CN109913222A - A silicon wafer polishing liquid - Google Patents
A silicon wafer polishing liquid Download PDFInfo
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- CN109913222A CN109913222A CN201910123412.7A CN201910123412A CN109913222A CN 109913222 A CN109913222 A CN 109913222A CN 201910123412 A CN201910123412 A CN 201910123412A CN 109913222 A CN109913222 A CN 109913222A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 75
- 239000010703 silicon Substances 0.000 title claims abstract description 75
- 239000007788 liquid Substances 0.000 title claims abstract description 57
- 238000005498 polishing Methods 0.000 title claims abstract description 40
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 50
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 23
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 12
- 239000012498 ultrapure water Substances 0.000 claims abstract description 12
- IPTLKMXBROVJJF-UHFFFAOYSA-N azanium;methyl sulfate Chemical compound N.COS(O)(=O)=O IPTLKMXBROVJJF-UHFFFAOYSA-N 0.000 claims abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 37
- 150000003863 ammonium salts Chemical class 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 12
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 9
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005695 Ammonium acetate Substances 0.000 claims description 2
- 229940043376 ammonium acetate Drugs 0.000 claims description 2
- 235000019257 ammonium acetate Nutrition 0.000 claims description 2
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 28
- 238000006243 chemical reaction Methods 0.000 abstract description 20
- 238000003756 stirring Methods 0.000 abstract description 15
- 238000012545 processing Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 206010024769 Local reaction Diseases 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000011149 active material Substances 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 description 31
- 238000005530 etching Methods 0.000 description 26
- 239000000243 solution Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 16
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000003746 surface roughness Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000003643 water by type Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000001272 nitrous oxide Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000000873 masking effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910004077 HF-HNO3 Inorganic materials 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
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- Weting (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The present invention relates to a kind of silicon wafer polishing liquid.The silicon wafer polishing liquid is mainly used for wafer thinning, so that it is removed certain thickness and still maintains good surface quality.The polishing liquid is made of hydrofluoric acid, nitric acid, sulfuric acid, ammonium salt and ultrapure water.The etch temperature control of polishing liquid is 28 ~ 32 DEG C, preferably 30 DEG C.Using stirring technique, stirring rate control to 300 ~ 350 r/min, preferably 330 r/min, to reduce the HNO of local reaction generation2Active material and reaction heat prevent local reaction linear velocity from increasing, and cause corrosion uneven.Silicon chip surface quality is an important index, how much its roughness size and defect will affect the polishing subsequent processing of silicon wafer, the surface damage layer and micro-crack area that front end is generated by mechanical lapping can be removed by carrying out chemical attack to silicon wafer using the polishing liquid, to obtain the surface that roughness is low, defect is few.
Description
Technical field
The invention belongs to wet electronic chemical product and wafers to manufacture interleaving techniques field, and in particular to a kind of silicon wafer polishing liquid and
It uses technique.
Background technique
Semiconductor crystal wafer manufacture in, due to back-end chip manufacture in some special procedures, need to silicon chip surface into
Grinding process within 10 microns of row, while surface will have extraordinary roughness and flatness, and lack to the lattice on surface
Sunken requirement is also very high.And for the mode that mechanical lapping is thinned, silicon face has the mechanical damages such as scratch.Traditional acid corrosion
Liquid, since the autocatalytic cleavage of acid solution keeps its etch-rate too fast, it is difficult to which control is being applied to industrial metaplasia within 10 microns
It produces in real process, in order to obtain stable etch-rate, technical staff needs to utilize the attached dresses such as cooling device, circulator
It sets to control reaction, which again increases process costs.And wafer reducer, although the need of client can be met in removal amount
It asks, but due in traditional HF-HNO3The biggish liquid of the viscosity such as sulfuric acid or phosphoric acid be joined in system to control etching
Rate is too fast, and the gaseous product of reaction is but difficult to be diffused into solution, and can be attached to silicon chip surface for a period of time, makes in this way
Must corrode cannot occur in the masking position of bubble, cause etching uneven.Therefore professional quarters have to use rotary spray instead
Product is thrown out using high-speed rotating centrifugal force, disengages it from silicon chip surface, which substantially increases production costs by technique.
