CN102559056B - Chemical mechanical polishing liquid for polishing alloy phase change materials - Google Patents
Chemical mechanical polishing liquid for polishing alloy phase change materials Download PDFInfo
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- CN102559056B CN102559056B CN201010591176.0A CN201010591176A CN102559056B CN 102559056 B CN102559056 B CN 102559056B CN 201010591176 A CN201010591176 A CN 201010591176A CN 102559056 B CN102559056 B CN 102559056B
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Abstract
The invention discloses a chemical mechanical polishing liquid for polishing alloy phase change materials. The polishing liquid contains water, ground particles, an oxidant and a removal rate accelerator, wherein the removal rate accelerator is one ore more kinds of soluble compounds containing tungsten. In the invention, through adding the optimized removal rate accelerator in the polishing liquid, the lower SiO2 removal rate is remained while the removal rate of GST (germanium-stibonium-tellurium) alloy is increased, and the static corrosion of the polishing liquid on the GST material is remained at a lower level.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid, particularly relate to a kind of chemical mechanical polishing liquid for polishing alloy phase change material.
Background technology
Phase-change material (Phase Change Material, PCM) be a kind ofly can respond its physical action applied of outer bound pair (as optical, electrical, heat) and change the material of own physical state (as crystalline state, conductivity), this type of material has been widely used in the information recording devices such as CD.Phase-change material is incorporated among integrated circuit (IC)-components by the technology of newly-developed, make can high micro, can be three-dimensional stacked and there is the memory device of capability of fast response, also known as " phase change random access memory devices " (Phase-change Random Access Memory, PRAM), wherein the phase-change material of most use value is germanium-antimony-tellurium (GST) alloy, such as, have chemical formula Ge
2sb
2te
5(GST225) alloy.Because GST alloy still can keep excellent information storage capability under the state of extremely low dimension (about 5 nanometer), so the memory device adopting Ge-Sb-Te alloy to make has very high information storage density, therefore, phase change random access memory devices is considered to the memory of new generation having competitiveness.
The mode of conventional construction phase-change memory cell is first by method depositing phase change material in the pore defined by dielectric substance of magnetron sputtering, then by the method for reactive ion etching (RIE), unnecessary phase-change material above pore is removed, but high to substrate surface injury tolerance like this, cause product surface evenness low.Therefore the method for chemico-mechanical polishing (Chemical Mechanical Polishing, CMP) is mostly adopted now.Relative to conventional machining process, chemico-mechanical polishing requires usually while removing unnecessary material quickly, keeps the high-flatness of substrate surface after polishing and low damage.
But the polishing slurries of routine is all for the polishing to single metal material such as aluminium, copper, tungsten, as being directly used in the polishing of alloy phase-change material, the substrate surface poor flatness obtained after processing.Its main cause is, the hardness of phase-change material is lower, and the polishing slurries of high abrasive grains content can make the surface of phase-change material occur cut.On the other hand, some chemical mechanical polishing slurries evenly can not remove all components of phase-change material, and after causing polishing, phase-change material residue and residual is stayed on the dielectric layer, and in the subsequent step of device manufacture, cause further problem.In addition, in current phase-change material CMP (Chemical Mechanical Polishing) process, the barrier layer of polishing is generally silicon dioxide, therefore, when carrying out polishing to the wafer of circuit devcie of arranging, the uniformity of polishing and surface blemish (surface indentation and erosion) can be subject to the impact of the many factors such as polishing and static etch rate, the polishing uniformity of silicon dioxide film and the polishing selectivity between phase-change material and silicon dioxide film of such as phase-change material.
