CN1335382A - Scavenger composition for superlarge scale IC chip and its prepn - Google Patents
Scavenger composition for superlarge scale IC chip and its prepn Download PDFInfo
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- CN1335382A CN1335382A CN 01115162 CN01115162A CN1335382A CN 1335382 A CN1335382 A CN 1335382A CN 01115162 CN01115162 CN 01115162 CN 01115162 A CN01115162 A CN 01115162A CN 1335382 A CN1335382 A CN 1335382A
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- deionized water
- coconut oil
- surfactant
- ethanol
- cleansing composition
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Abstract
The composite scavenger for superlarge scale IC chip consists of nonyl phenol polyethenoxy ether, coconut oil diethanolamide, oxypropylene oxyethylene glycerin ether betaine type surfactant, amino acid surfactant, EDTA, citric acid, iodine, isopropyl alcohol, ethanol, ethanolamine and deionized water. It is prepared through ion exchange to purity the components to MOS purity, mixing, recompounding, stirring, defoaming, and filtering. It may be used to replace sulfuric acid, nitric acid, hydrochloric acid, hydrogen peroxide, ammonia water and other chemicals in traditional scavenger and has similar cleaning effect but greatly reduce cost. It has no toxicity, no corrosion, no harm to human body and no environmental pollution.
Description
(1) technical field
The present invention relates to a kind of cleansing composition that is used for VLSI (very large scale integrated circuit) chip and preparation method thereof, belong to the chemical production field.
(2) background technology
The conventional clean technology that adopts in the industrial production is to use chemical reagent such as sulfuric acid, nitric acid, hydrochloric acid, hydrogen peroxide and ammoniacal liquor to carry out ultrasonic or boils at present, it is higher that these reagent be can't help cost, and corrodibility is very strong, harm operator's safety and health, contaminate environment.With the development of microelectronics industry, more and more harsher to the requirement of physical and chemical indexs such as its purity and granularity, the cost of clean-out system also is greatly improved.
(3) summary of the invention
In order to overcome the shortcoming of prior art, the invention provides a kind of cleansing composition that is used for super large-scale integration and preparation method thereof.
The present invention is achieved through the following technical measures.
Cleansing composition of the present invention basic composition is:
Weight percentages (%)
Coconut oil diethanol amide 2～15
Polyoxypropylene oxygen Ethylene Glycol ether (3000～3600) 0～5
Betaine type amphoteric surfactant 0～2
Amino acid type surfactant 0～2
Ethylenediamine tetraacetic acid (EDTA) 0～2
Citric acid 0.5～2
Virahol 0～6
Thanomin 1～3
The deionized water surplus
Described betaine type amphoteric surfactant is dodecyl dimethyl or octadecyl dihydroxy ethyl trimethyl-glycine.
Described amino acid type surfactant is N-dodecyl L-Ala or two fatty amide ethylidene glycine.
The present invention is preferably as follows composition:
Weight percentages (%)
Coconut oil diethanol amide 4～12
Polyoxypropylene oxygen Ethylene Glycol ether (3000～3600) 1.5～4
Citric acid 1～1.5
Ethanol 4.5～6.5
Thanomin 1.5～3
The deionized water surplus
The present invention also can be preferably as follows composition:
Weight percentages (%)
Coconut oil diethanol amide 4～10
Octadecyl dihydroxy ethyl trimethyl-glycine 1～2
N-dodecyl L-Ala 1～2
Ethylenediamine tetraacetic acid (EDTA) 1～2
Citric acid 0.5～1.5
Iodine 0.1～0.3
Virahol 2～5
Ethanol 5～6
Thanomin 1.5～2.5
The deionized water surplus
Preparation method of the present invention comprises the steps:
1. pre-treatment: it is pure that polyoxyethylene nonylphenol ether, coconut oil diethanol amide, polyoxypropylene oxygen Ethylene Glycol ether, amino acid type surfactant and betaine type amphoteric surfactant are reached MOS by the ion-exchange purification, deionized water is heated to 50～65 ℃ again;
2. with above-mentioned coconut oil diethanol amide 2～15 (weight percent % down together), polyoxypropylene oxygen Ethylene Glycol ether (3000～3600) 0～5, betaine type amphoteric surfactant 0～2, amino acid type surfactant 0～2, join in 50～65 ℃ the deionized water, maintain the temperature at 50～60 ℃ of scopes, under the normal pressure, stir, get homogeneous transparent liquid;
3. ethylenediamine tetraacetic acid (EDTA) 0～2, citric acid 0.5～2, and iodine 0～0.5, Virahol 0～6 is stirred to dissolving fully;
4. stopped to stir froth breaking 24 hours;
5. composite good solution is purified by ion exchange resin;
6. reconcile solution pH value to 9～10.5 with thanomin;
7. reconcile the viscosity of solution with ethanol, under the normal temperature, to 5～20 centipoises;
8. above-mentioned solution is filtered can under 100 grades of ultra-clean conditions.
