JP6559544B2 - Super abrasive tool manufacturing method - Google Patents
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- JP6559544B2 JP6559544B2 JP2015219487A JP2015219487A JP6559544B2 JP 6559544 B2 JP6559544 B2 JP 6559544B2 JP 2015219487 A JP2015219487 A JP 2015219487A JP 2015219487 A JP2015219487 A JP 2015219487A JP 6559544 B2 JP6559544 B2 JP 6559544B2
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- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 238000007747 plating Methods 0.000 claims description 104
- 239000002253 acid Substances 0.000 claims description 63
- 238000010438 heat treatment Methods 0.000 claims description 47
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 32
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 31
- 229910017604 nitric acid Inorganic materials 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 14
- 238000012545 processing Methods 0.000 claims description 3
- 239000002585 base Substances 0.000 description 24
- 229910003460 diamond Inorganic materials 0.000 description 21
- 239000010432 diamond Substances 0.000 description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 18
- 239000006061 abrasive grain Substances 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 15
- 239000008139 complexing agent Substances 0.000 description 13
- 238000004070 electrodeposition Methods 0.000 description 13
- 239000002184 metal Substances 0.000 description 13
- 229910052759 nickel Inorganic materials 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- -1 cemented carbide Chemical compound 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000003125 aqueous solvent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000009713 electroplating Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000010949 copper Substances 0.000 description 4
- 239000001509 sodium citrate Substances 0.000 description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000010953 base metal Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical class NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical class OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical class OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical class CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000002113 nanodiamond Substances 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical class OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical class OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical class OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- QEVGZEDELICMKH-UHFFFAOYSA-N Diglycolic acid Chemical class OC(=O)COCC(O)=O QEVGZEDELICMKH-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Chemical class 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910018104 Ni-P Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- 229910018536 Ni—P Inorganic materials 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000796 S alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Chemical class [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Chemical class OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Chemical class 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- TVMUHOAONWHJBV-UHFFFAOYSA-N dehydroglycine Chemical class OC(=O)C=N TVMUHOAONWHJBV-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical class OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 1
- 239000004310 lactic acid Chemical class 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000001630 malic acid Chemical class 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011975 tartaric acid Chemical class 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Description
本発明は、基材の表面に超砥粒をめっき層により固定した超砥粒工具を製造する技術に関する。 The present invention relates to a technique for manufacturing a superabrasive tool in which superabrasive grains are fixed to a surface of a substrate by a plating layer.
超砥粒工具（典型的には電着工具）は、例えば、ダイヤモンド、ＣＢＮなどの超砥粒を金属めっき層によって縦型形状、カップ形状、円盤形状などの基材（台金）の表面に固着した工具であり、超硬合金、セラミック、ガラス、半導体材料、鋳鉄、各鋼などの精密研削用工具として用いられている。この種の超砥粒工具は、上記超砥粒を分散させたメッキ液内に上記基材を浸漬し、該基材の表面に超砥粒をニッケルなどの金属めっきを用いて固着することにより形成されている（例えば特許文献１〜３）。 Superabrasive tools (typically electrodeposition tools), for example, diamond or CBN superabrasive grains on the surface of a base material (base metal) such as a vertical shape, cup shape, or disk shape by a metal plating layer. It is a fixed tool and is used as a tool for precision grinding of cemented carbide, ceramic, glass, semiconductor material, cast iron, each steel and the like. This type of superabrasive tool is obtained by immersing the base material in a plating solution in which the superabrasive grains are dispersed and fixing the superabrasive grains to the surface of the base material using a metal plating such as nickel. (For example, patent documents 1 to 3).
この種の超砥粒工具においては、切れ味を良好にするため、基材表面に固着された超砥粒の固着密度（析出量）が密であることが要求されている。超砥粒の固着密度を高める方法としては、例えば基材を浸漬しためっき液中に超砥粒を大量に添加することが考えられる。しかし、単純に超砥粒の添加量を増やすだけでは、超砥粒の添加量に対して、基材に固着する超砥粒の割合が著しく低く、電着効率が悪い。また、基材に固着しなかった大量の超砥粒は、回収して再利用する必要があるため、再利用のためのコストがかかるという欠点もある。この点について、特許文献１には、ナノダイヤモンド粒子を懸濁しためっき浴を、酸素を含有する気体で攪拌することで、大量のナノダイヤモンド粒子を金属マトリクス中に分散させる技術が記載されている。しかし、このような技術によっても、超砥粒の固着密度に関する近年の要求レベルを十分に満足させるには不十分であり、なお改善の余地がある。 In this type of superabrasive tool, in order to improve the sharpness, it is required that the fixing density (precipitation amount) of the superabrasive particles fixed on the surface of the substrate is dense. As a method for increasing the fixing density of superabrasive grains, for example, adding a large amount of superabrasive grains in a plating solution in which a substrate is immersed may be considered. However, simply increasing the amount of superabrasive grains, the ratio of superabrasive grains adhering to the substrate is extremely low with respect to the amount of superabrasive grains added, resulting in poor electrodeposition efficiency. In addition, since a large amount of superabrasive grains that have not adhered to the substrate need to be recovered and reused, there is also a disadvantage that costs for reuse are required. In this regard, Patent Document 1 describes a technique for dispersing a large amount of nanodiamond particles in a metal matrix by stirring a plating bath in which nanodiamond particles are suspended with a gas containing oxygen. . However, even such a technique is insufficient to sufficiently satisfy the recent required level regarding the fixing density of superabrasive grains, and there is still room for improvement.
本発明はかかる点に鑑みてなされたものであり、その主な目的は、基材の表面に超砥粒が高密度に固着した超砥粒工具を製造する方法を提供することである。 This invention is made | formed in view of this point, The main objective is to provide the method of manufacturing the superabrasive tool with which the superabrasive grain fixed to the surface of the base material with high density.
本発明者は、基材の表面に超砥粒をめっき層により固着する超砥粒工具の製造方法において、使用する超砥粒を濃硫酸と濃硝酸とを含む混酸中であらかじめ加熱処理することにより超砥粒の固着密度（析出量）を高めることに思い至り、さらに従来に比して濃硫酸の含有率を大幅に減らした混酸を用いることで、基材表面に超砥粒がより高密度に固着した超砥粒工具が得られることを見出し、本発明を完成した。 The present inventor pre-heats superabrasive grains to be used in a mixed acid containing concentrated sulfuric acid and concentrated nitric acid in a manufacturing method of a superabrasive tool in which superabrasive grains are fixed to the surface of a substrate by a plating layer. This leads to an increase in the fixing density (precipitation amount) of superabrasive grains, and by using a mixed acid in which the content of concentrated sulfuric acid is greatly reduced compared to the conventional, superabrasive grains are made higher on the substrate surface. The present inventors have found that a superabrasive tool fixed to the density can be obtained.
