CN1858133A - Polishing liquid for chemical and mechanical polsihing of computer hard disc base sheet - Google Patents
Polishing liquid for chemical and mechanical polsihing of computer hard disc base sheet Download PDFInfo
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- CN1858133A CN1858133A CN 200610013979 CN200610013979A CN1858133A CN 1858133 A CN1858133 A CN 1858133A CN 200610013979 CN200610013979 CN 200610013979 CN 200610013979 A CN200610013979 A CN 200610013979A CN 1858133 A CN1858133 A CN 1858133A
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- polishing fluid
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- oxygenant
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Abstract
The present invention discloses a kind of alkaline polishing liquid with nanometer silica aquasol as abrasive for polishing memory hard disc base wafer. The polishing liquid consists of silica sol 50-90 wt%, chelating agent 0.5-10 wt%, pH regulator 0.5-5 wt%, surfactant 0.5-5 wt%, oxidant 0.5-10 wt% and deionized water for the rest. The present invention has strong chelating effect under alkaline condition, abrasive of silica aquasol in small grain size, high concentration and high dispersivity, polishing process with chemical effect mainly, and chelating agent and activator the ensure the ultimate polishing quality.
Description
Technical field
The present invention relates to computer memory hard disk manufacturing technical field, more particularly, relate to a kind of polishing fluid that is used for computer hard disc substrate.
Background technology
In recent years, the computer technology fast development, Personal Computer constantly advances towards high-performance, miniaturization.For adapting to this trend, develop towards large vol, high rotating speed, volume is little and security is higher direction as the major parts hard disk of computer data storage is corresponding, thereby hand disk wafer is proposed higher requirement.Because the disc direct relation the size of hard-disk capacity, so raising monolithic capacity promptly improves the key that the storage density of disc just becomes head it off.Along with the development of hand disk wafer technology, substrate surface planeness, roughness become the determinative of the size that affects hard disc storage capacity.
Smallest record area, raising hard-disk capacity in order to reduce hard disk drive require the distance between magnetic head and the disk magneticmedium further to reduce, so also more and more higher to the requirement of magnetic disk surface quality.Big or when having other surface imperfection when magnetic disk substrate surfaceness, percent ripple, usually cause the damage phenomenon of magnetic head, disk, thereby cause the hard disk can't works better or losing of reading and writing data.So, before finishing the manufacturing hand disk wafer, hand disk wafer is carried out chemically machinery polished, it is extremely important making substrate surface roughness, percent ripple reach minimum, also must remove surface imperfection such as cut, the limit of collapsing simultaneously.
Chemically machinery polished is to utilize the chemical solution be mixed with minimum abrasive grains to change the chemical bond of wafer surface, and mechanical polishing in addition, with a kind of chemistry and the mechanical technology that combines that obtains the wafer surface planarization.This technology collection tribology, hydromeehanics, chemistry are the ultraprecise planarization process technology of one.Surface brittleness crackle and the indenture that the hard grind material causes in the single mechanical mill, protuberance and the cut of avoiding abrasive grain to cause can be prevented, perfectly surface can be obtained.
Hard disc of computer dish substrate CMP (chemically machinery polished) know-why more complicated, the mechanism of generally acknowledging is thought: NiP apply plate the oxygenant oxidation in the polished liquid in aluminium alloy hand disk wafer surface, generate layer oxide film from the teeth outwards, its intensity is lower.Thereby harddisk surface is become fragile, then the nanometer SiO in the polishing fluid
2Particle grinds off this zone of oxidation as abrasive particle, and the unsalted surface that exposes after grinding off again can be oxidized, is ground off, so circulation again.Thereby can be ground off earlier and realized surperficial leveling because the dish substrate surface has the part of projection.
