CN101586005A - Chemical-mechanical polishing solution for SiSb based phase-changing materials - Google Patents
Chemical-mechanical polishing solution for SiSb based phase-changing materials Download PDFInfo
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- CN101586005A CN101586005A CNA2009100543914A CN200910054391A CN101586005A CN 101586005 A CN101586005 A CN 101586005A CN A2009100543914 A CNA2009100543914 A CN A2009100543914A CN 200910054391 A CN200910054391 A CN 200910054391A CN 101586005 A CN101586005 A CN 101586005A
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Abstract
The invention relates to chemical-mechanical polishing solution for SiSb based phase-changing materials, comprising: 0.2-30wt. % of oxidic polishing grains, 0.01-5wt. % of oxidant, 0.01-4wt. % of surfactant, 0.01-3wt. % of organic addition agent, and the remainder pH modifier and aqueous medium. The polishing of the SiSb based phase-changing materials by the chemical-mechanical polishing solution has controllable speeds, good surface qualities and low damages, which can meet the requirements of CMP processing in the manufacturing of nano-electronic phase-change memories. By the chemical-mechanical polishing solution, the polishing speed of the SiSb based phase-changing materials can be controlled to be 5-2000nm/min; and the surface roughness is reduced to be less than 0.7nm.
Description
Technical field
The invention belongs to the technical field of phase change material, particularly relate to a kind of SiSb based phase-change material chemical mechanical polishing liquid with chemical mechanical polishing liquid.
Background technology
Phase transition storage reads at a high speed because of having, high erasable number of times, non-volatile, component size is little, strong motion low in energy consumption, anti-and radioprotective, cost have advantages such as competitive power, and is thought the most possible nonvolatile memory of future generation that replaces present flash memories by international semiconductor employer's organization.
The ultimate principle of phase transition storage technology is to be storage media with the chalcogenide compound, utilize electric energy (heat) to make material change writing and wiping of realization information mutually between crystalline state (low-resistance) and non-crystalline state (high resistant), the variation of then leaning on measuring resistance of reading of information realizes.Storage unit comprises that phase change material is deposited in the pore by the pore of dielectric substance definition, and phase change material is connection electrode on an end of pore.The electrode contact makes electric current produce joule heating by this passage and is programmed in this unit, perhaps reads this unitary resistance states.
At present, when making up phase-change memory cell, current way is: the method sediment phase change material that passes through magnetron sputtering earlier is in the pore by the dielectric substance definition, by the method for reactive ion etching (RIE) or chemically machinery polished (CMP), the phase change material of thin empty top is removed then.Than RIE, CMP is because of having surface low damnification and the advantage that can realize overall planarization, and the parent who has been subjected to many researchists and semiconductor company looks at.
SiSb is as a kind of high performance phase-change storage material, performance advantage with each side, as: environmental friendliness do not have tellurium, be convenient to CMOS technology is compatible fully, composition is simple before and after processing and performance cutting, the phase transformation that variable density is little, high data retention ability etc.(Appl.Phys.Lett.91 222,102 2007 for people such as T.Zhang, Advantage of SiSb phase-change material and its application s inphase-change memory).
For satisfying the demand of CMP technology in the preparation nano-electron SiSb base phase transition storage, need controlled with no damage the SiSb based phase-change material being removed, also wish to reduce as far as possible the loss of lower floor's insulating material simultaneously.Yet at the CMP of SiSb base phase-change storage material, not seeing so far has report.
Summary of the invention
Technical problem to be solved by this invention provides a kind of SiSb based phase-change material chemical mechanical polishing liquid, by this chemical mechanical polishing pulp, the polishing speed of SiSb based phase-change material can be controlled in 5～2000nm/min, surfaceness has been reduced to below the 0.7nm simultaneously, utilize that above-mentioned polishing fluid is controlled to SiSb based phase-change material speed, surface quality good and the polishing of low damage, can satisfy the needs of CMP technology in the preparation sodium electronic phase-variable memory.
