CN1754930A - Coating fluid for forming silicon dioxide capsule - Google Patents
Coating fluid for forming silicon dioxide capsule Download PDFInfo
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- CN1754930A CN1754930A CN 200510086052 CN200510086052A CN1754930A CN 1754930 A CN1754930 A CN 1754930A CN 200510086052 CN200510086052 CN 200510086052 CN 200510086052 A CN200510086052 A CN 200510086052A CN 1754930 A CN1754930 A CN 1754930A
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- silane
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Abstract
The invention provides a coating fluid which is used for forming a silicon dioxide envelope, wherein, the coating fluid contains siloxane polymer and solvent which contains n-butyl alcohol and 3- methoxyl methyl propionate. Therefore, the coating fluid used for forming the silicon dioxide envelope which can bury a tiny clearance without interruption can be obtained.
Description
Technical field
The present invention relates to a kind of silica-based film formation coating fluid.
Background technology
All the time, as the planarization film or the interlayer dielectric that use in the substrate of semiconductor element or liquid crystal cell is made, normally used is the silica-based film that adopts SOG (spin on glass) manufactured.In the method, will in solvent, make it that hydrolysis reaction take place and obtain coating fluid by the dissolvane TMOS, afterwards this coating fluid will be coated on the base material, carry out heat treated again, form silica-based film thus.
About form the coating fluid (silica-based film forms and uses coating fluid) that uses in the method for silica-based film by this SOG method, various proposals (for example, following patent documentation 1,2,3) are arranged.
In recent years, in the field of semiconductor element or liquid crystal cell, requirement such as, high speed highly integrated, multifunction in order to respond, the miniaturization that is formed at the pattern on the substrate has obtained fast development.For this reason, in planarization film or interlayer dielectric, require no gap to bury narrower space (space), but the formation of silica-based film in the past is difficult to satisfy this requirement with coating fluid (void).
Patent documentation 1: the spy opens the 2001-131479 communique
Patent documentation 2: the spy opens the 2001-115029 communique
Patent documentation 3: the spy opens the 2004-96076 communique
Summary of the invention
The present invention is exactly the invention of finishing in order to address the above problem, and its purpose is to provide a kind of silica-based film that can seamlessly bury slight void to form and uses coating fluid.
In order to achieve the above object, silica-based film of the present invention forms with containing siloxane polymer and solvent in the coating fluid, it is characterized in that above-mentioned solvent contains propyl carbinol and 3-methoxypropionic acid methyl esters.
By the present invention, it is outstanding and can seamlessly bury slight void and the silica-based film that forms silica-based film forms and uses coating fluid to obtain burial.
Embodiment
The siloxane polymer that contains in silica-based film of the present invention forms with coating fluid can suitably use as the formation material of the silica-based film by the making of SOG method and material known.The reaction product that at least a kind of material that preferred use is selected from the silane compound with following general formula (I) expression generates behind hydrolysis reaction.
R
4-nSi(OR’)
n …(I)
In general formula (I), R represents hydrogen atom, alkyl or phenyl, and R ' represents alkyl or phenyl, and n represents 2～4 integer.When being combined with a plurality of R on Si, these a plurality of R can be identical, also can be different.In addition, base can be identical for bonded a plurality of (OR ') on Si, also can be different.
As the alkyl of R, preferred carbonatoms is 1～20 a straight chain shape or a catenate alkyl, and more preferably carbonatoms is 1～4 a straight chain shape or a catenate alkyl.
As the alkyl of R ', preferred carbonatoms is 1～5 a straight chain shape or a catenate alkyl.As the alkyl of R ', from the viewpoint of hydrolysis rate, particularly preferred carbonatoms is 1 or 2.
In the reaction product that obtains making above-mentioned silane compound generation hydrolysis reaction, can contain low-molecular-weight hydrolyzate and intermolecular generation dehydration condensation and the condenses (siloxane oligomer) that generates in the reaction that is hydrolyzed.When containing this hydrolyzate or condenses, the siloxane polymer among the present invention refers to comprise these whole siloxane polymer.