Wherein the input primary variables in the CMP process is the tincture in the polishing fluid: oxygenant, complexing agent, corrosion inhibitor, promoting agent etc.In recent years, oneself has had some patent reports polishing composition and the finishing method of magnetic disk substrate of memory, hard disk was as patent publication No. CN 1379074A, CN1357586A, CN 1316477A, CN 1213118C.Along with the raising of hard disk manufacturing merchant to the substrate surface processing quality of memory, hard disk, the chemically machinery polished polishing fluid that oneself has the control of getable final surfaceness, percent ripple and surface imperfection, can not satisfy the needs of memory, hard disk fast development, the world occupies the leading company of selling market maximum at present: the polishing fluid that Japanese Kao, U.S. Cabot etc. produce all shows strongly-acid, so in polishing process, machine has been caused corrosion, environment has been caused pollution, and the people has been had certain harm.In the prior art with aluminium sesquioxide as abrasive material because hardness is big, cause scuffing easily; And its viscosity is strong, and follow-up cleaning is not easy.Simultaneously, acid polishing slurry mainly is the chemically machinery polished effect based on machinery, in the polishing process, because the instability of polishing fluid transmission, and in the increase of polishing speed, the increase of polishing fluid flow, polishing fluid usually is being enriched in substrate edge, is easy to generate the limit phenomenon of collapsing like this.
Summary of the invention
Technical problem to be solved by this invention is, overcome the deficiencies in the prior art, a kind of magnetic disk substrate polishing fluid that is used for memory, hard disk is provided, under the alkaline environment, it has strong sequestering action, abrasive material is that particle diameter is little, the concentration height, the silica hydrosol of good dispersity, in the polishing process based on chemical action, by adding sequestrant, promoting agent solves final surfaceness, traditional problem such as percent ripple and surface imperfection, and existing by using alkalescence polishing liquid and silicon sol abrasive material to solve with the existing problem of aluminium sesquioxide as the acid polishing slurry of abrasive material.
The present invention is used for the polishing fluid of computer hard disc substrate chemically machinery polished, is achieved by following technical proposals, and the composition of described polishing fluid and weight % are than composed as follows:
Sequestrant 0.5-10; PH value conditioning agent 0.5-5;
Silicon sol 50-90; Tensio-active agent 0.5-5;
Oxygenant 0.5-10; The deionized water surplus.
The composition of the optimal components ratio of described polishing fluid of the present invention and weight % are than composed as follows:
Sequestrant 1.5-4; PH value conditioning agent 2.5-4.5;
Silicon sol 70-85; Tensio-active agent 1.5-4.5;
Oxygenant 1.5-4; The deionized water surplus.
Its particle diameter of silicon sol of the present invention is that 20~50nm, concentration are 40~50%.
Sequestrant of the present invention is FA/O (the water-soluble sequestrant with the non-metallic ion that is 13 above chelate rings) or EDTA.
PH value conditioning agent of the present invention is a hydroxyl polyamines class organic bases, as trolamine, tetramethyl-oxyammonia, tetrahydroxyethyl-ethylene diamine.
Promoting agent of the present invention is a tween, as FA/O tween, JFC type, O series.
Oxygenant of the present invention is a soluble superoxide under the alkaline medium, as hydrogen peroxide, peroxide trisodium phosphate (Na
4P
2O
810H
2O).
The present invention has following beneficial effect compared with prior art:
1. the present invention is an alkalescence polishing liquid, and equipment is not had corrosion, and the silicon sol good stability, pollutes many drawbacks such as heavy, easy gel thereby solved acid polishing slurry; When pH value 9 is above, easily generate the compound of solubility, thereby easily break away from the surface.
2. among the present invention, polishing fluid mainly plays the chemically machinery polished based on chemical action in polishing process, and the adding of sequestrant makes Ni form the macromole soluble organic easily, and it is stable to form thing, is easy to clean; Phosphorus is converted into soluble phosphate simultaneously; Polishing fluid is nontoxic, cost is low; Promoting agent has increased just selects ratio, greatly reduce surface tension, reduced affected layer, improved substrate surface homogeneity, make the concave-convex surface difference reduce greatly, thereby the rate of exchange of effectively raising has strengthened transport process, reaches high smooth high smooth finish surface; By creating the physics adsorbent is main environment, and the control substrate surface is in the physical adsorption state of easy cleaning for a long time, prevents that effectively particle from depositing again, realizes concentrating efficient the cleaning.
3. SiO among the present invention
2Its particle diameter of abrasive material little (20~50nm), concentration height (>40%), hardness little (little), good dispersion degree to the substrate damage degree, can reach the high smooth low-damage polish of two-forty, pollute for a short time, solved Al
2O
3Many drawbacks such as abrasive hardness is big; The problem of difficulty is cleaned in scuffing that causes when effectively solving aluminium sesquioxide for abrasive material and back, improves the yield rate of product; Simultaneously, also avoided the easily generation of the limit phenomenon of collapsing of generation in the acid polishing slurry polishing; The back is cleaned simple, can reduce the expense in the cleaning of back.