Therefore a kind of controllable-rate is configured, the surface of smooth uniform low defect just can be obtained under the conditions of stirring soaking technology
Polishing liquid it is imperative.This will greatly reduce the cost of wafer manufacture, facilitate the development for pushing IC industry.
Summary of the invention
The present invention is directed to the deficiency of chemical corrosion liquid and wafer reducer in the manufacture of existing wafer, and the first purpose is to provide
A kind of silicon wafer is polished liquid.
The second purpose of the present invention is to provide a kind of use techniques of silicon wafer polishing liquid.
For achieving the above object, the technical solution adopted by the present invention are as follows:
Wherein, the silicon wafer polishing liquid is made of hydrofluoric acid, nitric acid, sulfuric acid, ammonium salt and ultrapure water.
The hydrofluoric acid is electronic-stage hydrofluoric acid, mass concentration 45-52%；
The nitric acid is electronic grade nitric acid, mass concentration 65-72%；
The sulfuric acid is the electron level concentrated sulfuric acid, and mass concentration is 97%~98%；
The ammonium salt is excellent pure grade, and content >=99.95%, wherein the mass concentration of ammonium fluoride is 35-42%；
The water is the ultrapure water that resistivity is 17-18M Ω cm at 25 DEG C.
Its preferred embodiment are as follows:
The hydrofluoric acid is electronic-stage hydrofluoric acid, and concentration is about 50%；
The nitric acid is electronic grade nitric acid, and concentration is about 70%；
The sulfuric acid is the electron level concentrated sulfuric acid, and concentration is about 97%~98%；
The ammonium salt is excellent pure grade, and content >=99.95%, wherein the concentration of ammonium fluoride is 40%.
The water is the ultrapure water of resistivity 18M Ω cm (25 DEG C).
The mass fraction of hydrofluoric acid is 1%~3% in the polishing liquid；The mass fraction of nitric acid is 5%~10%；Sulphur
The mass fraction of acid is 60%~80%；The mass fraction of ammonium salt is 1%-10%；The mass fraction of deionized water is surplus.
Ammonium salt in the polishing liquid include ammonium fluoride, ammonium chloride, ammonium sulfate, ammonium hydrogen sulfate, ammonium nitrate, in ammonium acetate
At least one.And preferred fluorinated ammonium, ammonium sulfate, ammonium hydrogen sulfate.
The ammonium salt provides ammonium ion to solution, and the ammonium nitrate generated in conjunction with nitrate anion is under strong acidic environment
Easily decomposes generation nitrous oxide (N2O) gas, NH4NO3→N2O↑+2H2O.A large amount of gas plays during rise
Stirring action.Gas Stirring promotes bubble to exchange rapidly between silicon chip surface and solution, avoids the masking effect of bubble, and
It accelerates reaction product and localized heat is spread into solution, while with a large amount of introducings of bubble, increasing the mass transfer of hydrofluoric acid
Resistance is conducive to the formation of etch pit structure, obtains more smooth uniform surface.
The polishing liquid is 28~32 DEG C, preferably 30 DEG C using the etch temperature control of technique.
The polishing liquid uses stirring technique, stirring rate control to 300~350r/ using the corrosion process of technique
Min, preferably 330r/min, to reduce the HNO of local reaction generation2Active material and reaction heat prevent local reaction linear velocity
Increase, causes corrosion uneven.
Wherein, polishing liquid is contained with the etching groove of PFA material, the temperature setting of heating sensor is 30 DEG C, and setting is stirred
Mixing rate is 300~350r/min.Then silicon wafer horizontal is put into solution and reacts 2-3min.Silicon wafer after reaction is put
Enter in the container containing a large amount of deionized waters, rinses, drying.