The weight-average molecular weight (Mw) of the siloxane polymer that contains in silica-based film of the present invention forms with coating fluid (adopts the polystyrene conversion benchmark of gel permeation chromatography, below identical) be preferably 1000～3000, preferred scope is 1200～2700, and further preferred range is 1500～2000.Mw by making this siloxane polymer can obtain good film and form ability more than the lower limit of above-mentioned scope, by making it below the higher limit of above-mentioned scope, can obtain good burial and flatness.
N in the above-mentioned general formula (I) is 4 o'clock the available following general formula of silane compound (i) (II) expression.
Si(OR
1)
a(OR
2)
b(OR
3)
c(OR
4)
d …(II)
In the formula, R
1, R
2, R
3And R
4Represent the alkyl or phenyl identical respectively independently with above-mentioned R '.
A, b, c and d are the integer of the condition of satisfied 0≤a≤4,0≤b≤4,0≤c≤4,0≤d≤4 and a+b+c+d=4.
N in the general formula (I) is the (ii) available following general formula of 3 o'clock silane compound (III) expression.
R
5Si(OR
6)
e(OR
7)
f(OR
8)g …(III)
In the formula, R
5Expression hydrogen atom, the alkyl or phenyl identical with above-mentioned R.R
6, R
7And R
8Represent the alkyl or phenyl identical independently of each other with R '.
E, f and g are for satisfying 0≤e≤3,0≤f≤3,0≤g≤and the integer of the condition of e+f+g=3.
N in the general formula (I) is the (iii) available following general formula of 2 o'clock silane compound (IV) expression.
R
9R
10Si(OR
11)
h(OR
12)
i …(IV)
In the formula, R
9And R
10Expression hydrogen atom, the alkyl or phenyl identical with above-mentioned R.R
11And R
12Represent the alkyl or phenyl identical independently of each other with R '.
H and i are the integer of the condition of satisfied 0≤h≤2,0≤i≤2 and h+i=2.
Concrete example as silane compound (i), can enumerate tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane, four butoxy silanes, four pentyloxy silane, tetraphenoxy-silicane alkane, trimethoxy one Ethoxysilane, the dimethoxy diethoxy silane, triethoxy one methoxy silane, trimethoxy one propoxy-silane, one methoxyl group, three butoxy silanes, one methoxyl group, three pentyloxy silane, one methoxyl group triple phenoxyl silane, dimethoxy dipropoxy silane, tripropoxy one methoxy silane, trimethoxy one butoxy silane, dimethoxy dibutoxy silane, triethoxy one propoxy-silane, diethoxy dipropoxy silane, three butoxy, one propoxy-silane, dimethoxy one oxyethyl group one butoxy silane, diethoxy one methoxyl group one butoxy silane, diethoxy one propoxy-one butoxy silane, dipropoxy one methoxyl group one Ethoxysilane, dipropoxy one methoxyl group one butoxy silane, dipropoxy one oxyethyl group one butoxy silane, dibutoxy one methoxyl group one Ethoxysilane, dibutoxy one oxyethyl group one propoxy-silane, tetraalkoxysilanes such as one methoxyl group, one oxyethyl group, one propoxy-, one butoxy silane, wherein preferred tetramethoxy-silicane, tetraethoxysilane.