すなわち、本発明によって提供される超砥粒工具の製造方法は、基材の表面に超砥粒をめっき層により固定した超砥粒工具を製造する方法である。この製造方法は、濃硫酸と濃硝酸とを１０：９０〜５０：５０の体積比で含む混酸中に超砥粒を分散させて加熱する混酸加熱処理工程を包含する。また、前記混酸加熱処理を施した超砥粒を含むめっき液に基材を浸漬してめっき処理を施すことにより、該基材の表面に前記超砥粒をめっき層により固着するめっき処理工程を包含する。かかる態様の製造方法によれば、基材の表面に超砥粒が高密度に固着した超砥粒工具を製造することができる。 That is, the method for producing a superabrasive tool provided by the present invention is a method for producing a superabrasive tool in which superabrasive grains are fixed to the surface of a substrate by a plating layer. This production method includes a mixed acid heat treatment step in which superabrasive grains are dispersed and heated in a mixed acid containing concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 10:90 to 50:50. In addition, a plating treatment step of fixing the superabrasive grains to the surface of the base material by a plating layer by immersing the base material in a plating solution containing the superabrasive grains subjected to the mixed acid heating treatment and performing a plating treatment. Include. According to the manufacturing method of this aspect, it is possible to manufacture a superabrasive tool in which superabrasive grains are fixed on the surface of a base material at a high density.
ここで開示される製造方法の好ましい一態様では、前記混酸加熱処理工程における加熱温度が３００℃〜５００℃であり、加熱時間が３０分〜２４０分である。このような加熱温度および加熱時間の範囲内であると、超砥粒の固着密度がより良く向上し得る。 In a preferred embodiment of the production method disclosed herein, the heating temperature in the mixed acid heat treatment step is 300 ° C. to 500 ° C., and the heating time is 30 minutes to 240 minutes. Within the range of such heating temperature and heating time, the fixing density of the superabrasive grains can be further improved.
ここで開示される製造方法の好ましい一態様では、前記めっき処理工程は、前記めっき液を４０ｒａｄ／ｓ〜１４０ｒａｄ／ｓ（例えば４０ｒａｄ／ｓ〜６０ｒａｄ／ｓ）の攪拌速度で攪拌しながら行われる。めっき液の攪拌速度を上記範囲内にすることで、基材表面に超砥粒がより高密度に固着された超砥粒工具を製造することができる。 In a preferable aspect of the manufacturing method disclosed herein, the plating treatment step is performed while stirring the plating solution at a stirring speed of 40 rad / s to 140 rad / s (for example, 40 rad / s to 60 rad / s). By setting the stirring speed of the plating solution within the above range, it is possible to produce a superabrasive tool in which superabrasive grains are fixed at a higher density on the substrate surface.
ここで開示される製造方法の好ましい一態様では、前記めっき液は、クエン酸を含む。めっき液にクエン酸を含有させることにより、砥石として使用しても超砥粒の脱落が少ない長寿命な超砥粒工具を製造することができる。 In a preferred embodiment of the production method disclosed herein, the plating solution contains citric acid. By containing citric acid in the plating solution, it is possible to produce a long-abrasive superabrasive tool in which superabrasive grains are less dropped even when used as a grindstone.
ここで開示される製造方法の好ましい一態様では、前記超砥粒の平均粒子径が０．０１μｍ〜１μｍである。このような超砥粒の平均粒子径の範囲内であると、より高性能な超砥粒工具を製造することができる。 In a preferred embodiment of the production method disclosed herein, the average particle diameter of the superabrasive grains is 0.01 μm to 1 μm. When it is within the range of the average particle diameter of such superabrasive grains, a higher performance superabrasive tool can be manufactured.
以下、本発明の好適な実施形態を説明する。なお、本明細書において特に言及している事項（例えば、超砥粒工具の製造方法）以外の事柄であって本発明の実施に必要な事柄（基材の成形方法、超砥粒の合成方法など）は、当該分野における従来技術に基づく当業者の設計事項として把握され得る。本発明は、本明細書及び図面に開示されている内容と当該分野における技術常識とに基づいて実施することができる。本明細書において「超砥粒工具」とは、基材の表面に超砥粒をめっき層により固着した工具（例えば電着工具）をいう。 Hereinafter, preferred embodiments of the present invention will be described. In addition, matters other than matters specifically mentioned in the present specification (for example, a method for producing a superabrasive tool) and matters necessary for carrying out the present invention (a method for forming a base material, a method for synthesizing a superabrasive grain) Etc.) can be understood as a design matter of those skilled in the art based on the prior art in the field. The present invention can be carried out based on the contents disclosed in this specification and the drawings and common general technical knowledge in the field. In this specification, the “superabrasive tool” refers to a tool (for example, an electrodeposition tool) in which superabrasive grains are fixed to the surface of a substrate with a plating layer.
ここに開示される製造方法は、基材の表面に超砥粒をめっき層により固着した超砥粒工具の製造方法に関するものである。図１を参照しつつ本実施形態に係る超砥粒工具の製造方法について説明する。 The manufacturing method disclosed here relates to a manufacturing method of a superabrasive tool in which superabrasive grains are fixed to the surface of a substrate by a plating layer. A method for manufacturing a superabrasive tool according to the present embodiment will be described with reference to FIG.
本実施形態に係る超砥粒工具は、図１に示すように、混酸加熱処理工程（ステップＳ１０）とめっき処理工程（ステップＳ２０）とを経て製造することができる。混酸加熱処理工程には、濃硫酸と濃硝酸とを１０：９０〜５０：５０の体積比で含む混酸中に超砥粒を分散させて加熱することが含まれる。また、めっき処理工程には、混酸加熱処理を施した超砥粒を含むめっき液に基材を浸漬してめっき処理を施すことが含まれる。以下、各工程を詳細に説明する。 As shown in FIG. 1, the superabrasive tool according to the present embodiment can be manufactured through a mixed acid heat treatment step (step S10) and a plating treatment step (step S20). The mixed acid heat treatment step includes dispersing and heating superabrasive grains in a mixed acid containing concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 10:90 to 50:50. Further, the plating treatment step includes immersing the base material in a plating solution containing superabrasive grains subjected to the mixed acid heating treatment to perform the plating treatment. Hereinafter, each process will be described in detail.
＜混酸加熱処理工程＞
ステップＳ１０の混酸熱処理工程では、濃硫酸と濃硝酸とを１０：９０〜５０：５０の体積比で含む混酸中に超砥粒を分散させて加熱する。
<Mixed acid heat treatment process>
In the mixed acid heat treatment step of Step S10, superabrasive grains are dispersed and heated in a mixed acid containing concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 10:90 to 50:50.
＜超砥粒＞
使用する超砥粒としては、従来から超砥粒工具に用いられているものであれば特に制限なく用いることができる。例えば、ダイヤモンド、ＣＢＮ（立方晶硼素）などの超砥粒を好ましく使用することができる。ダイヤモンド砥粒としては、合成ダイヤモンド（人工的に作られたダイヤモンド）や天然ダイヤモンド等が用いられる。また、これらの混合物から形成された超砥粒であってもよい。特にダイヤモンド砥粒の使用が好ましい。使用する超砥粒の形状（外形）は特に限定されず、不規則形状（例えばニードル状、フラット状、ブロッキー状、キューブ状）のものや、球形又はそれに近い形状の超砥粒を好適に使用することができる。かかる超砥粒としては、レーザー散乱法に基づく平均粒子径が概ね０．０１μｍ〜１μｍのものが適当であり、また平均粒径が０．０５μｍ〜０．９μｍであるものが好適であり、０．１μｍ〜０．８μｍであるものがさらに好ましく、０．４μｍ〜０．６μｍであるものが特に好ましい。
<Super abrasive grains>
As the superabrasive grains to be used, any superabrasive grains conventionally used in superabrasive tools can be used without particular limitation. For example, superabrasive grains such as diamond and CBN (cubic boron) can be preferably used. As diamond abrasive grains, synthetic diamond (artificial diamond) or natural diamond is used. Moreover, the superabrasive grain formed from these mixtures may be sufficient. The use of diamond abrasive grains is particularly preferable. The shape (outer shape) of the superabrasive grains to be used is not particularly limited, and irregularly shaped (for example, needle-shaped, flat-shaped, blocky-shaped, cube-shaped) or spherical or near-shaped superabrasive grains are preferably used. can do. As such superabrasive grains, those having an average particle diameter of approximately 0.01 μm to 1 μm based on the laser scattering method are suitable, and those having an average particle diameter of 0.05 μm to 0.9 μm are suitable. More preferably, it is 1 μm to 0.8 μm, and particularly preferably 0.4 μm to 0.6 μm.
