CN102408836A - Nanometer polishing solution for titanium oxide film chemical mechanical planarization and application - Google Patents
Nanometer polishing solution for titanium oxide film chemical mechanical planarization and application Download PDFInfo
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- CN102408836A CN102408836A CN2011103202957A CN201110320295A CN102408836A CN 102408836 A CN102408836 A CN 102408836A CN 2011103202957 A CN2011103202957 A CN 2011103202957A CN 201110320295 A CN201110320295 A CN 201110320295A CN 102408836 A CN102408836 A CN 102408836A
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Abstract
A nanometer polishing solution for titanium oxide film chemical mechanical planarization is formed by mixing a nanometer abrasive, a pH adjusting agent, a surfactant, a defoamer, a bactericide, an assistant cleaning agent, and a solvent, wherein the nanometer abrasive is cerium oxide or silica; the pH adjusting agent is a composite pH adjusting agent composed of an inorganic pH adjusting agent and an organic pH adjusting agent; the surfactant comprises silane polyglycol ether, polyglycol ether or dodecyl glycol ether; the defoamer is polydimethylsilane; the bactericide is isomeric thiazolinone; the assistant cleaning agent is isopropanol; and the solvent is deionized water; the nanometer polishing solution is applicable to the preparation of resistive random access memories based on titanium oxide film materials. The advantages of the invention are that: the polishing speed is stable and controllable; the film has less surface damage, is easy to clean, does not cause environment pollution, and has long storage time. When the polishing solution is used to perform chemical mechanical planarization of a resistive random material of a titanium oxide film material so as to prepare a resistive random access memory, the method is simple and practical, and is completely compatible with integrated circuit technology.
Description
Technical field
The present invention relates to microelectronics subsidiary material and technology field, particularly a kind of nanometer burnishing liquid and application that is used for the thin film of titanium oxide chemical-mechanical planarization.
Background technology
Along with microelectronics and computer technology rapid development, more and more urgent to the demand of jumbo nonvolatile storer.And based on quickflashing (flash) storer of FGS floating gate structure because the unlimited problem such as attenuate of higher operating voltage, complicated circuitry structure and FGS floating gate structure, what seriously restricted flash memory further is applied to every field.Particularly work as and make that owing to can't further improving integration density the demand of seeking the alternative flash memory of novel storer is more urgent after the technology node gets into 45nm.Various non-volatility memorizers in being based on the new theory novel material arise at the historic moment, and the resistance-type memory (being resistance-variable storing device) that utilizes electric current to send a telegraph the exploitation of resistance transition effect is exactly one of them.Resistance-variable storing device (Resistive Random Access Memory; RRAM) be a kind of novel non-volatility memorizer; It has that operating voltage is low, read or write speed is fast, the repeatable operation weather resistance is strong, storage density is high, data hold time is long, low in energy consumption, cost is low, and characteristics such as CMOS process compatible, is described as the strongest rival of non-volatility memorizer of future generation.The critical material of resistance-variable storing device is recordable transition metal oxide film material; The titania meterial that wherein has resistance change characteristic enjoys the concern of all circles, (the Appl. Phys. Lett. 95,093508 of the Seoul National University of Korea S; 2009), (the Appl. Phys. Lett. 93 of Chinese Zhongshan University; 043502,2008), (the Appl. Phys. Lett. 92,043510 of Tokyo Univ Japan; 2008), (the Thin Solid Films 516 of Asia university; 2008,8693 – 8696), HP Lab etc. all makes The Research of Relevant Technology carrying out titanium oxide resistance change nature and resistance-change memory device thereof, visible resistance-variable storing device based on titanium oxide will will have good application prospects in the resistance-variable storing device devices field.But the method for existing various growth titanium oxide such as: the thin film of titanium oxide of growths such as sputter, pulsed laser deposition, low-pressure chemical vapor deposition, electron beam evaporation, ald, sol-gel all has very big surfaceness and surface to contain needle pore defect; These all will have a strong impact on the growth of subsequent thin film, thereby badly influence the performance that whole resistance becomes device.Especially after the technology node gets into 40nm,, thereby the manufacturing and the application of thin film of titanium oxide and related device thereof have seriously been restricted because the bigger roughness of titania surface that grows out has limited the realization of high-precision photoetching.So the growth thin film of titanium oxide must pass through flattening surface and just can be applied in the actual device manufacturing and go to reduce its surfaceness.Make gordian technique based on the resistance-variable storing device of thin film of titanium oxide material in addition and be how to form the pattern structure that resistance becomes material, and then form storage unit.In conjunction with chemical-mechanical planarization in the device interconnection extensive applications; The resistance-variable storing device how to make based on titanium oxide through the chemical-mechanical planarization of titanium oxide becomes current research focus, and the chemical-mechanical planarization work of relevant titanium oxide also becomes one of the focus in this field.
