CN105418927B - A kind of low-dielectric constant film and preparation method thereof - Google Patents
A kind of low-dielectric constant film and preparation method thereof Download PDFInfo
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- CN105418927B CN105418927B CN201410465737.0A CN201410465737A CN105418927B CN 105418927 B CN105418927 B CN 105418927B CN 201410465737 A CN201410465737 A CN 201410465737A CN 105418927 B CN105418927 B CN 105418927B
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Abstract
The invention discloses a kind of low-dielectric constant films and preparation method thereof.The present invention is using fluorine-containing naphthylethyl organic silicon monomer and alkyl dichlorosilane as starting material, and using tetramethyl divinyl siloxanes as end-capping reagent, fluorine-containing naphthylethyl vinyl silicone oil is made by condensation reaction；The fluorine-containing naphthylethyl vinyl silicone oil and the mixing of containing hydrogen silicone oil or hydrogen-containing siloxane, are applied on silicon wafer and form thin film, make the film that hair occur using ultraviolet light and answer, then make annealing treatment to film, the low-dielectric constant film is made.The dielectric constant of low-dielectric constant film obtained is up to 2.0~2.5 in the present invention, therefore can be used as the advanced low-k materials on 45nm great scale integrated circuit below.The preparation method of the low-dielectric constant film is simple, is conducive to industrialized production.
Description
Technical field
The invention belongs to advanced low-k materials technical fields, and in particular to a kind of low-dielectric constant film and its system
Preparation Method.
Background technique
With the development of great scale integrated circuit, the integrated level of circuit is higher and higher, and the interconnection line density in chip is not
Disconnected to increase, the width and spacing of interconnection line constantly reduce, therefore the ghost effect as caused by interconnection resistance (R) and capacitor (C)
It is more and more obvious, and then makes signal that significant delays occur.To solve this problem, most efficient method is using low-k
Interconnecting material.The main number with polar molecule in the polarizability of constituent material molecule and unit volume of the dielectric constant of material
Correlation, therefore the dielectric constant of material can be reduced by two kinds of approach: first is that reducing the polarizability of constituent material molecule；Second is that
Reduce the density of polar molecule in unit volume.
Air of the industry by using boring technique by dielectric constant equal to 1 is introduced into the micropore of solid film at present,
To reduce the density of polar molecule in unit volume, the dielectric constant of solid film can be so reduced.But microporous solids
The size of film mesoporous is difficult to control, and the presence in hole is often led to that thin film mechanical performance is bad, water imbibition increases, Jin Erying
Ring film performance.
Silica material has good chemical stability and thermal stability, has good compatibility with silicon substrate, because
This is most with prospects in numerous advanced low-k materials.Industry is mostly used tetramethylsilane, dimethylformamide dimethyl oxygen at present
Base silane, the raw material as low-k deposition film such as octamethylcy-clotetrasiloxane, however as the continuous hair of integrated circuit
Exhibition, traditional organosilicon materials are no longer satisfied the market demand.
Big fluoro-containing group is introduced on silicon, can drop low molecular polarizability, increases the free volume of polymer, thus
Achieve the purpose that reduce dielectric constant.Because C-F has smaller dipole and lower polarizability compared with c h bond, while fluorine atom can also
Increase free volume, and these two aspects can reduce the dielectric constant of solid film.Bridge structure flexible and interchain phase can be limited
The big group mutually attracted can increase the free volume of polymer.The free volume of polymer increases, and can reduce unit
The number of polar groups in volume, to achieve the purpose that reduce dielectric constant.
As integrated circuit reaches 45nm with lower node, ultra-low dielectric materials of the dielectric constant k value less than 2.5 are needed, are passed
Polymer material unite often due to k value is higher, it is difficult to meet the requirements, explore new advanced low-k materials and be still important research
Direction.
Summary of the invention
The object of the present invention is to provide a kind of low-dielectric constant films and preparation method thereof, mainly solve existing
Traditional polymer material is difficult to the technical issues of ultra-low dielectric constant material needed for meeting modern integrated circuits in technology.