A kind of SiSb based phase-change material chemical mechanical polishing liquid of the present invention comprises following component:
Oxycompound polishing particles 0.2-30wt%
Oxygenant 0.01-5wt%
Tensio-active agent 0.01-4wt%
Organic additive 0.01-3wt%
All the other wt% of pH regulator agent and aqueous medium;
Described oxycompound polishing particles is aluminum oxide, cerium oxide, zirconium white, titanium oxide or colloidal silica, particle size range 10-1500nm;
Preferred particle size range is 30-200nm.
Described oxygenant is the Tripotassium iron hexacyanide, hydrogen peroxide or ammonium persulphate;
Described tensio-active agent is polyoxyethylene sodium sulfate AES, sodium polyacrylate, polyoxyethylene ether phosphate, alkyl alcohol polyoxyethylene groups ether or cetyl trimethylammonium bromide;
Described organic additive is acetate, formic acid, oxalic acid, citric acid, terephthalic acid, Whitfield's ointment, proline(Pro), Padil, Succinic Acid or tartrate;
Described pH regulator agent is nitric acid, phosphoric acid, potassium hydroxide, hydroxyethyl second diamino or tetramethyl-hydrogen ammonia, the scope 1-11 of pH value;
Described aqueous medium is a deionized water.
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component:
Oxycompound polishing particles 0.2-6wt%
Oxygenant 1-4wt%
Tensio-active agent 0.05-2wt%
Organic additive 0.05-1wt%
All the other wt% of pH regulator agent and aqueous medium.
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: 30wt% cerium oxide particle, 0.01wt% hydrogen peroxide, 4wt% sodium polyacrylate, 0.3wt% proline(Pro), nitre acid for adjusting pH value are 3, and all the other are deionized water; The particle diameter of described cerium oxide particle is 10nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: 2wt% titan oxide particles, the 1.5wt% Tripotassium iron hexacyanide, 0.5wt% polyoxyethylene sodium sulfate, 0.2wt% citric acid, phosphorus acid for adjusting pH value are 5, and all the other are deionized water; The particle diameter of described cerium oxide particle is 150nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: it is 11 that 4wt% alumina particle, 3wt% ammonium persulphate, 0.5wt% polyoxyethylene sodium sulfate, 1wt% Whitfield's ointment, potassium hydroxide are regulated the pH value, and all the other are deionized water; The particle diameter of described alumina particle is 80nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: 3wt% zirconia particles, 2wt% hydrogen peroxide, 0.3wt% polyoxyethylene ether phosphate, 0.1wt% Padil, phosphorus acid for adjusting pH value are 1, and all the other are deionized water; The particle diameter of described zirconia particles is 100nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: it is 3 that 1wt% silicon oxide particle, 1wt% cross the Tripotassium iron hexacyanide, 0.3wt% polyoxyethylene ether phosphate, 0.3wt% oxalic acid, nitre acid for adjusting pH value, and all the other are deionized water; The particle diameter of described silicon oxide particle is 200nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: 30wt% titan oxide particles, 0.5wt% ammonium persulphate, 0.01wt% sodium polyacrylate, 3wt% terephthalic acid, nitre acid for adjusting pH value are 4, and all the other are deionized water; The particle diameter of described titan oxide particles is 1500nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: 6wt% zirconia particles, the 4wt% Tripotassium iron hexacyanide, 0.5wt% polyoxyethylene sodium sulfate, 0.3wt% Succinic Acid, nitre acid for adjusting pH value are 2, and all the other are deionized water; The particle diameter of described zirconia particles is 30nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: it is 10 that 5wt% alumina particle, 5wt% hydrogen peroxide, 1wt% sodium polyacrylate, 0.01wt% acetate, tetramethyl-hydrogen ammonia are regulated the pH value, and all the other are deionized water; The particle diameter of described alumina particle is 1000nm;
Described SiSb based phase-change material chemical mechanical polishing liquid comprises following component: it is 9 that 5wt% cerium oxide particle, 3wt% hydrogen peroxide, 0.3wt% polyoxyethylene ether phosphate, 2wt% formic acid, hydroxyethyl second diamino are regulated the pH value, and all the other are deionized water; The particle diameter of described cerium oxide particle is 60nm.
