CN102559056A - Chemical mechanical polishing liquid for polishing alloy phase change materials - Google Patents

Chemical mechanical polishing liquid for polishing alloy phase change materials Download PDF

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CN102559056A
CN102559056A CN2010105911760A CN201010591176A CN102559056A CN 102559056 A CN102559056 A CN 102559056A CN 2010105911760 A CN2010105911760 A CN 2010105911760A CN 201010591176 A CN201010591176 A CN 201010591176A CN 102559056 A CN102559056 A CN 102559056A
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chemical mechanical
polishing liquid
mechanical polishing
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CN102559056B (en
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庞可亮
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Anji Microelectronics Shanghai Co Ltd
Anji Microelectronics Co Ltd
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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

A kind of chemical mechanical polishing liquid that is used to polish alloy phase change material
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid, relate in particular to a kind of chemical mechanical polishing liquid that is used to polish alloy phase change material.
Background technology
Phase change material (Phase Change Material; PCM) be a kind ofly can respond its physical action that applies of outer bound pair (like light, electricity, heat) and change the material of self physical condition (like crystalline state, specific conductivity), this type of material has been widely used in the information recording devices such as CD.The technology of newly-developed is incorporated into phase change material among the IC-components; Processing can high micro, can be three-dimensional stacked and memory device with capability of fast response; Also claim " phase change random access memory devices " (Phase-change Random Access Memory; PRAM), wherein the phase change material of tool use value is germanium-antimony-tellurium (GST) alloy, for example has chemical formula Ge 2Sb 2Te 5(GST225) alloy.Because the GST alloy still can keep excellent information storage capability under the state of extremely low dimension (about 5 nanometers); So the memory device that adopts Ge-Sb-Te alloy to process has very high information storage density; Therefore, phase change random access memory devices is considered to have the storer of new generation of competitive power.
The mode of conventional construction phase-change memory cell is method in the pore that by dielectric substance defined the sediment phase change material of elder generation through magnetron sputtering; Pass through the method for reactive ion etching (RIE) then; The unnecessary phase change material of pore top is removed; But high to the substrate surface injury tolerance like this, cause the product surface planeness low.Therefore mostly adopt chemically machinery polished (Chemical Mechanical Polishing, method CMP) now.With respect to conventional machining process, chemically machinery polished requires usually when removing unnecessary material quickly, keeps the high-flatness and low damage of polishing back substrate surface.
But conventional polishing slurries all is used for the polishing to single metal material such as aluminium, copper, tungsten, as it directly being used for polishing to alloy phase change material, and the substrate surface poor flatness that obtains after the processing.Its major 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 cut occur.On the other hand, some chemical mechanical polishing slurries can not evenly remove all components of phase change material, cause polishing back phase change material residue and residual and stay on the dielectric layer, and in the subsequent step of device manufacturing, cause further problem.In addition; In present phase change material CMP process; The blocking layer of polishing is generally silicon-dioxide; Therefore when the wafer to the circuit devcie of arranging polished, the uniformity coefficient of polishing and surface spots (surface depression and erosion) can receive polishing and static etch rate, the polishing uniformity coefficient of silicon dioxide film and the influence of various factors such as polishing selectivity between phase change material and the silicon dioxide film such as phase change material.
To the problem that above-mentioned chemical Mechanical Polishing Technique is run in phase change material polishing, Chinese patent CN101333420A provides a kind of and has contained nitrogen compound, had the polishing fluid of abrasive grains optionally and oxygenant; CN101372606A adopts cerium oxide as abrasive grains; CN101736344A adopts quarternary ammonium salt compound and the polishing slurries of oxygen-free agent of colloid silica abrasive particle, the 0 ~ 5wt% of mean particle size≤50 nanometers contain water and 1 ~ 40wt%; U.S. Pat 2007/0178700A1 provides a kind of phase change material rumbling compound that contains sequestrant; US2008/0190035A1 provides a kind of phase change material rumbling compound that comprises static corrosion suppressor factor and diameter less than the polish abrasive of 30nm.Above-mentioned patent is through improving abrasive, or adds the static corrosion suppressor factor, the static etch rate that reduces the phase change material base material with reduce the substrate surface cut, and obtain certain effect, but effect is unsatisfactory.Chinese patent CN100335581C provides a kind of polishing fluid that does not have abrasive material, effectively improved the planeness on phase change material surface, but polishing speed is low excessively.