Used technical solution is as follows to solve above-mentioned technical problem by the present invention:
A kind of low-dielectric constant film, the preparation method of the low-dielectric constant film are as follows: with fluorine-containing naphthylethyl
Organic silicon monomer and alkyl dichlorosilane are starting material, anti-by being condensed using tetramethyl divinyl siloxanes as end-capping reagent
Fluorine-containing naphthylethyl vinyl silicone oil should be made, the fluorine-containing naphthylethyl vinyl silicone oil and containing hydrogen silicone oil or hydrogen-containing siloxane mix
It closes, is applied on silicon wafer and forms thin film, make the film that hair occur using ultraviolet light and answer, then anneal to film
Processing, is made the low-dielectric constant film；Shown in the structure such as formula (I) of the fluorine-containing naphthylethyl organic silicon monomer,
Wherein, RfFor-(CH2)m(CF2)nF or-(CH2)m(CF2)nH, wherein m be 1~2 integer, n be 1~10 it is whole
Number；R1For methyl or phenyl；R2For-H or Rf；R3For-H or Rf。
Further, the alkyl dichlorosilane is dimethyldichlorosilane, diphenyl dichlorosilane or aminomethyl phenyl two
Chlorosilane.
Further, the dielectric constant of the low-dielectric constant film is 2.0~2.5.
The preparation method of the low-dielectric constant film, includes the following steps:
Step 1, the fluorine-containing naphthylethyl organic silicon monomer and alkyl dichlorosilane are uniformly mixed, instill water and solvent
In mixed liquor, after being added dropwise, 30~80 DEG C, 1~8h of insulation reaction are heated to, solvent and water is distilled off, tetramethyl is added
Divinyl disiloxane and catalyst are heated to 60~150 DEG C, 2~8h of insulation reaction, and fluorine-containing naphthylethyl vinyl silicon is made
Oil；
Step 2, aforementioned fluorine-containing naphthylethyl vinyl silicone oil and containing hydrogen silicone oil or hydrogen-containing siloxane are added in solvent and are mixed
It closes uniformly, is applied on silicon wafer and forms thin film, the film is irradiated using ultraviolet light, brings it about reaction, then
The film is made annealing treatment, the advanced low-k materials are made.
Further, the alkyl dichlorosilane is dimethyldichlorosilane, diphenyl dichlorosilane or aminomethyl phenyl two
Chlorosilane；The catalyst is the concentrated sulfuric acid or trifluoromethanesulfonic acid；The solvent be toluene, hexane, tetrahydrofuran, ethyl acetate or
Ethyl alcohol.
Further, the content of containing hydrogen silicone oil or hydrogen-containing siloxane is 0.1%~1.6% in the step 2.
Further, the hydrogen-containing siloxane is 1,3,5,7- tetramethyl-ring tetrasiloxanes.
The condition that ultraviolet light irradiates film in the step 2 are as follows: the wavelength of the ultraviolet light is received for 240~260
Rice, power are 15~30 watts, and UV-light luminous pipe is 15~20cm at a distance from film, and the ultraviolet light irradiation time is 3~8 days.
The fluorine-containing naphthylethyl organic silicon monomer, alkyl dichlorosilane, tetramethyl divinyl disiloxane mole
Than being followed successively by 1~500:1~2000:1~10；Fluorine-containing naphthylethyl vinyl silicone oil, containing hydrogen silicone oil, solvent mass ratio be followed successively by
1~100:1~50:1~1000；Fluorine-containing naphthylethyl vinyl silicone oil, hydrogen-containing siloxane, solvent mass ratio be followed successively by 1~
100:1~50:1~1000.
The mode that film is made annealing treatment in the step 2 are as follows: film is put into nitrogen environment and is carried out at annealing
Reason, annealing temperature are 200~400 DEG C, and annealing time is 10~30 minutes.
