CN103484025B - Self-stop GST (Ge2Sb2Te5) chemical mechanical polishing solution as well as preparation method and application thereof - Google Patents
Self-stop GST (Ge2Sb2Te5) chemical mechanical polishing solution as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the field of chemical mechanical polishing, in particular to a self-stop chemical mechanical polishing solution effectively applied to a phase-change material GST (Ge2Sb2Te5) as well as a preparation method and application of the self-stop chemical mechanical polishing solution. The self-stop chemical mechanical polishing solution is made from the following raw materials in parts by weight: 0.2-30 parts of polishing particles, 0.0001-5 parts of an organic protective agent, 0.01-5 parts of an oxidant, 0.01-4 parts of a surfactant, 85-95 parts of a water-based medium and a proper amount of a pH regulating agent; the pH value of the self-stop GST chemical mechanical polishing solution is 2-6. According to the self-stop chemical mechanical polishing solution which is applied to the phase-change material GST graph piece, the protective agent in the self-stop chemical mechanical polishing solution can be attached to the surface of the phase-change material GST when the phase-change material GST is lower than silicon oxide to form a protection film on the surface of the phase-change material GST so as to protect the phase-change material GST and avoid the formation of a butterfly-shaped pit.
Description
Technical field
The present invention relates to CMP art, particularly relate to a kind of can the self-stopping technology chemical mechanical polishing liquid being effectively applied to phase change material GST and its preparation method and application.
Background technology
Phase transition storage because having the at a high speed advantage such as readings, high erasable number of times, non-volatile, component size is little, low in energy consumption, anti-strong motion and radioprotective, and is thought the current flash memories of most possible replacement and become future memory main product and become the device of commercial product at first by international semiconductor employer's organization.
The ultimate principle of Phase change memory technology take chalcogenide compound as storage media, utilize electric energy (heat) to make material between crystalline state (low-resistance) and non-crystalline state (high resistant), mutually change write and the erasing of the information that realizes, the reading of information then realizes by the change of measuring resistance.Typical phase change material is chalcogenide alloy film, and the most ripe material is GeSbTe alloy.Storage unit comprises the pore defined by dielectric substance, and phase change material deposition is in pore, and phase change material is connection electrode on one end of pore.Electrode contact makes electric current be programmed to this unit by this passage generation joule heating, or reads the resistance states of this unit.
At present, when building phase-change memory cell, current way is: first by the method depositing phase change material of magnetron sputtering in the pore defined by dielectric substance, then pass through the method for reactive ion etching (RIE) or chemically machinery polished (CMP), the phase change material of thin empty top is removed.Compared to RIE, CMP because having surface low damnification and the advantage that can realize global planarizartion, the parent receiving many researchists and semiconductor company looks at.
For meeting the demand preparing CMP in sodium electronic phase-variable memory, needing controlled with no damage phase change material being removed, also wishing the loss reducing lower floor's insulating material as far as possible simultaneously.
Summary of the invention
The shortcoming of prior art in view of the above, the invention provides a kind of for phase change material Ge
2sb
2te
5(GST) self-stopping technology chemically machinery polished (CMP) liquid, for solving the problems of the prior art, described self-stopping technology chemical mechanical polishing liquid is mainly used in the polishing of GST pattern piece.Inventor herein finds a kind of organism protective material through extensive research, can form protective membrane on the surface of GST, at the height of GST lower than SiO
2time, be attached to the surface of GST, play the effect of protection GST.This provide protection reduces the height in butterfly hole, and controllable-rate, surface low damnification and the polishing of noresidue, the needs preparing CMP in sodium electronic phase-variable memory can be met.
For achieving the above object and other relevant objects, first aspect present invention provides a kind of self-stopping technology chemical mechanical polishing liquid, and its raw material by weight, comprises following component:
The scope of the pH value of described self-stopping technology chemical mechanical polishing liquid is 2-6.
Preferably, described self-stopping technology chemical mechanical polishing liquid, its raw material by weight, comprises following component:
The scope of the pH value of described self-stopping technology chemical mechanical polishing liquid is 2-6.
Those skilled in the art according to practical situation, can add qs pH adjuster, to reach required pH value.
Preferably, described pH adjusting agent is selected from one or more the combination in ammoniacal liquor, hydroxyethyl second two ammonia soln, aqueous nitric acid and aqueous hydrochloric acid.