4. in polishing process, the present invention can reduce metal ion pollution.
5. the present invention's manufacturing cost price of filling a prescription is lower, and result of use can the substituting import one product.
The beneficial effect of each component is respectively among the present invention:
The FA/O sequestrant, it does not contain sodium ion and has 13 above chelate rings, the adding of sequestrant, increased the effective solubleness of metal ion in slurry, help the dissolving of Ni and Ni oxide particle, form the solvable complex of macromole, be easy to clean, reduced particle to the damage of glazed surface or particle deposition again, thereby also just reduced surface damage layer on the activated polishing surface; Promoting agent also has control action kou to particle, and promoting agent spreads over glazed surface uniformly, on the one hand, has strengthened the uniformity consistency of polishing slurries; On the one hand, particle is had " picking-up " effect, making particle is physical adsorption on the surface.Because the energy of physical adsorption is less, particle is easily taken away by the turbulent slurry, thereby has improved surperficial exquisiteness, helps to polish the carrying out that the back is cleaned.
The pH modulator, in alkalescence polishing liquid of the present invention, the selection of alkali is very important.The normal highly basic such as NaOH, KOH that use are as pH value modulator in the polishing fluid of bibliographical information.But this has a very big problem, and alkalimetal ion can enter in substrate or the medium layer in polishing process, thereby causes the effects such as local punchthrough effect, leakage current increase of device, the reliability of chip operation is reduced, reduce device lifetime; And if use silicon sol as abrasive material, the strong electrolyte cupric ion can make silica sol gel, thereby polishing fluid is scrapped.The present invention selects not, and the organic bases of metal ion has just solved this these problems.Organic bases is as pH value conditioning agent, and high energy is transferred to the pH value more than 12; And can also serve as buffer reagent, when polishing fluid local pH value changed, the hydroxyl of release itself was adjusted the pH value rapidly, make polishing fluid keep stable p H value, thereby it was even to make the oxide surface place remove speed, can obtain the better parallel degree.Simultaneously, when pH value>12.5, SiO
2Micelle is converted into solubility water liquid, and micelle disappears, and does not have the abrasive material effect, makes SiO when the adding organic amine can play under the high pH value
2Stable effect also has very important significance to improving slurry stability.
SiO among the present invention
2Its particle diameter of abrasive material little (20~50nm), concentration height (40~50%), hardness be 6~7 (little to the substrate damage degree), good dispersion degree, maximum particle diameter can not surpass the 5nm of the particle diameter upper limit, can solve the scratch resistant problem of hand disk wafer abrasive material; And good fluidity, nothing precipitate, polishing after product viscosity is little, and follow-up cleaning is simple; And abrasive silica is nontoxic, pollution-free, is the ideal abrasive material.
Tensio-active agent plays important effect in the substrate polishing.It affects dispersiveness, the particle absorption back of polishing fluid and cleans problems such as complexity and metal ion contamination.The promoting agent that the present invention selects for use the transfer rate that not only can improve the quality improves concavo-convex speed difference, to improve planeness; And can reduce surface tension, and reduce roughness, reduce the damage mist, can also preferentially adsorbed, form the physical adsorption surface of long-term easy cleaning, to improve condition of surface.
Oxygenant can be oxidized to substrate surface softer zone of oxidation in the polishing process, like this, under the worn effect of abrasive material, can easier strip down, and can improve polishing speed like this.Substrate polishing fluid oxygenant commonly used has K
3[Fe (CN)
6], Fe (NO
3)
3, KIO
3With hydrogen peroxide etc.K
3Fe (CN)
6, Fe (NO
3)
3Can introduce Fe
3+, KIO
3Can introduce K
+, form ion and stain, influence device performance, and K
3Fe (CN)
6Also have severe toxicity, this is very disadvantageous to being applied to production, and can cause serious environmental to pollute.And the used oxygenant of the present invention, it is metal ion not, can not cause that metal ion stains; And reaction product is pollution-free, is easy to clean.
Embodiment
Below in conjunction with embodiment the present invention is described further.