As silane compound concrete example (ii), can enumerate Trimethoxy silane, triethoxyl silane, tripropoxy silane, three pentyloxy silane, triple phenoxyl silane, dimethoxy one Ethoxysilane, diethoxy one methoxy silane, dipropoxy one methoxy silane, dipropoxy one Ethoxysilane, two pentyloxys, one methoxy silane, two pentyloxys, one Ethoxysilane, two pentyloxys, one propoxy-silane, two phenoxy groups, one methoxy silane, two phenoxy groups, one Ethoxysilane, two phenoxy groups, one propoxy-silane, methoxy ethoxy propoxy-silane, one propoxy-dimethoxy silane, one propoxy-diethoxy silane, one butoxy dimethoxy silane, one pentyloxy diethoxy silane, one phenoxy group diethoxy silane, methyltrimethoxy silane, Union carbide A-162, methyl tripropoxy silane, methyl three pentyloxy silane, ethyl trimethoxy silane, ethyl tripropoxy silane, ethyl three pentyloxy silane, ethyl triple phenoxyl silane, propyl trimethoxy silicane, propyl-triethoxysilicane, propyl group three pentyloxy silane, propyl group triple phenoxyl silane, butyl trimethoxy silane, the butyl triethoxyl silane, butyl tripropoxy silane, butyl three pentyloxy silane, butyl triple phenoxyl silane, methyl one methoxyl group diethoxy silane, ethyl one methoxyl group diethoxy silane, propyl group one methoxyl group diethoxy silane, butyl one methoxyl group diethoxy silane, methyl one methoxyl group dipropoxy silane, methyl one methoxyl group diamyl TMOS, methyl one methoxyl group hexichol TMOS, ethyl one methoxyl group dipropoxy silane, ethyl one methoxyl group diamyl TMOS, ethyl one methoxyl group hexichol TMOS, propyl group one methoxyl group dipropoxy silane, propyl group one methoxyl group diamyl TMOS, propyl group one methoxyl group hexichol TMOS, butyl one methoxyl group dipropoxy silane, butyl one methoxyl group diamyl TMOS, butyl one methoxyl group hexichol TMOS, methyl methoxy base oxethyl propoxy-silane, propyl group methoxy ethoxy propoxy-silane, butyl methoxy ethoxy propoxy-silane, methyl one methoxyl group one oxyethyl group one butoxy silane, ethyl one methoxyl group one oxyethyl group one butoxy silane, propyl group one methoxyl group one oxyethyl group one butoxy silane, butyl one methoxyl group one oxyethyl group one butoxy silane etc., wherein preferred Trimethoxy silane, triethoxyl silane, methyltrimethoxy silane.
As silane compound concrete example (iii), can enumerate dimethoxy silane, diethoxy silane, dipropoxy silane, the diamyl TMOS, the hexichol TMOS, methoxy ethoxy silane, methoxy propoxy silane, methoxyl group pentyloxy silane, the anisole TMOS, the ethoxy-c TMOS, oxyethyl group pentyloxy silane, the phenoxy ethoxy base silane, methyl dimethoxysilane, methyl methoxy base oxethyl silane, methyldiethoxysilane, methyl methoxy base propoxy-silane, methyl methoxy base pentyloxy silane, methyl methoxy phenoxyl silane, ethyl dipropoxy silane, ethyl methoxy propoxy silane, ethyl diamyl TMOS, ethyl hexichol TMOS, propyl group dimethoxy silane, propyl group methoxy ethoxy silane, propyl group ethoxy-c TMOS, the propyl group diethoxy silane, propyl group diamyl TMOS, propyl group hexichol TMOS, butyl dimethoxy silane, butyl methoxy ethoxy silane, the butyl diethoxy silane, butyl ethoxy-c TMOS, butyl dipropoxy silane, butyl methyl diamyl TMOS, butyl methyl hexichol TMOS, dimethyldimethoxysil,ne, dimethyl methoxy base oxethyl silane, dimethyldiethoxysilane, dimethyl diamyl TMOS, dimethyldiphenyloxysilane, dimethyl ethoxy-c TMOS, dimethyl dipropoxy silane, diethyl dimethoxy silane, diethyl methoxy propoxy silane, the diethyl diethoxy silane, diethyl ethoxy-c TMOS, dipropyl dimethoxy silane, the dipropyl diethoxy silane, dipropyl diamyl TMOS, dipropyl hexichol TMOS, dibutyl dimethoxy silane, the dibutyl diethoxy silane, dibutyl dipropoxy silane, dibutyl methoxyl group pentyloxy silane, dibutyl anisole pentyloxy silane, methylethyl dimethoxy silane, the methylethyl diethoxy silane, methylethyl dipropoxy silane, methylethyl diamyl TMOS, methylethyl hexichol TMOS, methyl-propyl dimethoxy silane, the methyl-propyl diethoxy silane, methyl butyl dimethoxy silane, the methyl butyl diethoxy silane, methyl butyl dipropoxy silane, methylethyl ethoxy-c TMOS, ethyl propyl dimethoxy silane, ethyl propyl methoxy ethoxy silane, dipropyl dimethoxy silane, dipropyl methoxy ethoxy silane, propyl group butyl dimethoxy silane, propyl group butyl diethoxy silane, dibutyl methoxy ethoxy silane, dibutyl methoxy propoxy silane, dibutyl ethoxy-c TMOS etc., wherein preferred dimethoxy silane, diethoxy silane, methyl dimethoxysilane, methyldiethoxysilane.