At present; Chemical-mechanical planarization (Chemical Mechanical Planarization; CMP) as unique a kind of technology that can realize overall planarization; Become a kind of indispensable technology in the VLSI technology, and be widely used in the middle of the mutual system of deep-submicron multiple layer of copper.ITRS (International Technology Roadmap for Semiconductors; ITRS) proposed in 2007; The research work utmost point of chemical-mechanical planarization that is used for the novel material of non-volatility memorizer need carry out, and the formation of deep groove structure and the removal of excess stock all need chemical-mechanical planarization to accomplish.
For improving constantly storage density, voltage, power consumption when reducing resistance and becoming require that characteristic dimension is contracted to nano level in the resistance-variable storing device device cell.In view of the technology below 0.25 micron in the semiconductor technology, material surface must carry out overall planarization through chemical-mechanical planarization, can utilize general photolithographic exposure technology to carry out the processing of submicron-scale.Secondly, through chemical-mechanical planarization, can improve the planeness of film; Increase the contact area between interface, the interface that reduces between electrode and the resistance variation film is caught current density, and then improves the electrical characteristic and the fatigue resistence of resistance variation film material; Reduce defective simultaneously, the safety of enhance device.And, for the resistance-variable storing device device preparing process is compatible mutually with CMOS technology,, need study this critical process of chemical-mechanical planarization of resistance change material so that cost of manufacture is minimum.The resistance-variable storing device device unit construction relates to the formation of nanostructure, comprises the formation of nanoporous, the chemical-mechanical planarization of nano-filled and excess stock.For forming interstitital texture, can only become the filling and the chemical-mechanical planarization formation device cell of material through resistance.Document through consulting domestic and international patent, the mechanical polishing of the relevant resistance change of document material oxidation titanizing does not appear in the newspapers.And because the component of polishing fluid has very large influence to the practicality and the surface of polished quality of polishing, the component of therefore studying polishing fluid has not only determined the quality of polishing also to determine the efficient of polishing.Can foresee carrying out of resistance-change memory material oxidation titanium film chemical machinery planarization and will possibility be provided for the further high-performance of resistance-variable storing device device, low-cost development.
Because the necessary overall planarization of Deep Submicron IC process materials; Chemical-mechanical planarization research for the resistance-change memory thin-film material; To become the bottleneck technology of more high-performance resistance-variable storing device development of future generation; Have only the height of having realized material surface smooth, just can carry out high-resolution photolithographic exposure and form the nanoscale features size, make that required voltage was lower when the storage material resistance became, power consumption is littler, volume-diminished, storage density increase, cost reduces.Therefore the research of RRAM resistance variation film material not only has bigger scientific meaning, and has the huge commercial value of potential.
Summary of the invention
The objective of the invention is to above-mentioned technical Analysis and existing problems; A kind of nanometer burnishing liquid and application that is used for the thin film of titanium oxide chemical-mechanical planarization is provided; Adopt this nanometer burnishing liquid; Can realize hindering the overall planarization that becomes material oxidation titanium transition metal oxide resistance variation film material, satisfy the requirement of preparation high-performance resistance-variable storing device, have good application prospects.
