CN106283092B - A kind of preparation method of no amino fluoride salt electric substrate cleaning combination - Google Patents
A kind of preparation method of no amino fluoride salt electric substrate cleaning combination Download PDFInfo
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- CN106283092B CN106283092B CN201610636288.0A CN201610636288A CN106283092B CN 106283092 B CN106283092 B CN 106283092B CN 201610636288 A CN201610636288 A CN 201610636288A CN 106283092 B CN106283092 B CN 106283092B
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- electric substrate
- phase detergent
- substrate cleaning
- fluoride salt
- cleaning combination
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/14—Other polishing compositions based on non-waxy substances
- C09G1/16—Other polishing compositions based on non-waxy substances on natural or synthetic resins
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The present invention relates to a kind of preparation methods of no amino fluoride salt electric substrate cleaning combination, belong to electric substrate cleaning technique field.The alkaline matter of ammonia is also easy to produce in cleaning process for the problem that containing in alkaline cleaner, can dissolve by generating the form of complex compound or corrode metal, the present invention provides a kind of preparation methods of no amino fluoride salt electric substrate cleaning combination.The present invention is with sodium cellulose glycolate, dodecyl sodium sulfate, nano silicon dioxide prepares porous silica for raw material, and the metal-chelator that poly- propionamide is prepared with sulfanilamide (SN) is covered on its surface, solid phase detergent is made, it with liquid phase detergent prepared by polyacrylamide, hydrogen peroxide and tetralkyl ammonium fluorides is mixed again, is made without amino fluoride salt electric substrate cleaning combination.The present invention covers copper electric substrate surface impurity, and be abrasive material with solid phase detergent after dissolving machinery planarization by liquid phase detergent, polishes substrate surface, while chelate the metal ion of dissolving.
Description
Technical field
The present invention relates to a kind of preparation methods of no amino fluoride salt electric substrate cleaning combination, and it is clear to belong to electric substrate
Wash technical field.
Background technology
As IC chip is to micromation, densification, high speed, highly reliableization and highly integrated development, chip
Characteristic size is less and less, and the copper interconnecting line number of plies is higher and higher.It will in order to meet photoetching in integrated circuit copper interconnecting preparation process
The overall situation and Localised nanoscopic flatness asked, every layer must planarize.And chemical-mechanical planarization be it is currently the only can be real
The method of existing global and local planarization is that integrated circuit prepares one of key process technology.Wherein, barrier layer is put down for copper-connection
The final step of smoothization directly determines device reliability and chip yield and yields, and is related to a variety of physico-chemical properties not
Same nano-level thin-membrane material is carried out at the same time in same plane, this needs multiple material rate selectivities excellent, causes to planarize
Difficulty is maximum, and benzotriazole is to inhibit copper interface and the corrosion of surface non-homogenized the most frequently used in Chemical Mechanical Polishing (CMP)
Reagent.Benzotriazole is chemically reacted with copper surface in the process, generates 1 layer of very thin film, and the copper for protecting recess is thin
Film is not gone
It removes, improves planarization efficiency.Benzotriazole is toxic, and not environmentally, temperature is 400 DEG C big in heat treatment process
When, benzotriazole is volatile, generates hole, copper ion is caused to influence copper interconnection reliability to Medium Diffusion（Electromigration, leakage
Electric current, through when dielectric breakdown）, and complicated component, cleaning cost is higher, so oneself warp becomes throwing to the removal of benzotriazole
The problem cleaned after light.
At present, cleaning agent is acidic cleaner after the machinery planarization of international mainstream, and insufficient place is needed strong
The contaminations such as particle, organic matter, metal ion could be removed under mechanism, and will appear the non-equal of surface interface after cleaning
Corrosion is homogenized, acidic cleaning solution has not adapted to the development of integrated circuit, and the research and development and application of alkaline cleaning fluid become a weight
Research direction is wanted, and can be complicated in alkaline cleaner containing the alkaline matter that ammonia is also easy to produce in cleaning process by generating
The form of object is closed to dissolve or corrode metal, therefore, research of the electric substrate detergent without ammonification is particularly important.
