CN102010665B - Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit - Google Patents
Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit Download PDFInfo
- Publication number
- CN102010665B CN102010665B CN 201010231732 CN201010231732A CN102010665B CN 102010665 B CN102010665 B CN 102010665B CN 201010231732 CN201010231732 CN 201010231732 CN 201010231732 A CN201010231732 A CN 201010231732A CN 102010665 B CN102010665 B CN 102010665B
- Authority
- CN
- China
- Prior art keywords
- polishing fluid
- closed reactor
- multilayer wiring
- integrated circuit
- polishing solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention relates to a method for preparing a polishing solution of a tungsten plug in the multilayer wiring of an ultralarge-scale integrated circuit. The polishing solution is a nano SiO2 grinding material with the concentration of 30%-50%, the grain size of 15-25 nm, and the Moh's hardness of 7 so as to benefit material removal and surface leveling, and the pH value of the polishing solution is 9-12 so that the polishing solution not only can meet the requirement on effective removal but also ensure the stability of silica sol. By adopting a negative-pressure vortex stirring preparation method, the method avoids the pollution of organic matters, large particles, metal ions and the like in the traditional preparation methods of compounding, mechanical stirring and the like, can achieve the requirement on ultra purification and has no corrosion on polishing equipment, and post cleaning is simple. The polishing solution has the advantages of small pollution, environmental protection, low cost and wide application range.
Description
Technical field
The invention belongs to the polishing fluid preparation method, particularly relate to the polishing fluid preparation method of tungsten plug in multilayer wiring.
Background technology
At present, the wiring number of plies of super large-scale integration is in continuous increase, and every one deck all requires leveling, and chemically machinery polished is unique method that can realize leveling.The research work of CMP mainly concentrates on the U.S. in the past take SEMTECH as main association, and at first the CMP technology entered the processing line application in the U.S. early than 1994 under its promotion.Subsequently, Japan also begins CMP technique is introduced the oxide film planarization technology of its 0.5 μ m processing line at the beginning of nineteen ninety-five, began the planarization technology for tungsten in 1996, now developed into the whole world, as the JESS of the association work in Europe, the French LETI of research company and CNET, the FRALDHOFER institute of Germany, the Korea S in Asia and China Taiwan be also in Study on Acceleration and exploitation, and present the high competition impetus.There is the effect of a series of complicated chemical and machinery in the technology of tungsten CMP, and many parameter such as pressure and temperature, pH values etc. of affecting are arranged, relate to physics of metals, solid-state physics, the multiple subjects such as materialogy and microelectronics also exist many fishes theoretical question to be solved.In chemically machinery polished, polishing fluid plays an important role to polishing speed and polishing effect, and the proportioning of polishing fluid is not disclosed as trade secret always.At present, the Wolfram polishing liquid produced of world-famous major company such as Cabot.Rohm and Haas is for acid.As the Semi-Sperse W2000 Wolfram polishing liquid of Cabot company, the pH value is between 2.1-2.9; The MSW2000 series of Rohm and Haas, the pH value is 3.9; These polishing fluids are take the higher aluminium sesquioxide of hardness as abrasive material.The polishing mechanism of acid polishing slurry is with strong mechanical effect, first grinds the method for the dissolving of acidifying again with the very high aluminium sesquioxide of hardness.Select to form unimolecular film than adding benzene this three (BTA) to increase film at recess in solution in order to improve height, recess is subjected to film to hinder to improve height and selects ratio when remove at protruding place.But complex technical process, speed is low, and the bits grain easily returns and again is adsorbed on the surface.Yet the acid polishing slurry etching apparatus causes that easily metal ion stains; As abrasive material, because alchlor hardness is large, easily cause scuffing with aluminium sesquioxide; And its viscosity is strong, and follow-up being difficult to cleans.Take silica hydrosol as abrasive material, unstable under high pH value, and the pH value is greater than the dissolving that silicon sol can occur in 12.5 o'clock.Along with the development of microelectronics, the requirement of chemically machinery polished is also being improved constantly.Because alkaline environment is fit to the environment that microelectronics is produced, therefore research and develop alkalescence polishing liquid to adapt to developing rapidly of microelectronic industry, be one of difficult problem of needing to be resolved hurrily of this field.
Summary of the invention
The present invention is in order to solve harmful pollutions such as organism that in known multilayer wiring, the tungsten plug polishing fluid exists, metal ion, macrobead in preparation process, and discloses a kind of simple and easy to do, free of contamination tungsten plug polishing fluid preparation method.