For the problem that above-mentioned chemical Mechanical Polishing Technique runs in phase-change material polishing, Chinese patent CN101333420A provides a kind of containing nitrogen compound, the polishing fluid with optionally abrasive grains and oxidant; CN101372606A adopts cerium oxide as abrasive grains; CN101736344A adopts the cataloid abrasive particle of particle mean size≤50 nanometer containing water and 1 ~ 40wt%, the quarternary ammonium salt compound of 0 ~ 5wt% and the polishing slurries of oxygen-free agent; US Patent No. 2007/0178700A1 provides a kind of phase-change material polishing agent containing chelating agent; US2008/0190035A1 provides a kind of phase-change material polishing agent comprising static corrosion inhibitor and diameter and be less than the polish abrasive of 30nm.Above-mentioned patent by improving grinding agent, or adds static corrosion inhibitor, reduce the static etch rate of phase-change material base material and reduce substrate surface cut, and obtaining certain effect, but effect is unsatisfactory.Chinese patent CN100335581C provides a kind of polishing fluid without abrasive material, effectively improve the evenness on phase-change material surface, but polishing speed is too low.
Summary of the invention
The invention provides a kind of removal rate enhancing agent of the heteropoly acid (or its salt) containing wolframic acid (or its salt) or tungstenic, for the chemical mechanical polishing liquid of polishing phase-change material, its object is to overcome the weak point of existing polishing fluid to the polishing of phase-change material base material, to improve the polishing effect to phase-change material base material.
A kind of chemical mechanical polishing liquid for polishing alloy phase change material of the present invention is achieved through the following technical solutions its object:
For a chemical mechanical polishing liquid for polishing alloy phase change material, wherein, water, abrasive grains, oxidant and removal rate enhancing agent is comprised; Described promoter at least comprises one or more solubility Tungstenic compounds.
The above-mentioned chemical mechanical polishing liquid for polishing alloy phase change material, wherein, described Tungstenic compound is for containing (WO
3)
m(H
2o)
nthe heteropoly acid of the various wolframic acids of general formula, various tungstates, tungstenic, or the heteropolyacid salt of tungstenic; Wherein m, n are positive integer, 1≤m≤12,1≤n≤20.
Above-mentioned chemical mechanical polishing liquid, wherein, described Tungstenic compound is positive wolframic acid, positive tungstates, metatungstic acid, metatungstate, phosphotungstic acid, phosphotungstate, silico-tungstic acid, or silicotungstate.
Above-mentioned chemical mechanical polishing liquid, wherein, described salt is sylvite or ammonium salt.
Above-mentioned chemical mechanical polishing liquid, wherein, described Tungstenic compound is potassium tungstate.
Above-mentioned chemical mechanical polishing liquid, wherein, the weight percentage of described removal rate enhancing agent is 0.001 ~ 2.0 %.
Above-mentioned chemical mechanical polishing liquid, wherein, described oxidant is one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, high boric acid, potassium permanganate and ferric nitrate.
Above-mentioned chemical mechanical polishing liquid, wherein, wherein, described oxidant weight percentage is 0.01 ~ 10.0 %.
Above-mentioned chemical mechanical polishing liquid, wherein, described abrasive grains to comprise in the silicon dioxide of silicon dioxide, aluminium oxide, adulterated al or aluminium coating, ceria, titanium dioxide or macromolecule abrasive grains one or more.
Above-mentioned chemical mechanical polishing liquid, wherein, described Silica abrasive particle comprises forging silicon dioxide or cataloid.
Above-mentioned chemical mechanical polishing liquid, wherein, wherein, the weight percentage of described abrasive grains is 0.01 ~ 5.0 %.
Above-mentioned chemical mechanical polishing liquid, wherein, described promoter also comprises nitric acid or nitrate.
Above-mentioned chemical mechanical polishing liquid, wherein, wherein, described nitric acid or nitrate weight percentage are 0 ~ 0.01 %.
The advantage of a kind of chemical mechanical polishing liquid for polishing alloy phase change material of the present invention is adopted to be:
1. the present invention by adding removal rate enhancing agent in polishing fluid, improves GST and remove speed, and maintain lower SiO
2remove speed.
2. the present invention is by removing the combination of rate enhancing agent, keeping higher GST to remove on the basis of speed (>=300nm/min), the total content removing rate enhancing agent can be reduced to 0.1%, thus reduce polishing cost.
3. the removal rate enhancing agent in the present invention also has the effect suppressing GST static corrosion simultaneously, and its GST that can either improve polishing fluid removes speed, also makes the static corrosion of polishing fluid to GST material remain on lower level.
