CN105273638A - Anti-cleavage suspended grinding fluid for gallium oxide wafer and preparation method thereof - Google Patents
Anti-cleavage suspended grinding fluid for gallium oxide wafer and preparation method thereof Download PDFInfo
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- CN105273638A CN105273638A CN201510658056.0A CN201510658056A CN105273638A CN 105273638 A CN105273638 A CN 105273638A CN 201510658056 A CN201510658056 A CN 201510658056A CN 105273638 A CN105273638 A CN 105273638A
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- lapping liquid
- gallium oxide
- oxide wafer
- cleavage
- grinding
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- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 77
- 238000003776 cleavage reaction Methods 0.000 title claims abstract description 55
- 239000012530 fluid Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000227 grinding Methods 0.000 title abstract description 78
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 17
- 239000003350 kerosene Substances 0.000 claims abstract description 15
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 138
- 239000000725 suspension Substances 0.000 claims description 48
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 26
- -1 polyoxyethylene octylphenol Polymers 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000013543 active substance Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000001913 cellulose Substances 0.000 claims description 8
- 229920002678 cellulose Polymers 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003002 pH adjusting agent Substances 0.000 claims description 7
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 239000006260 foam Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- KXJGSNRAQWDDJT-UHFFFAOYSA-N 1-acetyl-5-bromo-2h-indol-3-one Chemical compound BrC1=CC=C2N(C(=O)C)CC(=O)C2=C1 KXJGSNRAQWDDJT-UHFFFAOYSA-N 0.000 claims description 5
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001856 Ethyl cellulose Substances 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 4
- HPEUJPJOZXNMSJ-UHFFFAOYSA-N Methyl stearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC HPEUJPJOZXNMSJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- MDFFNEOEWAXZRQ-UHFFFAOYSA-N aminyl Chemical compound [NH2] MDFFNEOEWAXZRQ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 4
- 229920001249 ethyl cellulose Polymers 0.000 claims description 4
- 150000007530 organic bases Chemical group 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 229940059574 pentaerithrityl Drugs 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims description 2
- CAMHHLOGFDZBBG-UHFFFAOYSA-N epoxidized methyl oleate Natural products CCCCCCCCC1OC1CCCCCCCC(=O)OC CAMHHLOGFDZBBG-UHFFFAOYSA-N 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 229930195735 unsaturated hydrocarbon Natural products 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- 238000002474 experimental method Methods 0.000 abstract description 10
- 230000007547 defect Effects 0.000 abstract description 9
- 230000007017 scission Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 230000006378 damage Effects 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 230000003750 conditioning effect Effects 0.000 abstract description 5
- 238000005520 cutting process Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract 1
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 239000003899 bactericide agent Substances 0.000 abstract 1
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 235000012431 wafers Nutrition 0.000 description 91
- 238000012545 processing Methods 0.000 description 24
- 239000002585 base Substances 0.000 description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 9
- 230000003746 surface roughness Effects 0.000 description 9
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 8
- 229910052733 gallium Inorganic materials 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- 239000006061 abrasive grain Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 239000003082 abrasive agent Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 description 3
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229960004418 trolamine Drugs 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000002178 crystalline material Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052580 B4C Inorganic materials 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003860 storage Methods 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 an anti-cleavage suspended grinding fluid for a gallium oxide wafer and a preparation method thereof. The fluid is prepared from aluminium oxide micropowder, a dispersing thixotropic agent, a surfactant, kerosene, an alkane, a pH value conditioning agent, an antifoaming agent, a bactericide and a cleaning auxiliary agent. The anti-cleavage suspended grinding fluid is preferably obtained through a large amount of experiments. The grinding fluid is good in stability, and is applicable to rough grinding and smooth grinding of the gallium oxide wafer. The material removal speed is fast, and the wafer surface is smooth and does not have obvious scratches or pits. The grinding fluid is capable of reducing mechanics expansion effect during grinding on surface micro cracks, stress damage layers and other defects left after cutting is performed , is capable of effectively inhibiting cleavage defects during grinding of the gallium oxide wafer, also is low in cost and beneficial for popularization application, and overcomes many disadvantages in the prior art.
Description
Technical field
The present invention relates to gallium oxide wafer (β-Ga
2o
3) grinding technology field, be particularly a kind ofly applicable to that gallium oxide wafer is efficient, high quality is thick/the anti-cleavage suspension lapping liquid of smooth grinding and preparation method thereof.