Preferably, the particle diameter of described polishing particles is 80-120nm.
Preferred, described polishing particles is silicon dioxide gel.
Preferred further, the solvent of described silicon dioxide gel is water, and solid content is 25-35wt%.
Preferably, described organism protective material is selected from one or more the combination in Allyl thiourea (CAS No:109-57-9), thiazolidine thioketones (CAS No:2682-49-7), sulphosalicylic acid (CAS No:5965-83-3), carboxymethyl cellulose (CAS No:9004-32-4), Natvosol (CAS No:9004-62-0) and empgen BB (dodecyl-dimethyl amine second lactone) (CAS No:683-10-3).
The molecular-weight average of described carboxymethyl cellulose is 900-15000.
The molecular-weight average of described Natvosol is 540-31000.
Preferably, one or more the combination in described oxygenant chosen from Fe potassium cyanide, potassium permanganate, Periodic acid and hydrogen peroxide.
Preferred, the concentration of described hydrogen peroxide is about 30wt%.
Self-stopping technology chemical mechanical polishing liquid for phase change material GST pattern piece provided by the invention comprises oxygenant.For medal polish, the process that It is generally accepted is that burning forms the soft aquation zone of oxidation of matter, and then zone of oxidation is removed, and again exposes fresh metal.Process like this is reciprocal, thus realizes carrying out continuously of polishing process.For phase change film material GST, Sb and Te has metallicity clearly.Therefore, in the polishing process of phase change material GST, oxygenant carries out having extremely important effect continuously for polishing process.
Preferably, described tensio-active agent is aniorfic surfactant.
Preferred, described tensio-active agent is selected from one or more the combination in polyoxyethylenated alcohol sodium sulfate (Sodium Alcohol EtherSulphate, AES), sodium polyacrylate and aliphatic alcohol polyoxyvinethene phosphate.
Automatic stopping chemical mechanical polishing liquid in phase change material GST pattern piece provided by the invention comprises at least one tensio-active agent.Tensio-active agent, with its distinctive structure and certain charged situation, can improve the stability of polishing fluid, thus be beneficial to the chemically machinery polished of phase change material GST.
The molecular-weight average of described polyoxyethylenated alcohol sodium sulfate (AES) is 357-412.
The molecular-weight average of described sodium polyacrylate is 900-25000.
The molecular-weight average of described aliphatic alcohol polyoxyvinethene phosphate is 850-52000.
Preferably, described aqueous medium is water.
Preferred, described aqueous medium is deionized water.
Second aspect present invention provides the preparation method of described self-stopping technology chemical mechanical polishing liquid, comprises the steps:
1) by formula, oxygenant is added in aqueous medium, fully stir;
2) by formula, in step 1 gained mixture, add tensio-active agent, after fully stirring, use pH adjusting agent that the pH of mixed solution is adjusted to 2-6;
3) by formula, in step 2 gained mixture, add organic protective agent, fully stir;
4) by formula, in step 3 gained mixture, add polish abrasive, after fully stirring, namely obtain described self-stopping technology chemical mechanical polishing liquid.
Third aspect present invention provides the application of described self-stopping technology chemical mechanical polishing liquid in phase change material polishing field.
Provided by the invention for phase change material GST pattern piece self-stopping technology chemical mechanical polishing liquid; the organism protective material wherein contained can be attached to the surface of GST when the height of GST is lower than silicon oxide; a kind of protective membrane is formed on the surface of GST; play the effect of protection GST, thus avoid the formation in butterfly hole.
