JP7313664B2 - Electropolishing method - Google Patents
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- JP7313664B2 JP7313664B2 JP2019112006A JP2019112006A JP7313664B2 JP 7313664 B2 JP7313664 B2 JP 7313664B2 JP 2019112006 A JP2019112006 A JP 2019112006A JP 2019112006 A JP2019112006 A JP 2019112006A JP 7313664 B2 JP7313664 B2 JP 7313664B2
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- 238000000034 method Methods 0.000 title claims description 7
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 39
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 30
- 229910052758 niobium Inorganic materials 0.000 claims description 11
- 239000010955 niobium Substances 0.000 claims description 11
- 239000008151 electrolyte solution Substances 0.000 claims description 10
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000005498 polishing Methods 0.000 description 41
- 239000000523 sample Substances 0.000 description 16
- 238000002474 experimental method Methods 0.000 description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000002939 deleterious effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229950006191 gluconic acid Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002821 niobium Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Description
本発明は電解研磨方法に関し、特に、ニオブの電解研磨方法に関するものである。 The present invention relates to an electropolishing method, and more particularly to a niobium electropolishing method.
ビッグバン状態を形成する装置としてリニアコライダが建設されようとしている（ILC計画）。リニアコライダには図９に示すように、軸方向に周期的に径が変化するニオブの空洞管１００が使用される。この実験で所定の効果を得るための要素の１つとして、このニオブの空洞管１００の内面が平滑になっているか否かがある。
A linear collider is about to be built as a device to form a big bang state (ILC plan). As shown in FIG. 9, the linear collider uses a
ところが、空洞管１００は、成形時に過大な圧力や熱を掛けるところから、その内表面の組織は不均一に歪んだ状態となっている。この表面状態をこのままにしておくと、電気的特性、磁気的特性も不均一な状態となり、結果として、電子や陽子に所定の速度を与えることができなくなる。そこで、空洞管の内面を所定の厚さ、研磨する方法が開発されている。
However, since the
ニオブに限らず、上記のような空洞管を研磨する方法としては、特許文献１に開示する化学研磨と特許文献２に開示する電解研磨が一般的に使用されているが、いずれの方法であても、電解液として濃硫酸、フッ酸、燐酸、硝酸等強い酸化力を持つ液の一種あるいはその混合液が使用される。
Chemical polishing disclosed in
一方、本願出願人は上記のような複数の膨らみのある空洞管の内面を研磨するための電極を特許5807938（USP9689068）を開発している。当該電極を使用して電解研磨をする場合においても電解液として、上記濃硫酸等を使用することに変わりはない。 On the other hand, the applicant of the present application has developed a patent 5807938 (USP9689068) for an electrode for polishing the inner surface of a hollow tube having a plurality of bulges as described above. Even when electropolishing is performed using the electrode, the concentrated sulfuric acid or the like is still used as the electrolytic solution.
上記のうち、濃硫酸＋フッ酸が一般的な電解研磨液であるが、いずれも非常に酸化力が強く、劇物に指定されており、誤って皮膚に触れたり、蒸気を吸ったりすると健康障害を生じることになる。従って、これら薬品の取り扱いは極めて慎重を要することになる。 Among the above, concentrated sulfuric acid and hydrofluoric acid are common electropolishing liquids, but both of them have extremely strong oxidizing power and are designated as deleterious substances. Therefore, handling of these chemicals requires extreme caution.
本発明は、上記従来の事情に鑑みて提案されたものであって、取り扱いが容易な物質を用いた電解液とその電解液を用いた電解方法を提供することを目的とする。 The present invention has been proposed in view of the above-described conventional circumstances, and an object of the present invention is to provide an electrolytic solution using a substance that is easy to handle, and an electrolysis method using the electrolytic solution.