Background technology
Gallium oxide (β-Ga
2o
3) as novel gan (GaN) substrate material, with traditional sapphire (Al
2o
3), the material such as silicon carbide (SiC) compares, and has that lattice mismatch rate is lower, energy gap reaches 4.8 ~ 4.9eV, visible light wave range transmitance is greater than 80%, the shortlyest reaches the excellent photoelectric properties such as 260nm through wavelength.The light transmission of this material is born and Al
2o
3compare favourably, electroconductibility aspect and SiC are rather similar, and can carry out large size single crystal growth by melting method, are to replace Al
2o
3with the desirable GaN substrate material of SiC, therefore, it has boundless market outlook at field of photoelectric devices.
Along with development that is highlighted, efficient LED technology, substrate wafer surface Ultraprecision Machining is faced with more harsh requirement, and on the basis of guaranteeing wafer surface high integrity, the requirement of effects on surface roughness reaches Subnano-class.Slightly/smooth grinding processing is intended to the kerf, tiny crack and the sub-surface damage layer that produce when removing cut crystal, is obtain ultra-smooth by chemically machinery polished (CMP) to can't harm the critical process step before surface.Gallium oxide (β-Ga
2o
3) crystalline material has traditional Al
2o
3, the photoelectron material such as SiC hard Brittleness, Mohs' hardness is 5 ~ 6, and due in thick/smooth grinding course of processing, grit size is comparatively large, grinding pressure is relatively high, very easily produces the defect such as cut, pit in wafer surface.In addition this material also has unique easy cleavage characteristic, cleavage surface is 100, susceptibility is had to the grinding pressure in thick/smooth grinding course of processing, internal stress, process temperature, especially easily produce the defect such as cleavage crack, and then affect the whole efficiency of follow-up polishing and the quality of gallium oxide wafer.
At present, Al is applicable to
2o
3, the crystalline material wafer such as SiC lapping liquid, the proportioning of the choosing of abrasive material, lapping liquid is not all considered the physicochemical characteristic of gallium oxide material itself, use this type of lapping liquid to carry out slightly/smooth grinding to gallium oxide wafer and add man-hour, be difficult to obtain the high quality wafer that wafer surface integrity is higher and wafer surface affected layer is lower, had a strong impact on the following process quality of wafer.Therefore, for gallium oxide wafer thick/smooth grinding complete processing, the research of especially special anti-cleavage suspension lapping liquid, seems particularly urgent.
Summary of the invention
Goal of the invention: under the present invention be directed to prior art situation, gallium oxide wafer is thick/and smooth grinding working (machining) efficiency is lower, wafer surface quality is not high, easily produces the problem such as cleavage crack, cut, obtains a kind of gallium oxide wafer anti-cleavage suspension lapping liquid and preparation method thereof by lot of experiments screening.Lapping liquid suspended state provided by the invention is comparatively stable, place through the long period and precipitate without obvious component materials, abrasive grains is uniformly dispersed, this lapping liquid is used to carry out slightly/smooth grinding processing to wafer, material removal rate is very fast, the high quality wafer that surface integrity is higher and surface damage layer is lower can be obtained, can the deficiencies in the prior art be overcome.