Summary of the invention
The invention provides a kind of chemical mechanical polishing liquid removal speed promotor, that be used to polish phase change material that contains the heteropolyacid (or its salt) of wolframic acid (or its salt) or tungstenic; Its purpose 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 the phase change material base material.
The chemical mechanical polishing liquid that the present invention is a kind of to be used to polish alloy phase change material is realized its purpose through following technical scheme:
A kind of chemical mechanical polishing liquid that is used to polish alloy phase change material wherein, comprises water, abrasive grains, oxygenant and removal speed promotor; Said promotor comprises one or more solubility Tungstenic compounds at least.
The above-mentioned chemical mechanical polishing liquid that is used to polish alloy phase change material, wherein, said Tungstenic compound is for containing (WO 3) m(H 2O) nThe heteropolyacid of the various wolframic acids of general formula, various tungstate, 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, said Tungstenic compound is positive wolframic acid, positive tungstate, metatungstic acid, metatungstate, phospho-wolframic acid, Lin Wusuanyan, silicotungstic acid, or silicotungstate.
Above-mentioned chemical mechanical polishing liquid, wherein, said salt is sylvite or ammonium salt.
Above-mentioned chemical mechanical polishing liquid, wherein, described Tungstenic compound is a potassium wolframate.
Above-mentioned chemical mechanical polishing liquid, wherein, the weight percentage of said removal speed promotor is 0.001 ~ 2.0 %.
Above-mentioned chemical mechanical polishing liquid, wherein, said oxygenant is one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid 99, perchloric acid, high boric acid, potassium permanganate and the iron nitrate.
Above-mentioned chemical mechanical polishing liquid, wherein, wherein, said oxygenant weight percentage is 0.01 ~ 10.0 %.
Above-mentioned chemical mechanical polishing liquid, wherein, said abrasive grains comprises in silicon-dioxide, cerium dioxide, titanium oxide or the polymer abrasive grains of silicon-dioxide, aluminum oxide, adulterated al or aluminium coating one or more.
Above-mentioned chemical mechanical polishing liquid, wherein, said silicon-dioxide abrasive grains comprises forging silicon-dioxide or colloid silica.
Above-mentioned chemical mechanical polishing liquid, wherein, wherein, the weight percentage of said abrasive grains is 0.01 ~ 5.0 %.
Above-mentioned chemical mechanical polishing liquid, wherein, said promotor also comprises nitric acid or nitrate salt.
Above-mentioned chemical mechanical polishing liquid, wherein, wherein, said nitric acid or nitrate salt weight percentage are 0 ~ 0.01 %.
Adopt a kind of advantage that is used to polish the chemical mechanical polishing liquid of alloy phase change material of the present invention to be:
1. the present invention removes speed promotor through in polishing fluid, adding, and has improved GST and has removed speed, and kept lower SiO 2Remove speed.
2. the present invention is through removing the combination of speed promotor, (on >=300nm/min) the basis, can total content that remove speed promotor be reduced to 0.1%, thereby reduce the polishing cost keeping higher GST to remove speed.
3. the removal speed promotor among the present invention also has the effect that suppresses the GST static corrosion simultaneously, and its GST that can either improve polishing fluid removes speed, also makes polishing fluid that the static corrosion of GST material is remained on lower level.
Description of drawings
Fig. 1 contains the solution and the comparative solution galvanic corrosion Ta Feier curve of removal speed promotor according to the invention (potassium wolframate);
Wherein, curve 2 is for being soaked in the galvanic corrosion tower Fil curve of the GST electrode in the aqueous solution (pH value 6.5) that contains have an appointment 1wt% potassium wolframate and about 2wt% hydrogen peroxide; Curve 1 is the galvanic corrosion tower Fil curve that is soaked in the GST electrode in the aqueous solution (pH value 6.5) that contains have an appointment 1wt% saltpetre and about 2wt% hydrogen peroxide as a comparison.
Embodiment
The invention provides a kind of chemical mechanical polishing liquid that is used to polish alloy phase change material, comprise water, abrasive grains, oxygenant, removal speed promotor.Wherein, said removal speed promotor is one or more solubility Tungstenic compounds, as has 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 heteropolyacid and the salt thereof of tungstenic comprise positive wolframic acid, metatungstic acid, phospho-wolframic acid, silicotungstic acid and their salt, like sylvite or ammonium salt.Said removal speed accelerator content is 0.001 ~ 2.0wt% of polishing fluid.