Beneficial effects of the present invention
The advantages and beneficial effects of the present invention are: in the present invention, by introducing ammonium salt, to solution provide ammonium root from
Son, the ammonium nitrate generated in conjunction with nitrate anion easily decomposes generation nitrous oxide (N under strong acidic environment2O) gas, gas
Stirring promotes bubble to exchange rapidly between silicon chip surface and solution, avoids the masking effect of bubble, and accelerate reaction product
It is spread with localized heat into solution, while with a large amount of introducings of bubble, increasing the mass transfer resistance of hydrofluoric acid, being conducive to etch pit
The formation of structure obtains more smooth uniform surface.Manufacturing cost has also been taken into account simultaneously, has optimized using technique, is obtaining
While stable etch-rate and optimal etching surface, cost has been saved for the replacement of technique.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to comparative example, reality
It applies example or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description
It is some comparative examples and embodiment of the invention, for those of ordinary skill in the art, what is do not made the creative labor
Under the premise of, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is the wafer topography that embodiment 2 carries out that silicon etching experiment obtains.
Fig. 2 is the wafer topography that comparative example 1 carries out that silicon etching experiment obtains.
Specific embodiment
For a better understanding of the present invention, the present invention is done below with reference to chart and embodiment and is further described in detail,
But the scope of protection of present invention is not limited by the following examples.
Embodiment 1
Present embodiments provide a kind of silicon wafer polishing liquid and its using technique, specifically:
The hydrofluoric acid used is that mass fraction is 50%, and nitric acid is that mass fraction is 70%, and sulfuric acid is that mass fraction is
97.5%, ammonium salt is the ammonium fluoride that mass fraction is 40%, and water is the ultrapure water of resistivity 18M Ω cm (25 DEG C).
Using above-mentioned raw materials prepare 200g silicon polish liquid, by weight content prepare 14.3% water, 75.8% sulfuric acid,
7.3% nitric acid, 1.6% hydrofluoric acid, the mixed solution of 1% ammonium fluoride.
Using following processing step:
1) the above-mentioned silicon polishing liquid prepared is first poured into etching groove；
2) temperature setting of heating sensor is 30 DEG C；
3) stirring rate is set as 330r/min；
4) then silicon wafer horizontal is put into solution and reacts 2min, detect polishing liquid not with infrared radiation thermometer in reaction process
With the local temperature of position, etch temperature maintains 30~31 DEG C；
5) in etching process, a large amount of white minute bubbles is generated after reacting 5s, are constantly expanded from silicon chip surface into solution
Scatter, and due to the effect of buoyancy, risen to liquid level rapidly, will not staticaccelerator adsorption in silicon chip surface, keep dynamic equilibrium, bubble
Diameter be 0.8~1mm；
6) silicon wafer after reaction is put into the container containing a large amount of deionized waters, is rinsed, drying, silicon chip surface exquisiteness
It is smooth, without white bubble impression；
7) its etch-rate and etching surface roughness are detected, and the result that will test is reported in Table 1 below.
Embodiment 2
Present embodiments provide a kind of silicon wafer polishing liquid and its using technique, specifically:
The hydrofluoric acid used is that mass fraction is 50%, and nitric acid is that mass fraction is 70%, and sulfuric acid is that mass fraction is
97.5%, ammonium salt is the ammonium sulfate that mass fraction is 99.95%, and water is the ultrapure water of resistivity 18M Ω cm (25 DEG C).
Using above-mentioned raw materials prepare 200g silicon polish liquid, by weight content prepare 11% water, 73.4% sulfuric acid,
7.1% nitric acid, 1.5% hydrofluoric acid, the mixed solution of 7% ammonium sulfate.
