CN1778830A - Cleaning substrate of substrate processing equipment and heat resistant resin preferable therefor - Google Patents
Cleaning substrate of substrate processing equipment and heat resistant resin preferable therefor Download PDFInfo
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- CN1778830A CN1778830A CN 200510124931 CN200510124931A CN1778830A CN 1778830 A CN1778830 A CN 1778830A CN 200510124931 CN200510124931 CN 200510124931 CN 200510124931 A CN200510124931 A CN 200510124931A CN 1778830 A CN1778830 A CN 1778830A
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Abstract
The present invention provides a cleaning substrate of a substrate processing equipment, which comprises a cleaning layer comprising a heat resistant resin with a storage modulus (1 Hz) at 20 DEG C. up to 150 DEG C. being 5x10<SUP>7 </SUP>Pa to 1x10<SUP>9 </SUP>Pa on at least one face of the substrate; and a polyimide resin suitable as the heat resistant resin for the cleaning layer and usable under circumstances possibly involving the generation of serious disadvantages due to silicone contamination, such as for HDD application and some semiconductor applications.
Description
Technical field
The present invention relates to the cleaning substrate of substrate processing equipment, and relate to preferred heat-resistant resin as the cleaning substrate clean layer.
Background technology
The polyimide of low elasticity is often used as insulating film, the semi-conductor bonding film of protective membrane in the semi-conductor, multi-layer circuit substrate, (referring to the patent documentations 1,2,3,4 and 5) such as tectums of flexible circuit substrate as a kind of low-stress and thermotolerance material.
Because the polyimide of these low elasticities is to be obtained by diamines that contains siloxanes or tetracarboxylic anhydride generation copolyreaction, yet, these polyimide must not be used for relating to the application that produces defective owing to siloxanes impurity, and for example HDD uses and some semiconductor application.
As mentioned above, need low elasticity, can be used in HDD and the semi-conductive production unit and can not produce the heat-resistant resin of pollution.
In addition, some are used for the dust separating cleaning substrate of these device interiors and are included in the layer (referring to patent documentation 6 and 7) that comprises synthetic resins (for example acrylic resin) on the siloxane sheet.Yet the thermotolerance of talkative these substrates is not gratifying in the desired thermotolerance of pre-treatment step especially.Therefore, the cleaning substrate that needs high heat resistance.
Especially, in the first half of producing semiconductor devices (especially PVD equipment) is handled, at high temperature use dedusting sheet (dusting wafer) usually.Therefore, require it to have different physicalies, for example thermotolerance and the stability in the temperature range that is used for these equipment dustproof (dust proofing).
[patent documentation 1] JP-A-5-170901
[patent documentation 2] JP-A-6-73178
[patent documentation 3] JP-A-6-207024
[patent documentation 4] JP-A-6-73178
[patent documentation 5] JP-A-2002-50854
[patent documentation 6] JP-A-2001-351960
[patent documentation 7] JP-A-2002-18377
Summary of the invention
According to the present invention, a kind of cleaning substrate of the substrate processing equipment such as semiconductor devices is provided, it also has favourable cleaning performance except having salient features (for example transferability and reach the required time limit of vacuum).In addition, according to the present invention, also provide the heat resistance resin, it is preferably used as cleaning substrate, and can be used for relating to the application that produces major defect owing to siloxanes impurity, for example is used for HDD and uses and some semiconductor application.
Solve these problems by following structure.
(1) a kind of cleaning substrate of substrate processing equipment, the clean layer that wherein comprises comprises:
Substrate and
Being positioned at least one of substrate lip-deep is 5 * 10 (1Hz) at 20 ℃～150 ℃ following storage moduluses (storagemodulus)
7Pa to 1 * 10
9The heat-resistant resin of Pa.
(2) according to the cleaning substrate of the substrate processing equipment of above-mentioned (1), wherein heat-resistant resin is for the tetracarboxylic dianhydride with contain polyether structure at least and have the heat-resistant resin (being referred to as heat-resistant resin A hereinafter sometimes) that the compound of at least two terminal amine structural constituents is polymerized as diamines.
(3) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (1):
Wherein a represents the integer more than or equal to 2.
(4) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the following formula (R1):
Wherein a represents the integer more than or equal to 2, and the Ar representative contains the structure of at least one aromatic nucleus.
(5) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (2):
Wherein b, c and d represent the integer more than or equal to 0 independently of one another, and condition is that b+c+d is more than or equal to 2.
(6) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the formula (R2):
Wherein b, c and d represent the integer more than or equal to 0 independently of one another, and condition is that b+c+d is more than or equal to 2.The Ar representative contains the structure of at least one aromatic nucleus.
(7) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (3):
Wherein e, f and g represent the integer more than or equal to 0 independently of one another, and condition is that e+f+g is more than or equal to 2.
(8) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the formula (R3):
Wherein e, f and g represent the integer more than or equal to 0 independently of one another, and condition is that e+f+g is more than or equal to 2.The Ar representative contains the structure of at least one aromatic nucleus.
(9) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (4):
Wherein h represents the integer more than or equal to 1.