ニオブ、チタン、タンタルの少なくとも１種の電解研磨をするについて、グリコール酸溶液にフッ化アンモニウムの正塩のみを所定量溶解させた電解液中で、室温から５０℃の範囲で、電極間距離を６ｃｍで、電圧を２５Ｖ以下で３０分以上実行する。前記電解液のグリコール酸溶液は、３０～９０質量％であり、前記フッ化アンモニウムの正塩がグリコール酸溶液に対して外掛けで、２～１０質量％である。尚、前記フッ化アンモニウムは正塩のみを使用するものとする。 Electrolytic polishing of at least one of niobium, titanium, and tantalum is performed in an electrolytic solution obtained by dissolving a predetermined amount of ammonium fluoride orthosalt in a glycolic acid solution , at a temperature ranging from room temperature to 50° C., with a distance between electrodes of 6 cm, and a voltage of 25 V or less for 30 minutes or more. The glycolic acid solution of the electrolytic solution is 30 to 90% by mass, and the normal salt of ammonium fluoride is 2 to 10% by mass based on the glycolic acid solution. It should be noted that only a normal salt is used as the ammonium fluoride.
上記グリコール酸でニオブ等の金属の表面は酸化膜が形成される。この酸化膜をフッ化アンモニウムに電流を流すことによって削り取ることになる。グリコール酸およびフッ化アンモニウムは、劇物指定はされておらず、作業者の取り扱いは容易となる。加えて、研磨の仕上がり状態は濃硫酸とフッ酸を使用した場合と遜色はない。 The glycolic acid forms an oxide film on the surface of metal such as niobium. This oxide film is scraped off by applying an electric current to the ammonium fluoride. Glycolic acid and ammonium fluoride are not designated as deleterious substances, making them easy for workers to handle. In addition, the finished state of polishing is comparable to that obtained by using concentrated sulfuric acid and hydrofluoric acid.
＜基本＞
本発明は、３０質量％～９０質量％のグリコール酸にフッ化アンモニウムを外掛けで、２質量％～１０質量％添加した電解液を、金属（ニオブ、チタン、タンタル）の電解研磨に使用する。
<Basics>
The present invention uses an electrolytic solution in which 2% to 10% by mass of ammonium fluoride is added to 30% to 90% by mass of glycolic acid for electrolytic polishing of metals (niobium, titanium, tantalum).
上記の電解液で、まずグリコール酸が、金属表面を酸化して酸化膜を形成する。その酸化膜をフッ化アンモニウムで電解研磨することになる。 In the above electrolytic solution, glycolic acid first oxidizes the metal surface to form an oxide film. The oxide film is electrolytically polished with ammonium fluoride.
グリコール酸の濃度は３０質量％～９０質量％である。３０質量％より濃度が低いと、十分な酸化膜が得られない。酸化膜の厚みは９０質量％以上では濃度依存性はなく、それ以上に高い濃度にする必要はない。 The concentration of glycolic acid is 30% to 90% by weight. If the concentration is lower than 30% by mass, a sufficient oxide film cannot be obtained. When the thickness of the oxide film is 90 mass % or more, there is no concentration dependence, and it is not necessary to make the concentration higher than that.
電解研磨時の電圧を同じにしても、フッ化アンモニウムの濃度と浴温度に応じて電流が異なるところから、フッ化アンモニウムの濃度と浴温度は研磨レートを決定する要因となる。フッ化アンモニウムが外掛けで２質量％以下では、研磨レートが小さくなり、光沢性に劣ることになる。特に低温（室温以下）下ではその傾向が顕著に現れることになる。逆にフッ化アンモニウムが外掛けで１０質量％以上では、研磨レートが大きくなり、面荒れの原因になる。特に浴温度が５０℃以上ではこの傾向が大きくなる。 Even if the voltage during electropolishing is the same, the current varies depending on the concentration of ammonium fluoride and the bath temperature. Therefore, the concentration of ammonium fluoride and the bath temperature are the factors that determine the polishing rate. If the amount of ammonium fluoride is 2% by mass or less, the polishing rate will be low and the glossiness will be poor. Especially at low temperatures (below room temperature), this tendency appears remarkably. Conversely, if the amount of ammonium fluoride is 10% by mass or more, the polishing rate increases, causing surface roughness. Especially when the bath temperature is 50° C. or higher, this tendency increases.
電圧の研磨レートに及ぼす影響は浴温度より小さいが、研磨状態に影響する。高い電圧（例えば２５V）では小さい凹凸が緩和され、表面がスムーズになる傾向がある。 The effect of voltage on the polishing rate is smaller than that of the bath temperature, but it affects the polishing state. Higher voltages (eg, 25 V) tend to soften small irregularities and smooth the surface.