In GST pattern piece polishing process, due to GST/SiO
2there is certain Selection radio, to GST pattern piece polishing fluid general requirement: not only will have high polishing speed, also will have high Selection radio simultaneously.In polishing process, GST pattern piece polishing fluid owing to having high Selection radio, so when the cross section of polishing GST time, due to high selectivity, the speed of the removal speed of GST about silicon oxide far away, easily cause the formation that butterfly is cheated, this result has had a strong impact on the carrying out of next step technique.Inventor have developed a kind of GST acid polishing slurry of self-stopping technology, contains a kind of organism protective material in described polishing fluid, can be attached to the surface of GST in polishing process.Because this organism is easily removed, so this protective material does not have influence on the removal speed of GST.When throwing GST cross section, when the height of GST is lower than silicon oxide, organism can be attached to the surface of GST, plays the effect of protection GST, and this provide protection reduces the height in butterfly hole, i.e. the problem of so-called dishing, reaches self-stopping technology GST and remove.This protective material can not stick to the surface of GST simultaneously, just can remove by the process of cleaning the protective material being attached to GST surface.Oxygenant, tensio-active agent and aqueous medium is further comprises in this polishing fluid, reduce surfaceness simultaneously, the removal speed of GST reaches 200nm/min, and controllable-rate, surface low damnification, the needs preparing CMP in sodium electronic phase-variable memory can be met.
Accompanying drawing explanation
Fig. 1 is shown as GST pattern piece structure.
Fig. 2 is shown as the butterfly hole in GST pattern piece.
Fig. 3 is shown as GST pattern piece polishing process.
Fig. 4 is shown as the structure iron being polished to GST cross section.
Fig. 5 is shown as and does not add protectant polishing test result figure.
Fig. 6 is shown as and adds protectant polishing test result figure.
Element numbers explanation
1 SiO
2
2 GST
3 organism protective materials
4 polishing particles
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Notice, in the following example, the concrete processing unit that indicates or device all adopt conventional equipment in this area or device; All force value and scope all refer to absolute pressure.
In addition should be understood that the one or more method stepss mentioned in the present invention do not repel and can also to there is additive method step or can also insert additive method step before and after described combination step between these steps clearly mentioned, except as otherwise noted; Will also be understood that, the relation that is connected between the one or more equipment/devices mentioned in the present invention is not repelled and can also to be there are other equipment/devices or can also insert other equipment/devices before and after described clustered aggregates/device between these two equipment/devices clearly mentioned, except as otherwise noted.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
The invention provides a kind of for phase change material Ge
2sb
2te
5(GST) self-stopping technology chemically machinery polished (CMP) liquid, containing organism protective material in its polishing fluid, is mainly used in solving in the polishing process of GST pattern piece, due to the butterfly hole that high selectivity causes.As indicated with 1, this structural requirement GST is with SiO for the structure iron of the pattern piece of conventional GST
2have certain Selection radio, generally, the formation that high Selection radio easily causes butterfly to cheat in polishing process, as shown in Figure 2, causes defect to next step technique.For occurring that in GST pattern piece polishing process the problem that butterfly is cheated, inventor add a kind of organism protective material in polishing fluid, protective membrane can be formed on the surface of GST, at the height of GST lower than SiO
2time, be attached to the surface of GST, play the effect of protection GST, reach the removal automatically stopping GST, thus avoid the formation in butterfly hole.
Organism protective material of the present invention can be attached to the surface of GST in polishing process, and its polishing process as shown in Figure 3.From figure, we can find out in polishing process, and organism is attached to the surface of GST, because this organism is easily removed, so this protective material does not have influence on the removal speed of GST.When throwing GST cross section, when the height of GST is lower than silicon oxide, organism is attached to the surface of GST, plays the effect of protection GST, and this provide protection reduces the height in butterfly hole, i.e. the problem of so-called dishing.Its schematic diagram as shown in Figure 4.Can see in the process of polishing, when the height of GST is lower than SiO from figure
2height time, organism is attached to the surface of GST, protects the removal of GST, thus avoid butterfly hole formation.Reach self-stopping technology GST to remove.This protective material can not stick to the surface of GST simultaneously, just can remove by the process of cleaning the protective material being attached to GST surface.Oxygenant, tensio-active agent and aqueous medium is further comprises in this polishing fluid.Achieve controllable-rate simultaneously, reduce surfaceness.
In various embodiments of the present invention, GST pattern piece polishing test condition is as follows:
Instrument: CMP tester (CETR CP-4)
Condition: pressure (Down Force): 3psi
Polishing pad rotating speed (Pad Speed): 100rpm
Rubbing head rotating speed (Carrier Speed): 100rpm
Temperature: 25 DEG C
Polishing fluid flow velocity (Feed Rate): 100ml/min
Polishing fluid: the polishing fluid of Example gained is tested.