(10) according to the cleaning substrate of the substrate processing equipment of above-mentioned (2), wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the formula (R4):
Wherein h represents the integer more than or equal to 1.The Ar representative contains the structure of at least one aromatic nucleus.
(11) a kind of to the dust separating method in substrate processing equipment surface, comprising contacting with the surface of substrate processing equipment according to the resin surface of the cleaning substrate of above-mentioned (1)～(10) described in each.
Particularly, the invention provides following heat-resistant resin.
(12) a kind of by the tetracarboxylic dianhydride with contain polyether structure at least and have the heat-resistant resin (heat-resistant resin A) that the compound of at least two terminal amine structures is polymerized as diamine components.
(13) according to the heat-resistant resin of above-mentioned (12), wherein containing polyether structure is the compound shown in the formula (1) with the compound with at least two terminal amine structures.
(14) a kind of heat-resistant resin with structural unit shown in the formula (R1).
(15) according to the heat-resistant resin of above-mentioned (12), wherein containing polyether structure is the compound shown in the formula (2) with the compound with at least two terminal amine structures.
(16) a kind of heat-resistant resin with structural unit shown in the formula (R2).
(17) according to the heat-resistant resin of above-mentioned (12), wherein containing polyether structure is the compound shown in the formula (3) with the compound with at least two terminal amine structures.
(18) a kind of heat-resistant resin with structural unit shown in the formula (R3).
(19) according to the heat-resistant resin of above-mentioned (12), wherein containing polyether structure is the compound shown in the formula (4) with the compound with at least two terminal amine structures.
(20) a kind of heat-resistant resin with structural unit shown in the formula (R4).
The cleaning substrate of substrate processing equipment of the present invention is the inside of clean semiconductor equipment (especially being in the semiconductor devices in the high vacuum) effectively, it can carry out effective cleaning and not reduce the vacuum tightness of these semiconductor devices inside this equipment in a short period of time, perhaps allows its inside more promptly to recover vacuum tightness.
Can be used in the cleaning substrate of substrate processing equipment (for example semiconductor devices) as clean layer according to above-mentioned (1) described heat-resistant resin.Use this heat-resistant resin to produce and can be used for the more dustproof sheet of wide temperature range, for example, in the first half of producing semiconductor devices is handled, be used for the dust-proof sheet.
In addition, heat-resistant resin A can be used as the high heat resistance polyimide with low-stress and small elastic modulus and uses, and is used for relating to the application that produces major defect owing to siloxanes impurity, and for example HDD uses and semiconductor application.
Embodiment
According to the present invention, had been found that the cleaning substrate that comprises clean layer at least one surface of substrate has the good performance that can overcome the problems referred to above,, it is 5 * 10 that this clean layer is included in 20 ℃～150 ℃ following storage moduluses (1Hz)
7Pa～1 * 10
9The heat-resistant resin of Pa.
Storage modulus (1Hz) under 20 ℃ to 150 ℃ is preferably 8 * 10
7Pa～8 * 10
8Pa is preferably 1 * 10 especially
8Pa～6 * 10
8Pa.
Heat-resistant resin as clean layer for example comprises; ladder polymer such as phenyl-T; polyquinoxaline and poly-benzoylene benzoglyoxaline (polybenzoylene benzimidazole); aromatic(based)polymer such as polyphenylene; polymeric amide; polyester-imide, polybenzimidazole, polycarbodiimide and aromatic poly.
Preferred especially polyimide, polymeric amide and polycarbodiimide be as clean layer, even also can not produce volatile gases or decompose monomer because they are exposed under 400 ℃ or the higher temperature.
In addition, according to the present invention, find that heat-resistant resin is preferably a kind of heat resistance resin (heat-resistant resin A), this resin by the tetracarboxylic dianhydride and the compound that contains polyether structure (comprising for example oxyalkylene) at least and have at least two terminal amine structures condense together as diamine components and obtain.
At this, polyimide resin comprises the imide resin and the polyamic acid of the imide bond with formation, and does not have the imidization reaction as this imide resin of precursor.
Preferred heat-resistant resin A not only can be used as the clean layer of cleaning substrate, but also can be used as high heat resistance polyimide resin with low-stress and small elastic modulus, to be used for relating to the application that produces major defect owing to siloxanes impurity, for example HDD uses and semiconductor application.
(compound that contains polyether structure and have at least two terminal amine structures)
According to the present invention, employed diamine components is the compound (being referred to as the PE diamine compound hereinafter) that contains polyether structure and have at least two terminal amine structures in synthetic heat-resistant resin A.Use this PE diamine compound can produce high heat resistance polyimide with low-stress and small elastic modulus.
Any PE diamine compound that contains polyether structure and have at least two terminal amine structures all is suitable and be not particularly limited, and preferably includes the PE diamine compound with two terminal amine structures that is for example prepared by oxyethane, propylene oxide, polytetramethylene glycol, polymeric amide or their mixture.