＜混酸＞
上記混酸熱処理工程で用いられる混酸は、少なくとも濃硫酸と濃硝酸とを混合した酸（混酸）である。ここでいう濃硫酸とは、硫酸の濃度が９０質量％以上（概ね９０質量％〜１００質量％、例えば９０質量％〜９９質量％、典型的には９５質量％〜９９質量％、例えば９８質量％〜９９質量％）の硫酸液をいう。また、濃硝酸とは、硝酸の濃度が５５質量％以上（概ね５５質量％〜１００質量％、例えば５５質量％〜９９質量％、典型的には６０質量％〜９９質量％、例えば９５質量％〜９９質量％、典型的には９８質量％〜９９質量％）の硝酸水溶液をいう。上記混酸は、硫酸および硝酸以外の酸を含んでもよいし、含まなくてもよい。硫酸および硝酸以外の酸としては、塩酸、リン酸、次亜リン酸、ホスホン酸、ホウ酸、スルファミン酸等の無機酸が例示される。実質的に濃硫酸および濃硝酸のみからなる混酸の使用が好ましい。
<Mixed acid>
The mixed acid used in the mixed acid heat treatment step is an acid (mixed acid) obtained by mixing at least concentrated sulfuric acid and concentrated nitric acid. Concentrated sulfuric acid as used herein refers to a sulfuric acid concentration of 90% by mass or more (approximately 90% to 100% by mass, such as 90% to 99% by mass, typically 95% to 99% by mass, for example 98% by mass. % -99 mass%) sulfuric acid solution. Concentrated nitric acid has a concentration of nitric acid of 55% by mass or more (approximately 55% to 100% by mass, such as 55% to 99% by mass, typically 60% to 99% by mass, for example 95% by mass. To 99 mass%, typically 98 mass% to 99 mass%). The mixed acid may or may not contain an acid other than sulfuric acid and nitric acid. Examples of acids other than sulfuric acid and nitric acid include inorganic acids such as hydrochloric acid, phosphoric acid, hypophosphorous acid, phosphonic acid, boric acid and sulfamic acid. It is preferable to use a mixed acid consisting essentially of concentrated sulfuric acid and concentrated nitric acid.
上記混酸中での濃硫酸と濃硝酸との体積比は、概ね１０：９０〜５０：５０の範囲であり、好ましくは２０：８０〜５０：５０であり、より好ましくは２５：７５〜５０：５０であり、さらに好ましくは４０：６０〜５０：５０である。濃硫酸と濃硝酸との体積比を１０：９０〜５０：５０とした混酸中に超砥粒を分散させて加熱することで、後述するめっき処理工程おいて超砥粒の固着密度（析出量）が向上する。このような効果が得られる理由としては、特に限定的に解釈されるものではないが、例えば以下のように考えられる。すなわち、濃硫酸と濃硝酸との体積比を１０：９０〜５０：５０とした混酸中に超砥粒を分散させて加熱することで、超砥粒の表面に親水性が適度に付与される。このことが、めっき処理工程での超砥粒の固着密度（析出量）向上に寄与するものと考えられる。 The volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed acid is generally in the range of 10:90 to 50:50, preferably 20:80 to 50:50, and more preferably 25:75 to 50:50. 50, more preferably 40:60 to 50:50. The superabrasive grains are dispersed and heated in a mixed acid having a volume ratio of concentrated sulfuric acid to concentrated nitric acid of 10:90 to 50:50, so that the fixing density (precipitation amount) of the superabrasive grains in the plating process described later is performed. ) Will improve. The reason why such an effect is obtained is not particularly limited, but may be considered as follows, for example. That is, hydrophilicity is appropriately imparted to the surface of the superabrasive grains by dispersing and heating the superabrasive grains in a mixed acid in which the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 10:90 to 50:50. . This is considered to contribute to the improvement of the fixing density (precipitation amount) of the superabrasive grains in the plating process.
上記混酸中における硫酸の含有量は、超砥粒の固着密度向上の観点から、概ね１５０ｇ／Ｌ〜１０００ｇ／Ｌにすることが適当であり、好ましくは３００ｇ／Ｌ〜９００ｇ／Ｌ、より好ましくは５００ｇ／Ｌ〜９００ｇ／Ｌである。また、上記混酸中における硝酸の含有量は、超砥粒の固着密度向上の観点から、５００ｇ／Ｌ〜１５００ｇ／Ｌにすることが適当であり、好ましくは６００ｇ／Ｌ〜１２００ｇ／Ｌ、より好ましくは７００ｇ／Ｌ〜１０００ｇ／Ｌである。 The content of sulfuric acid in the mixed acid is suitably about 150 g / L to 1000 g / L, preferably 300 g / L to 900 g / L, more preferably from the viewpoint of improving the fixing density of superabrasive grains. 500 g / L to 900 g / L. Further, the content of nitric acid in the mixed acid is suitably 500 g / L to 1500 g / L, preferably 600 g / L to 1200 g / L, more preferably from the viewpoint of improving the fixing density of the superabrasive grains. Is 700 g / L to 1000 g / L.