Technical scheme: in order to realize above object, main technical schemes of the present invention is:
A kind of gallium oxide wafer anti-cleavage suspension lapping liquid, it is made up of the raw material of following weight percents:
Alumina powder 1 ~ 10%, dispersion thixotropic agent 1 ~ 5%, tensio-active agent 1 ~ 10%, kerosene 40 ~ 50%, alkane 20 ~ 30%, pH value regulator 1 ~ 3%, foam killer 0.01 ~ 0.03%, sterilant 0.01 ~ 0.02%, helps clean-out system 0.01 ~ 0.1%.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, it is made up of the raw material of following weight percents:
Alumina powder 5 ~ 10%, dispersion thixotropic agent 3 ~ 5%, tensio-active agent 5 ~ 10%, kerosene 45 ~ 50%, alkane 25 ~ 30%, pH value regulator 1 ~ 3%, foam killer 0.02%, sterilant 0.02%, helps clean-out system 0.05%.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, described alumina powder is α-Al
2o
3, purity more than 99.9%, grain size of micropowder is 0.5 ~ 15 μm, wherein selects the micron power 5 ~ 15 μm that particle diameter is larger during rough grinding, optional model: W7, W10, W14.The micron power 0.5 ~ 5 μm that particle diameter is less is selected, optional model: W0.5, W1, W1.5, W2.5, W3.5 during smooth grinding.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, described dispersion thixotropic agent is one or more mixtures in polyvinyl alcohol and derivatived cellulose, when being equal portions or other ratio for the allocation ratio between each component during several mixing, wherein derivatived cellulose is mainly Natvosol, cyanoethyl cellulose and ethyl cellulose.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, described tensio-active agent is one or more mixtures in polyoxyethylene octylphenol ether, polyoxyethylene nonylphenol ether, fatty alcohol-polyoxyethylene ether, aliphatic acid polyethenoxy ether, polyoxyethylene sorbitan monooleate and methyl stearate Soxylat A 25-7.Preferentially select polyoxyethylene octylphenol ether, polyoxyethylene nonylphenol ether, when for multiple mixing time each component between allocation ratio be equal portions or other ratio.Described tensio-active agent is Determination of Polyoxyethylene Non-ionic Surfactants, thus the secondary pollution that minimizing exogenous metal ions causes grinding wafers.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, the mixture that described kerosene is made up of alkane, aromatic hydrocarbons, cyclic hydrocarbon and unsaturated hydrocarbons, described alkane is the straight chain liquid alkane containing 11 ~ 13 carbon atoms.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, described pH value regulator is divided into alkalescence and acid two kinds, wherein alkaline conditioner is organic bases pH value regulator, by any one in thanomin, quadrol, triethylamine and trolamine or multiple mixture, when being equal portions or other ratio for the allocation ratio between each component during multiple mixing, organic bases all not metal ion; Wherein acid regulator is one or both mixtures in hydrochloric acid or phosphoric acid, when being equal portions or other ratio for the allocation ratio between each component during two kinds of mixing.
Preferably, above-described gallium oxide wafer anti-cleavage suspension lapping liquid, described foam killer is any one in polydimethylsiloxane, polyoxyethylene polyoxypropylene tetramethylolmethane ether and polyoxyethylene polyoxy propyl alcohol amidogen ether; Described sterilant is any one in different thiophene quinoline ketone and BIT; The described clean-out system that helps is isopropyl acetone.
The preparation method of gallium oxide wafer of the present invention anti-cleavage suspension lapping liquid, comprises the following steps:
(1) by weight percentage by kerosene and alkane mixing, fully stir fused, obtain lapping liquid base fluid, leave standstill, be cooled to room temperature, for subsequent use;
(2) under the condition stirred, by weight percentage alumina powder, dispersion thixotropic agent and tensio-active agent are joined in the base fluid of step (1) gained, stir, re-use ultrasonic disperse, obtain lapping liquid intermediate liquid, leave standstill, be cooled to room temperature, for subsequent use;
(3) help clean-out system to join in the intermediate liquid of step (2) gained in defoamer, sterilant river by weight percentage, fully stir, obtain accurate lapping liquid, leave standstill, be cooled to room temperature, for subsequent use;
(4) pH value of the middle accurate lapping liquid of gained of measuring process (3), add acidity or the alkaline pH adjuster of appropriate weight quota as required, slowly be added drop-wise in accurate lapping liquid under the condition stirred, regulate in the scope of pH value to 8.0 ~ 9.0 of lapping liquid, after being fully uniformly mixed, obtain gallium oxide wafer anti-cleavage suspension lapping liquid.
The preparation method of above-described gallium oxide wafer anti-cleavage suspension lapping liquid, described alumina powder is α-Al
2o
3, grain size of micropowder is 0.5 ~ 15 μm;
Dispersion thixotropic agent is one or more mixtures in polyvinyl alcohol and derivatived cellulose, and wherein derivatived cellulose is mainly Natvosol, cyanoethyl cellulose and ethyl cellulose.
The preparation method of above-described gallium oxide wafer anti-cleavage suspension lapping liquid, stirs and adopts electric magnetic whipping appts fully to stir.