Polyether structure in the PE diamine compound is to have two or more structures by the alkylideneoxygen group (alkyleneoxy group) of-A-O-representative.A represents alkylidene group.The O represention oxygen atom.
Alkylidene group with " A " expression has 1～10 carbon atom, preferred 2～5 carbon atoms and comprise for example methylene radical, ethylidene, propylidene and butylidene usually.
A plurality of these alkylideneoxygen groups can be identical or different.In addition, the alkylidene group with " A " expression can have substituting group (for example methyl, polyether group and amino-polyether group).
In the PE diamine compound, the quality of polyether structure is generally 50% or more, and preferred 70% or more.
The amine structure of two ends in the PE diamine compound can be identical or different.Any primary amine to tertiary amine structure all is gratifying.Amine structure is preferably primary amine.
Amine structure comprises for example methylamine, ethamine and propylamine.Amine structure is preferably propylamine.
The number-average molecular weight of PE diamine compound is 200～5,000, is preferably 600～4,000.
The PE diamine compound comprises for example compound shown in formula (1)～(4).
In formula (1), a represents the integer more than or equal to 2, is preferably 5～80.
In formula (2), b, c and d represent the integer more than or equal to 0 independently of one another, condition be (b+c+d) and more than or equal to 2, be preferably 5～50.
In formula (3), e, f and g represent the integer more than or equal to 0 independently of one another, condition be (e+f+g) and more than or equal to 2, be preferably 5～30.
In formula (4), h represents the integer more than or equal to 1, is preferably 1～4.
The PE diamine compound can be by the synthetic preparation of known method.In addition, also can be fit to use this commercially available compounds.
In order to react with the tetracarboxylic dianhydride, another diamine compound that does not have any polyether structure can be preferably and the PE diamine compound unite use as diamine compound.The diamine compound of associating use preferably includes aliphatie diamine for example as described below and aromatic diamine.
(aliphatie diamine)
Aliphatie diamine comprises for example quadrol/hexamethylene-diamine, 1,8-diamino octane, 1,10-diamino decane, 1,12-diamino dodecane, 4,9-two oxa-s-1,12-diamino dodecane and 1, two (the 3-aminopropyls)-1 of 3-, 1,3, the 3-tetramethyl disiloxane.
The molecular weight of these aliphatie diamines is generally 50～1, and 000, be preferably 100～300.
(aromatic diamine)
Aromatic diamine for example comprises 4,4 '-diaminodiphenyl oxide, 3,4 '-diaminodiphenyl oxide, 3,3 '-diaminodiphenyl oxide, mphenylenediamine, Ursol D, 4,4 '-diamino-diphenyl propane, 3,3 '-diamino-diphenyl propane, 4,4 '-diaminodiphenyl-methane, 3,3 '-diaminodiphenylmethane, 4,4 '-diaminodiphenyl sulfide, 3,3 '-diaminodiphenyl sulfide, 4,4 '-diaminodiphenylsulfone(DDS), 3,3 '-diaminodiphenylsulfone(DDS), 1, two (4-amino-benzene oxygen) benzene of 4-, 1, two (4-amino-benzene oxygen) benzene of 3-, 1, two (3-amino-benzene oxygen) benzene of 3-, 1, two (the 4-amino-benzene oxygens)-2 of 3-, 2-dimethylpropane and 4,4 '-the diamino benzophenone.
Wherein, preferred 4 and Ursol D.
(tetracarboxylic dianhydride)
Tetracarboxylic dianhydride with any special qualification all can use as the tetracarboxylic dianhydride in heat-resistant resin A of the present invention synthetic, for example comprise 3,3 ', 4,4 '-biphenyl tetracarboxylic dianhydride, 2,2 ', 3,3 '-biphenyl tetracarboxylic dianhydride, 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride (3,3 ', 4,4 '-benzophenonetetracarboxylicdianhydride), 2,2 ', 3,3 '-benzophenone tetracarboxylic dianhydride, 4,4 '-the oxydiphthalic acid dianhydride, 2, (2,2-bis (2 for hexafluoropropane dianhydride for 2-two (2,3-two carboxyphenyls), 3-dicarboxyphenyl) hexafluoropropane dianhydride), 2, two (3, the 4-carboxyphenyl) hexafluoropropane dianhydrides (6FDA) of 2-, two (2,3-two carboxyphenyls) methane dianhydride, two (3,4-two carboxyphenyls) methane dianhydride, two (2,3-two carboxyphenyls) sulfone dianhydride (bis (2,3-dicarboxyphenyl) sulfone dianhydride), two (3,4-two carboxyphenyls) sulfone dianhydride, pyromellitic acid anhydride and ethylene glycol bis 1,2,4-benzenetricarboxylic acid dianhydride (ethylene glycol bistrimelliticdianhydride).They can use separately, or two or more are used in combination.
Preferred tetracarboxylic dianhydride for example comprises 3,3 ', 4,4 '-phenylbenzene tetracarboxylic dianhydride, 4,4 '-oxydiphthalic acid dianhydride, 2, two (3, the 4-carboxyphenyl) hexafluoropropane dianhydride (6FDA) and the pyromellitic acid anhydrides of 2-.