＜混酸加熱処理＞
上記混酸熱処理工程においては、上記混酸中に前記超砥粒を分散させて加熱する混酸加熱処理が行われる。加熱温度は特に限定されるものではないが、濃硝酸の沸点以上の温度であることが好ましく、例えば３００℃以上であり、好ましくは３２０℃以上、より好ましくは３５０℃以上である。また、加熱温度は、濃硫酸の沸点以下の温度であることが好ましく、例えば５００℃以下であり、好ましくは４８０℃以下、より好ましくは４５０℃以下である。このような加熱温度の範囲内であると、後述するめっき処理工程おいて基材表面に超砥粒をより高密度に固着することができる。加熱時間は特に限定されるものではないが、例えば３０分以上で充分であり、好ましくは５０分以上、より好ましくは６０分以上である。加熱時間を３０分以上とすることで、超砥粒の表面に適度な親水性を付与することができる。その一方で、加熱時間が長すぎると、上記親水性付与効果が鈍化傾向になることに加えて、処理効率も低下するためメリットがあまりない。加熱時間は例えば２４０分以下、好ましくは１２０分以下、より好ましくは８０分以下である。このような加熱時間の範囲内であると、後述するめっき処理工程おいて基材表面に超砥粒をより高密度に固着することができる。なお、上記混酸加熱処理を効率よく行う観点から、混酸中で超砥粒をより細かく分散させる処理、例えば超音波処理を事前に行っていてもよい。上記混酸熱処理工程の後、水で洗浄して超砥粒に付着した混酸を洗い流し、分離・乾燥することで、混酸加熱処理された超砥粒を得ることができる。
<Mixed acid heat treatment>
In the mixed acid heat treatment step, mixed acid heat treatment is performed in which the superabrasive grains are dispersed and heated in the mixed acid. Although heating temperature is not specifically limited, It is preferable that it is the temperature more than the boiling point of concentrated nitric acid, for example, is 300 degreeC or more, Preferably it is 320 degreeC or more, More preferably, it is 350 degreeC or more. Moreover, it is preferable that heating temperature is the temperature below the boiling point of concentrated sulfuric acid, for example, 500 degrees C or less, Preferably it is 480 degrees C or less, More preferably, it is 450 degrees C or less. Within such a heating temperature range, the superabrasive grains can be fixed to the substrate surface at a higher density in the plating treatment step described later. The heating time is not particularly limited, but for example, 30 minutes or more is sufficient, preferably 50 minutes or more, more preferably 60 minutes or more. By setting the heating time to 30 minutes or longer, moderate hydrophilicity can be imparted to the surface of the superabrasive grains. On the other hand, if the heating time is too long, the effect of imparting hydrophilicity tends to slow down, and the processing efficiency also decreases, so there is not much merit. The heating time is, for example, 240 minutes or less, preferably 120 minutes or less, more preferably 80 minutes or less. Within such a heating time range, the superabrasive grains can be fixed to the surface of the base material at a higher density in the plating treatment step described later. In addition, from the viewpoint of efficiently performing the mixed acid heat treatment, a process for finely dispersing the superabrasive grains in the mixed acid, for example, an ultrasonic treatment may be performed in advance. After the mixed acid heat treatment step, the mixed acid heat-treated superabrasive grains can be obtained by washing with water to wash away the mixed acid adhering to the superabrasive grains, separating, and drying.
＜めっき処理工程＞
ステップＳ２０のめっき処理工程では、上記混酸加熱処理を施した超砥粒を含むめっき液に基材を浸漬してめっき処理を施すことにより、該基材表面に超砥粒をめっき層により固着する。
<Plating process>
In the plating treatment step of step S20, the substrate is immersed in a plating solution containing the superabrasive grains subjected to the mixed acid heating treatment to perform the plating treatment, thereby fixing the superabrasive grains to the surface of the substrate by the plating layer. .
＜基材＞
上記めっき処理の対象となり得る基材（台金）の材質は特に限定されない。この種の超砥粒工具に用いられる材質の基材であれば特に制限なく用いることができる。例えば、銅、アルミニウム、鋼、超硬合金、モリブデン、モリブデン合金、サーメット、チタンなどの金属、セラミックス、プラスチック等の材質の基材を好適に使用し得る。また、上記めっき処理の対象となり得る基材（台金）の形状は特に限定されない。縦型形状、カップ形状、円盤形状などの種々の形状の基材を好適に使用し得る。
<Base material>
The material of the base material (base metal) that can be the object of the plating treatment is not particularly limited. If it is a base material of the material used for this kind of superabrasive tool, it can use without a restriction | limiting especially. For example, a base material made of a metal such as copper, aluminum, steel, cemented carbide, molybdenum, molybdenum alloy, cermet, titanium, ceramics, plastic, or the like can be suitably used. Moreover, the shape of the base material (base metal) that can be the object of the plating treatment is not particularly limited. Various shapes of base materials such as a vertical shape, a cup shape, and a disk shape can be suitably used.
＜めっき液＞
めっき液は、溶媒と、前述した混酸加熱処理を施した超砥粒と、めっき層を構成する金属元素とを含み得る。この金属元素は典型的には金属イオンの形態であり得る。かかる金属元素としては、超砥粒工具の用途に応じて適宜材料を選択することができる。例えば、めっき層を構成する金属元素として、ニッケル（Ｎｉ）、コバルト（Ｃｏ）、クロム（Ｃｒ）、銅（Ｃｕ）、スズ（Ｓｎ）、亜鉛（Ｚｎ）、鉛（Ｐｂ）、鉄（Ｆｅ）、チタン（Ｔｉ）、モリブデン（Ｍｏ）、バナジウム（Ｖ）、金（Ａｕ）、銀（Ａｇ）、白金（Ｐｔ）等のうちの１種または２種以上が挙げられる。また、かかる金属元素のほかに、非金属元素が含まれてもよい。例えば、リン（Ｐ）、硫黄（Ｓ）、ホウ素（Ｂ）などの元素が含まれてもよい。めっき層を構成する材料の好適例として、Ｎｉ，Ｎｉ−Ｓ合金、Ｎｉ−Ｐ合金、Ｎｉ−Ｃｏ合金などが例示される。上記金属元素は、これらを構成元素とする各種の塩の形態でめっき液に添加され得る。塩の例としては、上述した金属元素を構成元素とする無機酸塩（例えば硫酸塩、硝酸塩、炭酸塩）、有機酸塩（例えば酢酸塩）、水酸化物、酸化物、ハロゲン化物などが挙げられる。これらの塩の１種を単独でまたは２種以上を組み合わせて用いることができる。
<Plating solution>
The plating solution may include a solvent, superabrasive grains that have been subjected to the mixed acid heat treatment described above, and a metal element that constitutes the plating layer. This metal element can typically be in the form of a metal ion. As such a metal element, a material can be appropriately selected according to the application of the superabrasive tool. For example, as a metal element constituting the plating layer, nickel (Ni), cobalt (Co), chromium (Cr), copper (Cu), tin (Sn), zinc (Zn), lead (Pb), iron (Fe) , Titanium (Ti), molybdenum (Mo), vanadium (V), gold (Au), silver (Ag), platinum (Pt) and the like. In addition to such metal elements, non-metal elements may be included. For example, elements such as phosphorus (P), sulfur (S), and boron (B) may be included. Ni, Ni-S alloy, Ni-P alloy, Ni-Co alloy etc. are illustrated as a suitable example of the material which comprises a plating layer. The metal element can be added to the plating solution in the form of various salts containing these as constituent elements. Examples of the salt include inorganic acid salts (for example, sulfates, nitrates, carbonates), organic acid salts (for example, acetates), hydroxides, oxides, halides, and the like containing the metal elements described above as constituent elements. It is done. One of these salts can be used alone or in combination of two or more.
めっき液中の金属元素（該金属元素を構成元素とする塩）の含有量は特に限定されないが、超砥粒を強固に保持する観点から、概ね０．０１モル／Ｌ以上であることが好ましく、より好ましくは０．０３モル／Ｌ以上、さらに好ましくは０．０５モル／Ｌ以上、特に好ましくは０．０８モル／Ｌ以上である。また、めっき液中の金属元素の含有量は、概ね５モル／Ｌ以下であることが好ましく、より好ましくは１モル／Ｌ以下、さらに好ましくは０．５モル／Ｌ以下、特に好ましくは０．２モル／Ｌ以下である。 The content of the metal element (salt having the metal element as a constituent element) in the plating solution is not particularly limited, but is preferably about 0.01 mol / L or more from the viewpoint of firmly holding the superabrasive grains. More preferably, it is 0.03 mol / L or more, More preferably, it is 0.05 mol / L or more, Most preferably, it is 0.08 mol / L or more. In addition, the content of the metal element in the plating solution is preferably about 5 mol / L or less, more preferably 1 mol / L or less, still more preferably 0.5 mol / L or less, particularly preferably 0.8. 2 mol / L or less.