Accompanying drawing explanation
Fig. 1 contains solution and the comparative solution electrochemical corrosion Tafel curve of removal rate enhancing agent (potassium tungstate) of the present invention;
Wherein, curve 2 is for being soaked in the electrochemical corrosion tower Fil curve containing the GST electrode in the aqueous solution (pH value 6.5) of have an appointment 1wt% potassium tungstate and about 2wt% hydrogen peroxide; Curve 1 is the electrochemical corrosion tower Fil curve be soaked in containing the GST electrode in the aqueous solution (pH value 6.5) of have an appointment 1wt% potassium nitrate and about 2wt% hydrogen peroxide as a comparison.
Embodiment
The invention provides a kind of chemical mechanical polishing liquid for polishing alloy phase change material, comprise water, abrasive grains, oxidant, removal rate enhancing agent.Wherein, described removal rate enhancing agent is one or more solubility Tungstenic compounds, as having chemical general formula (WO
3)
m(H
2o)
nthe various wolframic acids of (wherein, m, n are positive integer, 1≤m≤12,1≤n≤20), the heteropoly acid of tungstenic and salt thereof, comprise positive wolframic acid, metatungstic acid, phosphotungstic acid, silico-tungstic acid and their salt, as sylvite or ammonium salt.Described removal rate enhancing agent content is 0.001 ~ 2.0wt% of polishing fluid.
Described oxidant can be one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, high boric acid, potassium permanganate and ferric nitrate, and its consumption can within the scope of 0.01 ~ 10.0wt%; Described abrasive grains can be in the silicon dioxide of silicon dioxide, aluminium oxide, adulterated al or aluminium coating, ceria, titanium dioxide or macromolecule abrasive grains one or more, as forged silicon dioxide or cataloid, its content can within the scope of 0.01 ~ 5.0wt%; The binary additive such as nitric acid or nitrate (as potassium nitrate) can also be added in addition thus the polishing performance of enhancing polishing fluid.
In Fig. 1, curve 1 is GST electrode containing 2wt% H
2o
2+ 1wt% potassium nitrate, pH value is the Tafel curve recorded in the aqueous solution of 6.5, and curve 2 is GST electrode containing 2wt% H
2o
2+ 1wt% potassium tungstate, pH value is the Tafel curve recorded in the aqueous solution of 6.5.Work electrode used is GST electrode, and electrode material is amorphous state Ge
2sb
2te
5alloy cylinder, basal diameter 6.0 millimeters, height about 5 millimeters.Its side and upper bottom surface macromolecule resin and Teflon parcel, pick out contact conductor from upper bottom surface, the bottom surface exposed contacts with detected solution.Reference electrode used is saturated calomel electrode, and auxiliary electrode is platinum electrode.Electrode and detected solution form battery, and are connected to the CHI600B electrochemical workstation that Shanghai Chen Hua instrument company produces, and measuring-signal is by computer disposal and map.Process software is the CHI system (version number 5.10) of CH Instruments (U.S.) company.By calculating, corrosion current: potassium nitrate I
corr=43.1 μ A, potassium tungstate I
corr=4.9 μ A; Corrosion electric current density: potassium nitrate I
d=0.15mA/cm
2, potassium tungstate I
d=0.017mA/cm
2.Corrosion electric current density is directly proportional to the static etch rate of solution to metal material, is shown by the electrochemical data in Fig. 1, and relative to other general electrolyte (as potassium nitrate), potassium tungstate can alleviate the static corrosion of solution to GST material effectively.