Heat-resistant resin A preferred examples comprises having the resin of the resulting structures that reacts between diamine compound shown in formula (1)～(4) and the tetracarboxylic dianhydride.
Hereinafter, the Ar representative has the structure of at least one aromatic nucleus, preferably has 6～30 carbon atoms, comprises for example phenyl ring, biphenyl and phenyl ether.
A～h is identical with a～h implication in formula (1)～(4).
(preparation heat-resistant resin A)
Heat-resistant resin A of the present invention can react by PE diamine compound and tetracarboxylic dianhydride and obtain, and this reaction is carried out in solvent usually.
The PE diamine compound can carry out blend with stoichiometric method, until equating with tetracarboxylic dianhydride's consumption.Yet the consumption of preferred PE diamine compound is that stoichiometry is normal 5～60%, more preferably 5～30%.In this case, other diamine compound, for example above-mentioned aliphatie diamine and aromatic diamine can be used as diamine components and unite use.
The total amount of PE diamine compound and other diamine compound usually with tetracarboxylic dianhydride's consumption stoichiometry equivalent, also can be suitable excessive, for example above stoichiometry normal 100～500%.
Heat-resistant resin A of the present invention preferably comprises the structural unit that is derived from PE diamine compound and tetracarboxylic dianhydride reaction, and its quality is preferably 10～80% in dried total mass, and more preferably 20～50%.
The solvent that uses in the reaction comprises organic solvent, for example N,N-dimethylacetamide, N-N-methyl-2-2-pyrrolidone N-and N, and dinethylformamide, and be preferably the N-N-methyl-2-2-pyrrolidone N-.In addition, in order to adjust raw material and dissolving resin degree, can suitably mixed therein and use non-polar solvent, for example toluene and dimethylbenzene.
The concentration of solute in reaction soln is generally 5～50% quality, and temperature of reaction is generally envrionment temperature (for example 23 ℃)～220 ℃ and the reaction times is generally 1～10 hour, is preferably 3～6 hours.
By thermal treatment heat-resistant resin A (preferably in inert atmosphere, carrying out) at high temperature, can improve the thermotolerance of the heat-resistant resin A that the method according to this invention obtains more significantly.Heat treated condition in the process of heat treated condition and the cleaning substrate of following production substrate processing equipment is identical.
(production of the cleaning substrate of substrate processing equipment)
Can obtain the cleaning substrate of substrate processing equipment of the present invention by the following method: apply heat-resistant resin on substrate, next dry removing desolvated, and substrate is heat-treated, and preferably at high temperature heat-treats.
The clean layer that contains heat-resistant resin A can also contain other resin and additive except that heat-resistant resin A, be preferably 50% quality of clean layer total mass or lower, more preferably 10% quality or lower.
Use spin-coating method and spraying method as coating process, heat-resistant resin A directly is coated on the suitable substrate such as siloxane sheet.In addition, use pause coating method (comma coat process), gunite (fountain process) and notch board method (gravure process), heat-resistant resin A can be coated on PET film or the polyimide film, then it is transferred to or adheres to suitable substrate, for example on the siloxane sheet.
In addition, behind the dry solvent, the temperature of high-temperature heat treatment is suitably for 200 ℃ or higher, and is preferably 250 ℃～350 ℃, and the time of handling is generally 10 minutes～5 hours, be preferably 30 minutes～2 hours.For oxidation and the deterioration that prevents resin, need be in inert atmosphere (for example in nitrogen atmosphere and vacuum) thermal treatment resin.Can improve thermotolerance more significantly by thermal treatment, the volatile constituent that remains in simultaneously in the resin also can be removed fully.
The substrate that is equipped with clean layer in the above comprises but is not defined as various types of substrates especially that it depends on the type that will therefrom remove the substrate processing equipment of foreign matter in some sense.Especially, this substrate comprises for example flat pannel display substrate (for example semiconductor chip, LCD and PDP) and other substrate (substrate that for example is used for compact disk and MR magnetic head).
Clean layer is fit to be arranged at least one surface of substrate.Clean layer also can be arranged on its two surfaces.In addition, clean layer can very eligibly be arranged in all or only on part surface, for example on edge surface.
Clean layer ground thickness (dry back) is generally 1～50 μ m, is preferably 5～20 μ m.If thickness is blocked up, because the existence of planar water, the vacuum tightness of equipment reduces sometimes.If thickness is thin excessively, clean-up performance is degenerated sometimes.
Carry out dust separating substrate processing equipment according to the present invention and comprise but be not defined as especially, for example exposure sources, resist-coating equipment, developing apparatus, ashing (ashing) device, dry etching equipment, ion implantation device, PVD equipment, CVD equipment, outward appearance testing apparatus and wafer prober.
So just can be formed on 20 ℃ of-150 ℃ of following storage moduluses (1Hz) is 5 * 10
7Pa-1 * 10
9The clean layer of Pa, so the clean layer of gained has the better cleaning performance.