Said oxygenant can be one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid 99, perchloric acid, high boric acid, potassium permanganate and the iron nitrate, and its consumption can be in 0.01 ~ 10.0wt% scope; Said abrasive grains can be in silicon-dioxide, cerium dioxide, titanium oxide or the polymer abrasive grains of silicon-dioxide, aluminum oxide, adulterated al or aluminium coating one or more; As forging silicon-dioxide or colloid silica, its content can be in 0.01 ~ 5.0wt% scope; Can also add nitric acid or nitrate salt (like saltpetre) in addition thus etc. binary additive strengthen the polishing performance of polishing fluid.
Among Fig. 1, curve 1 is containing 2wt% H for the GST electrode 2O 2+ 1wt% saltpetre, pH value are the Ta Feier curve that records in 6.5 the aqueous solution, and curve 2 is containing 2wt% H for the GST electrode 2O 2+ 1wt% potassium wolframate, pH value are the Ta Feier curve that records in 6.5 the aqueous solution.Used working electrode is the GST electrode, and electrode materials is non-crystalline state Ge 2Sb 2Te 5The alloy right cylinder, 6.0 millimeters of bottom surface diameters, high about 5 millimeters.Its side and upper bottom surface pick out contact conductor with macromolecule resin and Teflon parcel from upper bottom surface, and the bottom surface that exposes contacts with detected solution.Used reference electrode is a SCE, and supporting electrode is a platinum wire electrode.Electrode and detected solution are formed battery, and are connected to the CHI600B electrochemical workstation that Shanghai occasion China instrument company produces, and measurement signal is by CP and mapping.Process software is the CHI system (version number 5.10) of CH Instruments (U.S.) company.Through calculating corrosion current: saltpetre I Corr=43.1 μ A, potassium wolframate I Corr=4.9 μ A; Corrosion electric current density: saltpetre I d=0.15mA/cm 2, potassium wolframate I d=0.017mA/cm 2Corrosion electric current density is directly proportional with the static etch rate of solution to metallic substance, is shown by the electrochemical data among Fig. 1, and with respect to other general electrolyte (like saltpetre), potassium wolframate can alleviate the static corrosion of solution to the GST material effectively.
Below be specific embodiments more of the present invention, be used to further specify advantage of the present invention, but the present invention does not receive the restriction of following examples.Chemical reagent among the embodiment and abrasive are commercially available, and chemical reagent purity is more than the CP.Said reagent, abrasive and additive are simply mixed the back according to said proportioning to be supplied weight percent to 100% with deionized water and promptly makes polishing fluid.Be for the pairing CAS of some chemical reagent number: potassium wolframate (CAS:7790-60-5), phospho-wolframic acid (CAS:12501-23-4), silicotungstic acid (CAS:12027-38-2).Polishing condition among the embodiment is: polishing machine platform Logitech (Britain) 1PM52 type; 12 inches politex polishing pads; 4cm ' 4cm square wafer coupons (wafer); 70 rev/mins of grinding stage rotating speeds; About 150 rev/mins of grinding head rotation rotating speed; The about 3psi of grinding pressure (pound/square inch); Polishing fluid rate of addition 100 ml/min.Polish that the GST layer thickness is recorded by electron microscope (SEM) on the used GST wafer before polishing; Its scope 300 to 500nm; When being polished to the base plate (being generally the crystal silicon material) that exposes 50% area, be regarded as polishing end point, promptly get GST with GST layer original thickness divided by polishing institute time-consuming and remove speed.Polish used SiO 2The last SiO of wafer 2Layer thickness is recorded by NANOMETRICS films test appearance, promptly gets SiO with the thickness difference that records before and after the polishing divided by the polishing consumption time 2Remove speed.The experimental technique of unreceipted actual conditions among the embodiment, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1 ~ 3:
The contrast table of the removal speed when table 1 contains the chemical mechanical polishing liquid embodiment 1 ~ 3 that removes speed promotor and is used for the phase change material polishing chemical mechanical polishing liquid Comparative Examples that does not contain said removal speed promotor for employing the present invention; Wherein embodiment 1 ~ 3 comprises the different polishing particle, and different removal speed promotor.
Figure 2010105911760100002DEST_PATH_IMAGE001
can know through table 1, through adding the GST polishing speed of polishing fluid embodiment 1 ~ 3 that phospho-wolframic acid, silicotungstic acid, potassium wolframate etc. remove speed promotor obviously greater than not adding the polishing fluid Comparative Examples of removing speed promotor.
Embodiment 4 ~ 6:
Table 2 is that the embodiment of the invention 4 ~ 6 is oxygenant at the hydrogen peroxide that uses 2.0wt%, and the GST when using the different polishing grain removes speed, removes the speed contrast table with Comparative Examples GST.