Be used to obtain the silane compound of above-mentioned reaction product, can from above-mentioned silane compound (i)～(iii), suitably select.
Preferred combination is silane compound (i) and silane compound combination (ii).When using silane compound (i) and silane compound (ii), their usage ratio be preferably silane compound (i) in the scope of 5～90 moles of %, silane compound is (ii) in the scope of 95～10 moles of %; More preferably silane compound (i) in the scope of 10～80 moles of %, silane compound is (ii) in the scope of 90～20 moles of %; More preferably silane compound (i) in the scope of 15～75 moles of %, silane compound is (ii) in the scope of 85～25 moles of %.In addition, the R in the (ii) more preferably above-mentioned general formula of silane compound (III)
5Be alkyl or phenyl, the compound of alkyl preferably.
Above-mentioned reaction product can be by method modulation as follows, promptly under the condition that acid catalyst, water, organic solvent exist, make from central compound generation hydrolysis, the condensation reaction of selecting more than a kind of above-mentioned silane compound (i)～(iii), thereby modulate.
Can use in the middle of organic acid, the mineral acid any as above-mentioned acid catalyst.
As mineral acid, can use sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid etc., wherein preferably phosphoric acid, nitric acid.
As above-mentioned organic acid, the organic acid that can use carboxylic acids such as formic acid, oxalic acid, fumaric acid, toxilic acid, Glacial acetic acid, diacetyl oxide, propionic acid, butanic acid and have the sulfur acid residue.
As organic acid with above-mentioned sulfur acid residue, can enumerate organic sulfonic acid, as these carboxylates, can enumerate organo-sulfate, organic sulfite etc.Wherein, preferred especially organic sulfonic acid, for example compound of representing with following logical formula V.
R
13-X …(V)
(in the formula, R
13Be to have substituent alkyl, X is a sulfonic group)
In above-mentioned logical formula V, as R
13Alkyl, preferred carbonatoms is 1～20 alkyl, this alkyl can be saturated alkyl, also can be unsaturated alkyl, can be in the middle of straight chain shape, a chain, the ring-type any.
As alkyl R
13During for cyclic group, for example can be aromatic hydrocarbyls such as phenyl, naphthyl, anthryl, wherein preferred phenyl.On the aromatic nucleus in this aromatic hydrocarbyl, can be combined with one or more carbonatomss as substituting group is 1～20 alkyl.As the substituent alkyl on this aromatic nucleus can be saturated hydrocarbyl, also can be unsaturated alkyl, can be in the middle of straight chain shape, a chain, the ring-type any.
In addition, alkyl R
13Can have one or more substituting groups,, can be exemplified as halogen atom, sulfonic group, carboxyl, hydroxyl, amino, cyano group etc. such as fluorine atom as this substituting group.
As organic sulfonic acid, improve the viewpoint of effect, preferred especially nine fluorine butane sulfonic acid, methanesulfonic, trifluoromethayl sulfonic acid, Witco 1298 Soft Acid or their mixture etc. from the shape of corrosion-resisting pattern bottom with above-mentioned general formula (V) expression.
Above-mentioned acid catalyst can play the use of the catalyzer when making the silane compound hydrolysis under the situation that has water to exist, the amount of employed acid catalyst can be modulated into as follows, that is, the concentration in the reaction system of hydrolysis reaction is in 1～1000ppm, scope particularly preferably in 5～800ppm.
About the addition of water, owing to therefore the percent hydrolysis of siloxane polymer can change, so can determine according to needed percent hydrolysis.
The percent hydrolysis of the siloxane polymer in this specification sheets is meant in quantity existence, water molecules (mole number) of the reaction system of the hydrolysis reaction that is used for synthetic this siloxane polymer ratio (unit: %) of the quantity (mole number) of the alkoxyl group in the silane compound relatively.