以上のことから、本発明の電解研磨は、グリコール酸濃度は３０～９０質量％、フッ化アンモニウムがグリコール酸溶液に対して外掛けで２～１０質量％、浴温度は室温から５０℃以下、電圧は２５V以下で実行される。 Based on the above, the electropolishing of the present invention is carried out at a glycolic acid concentration of 30 to 90% by mass, ammonium fluoride of 2 to 10% by mass with respect to the glycolic acid solution, a bath temperature of room temperature to 50° C. or less, and a voltage of 25 V or less.
＜実験１＞
本発明は、グリコール酸にフッ化アンモニウムを添加した電解液を、金属（ニオブ、チタン、タンタル）の電解研磨に使用する。ここでフッ化アンモニウムの量の影響を調べる目的で、７０質量％のグリコール酸(300ml)に、粉末のフッ化アンモニウムの量を１０g、１５g、２０gと変えて添加したサンプル液を用意した。グリコール酸100mlは１２３．２gであるので、粉末のフッ化アンモニウムの量１０g、１５g、２０gは、それぞれ、外掛けで２．７質量％、４．０質量％、５．４質量％となる
更に、フッ化アンモニウム添加量１０g、１５g、２０gについて各２種[(1)(2)] [(3)(4)] [(5)(6)]のサンプルを用意し、ニオブについて、電極間距離６ｃｍで電解研磨をした。尚、陽極は当然研磨対象となるニオブ、陰極もこの場合にオブを使用したが、白金等電解液で表面状態が変わらない物質であれば、特にこだわらない。
<
In the present invention, an electrolytic solution obtained by adding ammonium fluoride to glycolic acid is used for electrolytic polishing of metals (niobium, titanium, tantalum). Here, for the purpose of examining the effect of the amount of ammonium fluoride, sample solutions were prepared by adding 10 g, 15 g, and 20 g of powdered ammonium fluoride to 70% by mass glycolic acid (300 ml). Since 100 ml of glycolic acid is 123.2 g, the amounts of powdered ammonium fluoride of 10 g, 15 g, and 20 g are 2.7% by mass, 4.0% by mass, and 5.4% by mass respectively. did In this case, niobium was used as the anode and obium was used as the cathode.
各サンプル(1)～(6)について電流・電圧特性を調べると、図１に示すように、電流はフッ化アンモニウムの量が増えると大きくなるが、いずれのサンプルも電圧が８V以上でほぼフラットになる。すなわち、電流のフッ化アンモニウムの量への依存性は大きいが、電圧依存性は８V以上ではほとんど無い。尚、図１において、フッ化アンモニウム濃度が同じ（例えば、サンプル(3）と(4))であてもVI特性が若干異なるのは、浴温度が異なるためと考えられる（浴温度とVI特性との関係は後述する）。 Examining the current-voltage characteristics of each sample (1) to (6), as shown in Fig. 1, the current increases as the amount of ammonium fluoride increases, but all samples are almost flat at voltages of 8 V or higher. That is, although the dependence of the current on the amount of ammonium fluoride is large, there is almost no voltage dependence above 8V. In FIG. 1, even if the ammonium fluoride concentration is the same (for example, samples (3) and (4)), the VI characteristics are slightly different, probably because the bath temperature is different (the relationship between bath temperature and VI characteristics will be described later).
上記の確認を踏まえて、１０V以上の電圧で、各サンプルについて、研磨量のフッ化アンモニウムの濃度への依存性と浴温度への依存性を調べた結果を表１に示す。当該表１から得られた研磨量から算出される研磨レート(μｍ／ｍｉｎ)をグラフで表すと、図２の
ごとくになる。
Based on the above confirmation, Table 1 shows the results of examining the dependence of the polishing amount on the concentration of ammonium fluoride and the dependence of the bath temperature on each sample at a voltage of 10 V or higher. A graph of the polishing rate (μm/min) calculated from the polishing amount obtained from Table 1 is shown in FIG.