Compared with prior art, beneficial effects of the present invention are as follows:
1, the synthetic method of low-dielectric constant film of the present invention is simple, is conducive to industrialized production.Low
In the preparation process of dielectric constant material film, the object of change fluorine-containing naphthylethyl organic silicon monomer and alkyl dichlorosilane can be passed through
The ratio of the amount of matter changes the content of fluorine-containing naphthylethyl in molecule；By change tetramethyl divinyl siloxanes dosage come
Change the size of fluorine-containing naphthylethyl vinyl silicone oil molecular weight；By the content and hydrogen-based silicone oil that adjust fluorine-containing naphthylethyl in molecule
Hydrogen content adjust the electricity and otherwise performance of low-dielectric constant film.
2, the dielectric constant of the low-dielectric constant film is up to 2.0~2.5.Due to C-F have compared with c h bond it is lesser
Dipole and lower polarizability, while fluorine atom also can increase free volume, and these two aspects can reduce Jie of solid film
Electric constant.In addition, can limit the big group that interchain attracts each other can increase the free volume of polymer, the freedom of polymer
Volume increases, and the number of polar groups in unit volume can be reduced, so as to reduce dielectric constant.Introduce big on silicon
Low molecular polarizability can drop in fluoro-containing group, increase the free volume of polymer, to reach the mesh for reducing dielectric constant
's.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail below by way of specific embodiment.
Embodiment 1
Take a 1000ml three-necked flask, be equipped with magnetic heating stirrer, thermometer, water segregator, constant pressure funnel and
Reflux condenser.200ml toluene, 30g water are successively added into flask；In addition by 73g5- (1,1,1- trifluoro propyl) naphthylethyl
Dimethyl dichlorosilane (DMCS) and 50g dimethyldichlorosilane instill in flask after mixing, after being added dropwise, are heated to 60 DEG C, protect
Temperature reaction 2h, is distilled off water and toluene, adds 1.5g tetramethyl divinyl disiloxane and the 5g concentrated sulfuric acid, be heated to
110 DEG C, insulation reaction 8h is cooled to room temperature, and 200ml toluene is added, is washed to neutrality, toluene and low-boiling-point substance is distilled off, obtain
Fluorine-containing naphthylethyl vinyl silicone oil 82.5g, yield 89.5%.
By fluorine-containing naphthylethyl vinyl silicone oil obtained above and containing hydrogen silicone oil (hydrogen content 1.2%), toluene according to quality
It is uniformly mixed than 5:1:8, is coated on low-resistance single crystal silicon substrate using spin-coating method, forms thin film on a silicon substrate, revolved
During painting, revolving speed is 350 revs/min, and rotational time is 30 seconds, then the film of the formation described in ultraviolet light, wherein
The wavelength of ultraviolet light is 255 nanometers, and power is 20 watts, and the vertical range between UV-light luminous pipe and film is 15 centimetres, purple
The irradiation time of outer light is 5 days, and resulting film is then placed in N2In environment, and carry out at 300 DEG C annealing in 20 minutes
Low-dielectric constant film, dielectric constant 2.46 is made in processing.
Embodiment 2
Take a 1000ml three-necked flask, be equipped with magnetic heating stirrer, thermometer, water segregator, constant pressure funnel and
Reflux condenser.250ml toluene, 40g water, in addition by 110g5- (1,1,1- trifluoro propyl) naphthylethyl are successively added into flask
Dimethyl dichlorosilane (DMCS) and 40g dimethyldichlorosilane instill in bottle after mixing, after being added dropwise, are heated to 60 DEG C, heat preservation
2h is reacted, water and toluene is distilled off, adds 1.2g tetramethyl divinyl disiloxane and the 8g concentrated sulfuric acid, is heated to 110
DEG C, insulation reaction 8h is cooled to room temperature, and 250ml toluene is added, is washed to neutrality, toluene and low-boiling-point substance is distilled off, obtain fluorine-containing
Naphthylethyl vinyl silicone oil 102g, yield 86.8%.