Be below specific embodiments more of the present invention, for further illustrating advantage of the present invention, but the present invention being not limited by the following examples.Chemical reagent in embodiment and grinding agent are commercially available, and chemical reagent purity is more than chemical pure.Percentage by weight to 100% i.e. obtained polishing fluid is supplied with deionized water after described reagent, grinding agent and additive simply being mixed according to described proportioning.No. CAS corresponding to some chemical reagent is: potassium tungstate (CAS:7790-60-5), phosphotungstic acid (CAS:12501-23-4), silico-tungstic acid (CAS:12027-38-2).Polishing condition in embodiment is: polishing machine platform Logitech(Britain) 1PM52 type; 12 inches of politex polishing pads; 4cm ' 4cm square wafer coupons (wafer); Grinding table rotating speed 70 revs/min; Grinding head rotation rotating speed about 150 revs/min; Grinding pressure is about 3psi(pound/square inch); Polishing fluid rate of addition 100 ml/min.On the GST wafer that polishing is used, GST layer thickness is recorded by electron microscope (SEM) before polishing, its scope is at 300 to 500nm, being considered as polishing end point when being polished to base plate (being generally crystal silicon material) of exposing 50% area, namely obtaining GST with GST layer original thickness divided by polishing spent time and removing speed.The SiO that polishing is used
2the upper SiO of wafer
2layer thickness is recorded by NANOMETRICS films test instrument, namely obtains SiO by the thickness difference recorded before and after polishing divided by polishing consumes time
2remove speed.The experimental technique of unreceipted actual conditions in embodiment, usually conveniently condition, or according to the condition that manufacturer advises.
embodiment 1 ~ 3:
Table 1 is adopt the present invention to contain remove the chemical mechanical polishing liquid embodiment 1 ~ 3 of rate enhancing agent and do not contain the contrast table of chemical mechanical polishing liquid comparative example for removal speed during phase-change material polishing of described removal rate enhancing agent, wherein embodiment 1 ~ 3 comprises different abrasive grains, and different removal rate enhancing agent.
known by table 1, the GST polishing speed removing the polishing fluid embodiment 1 ~ 3 of rate enhancing agent by adding phosphotungstic acid, silico-tungstic acid, potassium tungstate etc. is obviously greater than the polishing fluid comparative example of not adding and removing rate enhancing agent.
embodiment 4 ~ 6:
Table 2 is the embodiment of the present invention 4 ~ 6 is oxidant at the hydrogen peroxide of use 2.0wt%, and GST when using different abrasive grains removes speed, removes RATES show with comparative example GST.
from table 2, in comparing by above-described embodiment 4 ~ 6 and comparative example, can find out, the present invention add a small amount of remove rate enhancing agent after, relative to comparative example, still have higher GST removal speed.And by changing abrasive grains, or regulate additive level, can effectively regulate GST to remove speed.
embodiment 7 ~ 10:
On the basis of above-described embodiment, the present invention removes rate enhancing agent can also comprise nitric acid or nitrate.
Table 3 is the embodiment of the present invention 7 ~ 10, using the hydrogen peroxide of 2.0wt% as oxidant, content is the cataloid (spheric granules of 2.0wt%, particle diameter is about 80nm) as abrasive grains, change the GST polish removal rate of the polishing fluid removing rate enhancing agent composition and content thereof, and GST removes speed and SiO
2remove the list of rate ratio.
from table 3, we can find, after with the addition of nitric acid or nitrate, when reducing potassium tungstate consumption, higher GST still can be kept to remove speed, the polishing effect of GST base material is enhanced.
Wherein, wt% of the present invention all refers to weight percentage.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (10)
1. for a chemical mechanical polishing liquid for polishing alloy phase change material, it is characterized in that, comprise water, abrasive grains, oxidant and removal rate enhancing agent; Described promoter at least comprises one or more solubility Tungstenic compounds, the weight percentage of wherein said removal rate enhancing agent is 0.001 ~ 2.0%, described oxidant weight percentage is 0.01 ~ 10.0%, and the weight percentage of described abrasive grains is 0.01 ~ 5.0%.
2. the chemical mechanical polishing liquid for polishing alloy phase change material according to claim 1, is characterized in that, described Tungstenic compound is for containing (WO
3)
m(H
2o)
nthe heteropoly acid of the various wolframic acids of general formula, various tungstates, tungstenic, or the heteropolyacid salt of tungstenic; Wherein m, n are positive integer, 1≤m≤12,1≤n≤20.
