CN104449564A - Monodisperse grinding fluid and preparation method thereof and method for preparing inorganic oxide sol - Google Patents
Monodisperse grinding fluid and preparation method thereof and method for preparing inorganic oxide sol Download PDFInfo
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- CN104449564A CN104449564A CN201310438757.4A CN201310438757A CN104449564A CN 104449564 A CN104449564 A CN 104449564A CN 201310438757 A CN201310438757 A CN 201310438757A CN 104449564 A CN104449564 A CN 104449564A
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- 229910052809 inorganic oxide Inorganic materials 0.000 title claims abstract description 189
- 238000002360 preparation method Methods 0.000 title claims description 37
- 238000000227 grinding Methods 0.000 title abstract description 10
- 238000000034 method Methods 0.000 title abstract description 6
- 239000012530 fluid Substances 0.000 title abstract 7
- 239000002245 particle Substances 0.000 claims abstract description 69
- 239000002904 solvent Substances 0.000 claims abstract description 42
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 239000006174 pH buffer Substances 0.000 claims abstract description 20
- 238000009826 distribution Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 78
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- 239000013543 active substance Substances 0.000 claims description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- -1 polyoxyethylene Polymers 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 229960001866 silicon dioxide Drugs 0.000 claims description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000007805 chemical reaction reactant Substances 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229920006122 polyamide resin Polymers 0.000 claims description 4
- 229920000136 polysorbate Polymers 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical group [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- 239000004160 Ammonium persulphate Substances 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 239000010949 copper Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000006748 scratching Methods 0.000 description 4
- 230000002393 scratching effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012163 sequencing technique Methods 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses monodisperse grinding fluid. The monodisperse grinding fluid comprises 2-20 parts of nanometer inorganic oxides, 0-15 parts of metal oxidizing agents, 0-10 parts of an anti-settling agent, 0.1-5 parts of a surfactant, 0-10 parts of pH buffer agents and 40-97 parts of a solvent, wherein the relative standard deviation of the particle size of the nanometer inorganic oxides is less than or equal to 10 percent. The invention also discloses a method for preparing the monodisperse grinding fluid and a method for preparing inorganic oxide sol. In the monodisperse grinding fluid, the particle size distribution of the nanometer inorganic oxides in the monodisperse grinding fluid is uniform, and when a wafer is ground by adopting the monodisperse grinding fluid, the wafer is prevented from being scratched.
Description
Technical field
The present invention relates to technical field of manufacturing semiconductors, particularly relate to a kind of single dispersing lapping liquid and preparation method thereof, inorganic oxide sol preparation method.
Background technology
In recent years, along with highly integrated, the high performance of semiconductor integrated circuit, develop the Micrometer-Nanometer Processing Technology made new advances.Cmp (CMP) is also one of them, utilizes the abrasive between pressurized wafer and grinding pad to carry out the semiconductor processing technology of the chemical milling of mechanical workout and lapping liquid during cmp simultaneously.
The kind of lapping liquid is divided into oxide compound lapping liquid, metal polishing slurry and polysilicon lapping liquid substantially according to the kind of grinding object.Especially metal polishing slurry is the lapping liquid that the CMP of the metal wiring layer be applicable in unicircuit uses, and recently, along with the rise of production of integrated circuits utilizing thin copper film, carries out the research of Cu CMP lapping liquid.Hundreds of the active parts be formed in unicircuit are interconnected to form functional circuit, and are interconnected by multistage mode of connection.Each metal lines such as the first metal layer, the second metal level and the 3rd metal level carry out electrical isolation by dielectric substances such as silicon-dioxide.Especially, along with using copper as each metal line layer material in unicircuit, and use low-k (Low-k) material to make megohmite, the incidence scratching phenomenon when implementing CMP becomes very high.
But in the lapping liquid of prior art, the particle size distribution of silicon-dioxide or cerium dioxide is wide, as shown in Figure 1, because the size of silicon-dioxide differs, therefore a lot of cut can be brought out when grinding the thin film layer of the soft material such as copper and low dielectric constant materials, as shown in Figure 2.Therefore, how providing a kind of monodispersed lapping liquid, minimizing to the scuffing of wafer, having become the problem that those skilled in the art need to solve when carrying out CMP.