Invention content
The technical problems to be solved by the invention：For containing the alkali that is also easy to produce in cleaning process ammonia in alkaline cleaner
Property substance, can be by generating the form of complex compound to dissolve or corrode metal the problem of, the present invention provides a kind of no ammonia
The preparation method of fluoride salt electric substrate cleaning combination.The present invention is received with sodium cellulose glycolate, dodecyl sodium sulfate
Rice silica prepares porous silica for raw material, and the metal-chelating that poly- propionamide is prepared with sulfanilamide (SN) is covered on its surface
Agent is made solid phase detergent, then its liquid phase detergent prepared with polyacrylamide, hydrogen peroxide and tetralkyl ammonium fluorides is mixed
It closes, is made without amino fluoride salt electric substrate cleaning combination.The present invention is covered after dissolving machinery planarization by liquid phase detergent
Copper electric substrate surface impurity, and be abrasive material with solid phase detergent, polishing covers copper electric substrate surface, while chelate the gold of dissolving
Belong to ion.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）4 ~ 6g sodium cellulose glycolates, 4 ~ 6g dodecyl sodium sulfates are weighed respectively, and 5 ~ 10g nano silicon dioxides add
Enter in 600 ~ 800mL deionized waters, be placed in 15 ~ 20min of ultrasonic disperse in 300W ultrasonic disperse machines, be configured to suspension, it will be outstanding
Turbid is put into 60 ~ ﹣ of ﹣, 50 DEG C of vacuum drying chambers, vacuum degree is evacuated to as 1 ~ 10Pa, after being freeze-dried 20 ~ 30h, by desciccate
It is fitted into resistance furnace and calcines, be warming up to 1000 ~ 1200 DEG C with 5 ~ 10 DEG C/min, keep 3 ~ 4h of temperature, cooled to room temperature takes
Go out, obtain porous silica, it is spare；
（2）7 ~ 8g polyacrylamides are weighed, are added in 500 ~ 600mL deionized waters, are stirred with 300 ~ 400r/min to poly-
Acrylamide is completely dissolved, and with mass fraction be 10% methylamine water solution adjust pH value of solution be 8 ~ 11, continue stirring 20 ~
30min is heated to 60 ~ 70 DEG C, adds in 17 ~ 18g sulfanilamide (SN), keeps 3 ~ 4h of thermotonus, obtains metal-chelator；
（3）Weigh 1 ~ 2g above-mentioned steps（1）The porous silica of preparation is added in the above-mentioned metal-chelators of 10 ~ 12mL,
15 ~ 20min is stirred with 200 ~ 300r/min, is transferred in Rotary Evaporators, is evaporated to former mixeding liquid volume 40 ~ 50%, is packed into
It is dried in 105 ~ 110 DEG C of drying boxes to constant weight, obtains solid phase detergent；
（4）1 ~ 2g polyacrylamides are weighed, it is 10% hydrogen peroxide to add in 20 ~ 30mL mass fractions, is stirred with 200 ~ 300r/min
It mixes to polyacrylamide and is completely dissolved, add in 0.5 ~ 1.0g tetralkyl ammonium fluorides, continue 1 ~ 2h of stirring, obtain liquid phase detergent, by 1
~ 2g above-mentioned solid phases detergent is uniformly mixed with liquid phase detergent, is added in 70 ~ 80mL deionized waters, and is 10% with mass fraction
It is 7 ~ 10 that methylamine water solution, which adjusts pH of mixed, obtains no amino fluoride salt electric substrate cleaning combination.
The present invention application process be：By the electric substrate after machinery planarization be immersed in the present invention prepare without ammonia be fluorinated
In object salt electric substrate cleaning combination, and be fitted into polishing machine 40 ~ 50s of polishing, take out substrate, finally with pressure for 0.3 ~
0.5MPa gas flow purging substrate surfaces, electric substrate surface impurity removal rate are 95 ~ 98%.
The method have the benefit that：
（1）The present invention is prepared fast for electric substrate cleaning speed without amino fluoride salt electric substrate cleaning combination,
Cleaning performance is good；
（2）The present invention is prepared simple without amino fluoride salt electric substrate cleaning combination preparation process, is suitble to industrialization
It promotes.