Using following processing step:
1) the above-mentioned silicon polishing liquid prepared is first poured into etching groove；
2) temperature setting of heating sensor is 30 DEG C；
3) stirring rate is set as 330r/min；
4) then silicon wafer horizontal is put into solution and reacts 2min, detect polishing liquid not with infrared radiation thermometer in reaction process
With the local temperature of position, etch temperature maintains 30~30.5 DEG C；
5) in etching process, reaction initially generates a large amount of white minute bubbles, from silicon chip surface constantly to solution
In spread apart, and due to the effect of buoyancy, risen to liquid level rapidly, will not staticaccelerator adsorption in silicon chip surface, keep dynamic equilibrium,
The diameter of bubble is 0.8~1mm；
6) silicon wafer after reaction is put into the container containing a large amount of deionized waters, is rinsed, drying, silicon chip surface exquisiteness
It is smooth, without white bubble impression, as shown in Figure 1；
7) its etch-rate and etching surface roughness are detected, and the result that will test is reported in Table 1 below.
Embodiment 3
Present embodiments provide a kind of silicon wafer polishing liquid and its using technique, specifically:
The hydrofluoric acid used is that mass fraction is 50%, and nitric acid is that mass fraction is 70%, and sulfuric acid is that mass fraction is
97.5%, ammonium salt is that mass fraction is 99.95% ammonium sulfate and 40% ammonium fluoride, and water is resistivity 18M Ω cm (25
DEG C) ultrapure water.
Using above-mentioned raw materials prepare 200g silicon polish liquid, by weight content prepare 12.1% water, 72.2% sulfuric acid,
7.2% nitric acid, 1.5% hydrofluoric acid, 1.5% ammonium fluoride, the mixed solution of 5.5% ammonium sulfate.Using following technique
Step:
1) the above-mentioned silicon polishing liquid prepared is first poured into etching groove；
2) temperature setting of heating sensor is 30 DEG C；
3) stirring rate is set as 330r/min；
4) then silicon wafer horizontal is put into solution and reacts 2min, detect polishing liquid not with infrared radiation thermometer in reaction process
With the local temperature of position, etch temperature maintains 30~30.5 DEG C；
5) in etching process, reaction initially generates a large amount of white minute bubbles, from silicon chip surface constantly to solution
In spread apart, and due to the effect of buoyancy, risen to liquid level rapidly, will not staticaccelerator adsorption in silicon chip surface, keep dynamic equilibrium,
The diameter of bubble is 0.8~1mm；
6) silicon wafer after reaction is put into the container containing a large amount of deionized waters, is rinsed, drying, silicon chip surface exquisiteness
It is smooth, without white bubble impression；
7) its etch-rate and etching surface roughness are detected, and the result that will test is reported in Table 1 below.
Comparative example 1:
The silicon polishing liquid that comparative example 1 provides no ammonium salt component uses technique with corresponding, specifically:
The hydrofluoric acid used is that mass fraction is 50%, and nitric acid is that mass fraction is 70%, and sulfuric acid is that mass fraction is
97.2%, water is the ultrapure water of resistivity 18M Ω cm (25 DEG C).
Using above-mentioned raw materials prepare 200g silicon polish liquid, by weight content prepare 15.2% water, 75% sulfuric acid,
7.8% nitric acid, the mixed solution of 2% hydrofluoric acid.
Using following processing step:
1) the above-mentioned silicon polishing liquid prepared is first poured into etching groove；
2) temperature setting of heating sensor is 30 DEG C；
3) stirring rate is set as 330r/min；
4) then silicon wafer horizontal is put into solution and reacts 2min, detect polishing liquid not with infrared radiation thermometer in reaction process
With the local temperature of position, maximum temperature is etched up to 35 DEG C；
5) in etching process, after reacting 10s, start to generate biggish white bubble and be attached to silicon chip surface, etch 20s
Afterwards, bubble is covered with entire silicon wafer, and bubble is almost stationary, and the diameter of bubble is 4~5mm；
6) silicon wafer after reaction is put into the container containing a large amount of deionized waters, is rinsed, drying, silicon chip surface occurs
Macroscopic white bubble impression, as shown in Figure 2；
7) its etch-rate and etching surface roughness are detected, and the result that will test is reported in Table 1 below.