Summary of the invention
The object of the invention is to, a kind of single dispersing lapping liquid and preparation method thereof, inorganic oxide sol preparation method are provided, the scuffing to wafer can be reduced.
For solving the problems of the technologies described above, the invention provides a kind of single dispersing lapping liquid, comprising following component by described single dispersing lapping liquid weight 100 parts:
Wherein, the relative standard deviation of the particle diameter of described nano inorganic oxide is less than or equal to 10%.
Further, in described single dispersing lapping liquid, the size distribution of described nano inorganic oxide is 20nm ~ 2 μm.
Further, in described single dispersing lapping liquid, described nano inorganic oxide is silicon-dioxide, titanium dioxide or aluminium sesquioxide.
Further, in described single dispersing lapping liquid, described metal onidiges is hydrogen peroxide or ammonium persulphate.
Further, in described single dispersing lapping liquid, described anti-settling agent is polyoxyethylene glycol or polyamide resin.
Further, in described single dispersing lapping liquid, described tensio-active agent is tween, Span or alkylphenol polyoxyethylene.
Further, in described single dispersing lapping liquid, described pH buffer reagent is ammonium citrate or ammonium acetate.
Further, in described single dispersing lapping liquid, described solvent is pure water or ethanol.
Further, the present invention also provides a kind of preparation method of inorganic oxide sol, comprising:
Step one: solvent is provided;
Step 2: in described solvent, adds the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent;
Step 3: the particle diameter detecting described nano inorganic oxide;
Step 4: judge, as described in the particle diameter of nano inorganic oxide reach predetermined particle diameter, then obtain inorganic oxide sol; As described in the particle diameter of nano inorganic oxide do not reach as described in predetermined particle diameter, then repeating step two and step 3, till the particle diameter of described nano inorganic oxide reaches described predetermined particle diameter.
Further, in the preparation method of described inorganic oxide sol, detected the particle diameter of described nano inorganic oxide by laser particle analyzer or transmission electron microscope.
Further, the present invention also provides a kind of preparation method of single dispersing lapping liquid, comprising:
Prepare inorganic oxide sol;
Described inorganic oxide sol is concentrated;
Carry out Wet planet dispersion to concentrated described inorganic oxide sol to purify;
One or more in metal onidiges, anti-settling agent, tensio-active agent and pH buffer reagent are added, to form single dispersing lapping liquid in concentrated described inorganic oxide sol.
Further, in the preparation method of described inorganic oxide sol, the described step preparing inorganic oxide sol comprises:
Step one: solvent is provided;
Step 2: in described solvent, adds the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent;
Step 3: the particle diameter detecting described nano inorganic oxide;
Step 4: judge, as described in the particle diameter of nano inorganic oxide reach predetermined particle diameter, then obtain inorganic oxide sol; As described in the particle diameter of nano inorganic oxide do not reach as described in predetermined particle diameter, then repeating step two and step 3, till the particle diameter of described nano inorganic oxide reaches described predetermined particle diameter.
Further, in the preparation method of described inorganic oxide sol, rotary evaporating device is adopted to be concentrated by described inorganic oxide sol.
Further, in the preparation method of described inorganic oxide sol, in concentrated described inorganic oxide sol, the content of described nano inorganic oxide is 50wt% ~ 60wt%.
Further, in the preparation method of described inorganic oxide sol, under vacuum conditions Wet planet dispersion is carried out to concentrated described inorganic oxide sol and purify.
Further, in the preparation method of described inorganic oxide sol, in concentrated described inorganic oxide sol, the step of one or more added in metal onidiges, anti-settling agent, tensio-active agent and pH buffer reagent comprises:
Step 1): in concentrated described inorganic oxide sol, add described pH buffer reagent, stir;
Step 2): in concentrated described inorganic oxide sol, add described anti-settling agent and tensio-active agent, stir;
Step 3): in concentrated described inorganic oxide sol, add described metal onidiges, stir.