3. chemical mechanical polishing liquid according to claim 2, is characterized in that, described Tungstenic compound is positive wolframic acid, positive tungstates, metatungstic acid, metatungstate, phosphotungstic acid, phosphotungstate, silico-tungstic acid, or silicotungstate.
4. chemical mechanical polishing liquid according to claim 3, is characterized in that, described salt is sylvite or ammonium salt.
5. chemical mechanical polishing liquid according to claim 4, is characterized in that, described Tungstenic compound is potassium tungstate.
6. chemical mechanical polishing liquid according to claim 1, it is characterized in that, described oxidant is one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic acid, persulfate, percarbonate, periodic acid, perchloric acid, high boric acid, potassium permanganate and ferric nitrate.
7. chemical mechanical polishing liquid according to claim 1, is characterized in that, described abrasive grains to comprise in the silicon dioxide of silicon dioxide, aluminium oxide, adulterated al or aluminium coating, ceria, titanium dioxide or macromolecule abrasive grains one or more.
8. chemical mechanical polishing liquid according to claim 7, is characterized in that, described Silica abrasive particle comprises forging silicon dioxide or cataloid.
9. chemical mechanical polishing liquid according to claim 1, it is characterized in that, described promoter also comprises nitric acid or nitrate.
10. chemical mechanical polishing liquid according to claim 9, is characterized in that, wherein, described nitric acid or nitrate weight percentage are 0 ~ 0.01%.
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| JP6393231B2 (en) * | 2015-05-08 | 2018-09-19 | 信越化学工業株式会社 | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate |
| CN104987839A (en) * | 2015-06-30 | 2015-10-21 | 安徽德诺化工有限公司 | Sapphire substrate grinding fluid used for LED |
| CN109975207B (en) * | 2019-03-30 | 2020-09-04 | 西北有色金属研究院 | Method for observing Zamak2 zinc alloy color metallographic structure |
| CN113913116B (en) * | 2021-11-11 | 2022-09-09 | 中国电子科技集团公司第二十六研究所 | Polishing solution for polishing germanium single crystal and germanium single crystal polishing method |
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| JP4092015B2 (en) * | 1998-07-21 | 2008-05-28 | 花王株式会社 | Polishing liquid composition |
| US6454821B1 (en) * | 2000-06-21 | 2002-09-24 | Praxair S. T. Technology, Inc. | Polishing composition and method |
| US7077880B2 (en) * | 2004-01-16 | 2006-07-18 | Dupont Air Products Nanomaterials Llc | Surface modified colloidal abrasives, including stable bimetallic surface coated silica sols for chemical mechanical planarization |
| US7186653B2 (en) * | 2003-07-30 | 2007-03-06 | Climax Engineered Materials, Llc | Polishing slurries and methods for chemical mechanical polishing |
| CN1900206B (en) * | 2005-07-21 | 2011-01-05 | 安集微电子（上海）有限公司 | Chemical and mechanical polishing liquid and its use |
| US8541310B2 (en) * | 2007-05-04 | 2013-09-24 | Cabot Microelectronics Corporation | CMP compositions containing a soluble peroxometalate complex and methods of use thereof |
| KR100856543B1 (en) * | 2007-05-30 | 2008-09-04 | 재단법인서울대학교산학협력재단 | Method for forming oxidation barrier or diffusion barrier of metal line of semiconductor device |
| KR20090002501A (en) * | 2007-06-29 | 2009-01-09 | 제일모직주식회사 | Cmp slurry composition for the phase change memory materials and polishing method using the same |
| CN101665662A (en) * | 2008-09-05 | 2010-03-10 | 安集微电子科技(上海)有限公司 | Chemical mechanical polishing solution |
| CN101372606B (en) * | 2008-10-14 | 2013-04-17 | 中国科学院上海微系统与信息技术研究所 | Method for polishing sulfur compound phase-change material by cerium oxide chemico-mechanical polishing solution |
| CN101586005A (en) * | 2009-07-03 | 2009-11-25 | 中国科学院上海微系统与信息技术研究所 | Chemical-mechanical polishing solution for SiSb based phase-changing materials |
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