The present invention realizes by following technical proposals:
In a kind of great scale integrated circuit multilayer wiring, the preparation method of the polishing fluid of tungsten plug, is characterized in that, comprises the steps:
(1) use resistance as the ultrapure water more than 18M Ω, closed reactor and feed pipe to be cleaned, make the resistance that cleans rear waste liquid be not less than 16M Ω, generally need to clean more than three times; Described closed reactor is any in polypropylene, polyethylene, polymethyl methacrylate.
(2) feed pipe after the silicon sol that with mass percent concentration be 50%, particle diameter is 15-25nm, Mohs' hardness 7 cleans by step (1) joins in the airtight reactor that step (1) cleaned, closed reactor is vacuumized to make be the complete eddy current state of negative pressure in closed reactor, the formation vortex stirring;
(3) in the silicon sol solution that step (2) obtains, the limit is carried out the vortex stirring limit promoting agent, FA/O sequestrant, oxygenant is joined in closed reactor successively, continues to keep complete eddy current state;
(4) amine alkali is pumped under the state of complete eddy current in the solution that step (3) obtains, obtains the polishing fluid that pH value is 9-12 after fully stirring in eddy current 5-15 minute, carry out can and get final product.
The polishing fluid that obtains consisting of by mass percentage: mass percent concentration is 50%, particle diameter is the silicon sol 80-96.4% of 15-25nm, Mohs' hardness 7, promoting agent 0.5-5%, oxygenant 0.5-4%, FA/O sequestrant 0.1-5%, amine alkali 3-10%, and the polishing fluid total amount is no more than 4/5 of closed reactor capacity.
Above-mentioned each weight percent is all take the polishing fluid that obtains at last as benchmark.
Described amine alkali is any in hydroxyethylethylene diamine, trolamine, tetramethyl ammonium hydroxide.
Described oxygenant is soluble under alkaline medium, the superoxide of metal ion not, selects to add hydrogen peroxide or peroxide tetra-sodium.
Described tensio-active agent is O π-7 ((C
10H
21-C
6H
4-O-CH
2CH
2O)
7-H), the secondary alkyl ethoxylated (JFC) of polyoxyethylene, O π-10 ((C
10H
21-C
6H
4-O-CH
2CH
2O)
10-H), O-20 (C
12-18H
25-37-C
6H
4-O-CH
2CH
2O)
70-H), in any.The FA/O sequestrant is Jingling Microelectric Material Co., Ltd., Tianjin commercially available prod, for ethylenediamine tetraacetic acid (EDTA) four (tetrahydroxyethyl-ethylene diamine), can be abbreviated as NH
2RNH
2, its structural formula is as follows,
The present invention has following technique effect:
1, preparation method of the present invention forms complete eddy current state by the liquid make reactor under negative pressure state in, liquid in reactor is realized stirring, and, reactor uses transparent non-metallic material, can avoid the objectionable impuritiess such as organism, metal ion, macrobead to enter into polishing fluid, thereby reduce the concentration of metal ion, avoid the appearance of silicon sol coacervation, be conducive to improve the quality of finish of tungsten plug.
2, in preparation method of the present invention, the polishing fluid total amount is no more than 4/5 of closed reactor capacity, can make system be the eddy current state fully under negative pressure, can prevent laminar region Nano silica sol generation gelatin phenomenon and can't use, and improves the yield rate of polishing fluid.
3, in preparation method of the present invention, promoting agent adds under negative pressure eddy current state gradually, and the FA/O promoting agent coats the Nano silica sol that adds, and can improve the ability to bear that silicon sol changes potential of hydrogen, and gel or dissolving do not occur when adding amine alkali to regulate the pH value.
4, in preparation method of the present invention, sequestrant adds under negative pressure eddy current state gradually, but chelated metal ions reduces systemic contamination.
5, in preparation method of the present invention, amine alkali adds under negative pressure eddy current state gradually, can prevent the too high gel that causes Nano silica sol of local pH value or dissolving and can't use, and has improved the yield rate of polishing fluid.
6, polishing fluid of the present invention is alkalescence, and without corrosion, the silicon sol good stability has solved acid polishing slurry and polluted many drawbacks such as heavy, easy gel to equipment.