Compared with prior art, single dispersing lapping liquid provided by the invention and preparation method thereof, inorganic oxide sol preparation method have the following advantages:
Single dispersing lapping liquid provided by the invention and preparation method thereof, inorganic oxide sol preparation method, this single dispersing lapping liquid comprises the nano inorganic oxide of 2-20 part, the metal onidiges of 0-15 part, the anti-settling agent of 0-10 part, the tensio-active agent of 0.1-5 part, the pH buffer reagent of 0-10 part and the solvent of 40-97 part, wherein, the relative standard deviation of the particle diameter of described nano inorganic oxide is less than or equal to 10%, compared with prior art, the even particle size distribution of nano inorganic oxide described in described single dispersing lapping liquid, when adopting described single dispersing lapping liquid to grind wafer, can not scratch wafer.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of silicon-dioxide in the lapping liquid of prior art;
The schematic diagram that when Fig. 2 is the enforcement CMP of prior art, wafer scratches;
Fig. 3 is the schema of the preparation method of inorganic oxide sol in one embodiment of the invention;
Fig. 4 is the schema of the preparation method of single dispersing lapping liquid in one embodiment of the invention;
Fig. 5 is the transmission electron microscope photo of silicon-dioxide in the lapping liquid of first embodiment of the invention;
Fig. 6 is the schematic diagram implementing wafer after CMP in first embodiment of the invention;
Fig. 7 is the transmission electron microscope photo of silicon-dioxide in the lapping liquid of second embodiment of the invention;
Fig. 8 is the transmission electron microscope photo of silicon-dioxide in the lapping liquid of third embodiment of the invention.
Embodiment
Below in conjunction with schematic diagram, single dispersing lapping liquid of the present invention and preparation method thereof, inorganic oxide sol preparation method are described in more detail, which show the preferred embodiments of the present invention, should be appreciated that those skilled in the art can revise the present invention described here, and still realize advantageous effects of the present invention.Therefore, following description is appreciated that extensively knowing for those skilled in the art, and not as limitation of the present invention.
In order to clear, whole features of practical embodiments are not described.They in the following description, are not described in detail known function and structure, because can make the present invention chaotic due to unnecessary details.Will be understood that in the exploitation of any practical embodiments, a large amount of implementation detail must be made to realize the specific objective of developer, such as, according to regarding system or the restriction about business, change into another embodiment by an embodiment.In addition, will be understood that this development may be complicated and time-consuming, but be only routine work to those skilled in the art.
In the following passage, more specifically the present invention is described by way of example with reference to accompanying drawing.According to the following describes and claims, advantages and features of the invention will be clearer.It should be noted that, accompanying drawing all adopts the form that simplifies very much and all uses non-ratio accurately, only in order to object that is convenient, the aid illustration embodiment of the present invention lucidly.
Core concept of the present invention is, one single dispersing lapping liquid is provided, this single dispersing lapping liquid comprises the nano inorganic oxide of 2-20 part, the metal onidiges of 0-15 part, the anti-settling agent of 0-10 part, the tensio-active agent of 0.1-5 part, the pH buffer reagent of 0-10 part and the solvent of 40-97 part, wherein, the relative standard deviation of the particle diameter of described nano inorganic oxide is less than or equal to 10%, compared with prior art, the even particle size distribution of nano inorganic oxide described in described single dispersing lapping liquid, when adopting described single dispersing lapping liquid to grind wafer, can not scratch wafer.
Wherein, described nano inorganic oxide accounts for 2-20 part in described single dispersing lapping liquid, such as 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts etc., specifically determines according to the requirement of described single dispersing lapping liquid.Described nano inorganic oxide is silicon-dioxide, titanium dioxide or aluminium sesquioxide, but described nano inorganic oxide is not limited to inorganic oxide listed above, as long as there is certain degree of hardness and the metastable inorganic oxide of chemical property, also within thought range of the present invention.Preferably, the median size of described nano inorganic oxide is 20nm ~ 2 μm, such as 50nm, 100nm, 200nm, 300nm, 400nm, 500nm, 800nm etc., when the median size of described nano inorganic oxide is 20nm ~ 2 μm, described single dispersing lapping liquid has good nonferromagnetic substance, but the median size of described nano inorganic oxide is not limited to as 20nm ~ 2 μm.The relative standard deviation of the particle diameter of described nano inorganic oxide is less than or equal to 10%, even particle size distribution, when adopting described single dispersing lapping liquid to grind wafer, can not scratch wafer.