In the present invention, the percent hydrolysis of siloxane polymer is preferably 50～200%, and preferred scope is 75～180%.By making this percent hydrolysis more than the lower value of above-mentioned scope, can stablize the well membranous of acquisition silica-based film.Below the higher limit that is above-mentioned scope, can improve silica-based film and form the storage stability of using coating fluid.
As the organic solvent in the reaction system of hydrolysis reaction, can be exemplified as methyl alcohol, ethanol, propyl alcohol, monohydroxy-alcohols such as propyl carbinol, 3-methoxypropionic acid methyl esters, alkyl carboxylates such as 3-ethoxyl ethyl propionate, ethylene glycol, glycol ether, propylene glycol, glycerine, TriMethylolPropane(TMP), polyvalent alcohols such as hexanetriol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, the diglycol monotertiary propyl ether, diethylene glycol monobutyl ether, propylene glycol monomethyl ether, dihydroxypropane single-ether, propylene glycol monopropyl ether, the monoether class of polyvalent alcohols such as propylene glycol monobutyl ether or their monoacetate class, ritalin, vinyl acetic monomer, ester classes such as N-BUTYL ACETATE, acetone, methylethylketone, ketones such as methyl isoamyl ketone; Hydroxyl groups such as glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol bisthioglycolate propyl ether, ethylene glycol dibutyl ether, Propylene Glycol Dimethyl Ether, propylene glycol diethyl ether, diglyme, diethyl carbitol, glycol ether methyl ethyl ether are entirely by polyvalent alcohol ethers of alkyl etherificate etc.
Above-mentioned organic solvent can use separately, can make up more than 2 kinds and use.
Silica-based film of the present invention forms with in the coating fluid, contain propyl carbinol and 3-methoxypropionic acid methyl esters as the neccessary composition in the solvent, so, preferably use the mixed solvent of propyl carbinol and 3-methoxypropionic acid methyl esters as the organic solvent in the reaction system of synthetic siloxane polymer.
When using the mixed solvent of propyl carbinol and 3-methoxypropionic acid methyl esters, preferably in 20/80～80/20 scope, preferred scope is 30/70～70/30 to their mass ratio (propyl carbinol/3-methoxypropionic acid methyl esters).
Mass ratio by making propyl carbinol and 3-methoxypropionic acid methyl esters is in above-mentioned scope, depression in the time of can suppressing to be coated with is improved coating and improves the effect that the ageing stability of the effect of burial, effect that the organic gas amount that produces reduces and coating fluid is improved when forming silica-based film.Special in the amount that makes propyl carbinol when the lower value of above-mentioned scope is above, be not prone to bad situations such as depression in the coating process.In addition, the amount by making 3-methoxypropionic acid methyl esters can be improved the storage stability of coating fluid more than the lower value of above-mentioned scope.
By the reaction that in such reaction system, is hydrolyzed, can obtain siloxane polymer.Finish this hydrolysis reaction and need about 5～100 hours usually,, be preferably in the temperature range that is no more than 80 ℃ and heat if will shorten the reaction times.
After reaction finishes, can obtain containing synthetic siloxane polymer and the reaction soln of the organic solvent that is used to react.This reaction soln can be directly forms as silica-based film use coating fluid, but in order to be adjusted to the ideal solid component concentration, preferably will further add diluting solvent and the liquid that carried out dilution as silica-based film formation coating fluid.
Silica-based film of the present invention is formed the SiO that uses coating fluid
2Conversion concentration is not particularly limited, but is preferably about 1～30 quality %, more preferably about 5～25 quality %.
As above-mentioned diluting solvent, preferably use as suitably selecting in the cited solvent of the organic solvent the hydrolysis reaction, but common organic solvent in addition also can use from above-mentioned.
Preferred diluting solvent is the mixed solvent of above-mentioned propyl carbinol and 3-methoxypropionic acid methyl esters.
In silica-based film forms with the solvent in the coating fluid, in the scope of not damaging effect of the present invention, can contain the solvent except that propyl carbinol and 3-methoxypropionic acid methyl esters, but the total content of propyl carbinol and 3-methoxypropionic acid methyl esters preferably accounts for silica-based film and forms more than the 50 quality % that use the solvent in the coating fluid, more preferably more than the 80 quality %, more preferably more than 98%, most preferably be 100 quality %.