7, polishing fluid of the present invention selects Nano silica sol as the polishing fluid abrasive material, and its particle diameter is little, good dispersion degree, and metal ion content is low.Little to the tungsten plug surface damage, can reach two-forty, high smooth, low-damage polish, metal ion pollution is little simultaneously.
8, adopt high density, the high pH polishing fluid of present technique preparation to be convenient to transportation, to store, and can make cost, and the inventive method is simple.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
Closed reactor and feed pipe are cleaned four times, use resistance to be the ultrapure water 2000g more than 18M Ω at every turn; Then the silicon sol 3856g that with mass percent concentration be 50%, particle diameter is 15-25nm, Mohs' hardness 7 joins in the airtight reactor that cleaned, and closed reactor is vacuumized to make be the complete eddy current state of negative pressure in closed reactor, forms vortex stirring; The vortex stirring limit is carried out with O in the limit
II-720g, FA/O sequestrant 4g, hydrogen peroxide 5g join in closed reactor successively, continue to keep the eddy current state; In at last trolamine 120g being pumped into closed reactor under the state of eddy current, fully to obtain the pH value after 8 minutes be 9.86 polishing fluid to vortex stirring, then can.
Embodiment 2
Closed reactor and feed pipe are cleaned three times, use resistance to be the ultrapure water 2000g of 18M Ω at every turn; Then the silicon sol 3600g that with mass percent concentration be 50%, particle diameter is 15-25nm, Mohs' hardness 7 joins in the airtight reactor that cleaned, and closed reactor is vacuumized to make be the complete eddy current state of negative pressure in closed reactor, forms vortex stirring; The limit is carried out the vortex stirring limit O-2080g, FA/O sequestrant 72g, peroxide tetra-sodium 40g is joined in closed reactor successively, continues to keep the eddy current state; At last with tetramethyl ammonium hydroxide 200g under the state of eddy current in the suction closed reactor, fully obtain the pH value after vortex stirring and be 10.23 polishing fluid, then can.
Embodiment 3
Closed reactor and feed pipe are cleaned four times, use resistance to be the ultrapure water 2000g more than 18M Ω at every turn; Then the silicon sol 3440g that with mass percent concentration be 50%, particle diameter is 15-25nm, Mohs' hardness 7 joins in the airtight reactor that cleaned, and closed reactor is vacuumized to make be the complete eddy current state of negative pressure in closed reactor, forms vortex stirring; The limit is carried out the vortex stirring limit JFC140g, FA/O sequestrant 132g, hydrogen peroxide 45g is joined in closed reactor successively, continues to keep the eddy current state; At last with hydroxyethylethylene diamine 280g under the state of eddy current in the suction closed reactor, fully obtain the pH value after vortex stirring and be 11.20 polishing fluid, then can.
Claims (4)
1. the preparation method of the polishing fluid of tungsten plug in a great scale integrated circuit multilayer wiring, is characterized in that, comprises the steps:
(1) use resistance as the ultrapure water of 18M Ω, closed reactor and feed pipe to be cleaned three times at least, make the resistance that cleans rear waste liquid be not less than 16M Ω; Described closed reactor is any in polypropylene, polyethylene, polymethylmethacrylate;
(2) with mass percent concentration be 50%, particle diameter is the SiO of 15-25nm, Mohs' hardness 7
2The feed pipe that colloidal sol cleaned by step (1) joins in the airtight reactor that step (1) cleaned, closed reactor is vacuumized to make be the complete eddy current state of negative pressure in closed reactor, forms vortex stirring;
(3) in the silicon sol solution that step (2) obtains, the vortex stirring limit is carried out with promoting agent 0.5-5%, FA/O sequestrant 0.1-5%, oxygenant 0.5-4% in the limit, joins successively in closed reactor, continues to keep complete eddy current state;
(4) at last amine alkali 3-10% is pumped under the state of complete eddy current in the solution that step (3) obtains, fully obtains the polishing fluid that pH value is 9-12 after vortex stirring 5-15 minute, carry out can to get final product;
The polishing fluid that obtains contains that mass percent concentration is 50%, particle diameter is the SiO of 15-25nm Mohs' hardness 7
2Colloidal sol 80-95.4%, the per-cent of above-mentioned promoting agent, oxygenant, FA/O sequestrant and amine alkali are all take the polishing fluid that obtains at last as benchmark.
2. the preparation method of the polishing fluid of tungsten plug in great scale integrated circuit multilayer wiring according to claim 1, is characterized in that, described amine alkali is any in hydroxyethylethylene diamine, trolamine, tetramethyl ammonium hydroxide.