Use cleansing composition of the present invention can replace the chemical reagent such as sulfuric acid, nitric acid, hydrochloric acid, hydrogen peroxide and ammoniacal liquor that use in the conventional clean technology fully, cleaning performance is equivalent to or slightly is better than the conventional clean technology, cleaning cost is lower than or is significantly less than conventional clean technology and nontoxic, non-corrosiveness, human body is not had harm, environmentally safe, simple to operate, original cleaning equipment is not needed big change, and its technology of preparing is not subjected to the restriction of unicircuit tempo.The technical indicator assay of cleansing composition of the present invention is:
Interventions Requested technical requirements assay
Outward appearance weak yellow liquid weak yellow liquid
PH value (20 ℃, stoste) 9.0～10.0 9.1
Density (25 ℃) 1.00 ± 0.02 1.00g/cm
3
Viscosity (25 ℃) 5～20 10mpa.s
Active agent content (%) 〉=99
Cleansing composition granularity of the present invention be particle diameter more than 0.5 micron under working conditions less than 50/ml.Purity be the content of detrimental impurity under working conditions less than 10ppb.
(4) description of drawings
Fig. 1 is that the conventional acid alkaline cleaner cleans the photo under the back AFM (atomic force microscope).
Fig. 2 is that scavenging solution of the present invention cleans the photo under the AFM of back.
Fig. 3 is that scavenging solution of the present invention cleans back MOS (metal-oxide semiconductor (MOS) abbreviation) electric capacity temperature front and back High Frequency C-V curve partially.
Fig. 4 is that the conventional acid alkaline cleaner cleans mos capacitance temperature front and back High Frequency C-V curve partially.
Fig. 5 is that scavenging solution of the present invention cleans total dose irradiation front and back MOS High Frequency C-V curve.
Fig. 6 is that conventional scavenging solution cleans total dose irradiation front and back MOS High Frequency C-V curve.
Fig. 7 is the electric lead curve that conventional scavenging solution cleaning silicon chip MOS measures.
Fig. 8 is the electric lead curve that scavenging solution cleaning silicon chip MOS of the present invention measures.
(5) specific embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1:100 kilogram cleaning agent
Weight percentages (%)
4 kilogram 4 of NPE
The bright chemical plant of place of production Jining of Shandong Province
6 kilogram 6 of coconut oil diethanol amide
Ten thousand li chemical plant, Hangzhou, the place of production
Polyoxypropylene oxygen Ethylene Glycol ether 1.5 1.5
The chemical plant that faces south, changzhou, the place of production
1 kilogram 1 of citric acid
Tianjin, place of production chemical reagent factory
4.5 kilogram 4.5 of 95% ethanol
Shandong Province, place of production chemical research institute
1.5 kilogram 1.5 of monoethanolamine
Place of production China (Shanghai) 5-linked chemical plant
Deionized water (self-produced 18,000,000) surplus
Preparation method of the present invention comprises the steps:
1. preliminary treatment: with NPE, coconut oil diethanol amide, polyoxypropylene oxygen Ethylene Glycol ether, It is pure that polyether surfactant and amino acid type surfactant reach MOS by the ion-exchange purification, again with 18,000,000 Deionized water be heated to 60 ℃; MOS is the abbreviation of metal-oxide semiconductor (MOS).