In addition, clean layer at ambient temperature (for example, 23 ℃) modulus in tension of having be 1.5GPa or lower.Modulus in tension is preferably 1.5GPa or lower, more preferably 0.1～0.8GPa.Because this modulus in tension, the clean layer of gained just can have better dustproof distribution (profile).When modulus in tension was lower than 0.1GPa, clean layer finally can adhere to the contact surface of substrate processing equipment, caused can not shifting sometimes.
Substrate processing equipment can be provided according to the present invention, dust can be therefrom removed by aforesaid method.
Embodiment
Below, with reference to embodiment the present invention is more specifically described, yet the present invention is not limited to these embodiment.
(storage modulus)
The sample that is of a size of 5.0 * 22.6mm is measured under the 1Hz frequency, distortion (diatortion) be 0.3% and temperature rise rate be 10 ℃/min, utilize commodity to be called the device measuring visco-elasticity of RS-11 (making) by Rheometric ScientificInc..
(modulus in tension)
Use is according to the method for JIS K7127 method of testing.Measuring temperature is 23 ℃.
(clean-up performance)
(NittohSeiki makes to utilize the lining form peel-off device (liner film peel-off apparatus) of producing cleaning foil; HR300CW) (device A), the assessment clean-up performance.At first, 20 aluminium flakes that cut into 1mm * 1mm size in advance are arranged on the chuck table of equipment (chuck table).Then, clean layer one side of cleaning substrate is transferred to device A with the form of dummy (dummy), next vacuum suck is at chuck table (0.5kg/cm
2) on, so that clean layer is together bonded to each other securely with the chuck table part that contacts this clean layer.Then, remove vacuum suck, to remove cleaning substrate from chuck table.At this moment, be the dustproof rate of basic measurement with the aluminium flake number that is retained on the chuck table.Replication three times, calculating mean value.
(transferability)
Mode according to identical shifts with equipment on chuck table, to carry out vacuum suck.After removing vacuum, the ability of with lift pins (lift pin) cleaning element (CW) being peeled off from chuck table (CT) with 5 level evaluations.When the transferability index is 3 or when higher, can peel off.
Transferability index (gratifying level is 3 or higher)
5: highly stable (being equivalent to silicon wafer)
4: from the process that CT shifts, CW more or less shakes, and comprises the low-down noise of peeling off.
3: from the process that CT shifts, CW more or less shakes, and comprises the low noise of peeling off.
2: from the process that CT shifts, CW shakes, and comprises the quite higher noise of peeling off.
1: from the process that CT shifts, CW shakes, and comprises the very high noise of peeling off.
(reaching the required time of vacuum)
As reaching the needed time of vacuum, with 1cm
2The cleaning transfer element put into and heat up and spectrometry mass (the Electron Science manufacturing of release type; EMD-WA 1000S) in the time of in, measurement returned to initial vacuum tightness 1 * 10 when temperature was remained 50 ℃
-9Torr (1.33 * 10
-7Pa) required time.At this, the condition of measuring is as follows: cavity temperature remains on 50 ℃; Sample size is 1cm
2, and initial vacuum tightness is 3 * 10
-10Torr (4.0 * 10
-8Pa).After putting into sample, determine that vacuum tightness returns to 1 * 10
-9Torr (1.33 * 10
-7Pa) required time.
When the time very in short-term, it is less that the preferred time is produced influence to vacuum.
Embodiment 1
[Sun Technochemical produces with the 32.2g polyether diamine; XTJ-502 (ED-2003)] and the 9.4g Ursol D be dissolved in the 286.3g N-N-methyl-2-2-pyrrolidone N-(NMP).Then, it is described below 3,3,4 to add 30g, and 4-biphenyl tetracarboxylic dianhydride (being abbreviated as BPDA hereinafter) is to react.The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
Embodiment 2
[Sun Technochemical produces with the 32.3g polyether diamine; XTJ-500 (ED-600)] and 12.6g4,4 '-diaminodiphenyl oxide is dissolved among the 279.9g NMP.Then, add 25g pyromellitic acid anhydride described below (being abbreviated as PMDA hereinafter) to react.The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
Embodiment 3
[Sun Technochemical produces with the 29.0g polyether diamine; XTJ-502 (ED-2003)] and the 15.6g 4 be dissolved among the 258.2g NMP.Then, add 20g PMDA to react.The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
Embodiment 4
[Sun Technochemical produces with the 44.0g polyether diamine; XTJ-510 (D4000)] and 25.3g4,4 '-diaminodiphenyl oxide is dissolved among the 397.4g NMP.Then, add 30g PMDA to react.The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
Embodiment 5
(Sun Technochemical produces with the 40.7g polyether diamine; XTJ-542) and the 10.1g 4 be dissolved among the 283.4g NMP.Then, add 20.0g PMDA to react.The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
The polyether diamine type (Sun Technochemical production) that uses among the embodiment 1～5 is as follows:
XTJ-500 (ED-600): the compound of formula (2), wherein c=9.0; B+c+d=3.6;
XTJ-502 (ED-2003): the compound of formula (2), wherein c=38.7; B+d=6;
XTJ-510 (D4000): the compound of formula (1), wherein a=68;
XTJ-542: the compound of formula (3), wherein e+g=6.0; F=9.0;
When heat-resistant resin film being appointed as dustproof surface, the clean-up performance by having 8 inches siloxanes wafers of heat-resistant resin film on its of preparation among the preceding method assessment embodiment 1～5, reach required time of vacuum and transferability.The heat-resistant resin film that will form on sheet glass is peeled off from sheet glass, to determine its storage modulus and modulus in tension according to aforesaid method.