Comparative example 2:
Comparative example 2, which provides, uses silicon polishing liquid and its etch effect under condition of different temperatures, specifically:
The hydrofluoric acid used is that mass fraction is 50%, and nitric acid is that mass fraction is 70%, and sulfuric acid is that mass fraction is
97.5%, ammonium salt is the ammonium sulfate that mass fraction is 99.95%, and water is the ultrapure water of resistivity 18M Ω cm (25 DEG C).
Using above-mentioned raw materials prepare 200g silicon polish liquid, by weight content prepare 11% water, 73.4% sulfuric acid,
7.1% nitric acid, 1.5% hydrofluoric acid, the mixed solution of 7% ammonium sulfate.
Using following processing step:
1) the above-mentioned silicon polishing liquid prepared is first poured into etching groove；
2) temperature setting of heating sensor is 45 DEG C；
3) stirring rate is set as 330r/min；
4) then silicon wafer horizontal is put into solution and reacts 2min, detect polishing liquid not with infrared radiation thermometer in reaction process
With the local temperature of position, maximum temperature is etched up to 48 DEG C；
5) in etching process, reaction initially generates a large amount of white minute bubbles, from silicon chip surface constantly to solution
In spread apart, and due to the effect of buoyancy, risen to liquid level rapidly, will not staticaccelerator adsorption in silicon chip surface, keep dynamic equilibrium,
The diameter of bubble is 1~2mm；
6) silicon wafer after reaction is put into the container containing a large amount of deionized waters, is rinsed, drying, silicon chip surface does not have
White bubble impression；
7) its etch-rate and etching surface roughness are detected, and the result that will test is reported in Table 1 below.
Comparative example 3:
Comparative example 3, which provides, uses silicon polishing liquid and its etch effect under stopping stirring, specifically:
The hydrofluoric acid used is that mass fraction is 50%, and nitric acid is that mass fraction is 70%, and sulfuric acid is that mass fraction is
97.5%, ammonium salt is the ammonium sulfate that mass fraction is 99.95%, and water is the ultrapure water of resistivity 18M Ω cm (25 DEG C).
Using above-mentioned raw materials prepare 200g silicon polish liquid, by weight content prepare 11% water, 73.4% sulfuric acid,
7.1% nitric acid, 1.5% hydrofluoric acid, the mixed solution of 7% ammonium sulfate.
Using following processing step:
1) the above-mentioned silicon polishing liquid prepared is first poured into etching groove；
2) temperature setting of heating sensor is 30 DEG C；
3) stirring rate is set as 0r/min；
4) then silicon wafer horizontal is put into solution and reacts 2min, detect polishing liquid not with infrared radiation thermometer in reaction process
With the local temperature of position, local maximum temperature is up to 33 DEG C；
5) in etching process, a large amount of white minute bubbles is generated after reacting 8s, are slowly expanded from silicon chip surface into solution
Scatter, and risen to liquid level, will not staticaccelerator adsorption in silicon chip surface, keep dynamic equilibrium, the diameter of bubble is 0.8~1mm；
6) silicon wafer after reaction is put into the container containing a large amount of deionized waters, is rinsed, drying, silicon chip surface part
There is a small amount of white bubble impression in place；
7) its etch-rate and etching surface roughness are detected, and the result that will test is reported in Table 1 below.
Comparative example 4:
The roughness of silicon chip surface before detection etches, and the result that will test is reported in Table 1 below.
By the comparison of experimental data in table 1 it can be concluded that, embodiment 1, embodiment 2, embodiment 3, due to joined this
The ammonium salt component of invention, surface roughness can maintain stable etching compared with significantly reducing for comparative example 1 and comparative example 4
Rate.Wherein, comparative example 2 and comparative example 2, comparative example 3 have advanced optimized the optimal use technique of the polishing liquid, for this
The industrial application of polishing liquid provides technical support.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and is not the limitation to embodiment.For
For those of ordinary skill in the art, other various forms of variations or change can also be made on the basis of the above description
It is dynamic.There is no necessity and possibility to exhaust all the enbodiments.And the obvious changes or variations therefore amplified
Within the protection scope of the invention.