Form with in the coating fluid at the silica-based film that contains above-mentioned reaction soln, contain the alcohol that the hydrolysis reaction by silane compound generates, under the excessive situation of sneaking into of alcohol, remove alcohol by underpressure distillation and get final product.It is 39.9 * 10 that underpressure distillation is preferably in vacuum tightness
2～39.9 * 10
3Pa, preferred 66.5 * 10
2～26.6 * 10
3Pa and temperature are to carry out 2～6 hours under 20 ℃～50 ℃ the condition.
Silica-based film of the present invention forms with coating fluid and is preferred for forming silica-based film as planarization film or interlayer dielectric.As using silica-based film of the present invention to form the method that forms silica-based film with coating fluid, can use common SOG method.
For example, at first forms the regulation thickness for silica-based film is formed with coating fluid on matrix, coating processes such as employing rotary coating, curtain coating coating, roll coating are coated with and form and film.The thickness of filming can suitably be selected according to the matrix kind of using.
Then, on hot plate, cure.The stoving temperature of this moment for example is about 80～500 ℃, more preferably about 80～300 ℃.It is 10～360 seconds that common this cures the required time, is preferably 90～210 seconds.Curing processing can divide a plurality of stages to carry out under the condition that changes stoving temperature.
Subsequently, burn till by high temperature and can obtain silica-based film.Firing temperature more than 350 ℃, is preferably about 350～450 ℃ usually.
Silica-based film of the present invention forms concavo-convex space can seamlessly burying matrix surface with coating fluid, and its burial is outstanding, can form the silica-based film that fine is used as planarization film or interlayer dielectric.
For example as described later shown in the embodiment, can realize seamlessly to bury the L﹠amp that width is 0.1 μ m; The outstanding burial of S pattern (1: 1).
[embodiment 1]
Mixed methyl Trimethoxy silane 367.7g (2.7 moles), tetramethoxy-silicane 411.0g (2.7 moles), propyl carbinol 690.5g, 3-methoxypropionic acid methyl esters 690.5g, and stir.Then, add water 340.2g (19.0 moles), concentration is the nitric acid 58.9 μ l of 60 quality %, and then stir and made it that hydrolysis reaction takes place in 3 hours.Percent hydrolysis is about 100%.
Subsequently, by under 26 ℃, making its reaction 2 days, obtain containing the reaction soln of siloxane polymer.The weight-average molecular weight of the siloxane polymer in the reaction soln (Mw) is 1559.
In the above-mentioned reaction soln of 2415.2g, mix propyl carbinol 388.8g and 3-methoxypropionic acid methyl esters 388.8g, obtain silica-based film formation coating fluid as diluting solvent.
(evaluation of burial)
Preparation is formed with the 1:1L﹠amp of 0.1 μ m on Silicon Wafer; The matrix of S pattern.
Adopt spin-coating method on this matrix, to be coated on the silica-based film that obtains in above-mentioned and form and use coating fluid, cure processing with hot plate.Cure heating condition in the processing and be cure under 80 ℃ 1 minute, then cure under 150 ℃ 1 minute, then under 200 ℃, cured 1 minute, carry out the multistage and cure.Subsequently, in air, burn till under 400 ℃ and obtain silica-based film.
For the silica-based film that obtains, adopt SEM (scanning electron microscope) to observe the cross section, found that not produce the gap in the space between pattern that also do not bury badly, burial is good.
(embodiment 2)
In the foregoing description 1, change percent hydrolysis, be modulated into silica-based film formation coating fluid.
That is, mixed methyl Trimethoxy silane 176.8g (1.3 moles), tetramethoxy-silicane 197.6g (1.3 moles), propyl carbinol 249.0g, 3-methoxypropionic acid methyl esters 249.0g, and stir.Then, add water 327.6g (18.3 moles), concentration is the nitric acid 28.3 μ l of 60 quality %, and then stir and made it that hydrolysis reaction takes place in 3 hours.Percent hydrolysis is about 200%.