めっき液に用いられる溶媒としては、水系溶媒の使用が好ましい。水系溶媒としては、水または水を主体とする混合溶媒が好ましく用いられる。かかる混合溶媒を構成する水以外の溶媒成分としては、水と均一に混合し得る有機溶媒（低級アルコール、低級ケトン等）の一種または二種以上を適宜選択して用いることができる。例えば、該水系溶媒の８０質量％以上（より好ましくは９０質量％以上、さらに好ましくは９５質量％以上）が水である水系溶媒の使用が好ましい。特に好ましい例として、実質的に水からなる水系溶媒が挙げられる。 As a solvent used in the plating solution, an aqueous solvent is preferably used. As the aqueous solvent, water or a mixed solvent mainly composed of water is preferably used. As a solvent component other than water constituting such a mixed solvent, one or more organic solvents (lower alcohol, lower ketone, etc.) that can be uniformly mixed with water can be appropriately selected and used. For example, it is preferable to use an aqueous solvent in which 80% by mass or more (more preferably 90% by mass or more, more preferably 95% by mass or more) of the aqueous solvent is water. A particularly preferred example is an aqueous solvent substantially consisting of water.
めっき液には、必要に応じて錯化剤を含有させることができる。錯化剤としては、クエン酸、マロン酸、酒石酸、乳酸、グリシン、イミノ酢酸、リンゴ酸、グリコール酸、ジグリコール酸、アスコルビン酸およびその金属塩、もしくはアンモニウム塩等が挙げられる。これらの錯化剤の１種を単独でまたは２種以上を組み合わせて用いることができる。中でも、クエン酸またはその塩の使用が好ましい。クエン酸塩の具体例としては、クエン酸ナトリウム、クエン酸カリウムなどのアルカリ金属塩が挙げられる。このような錯化剤を含有させることによって、電着された超砥粒とめっき層との密着力が向上し、加工時の超砥粒の脱落が少ない、長寿命の超砥粒工具を得ることができる。 The plating solution may contain a complexing agent as necessary. Examples of the complexing agent include citric acid, malonic acid, tartaric acid, lactic acid, glycine, iminoacetic acid, malic acid, glycolic acid, diglycolic acid, ascorbic acid and its metal salt, or ammonium salt. One of these complexing agents can be used alone or in combination of two or more. Among these, use of citric acid or a salt thereof is preferable. Specific examples of the citrate include alkali metal salts such as sodium citrate and potassium citrate. By containing such a complexing agent, the adhesion between the electrodeposited superabrasive grains and the plating layer is improved, and a superabrasive tool with a long life is obtained in which the superabrasive grains do not fall off during processing. be able to.
めっき液中の錯化剤の含有量は、目的とするめっき膜の種類や膜厚等に応じて適宜変更し得るが、耐久性向上の観点から、概ね０．０３モル／Ｌ以上であることが好ましく、より好ましくは０．１モル／Ｌ以上、さらに好ましくは０．１５モル／Ｌ以上、特に好ましくは０．２５モル／Ｌ以上である。また、めっき液中の錯化剤の含有量は、概ね３モル／Ｌ以下であることが好ましく、より好ましくは１モル／Ｌ以下、さらに好ましくは０．８モル／Ｌ以下、特に好ましくは０．５モル／Ｌ以下である。このような錯化剤の含有量の範囲内であると、本発明の効果がより好適に発揮され得る。 The content of the complexing agent in the plating solution can be appropriately changed according to the type and thickness of the target plating film, but is generally 0.03 mol / L or more from the viewpoint of improving durability. Is more preferably 0.1 mol / L or more, further preferably 0.15 mol / L or more, and particularly preferably 0.25 mol / L or more. The complexing agent content in the plating solution is preferably about 3 mol / L or less, more preferably 1 mol / L or less, still more preferably 0.8 mol / L or less, and particularly preferably 0. .5 mol / L or less. The effect of this invention can be exhibited more suitably as it is in the range of content of such a complexing agent.
めっき液のｐＨは、例えば８以上、典型的には９以上（例えば９．５以上）とすることができる。また、めっき液のｐＨは、例えば１２以下、典型的には１１以下（例えば１０．５以下）とすることができる。前記混酸加熱処理された超砥粒を、このようなｐＨを有するめっき液において用いることで、本発明の効果がより好適に発揮され得る。 The pH of the plating solution can be 8 or more, typically 9 or more (for example, 9.5 or more). Further, the pH of the plating solution can be 12 or less, typically 11 or less (for example, 10.5 or less). By using the superabrasive grains subjected to the mixed acid heat treatment in a plating solution having such a pH, the effects of the present invention can be more suitably exhibited.
ここに開示されるめっき液は、本発明の効果が著しく妨げられない範囲で、各種の添加材を副成分として含有することができる。そのような添加剤としては、ｐＨ調整剤、界面活性剤、酸化防止剤、粘度調整剤、防腐剤等が例示される。例えばｐＨ調整剤の具体例として、水酸化ナトリウム、水酸化カリウムなどの塩基性化合物が例示される。 The plating solution disclosed here can contain various additives as subcomponents as long as the effects of the present invention are not significantly hindered. Examples of such additives include pH adjusters, surfactants, antioxidants, viscosity adjusters, preservatives and the like. For example, basic compounds such as sodium hydroxide and potassium hydroxide are exemplified as specific examples of the pH adjuster.
＜めっき処理＞
めっき処理工程においては、前記超砥粒を分散させためっき液に基材を浸漬してめっき処理を施す。このめっき処理は、電解めっき処理であってもよいし、無電解めっき処理であってもよい。好ましくは電解めっき処理である。めっき液に分散させる超砥粒の量は特に限定されないが、超砥粒の固着密度向上の観点から、概ね０．５ｇ／Ｌ以上であることが好ましく、より好ましくは１ｇ／Ｌ以上、さらに好ましくは３ｇ／Ｌ以上、特に好ましくは５ｇ／Ｌ以上である。また、めっき液に分散させる超砥粒の量は、概ね２０ｇ／Ｌ以下であることが好ましく、より好ましくは１５ｇ／Ｌ以下、さらに好ましくは１０ｇ／Ｌ以下、特に好ましくは８ｇ／Ｌ以下である。
<Plating treatment>
In the plating process, the substrate is immersed in a plating solution in which the superabrasive grains are dispersed to perform the plating process. This plating process may be an electrolytic plating process or an electroless plating process. Electrolytic plating treatment is preferable. The amount of superabrasive particles to be dispersed in the plating solution is not particularly limited, but is preferably approximately 0.5 g / L or more, more preferably 1 g / L or more, and still more preferably from the viewpoint of improving the fixing density of superabrasive grains. Is 3 g / L or more, particularly preferably 5 g / L or more. The amount of superabrasive particles dispersed in the plating solution is preferably approximately 20 g / L or less, more preferably 15 g / L or less, still more preferably 10 g / L or less, and particularly preferably 8 g / L or less. .