By aforementioned fluorine-containing naphthylethyl vinyl silicone oil obtained and 1,3,5,7- tetrahydro -1,3,5,7- tetramethyl cyclotetrasiloxane silicon oxygen
Alkane, toluene are uniformly mixed according to mass ratio 5:1:10, are coated on low-resistance single crystal silicon substrate using spin-coating method, on a silicon substrate
Thin film is formed, in spin coating process, revolving speed is 350 revs/min, rotational time 30 seconds, is then formed with ultraviolet light
Film, wherein the wavelength of ultraviolet light be 255 nanometers, power be 20 watts, the vertical range between UV-light luminous pipe and film
It is 15 centimetres, the irradiation time of ultraviolet light is 5 days, and resulting film is placed in N2In environment, and carried out 20 minutes at 300 DEG C
Annealing, be made low-dielectric constant film, dielectric constant 2.23.
The structural formula of 5- (1,1,1- trifluoro propyl) naphthylethyl dimethyl dichlorosilane (DMCS) in above-described embodiment 1 and embodiment 2
It is as follows:
5- (1,1,1- trifluoro propyl) the naphthylethyl dimethyl dichlorosilane (DMCS) the preparation method is as follows:
(1) a 500ml four-hole boiling flask is taken, magnetic heating stirrer, thermometer, constant pressure funnel and returned cold are equipped with
Condenser.It is passed through nitrogen into flask, is added 6g treated magnesium chips and 200ml anhydrous ether, open magnetic heating stirrer, add
0.1ml iodomethane is added to 30 DEG C in heat, then bromo- 1,1,1- trifluoro propane of 40g3- is added dropwise, after being added dropwise to complete, insulation reaction 2h,
It is cooled to room temperature, reaction solution is transferred in constant pressure funnel by syringe.A 1L four-hole boiling flask is separately taken, magnetic force is equipped with and adds
The low liquid funnel of thermal agitation device, thermometer, constant pressure and reflux condenser.Be passed through nitrogen into flask, be added 500ml anhydrous ether and
70g1,5- dibromine naphthalene open magnetic heating stirrer, the aforementioned reaction solution being transferred in constant pressure funnel are heated to 30
DEG C, it instills to anhydrous ether and 1, in the mixed liquor of 5- dibromine naphthalene, after being added dropwise to complete, insulation reaction 3h is cooled to room temperature, mistake
Filter, rectification under vacuum obtain intermediate product A45.9g.
(2) a 500ml four-hole boiling flask is taken, magnetic heating stirrer, thermometer, constant pressure funnel and returned cold are equipped with
Condenser.It is passed through nitrogen into flask, is added 4.5g treated magnesium chips and 250ml anhydrous ether, open stirring, be heated to 30
DEG C, 0.1ml iodomethane is added, then 45g intermediate product A is added dropwise, after being added dropwise to complete, insulation reaction 2h is cooled to room temperature, and will be reacted
Liquid is transferred in constant pressure funnel by syringe.
A 1L four-hole boiling flask is separately taken, magnetic heating stirrer, thermometer, the low liquid funnel of constant pressure and reflux condensation mode are equipped with
Device.It is passed through nitrogen into flask, 300ml anhydrous ether and the bromo- 2- chloroethanes of 23g1- is added, opens magnetic heating stirrer, it will
The aforementioned reaction solution being transferred in constant pressure funnel is heated to 30 DEG C, instills mixed to anhydrous ether and the bromo- 2- chloroethanes of 1-
It closes in liquid, after being added dropwise to complete, insulation reaction 3h is cooled to room temperature, and filtering, rectification under vacuum obtains intermediate product B26.6g.
(3) a 500ml four-hole boiling flask is taken, magnetic heating stirrer, thermometer, constant pressure funnel and returned cold are equipped with
Condenser.It is passed through nitrogen into flask, is added 2.5g treated magnesium chips and 200ml anhydrous ether, open magnetic heating stirrer,
30 DEG C are heated to, 0.1ml iodomethane is added, then 25g intermediate product B is added dropwise, after being added dropwise to complete, insulation reaction 2h is cooled to room
Reaction solution is transferred in constant pressure funnel by temperature by syringe.