サンプル(1)(2)の対、(3)(4)の対、(5)(6)の対でフッ化アンモニウムの量が増えていることを考慮すると、研磨レートはフッ化アンモニウムの量に依存する。例えば温度が近似したサンプル(1)、(4)、(5)、あるいは、サンプル(2)、(3)、(6)を比較すると、研磨レートのフッ化アンモニウムの量への依存は顕著に示されている。また、上記各対を構成するサンプル（サンプル (3)と(4)、(5)と(6)）はそれぞれ浴温度が異なるので、研磨レートは浴温度にも依存することが理解できる。尚、サンプル(1)とサンプル(2)の研磨レートは同じになっているが、サンプル(1)、サンプル(2)はフッ化アンモニウムの量が2.7質量％と低いことと、サンプル (1)と(2)では温度差が他の２組と比べて少ないことで、研磨レートが同じになっているものと考えられる。 Considering that the amount of ammonium fluoride is increased in the pairs of samples (1)(2), (3)(4), and (5)(6), the polishing rate depends on the amount of ammonium fluoride. For example, comparing samples (1), (4), (5) or samples (2), (3), (6) with similar temperatures clearly shows the dependence of the polishing rate on the amount of ammonium fluoride. Moreover, since the samples constituting each pair (Samples (3) and (4), (5) and (6)) have different bath temperatures, it can be understood that the polishing rate also depends on the bath temperature. Although the polishing rates of sample (1) and sample (2) are the same, it is considered that the polishing rates of samples (1) and (2) are the same because the amount of ammonium fluoride in samples (1) and (2) is as low as 2.7% by mass, and the temperature difference between samples (1) and (2) is smaller than the other two pairs.
＜実験２＞
次いで、グリコール酸とフッ化アンモニウムの濃度を一定（グリコール酸(300ml)、フッ化アンモニウム(15g)）にし、温度を変えることによって、研磨レートの温度依存性を調べる実験をし、同時に同じ温度で電圧を変えることも行った。従って、サンプル(1) 室温、１５V、サンプル(2) 室温２５V、サンプル(3) ５０℃近辺１５V、サンプル(4) ５０℃近辺２５V、サンプル(5) ５℃近辺１５V、サンプル(6)５℃近辺２５Vの６種の実験をおこなった。
<
Next, an experiment was conducted to examine the temperature dependence of the polishing rate by changing the temperature while keeping the concentrations of glycolic acid and ammonium fluoride constant (glycolic acid (300ml), ammonium fluoride (15g)), and at the same time changing the voltage at the same temperature. Therefore, six types of experiments were conducted: sample (1) room temperature, 15 V, sample (2)
実験の時間的推移において、電流、温度の変化は図３（５０℃近辺）、図４（２０℃近辺）、図５（５℃近辺）に示す通りである。いずれの温度においても電圧が１５V（上段）より２５V（下段）のほうが電流は大きくなっているが、１５Vより２５Vのほうが５℃程度高い温度での実験であることを考慮する必要がある（特に５０℃と２０℃）。 Changes in current and temperature over time in the experiment are shown in FIG. 3 (around 50° C.), FIG. 4 (around 20° C.), and FIG. 5 (around 5° C.). At any temperature, the current is larger at 25V (lower) than at 15V (upper), but it is necessary to consider that the experiment was conducted at a temperature about 5°C higher at 25V than at 15V (especially 50°C and 20°C).
上記６種のサンプルについての実験の結果を表２に示し、当該表２の結果得られた研磨量に基づいて算出した研磨レートを図６に示す。 Table 2 shows the results of the experiments on the above six samples, and FIG. 6 shows the polishing rate calculated based on the polishing amount obtained as a result of Table 2.
図６において、室温（サンプル(1)(2)）、５０℃近辺（サンプル(3)、(4)）、５℃近辺（サンプル(5)、(6)）と、浴温度が高い方が研磨レートは高くなる。同じ温度の対（例えばサンプル(3)と(4)）で電圧が異なる場合も、研磨レートに差が出ているものの、電圧の依存性は温度依存性程大きくはないと考えられる。例えば、サンプル(4)(２５V)はサンプル(3)（１５V）よりも研磨量は多くなっているが、温度が数度高い状態での実験であることを考慮すると、研磨量の電圧依存性は、温度依存性より小さいものと考えられる。 In FIG. 6, the higher the bath temperature, the higher the room temperature (samples (1) and (2)), the higher the bath temperature (samples (3), (4)), the higher the polishing rate, the higher the temperature (samples (3), (4)), the higher the polishing rate. Even when the voltage is different for the same pair of temperatures (for example, samples (3) and (4)), although there is a difference in the polishing rate, the voltage dependence is not as large as the temperature dependence. For example, sample (4) (25 V) has a larger polishing amount than sample (3) (15 V), but considering that the experiment was conducted at a temperature several degrees higher, voltage dependence of the polishing amount is considered to be smaller than temperature dependence.