Technical scheme of the present invention:
A kind of nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization; By nano-abrasive, pH regulator agent, tensio-active agent, skimmer, sterilant, help clean-out system and solvent to form, the weight percent of each component is: nano-abrasive be 1.0-30.0wt%, pH regulator agent add-on be make that nanometer burnishing liquid pH value is 3 ~ 12, tensio-active agent is that 0.01-1.0wt%, skimmer are that 20-200ppm, sterilant are 10-50ppm, to help clean-out system be that 0.01-0.1wt%, surplus are solvent.
Said nano-abrasive is the mixture of one or both arbitrary proportions in cerium oxide and the silicon-dioxide, and wherein cerium oxide is its water dispersion, and silicon-dioxide is colloidal solution; The median size of nano-abrasive is less than 200nm.
Said pH regulator agent is the compound pH regulator agent of being made up of inorganic pH regulator agent and organic pH regulator agent, and wherein inorganic pH regulator agent is KOH, HNO
3Or H
2SO
4, organic pH regulator agent is the mixture for one or both arbitrary proportions in TMAH, tetraethyl ammonium hydroxide, oxyamine, acetic acid, sulfonic acid and the Hydrocerol A; The ratio of inorganic pH regulator agent and organic pH regulator agent is 1:1-8.
Said tensio-active agent is that silane gathers the diethyl alcohol ether, gathers the mixture of one or both arbitrary proportions in diethyl alcohol ether and the dodecyl glycol ether.
Said skimmer is a polydimethyl silane.
Said sterilant is the isomery thiazolinone.
The said clean-out system that helps is a Virahol.
Said solvent is a deionized water.
A kind of said application that is used for the nanometer burnishing liquid of thin film of titanium oxide chemical-mechanical planarization is used for the preparation based on the resistance-variable storing device of thin film of titanium oxide material, and step is following:
1) at substrate Si/SiO
2Last deposition lower conducting dome deposits SiO on lower conducting dome
2Medium layer is to SiO
2Medium layer carries out the perforate etching, and the deposition resistance becomes material oxidation titanium resistance variation film material then, fills and covers all array holes;
2), utilize described nanometer burnishing liquid that unnecessary titanium oxide resistance variation film material layer is removed and planarization through chemical-mechanical planarization;
3) the deposition top electrode promptly can be made into the resistance-variable storing device based on the nickel oxide film material behind the lead-in wire.
Technical Analysis of the present invention:
Mechanical friction when the main effect of abrasive is CMP.The pH regulator agent mainly is the pH value of regulating polishing fluid, makes polishing fluid stable, helps the carrying out of CMP; Select for use compound acid or alkali as the pH regulator agent, mineral alkali KOH or mineral acid HNO
3Can strengthen the chemical action of polishing fluid, organic bases or organic acid can be good at keeping the pH value stabilization of solution, guarantee that the consistent of chemical action stablize, thereby realize the stable of polishing speed.Influence of surfactant is to make the high stability of abrasive in the polishing fluid to be preferentially adsorbed on material surface in the CMP process that the chemical corrosion effect reduces; Because it is little that recess receives frictional force; Thereby protruding place is bigger than recess polishing speed, has played and has improved polishing convex-concave selectivity, has strengthened and has just selected ratio; Reduce surface tension, reduced surface disturbance.The adding of tensio-active agent causes foamy to produce usually in the polishing fluid, and unfavorable control with explained hereafter realizes low bubble or still polishing fluid through adding the minute quantity skimmer, is convenient to manipulate.Contain many organism in the polishing fluid, long-term storage forms mould easily, causes polishing fluid rotten, in polishing fluid, adds a small amount of sterilant for this reason.Help the adding of clean-out system to help to reduce particulate absorption, reduce the cleaning cost in later stage.