Described anti-settling agent accounts for 0-10 part in described single dispersing lapping liquid, such as 0.5 part, 1 part, 1.5 parts, 2.5 parts, 5 parts, 8 parts etc., described anti-settling agent can prevent described nano inorganic oxide sedimentation, but also can not add described anti-settling agent, also within thought range of the present invention.Preferably, described anti-settling agent is polyoxyethylene glycol or polyamide resin, and polyoxyethylene glycol or polyamide resin are to having the ability preventing described nano inorganic oxide sedimentation preferably.
Described tensio-active agent accounts for 0.1-5 part in described single dispersing lapping liquid, such as 0.2 part, 0.5 part, 1 part, 1.5 parts, 2 parts, 3 parts, 4 parts etc., described tensio-active agent can improve the dispersiveness of described nano inorganic oxide, prevents described nano inorganic oxide from reuniting.Preferably, described tensio-active agent is tween, Span or alkylphenol polyoxyethylene, and tween, Span or alkylphenol polyoxyethylene can improve the dispersiveness of described nano inorganic oxide preferably.
Described pH buffer reagent accounts for 0-10 part in described single dispersing lapping liquid, and such as 0.5 part, 1 part, 1.5 parts, 2.5 parts, 5 parts, 8 parts etc., described pH buffer reagent can regulate the pH value of described single dispersing lapping liquid.Preferably, described pH buffer reagent is ammonium citrate or ammonium acetate.
Described solvent accounts for 40-97.9 part in described single dispersing lapping liquid, such as 45 parts, 50 parts, 60 parts, 70 parts, 80 parts, 90 parts etc.Preferably, described solvent is water or ethanol, but described solvent is not limited to as water or ethanol, can also be acetone etc.
In conjunction with above-mentioned core concept, the present invention also provides a kind of preparation method of inorganic oxide sol, as shown in Figure 3, comprising:
Carry out step S11: provide solvent, preferably, described solvent is pure water or ethanol.
Carry out step S12: in described solvent, add the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent.Wherein, predetermined amount can be selected according to the median size of described nano inorganic oxide of final needs and the amount of inorganic oxide sol, does not specifically limit.
Carry out step S13: the particle diameter detecting described nano inorganic oxide.Preferably, the particle diameter of described nano inorganic oxide can be detected by the method such as laser particle analyzer or transmission electron microscope.
Carry out step S14: judge, as described in the particle diameter of nano inorganic oxide reach predetermined particle diameter, then obtain inorganic oxide sol; As described in the particle diameter of nano inorganic oxide do not reach as described in predetermined particle diameter, then repeating step S12 and step S13, till the particle diameter of described nano inorganic oxide reaches described predetermined particle diameter.
In conjunction with above-mentioned core concept, the present invention also provides a kind of preparation method of single dispersing lapping liquid, as shown in Figure 4, comprising:
Carry out step S21: prepare inorganic oxide sol, preferably, the method for step S11-S14 can be adopted to prepare.
Carry out step S22: concentrated by described inorganic oxide sol, preferably, rotary evaporating device can be adopted to be concentrated by described inorganic oxide sol.General, before carrying out step S22, the content of described nano inorganic oxide is 5wt% ~ 20wt%, and after carrying out step S22, the content of concentrated described nano inorganic oxide is 50wt% ~ 60wt%.
Carry out step S23: Wet planet dispersion is carried out to concentrated described inorganic oxide sol and purifies, preferably, under vacuum conditions Wet planet dispersion is carried out to concentrated described inorganic oxide sol and purify.Concrete, under vacuum conditions, concentrated described inorganic oxide sol is put into planetary ball mill, and constantly in concentrated described inorganic oxide sol, add described solvent.Under vacuum conditions, the impurity in concentrated described inorganic oxide sol can evaporate, thus purifies to concentrated described inorganic oxide sol; By the rotation of planetary ball mill, concentrated described inorganic oxide sol is distributed to the described solvent constantly added, thus obtains good dispersity, concentrated described inorganic oxide sol that purity is high.Due in step S23, described inorganic oxide is dispersion state in a solvent, so after Wet planet dispersion is purified, in concentrated described inorganic oxide sol, the purity of described inorganic oxide is high, good dispersity.