Embodiment 1
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (30wt%, particle diameter: 100nm): 2 parts;
Oxygenant: hydrogen peroxide (30wt%): 5 parts;
Tensio-active agent: polyoxyethylenated alcohol sodium sulfate: 1 part;
Organism protective material: 0 part;
Aqueous medium: deionized water: 92 parts;
PH value=3(10wt% aqueous nitric acid is adjusted).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding required hydrogen peroxide by formula in a reservoir; 3rd: the amount adding required polyoxyethylene sodium sulfate by formula in a reservoir; 4th: debug pH value to 3 with the dust technology of 10wt%, consumption is about 0.3 weight part; 5th: add by formula the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.
Polishing test result as shown in Figure 5.
Embodiment 2
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (30wt%, particle diameter: 100nm) content: 2 parts;
Oxygenant: hydrogen peroxide (30wt%): 5 parts;
Tensio-active agent: polyoxyethylenated alcohol sodium sulfate: 1 part
Organism protective material: carboxymethyl cellulose: 1 part;
Aqueous medium: deionized water: 91 parts;
PH value=3(10wt% diluted nitric acid aqueous solution is adjusted).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding required hydrogen peroxide by formula in a reservoir; 3rd: the amount adding required polyoxyethylene sodium sulfate by formula in a reservoir; 4th: debug pH value to 3 with the dust technology of a small amount of 10wt%; 5th: add carboxymethyl cellulose in a solvent by formula; 6th: add the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.
Polishing test result as shown in Figure 6.
From Fig. 5 with the contrast of Fig. 6, we can draw, do not add in GST polishing fluid organism protectant time, have the formation that butterfly is cheated after polishing; Polishing fluid after interpolation, does not have the formation that butterfly is cheated after polishing.Demonstrate in the process of polishing, organism protective material serves the effect of effective protection GST, thus avoids the formation in butterfly hole, reaches the effect of self-stopping technology.
Embodiment 3
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (30wt%, particle diameter: 120nm) content: 1 part;
Oxygenant: potassium permanganate: 0.1 part;
Tensio-active agent: sodium polyacrylate: 0.05 part
Organism protective material: Allyl thiourea: 0.01 part;
Aqueous medium: deionized water: 85 parts;
PH value=6(28wt% ammoniacal liquor is adjusted).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding required potassium permanganate by formula in a reservoir; 3rd: the amount adding required sodium polyacrylate by formula in a reservoir; 4th: by 28wt% ammoniacal liquor debugging pH value to 6; 5th: add Allyl thiourea in a solvent by formula; 6th: add the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.The polishing test result of the present embodiment gained polishing fluid is close with embodiment 2, effectively can protect GST, avoid the formation that butterfly is cheated.
Embodiment 4
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (30wt%, particle diameter: 80nm) content: 6 parts;
Oxygenant: Periodic acid: 4 parts;
Tensio-active agent: aliphatic alcohol polyoxyvinethene phosphate: 2 parts
Organism protective material: thiazolidine thioketones: 0.5 part;
Aqueous medium: deionized water: 95 parts;
PH value=2(10wt% aqueous hydrochloric acid is adjusted).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding required Periodic acid by formula in a reservoir; 3rd: the amount adding desired fats polyoxyethylenated alcohol phosphoric acid ester by formula in a reservoir; 4th: by 10wt% aqueous hydrochloric acid debugging pH value to 2; 5th: add thiazolidine thioketones in a solvent by formula; 6th: add the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.The polishing test result of the present embodiment gained polishing fluid is close with embodiment 2, effectively can protect GST, avoid the formation that butterfly is cheated.
Embodiment 5
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (25wt%, particle diameter: 80nm) content: 3 parts;
Oxygenant: the Tripotassium iron hexacyanide: 3 parts;
Tensio-active agent: aliphatic alcohol polyoxyvinethene phosphate: 1 part
Organism protective material: sulphosalicylic acid: 0.4 part;
Aqueous medium: deionized water: 90 parts;
PH value=5(10wt% hydroxyethyl diamine aqueous solution is adjusted).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding the required Tripotassium iron hexacyanide by formula in a reservoir; 3rd: the amount adding desired fats polyoxyethylenated alcohol phosphoric acid ester by formula in a reservoir; 4th: by 10wt% hydroxyethyl diamine aqueous solution debugging pH value to 5; 5th: add sulphosalicylic acid in a solvent by formula; 6th: add the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.The polishing test result of the present embodiment gained polishing fluid is close with embodiment 2, effectively can protect GST, avoid the formation that butterfly is cheated.