3. the preparation method of the polishing fluid of tungsten plug in great scale integrated circuit multilayer wiring according to claim 1, it is characterized in that: described oxygenant is hydrogen peroxide or peroxide tetra-sodium.
4. the preparation method of the polishing fluid of tungsten plug in great scale integrated circuit multilayer wiring according to claim 1, it is characterized in that: the polishing fluid total amount is no more than 4/5 of closed reactor capacity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010231732 CN102010665B (en) | 2010-07-21 | 2010-07-21 | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010231732 CN102010665B (en) | 2010-07-21 | 2010-07-21 | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102010665A CN102010665A (en) | 2011-04-13 |
| CN102010665B true CN102010665B (en) | 2013-06-05 |
Family
ID=43841001
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010231732 Expired - Fee Related CN102010665B (en) | 2010-07-21 | 2010-07-21 | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102010665B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858133A (en) * | 2006-05-31 | 2006-11-08 | 河北工业大学 | Polishing liquid for chemical and mechanical polsihing of computer hard disc base sheet |
| CN101096573A (en) * | 2006-06-30 | 2008-01-02 | 天津晶岭电子材料科技有限公司 | Polishing liquid for silica dioxide medium and preparation method thereof |
-
2010
- 2010-07-21 CN CN 201010231732 patent/CN102010665B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858133A (en) * | 2006-05-31 | 2006-11-08 | 河北工业大学 | Polishing liquid for chemical and mechanical polsihing of computer hard disc base sheet |
| CN101096573A (en) * | 2006-06-30 | 2008-01-02 | 天津晶岭电子材料科技有限公司 | Polishing liquid for silica dioxide medium and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102010665A (en) | 2011-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101671527A (en) | Copper chemical mechanical polishing solution with high removing rate and low damage, and preparation method thereof | |
| CN102888193A (en) | Chemical mechanical polishing solution for processing surface of sapphire or carborundum wafer for LED (Light Emitting Diode) substrate slice and preparation method thereof | |
| CN102660195B (en) | Surface modified nano-abrasive silicon slice polishing liquid | |
| CN101665665A (en) | Polishing solution for reducing copper chemical mechanical polishing roughness | |
| CN102796460B (en) | Silicon dioxide-based CMP (Chemical Mechanical Polishing) solution and preparation method thereof | |
| CN103992743A (en) | Polishing solution containing ceric oxide powder/colloid silicon dioxide mixed abrasive and preparing process thereof | |
| TW200420716A (en) | Polishing composition | |
| CN101081966A (en) | Polishing liquid for gallium arsenide wafer and preparation method thereof | |
| CN101096577A (en) | Antifreeze polishing liquid and preparation method thereof | |
| CN101096573A (en) | Polishing liquid for silica dioxide medium and preparation method thereof | |
| CN101935596B (en) | Polishing post-cleaning solution of sulfur series compound phase-change material | |
| CN101781525A (en) | Wafer rough polishing solution | |
| CN102010665B (en) | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit | |
| CN102010659B (en) | Preparation method of polishing solution for grinding and polishing lithium niobate optical chips | |
| CN104017501A (en) | Ultrasonic atomization-type polishing solution suitable for TFT-LCD (Thin Film Transistor-Liquid Crystal Display) glass substrate | |
| CN102010664B (en) | Method for preparing CMP (Chemical Mechanical Polishing) polishing solution of hard disc indium phosphide substrate | |
| CN102010658B (en) | Preparation method of chemical and mechanical polishing liquid of tungsten-molybdenum alloy material | |
| CN1858130A (en) | Polishing liquid for tungsten plug in large scale integrated circuit multilayer wiring | |
| CN102010660B (en) | Preparation method of chemical mechanical tantalum polishing solution | |
| CN104451691A (en) | Copper chemical mechanical finishing polishing solution applicable to low pressure | |
| CN100360631C (en) | Rare earth polishing liquor for organic alkaline corrosive medium | |
| CN102010663A (en) | Method for preparing chemical mechanical polishing solution of silicon dioxide dielectric | |
| CN103387795A (en) | Polishing paste and silicon ingot polishing method | |
| CN102010662B (en) | Preparation method of ceramic-glass polishing solution | |
| CN102010661A (en) | Method for preparing chemical and mechanical polishing liquid in ULSI (Ultra Large Scale Integrated) copper surface high-precision machining process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130605 Termination date: 20170721 |