ここで開示される好ましい技術では、上記めっき処理は、上記めっき液を攪拌しながら行われる。めっき液を攪拌しながらめっき処理を行うことにより、基材表面に超砥粒をより高密度に固着することができる。めっき液を攪拌する手段としては、スターラー等の攪拌手段が例示される。攪拌速度としては特に限定されないが、超砥粒の固着密度向上の観点から、概ね２０ｒａｄ／ｓ以上にすることが適当であり、好ましくは３０ｒａｄ／ｓ以上、より好ましくは４０ｒａｄ／ｓ以上、さらに好ましくは５０ｒａｄ／ｓ以上である。また、めっき処理中の攪拌速度は、概ね２００ｒａｄ／ｓ以下にすることが適当であり、好ましくは１６０ｒａｄ／ｓ以下である。例えば、攪拌速度は、１００ｒａｄ／ｓ以下であってもよく、典型的には８０ｒａｄ／ｓ以下（例えば７０ｒａｄ／ｓ以下、典型的には６０ｒａｄ／ｓ以下）であってもよい。ここで開示される技術は、上記攪拌速度が４０ｒａｄ／ｓ〜１６０ｒａｄ／ｓ（例えば４０ｒａｄ／ｓ〜６０ｒａｄ／ｓ）である態様で好ましく実施され得る。 In the preferred technique disclosed herein, the plating treatment is performed while stirring the plating solution. By performing the plating treatment while stirring the plating solution, the superabrasive grains can be fixed on the surface of the base material with higher density. Examples of means for stirring the plating solution include stirring means such as a stirrer. The stirring speed is not particularly limited, but from the viewpoint of improving the fixing density of superabrasive grains, it is appropriate that the stirring speed is generally 20 rad / s or more, preferably 30 rad / s or more, more preferably 40 rad / s or more, and still more preferably. Is 50 rad / s or more. Moreover, it is appropriate that the stirring speed during the plating treatment is approximately 200 rad / s or less, preferably 160 rad / s or less. For example, the stirring speed may be 100 rad / s or less, and typically 80 rad / s or less (for example, 70 rad / s or less, typically 60 rad / s or less). The technique disclosed here can be preferably implemented in a mode in which the stirring speed is 40 rad / s to 160 rad / s (for example, 40 rad / s to 60 rad / s).
上記めっき処理が電解めっき処理である場合、電流密度としては、特に限定されないが、超砥粒の固着密度向上の観点から、概ね０．５Ａ／ｄｍ２以上にすることが適当であり、好ましくは１Ａ／ｄｍ２以上、より好ましくは３Ａ／ｄｍ２以上である。また、電解めっき処理の電流密度は、概ね２０Ａ／ｄｍ２以下にすることが適当であり、好ましくは１２Ａ／ｄｍ２以下、より好ましくは８Ａ／ｄｍ２以下である。このような電流密度の範囲内であると、基材の表面にめっき層を効率よく形成することができる。 When the plating treatment is an electrolytic plating treatment, the current density is not particularly limited. However, from the viewpoint of improving the fixing density of superabrasive grains, it is appropriate that the current density is approximately 0.5 A / dm 2 or more, preferably 1 A / dm 2 or more, more preferably 3 A / dm 2 or more. Moreover, it is appropriate that the current density of the electrolytic plating treatment is approximately 20 A / dm 2 or less, preferably 12 A / dm 2 or less, more preferably 8 A / dm 2 or less. A plating layer can be efficiently formed in the surface of a base material within the range of such a current density.
上記めっき処理により形成されるめっき層の厚みは特に限定されない。めっき層の厚みは、超砥粒を強固に保持する観点から、超砥粒の平均粒子径の１／８以上であることが好ましく、１／５以上であることがより好ましく、１／４以上であることがさらに好ましく、１／３以上であることが特に好ましい。また、めっき層の厚みは、超砥粒工具の切れ味を良好にする観点から、超砥粒の平均粒子径の２／３以下であることが好ましく、３／５以下であることがより好ましく、１／２以下であることがさらに好ましい。めっき層の厚みの具体例としては、概ね０．０２μｍ以上、好ましくは０．０５μｍ以上、より好ましくは０．１μｍ以上、さらに好ましくは０．１５μｍ以上である。また、めっき層の厚みの具体例としては、概ね３μｍ以下、好ましくは１．５μｍ以下、より好ましくは１μｍ以下、さらに好ましくは０．５μｍ以下である。このようなめっき層の厚みの範囲内であると、超砥粒工具の切れ味を良好に保ちつつ、超砥粒が脱落し難い超砥粒工具とすることができる。 The thickness of the plating layer formed by the plating process is not particularly limited. The thickness of the plating layer is preferably 1/8 or more, more preferably 1/5 or more, and more preferably 1/4 or more of the average particle diameter of the superabrasive grains from the viewpoint of firmly holding the superabrasive grains. It is more preferable that it is 1/3 or more. The thickness of the plating layer is preferably 2/3 or less of the average particle diameter of the superabrasive grains, more preferably 3/5 or less, from the viewpoint of improving the sharpness of the superabrasive tool. More preferably, it is 1/2 or less. A specific example of the thickness of the plating layer is approximately 0.02 μm or more, preferably 0.05 μm or more, more preferably 0.1 μm or more, and further preferably 0.15 μm or more. Moreover, as a specific example of the thickness of a plating layer, it is about 3 micrometers or less, Preferably it is 1.5 micrometers or less, More preferably, it is 1 micrometer or less, More preferably, it is 0.5 micrometer or less. Within such a thickness range of the plating layer, it is possible to obtain a superabrasive tool in which superabrasive grains are difficult to fall off while keeping the sharpness of the superabrasive tool good.
このようにして、基材の表面に超砥粒をめっき層により固着した超砥粒工具を製造することができる。 In this way, it is possible to manufacture a superabrasive tool in which superabrasive grains are fixed to the surface of the substrate with a plating layer.
＜超砥粒工具＞
ここに開示される超砥粒工具は、濃硫酸と濃硝酸とを１０：９０〜５０：５０の体積比で含む混酸中に超砥粒を分散させて加熱する混酸加熱処理工程と、該混酸加熱処理された超砥粒を含むめっき液に基材を浸漬してめっき処理を施すことにより、該基材の表面に超砥粒をめっき層により固着するめっき処理工程とを経て製造されたものである。そのため、得られた超砥粒工具は、基材の表面に超砥粒が高密度に固着したものとなり得る。典型的には、基材表面に形成されためっき層と超砥粒との合計容量（体積）を１００容量％とした場合に、超砥粒の含有量が１５容量％以上（例えば１５容量％〜４０容量％）、好ましくは１８容量％以上（例えば１８容量％〜３０容量％）、より好ましくは２０容量％以上、さらに好ましくは２５容量％以上、特に好ましくは２８容量％以上である。このように基材表面に超砥粒が高含有量（高密度）に保持された超砥粒工具は、良好な切れ味を発揮し得る。
<Super abrasive tool>
The superabrasive tool disclosed herein includes a mixed acid heat treatment step in which superabrasive grains are dispersed and heated in a mixed acid containing concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 10:90 to 50:50, and the mixed acid. It is manufactured through a plating treatment step in which superabrasive grains are fixed to the surface of the base material by a plating layer by immersing the base material in a plating solution containing heat-treated superabrasive grains. It is. Therefore, the obtained superabrasive tool can be one in which superabrasive grains are fixed on the surface of the base material at high density. Typically, when the total capacity (volume) of the plating layer formed on the substrate surface and the superabrasive grains is 100% by volume, the superabrasive grain content is 15% by volume or more (for example, 15% by volume). To 40% by volume), preferably 18% by volume or more (for example, 18% to 30% by volume), more preferably 20% by volume or more, still more preferably 25% by volume or more, and particularly preferably 28% by volume or more. Thus, the superabrasive tool in which the superabrasive grains are held at a high content (high density) on the substrate surface can exhibit a good sharpness.