In anti-cleavage suspension lapping liquid provided by the invention, alumina lap micro mist mainly realizes the removal of gallium oxide wafer surface larger cutting stria, tiny crack and affected layer with mechanical friction effect.The rough grinding liquid that lapping liquid is divided into abrasive grains larger and the less smooth grinding liquid of abrasive grains, for gallium oxide wafer thick/smooth grinding processing, can effectively avoid wafer surface to produce the comparatively serious defect such as cut, pit.In addition, this lapping liquid can also reduce to the mechanics expansion effect that the defect such as crizzle, stress damage layer residual after cutting produces in process of lapping, the generation of cleavage defect in effective inhibited oxidation gallium wafer grinding process.Traditional diamond lap abrasive material that the present invention does not adopt price higher, but select according to gallium oxide material behavior the alumina lap abrasive material that price is lower, effectively can reduce the cost of lapping liquid, industrially more easily promote.The alkaline pH adjuster that anti-cleavage suspension lapping liquid provided by the invention is selected is organic bases thanomin, quadrol, triethylamine and trolamine, can avoid the secondary pollution that exogenous metal ions brings, and serves maintain stable effect to the pH value of lapping liquid.The present invention screens the dispersion thixotropic agent, the nonionogenic tenside that obtain by lot of experiments, the high stability of abrasive micro-powder in lapping liquid can be kept, the long suspension characteristic of lapping liquid can be realized, thus steadily thick/smooth grinding processing efficiently can be realized, guarantee high-quality gallium oxide wafer surface quality.The present invention adds appropriate polyoxyethylene-type surfactant, and the low bubble that can realize anti-cleavage lapping liquid is even still.The existence of organic composition in lapping liquid, easily causes the generation of mould, makes lapping liquid go bad, and sterilant can the growth of effective mould fungus inhibition, thus solves the problem of lapping liquid long storage time.Help clean-out system effectively can reduce granular absorption, reduce the cost of the follow-up cleaning of gallium oxide wafer.
Beneficial effect: compared to the prior art, the present invention has the following advantages:
1. the rough grinding liquid that lapping liquid involved in the present invention is divided into abrasive grains larger and the less smooth grinding liquid of abrasive grains, be respectively used to gallium oxide wafer thick/smooth grinding processing, material removal rate is fast, wafer surface is comparatively smooth, without obvious cut, pit, can reduce to the mechanics expansion effect that the defect such as crizzle, stress damage layer residual after cutting produces in process of lapping, the generation of cleavage defect in effective inhibited oxidation gallium wafer grinding process.
2. lapping liquid involved in the present invention is weakly alkaline, and to grinding plant non-corrosiveness, attrition process terminates rear easy to clean, and lapping liquid can be avoided many drawbacks of environment etc.
3. lapping liquid involved in the present invention is after long-time placement, and dispersing uniformity is excellent, and suspension characteristic is stablized, and is convenient to transport, stores, and select lower-cost alumina lap abrasive material, effectively can reduce thick/smooth grinding cost.
4. after the suspension lapping liquid using the inventive method to prepare grinds gallium oxide wafer, wafer leveling is good, the attrition process surface of low affected layer can be obtained, rough grinding material removing rate is 4.8 μm/min, surface roughness Ra numerical value reaches 2.1 μm, smooth grinding material removing rate is 1.1 μm/min, and surface roughness Ra numerical value can reach 140nm.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
The preparation method of embodiment 1 gallium oxide wafer anti-cleavage suspension lapping liquid, comprises the following steps:
(1) kerosene 2450g and alkane 1400g is mixed, use electric magnetic whipping appts to carry out 15min and fully stir fused, obtain lapping liquid base fluid, leave standstill, be cooled to room temperature, for subsequent use;
(2) under the condition of electric magnetic whipping appts stirring, the alumina powder 450g of W7 model, polyvinyl alcohol 200g, polyoxyethylene octylphenol ether 400g are joined in the base fluid of (1) step gained, abundant stir about 15min, re-use ultrasonic disperse, ultrasonic disperse adopts 500W, and jitter time is 15min, obtains lapping liquid intermediate liquid, leave standstill, be cooled to room temperature, for subsequent use;
(3) polydimethylsiloxane 1g, different thiophene quinoline ketone 1g, isopropyl acetone 2.5g are joined in the intermediate liquid of (2) step gained, fully stir 15min, obtain accurate lapping liquid, leave standstill, be cooled to room temperature, for subsequent use;
(4) pH value of the accurate lapping liquid of gained in (3) is measured, under the condition stirred, acid, alkali pH value regulator are slowly added drop-wise in accurate lapping liquid as required, regulate the pH value of lapping liquid to weakly alkaline, within the claimed range of 8.0 ~ 9.0, wherein acid ph value conditioning agent is hydrochloric acid, alkaline pH adjuster is thanomin, after being fully uniformly mixed, the anti-cleavage suspension lapping liquid obtained for gallium oxide wafer rough grinding processing is about 5000g.