The composition of polishing fluid embodiment 1~embodiment 5 of the present invention and weight (kg) are composed as follows:
Sequestrant | PH value conditioning agent | Silicon sol | Tensio-active agent | Oxygenant | Deionized water | |
1 | FA/O 0.5 | Trolamine 0.5 | Concentration 40%, particle diameter 25~30nm, 90kg | FA/O tween 0.5 | Hydrogen peroxidase 10 .5 | 8 |
2 | FA/O 1.5 | Tetramethyl-oxyammonia 5 | Concentration 40%, particle diameter 35~40nm, 60kg | FA/O tween 1.5 | Peroxide trisodium phosphate 2 | 30 |
3 | FA/O 4 | The tetraethyl-hydroxyethylethylene diamine | Concentration 40%, particle diameter 45~ | The FA/O tween | Hydrogen peroxide 4 | 13 |
4.5 | 50nm,70kg | 4.5 | ||||
4 | EDTA 5 | Trolamine 2 | Concentration 50%, particle diameter 35~40nm, 58 | JFC 5 | Peroxide pyro acid phosphorus sodium 5 | 25 |
5 | EDTA 1 | Trolamine 2.5 | Concentration 50%, particle diameter 25~30nm, 85kg | JFC 0.5 | Peroxide trisodium phosphate 1 | 10 |
Sketch the preparation process of polishing fluid of the present invention with embodiment 1:
Get concentration 40%, particle diameter 25~30nm silicon sol 90kg, FA/O sequestrant 0.5kg, organic bases trolamine 0.5kg, FA/O tween 0.5kg, hydrogen peroxidase 10 .5kg, deionized water 8kg; In the silicon sol under the continuously stirring, slowly add the FA/O sequestrant of above-mentioned value successively, the organic bases trolamine, the FA/O tween, hydrogen peroxide, deionized water is stirred to the even computer hard disc substrate polishing fluid that gets.
Claims (7)
1. a polishing fluid that is used for the computer hard disc substrate chemically machinery polished is characterized in that, the composition of described polishing fluid and weight % are than composed as follows:
Sequestrant 0.5-10; PH value conditioning agent 0.5-5;
Silicon sol 50-90; Tensio-active agent 0.5-5;
Oxygenant 0.5-10; The deionized water surplus.
2. polishing fluid according to claim 1 is characterized in that, the composition of described polishing fluid and weight % are than composed as follows:
Sequestrant 1.5-4; PH value conditioning agent 2.5-4.5;
Silicon sol 70-85; Tensio-active agent 1.5-4.5;
Oxygenant 1.5-4; The deionized water surplus.
3. polishing fluid according to claim 1 and 2 is characterized in that, described sequestrant is FA/O or EDTA.
4. polishing fluid according to claim 1 and 2 is characterized in that, described pH value conditioning agent is a hydroxyl polyamines class organic bases, and described organic bases is trolamine, tetramethyl-oxyammonia or tetraethyl-hydroxyethylethylene diamine.
5. polishing fluid according to claim 1 and 2 is characterized in that, described promoting agent is a tween, is FA/O tween or JFC type.
6. polishing fluid according to claim 1 and 2 is characterized in that, described oxygenant is a soluble superoxide under the alkaline medium, and described superoxide is hydrogen peroxide or peroxide trisodium phosphate.
7. polishing fluid according to claim 1 and 2 is characterized in that, its particle diameter of described silicon sol is that 20~50nm, concentration are 40~50%.