2. with NPE, (by same under the above-mentioned percentage by weight %) coconut oil diethanol amide, polyoxy third Alkene oxygen Ethylene Glycol ether (molecular weight 3000～3600) joins in 60 ℃ 18,000,000 deionized waters, keeps temperature 60 C, Under the normal pressure, stir, get homogeneous transparent liquid;
3. add again citric acid, be stirred to fully dissolving;
4. stop to stir, left standstill froth breaking 24 hours;
5. composite good solution is purified by ion exchange resin;
6. transfer solution pH value to 10.5 with monoethanolamine;
7. transfer the viscosity of solution with 95% ethanol, under the normal temperature, to 10 centipoises;
8. mentioned solution is filtered can under 100 grades of ultra-clean conditions.
Monitoring result of the present invention
Sample monitoring project method is according to monitoring result (mg/L)
Poaching wastewater COD potassium dichromate method 43.6
Biochemical water oxygen demand dilution and inocalation method 9.0
When using the present invention to clean, adopt the deionized water of 95% (percentage by weight) to be made into cleaning fluid, utilize ultrasonic Process, can effectively remove and be washed part surface dust, organic matter, the physical absorptions such as grease.
This cleaning agent is as follows with the cleaning performance contrast before silicon MOS device gate oxidation of conventional acid alkaline cleaner:
1. experimental result
Analyze metal on the residual silicon chip, analyzed metal has Cr, Cu, Fe, K, Mn, Na, Ni and Zn etc. adopt the Atomic Absorption Spectrometer analysis result to show, with the silicon chip of cleaning agent cleaning of the present invention, above-mentioned metal residue is in the distinguishable scope of instrument, be equal to the silicon chip effect that normal silicate base cleaning fluid cleans, to Na, the such alkali metal residue of K is less than 3.1Pg/cm2, satisfy the front cleaning requirement of MOS device gate oxidation.
With AFM photo is observed and taken to two kinds of cleaning silicon chip surface topographies, the result shows the present invention The smooth no etch pit of silicon chip surface that cleans, the silicon chip surface that soda acid commonly used cleans has the microcorrosion hole. The former cleans rear silicon chip Pattern is better than latter's (seeing Fig. 1 and Fig. 2).
The mos capacitance measurement result
Two kinds of cleaning methods present intimate identical mos capacitance High Frequency C-V curve (seeing Fig. 3 and Fig. 4), calculate SiO2The nearly SiO in-Si interface2Interior fixed charge density all is about 1 * 1011/cm
2 The temperature of row partially experimental result shows, temperature partially after two Plant cleaning method mos capacitance curves shift amount≤0.1 volt (seeing Fig. 3 and Fig. 4), corresponding mobile ion stains less than 5 * 1010/cm
2 Be 5 * 10 through accumulated dose5Behind Rad (Si) gamma Rays, two kinds of cleaning method mos capacitance curve movements are 0.8v (seeing Fig. 5 and Fig. 6), and corresponding radiation trapping charge density is 1.1 * 1011/cm
2。
MOS electricity lead curve measurement result
Two kinds of cleaning method silicon chip mos capacitances have been measured respectively 8 electric lead curves (seeing Fig. 7 and Fig. 8), calculated thus the cleaning mos capacitance, its average interface state density is 1.25 * 1010/cm
2.ev, the average interface state density of conventional cleaning mos capacitance is 1.1 * 1010/cm
2.ev, in error range, can think that both have the same interface density of states.
Disruptive field intensity is measured
The mos capacitance SiO of this cleansing composition2The breakdown voltage maximum is about 60 volts, and maximum disruptive field intensity is 1.2 * 107V/cm, MBV are about 50 volts, and minimum disruptive field intensity is 1 * 107V/cm, conventional cleaning fluid MOS electric capacity SiO2Breakdown voltage maximum and MBV have almost identical numerical value.