Comparative example 1
Coated with resins on 8 inches siloxanes wafers not, and with minute surface as adhesive face, the assessment clean-up performance, reach required time of vacuum and transferability.
Comparative example 2
With 30.0g 1,2-two trimellitic acid second diester tetracarboxylic dianhydride (ethylene-1,2-bistrimellitatetetracarboxylic dianhydride) (be abbreviated as TMEG hereinafter) and 65.8g to have the diamines (900 normal amine and content are 18% vinyl cyanide) of following structure and 15.0g 2,2 '-two [4-(4-amino-benzene oxygen) phenyl] propane (being abbreviated as BAPP hereinafter) mixed and react under nitrogen atmosphere at 120 ℃ in 110g N-N-methyl-2-2-pyrrolidone N-(being abbreviated as NMP hereinafter).
The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
Comparative example 3
With 200 parts Macrogol 200 dimethacrylates (Shin-nakamura Chemical Co., Ltd. production; Commodity are called NK ester 4G), 3 parts polyisocyanate compounds (NipponPolyurethane Industry Co., Ltd. produces; Commodity are called Coronate L), (Mitsubishi Gas Chemical Company Inc. produces for 2 parts epoxy series compound; Commodity are called Tetrad C) and 3 parts of benzyldimethylketals as Photoepolymerizationinitiater initiater (benzyldimethyl ketal) (ChibaSpecialty Chemical production; Commodity are called Irugacure-651) (weight-average molecular weight is 700 with 100 parts the acryloyl polymkeric substance that is obtained by 75 parts of 2-EHAs, 20 parts methyl acrylate and 5 parts of vinylformic acid d monomer mixed solution, 000) homogeneous phase is mixed, solidifies the binder solution of (UV setting) type with preparation UV.
Perhaps, with 73 parts of 2-EHAs, 10 parts n-butyl acrylate, 15 parts N, N-DMAA, 5 parts vinylformic acid, 0.15 part are as 2 of initiators for polymerization, it is 200g that the ethyl acetate of 2 '-Diisopropyl azodicarboxylate and 100 parts is blended into total amount, pack into then in the 500ml there-necked flask reactor that is equipped with thermometer, agitator, nitrogen inlet and reflux exchanger, be blown under the condition of nitrogen stir about 1 hour, so that replace wherein air with nitrogen.Next internal temperature is adjusted to 58 ℃.The maintenance internal state obtained binder polymer solution to carry out polymerization in about 4 hours.With 3 parts of polyisocyanate compounds (Nippon Polyurethane Industry Co., Ltd. production; Commodity are called Coronate L) evenly mixed with 100 parts of binder polymer solution, obtain binder solution A.
Use the siloxane series releasing agent to continuous polycondensation film (Mitsubishi Polyester Film, GmbH production; Commodity are called MRF50N100; Thickness is 50 μ m, and width is 250mm) a face handle.With binder solution A be coated on the successive polyester film through surface that the siloxanes demoulding is handled to obtain the dry thickness of 5 μ m.The successive vinyl-vinyl acetate copolymer is covered (up to thickness is 100 μ m, and width is 250mm) on the binder layer.In addition, the binder solution A with the UV curing is coated on the film to obtain the dry thickness of 5 μ m, so that binder layer is set to clean layer.After the siloxane series releasing agent was handled one side, (Mitsubishi Polyester Film company limited produced with the continuous polycondensation film; Commodity are called MRF 50 N100; Thickness is 50 μ m, and width is 250mm) siloxanes demoulding treat surface bond on this surface, with prepared layer compressing tablet A.
By making total radiation is 1,000mJ/cm
2, centre wavelength is the uviolizing laminate A of 365nm, obtain having the cleaning foil A that UV solidifies clean layer.
Peel off the common protective membrane that cleaning foil A goes up binder layer one side, film is bonded on the minute surface of 8 inches siloxane sheets, make cleaning transfer element A thus.
Comparative example 4
The 27.5g 4 is dissolved among the 230.2g NMP.Then, add 30.0gPMDA to react.The refrigerative resin solution of gained is coated in spin coater on the minute surface of 8 inches siloxane sheets and on the sheet glass, 90 ℃ dry 20 minutes down.Under 280 ℃, thermal treatment is 2 hours in nitrogen atmosphere with it, and forming thickness is the heat-resistant resin film of 20 μ m.
When heat-resistant resin film being appointed as dustproof surface, by the preceding method assessment to the clean-up performance that is formed with 8 inches siloxanes wafers of heat-resistant resin film on its of preparation in the above-mentioned comparative example 2～4, reach required time of vacuum and transferability.