Get and above-mentionedly carry out rough grinding experiment for gallium oxide wafer anti-cleavage suspension lapping liquid, use Unipol-1502 automatic precision polisher lapper to carry out rough grinding processing to gallium oxide wafer, wafer profile is of a size of 15 × 15mm, grinding pressure 400g/cm
2, lap speed is 60RPM, and lapping liquid flow is 30ml/min.Rough grinding process finishing rear oxidation gallium wafer surface integrity is better, observe under light and there is shadow scratch, using VK-X100/X200 shape measure laser microscope to detect 25 × 25 μm of plane domain inside surface roughness Ra numerical value is 2.1 μm, adopt SartorisuCP225D type precision electronic balance (precision 0.01mg), weigh to gallium oxide wafer before and after rough grinding, calculating this lapping liquid abrasive substance clearance is 4.8 μm/min.As can be seen here, the lapping liquid in the embodiment of the present invention 1 is applicable to the rough grinding processing of gallium oxide wafer.
The preparation method of embodiment 2 gallium oxide wafer anti-cleavage suspension lapping liquid, comprises the following steps:
(1) kerosene 2280g and alkane 1500g is mixed, use electric magnetic whipping appts to carry out 15min and fully stir fused, obtain lapping liquid base fluid, leave standstill, be cooled to room temperature, for subsequent use;
(2) under the condition of electric magnetic whipping appts stirring, the alumina powder 480g of W10 model, polyvinyl alcohol 110g, cyanoethyl cellulose 110g, polyoxyethylene nonylphenol ether 420g are joined in the base fluid of (1) step gained, abundant stir about 15min, re-use ultrasonic disperse, ultrasonic disperse adopts 500W, and jitter time is 15min, obtains lapping liquid intermediate liquid, leave standstill, be cooled to room temperature, for subsequent use;
(3) polyoxyethylene polyoxypropylene tetramethylolmethane ether 1g, BIT 1g, isopropyl acetone 2.5g are joined in the intermediate liquid of (2) step gained, fully stir 15min, obtain accurate lapping liquid, leave standstill, be cooled to room temperature, for subsequent use;
(4) pH value of the accurate lapping liquid of gained in (3) is measured, under the condition stirred, acid, alkali pH value regulator are slowly added drop-wise in accurate lapping liquid as required, regulate the pH value of lapping liquid to weakly alkaline, within the claimed range of 8.0 ~ 9.0, wherein acid ph value conditioning agent is phosphoric acid, alkaline pH adjuster is quadrol, after being fully uniformly mixed, the anti-cleavage suspension lapping liquid obtained for gallium oxide wafer rough grinding processing is about 5000g.
Get and above-mentionedly carry out rough grinding experiment for gallium oxide wafer anti-cleavage suspension lapping liquid, use Unipol-1502 automatic precision polisher lapper to carry out rough grinding processing to gallium oxide wafer, wafer profile is of a size of 15 × 15mm, grinding pressure 420g/cm
2, lap speed is 60RPM, and lapping liquid flow is 35ml/min.Rough grinding process finishing rear oxidation gallium wafer surface integrity is better, observe under light and there is shadow scratch, using VK-X100/X200 shape measure laser microscope to detect 25 × 25 μm of plane domain inside surface roughness Ra numerical value is 2.8 μm, adopt SartorisuCP225D type precision electronic balance (precision 0.01mg), weigh to gallium oxide wafer before and after rough grinding, calculating this lapping liquid abrasive substance clearance is 5.2 μm/min.As can be seen here, the lapping liquid in the embodiment of the present invention 2 is equally applicable to the rough grinding processing of gallium oxide wafer.