Embodiment 2:
As described in embodiment 1, different is,
Weight percentages (%)
6 kilogram 6 of NPE
8 kilogram 8 of coconut oil diethanol amide
2 kilogram 2 in polyoxypropylene oxygen Ethylene Glycol ether
1.5 kilogram 1.5 of citric acid
5 kilogram 5 of 95% ethanol
2 kilogram 2 of monoethanolamine
Deionized water surplus surplus
Reconcile solution pH value to 9.5 with monoethanolamine;
Reconcile the viscosity of solution with ethanol, under the normal temperature, to 15 centipoises.
Embodiment 3:
As described in embodiment 1, different is:
Weight percentages (%)
6 kilogram 6 of NPE
8 kilogram 8 of coconut oil diethanol amide
3 kilogram 3 in polyoxypropylene oxygen Ethylene Glycol ether
1 kilogram 1 of citric acid
6 kilogram 6 of 95% ethanol
3 kilogram 3 of monoethanolamine
Deionized water surplus surplus
Transfer solution pH value to 9 with monoethanolamine;
With the viscosity of ethanol accent solution, under the normal temperature, to 20 centipoises. Embodiment 4:100 kilogram cleaning agent
Weight percentages (%)
6 kilogram 6 of NPE
8 kilogram 8 of coconut oil diethanol amide
1 kilogram 1 of octadecyl dihydroxy ethyl betaine
Beijing Chemical Research Institute, the place of production
1 kilogram 1 of N-dodecyl alanine
Place of production Xiangfan City of Hubei Province chemical fertilizer factory
1 kilogram 1 of ethylenediamine tetra-acetic acid
Jinan, place of production reagent head factory
0.5 kilogram 0.5 of citric acid
Tianjin, place of production chemical reagent one factory
0.15 kilogram 0.15 of iodine
Shandong Province, place of production chemical research institute
3 kilogram 3 of isopropyl alcohol
Shandong Province, place of production chemical research institute
4 kilogram 4 of 95% ethanol
1.5 kilogram 1.5 of monoethanolamine
Deionized water (self-produced 18,000,000) surplus
Preparation method of the present invention comprises the steps:
1. earlier with NPE, coconut oil diethanol amide, octadecyl dihydroxy ethyl betaine, N-The dodecyl alanine is purified by ion-exchange, and to reach MOS pure, again 18,000,000 deionized water is heated to 60 ℃;
2. press NPE, (by same under the above-mentioned percentage by weight %) coconut oil diethanol amide, octadecane Base dihydroxy ethyl betaine, N-dodecyl alanine join in 60 ℃ 18,000,000 the deionized water, keep Temperature, stirs under the normal pressure 60 ℃ of scopes, gets homogeneous transparent liquid;
3. add ethylenediamine tetra-acetic acid, citric acid, ethylenediamine tetra-acetic acid by above-mentioned percentage by weight again, be stirred to CL;
4. stopped to stir froth breaking 24 hours;
5. composite good solution is purified by ion exchange resin;
6. transfer solution pH value to 10.5 with monoethanolamine;
7. transfer the viscosity of solution with ethanol, under the normal temperature, to 10 centipoises;
8. with mentioned solution after filtration, can under 100 grades of ultra-clean conditions.
Use and adopt when of the present invention 95% deionized water to be made into cleaning fluid, utilize ultrasonic processing, can effectively remove quilt Wash ionic and the atomic impurity on part surface.
Embodiment 5:
As described in embodiment, different is,
Weight percentages (%)
8 kilogram 8 of NPE
10 kilogram 10 of coconut oil diethanol amide
2 kilogram 2 of octadecyl dihydroxy ethyl betaine
2 kilogram 2 of N-dodecyl alanine
2 kilogram 2 of ethylenediamine tetra-acetic acid
0.5 kilogram 0.5 of citric acid
0.2 kilogram 0.2 of iodine
5 kilogram 5 of isopropyl alcohol
6 kilogram 6 of ethanol
2.5 kilogram 2.5 of monoethanolamine
Deionized water surplus surplus
Transfer solution pH value to 10.5 with monoethanolamine;
With the viscosity of ethanol accent solution, under the normal temperature, to 20 centipoises.