A 1L four-hole boiling flask is separately taken, magnetic heating stirrer, thermometer, the low liquid funnel of constant pressure and reflux condensation mode are equipped with
Device.It is passed through nitrogen into flask, 200ml anhydrous ether and 15g methyl trichlorosilane is added, opens magnetic heating stirrer, it will
The aforementioned reaction solution being transferred in constant pressure funnel is heated to 30 DEG C, instills to the mixing of anhydrous ether and methyl trichlorosilane
In liquid, after being added dropwise to complete, insulation reaction 5h is cooled to room temperature, and filtering, rectification under vacuum obtains target product 5- (1,1,1- trifluoropropyl
Base) naphthylethyl dimethyl dichlorosilane (DMCS) 27.3g.5- (1,1,1- trifluoro propyl) naphthylethyl dimethyl dichlorosilane (DMCS)1H-NMR
(400MHz,CDCl3,δ/ppm):8.06(d,1H,Ar-H),7.94(d,1H,Ar-H),7.34(br,2H,2Ar-H),7.47
(br,2H,2Ar-H),3.31(t,2H,CH2),2.89(t,2H,CH2),2.28(t,2H,CH2CF3),1.44(t,2H,CH2Si),
0.59(s,2H,CH3Si).
Embodiment 3
Take a 1000ml three-necked flask, be equipped with magnetic heating stirrer, thermometer, water segregator, constant pressure funnel and
Reflux condenser.200ml toluene, 30g water are successively added into flask；In addition by 73g5- (the fluoro- 2,2- bis- fluoro- 3 of 1,1,1- tri-,
3- difluorobutyl groups) naphthylethyl diphenyl dichlorosilane and 50g diphenyl dichlorosilane instill in flask after mixing, be added dropwise
Afterwards, 60 DEG C are heated to, water and toluene is distilled off in insulation reaction 2h, add 1.5g tetramethyl divinyl disiloxane and
The 5g concentrated sulfuric acid is heated to 110 DEG C, and insulation reaction 8h is cooled to room temperature, and 200ml toluene is added, is washed to neutrality, is distilled off
Toluene and low-boiling-point substance obtain fluorine-containing naphthylethyl vinyl silicone oil 80.2g.
By fluorine-containing naphthylethyl vinyl silicone oil obtained above and containing hydrogen silicone oil (hydrogen content 1.2%), toluene according to quality
It is uniformly mixed than 5:1:8, is coated on low-resistance single crystal silicon substrate using spin-coating method, forms thin film on a silicon substrate, revolved
During painting, revolving speed is 350 revs/min, and rotational time is 30 seconds, then the film of the formation described in ultraviolet light, wherein
The wavelength of ultraviolet light is 255 nanometers, and power is 20 watts, and the vertical range between UV-light luminous pipe and film is 15 centimetres, purple
The irradiation time of outer light is 5 days, and resulting film is then placed in N2In environment, and carry out at 300 DEG C annealing in 20 minutes
Low-dielectric constant film, dielectric constant 2.35 is made in processing.
5- (the tri- fluoro- 3,3- difluorobutyl groups of fluoro- 2,2- bis- of 1,1,1-) naphthylethyl diphenyl dichlorosilane in the embodiment 3
Structural formula it is as follows:
The preparation method of 5- (the tri- fluoro- 3,3- difluorobutyl groups of fluoro- 2,2- bis- of 1,1,1-) the naphthylethyl diphenyl dichlorosilane
It is as follows:
(1) a 500ml four-hole boiling flask is taken, magnetic heating stirrer, thermometer, constant pressure funnel and returned cold are equipped with
Condenser.It is passed through nitrogen into flask, is added 6g treated magnesium chips and 200ml anhydrous ether, open magnetic heating stirrer, add
0.1ml iodomethane is added to 30 DEG C in heat, then 67.56g BrCH is added dropwise2CF2CF2CF3, after being added dropwise to complete, insulation reaction 2h is cold
But to room temperature, reaction solution is transferred in constant pressure funnel by syringe.