Carry out step S24: in concentrated described inorganic oxide sol, add one or more in metal onidiges, anti-settling agent, tensio-active agent and pH buffer reagent, to form single dispersing lapping liquid.Wherein, the sequencing of step S23 and step S24 does not limit, and first can carry out step S23, also first can carry out step S24, or while carrying out Wet planet dispersion purification, carries out step S24.Preferably, step S24 comprises the following steps:
Step 1): in concentrated described inorganic oxide sol, add described pH buffer reagent, stir;
Step 2): in concentrated described inorganic oxide sol, add described anti-settling agent and tensio-active agent, stir;
Step 3): in concentrated described inorganic oxide sol, add described metal onidiges, stir.
Below enumerate several embodiments of described single dispersing lapping liquid and preparation method thereof, inorganic oxide sol preparation method, to clearly demonstrate content of the present invention, will be clear that, content of the present invention is not restricted to following examples, and other improvement by the routine techniques means of those of ordinary skill in the art are also within thought range of the present invention.
[the first embodiment]
Described nano inorganic oxide in this first embodiment is silicon-dioxide.
First, carry out step S21: prepare inorganic oxide sol, in the present embodiment, step S21 adopts following steps:
Carry out step S11: provide solvent, in the present embodiment, described solvent is ethanol;
Carry out step S12: in described solvent, add the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent.Due in the present embodiment, described nano inorganic oxide is silicon-dioxide, so the reaction starting material of inorganic oxide preferably select tetraethoxy and methane amide.In the present embodiment, described predetermined particle diameter is 150nm, so described predetermined amount can be set to the tetraethoxy of 50ml and the methane amide of 10ml;
Carry out step S13: the particle diameter detecting described nano inorganic oxide;
Carry out step S14: judge, in the present embodiment, the particle diameter of described nano inorganic oxide reaches 150nm, then obtain inorganic oxide sol;
Then, carry out step S22: adopt rotary evaporating device to be concentrated by described inorganic oxide sol, the content of nano inorganic oxide described in simmer down to is 55wt%.
Then, step S23 is carried out: under vacuum conditions Wet planet dispersion is carried out to concentrated described inorganic oxide sol and purify.
Finally, carry out step S24: while carrying out Wet planet dispersion purification, carry out following steps:
Step 1): in concentrated described inorganic oxide sol, add described pH buffer reagent, stir;
Step 2): in concentrated described inorganic oxide sol, add described anti-settling agent and tensio-active agent, stir;
Step 3): in concentrated described inorganic oxide sol, add described metal onidiges, stir.
Finally, obtain single dispersing lapping liquid, as shown in Figure 5, in described single dispersing lapping liquid, the median size of described nano inorganic oxide is 150nm, and is evenly distributed.Adopt the single dispersing lapping liquid of the present embodiment to carry out CMP, scratching does not appear in wafer surface, as shown in Figure 6.
[the second embodiment]
Described nano inorganic oxide in this second embodiment is silicon-dioxide, and described predetermined particle diameter is 300nm.
First, carry out step S21: prepare inorganic oxide sol, in the present embodiment, step S21 adopts following steps:
Carry out step S11: provide solvent, in the present embodiment, described solvent is ethanol;
Carry out step S12: in described solvent, add the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent.Due in the present embodiment, described nano inorganic oxide is silicon-dioxide, so the reaction starting material of inorganic oxide preferably select tetraethoxy and methane amide.In the present embodiment, described predetermined particle diameter is 300nm, so described predetermined amount can be set to the tetraethoxy of 50ml and the methane amide of 10ml;
Carry out step S13: the particle diameter detecting described nano inorganic oxide;
Carry out step S14: judge, the particle diameter of described nano inorganic oxide does not reach 300nm, then repeating step S12 and step S13, the tetraethoxy of 50ml and the methane amide of 10ml is added again in described solvent, detect the particle diameter of described nano inorganic oxide, the particle diameter of described nano inorganic oxide reaches 300nm.
Then, carry out step S22: adopt rotary evaporating device to be concentrated by described inorganic oxide sol, the content of nano inorganic oxide described in simmer down to is 50wt%.