Claims (6)
1. a cleansing composition that is used for VLSI (very large scale integrated circuit) chip is characterized in that, basic composition is:
Weight percentages (%)
Polyoxyethylene nonylphenol ether 2～10
Coconut oil diethanol amide 2～15
Polyether surfactant (3000～3600) 0～5
Betaine type amphoteric surfactant 0～2
Amino acid type surfactant 0～2
Ethylenediamine tetraacetic acid (EDTA) 0～2
Citric acid 0.5～2
Iodine 0～0.5
Virahol 0～6
Ethanol 4～6
Thanomin 1～3
The deionized water surplus
2. a kind of cleansing composition that is used for VLSI (very large scale integrated circuit) chip according to claim 1 is characterized in that, described betaine type amphoteric surfactant is dodecyl dimethyl or octadecyl dihydroxy ethyl trimethyl-glycine.
3. described a kind of cleansing composition that is used for VLSI (very large scale integrated circuit) chip according to claim 1 is characterized in that, described amino acid type surfactant is N-dodecyl L-Ala or two fatty amide ethylidene glycine.
4. a kind of cleansing composition that is used for VLSI (very large scale integrated circuit) chip according to claim 1 is characterized in that, and is composed as follows:
Weight percentages (%)
Polyoxyethylene nonylphenol ether 8～9
Coconut oil diethanol amide 4～12
Polyoxypropylene oxygen Ethylene Glycol ether (3000～3600) 1.5～4
Citric acid 1～1.5
Ethanol 4.5～6.5
Thanomin 1.5～3
The deionized water surplus
5. a kind of cleansing composition that is used for VLSI (very large scale integrated circuit) chip according to claim 1 is characterized in that, and is composed as follows:
Weight percentages (%)
Polyoxyethylene nonyl phenyl hexene ether 4～8
Coconut oil diethanol amide 4～10
Octadecyl dihydroxy ethyl beet base 1～2
N-dodecyl L-Ala 1～2
Ethylenediamine tetraacetic acid (EDTA) 1～2
Citric acid 0.5～1.5
Iodine 0.1～0.3
Virahol 2～5
Ethanol 5～6
Thanomin 1.5～2.5
The deionized water surplus
6. the preparation method of the described cleansing composition of claim 1, step is as follows: comprise the steps:
(1) pre-treatment: it is pure that polyoxyethylene nonylphenol ether, coconut oil diethanol amide, polyoxypropylene oxygen Ethylene Glycol ether, amino acid type surfactant and betaine type amphoteric surfactant are reached MOS by the ion-exchange purification, deionized water is heated to 50～65 ℃ again;
(2) with above-mentioned polyoxyethylene nonyl phenyl hexene ether 2～10 (% by weight percentage), coconut oil diethanol amide 2～15, polyoxypropylene oxygen Ethylene Glycol ether (3000～3600) 0～5, betaine type amphoteric surfactant 0～2, amino acid type surfactant 0～2 joins 50～65 ℃ deionized water, maintain the temperature at 50～60 ℃ of scopes, under the normal pressure, stir, get homogeneous transparent liquid;
(3) add ethylenediamine tetraacetic acid (EDTA) 0～2 again, citric acid 0.5～2, iodine 0～0.5, Virahol 0～6 is stirred to dissolving fully;
(4) stop to stir 24 hours, froth breaking;
(5) composite good solution is purified by ion exchange resin;
(6) reconcile solution pH value to 9～10.5 with thanomin;
(7) reconcile the viscosity of solution with ethanol, under the normal temperature, to 5～20 centipoises;
(8) above-mentioned solution is filtered can under 100 grades of ultra-clean conditions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011151625A CN1181173C (en) | 2001-07-23 | 2001-07-23 | Scavenger composition for superlarge scale IC chip and its prepn |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011151625A CN1181173C (en) | 2001-07-23 | 2001-07-23 | Scavenger composition for superlarge scale IC chip and its prepn |