A 1L four-hole boiling flask is separately taken, magnetic heating stirrer, thermometer, the low liquid funnel of constant pressure and reflux condensation mode are equipped with
Device.Be passed through nitrogen into flask, 500ml anhydrous ether and 70g1,5- dibromine naphthalene be added, open magnetic heating stirrer, will before
It states the reaction solution being transferred in constant pressure funnel and is heated to 30 DEG C, instill to anhydrous ether and 1, the mixed liquor of 5- dibromine naphthalene
In, after being added dropwise to complete, insulation reaction 6h is cooled to room temperature, and filtering, rectification under vacuum obtains intermediate product D49.64g.
(2) a 500ml four-hole boiling flask is taken, magnetic heating stirrer, thermometer, constant pressure funnel and returned cold are equipped with
Condenser.It is passed through nitrogen into flask, 4.5g magnesium chips and 250ml anhydrous ether is added, opens magnetic heating stirrer, is heated to 30
DEG C, 0.1ml iodomethane is added, then 49g intermediate product D is added dropwise, after being added dropwise to complete, insulation reaction 2h is cooled to room temperature, and will be reacted
Liquid is transferred in constant pressure funnel by syringe.
A 1L four-hole boiling flask is separately taken, magnetic heating stirrer, thermometer, the low liquid funnel of constant pressure and reflux condensation mode are equipped with
Device.It is passed through nitrogen into flask, 300ml anhydrous ether and the bromo- 2- chloroethanes of 23g1- is added, opens magnetic heating stirrer, it will
The aforementioned reaction solution being transferred in constant pressure funnel is heated to 30 DEG C, instills mixed to anhydrous ether and the bromo- 2- chloroethanes of 1-
It closes in liquid, after being added dropwise to complete, insulation reaction 6h is cooled to room temperature, and filtering, rectification under vacuum obtains intermediate product E31.71g.
(3) a 500ml four-hole boiling flask is taken, magnetic heating stirrer, thermometer, constant pressure funnel and returned cold are equipped with
Condenser.It is passed through nitrogen into flask, 2.5g magnesium chips and 200ml anhydrous ether is added, opens magnetic heating stirrer, is heated to 30
DEG C, 0.1ml iodomethane is added, then 30g intermediate product E is added dropwise, after being added dropwise to complete, insulation reaction 2h is cooled to room temperature, and will be reacted
Liquid is transferred in constant pressure funnel by syringe.
A 1L four-hole boiling flask is separately taken, magnetic heating stirrer, thermometer, the low liquid funnel of constant pressure and reflux condensation mode are equipped with
Device.It is passed through nitrogen into flask, 200ml anhydrous ether and 21g phenyl trichlorosilane is added, opens magnetic heating stirrer, it will
The aforementioned reaction solution being transferred in constant pressure funnel is heated to 30 DEG C, instills to the mixing of anhydrous ether and phenyl trichlorosilane
In liquid, after being added dropwise to complete, insulation reaction 8h is cooled to room temperature, and filtering, rectification under vacuum, obtaining target product 5-, (1,1,1- tri- is fluoro-
The fluoro- 3,3- difluorobutyl groups of 2,2- bis-) naphthylethyl diphenyl dichlorosilane 31.83g.Target product1H-NMR(400MHz,CDCl3,
δ/ppm):8.07(d,1H,Ar-H),8.04(d,1H,Ar-H),7.34(br,2H,2Ar-H),7.47(br,7H,Ar-H),
3.58(t,2H,CH2),2.89(t,2H,CH2),1.44(t,2H,CH2Si).
It above are only part preferred embodiment of the invention, the present invention is not limited in the content of embodiment.For ability
For technical staff in domain, can there are various change and change in the conception range of technical solution of the present invention, made
What changes and change, within that scope of the present invention.