The preparation method of embodiment 3 gallium oxide wafer anti-cleavage suspension lapping liquid, comprises the following steps:
(1) kerosene 1000g and alkane 590g is mixed, use electric magnetic whipping appts to carry out 15min and fully stir fused, obtain lapping liquid base fluid, leave standstill, be cooled to room temperature, for subsequent use;
(2) under the condition of electric magnetic whipping appts stirring, the alumina powder 100g of W0.5 model, Natvosol 80g, polyoxyethylene nonylphenol ether 180g are joined in the base fluid of (1) step gained, abundant stir about 20min, re-use ultrasonic disperse, ultrasonic disperse adopts 500W, and jitter time is 25min, obtains lapping liquid intermediate liquid, leave standstill, be cooled to room temperature, for subsequent use;
(3) polyoxyethylene polyoxy propyl alcohol amidogen ether 0.4g, BIT 0.4g, isopropyl acetone 1g are joined in the intermediate liquid of (2) step gained, fully stir 20min, obtain accurate lapping liquid, leave standstill, be cooled to room temperature, for subsequent use;
(4) pH value of the accurate lapping liquid of gained in (3) is measured, under the condition stirred, acid, alkali pH value regulator are slowly added drop-wise in accurate lapping liquid as required, wherein acid ph value conditioning agent is phosphoric acid, alkaline pH adjuster is triethylamine, regulate the pH value of lapping liquid to weakly alkaline, within the claimed range of 8.0 ~ 9.0, after being fully uniformly mixed, the anti-cleavage suspension lapping liquid obtained for gallium oxide wafer rough grinding processing is about 2000g.
Get and above-mentionedly carry out smooth grinding experiment for gallium oxide wafer anti-cleavage suspension lapping liquid, use Unipol-1502 automatic precision polisher lapper to carry out smooth grinding processing to gallium oxide wafer, wafer profile is of a size of 15 × 15mm, grinding pressure 300g/cm
2, lap speed is 80RPM, and lapping liquid flow is 20ml/min.Smooth grinding process finishing rear oxidation gallium wafer surface is complete, observe under light without obvious cut, using VK-X100/X200 shape measure laser microscope to detect 5 × 5 μm of plane domain inside surface roughness Ra numerical value is 140nm, adopt SartorisuCP225D type precision electronic balance (precision 0.01mg), weigh to gallium oxide wafer before and after smooth grinding, calculating this lapping liquid abrasive substance clearance is 1.1 μm/min.As can be seen here, the lapping liquid in the embodiment of the present invention 3 is applicable to the smooth grinding processing of gallium oxide wafer.
The preparation method of embodiment 4 gallium oxide wafer anti-cleavage suspension lapping liquid, comprises the following steps:
(1) kerosene 900g and alkane 600g is mixed, use electric magnetic whipping appts to carry out 15min and fully stir fused, obtain lapping liquid base fluid, leave standstill, be cooled to room temperature, for subsequent use;
(2) electric magnetic whipping appts stir condition under, by the alumina powder 150g of W1.5 model, Natvosol 50g,
ethyl cellulose50g, polyoxyethylene octylphenol ether 200g join in the base fluid of (1) step gained, and abundant stir about 20min, re-uses ultrasonic disperse, and ultrasonic disperse adopts 500W, and jitter time is 25min, obtains lapping liquid intermediate liquid, leaves standstill, is cooled to room temperature, for subsequent use;
(3) polyoxyethylene polyoxy propyl alcohol amidogen ether 0.4g, BIT 0.4g, isopropyl acetone 1g are joined in the intermediate liquid of (2) step gained, fully stir 20min, obtain accurate lapping liquid, leave standstill, be cooled to room temperature, for subsequent use;
(4) pH value of the accurate lapping liquid of gained in (3) is measured, under the condition stirred, acid, alkali pH value regulator are slowly added drop-wise in accurate lapping liquid as required, regulate the pH value of lapping liquid to weakly alkaline, within the claimed range of 8.0 ~ 9.0, wherein acid ph value conditioning agent is hydrochloric acid, alkaline pH adjuster is trolamine, after being fully uniformly mixed, the anti-cleavage suspension lapping liquid obtained for gallium oxide wafer rough grinding processing is about 2000g.