Advantage of the present invention is: polishing speed stable and controllable, coating surface disturbance be few, be prone to clean, free from environmental pollution, the storage time is long.Through adopting nanometer burnishing liquid provided by the invention, can realize hindering the overall planarization that becomes material oxidation titanium resistance variation film material, the roughness RMS of surface of polished (5 μ m * 5 μ m) satisfies the requirement of preparation high-performance RRAM less than 1.0nm.Utilize this polishing fluid that resistance change material oxidation titanium thin-film material is carried out chemical-mechanical planarization and prepare resistance-variable storing device, method is simple, and compatible fully with integrated circuit technology.
Description of drawings
Fig. 1 is for to have the SiO of array hole
2Last deposition titanium oxide polishing structures of samples synoptic diagram.
Fig. 2 is to structural representation behind the resistance change material oxidation titanium redundance CMP.
Fig. 3 is the resistance variation memory structure synoptic diagram.
Fig. 4 is the preceding AFM figure of thin film of titanium oxide polishing.
Fig. 5 is thin film of titanium oxide polishing back AFM figure.
Embodiment
Further illustrate substantive distinguishing features of the present invention and marked improvement through following examples.But the present invention only is confined to embodiment by no means.
Embodiment 1:
A kind of nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization is by nano-abrasive, pH regulator agent, tensio-active agent, skimmer, sterilant, help clean-out system and solvent to form.
The preparation of nanometer burnishing liquid: the silicon dioxide colloid 20wt% that contains 10 ~ 30nm in the polishing fluid; Dodecyl glycol ether 0.2wt%; Polydimethyl silane 50ppm; Isomery thiazolinone 10ppm; Virahol 0.03wt%; KOH and TMAH (volume ratio is 1:1) are the pH regulator agent, and pH is 8, and all the other are deionized water.During preparation above-mentioned raw materials is mixed direct computer experiment after the use magnetic stirrer stirs.
The realization of glossing: adopt the 6EC nSpire polishing machine of U.S. Strasbaugh, polishing pad is Rohm&Haas IC1000, and the rubbing head rotating speed is that 35rpm and polishing disk rotating speed are 40rpm, polishing fluid flow velocity 100ml/min, and overdraft is 2psi.
The specimen preparation of polishing is following: 1) at substrate Si/SiO
2The lower conducting dome W layer of last deposit thickness 100nm; 2) the medium layer SiO of deposit thickness 200nm on lower conducting dome W layer
23) pass through photoetching process to SiO
2Layer etching, the array hole of formation 1000nm; 4) at the SiO that is with array hole
2Last deposition titanium oxide resistance variation film material is filled and is covered all array holes.Fig. 1 is this polishing structures of samples synoptic diagram.
The polishing effect test: the resistance that has Dektak 150 contourgraphs to measure the polishing front and back becomes the thickness difference of material oxidation titanium film; Divided by the speed that polishing time just can obtain polishing, measure surface topography and the roughness that the resistance of polishing front and back becomes material oxidation titanium film with the AFM (AFM) of Agilent company.Fig. 4 is the preceding AFM figure of thin film of titanium oxide polishing, and Fig. 5 is thin film of titanium oxide polishing back AFM figure.
Polishing effect: resistance becomes material oxidation titanium polishing speed 52nm/min, SiO
2Polishing speed 12nm/min, polishing front surface roughness RMS (5 μ m * 5 μ m) is 8.7nm, surface of polished roughness RMS (5 μ m * 5 μ m) is 0.9nm, TiO
2/ SiO
2Select than being 4.3:1.Fig. 2 is to structural representation behind the resistance change material oxidation titanium redundance CMP.
Embodiment 2:
A kind of nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization is by nano-abrasive, pH regulator agent, tensio-active agent, skimmer, sterilant, help clean-out system and solvent to form.