SiSb based phase-change material of the present invention is applied to the polishing of SiSb based phase-change material with chemical mechanical polishing liquid.Described SiSb based phase-change material, its chemical general formula are Si
xSb
100-x, 0＜x＜100 wherein, preferred 5≤x≤20.
In polishing process, the polishing particles general action is can be crosslinked with polished materials chemistry, removes cross-linking products by self hardness and extraneous mechanical force then and is taken away by liquid.This process moves in circles, thereby has guaranteed carrying out continuously of polishing process.The oxide cmp particle of widespread use at present has titanium oxide, cerium oxide, colloidal silica, zirconium white, aluminum oxide etc., and their Mohs' hardness is followed successively by 5～6,7,7,8.5,9.Select for use soft titanium oxide of matter and cerium oxide to polish, the physical removal effect is weak and chemically reactive is strong, mainly removes based on chemical solution in the polishing process, can realize SiSb based phase-change material low rate, surface quality is good and the low polishing that damages; Select for use the hard aluminum oxide of matter, zirconium white and silicon oxide to polish, in the polishing process chemical action a little less than, mainly based on the machinery removal, can realize polishing to SiSb based phase-change material two-forty.By selecting different oxide cmp particles for use, can realize phase change material Si
xSb
100-xSpeed is controlled, surface quality good and the polishing of low damage.
For medal polish, the process that It is generally accepted is that burning forms the soft aquation zone of oxidation of matter, and zone of oxidation is removed by machinery then, exposes fresh metal again.So process is reciprocal, thereby realizes carrying out continuously of polishing process.For the SiSb based phase-change material, Si and Sb all have certain metallicity.Therefore, in the polishing process of SiSb based phase-change material, oxygenant has important role continuously for polishing process.
The present invention has added tensio-active agent in chemical mechanical polishing liquid, with its its specific structure and certain charged situation, can improve the stability of polishing fluid, thereby be beneficial to the chemically machinery polished of SiSb based phase-change material.
In using the polishing process of oxide cmp particle to the SiSb based phase-change material, after oxidized dose of Si and Sb were oxidized to high valence state, the outer empty p track of Si and Sb can form back donating bonding with the lone electron pair in the organic additive.Further removal after this coordination can promote Si and Sb oxidized, thus whole polishing process influenced.Different organic additives, different with the situation of band lone electron pair because of its space structure, organic additive can promote or inhibition this coordination.By adding different organic additives, can control above-mentioned polishing process, thereby it is controlled to reach polishing process speed, realize needed removal speed in the polishing process.
PH value conditioning agent helps stablizing polishing fluid, and makes polishing effect better.
Beneficial effect
By chemical mechanical polishing pulp provided by the invention, the polishing speed of SiSb based phase-change material can be controlled in 5～2000nm/min, surfaceness has been reduced to below the 0.7nm simultaneously, utilize that this polishing fluid is controlled to SiSb based phase-change material speed, surface quality good and the polishing of low damage, can satisfy the needs of CMP technology in the preparation sodium electronic phase-variable memory.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment
Si
xSb
100-xThe polishing test
(1) instrument: CMP tester (CETR CP-4)
(2) condition: pressure (Down Force): 3psi
Polishing pad rotating speed (Pad Speed): 100rpm
Rubbing head rotating speed (Carrier Speed): 100rpm
Temperature: 25 ℃
Polishing fluid flow velocity (Feed Rate): 100ml/min
(3) polishing fluid: the polishing fluid of getting the embodiment gained is tested.
The CP-4 polishing machine that adopts U.S. CE TR company is to Si
xSb
100-xAfter polishing, utilize AFM atomic force microscope test Si
xSb
100-xThe roughness RMS (Root Mean Square) in surface 2 μ m * 2 μ m zones.