好ましい一態様では、上記超砥粒工具は、クエン酸などの錯化剤を含むめっき液に基材を浸漬してめっき処理を施すことにより製造されたものである。そのため、砥石等として使用しても超砥粒の脱落が少ない長寿命な超砥粒工具であり得る。例えば、後述する擦り付け試験前後における走査型電子顕微鏡（Scanning Electron Microscope：ＳＥＭ）画像から把握される超砥粒の残存率が２５％以上（例えば２５％〜１００％）、より好ましくは３５％以上（例えば３５％〜９０％）、さらに好ましくは５０％以上（例えば５０％〜８０％）、特に好ましくは６０％以上を示すものであり得る。 In a preferred embodiment, the superabrasive tool is manufactured by immersing a base material in a plating solution containing a complexing agent such as citric acid and performing a plating treatment. Therefore, even if it is used as a grindstone or the like, it can be a superabrasive tool having a long life with less dropping of superabrasive grains. For example, the residual ratio of superabrasive grains ascertained from scanning electron microscope (SEM) images before and after a rubbing test described later is 25% or more (for example, 25% to 100%), more preferably 35% or more ( For example, it may be 35% to 90%), more preferably 50% or more (for example, 50% to 80%), and particularly preferably 60% or more.
ここで開示される超砥粒工具の好適例として、上記超砥粒の含有量が１５容量％〜４０容量％であり、かつ、上記擦り付け試験前後の超砥粒残存率が２５％〜１００％であるもの；上記超砥粒の含有量が２０容量％〜３５容量％であり、かつ、上記擦り付け試験前後の超砥粒残存率が４０％〜９０％であるもの；上記超砥粒の含有量が２５容量％〜３５容量％であり、かつ、上記擦り付け試験前後の超砥粒残存率が５０％〜８０％であるもの；等が挙げられる。 As a preferred example of the superabrasive tool disclosed here, the content of the superabrasive grain is 15% by volume to 40% by volume, and the superabrasive residual rate before and after the rubbing test is 25% to 100%. The content of the superabrasive grains is 20% by volume to 35% by volume, and the superabrasive residual rate before and after the rubbing test is 40% to 90%; the content of the superabrasive grains The amount of the superabrasive grains before and after the rubbing test is 50% to 80%, and the like.
次に、本発明に関するいくつかの実施例を説明するが、本発明をかかる実施例に示すものに限定することを意図したものではない。 Next, some examples relating to the present invention will be described, but the present invention is not intended to be limited to those shown in the examples.
本例では、基材の表面に超砥粒をめっき層により固着した超砥粒工具を作製し、超砥粒の析出量および耐久性を評価した。ここでは、超砥粒としてダイヤモンド砥粒を使用し、めっき層を構成する材料としてニッケルを使用した。 In this example, a superabrasive tool in which superabrasive grains were fixed to the surface of the substrate with a plating layer was produced, and the amount of superabrasive grains deposited and the durability were evaluated. Here, diamond abrasive grains were used as the superabrasive grains, and nickel was used as the material constituting the plating layer.
＜試験例１＞
（例１）
濃硫酸（硫酸濃度９８質量％）と濃硝酸（硝酸濃度９８質量％）とを１０：９０の体積比で混合した混酸中に超砥粒としてのダイヤモンド砥粒（平均粒子径０．５μｍ）を分散させ、４００℃で６０分間加熱する混酸加熱処理を行った。また、錯化剤としてのクエン酸ナトリウムと、硫酸ニッケルとを混合して、クエン酸ナトリウムを０．３モル／Ｌ、硫酸ニッケルを０．１モル／Ｌ含むめっき液を調製した。めっき液のｐＨは、水酸化ナトリウムを用いて１０となるように調整した。このめっき液に上記混酸加熱処理を施したダイヤモンド砥粒５ｇ／Ｌ分散させ、銅製の基材を浸漬し、めっき液をマグネチックスクーラーで攪拌しながら電解めっき処理を施すことにより、基材の表面にダイヤモンド砥粒をニッケルめっき層により固着した電着砥石を作製した。ここではめっき液の攪拌速度を１４０ｒａｄ／ｓ、電流密度を５Ａ／ｄｍ２とした。また、ニッケルめっき層の厚みは、ダイヤモンド砥粒の平均粒子径の１／３程度となるように調整した。
<Test Example 1>
(Example 1)
Diamond abrasive grains (average particle size 0.5 μm) as superabrasive grains in a mixed acid obtained by mixing concentrated sulfuric acid (sulfuric acid concentration 98 mass%) and concentrated nitric acid (nitric acid concentration 98 mass%) in a volume ratio of 10:90. The mixed acid heat treatment was performed by dispersing and heating at 400 ° C. for 60 minutes. Further, sodium citrate as a complexing agent and nickel sulfate were mixed to prepare a plating solution containing 0.3 mol / L sodium citrate and 0.1 mol / L nickel sulfate. The pH of the plating solution was adjusted to 10 with sodium hydroxide. The surface of the substrate is obtained by dispersing 5 g / L of the diamond abrasive grains subjected to the mixed acid heat treatment in this plating solution, immersing the copper base material, and subjecting the plating solution to an electrolytic plating process while stirring the magnetic plate with a magnetic school. An electrodeposition grindstone in which diamond abrasive grains were fixed by a nickel plating layer was prepared. Here, the stirring speed of the plating solution was 140 rad / s, and the current density was 5 A / dm 2 . The thickness of the nickel plating layer was adjusted to be about 1/3 of the average particle diameter of the diamond abrasive grains.
（例２）
本例では、混酸における濃硫酸と濃硝酸との体積比を２５：７５に変更したこと以外は例１と同じ手順で電着砥石を作製した。
(Example 2)
In this example, an electrodeposition grindstone was produced in the same procedure as in Example 1 except that the volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed acid was changed to 25:75.
（例３）
本例では、混酸における濃硫酸と濃硝酸との体積比を５０：５０に変更したこと以外は例１と同じ手順で電着砥石を作製した。
(Example 3)
In this example, an electrodeposition grindstone was produced in the same procedure as in Example 1 except that the volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed acid was changed to 50:50.
（例４）
本例では、混酸における濃硫酸と濃硝酸との体積比を７５：２５に変更したこと以外は例１と同じ手順で電着砥石を作製した。
(Example 4)
In this example, an electrodeposition grindstone was produced in the same procedure as in Example 1 except that the volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed acid was changed to 75:25.
（例５）
本例では、混酸における濃硫酸と濃硝酸との体積比を９０：１０に変更したこと以外は例１と同じ手順で電着砥石を作製した。
(Example 5)
In this example, an electrodeposition grindstone was produced in the same procedure as in Example 1 except that the volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed acid was changed to 90:10.
各例の電着砥石について、ニッケルめっき層とダイヤモンド砥粒との合計を１００容量％とした場合におけるダイヤモンド砥粒の含有量を測定した。ダイヤモンド砥粒の含有量は、得られたニッケルめっき層を硝酸で溶解し、基材から剥がれたダイヤモンド砥粒を遠心分離により沈降させ、乾燥後質量を測定することにより把握した。結果を表１の「超砥粒の含有量」欄に示す。 About the electrodeposition grindstone of each example, content of the diamond abrasive grain was measured when the total of the nickel plating layer and the diamond abrasive grain was 100% by volume. The content of the diamond abrasive grains was determined by dissolving the obtained nickel plating layer with nitric acid, precipitating the diamond abrasive grains peeled off from the base material by centrifugation, and measuring the mass after drying. The results are shown in the column “Content of superabrasive grains” in Table 1.