Then, step S23 is carried out: under vacuum conditions Wet planet dispersion is carried out to concentrated described inorganic oxide sol and purify.
Finally, carry out step S24: while carrying out Wet planet dispersion purification, carry out following steps:
Step 1): in concentrated described inorganic oxide sol, add described pH buffer reagent, stir;
Step 2): in concentrated described inorganic oxide sol, add described anti-settling agent and tensio-active agent, stir;
Step 3): in concentrated described inorganic oxide sol, add described metal onidiges, stir.
Finally, obtain single dispersing lapping liquid, as shown in Figure 7, in described single dispersing lapping liquid, the median size of described nano inorganic oxide is 300nm, and is evenly distributed.Adopt the single dispersing lapping liquid of the present embodiment to carry out CMP, scratching does not appear in wafer surface.
[the 3rd embodiment]
Described nano inorganic oxide in this 3rd embodiment is silicon-dioxide, and described predetermined particle diameter is 600nm.
First, carry out step S21: prepare inorganic oxide sol, in the present embodiment, step S21 adopts following steps:
Carry out step S11: provide solvent, in the present embodiment, described solvent is pure water;
Carry out step S12: in described solvent, add the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent.Due in the present embodiment, described nano inorganic oxide is silicon-dioxide, so the reaction starting material of inorganic oxide preferably select tetraethoxy and methane amide.In the present embodiment, described predetermined particle diameter is 600nm, so described predetermined amount can be set to the tetraethoxy of 100ml and the methane amide of 20ml;
Carry out step S13: the particle diameter detecting described nano inorganic oxide;
Carry out step S14: judge, the particle diameter of described nano inorganic oxide does not reach 600nm, then repeating step S12 and step S13, the tetraethoxy of 100ml and the methane amide of 20ml is added again in described solvent, detect the particle diameter of described nano inorganic oxide, several times repeatedly, till the particle diameter of described nano inorganic oxide reaches 600nm.
Then, carry out step S22: adopt rotary evaporating device to be concentrated by described inorganic oxide sol, the content of nano inorganic oxide described in simmer down to is 60wt%.
Then, step S23 is carried out: under vacuum conditions Wet planet dispersion is carried out to concentrated described inorganic oxide sol and purify.
Finally, carry out step S24: while carrying out Wet planet dispersion purification, carry out following steps:
Step 1): in concentrated described inorganic oxide sol, add described pH buffer reagent, stir;
Step 2): in concentrated described inorganic oxide sol, add described anti-settling agent and tensio-active agent, stir;
Step 3): in concentrated described inorganic oxide sol, add described metal onidiges, stir.
Finally, obtain single dispersing lapping liquid, as shown in Figure 8, in described single dispersing lapping liquid, the median size of described nano inorganic oxide is 600nm, and is evenly distributed.Adopt the single dispersing lapping liquid of the present embodiment to carry out CMP, scratching does not appear in wafer surface.
In sum, the invention provides a kind of single dispersing lapping liquid and preparation method thereof, inorganic oxide sol preparation method, this single dispersing lapping liquid comprises the solvent of the nano inorganic oxide of 2-20 part, the metal onidiges of 0-15 part, the anti-settling agent of 0-10 part, the tensio-active agent of 0.1-5 part, the pH buffer reagent of 0-10 part and 40-97 part, wherein, the relative standard deviation of the particle diameter of described nano inorganic oxide is less than or equal to 10%.Compared with prior art, the present invention has the following advantages:
The even particle size distribution of nano inorganic oxide described in described single dispersing lapping liquid, when adopting described single dispersing lapping liquid to grind wafer, can not scratch wafer.
Obviously, those skilled in the art can carry out various change and modification to the present invention and not depart from the spirit and scope of the present invention.Like this, if these amendments of the present invention and modification belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these change and modification.
Claims (16)
1. a single dispersing lapping liquid, comprises following component by described single dispersing lapping liquid weight 100 parts:
Wherein, the relative standard deviation of the particle diameter of described nano inorganic oxide is less than or equal to 10%.
2. single dispersing lapping liquid as claimed in claim 1, it is characterized in that, the size distribution of described nano inorganic oxide is 20nm ~ 2 μm.