Measure the storage modulus and the modulus in tension that on heat-resistant resin film that forms on the sheet glass and cleaning foil A, have the clean layer of ultraviolet curing of preparation in the comparative example 2 and 4 according to aforesaid method.
The assessment result of embodiment 1～5 and comparative example 1～4 is as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Storage modulus (20 ℃) (Pa) | 8.9×10 8 | ?2.0×10 8 | ?3.7×10 8 | ?4.5×10 8 | ?3.6×10 8 | ?- | ?1.0×10 9 | ?1.3×10 9 | ?2.8×10 9 |
| Storage modulus (100 ℃) (Pa) | 4.0×10 8 | ?8.5×10 7 | ?2.8×10 8 | ?2.9×10 8 | ?1.3×10 8 | ?- | ?3.2×10 7 | ?3.2×10 7 | ?2.4×10 9 |
| Storage modulus (150 ℃) (Pa) | 3.0×10 8 | ?5.5×10 7 | ?1.6×10 8 | ?2.5×10 8 | ?1.0×10 8 | ?- | ?1.5×10 7 | ?1.8×10 6 | ?2.1×10 9 |
| Modulus in tension (GPa) | 0.4 | ?0.1 | ?0.2 | ?0.2 | ?0.2 | ?- | ?0.5 | ?0.5 | ?1.5 |
| Dustproof rate (20 ℃) (%) | 100 | ?100 | ?100 | ?100 | ?100 | ?50 | ?90 | ?80 | ?70 |
| Dustproof rate (150 ℃) (%) | 100 | ?100 | ?100 | ?100 | ?100 | ?50 | ?- | ?- | ?70 |
| Reach the vacuum required time (minute) | 3.6 | ?3.4 | ?3.9 | ?3.2 | ?3.9 | ?3.0 | ?3.6 | ?3.5 | ?3.3 |
| Transferability (20 ℃) | 4 | ?4 | ?4 | ?4 | ?4 | ?5 | ?4 | ?4 | ?5 |
| Transferability (150 ℃) | 4 | ?3 | ?4 | ?4 | ?4 | ?5 | ?2 | ?1 | ?5 |
Have and comprise the cleaning substrate of clean layer that storage modulus of the present invention satisfies the heat-resistant resin of given environment and have ideal storage modulus and modulus in tension, so substrate can be brought into play favourable cleaning performance, but can as common wafer, not need just can reach vacuum for a long time, without any the problem of transferability.
Though with reference to its embodiment and describe the present invention in detail,, do not deviating under the scope of the present invention, can carry out variations and modifications, this is conspicuous to those skilled in the art.
The application is based on the Japanese patent application 2005-297735 of Japanese patent application 2004-304027 that submitted on October 19th, 2004 and submission on October 12nd, 2005, and its full content is hereby incorporated by.
Claims (20)
1. the cleaning substrate of a substrate processing equipment, comprising:
Substrate and
It is lip-deep and be 5 * 10 at 20 ℃～150 ℃ following storage moduluses (1Hz) to comprise at least one that be positioned at substrate
7Pa to 1 * 10
9The clean layer of the heat-resistant resin of Pa.
2. according to the cleaning substrate of the substrate processing equipment of claim 1, wherein heat-resistant resin is for the tetracarboxylic dianhydride with contain polyether structure at least and have the heat-resistant resin that the compound of at least two terminal amine structures is polymerized as diamine components.
3. according to the cleaning substrate of the substrate processing equipment of claim 2, the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (1):
Wherein a represents the integer more than or equal to 2.
4. according to the cleaning substrate of the substrate processing equipment of claim 2, wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the following formula (R1):
Wherein a represents the integer more than or equal to 2, and the Ar representative contains the structure of at least one aromatic nucleus.
5. according to the cleaning substrate of the substrate processing equipment of claim 2, the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (2):
Wherein b, c and d represent the integer more than or equal to 0 independently of one another, and condition is that b+c+d is more than or equal to 2.
6. according to the cleaning substrate of the substrate processing equipment of claim 2, wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the formula (R2):
Wherein b, c and d represent the integer more than or equal to 0 independently of one another, condition be b+c+d more than or equal to 2, and Ar representative contains the structure of at least one aromatic nucleus.
7. according to the cleaning substrate of the substrate processing equipment of claim 2, the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (3):
Wherein e, f and g represent the integer more than or equal to 0 independently of one another, and condition is that e+f+g is more than or equal to 2.
8. according to the cleaning substrate of the substrate processing equipment of claim 2, wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the formula (R3):
Wherein e, f and g represent the integer more than or equal to 0 independently of one another, condition be e+f+g more than or equal to 2, and Ar representative contains the structure of at least one aromatic nucleus.
9. according to the cleaning substrate of the substrate processing equipment of claim 2, the compound that wherein contains polyether structure and have at least two terminal amine structures is the compound shown in the formula (4):
Wherein h represents the integer more than or equal to 1.