表１に示すように、例１〜５は、混酸加熱処理に用いた混酸中における濃硫酸と濃硝酸の体積比が異なる。濃硫酸と濃硝酸の体積比を１０：９０〜５０：５０とした例１〜３は、濃硫酸と濃硝酸の体積比を７５：２５〜９０：１０とした例４、５に比べて、ダイヤモンド砥粒の含有量が多く、より良好な結果が得られた。この結果から、濃硫酸と濃硝酸の体積比を１０：９０〜５０：５０とした混酸中で混酸加熱処理を施すことによって、基材表面に超砥粒をより高密度に固着し得ることが確認された。 As shown in Table 1, Examples 1 to 5 differ in the volume ratio of concentrated sulfuric acid and concentrated nitric acid in the mixed acid used for the mixed acid heat treatment. Examples 1 to 3 in which the volume ratio of concentrated sulfuric acid and concentrated nitric acid was 10:90 to 50:50 were compared to Examples 4 and 5 in which the volume ratio of concentrated sulfuric acid to concentrated nitric acid was 75:25 to 90:10. The content of diamond abrasive grains was large, and better results were obtained. From this result, it is possible to fix the superabrasive grains to the substrate surface with higher density by performing mixed acid heat treatment in a mixed acid in which the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 10:90 to 50:50. confirmed.
＜試験例２＞
本例では、上述した電着砥石作製過程において、めっき液の攪拌速度、錯化剤の種類、混酸加熱処理の有無を異ならせて電着砥石を作製した。各例について、めっき液の攪拌速度、錯化剤の種類、混酸加熱処理の有無を表２に纏めて示す。なお、例６〜９、１２〜１５では、混酸における濃硫酸と濃硝酸との体積比は５０：５０で一定とした。
<Test Example 2>
In this example, an electrodeposition grindstone was produced by changing the stirring speed of the plating solution, the type of complexing agent, and the presence or absence of mixed acid heat treatment in the above-described electrodeposition grindstone production process. For each example, Table 2 summarizes the stirring speed of the plating solution, the type of complexing agent, and the presence or absence of mixed acid heat treatment. In Examples 6 to 9 and 12 to 15, the volume ratio of concentrated sulfuric acid to concentrated nitric acid in the mixed acid was constant at 50:50.
各例の電着砥石について、ニッケルめっき層とダイヤモンド砥粒との合計を１００容量％とした場合におけるダイヤモンド砥粒の含有量を測定した。
また、各例の電着砥石をガラス板に２３ｇ／ｃｍ２、６００回の条件で擦り付ける擦り付け試験を行い、擦り付け試験前後における電着砥石表面のＳＥＭ画像から、超砥粒の残存率を算出した。そして、得られた算出値が５０％以上のものを「○」、２５％以上５０％未満のものを「△」、２５％未満のものを「×」と評価した。結果を表２の「耐久性」欄に示す。
About the electrodeposition grindstone of each example, content of the diamond abrasive grain was measured when the total of the nickel plating layer and the diamond abrasive grain was 100% by volume.
In addition, a rubbing test in which the electrodeposition grindstone of each example was rubbed against a glass plate at 23 g / cm 2 and 600 times was performed, and the residual rate of superabrasive grains was calculated from SEM images of the electrodeposited grindstone surface before and after the rubbing test. . The obtained calculated values were evaluated as “◯” when the calculated values were 50% or more, “Δ” when the calculated values were 25% or more and less than 50%, and “X” when the calculated values were less than 25%. The results are shown in the “Durability” column of Table 2.
表２に示すように、混酸加熱処理を行った例６、９は、混酸加熱処理を行わなかった例１０、１１に比べてダイヤモンド砥粒の含有量が多く、より良好な結果が得られた。この結果から、濃硫酸と濃硝酸との混酸中で加熱処理を施すことによって、超砥粒の固着密度（析出量）を向上し得ることが確かめられた。また、めっき液の攪拌速度を４０ｒａｄ／ｓ〜６０ｒａｄ／ｓとした例６、７は、例８、９に比べると、ダイヤモンド砥粒の含有量がさらに多かった。超砥粒の固着密度の観点からは、めっき液の攪拌速度は４０ｒａｄ／ｓ〜６０ｒａｄ／ｓとすることが好ましい。また、錯化剤としてクエン酸ナトリウムを用いた例６〜１１は、例１２〜１５に比べると、擦り付け前後の超砥粒残存率がより高く、耐久性が向上していた。耐久性の観点からは、錯化剤としてクエン酸を用いることが好ましい。 As shown in Table 2, in Examples 6 and 9 in which the mixed acid heat treatment was performed, the content of diamond abrasive grains was larger than in Examples 10 and 11 in which the mixed acid heat treatment was not performed, and better results were obtained. . From this result, it was confirmed that the fixing density (precipitation amount) of the superabrasive grains can be improved by performing the heat treatment in a mixed acid of concentrated sulfuric acid and concentrated nitric acid. Further, in Examples 6 and 7 in which the stirring speed of the plating solution was 40 rad / s to 60 rad / s, the content of diamond abrasive grains was higher than that in Examples 8 and 9. From the viewpoint of the fixing density of the superabrasive grains, the stirring speed of the plating solution is preferably 40 rad / s to 60 rad / s. Further, Examples 6 to 11 using sodium citrate as a complexing agent had higher superabrasive residual ratio before and after rubbing and improved durability compared to Examples 12 to 15. From the viewpoint of durability, it is preferable to use citric acid as a complexing agent.
以上、本発明の具体例を詳細に説明したが、これらは例示にすぎず、特許請求の範囲を限定するものではない。特許請求の範囲に記載の技術には、以上に例示した具体例を様々に変形、変更したものが含まれる。 Specific examples of the present invention have been described in detail above, but these are merely examples and do not limit the scope of the claims. The technology described in the claims includes various modifications and changes of the specific examples illustrated above.
Claims (5)
硫酸濃度が９８質量％の濃硫酸と硝酸濃度が９８質量％の濃硝酸とを、１０：９０〜５０：５０の体積比（硫酸：硝酸）で含む混酸中に超砥粒を分散させ、３５０℃以上５００℃以下の加熱温度で加熱する混酸加熱処理工程と、
前記混酸加熱処理を施した超砥粒を含むめっき液に基材を浸漬してめっき処理を施すことにより、該基材の表面に前記超砥粒をめっき層により固着するめっき処理工程と
を包含する、超砥粒工具の製造方法。 A method for producing a superabrasive tool in which superabrasive grains are fixed to the surface of a substrate by a plating layer,
And concentrated nitric sulfuric acid and nitric acid concentration of the sulfuric acid concentration of 98 mass% is 98 mass%, 10: 90-50: volume ratio of 50: disperse the superabrasive in a mixed acid containing at (sulfuric nitric acid), 350 A mixed acid heat treatment step of heating at a heating temperature of from ℃ to 500 ℃ ,
Including a plating treatment step of fixing the superabrasive grains to the surface of the base material by a plating layer by immersing the base material in a plating solution containing the superabrasive grains subjected to the mixed acid heat treatment. A method for manufacturing a superabrasive tool.
The manufacturing method as described in any one of Claims 1-4 whose average particle diameter of the said superabrasive grain is 0.01 micrometer-1 micrometer.
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