1 embodiment 1 to 3 of table and comparative example 1 to 4 carry out the experimental result that silicon etching experiment measures.
Claims (3)
- The liquid 1. a kind of silicon wafer is polished, it is characterised in that: the silicon wafer polishing liquid is by hydrofluoric acid, nitric acid, sulfuric acid, ammoniumSalt and ultrapure water composition；The hydrofluoric acid is electronic-stage hydrofluoric acid, mass concentration 45-52%；The nitric acid is electronic grade nitric acid, mass concentration 65-72%；The sulfuric acid is the electron level concentrated sulfuric acid, and mass concentration is 97% ~ 98%；The ammonium salt is excellent pure grade, and content >=99.95%, wherein the mass concentration of ammonium fluoride is 35-42%；The water is the ultrapure water that resistivity is 17-18M Ω cm at 25 DEG C.
- The liquid 2. silicon wafer according to claim 1 is polished, it is characterised in that: in polishing liquid the mass fraction of hydrofluoric acid be 1% ~ 3%；The mass fraction of nitric acid is 5% ~ 10%；The mass fraction of sulfuric acid is 60% ~ 80%；The mass fraction of ammonium salt is 1%-10%；Go from The mass fraction of sub- water is surplus.
- The liquid 3. silicon wafer according to claim 1 is polished, it is characterised in that: the ammonium salt in polishing liquid includes ammonium fluoride, chlorination One or both of ammonium, ammonium sulfate, ammonium hydrogen sulfate, ammonium nitrate, ammonium acetate；And preferred fluorinated ammonium, ammonium sulfate or hydrogen sulfate Ammonium.
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| CN201910123412.7A CN109913222A (en) | 2019-02-18 | 2019-02-18 | A silicon wafer polishing liquid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112251233A (en) * | 2020-10-22 | 2021-01-22 | 湖北兴福电子材料有限公司 | Silicon etching solution for removing grinding lines |
| CN115895663A (en) * | 2022-12-28 | 2023-04-04 | 昆山金城试剂有限公司 | Silicon corrosive agent |
| CN116218529A (en) * | 2022-12-25 | 2023-06-06 | 湖北兴福电子材料股份有限公司 | P-silicon soaking corrosive liquid |
Citations (3)
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| CN109321253A (en) * | 2018-11-28 | 2019-02-12 | 湖北兴福电子材料有限公司 | An etching solution for silicon wafers |
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| CN1411612A (en) * | 1999-12-22 | 2003-04-16 | 默克专利有限公司 | Method for raw etching silicon solar cells |
| CN101131546A (en) * | 2006-08-21 | 2008-02-27 | 第一毛织株式会社 | Wet etching solution |
| CN109321253A (en) * | 2018-11-28 | 2019-02-12 | 湖北兴福电子材料有限公司 | An etching solution for silicon wafers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112251233A (en) * | 2020-10-22 | 2021-01-22 | 湖北兴福电子材料有限公司 | Silicon etching solution for removing grinding lines |
| CN112251233B (en) * | 2020-10-22 | 2021-09-07 | 湖北兴福电子材料有限公司 | Silicon etching solution for removing grinding lines |
| CN116218529A (en) * | 2022-12-25 | 2023-06-06 | 湖北兴福电子材料股份有限公司 | P-silicon soaking corrosive liquid |
| CN116218529B (en) * | 2022-12-25 | 2025-02-25 | 湖北兴福电子材料股份有限公司 | A P-silicon immersion etching solution |
| CN115895663A (en) * | 2022-12-28 | 2023-04-04 | 昆山金城试剂有限公司 | Silicon corrosive agent |
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