Embodiment 1
Polishing fluid (weight part) composed as follows:
Cerium oxide particle content (particle diameter 10nm): 30wt%;
Hydrogen peroxide: 0.01wt%;
Sodium polyacrylate: 4wt%;
Proline(Pro): 0.3wt%;
PH value (nitric acid accent): 3;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 2
Polishing fluid (weight part) composed as follows:
Titan oxide particles content (particle diameter 150nm): 2wt%;
The Tripotassium iron hexacyanide: 1.5wt%;
Polyoxyethylene sodium sulfate: 0.5wt%;
Citric acid: 0.2wt%;
PH value (phosphoric acid accent): 5;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 3
Polishing fluid (weight part) composed as follows:
Alumina particle content (particle diameter 80nm): 4wt%;
Ammonium persulphate: 3wt%;
Polyoxyethylene sodium sulfate: 0.5wt%;
Whitfield's ointment: 1wt%;
PH value (potassium hydroxide accent): 11;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 4
Polishing fluid (weight part) composed as follows:
Zirconia particles content (particle diameter 100nm): 3wt%
Hydrogen peroxide: 2wt%;
Polyoxyethylene ether phosphate: 0.3wt%;
Padil: 0.1wt%;
PH value (phosphoric acid accent): 1;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 5
Polishing fluid (weight part) composed as follows:
Titan oxide particles content (particle diameter 1500nm): 30wt%;
Ammonium persulphate: 0.5wt%;
Sodium polyacrylate: 0.01wt%;
Terephthalic acid: 3wt%;
PH value (nitric acid accent): 4;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 6
Polishing fluid (weight part) composed as follows:
Silicon oxide particle content (particle diameter 200nm): 1wt%;
The Tripotassium iron hexacyanide: 1wt%;
Polyoxyethylene ether phosphate: 0.3wt%;
Oxalic acid: 0.3wt%;
PH value (phosphoric acid accent): 3;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 7
Polishing fluid (weight part) composed as follows:
Zirconia particles content (particle diameter 30nm): 6wt%,
The Tripotassium iron hexacyanide: 4wt%;
Polyoxyethylene sodium sulfate: 0.5wt%;
Succinic Acid: 0.3wt%;
PH value (nitric acid accent): 2;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 8
Polishing fluid (weight part) composed as follows:
Alumina particle content (particle diameter 1000nm): 5wt%,
Hydrogen peroxide: 5wt%;
Sodium polyacrylate: 1wt%;
Acetate: 0.01wt%;
PH value (tetramethyl-hydrogen ammonia accent): 10;
All the other are deionized water.
The polishing test result is as shown in table 1.
Embodiment 9
Polishing fluid (weight part) composed as follows:
Cerium oxide particle content (particle diameter 60nm): 5wt%,
Hydrogen peroxide: 3wt%;
Polyoxyethylene ether phosphate: 0.3wt%;
Formic acid: 2wt%;
PH value (hydroxyethyl second diamino accent): 9;
All the other are deionized water.
The polishing test result is as shown in table 1.
Table 1
As shown in Table 1, chemical mechanical polishing pulp provided by the invention can be controlled in 5nm/min to 2000nm/min to the polishing speed of SiSb based phase-change material, and surfaceness has been reduced to below the 0.7nm simultaneously.
Utilize above-mentioned polishing fluid to phase change material Si
xSb
100-xSpeed is controlled, the polishing of surface low damnification and noresidue, can satisfy the needs of CMP technology in the preparation sodium electronic phase-variable memory.
Claims (7)
1. SiSb based phase-change material chemical mechanical polishing liquid comprises following component:
Oxycompound polishing particles 0.2-30wt%
Oxygenant 0.01-5wt%
Tensio-active agent 0.01-4wt%
Organic additive 0.01-3wt%
All the other wt% of pH regulator agent and aqueous medium;
Described oxycompound polishing particles is aluminum oxide, cerium oxide, zirconium white, titanium oxide or colloidal silica, particle size range 10-1500nm;
Described oxygenant is the Tripotassium iron hexacyanide, hydrogen peroxide or ammonium persulphate;
Described tensio-active agent is polyoxyethylene sodium sulfate AES, sodium polyacrylate, polyoxyethylene ether phosphate, alkyl alcohol polyoxyethylene groups ether or cetyl trimethylammonium bromide;
Described organic additive is acetate, formic acid, oxalic acid, citric acid, terephthalic acid, Whitfield's ointment, proline(Pro), Padil, Succinic Acid or tartrate;
Described pH regulator agent is nitric acid, phosphoric acid, potassium hydroxide, hydroxyethyl second diamino or tetramethyl-hydrogen ammonia, the scope 1-11 of pH value;
Described aqueous medium is a deionized water.