Specific embodiment
4 ~ 6g sodium cellulose glycolates, 4 ~ 6g dodecyl sodium sulfates are weighed respectively, and 5 ~ 10g nano silicon dioxides add in
In 600 ~ 800mL deionized waters, 15 ~ 20min of ultrasonic disperse in 300W ultrasonic disperse machines is placed in, is configured to suspension, it will be suspended
Liquid is put into 60 ~ ﹣ of ﹣, 50 DEG C of vacuum drying chambers, is evacuated to vacuum degree as 1 ~ 10Pa, after being freeze-dried 20 ~ 30h, desciccate is filled
Enter in resistance furnace and calcine, be warming up to 1000 ~ 1200 DEG C with 5 ~ 10 DEG C/min, keep 3 ~ 4h of temperature, cooled to room temperature takes
Go out, obtain porous silica, it is spare；
7 ~ 8g polyacrylamides are weighed, adds in 500 ~ 600mL deionized waters, is stirred with 300 ~ 400r/min to polypropylene
Amide is completely dissolved, and with mass fraction be 10% methylamine water solution adjust pH value of solution be 8 ~ 11, continue 20 ~ 30min of stirring, add
Heat adds in 17 ~ 18g sulfanilamide (SN) to 60 ~ 70 DEG C, keeps 3 ~ 4h of thermotonus, obtains metal-chelator；Weigh the above-mentioned porous dioxies of 1 ~ 2g
SiClx adds in the above-mentioned metal-chelators of 10 ~ 12mL, is stirred 15 ~ 20min with 200 ~ 300r/min, is transferred to rotary evaporation
In instrument, former mixeding liquid volume 40 ~ 50% is evaporated to, is fitted into 105 ~ 110 DEG C of drying boxes and dries to constant weight, obtain solid phase detergent；Claim
1 ~ 2g polyacrylamides are taken, it is 10% hydrogen peroxide to add in 20 ~ 30mL mass fractions, is stirred with 200 ~ 300r/min to polyacrylamide
Amine is completely dissolved, and is added in 0.5 ~ 1.0g tetralkyl ammonium fluorides, is continued 1 ~ 2h of stirring, obtain liquid phase detergent, by 1 ~ 2g above-mentioned solid phases
Detergent is uniformly mixed with liquid phase detergent, is added in 70 ~ 80mL deionized waters, and is 10% methylamine water solution with mass fraction
It is 7 ~ 10 to adjust pH of mixed, obtains no amino fluoride salt electric substrate cleaning combination.
Example 1
4g sodium cellulose glycolates, 4g dodecyl sodium sulfates are weighed respectively, and 5g nano silicon dioxides add in 600mL and go
In ionized water, ultrasonic disperse 15min in 300W ultrasonic disperse machines is placed in, is configured to suspension, suspension is put into 60 DEG C of vacuum of ﹣
In drying box, vacuum degree is evacuated to as 1Pa, after being freeze-dried 20h, desciccate is fitted into resistance furnace and is calcined, with 5 DEG C/min liters
Temperature keeps temperature 3h to 1000 DEG C, and cooled to room temperature is taken out, obtains porous silica；7g polyacrylamides are weighed, are added
Enter in 500mL deionized waters, stirred to polyacrylamide and be completely dissolved with 300r/min, and be 10% methylamine water with mass fraction
It is 8 that solution, which adjusts pH value of solution, continues to stir 20min, is heated to 60 DEG C, add in 17g sulfanilamide (SN), keeps thermotonus 3h, obtain metal
Chelating agent；The above-mentioned porous silicas of 1g are weighed, adds in the above-mentioned metal-chelators of 10mL, is stirred with 200r/min
15min is transferred in Rotary Evaporators, is evaporated to former mixeding liquid volume 40%, is fitted into 105 DEG C of drying boxes and is dried to constant weight, must consolidate
Phase detergent；1g polyacrylamides are weighed, it is 10% hydrogen peroxide to add in 20mL mass fractions, is stirred with 200r/min to polypropylene
Amide is completely dissolved, and adds in 0.5g tetralkyl ammonium fluorides, is continued to stir 1h, liquid phase detergent is obtained, by 1g above-mentioned solid phase detergent
It is uniformly mixed, is added in 70mL deionized waters with liquid phase detergent, and mixed liquor is adjusted for 10% methylamine water solution with mass fraction
PH is 7, obtains no amino fluoride salt electric substrate cleaning combination.
The present invention application process be：By the electric substrate after machinery planarization be immersed in the present invention prepare without ammonia be fluorinated
It in object salt electric substrate cleaning combination, and is fitted into polishing machine and polishes 40s, take out substrate, be finally 0.3MPa gas with pressure
Stream purging substrate surface, electric substrate surface impurity removal rate are 95%.