Get and above-mentionedly carry out smooth grinding experiment for gallium oxide wafer anti-cleavage suspension lapping liquid, use Unipol-1502 automatic precision polisher lapper to carry out smooth grinding processing to gallium oxide wafer, wafer profile is of a size of 15 × 15mm, grinding pressure 320g/cm
2, lap speed is 80RPM, and lapping liquid flow is 20ml/min.Smooth grinding process finishing rear oxidation gallium wafer surface is complete, observe under light without obvious cut, using VK-X100/X200 shape measure laser microscope to detect 5 × 5 μm of plane domain inside surface roughness Ra numerical value is 220nm, adopt SartorisuCP225D type precision electronic balance (precision 0.01mg), weigh to gallium oxide wafer before and after smooth grinding, calculating this lapping liquid abrasive substance clearance is 1.4 μm/min.As can be seen here, the lapping liquid in the embodiment of the present invention 4 is equally applicable to the smooth grinding processing of gallium oxide wafer.
Embodiment 5 contrast experiment:
As stated above, lapping liquid of the prior art is adopted (to form primarily of W10 boron carbide micro powder and kerosene, whipping appts need be adopted constantly to stir) carry out rough grinding experiment, Unipol-1502 automatic precision polisher lapper is used to carry out rough grinding processing to gallium oxide wafer, wafer profile is of a size of 15 × 15mm, grinding pressure 500g/cm
2, lap speed is 50RPM, and lapping liquid flow is 50ml/min.Rough grinding process finishing rear oxidation gallium wafer surface integrity is poor, there is penetrability cleavage crack in Partial wafer, under light, observe wafer surface there is more cut, and with a small amount of pit, using VK-X100/X200 shape measure laser microscope to detect 25 × 25 μm of plane domain inside surface roughness Ra numerical value is 4.1 μm, adopt SartorisuCP225D type precision electronic balance (precision 0.01mg), weigh to gallium oxide wafer before and after rough grinding, calculating this lapping liquid abrasive substance clearance is 3.7 μm/min.As can be seen here, under equal conditions, after lapping liquid rough grinding of the prior art, wafer surface quality effect is poor, can not meet the specification of quality of gallium oxide wafer rough grinding processing.
And adopt lapping liquid of the prior art
(form primarily of W0.5 diamond differential and kerosene, whipping appts need be adopted constantly to stir) carry out smooth grinding experiment, use Unipol-1502 automatic precision polisher lapper to carry out smooth grinding processing to gallium oxide wafer, wafer profile is of a size of 15 × 15mm, grinding pressure 380g/cm
2, lap speed is 70RPM, and lapping liquid flow is 35ml/min.Smooth grinding process finishing rear oxidation gallium wafer surface integrity is general, under light, observe surface there is obvious cut, using VK-X100/X200 shape measure laser microscope to detect 5 × 5 μm of plane domain inside surface roughness Ra numerical value is 180nm, adopt SartorisuCP225D type precision electronic balance (precision 0.01mg), weigh to gallium oxide wafer before and after smooth grinding, calculating this lapping liquid abrasive substance clearance is 0.9 μm/min.As can be seen here, its smooth grinding material removing rate of the suspension lapping liquid that the present invention relates under equal conditions and wafer surface quality are all better than lapping liquid of the prior art, are more applicable for the smooth grinding processing of gallium oxide wafer.
Embodiment 6 stability test
Get the gallium oxide wafer anti-cleavage suspension lapping liquid that above embodiment 1 ~ 4 prepares, after depositing 12 months, detect its dispersing uniformity excellent, suspension characteristic is stablized, show the stable performance of gallium oxide wafer provided by the invention anti-cleavage suspension lapping liquid, store convenient transportation.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a gallium oxide wafer anti-cleavage suspension lapping liquid, is characterized in that: it is made up of the raw material of following weight percents:
Alumina powder 1 ~ 10%, dispersion thixotropic agent 1 ~ 5%, tensio-active agent 1 ~ 10%, kerosene 40 ~ 50%, alkane 20 ~ 30%, pH value regulator 1 ~ 3%, foam killer 0.01 ~ 0.03%, sterilant 0.01 ~ 0.02%, helps clean-out system 0.01 ~ 0.1%.
2. gallium oxide wafer according to claim 1 anti-cleavage suspension lapping liquid, is characterized in that: it is made up of the raw material of following weight percents:
Alumina powder 5 ~ 10%, dispersion thixotropic agent 3 ~ 5%, tensio-active agent 5 ~ 10%, kerosene 45 ~ 50%, alkane 25 ~ 30%, pH value regulator 1 ~ 3%, foam killer 0.02%, sterilant 0.02%, helps clean-out system 0.05%.