Claims (11)
1. a kind of low-dielectric constant film, which is characterized in that the preparation method of the low-dielectric constant film are as follows: to contain
Fluoronaphthalene ethyl organic silicon monomer and alkyl dichlorosilane are starting material, using tetramethyl divinyl siloxanes as end-capping reagent, are led to
It crosses condensation reaction and fluorine-containing naphthylethyl vinyl silicone oil is made, the fluorine-containing naphthylethyl vinyl silicone oil and hydrogen-containing siloxane mixing apply
In forming thin film on silicon wafer, so that the film is reacted using ultraviolet light, then film is made annealing treatment,
The low-dielectric constant film is made；Shown in the structure such as formula (I) of the fluorine-containing naphthylethyl organic silicon monomer,
Wherein, RfFor-(CH2)m(CF2)nF or-(CH2)m(CF2)nH, the integer that wherein m is 1~2, the integer that n is 1~10；R1For
Methyl or phenyl；R2For-H or Rf；R3For-H or Rf。
2. low-dielectric constant film as described in claim 1, it is characterised in that: the alkyl dichlorosilane is dimethyl
Dichlorosilane, diphenyl dichlorosilane or dichloromethyl phenylsilane.
3. low-dielectric constant film as described in claim 1, it is characterised in that: the hydrogen-containing siloxane is Silicon Containing Hydrogen
Oil.
4. low-dielectric constant film as described in claim 1, it is characterised in that: the low-dielectric constant film
Dielectric constant is 2.0~2.5.
5. the preparation method of the described in any item low-dielectric constant films of claim 1-4, it is characterised in that including as follows
Step:
Step 1, the fluorine-containing naphthylethyl organic silicon monomer and alkyl dichlorosilane are uniformly mixed, instill the mixing of water and solvent
In liquid, after being added dropwise, 30~80 DEG C, 1~8h of insulation reaction are heated to, solvent and water is distilled off, tetramethyl diethyl is added
Alkenyl disiloxane and catalyst are heated to 60~150 DEG C, 2~8h of insulation reaction, and fluorine-containing naphthylethyl vinyl silicone oil is made；
Step 2, aforementioned fluorine-containing naphthylethyl vinyl silicone oil and hydrogen-containing siloxane are added in solvent and are uniformly mixed, is applied on silicon wafer
Thin film is formed, the film is irradiated using ultraviolet light, reaction is brought it about, then the film is carried out at annealing
Reason, is made the advanced low-k materials.
6. the preparation method of low-dielectric constant film as claimed in claim 5, it is characterised in that: the alkyl dichloro silicon
Alkane is dimethyldichlorosilane, diphenyl dichlorosilane or dichloromethyl phenylsilane；The catalyst is the concentrated sulfuric acid or trifluoro
Methanesulfonic acid；The solvent is toluene, hexane, tetrahydrofuran, ethyl acetate or ethyl alcohol.
7. the preparation method of low-dielectric constant film as claimed in claim 5, it is characterised in that: contain in the step 2
The content of hydrogen siloxane is 0.1%~1.6%.
8. the preparation method of low-dielectric constant film as claimed in claim 5, it is characterised in that: the hydrogen-containing siloxane
It is 1,3,5,7- tetramethyl-ring tetrasiloxanes.
9. the preparation method of low-dielectric constant film as claimed in claim 5, which is characterized in that purple in the step 2
The condition that outer light irradiates film are as follows: the wavelength of the ultraviolet light is 240~260 nanometers, and power is 15~30 watts, ultraviolet
Light luminous tube is 15~20cm at a distance from film, and the ultraviolet light irradiation time is 3~8 days.
10. the preparation method of low-dielectric constant film as claimed in claim 5, it is characterised in that: described contains fluoronaphthalene
Ethyl organic silicon monomer, alkyl dichlorosilane, tetramethyl divinyl disiloxane molar ratio be followed successively by 1~500:1~
2000:1~10；Fluorine-containing naphthylethyl vinyl silicone oil, hydrogen-containing siloxane, solvent mass ratio be followed successively by 1~100:1~50:1~
1000。
11. the preparation method of low-dielectric constant film as claimed in claim 5, which is characterized in that right in the step 2
The mode that film is made annealing treatment are as follows: film is put into nitrogen environment and is made annealing treatment, annealing temperature be 200~
400 DEG C, annealing time is 10~30 minutes.
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