Figure 940670DEST_PATH_IMAGE002
is from table 2; In through the foregoing description 4 ~ 6 comparison with Comparative Examples; Can find out; After the present invention adds a small amount of removal speed promotor,, still there is higher GST to remove speed with respect to Comparative Examples.And through changing abrasive grain, perhaps regulate additive level, can effectively regulate GST and remove speed.
Embodiment 7 ~ 10:
On the basis of the foregoing description, the present invention removes speed promotor can also comprise nitric acid or nitrate salt.
Table 3 is the embodiment of the invention 7 ~ 10; At the hydrogen peroxide that uses 2.0wt% as oxygenant; Content is the colloid silica (spheroidal particle of 2.0wt%; The about 80nm of particle diameter), change the GST polish removal rate of the polishing fluid of removing speed promotor composition and content thereof, and GST removes speed and SiO as abrasive grain 2Remove the tabulation of speed ratio.
Figure 44761DEST_PATH_IMAGE004
we can find from table 3; After having added nitric acid or nitrate salt; Under the situation that reduces the potassium wolframate consumption; Still can keep higher GST to remove speed, make the polishing effect of GST base material be enhanced.
Wherein, wt% according to the invention all refers to weight percentage.
More than specific embodiment of the present invention is described in detail, but it is just as example, the present invention is not restricted to the specific embodiment of above description.To those skilled in the art, any equivalent modifications that the present invention is carried out with substitute also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of being done under the spirit and scope of the present invention, all should contain within the scope of the invention.

Claims (13)

1. a chemical mechanical polishing liquid that is used to polish alloy phase change material is characterized in that, comprises water, abrasive grains, oxygenant and removal speed promotor; Said promotor comprises one or more solubility Tungstenic compounds at least.
2. the chemical mechanical polishing liquid that is used to polish alloy phase change material according to claim 1 is characterized in that said Tungstenic compound is for containing (WO 3) m(H 2O) nThe heteropolyacid of the various wolframic acids of general formula, various tungstate, 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, said Tungstenic compound is positive wolframic acid, positive tungstate, metatungstic acid, metatungstate, phospho-wolframic acid, Lin Wusuanyan, silicotungstic acid, or silicotungstate.
4. chemical mechanical polishing liquid according to claim 3 is characterized in that, said salt is sylvite or ammonium salt.
5. chemical mechanical polishing liquid according to claim 4 is characterized in that, described Tungstenic compound is a potassium wolframate.
6. chemical mechanical polishing liquid according to claim 1 is characterized in that, the weight percentage of said removal speed promotor is 0.001 ~ 2.0 %.
7. chemical mechanical polishing liquid according to claim 1; It is characterized in that said oxygenant is one or more in hydrogen peroxide, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, percarbonate, Periodic acid 99, perchloric acid, high boric acid, potassium permanganate and the iron nitrate.
8. chemical mechanical polishing liquid according to claim 7 is characterized in that, wherein, said oxygenant weight percentage is 0.01 ~ 10.0 %.
9. chemical mechanical polishing liquid according to claim 1 is characterized in that, said abrasive grains comprises in silicon-dioxide, cerium dioxide, titanium oxide or the polymer abrasive grains of silicon-dioxide, aluminum oxide, adulterated al or aluminium coating one or more.
10. chemical mechanical polishing liquid according to claim 8 is characterized in that, said silicon-dioxide abrasive grains comprises forging silicon-dioxide or colloid silica.
11. chemical mechanical polishing liquid according to claim 9 is characterized in that, wherein, the weight percentage of said abrasive grains is 0.01 ~ 5.0 %.
12., it is characterized in that said promotor also comprises nitric acid or nitrate salt according to the said chemical mechanical polishing liquid of claim 1.
13. chemical mechanical polishing liquid according to claim 12 is characterized in that, wherein, said nitric acid or nitrate salt weight percentage are 0 ~ 0.01 %.
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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
CN107532066A (en) * 2015-05-08 2018-01-02 信越化学工业株式会社 The Ginding process of synthetic quartz glass substrate grinding agent and synthetic quartz glass substrate
CN109975207A (en) * 2019-03-30 2019-07-05 西北有色金属研究院 A kind of observation method of 2 kirsite metallurgical structure of Zamak
CN113913116A (en) * 2021-11-11 2022-01-11 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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CN113913116A (en) * 2021-11-11 2022-01-11 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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