The preparation of nanometer burnishing liquid: contain the silicon dioxide colloid 5wt% of 10 ~ 30nm in the polishing fluid, the cerium oxide 4wt% of 40nm; Gather diethyl alcohol ether 0.1wt%, dodecyl glycol ether 0.1wt%; Polydimethyl silane 50ppm; Isomery thiazolinone 10ppm; Virahol 0.03wt%; KOH and azanol (volume ratio is 1:3) are the pH regulator agent, and pH is 9.01, and all the other are deionized water.During preparation above-mentioned raw materials is mixed direct computer experiment after the use magnetic stirrer stirs.
Glossing, polishing specimen preparation and polishing effect test are with embodiment 1.
Polishing effect: resistance becomes material oxidation titanium polishing speed 124nm/min, SiO
2Polishing speed 12.3nm/min, polishing front surface roughness RMS (5 μ m * 5 μ m) is 12.4nm, surface of polished roughness RMS (5 μ m * 5 μ m) is 0.63nm, TiO
2/ SiO
2Select than being 10:1.
Embodiment 3:
A kind of nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization is by nano-abrasive, pH regulator agent, tensio-active agent, skimmer, sterilant, help clean-out system and solvent to form.
The preparation of nanometer burnishing liquid: contain the silicon dioxide colloid 5wt% of 10 ~ 30nm in the polishing fluid, the cerium dioxide 2wt% of 80nm; Gather diethyl alcohol ether 0.3wt%; Polydimethyl silane 50ppm; Isomery thiazolinone 10ppm; Virahol 0.03wt%; H
2SO
4And acetic acid (volume ratio is 1:3) is the pH regulator agent, and pH is 6.02, and all the other are deionized water.During preparation above-mentioned raw materials is mixed direct computer experiment after the use magnetic stirrer stirs.
Glossing, polishing specimen preparation and polishing effect test are with embodiment 1.
Polishing effect: resistance becomes material oxidation titanium polishing speed 149.8nm/min, SiO
2Polishing speed 7nm/min, polishing front surface roughness RMS (5 μ m * 5 μ m) is 13.7nm, surface of polished roughness RMS (5 μ m * 5 μ m) is 0.45nm, TiO
2/ SiO
2Select than being 21.4:1.
Embodiment 4:
A kind of nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization is by nano-abrasive, pH regulator agent, tensio-active agent, skimmer, sterilant, help clean-out system and solvent to form.
The preparation of nanometer burnishing liquid: the cerium dioxide 5wt% that contains 80nm in the polishing fluid; Silane gathers diethyl alcohol ether 0.5wt%; Polydimethyl silane 50ppm; Isomery thiazolinone 10ppm; Virahol 0.03wt%; H
2SO
4And sulfonic acid (volume ratio is 1:2) is the pH regulator agent, and pH is 5.01, and all the other are deionized water.During preparation above-mentioned raw materials is mixed direct computer experiment after the use magnetic stirrer stirs.
Glossing, polishing specimen preparation and polishing effect test are with embodiment 1.
Polishing effect: resistance becomes material oxidation titanium polishing speed 196nm/min, SiO
2Polishing speed 5nm/min, polishing front surface roughness RMS is 9.8nm, surface of polished roughness RMS (5 μ m * 5 μ m) is 0.78nm, TiO
2/ SiO
2Select than being 39.2:1.
Embodiment 5:
A kind of preparation of the resistance-variable storing device based on the nickel oxide film material, step is following:
1) at the Si/SiO of substrate flat-satin
2The thick lower conducting dome W of last deposition 100nm, the thick SiO of deposition 200nm on lower conducting dome
2Medium layer, the technology of utilizing reactive ion etching is to SiO
2Medium layer carries out the perforate etching, having carved the deposition resistance change material oxidation titanium resistance variation film material on the array that sinks to the bottom in hole, it is filled cover all array holes then;
2) sample that has deposited resistance change material oxidation titanium film is carried out chemical-mechanical planarization, utilize nanometer burnishing liquid provided by the invention that unnecessary titanium oxide resistance variation film material layer is removed and planarization;
3) sample surfaces after polishing gets final product at the top electrode W of deposition one deck 100nm.