3. gallium oxide wafer according to claim 1 and 2 anti-cleavage suspension lapping liquid, is characterized in that: described alumina powder is α-Al
2o
3, grain size of micropowder is 0.5 ~ 15 μm.
4. gallium oxide wafer according to claim 3 anti-cleavage suspension lapping liquid, it is characterized in that: described dispersion thixotropic agent is one or more mixtures in polyvinyl alcohol and derivatived cellulose, and wherein derivatived cellulose is mainly Natvosol, cyanoethyl cellulose and ethyl cellulose.
5. gallium oxide wafer according to claim 4 anti-cleavage suspension lapping liquid, is characterized in that: described tensio-active agent is one or more mixtures in polyoxyethylene octylphenol ether, polyoxyethylene nonylphenol ether, fatty alcohol-polyoxyethylene ether, aliphatic acid polyethenoxy ether, polyoxyethylene sorbitan monooleate and methyl stearate Soxylat A 25-7.
6. gallium oxide wafer according to claim 5 anti-cleavage suspension lapping liquid, is characterized in that: the mixture that described kerosene is made up of alkane, aromatic hydrocarbons, cyclic hydrocarbon and unsaturated hydrocarbons, and described alkane is the straight chain liquid alkane containing 11 ~ 13 carbon atoms.
7. gallium oxide wafer according to claim 6 anti-cleavage suspension lapping liquid, is characterized in that: described pH value regulator is divided into alkalescence and acid two kinds, and wherein alkaline conditioner is organic bases pH value regulator; Wherein acid regulator is one or both mixtures in hydrochloric acid or phosphoric acid.
8. gallium oxide wafer according to claim 7 anti-cleavage suspension lapping liquid, is characterized in that: described foam killer is any one in polydimethylsiloxane, polyoxyethylene polyoxypropylene tetramethylolmethane ether and polyoxyethylene polyoxy propyl alcohol amidogen ether; Described sterilant is any one in different thiophene quinoline ketone and BIT; The described clean-out system that helps is isopropyl acetone.
9. the preparation method of gallium oxide wafer according to claim 1 anti-cleavage suspension lapping liquid, is characterized in that, comprise the following steps:
(1) by weight percent according to claim 1, kerosene and alkane are mixed, fully stir fused, obtain lapping liquid base fluid, leave standstill, be cooled to room temperature, for subsequent use;
(2) under the condition stirred, by weight percent according to claim 1, alumina powder, dispersion thixotropic agent and tensio-active agent are joined in the base fluid of step (1) gained, stir, re-use ultrasonic disperse, obtain lapping liquid intermediate liquid, leave standstill, be cooled to room temperature, for subsequent use;
(3) help clean-out system to join in the intermediate liquid of step (2) gained in defoamer, sterilant river by weight percent according to claim 1, fully stir, obtain accurate lapping liquid, leave standstill, be cooled to room temperature, for subsequent use;
(4) pH value of the middle accurate lapping liquid of gained of measuring process (3), add acidity or the alkaline pH adjuster of appropriate weight quota as required, slowly be added drop-wise in accurate lapping liquid under the condition stirred, regulate in the scope of pH value to 8.0 ~ 9.0 of lapping liquid, after being fully uniformly mixed, obtain gallium oxide wafer anti-cleavage suspension lapping liquid.
10. the preparation method of gallium oxide wafer according to claim 9 anti-cleavage suspension lapping liquid, described alumina powder is α-Al
2o
3, grain size of micropowder is 0.5 ~ 15 μm;
Dispersion thixotropic agent is one or more mixtures in polyvinyl alcohol and derivatived cellulose, and wherein derivatived cellulose is mainly Natvosol, cyanoethyl cellulose and ethyl cellulose.
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| CN106711032A (en) * | 2016-12-09 | 2017-05-24 | 盐城工学院 | High-efficiency and low-damage grinding method suitable for hard-brittle and easy-cleavage single crystal gallium oxide wafer |
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Effective date of registration: 20240315 Address after: Room 01-325, Floor 3, Building 13, Yard 53, Yanqi Street, Yanqi Economic Development Zone, Huairou District, Beijing 101400 Patentee after: Beijing gallium and Semiconductor Co.,Ltd. Country or region after: China Address before: 224051 No. 1 hope road middle road, Ting Hu District, Yancheng City, Jiangsu Patentee before: YANCHENG INSTITUTE OF TECHNOLOGY Country or region before: China |