3. single dispersing lapping liquid as claimed in claim 1 or 2, it is characterized in that, described nano inorganic oxide is silicon-dioxide, titanium dioxide or aluminium sesquioxide.
4. single dispersing lapping liquid as claimed in claim 1 or 2, it is characterized in that, described metal onidiges is hydrogen peroxide or ammonium persulphate.
5. single dispersing lapping liquid as claimed in claim 1 or 2, it is characterized in that, described anti-settling agent is polyoxyethylene glycol or polyamide resin.
6. single dispersing lapping liquid as claimed in claim 1 or 2, it is characterized in that, described tensio-active agent is tween, Span or alkylphenol polyoxyethylene.
7. single dispersing lapping liquid as claimed in claim 1 or 2, it is characterized in that, described pH buffer reagent is ammonium citrate or ammonium acetate.
8. single dispersing lapping liquid as claimed in claim 1 or 2, it is characterized in that, described solvent is pure water or ethanol.
9. a preparation method for inorganic oxide sol, comprising:
Step one: solvent is provided;
Step 2: the reaction starting material adding the inorganic oxide of predetermined amount in described solvent, to form nano inorganic oxide in described solvent;
Step 3: the particle diameter detecting described nano inorganic oxide;
Step 4: judge, as described in the particle diameter of nano inorganic oxide reach predetermined particle diameter, then obtain inorganic oxide sol; As described in the particle diameter of nano inorganic oxide do not reach as described in predetermined particle diameter, then repeating step two and step 3, till the particle diameter of described nano inorganic oxide reaches described predetermined particle diameter.
10. the preparation method of inorganic oxide sol as claimed in claim 9, be is characterized in that, detected the particle diameter of described nano inorganic oxide by laser particle analyzer or transmission electron microscope.
The preparation method of 11. 1 kinds of single dispersing lapping liquids, comprising:
Prepare inorganic oxide sol;
Described inorganic oxide sol is concentrated;
Carry out Wet planet dispersion to concentrated described inorganic oxide sol to purify;
One or more in metal onidiges, anti-settling agent, tensio-active agent and pH buffer reagent are added, to form single dispersing lapping liquid in concentrated described inorganic oxide sol.
The preparation method of 12. single dispersing lapping liquids as claimed in claim 11, it is characterized in that, the described step preparing inorganic oxide sol comprises:
Step one: solvent is provided;
Step 2: in described solvent, adds the reaction starting material of the inorganic oxide of predetermined amount, to form nano inorganic oxide in described solvent;
Step 3: the particle diameter detecting described nano inorganic oxide;
Step 4: judge, as described in the particle diameter of nano inorganic oxide reach predetermined particle diameter, then obtain inorganic oxide sol; As described in the particle diameter of nano inorganic oxide do not reach as described in predetermined particle diameter, then repeating step two and step 3, till the particle diameter of described nano inorganic oxide reaches described predetermined particle diameter.
The preparation method of 13. single dispersing lapping liquids as claimed in claim 11, is characterized in that, adopts rotary evaporating device to be concentrated by described inorganic oxide sol.
The preparation method of 14. single dispersing lapping liquids as claimed in claim 11, is characterized in that, in concentrated described inorganic oxide sol, the content of described nano inorganic oxide is 50wt% ~ 60wt%.
The preparation method of 15. single dispersing lapping liquids as claimed in claim 11, is characterized in that, carries out Wet planet dispersion under vacuum conditions purify to concentrated described inorganic oxide sol.
The preparation method of 16. single dispersing lapping liquids as claimed in claim 11, is characterized in that, in concentrated described inorganic oxide sol, the step of one or more added in metal onidiges, anti-settling agent, tensio-active agent and pH buffer reagent comprises:
Step 1): add described pH buffer reagent in concentrated described inorganic oxide sol, stir;
Step 2): in concentrated described inorganic oxide sol, add described anti-settling agent and tensio-active agent, stir;
Step 3): add described metal onidiges in concentrated described inorganic oxide sol, stir.
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| CN111234706A (en) * | 2020-03-26 | 2020-06-05 | 新乡学院 | A kind of water-based grinding composition and preparation method thereof |
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Application publication date: 20150325 |