Fig. 3 is this resistance-change memory structural representation.
Through adopting nanometer burnishing liquid provided by the invention, can realize the overall planarization of titanium oxide resistance variation film material, the roughness RMS of surface of polished (5 μ m * 5 μ m) satisfies the requirement of preparation high-performance RRAM less than 1.0nm.Utilize this polishing fluid that resistance change material oxidation titanium thin-film material is carried out chemical-mechanical planarization and prepare resistance-variable storing device, method is simple, and compatible fully with integrated circuit technology.
Claims (9)
1. nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization; It is characterized in that: by nano-abrasive, pH regulator agent, tensio-active agent, skimmer, sterilant, help clean-out system and solvent to form, the weight percent of each component is: nano-abrasive be 1.0-30.0wt%, pH regulator agent add-on be make that nanometer burnishing liquid pH value is 3 ~ 12, tensio-active agent is that 0.01-1.0wt%, skimmer are that 20-200ppm, sterilant are 10-50ppm, to help clean-out system be that 0.01-0.1wt%, surplus are solvent.
2. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1; It is characterized in that: said nano-abrasive is the mixture of one or both arbitrary proportions in cerium oxide and the silicon-dioxide; Wherein cerium oxide is its water dispersion, and silicon-dioxide is colloidal solution; The median size of nano-abrasive is less than 200nm.
3. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1, it is characterized in that: the compound pH regulator agent of said pH regulator agent for being made up of inorganic pH regulator agent and organic pH regulator agent, wherein inorganic pH regulator agent is KOH, HNO
3Or H
2SO
4, organic pH regulator agent is the mixture for one or both arbitrary proportions in TMAH, tetraethyl ammonium hydroxide, oxyamine, acetic acid, sulfonic acid and the Hydrocerol A; The ratio of inorganic pH regulator agent and organic pH regulator agent is 1:1-8.
4. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1, it is characterized in that: said tensio-active agent is that silane gathers the diethyl alcohol ether, gathers the mixture of one or both arbitrary proportions in diethyl alcohol ether and the dodecyl glycol ether.
5. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1, it is characterized in that: said skimmer is a polydimethyl silane.
6. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1, it is characterized in that: said sterilant is the isomery thiazolinone.
7. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1, it is characterized in that: the said clean-out system that helps is a Virahol.
8. according to the said nanometer burnishing liquid that is used for the thin film of titanium oxide chemical-mechanical planarization of claim 1, it is characterized in that: said solvent is a deionized water.
9. application that is used for the nanometer burnishing liquid of thin film of titanium oxide chemical-mechanical planarization according to claim 1 is characterized in that being used for the preparation based on the resistance-variable storing device of thin film of titanium oxide material, and step is following:
1) at substrate Si/SiO
2Last deposition lower conducting dome deposits SiO on lower conducting dome
2Medium layer is to SiO
2Medium layer carries out the perforate etching, and the deposition resistance becomes material oxidation titanium resistance variation film material then, fills and covers all array holes;
2), utilize described nanometer burnishing liquid that unnecessary titanium oxide resistance variation film material layer is removed and planarization through chemical-mechanical planarization;
3) the deposition top electrode promptly can be made into the resistance-variable storing device based on the nickel oxide film material behind the lead-in wire.
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| JP2018150520A (en) * | 2017-02-28 | 2018-09-27 | バーサム マテリアルズ ユーエス，リミティド ライアビリティ カンパニー | Chemical mechanical planarization of films comprising elemental silicon |
| CN114621683A (en) * | 2020-12-11 | 2022-06-14 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution and use method thereof |
| WO2022121822A1 (en) * | 2020-12-11 | 2022-06-16 | 安集微电子（上海）有限公司 | Chemical-mechanical polishing solution and method for using same |
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Application publication date: 20120411 |