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Cited By (12)
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CN101857775A (en) * | 2010-06-13 | 2010-10-13 | 北京国瑞升科技有限公司 | Lithium niobate crystal polishing solution and preparation method thereof |
CN101972753A (en) * | 2010-07-21 | 2011-02-16 | 河北工业大学 | Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing |
CN102010665A (en) * | 2010-07-21 | 2011-04-13 | 天津晶岭微电子材料有限公司 | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit |
CN102010658A (en) * | 2010-07-21 | 2011-04-13 | 天津晶岭微电子材料有限公司 | Preparation method of chemical and mechanical polishing liquid of tungsten-molybdenum alloy material |
CN102408837A (en) * | 2011-11-22 | 2012-04-11 | 清华大学 | Polishing composition capable of improving polishing precision of silicon wafer and preparation method thereof |
CN103450812A (en) * | 2013-01-10 | 2013-12-18 | 湖南皓志新材料股份有限公司 | Polishing solution for sapphire substrate |
CN103937414A (en) * | 2014-04-29 | 2014-07-23 | 杰明纳微电子股份有限公司 | Fine polishing liquid for hard disk substrate of computer |
CN104449404A (en) * | 2014-12-16 | 2015-03-25 | 河北工业大学 | Polishing solution for chemically mechanically polishing germanium crystal and application method |
CN109439202A (en) * | 2018-12-28 | 2019-03-08 | 天津洙诺科技有限公司 | A kind of silicon nitride CMP polishing fluid and its polishing liquid supply equipment |
CN110948377A (en) * | 2018-09-25 | 2020-04-03 | 长鑫存储技术有限公司 | Chemical mechanical polishing mixture and polishing method |
CN114952437A (en) * | 2022-05-27 | 2022-08-30 | 中国人民解放军国防科技大学 | Processing method of NiP modified layer |
CN115056117A (en) * | 2022-03-21 | 2022-09-16 | 康劲 | Polishing process for preventing scratches in CMP (chemical mechanical polishing) |
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Cited By (18)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101857775A (en) * | 2010-06-13 | 2010-10-13 | 北京国瑞升科技有限公司 | Lithium niobate crystal polishing solution and preparation method thereof |
CN101857775B (en) * | 2010-06-13 | 2013-11-06 | 北京国瑞升科技有限公司 | Lithium niobate crystal polishing solution and preparation method thereof |
CN101972753A (en) * | 2010-07-21 | 2011-02-16 | 河北工业大学 | Method for cleaning surface of magnesium aluminum alloy subjected to chemically mechanical polishing |
CN102010665A (en) * | 2010-07-21 | 2011-04-13 | 天津晶岭微电子材料有限公司 | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit |
CN102010658A (en) * | 2010-07-21 | 2011-04-13 | 天津晶岭微电子材料有限公司 | Preparation method of chemical and mechanical polishing liquid of tungsten-molybdenum alloy material |
CN102010665B (en) * | 2010-07-21 | 2013-06-05 | 天津晶岭微电子材料有限公司 | Method for preparing polishing solution of tungsten plug in multilayer wiring of ultralarge-scale integrated circuit |
CN102010658B (en) * | 2010-07-21 | 2013-06-05 | 天津晶岭微电子材料有限公司 | Preparation method of chemical and mechanical polishing liquid of tungsten-molybdenum alloy material |
CN102408837A (en) * | 2011-11-22 | 2012-04-11 | 清华大学 | Polishing composition capable of improving polishing precision of silicon wafer and preparation method thereof |
CN103450812A (en) * | 2013-01-10 | 2013-12-18 | 湖南皓志新材料股份有限公司 | Polishing solution for sapphire substrate |
CN103937414A (en) * | 2014-04-29 | 2014-07-23 | 杰明纳微电子股份有限公司 | Fine polishing liquid for hard disk substrate of computer |
CN103937414B (en) * | 2014-04-29 | 2018-03-02 | 杰明纳微电子股份有限公司 | A kind of precise polishing solution of hard disc of computer disk substrate |
CN104449404A (en) * | 2014-12-16 | 2015-03-25 | 河北工业大学 | Polishing solution for chemically mechanically polishing germanium crystal and application method |
CN104449404B (en) * | 2014-12-16 | 2016-08-10 | 河北工业大学 | The polishing fluid of germanium crystal chemically mechanical polishing and using method |
CN110948377A (en) * | 2018-09-25 | 2020-04-03 | 长鑫存储技术有限公司 | Chemical mechanical polishing mixture and polishing method |
CN109439202A (en) * | 2018-12-28 | 2019-03-08 | 天津洙诺科技有限公司 | A kind of silicon nitride CMP polishing fluid and its polishing liquid supply equipment |
CN115056117A (en) * | 2022-03-21 | 2022-09-16 | 康劲 | Polishing process for preventing scratches in CMP (chemical mechanical polishing) |
CN114952437A (en) * | 2022-05-27 | 2022-08-30 | 中国人民解放军国防科技大学 | Processing method of NiP modified layer |
CN114952437B (en) * | 2022-05-27 | 2023-08-18 | 中国人民解放军国防科技大学 | Processing method of NiP modified layer |
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