Example 2
5g sodium cellulose glycolates, 5g dodecyl sodium sulfates are weighed respectively, and 8g nano silicon dioxides add in 700mL and go
In ionized water, ultrasonic disperse 18min in 300W ultrasonic disperse machines is placed in, is configured to suspension, suspension is put into 55 DEG C of vacuum of ﹣
In drying box, vacuum degree is evacuated to as 5Pa, after being freeze-dried 25h, desciccate is fitted into resistance furnace and is calcined, with 8 DEG C/min liters
Temperature keeps temperature 3.5h to 1100 DEG C, and cooled to room temperature is taken out, obtains porous silica；Weigh 7.5g polyacrylamides
Amine is added in 550mL deionized waters, is stirred to polyacrylamide and be completely dissolved with 350r/min, and is 10% first with mass fraction
It is 10 that amine aqueous solution, which adjusts pH value of solution, continues to stir 25min, is heated to 65 DEG C, add in 17.5g sulfanilamide (SN), keeps thermotonus
3.5h obtains metal-chelator；The above-mentioned porous silicas of 1.5g are weighed, are added in the above-mentioned metal-chelators of 11mL, with 250r/
Min is stirred 18min, is transferred in Rotary Evaporators, is evaporated to former mixeding liquid volume 45%, is fitted into 108 DEG C of drying boxes dry
To constant weight, solid phase detergent is obtained；1.5g polyacrylamides are weighed, it is 10% hydrogen peroxide to add in 25mL mass fractions, with 250r/min
Stirring to polyacrylamide is completely dissolved, and adds in 0.8g tetralkyl ammonium fluorides, is continued to stir 1.5h, is obtained liquid phase detergent, will
1.5g above-mentioned solid phases detergent is uniformly mixed with liquid phase detergent, is added in 75mL deionized waters, and is 10% first with mass fraction
It is 9 that amine aqueous solution, which adjusts pH of mixed, obtains no amino fluoride salt electric substrate cleaning combination.
The present invention application process be：By the electric substrate after machinery planarization be immersed in the present invention prepare without ammonia be fluorinated
It in object salt electric substrate cleaning combination, and is fitted into polishing machine and polishes 45s, take out substrate, be finally 0.4MPa gas with pressure
Stream purging substrate surface, electric substrate surface impurity removal rate are 96%.
Example 3
6g sodium cellulose glycolates, 6g dodecyl sodium sulfates are weighed respectively, and 10g nano silicon dioxides add in 800mL and go
In ionized water, ultrasonic disperse 20min in 300W ultrasonic disperse machines is placed in, is configured to suspension, suspension is put into 50 DEG C of vacuum of ﹣
In drying box, vacuum degree is evacuated to as 10Pa, after being freeze-dried 30h, desciccate is fitted into resistance furnace and is calcined, with 10 DEG C/min
1200 DEG C are warming up to, keeps temperature 4h, cooled to room temperature is taken out, obtains porous silica；8g polyacrylamides are weighed,
It adds in 600mL deionized waters, is stirred to polyacrylamide and be completely dissolved with 400r/min, and be 10% methylamine with mass fraction
It is 11 that aqueous solution, which adjusts pH value of solution, continues to stir 30min, is heated to 70 DEG C, add in 18g sulfanilamide (SN), keeps thermotonus 4h, obtain golden
Belong to chelating agent；The above-mentioned porous silicas of 2g are weighed, adds in the above-mentioned metal-chelators of 12mL, is stirred with 300r/min
20min is transferred in Rotary Evaporators, is evaporated to former mixeding liquid volume 50%, is fitted into 110 DEG C of drying boxes and is dried to constant weight, must consolidate
Phase detergent；2g polyacrylamides are weighed, it is 10% hydrogen peroxide to add in 30mL mass fractions, is stirred with 300r/min to polypropylene
Amide is completely dissolved, and adds in 1.0g tetralkyl ammonium fluorides, is continued to stir 2h, liquid phase detergent is obtained, by 2g above-mentioned solid phase detergent
It is uniformly mixed, is added in 80mL deionized waters with liquid phase detergent, and mixed liquor is adjusted for 10% methylamine water solution with mass fraction
PH is 10, obtains no amino fluoride salt electric substrate cleaning combination.