図７（写真）は、上記各サンプルでの実験の研磨の結果の操作顕微鏡による表面写真（倍率2000）である。上記したように電圧の相違は、温度の相違より研磨レートに与える影響は小さいが、表面状態には若干現れている。すなわち、同じ温度でも電圧の高い方が、凹凸の細かさは緩和されている。また、凹凸の細かさは温度が高いほうでも緩和されている。 FIG. 7 (photograph) is a surface photograph (magnification: 2000) taken with an operating microscope of the result of polishing in the experiment on each of the above samples. As described above, the difference in voltage has a smaller effect on the polishing rate than the difference in temperature, but it appears in the surface condition to some extent. That is, even at the same temperature, the higher the voltage, the less fine the unevenness. Also, the fineness of the unevenness is moderated even at higher temperatures.
＜実験３＞
グリコール酸の７０重量％の溶液（３００ml）に対して、更に粉末グリコール酸を１０ｇ添加し濃度を高め、フッ化アンモニウム(１５g)を更に添加したサンプル液を用意する。この溶液に対してサンプル(1)、室温、１５V、１時間、サンプル(2)、室温、2５V、１時間、サンプル(3)、５０℃、2５V、２０分で電解研磨をした。それぞれ実験２のサンプル(1)、サンプル(2)、サンプル(4)に相当する。
<
A sample solution was prepared by adding 10 g of powdered glycolic acid to a 70% by weight solution (300 ml) of glycolic acid to increase the concentration, and further adding ammonium fluoride (15 g). This solution was electropolished at room temperature, 15 V for 1 hour, sample (2) at room temperature at 25 V for 1 hour, and sample (3) at 50° C., 25 V for 20 minutes. They correspond to samples (1), (2), and (4) of
研磨量は表３に示す通りであり、研磨レートは図８に示すように、上記実験２のサンプル(1)、サンプル(2)、サンプル(4)の結果とほぼ同等であり、グリコール酸の濃度の差による研磨レートの顕著な相違は見られなかった。尚、サンプル(1)とサンプル(2)の研磨レートの相違は、電圧の相違もあるが、どちらかというと温度の差によるものと考えられる。
The amount of polishing is as shown in Table 3, and the polishing rate, as shown in FIG. 8, is almost the same as the results of Samples (1), (2), and (4) in
尚、上記図２、図６、図８において、比較基準として濃硫酸＋フッ酸による研磨レートを示している。電圧は１０V、室温濃硫酸とフッ酸の比率は９：１程度である。 2, 6, and 8, the polishing rate with concentrated sulfuric acid and hydrofluoric acid is shown as a reference for comparison. The voltage is 10 V, and the ratio of concentrated sulfuric acid to hydrofluoric acid at room temperature is about 9:1.
以上説明したように、表面の光沢性は多少劣るものの、従来の濃硫酸とフッ酸を用いたニオブの電解研磨に代えて、有機酸であるグリコール酸を用いることができ、しかも従来の従来と同等のパーフォーマンスを得ることができ、より安全に作業を進めることができる。 As described above, although the glossiness of the surface is somewhat inferior, glycolic acid, which is an organic acid, can be used in place of the conventional electropolishing of niobium using concentrated sulfuric acid and hydrofluoric acid.
１００・・空洞管 100... Hollow tube
Claims (1)
することを特徴とする電解研磨方法。 At least one of niobium, titanium, and tantalum is added to an electrolytic solution in which only 2 to 10% by mass of ammonium fluoride orthosalt is dissolved in a 30 to 90% by mass glycolic acid solution, at a temperature of room temperature to 50 ° C. When the distance between the electrodes is 6 cm, the voltage is 25 V or less for 30 minutes or more.
An electropolishing method characterized by :
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| JP2006526071A (en) | 2003-05-09 | 2006-11-16 | ポリグラト−ホールディング ゲーエムベーハー | Electrolyte for electrochemical polishing of metal surfaces |
| JP2009108405A (en) | 2007-10-10 | 2009-05-21 | Ebara Corp | Electrolytic polishing method and apparatus of substrate |
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