Embodiment 6
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (35wt%, particle diameter: 80nm) content: 3 parts;
Oxygenant: Periodic acid: 2 parts;
Tensio-active agent: polyoxyethylenated alcohol sodium sulfate: 1 part
Organism protective material: Natvosol: 0.5 part;
Aqueous medium: deionized water: 95 parts;
PH value=3(10wt% diluted nitric acid aqueous solution is adjusted).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding required Periodic acid by formula in a reservoir; 3rd: the amount adding desired fats polyoxyethylenated alcohol sodium sulfate by formula in a reservoir; 4th: by 10wt% diluted nitric acid aqueous solution debugging pH value to 3; 5th: add Natvosol in a solvent by formula; 6th: add the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.The polishing test result of the present embodiment gained polishing fluid is close with embodiment 2, effectively can protect GST, avoid the formation that butterfly is cheated.
Embodiment 7
By weight, polishing fluid is composed as follows:
Polishing particles: silicon dioxide gel (30wt%, particle diameter: 80nm) content: 3 parts;
Oxygenant: hydrogen peroxide (28wt%): 2 parts;
Tensio-active agent: polyoxyethylenated alcohol sodium sulfate: 1 part
Organism protective material: empgen BB: 1 part;
Aqueous medium: deionized water: 90 parts;
PH value=3(10wt% diluted hydrochloric acid aqueous solution).
Specific configuration process is as follows: first: added by deionized water in the container of configuration solution; Second: the amount adding required hydrogen peroxide by formula in a reservoir; 3rd: the amount adding desired fats polyoxyethylenated alcohol sodium sulfate by formula in a reservoir; 4th: by 10wt% diluted hydrochloric acid aqueous solution debugging pH value to 3; 5th: add empgen BB in a solvent by formula; 6th: add the silicon dioxide gel that solid content is 30wt% in a solvent, namely abundant stirring obtains polishing fluid.The polishing test result of the present embodiment gained polishing fluid is close with embodiment 2, effectively can protect GST, avoid the formation that butterfly is cheated.
In sum, the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (5)
1., for a self-stopping technology chemical mechanical polishing liquid for phase change material GST pattern piece, its raw material by weight, comprises following component:
The scope of the pH value of described self-stopping technology chemical mechanical polishing liquid is 2-6;
Described polishing particles is silicon dioxide gel; Described organism protective material is selected from one or more the mixing in sulphosalicylic acid, carboxymethyl cellulose, Natvosol; One or more mixing in described oxygenant chosen from Fe potassium cyanide, potassium permanganate, Periodic acid and hydrogen peroxide; Described tensio-active agent is aniorfic surfactant, and described tensio-active agent is selected from one or more the combination in polyoxyethylenated alcohol sodium sulfate, sodium polyacrylate and aliphatic alcohol polyoxyvinethene phosphate.
2. self-stopping technology chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, described pH adjusting agent is selected from one or more the mixing in ammoniacal liquor, hydroxyethyl second two ammonia soln, aqueous nitric acid and aqueous hydrochloric acid.
3. self-stopping technology chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, described aqueous medium is deionized water.
4. the preparation method of the self-stopping technology chemical mechanical polishing liquid as described in claim as arbitrary in claim 1-3, comprises the steps:
1) by formula, oxygenant is added in aqueous medium, fully stir;
2) by formula, in step 1 gained mixture, add tensio-active agent, after fully stirring, use pH adjusting agent that the pH of mixed solution is adjusted to 2-6;
3) by formula, in step 2 gained mixture, add organic protective agent, fully stir;
4) by formula, in step 3 gained mixture, add polish abrasive, after fully stirring, namely obtain described self-stopping technology chemical mechanical polishing liquid.
5. the application of self-stopping technology chemical mechanical polishing liquid in phase change material polishing field as described in claim as arbitrary in claim 1-3.
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| CN111662641B (en) * | 2020-06-30 | 2021-10-26 | 中国科学院上海微系统与信息技术研究所 | High-selectivity chemical mechanical polishing solution and application thereof |
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