10. according to the cleaning substrate of the substrate processing equipment of claim 2, wherein heat-resistant resin is for having the heat-resistant resin of structural unit shown in the formula (R4):
Wherein h represents the integer more than or equal to 1, and the Ar representative contains the structure of at least one aromatic nucleus.
11. one kind to the dust separating method in substrate processing equipment surface, contacts with the surface of substrate processing equipment comprising the resin surface with the cleaning substrate of claim 1～10 in each.
12. a heat-resistant resin, its by the tetracarboxylic dianhydride and the compound that contains polyether structure at least and have at least two terminal amine structures be polymerized as diamine components.
13. according to the heat-resistant resin of claim 12, wherein containing polyether structure is the compound shown in the formula (1) with the compound with at least two terminal amine structures:
Wherein a represents the integer more than or equal to 2.
14. heat-resistant resin with structural unit shown in the formula (R1):
Wherein a represents the integer more than or equal to 2, and the Ar representative contains the structure of at least one aromatic nucleus.
15. according to the heat-resistant resin of claim 12, wherein containing polyether structure is the compound shown in the formula (2) with the compound with at least two terminal amine structures:
Wherein b, c and d represent the integer more than or equal to 0 independently of one another, and condition is that b+c+d is more than or equal to 2.
16. heat-resistant resin with structural unit shown in the formula (R2):
Wherein b, c and d represent the integer more than or equal to 0 independently of one another, condition be b+c+d more than or equal to 2, and Ar representative contains the structure of at least one aromatic nucleus.
17. according to the heat-resistant resin of claim 12, wherein containing polyether structure is the compound shown in the formula (3) with the compound with at least two terminal amine structures:
Wherein e, f and g represent the integer more than or equal to 0 independently of one another, and condition is that e+f+g is more than or equal to 2.
18. heat-resistant resin with structural unit shown in the formula (R3):
Wherein e, f and g represent the integer more than or equal to 0 independently of one another, condition be e+f+g more than or equal to 2, and Ar representative contains the structure of at least one aromatic nucleus.
19. according to the heat-resistant resin of claim 12, wherein containing polyether structure is the compound shown in the formula (4) with the compound with at least two terminal amine structures:
Wherein h represents the integer more than or equal to 1.
20. heat-resistant resin with structural unit shown in the formula (R4):
Wherein h represents the integer more than or equal to 1, and the Ar representative contains the structure of at least one aromatic nucleus.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP304027/04 | 2004-10-19 | ||
| JP2004304027 | 2004-10-19 | ||
| JP297735/05 | 2005-10-12 |
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|---|---|
| CN1778830A true CN1778830A (en) | 2006-05-31 |
| CN100535031C CN100535031C (en) | 2009-09-02 |
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| CNB2005101249313A Active CN100535031C (en) | 2004-10-19 | 2005-10-19 | Cleaning substrate of substrate processing equipment and heat resistant resin preferable therefor |
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| JP (1) | JP2011153325A (en) |
| CN (1) | CN100535031C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101541888B (en) * | 2006-10-04 | 2013-01-23 | 三菱瓦斯化学株式会社 | Two-part thermocurable polyimide resin composition and cured product thereof |
| CN111498429A (en) * | 2019-01-30 | 2020-08-07 | 日东电工株式会社 | Cleaning sheet and conveying member with cleaning function |
| CN111500185A (en) * | 2019-01-30 | 2020-08-07 | 日东电工株式会社 | Cleaning sheet and conveying member with cleaning function |
| CN112852333A (en) * | 2019-11-12 | 2021-05-28 | 山太士股份有限公司 | Probe cleaning sheet and method for cleaning probe |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11130858A (en) * | 1997-10-31 | 1999-05-18 | Hitachi Chem Co Ltd | Polyimide, its precursor, their production and photosensitive resin composition |
| JP2004211053A (en) * | 2002-06-26 | 2004-07-29 | Hitachi Chem Co Ltd | Filmy adhesive, adhesive sheet, and semiconductor device |
| JP2006096825A (en) * | 2004-09-28 | 2006-04-13 | Hitachi Chem Co Ltd | Polyimide resin and heat-resistant resin composition using the same |
-
2005
- 2005-10-19 CN CNB2005101249313A patent/CN100535031C/en active Active
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2011
- 2011-05-20 JP JP2011113782A patent/JP2011153325A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101541888B (en) * | 2006-10-04 | 2013-01-23 | 三菱瓦斯化学株式会社 | Two-part thermocurable polyimide resin composition and cured product thereof |
| CN111498429A (en) * | 2019-01-30 | 2020-08-07 | 日东电工株式会社 | Cleaning sheet and conveying member with cleaning function |
| CN111500185A (en) * | 2019-01-30 | 2020-08-07 | 日东电工株式会社 | Cleaning sheet and conveying member with cleaning function |
| CN112852333A (en) * | 2019-11-12 | 2021-05-28 | 山太士股份有限公司 | Probe cleaning sheet and method for cleaning probe |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100535031C (en) | 2009-09-02 |
| JP2011153325A (en) | 2011-08-11 |
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