Subsequently, by under 26 ℃, making its reaction 2 days, obtain containing the reaction soln of siloxane polymer.The weight-average molecular weight of the siloxane polymer in the reaction soln (Mw) is 1741.
In the above-mentioned reaction soln of 150g, mix propyl carbinol 24.8g and 3-methoxypropionic acid methyl esters 24.8g, obtain silica-based film formation coating fluid as diluting solvent.
Use coating fluid for the silica-based film formation that obtains, carried out the burial evaluation in the same manner with embodiment 1.The result does not produce the gap in the space between pattern, does not bury badly yet, and burial is good.
(comparative example 1)
In embodiment 2, do not use propyl carbinol and 3-methoxypropionic acid methyl esters, but use 690.5g acetone and Virahol (IPA) respectively, modulated silica-based film formation coating fluid.
Percent hydrolysis in the hydrolysis reaction is about 200%.The weight-average molecular weight of the siloxane polymer in the reaction soln (Mw) is 1956.
Use coating fluid for the silica-based film formation that obtains, carry out the burial evaluation in the same manner with embodiment 1.The result observes in the space between pattern and has produced little clearance, and the burial in fine pattern is relatively poor.
Claims (5)
1. a silica-based film forms and uses coating fluid, wherein contains siloxane polymer and solvent, it is characterized in that,
Contain propyl carbinol and 3-methoxypropionic acid methyl esters in the described solvent.
2, silica-based film as claimed in claim 1 forms and uses coating fluid, it is characterized in that the mass ratio of described propyl carbinol and 3 one methoxypropionic acid methyl esters is 20/80～80/20.
3, silica-based film as claimed in claim 1 forms and uses coating fluid, it is characterized in that, described silane compound is to make at least a kind of compound generation hydrolysis reaction selecting and the reaction product that obtains from the silane compound with following general formula (I) expression,
R
4-nSi(OR’)
n …(I)
In the formula, R represents hydrogen atom, alkyl or phenyl independently, and R ' represents alkyl or phenyl independently, and n represents 2～4 integer.
4, silica-based film as claimed in claim 1 forms and uses coating fluid, it is characterized in that,
The weight-average molecular weight of described siloxane polymer is 1000～3000.
5, use coating fluid as any described silica-based film formation in the claim 1～4, it is characterized in that,
The percent hydrolysis of described siloxane polymer is 50～200%.
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| JP2004282069 | 2004-09-28 | ||
| JP2004282069A JP4611701B2 (en) | 2004-09-28 | 2004-09-28 | Silica-based coating solution |
| JP2004-282069 | 2004-09-28 |
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| CN1754930A true CN1754930A (en) | 2006-04-05 |
| CN100432173C CN100432173C (en) | 2008-11-12 |
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| CN102163721B (en) * | 2006-12-15 | 2013-03-27 | 东京应化工业株式会社 | Negative electrode base member |
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| JP3631236B2 (en) * | 2002-07-12 | 2005-03-23 | 東京応化工業株式会社 | Method for producing silica-based organic coating |
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2004
- 2004-09-28 JP JP2004282069A patent/JP4611701B2/en active Active
-
2005
- 2005-06-27 TW TW94121483A patent/TWI295309B/en active
- 2005-07-19 CN CNB2005100860526A patent/CN100432173C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102163721B (en) * | 2006-12-15 | 2013-03-27 | 东京应化工业株式会社 | Negative electrode base member |
| US8551651B2 (en) | 2006-12-15 | 2013-10-08 | Tokyo Ohka Kogyo Co., Ltd. | Secondary cell having negative electrode base member |
| US8927147B2 (en) | 2006-12-15 | 2015-01-06 | Kanto Gakuin School Corporation | Negative electrode base member |
| US9105929B2 (en) | 2006-12-15 | 2015-08-11 | Tokyo Ohka Kogyo Co., Ltd. | Negative electrode base member |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2006096813A (en) | 2006-04-13 |
| TW200610787A (en) | 2006-04-01 |
| CN100432173C (en) | 2008-11-12 |
| TWI295309B (en) | 2008-04-01 |
| JP4611701B2 (en) | 2011-01-12 |
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