The present invention application process be：By the electric substrate after machinery planarization be immersed in the present invention prepare without ammonia be fluorinated
It in object salt electric substrate cleaning combination, and is fitted into polishing machine and polishes 50s, take out substrate, be finally 0.5MPa gas with pressure
Stream purging substrate surface, electric substrate surface impurity removal rate are 98%.
Claims (1)
1. a kind of preparation method of no amino fluoride salt electric substrate cleaning combination, it is characterised in that specifically preparation process is：
（1）4 ~ 6g sodium cellulose glycolates, 4 ~ 6g dodecyl sodium sulfates are weighed respectively, and 5 ~ 10g nano silicon dioxides add in
In 600 ~ 800mL deionized waters, 15 ~ 20min of ultrasonic disperse in 300W ultrasonic disperse machines is placed in, is configured to suspension, it will be suspended
Liquid is put into 60 ~ ﹣ of ﹣, 50 DEG C of vacuum drying chambers, is evacuated to vacuum degree as 1 ~ 10Pa, after being freeze-dried 20 ~ 30h, desciccate is filled
Enter in resistance furnace and calcine, be warming up to 1000 ~ 1200 DEG C with 5 ~ 10 DEG C/min, keep 3 ~ 4h of temperature, cooled to room temperature takes
Go out, obtain porous silica, it is spare；
（2）7 ~ 8g polyacrylamides are weighed, adds in 500 ~ 600mL deionized waters, is stirred with 300 ~ 400r/min to polypropylene
Amide is completely dissolved, and with mass fraction be 10% methylamine water solution adjust pH value of solution be 8 ~ 11, continue 20 ~ 30min of stirring, add
Heat adds in 17 ~ 18g sulfanilamide (SN) to 60 ~ 70 DEG C, keeps 3 ~ 4h of thermotonus, obtains metal-chelator；
（3）Weigh 1 ~ 2g above-mentioned steps（1）The porous silica of preparation is added in the above-mentioned metal-chelators of 10 ~ 12mL, with
200 ~ 300r/min is stirred 15 ~ 20min, is transferred in Rotary Evaporators, is evaporated to former mixeding liquid volume 40 ~ 50%, is packed into
It is dried in 105 ~ 110 DEG C of drying boxes to constant weight, obtains solid phase detergent；
（4）Weigh 1 ~ 2g polyacrylamides, it is 10% hydrogen peroxide to add in 20 ~ 30mL mass fractions, with 200 ~ 300r/min stir to
Polyacrylamide is completely dissolved, and is added in 0.5 ~ 1.0g tetralkyl ammonium fluorides, is continued 1 ~ 2h of stirring, obtain liquid phase detergent, by 1 ~ 2g
Above-mentioned solid phase detergent is uniformly mixed with liquid phase detergent, is added in 70 ~ 80mL deionized waters, and is 10% first with mass fraction
It is 7 ~ 10 that amine aqueous solution, which adjusts pH of mixed, obtains no amino fluoride salt electric substrate cleaning combination.
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| CN103146387A (en) * | 2013-03-19 | 2013-06-12 | 山东大学 | Process for preparing porous rare-earth luminescent material by freeze-drying method |
| CN104254906A (en) * | 2012-04-27 | 2014-12-31 | 和光纯药工业株式会社 | Cleaning agent for semiconductor substrates and method for processing semiconductor substrate surface |
| CN104592896A (en) * | 2014-12-31 | 2015-05-06 | 上海新安纳电子科技有限公司 | Chemical mechanical polishing solution |
-
2016
- 2016-08-05 CN CN201610636288.0A patent/CN106283092B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5382367A (en) * | 1987-08-07 | 1995-01-17 | Zinkan Enterprises Co. | Method of treating cooling water systems |
| CN102007196A (en) * | 2008-03-07 | 2011-04-06 | 高级技术材料公司 | Non-selective oxide etch wet clean composition and method of use |
| CN104254906A (en) * | 2012-04-27 | 2014-12-31 | 和光纯药工业株式会社 | Cleaning agent for semiconductor substrates and method for processing semiconductor substrate surface |
| CN103146387A (en) * | 2013-03-19 | 2013-06-12 | 山东大学 | Process for preparing porous rare-earth luminescent material by freeze-drying method |
| CN104592896A (en) * | 2014-12-31 | 2015-05-06 | 上海新安纳电子科技有限公司 | Chemical mechanical polishing solution |
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