean discs were then evaluated for the separation of ash residues (0 = no separation, at 10 = separation of is observed in Table 8.

TABLE 8

<td>Example No.</td><td>NMP</td><td>MEA</td><td>SDR</td><td>Catechol</td><td>h₂or</td><td>Aluminum corrosion</td><td>Ash residue separation</td>

<td> 23</td><td> 46</td><td> 21</td><td> 13</td><td> 7</td><td> 13</td><td> 0</td><td> 10</td>

<td> 24</td><td> 46</td><td> 25</td><td> 9</td><td> 7</td><td> 13</td><td> 2</td><td> 10</td>

<td> 25</td><td> 54</td><td> 21</td><td> 9</td><td> 3</td><td> 13</td><td> 1</td><td> 10</td>

Examples 26 to 29

Various cleaning compositions were prepared by mixing 46 g of a solvent selected from the following: 1-methyl-2-pyrrolidinone (NMP), N, N-dimethylacetamide (DMAC), or dimethyl sulfoxide (DMSO), 23 g of monoethanolamine ( MEA) or 1-amino-2-propanol (AMP); 11 g of diethylene glycol (DEG); 5 g of catechol (CAT); and 15 g of deionized water. The same type of Al technology patterned disc samples with "perforated" path structures as used in the previous examples were placed in these solutions, heated at 65 ° C for 20 minutes, after which they were separated, rinsed in deionized water for two minutes and dried by so

ES 2 335 786 T3 planted with dry nitrogen. The clean discs were then evaluated for ash residue separation (0 = no separation, at 10 = 100% separation) and aluminum corrosion (0 = no corrosion, at 10 = corrosion), as observed in Table 9.

TABLE 9

<td>Example No.</td><td></td><td></td><td></td><td></td><td></td><td>Aluminum corrosion</td><td>Ash residue separation</td>

<td> 26</td><td>NMP</td><td>MEA</td><td>SDR</td><td>Catechol</td><td>H₂OR</td><td> 0</td><td> 10</td>

<td> 27</td><td>NMP</td><td>AMP</td><td>SDR</td><td>Catechol</td><td>h₂or</td><td> 0</td><td> 8</td>

<td> 28</td><td>DMAC</td><td>MEA</td><td>SDR</td><td>Catechol</td><td>h₂or</td><td> 2</td><td> 10</td>

<td> 29</td><td>DMSO</td><td>MEA</td><td>SDR</td><td>Catechol</td><td>h₂or</td><td> 1</td><td> 9</td>