2. described a kind of SiSb based phase-change material chemical mechanical polishing liquid according to claim 1, it is characterized in that: described SiSb based phase-change material chemical mechanical polishing liquid comprises following component:
Oxycompound polishing particles 0.2-6wt%
Oxygenant 1-4wt%
Tensio-active agent 0.05-2wt%
Organic additive 0.05-1wt%
All the other wt% of pH regulator agent and aqueous medium;
The particle size range of described oxycompound polishing particles is 30-200nm.
3. described a kind of SiSb based phase-change material chemical mechanical polishing liquid according to claim 1, it is characterized in that: described SiSb based phase-change material chemical mechanical polishing liquid, comprise following component: 30wt% cerium oxide particle, 0.01wt% hydrogen peroxide, 4wt% sodium polyacrylate, 0.3wt% proline(Pro), nitre acid for adjusting pH value are 3, and all the other are deionized water; The particle diameter of described cerium oxide particle is 10nm.
4. described a kind of SiSb based phase-change material chemical mechanical polishing liquid according to claim 1, it is characterized in that: described SiSb based phase-change material chemical mechanical polishing liquid, comprise following component: 2wt% titan oxide particles, the 1.5wt% Tripotassium iron hexacyanide, 0.5wt% polyoxyethylene sodium sulfate, 0.2wt% citric acid, phosphorus acid for adjusting pH value are 5, and all the other are deionized water; The particle diameter of described cerium oxide particle is 150nm.
5. described a kind of SiSb based phase-change material chemical mechanical polishing liquid according to claim 1, it is characterized in that: described SiSb based phase-change material chemical mechanical polishing liquid, comprise following component: it is 11 that 4wt% alumina particle, 3wt% ammonium persulphate, 0.5wt% polyoxyethylene sodium sulfate, 1wt% Whitfield's ointment, potassium hydroxide are regulated the pH value, and all the other are deionized water; The particle diameter of described alumina particle is 80nm.
6. described a kind of SiSb based phase-change material chemical mechanical polishing liquid according to claim 1, it is characterized in that: described SiSb based phase-change material chemical mechanical polishing liquid, comprise following component: 3wt% zirconia particles, 2wt% hydrogen peroxide, 0.3wt% polyoxyethylene ether phosphate, 0.1wt% Padil, phosphorus acid for adjusting pH value are 1, and all the other are deionized water; The particle diameter of described zirconia particles is 100nm.
7. described a kind of SiSb based phase-change material chemical mechanical polishing liquid according to claim 1, it is characterized in that: described SiSb based phase-change material chemical mechanical polishing liquid, comprise following component: it is 3 that 1wt% silicon oxide particle, 1wt% cross the Tripotassium iron hexacyanide, 0.3wt% polyoxyethylene ether phosphate, 0.3wt% oxalic acid, nitre acid for adjusting pH value, and all the other are deionized water; The particle diameter of described silicon oxide particle is 200nm.
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| CN104017501A (en) * | 2014-06-12 | 2014-09-03 | 江南大学 | Ultrasonic atomization-type polishing solution suitable for TFT-LCD (Thin Film Transistor-Liquid Crystal Display) glass substrate |
| CN104593776A (en) * | 2014-12-24 | 2015-05-06 | 上海新安纳电子科技有限公司 | Chemical mechanical polishing liquid for titanium |
| CN104593776B (en) * | 2014-12-24 | 2017-11-03 | 上海新安纳电子科技有限公司 | A kind of chemical mechanical polishing liquid for titanium |
| CN109986456A (en) * | 2017-12-29 | 2019-07-09 | 长鑫存储技术有限公司 | The preparation method of chemical and mechanical grinding method, system and metal plug |
| CN109986456B (en) * | 2017-12-29 | 2020-11-03 | 长鑫存储技术有限公司 | Chemical mechanical polishing method and system and preparation method of metal plug |
| CN111004581A (en) * | 2019-12-16 | 2020-04-14 | 天津理工大学 | Chemical mechanical polishing solution for phase-change material composite abrasive and application thereof |
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