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| Publication Number | Publication Date |
|---|---|
| CN1335382A true CN1335382A (en) | 2002-02-13 |
| CN1181173C CN1181173C (en) | 2004-12-22 |
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|---|---|---|---|
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006125461A1 (en) * | 2005-05-25 | 2006-11-30 | Freescale Semiconductor, Inc | Treatment solution and method of applying a passivating layer |
| CN101000339B (en) * | 2007-01-22 | 2011-05-11 | 上海浩源生物科技有限公司 | Method for reusing microflow chip |
| CN104212658A (en) * | 2014-09-03 | 2014-12-17 | 朱滨 | Electrified cleaner for electric appliances and preparation method of electrified cleaner |
| CN104450332A (en) * | 2014-11-21 | 2015-03-25 | 苏州东辰林达检测技术有限公司 | Integrated circuit chip cleaning fluid and preparation method thereof |
| CN105039035A (en) * | 2015-06-30 | 2015-11-11 | 苏州东辰林达检测技术有限公司 | Cleaning agent for integrated circuit chip and preparation method of cleaning agent |
| CN105542990A (en) * | 2016-01-29 | 2016-05-04 | 苏州佳亿达电器有限公司 | Water-based LED (light emitting diode) chip cleaning agent |
| CN106967527A (en) * | 2017-04-07 | 2017-07-21 | 太仓协鑫光伏科技有限公司 | A kind of polysilicon chip cleaning agent and its application method |
| CN110484388A (en) * | 2019-09-12 | 2019-11-22 | 河北工业大学 | One kind low k dielectric materials cleaning agent and its cleaning method suitable for integrated circuit manufacture process |
| CN112961740A (en) * | 2021-02-22 | 2021-06-15 | 上海赛夫特半导体材料有限公司 | Cleaning agent for copper plating of circuit board and preparation method thereof |
| CN114317128A (en) * | 2021-12-28 | 2022-04-12 | 上海化学试剂研究所有限公司 | High-purity water-soluble silicon wafer cleaning agent and preparation method thereof |
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- 2001-07-23 CN CNB011151625A patent/CN1181173C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006125461A1 (en) * | 2005-05-25 | 2006-11-30 | Freescale Semiconductor, Inc | Treatment solution and method of applying a passivating layer |
| US7674725B2 (en) | 2005-05-25 | 2010-03-09 | Freescale Semiconductor, Inc. | Treatment solution and method of applying a passivating layer |
| CN101000339B (en) * | 2007-01-22 | 2011-05-11 | 上海浩源生物科技有限公司 | Method for reusing microflow chip |
| CN104212658A (en) * | 2014-09-03 | 2014-12-17 | 朱滨 | Electrified cleaner for electric appliances and preparation method of electrified cleaner |
| CN104450332A (en) * | 2014-11-21 | 2015-03-25 | 苏州东辰林达检测技术有限公司 | Integrated circuit chip cleaning fluid and preparation method thereof |
| CN105039035A (en) * | 2015-06-30 | 2015-11-11 | 苏州东辰林达检测技术有限公司 | Cleaning agent for integrated circuit chip and preparation method of cleaning agent |
| CN105542990A (en) * | 2016-01-29 | 2016-05-04 | 苏州佳亿达电器有限公司 | Water-based LED (light emitting diode) chip cleaning agent |
| CN106967527A (en) * | 2017-04-07 | 2017-07-21 | 太仓协鑫光伏科技有限公司 | A kind of polysilicon chip cleaning agent and its application method |
| CN110484388A (en) * | 2019-09-12 | 2019-11-22 | 河北工业大学 | One kind low k dielectric materials cleaning agent and its cleaning method suitable for integrated circuit manufacture process |
| CN112961740A (en) * | 2021-02-22 | 2021-06-15 | 上海赛夫特半导体材料有限公司 | Cleaning agent for copper plating of circuit board and preparation method thereof |
| CN114317128A (en) * | 2021-12-28 | 2022-04-12 | 上海化学试剂研究所有限公司 | High-purity water-soluble silicon wafer cleaning agent and preparation method thereof |
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