JP5095558B2 - Hybrid substrate cleaning method - Google Patents
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Description
本発明は、異種基板同士を貼り合わせたハイブリッド基板の洗浄方法に関する。 The present invention relates to a method for cleaning a hybrid substrate in which different substrates are bonded together.
ＳＯＩ（Ｓｉｌｉｃｏｎ Ｏｎ Ｉｎｓｕｌａｔｏｒ）基板は半導体素子において接合容量の低減やリーク電流の抑制、高周波特性などの効果からパワーデバイスや高周波デバイスなどの用途に用いられている。 SOI (Silicon On Insulator) substrates are used in applications such as power devices and high-frequency devices because of effects such as reduction of junction capacitance, suppression of leakage current, and high-frequency characteristics in semiconductor elements.
このようなＳＯＩ基板表面への汚染物質の付着は、半導体デバイスの歩留まりやデバイス特性を低下させる要因となっており、半導体基板の清浄度を向上させるために洗浄を行う必要がある。
特にＳＯＩ基板中に含まれる金属は、例えばＤＲＡＭ等のデバイスではゲート酸化膜の絶縁破壊や信頼性不良などをもたらす原因となる。
Such adhesion of contaminants to the surface of the SOI substrate is a factor that degrades the yield and device characteristics of the semiconductor devices, and it is necessary to perform cleaning in order to improve the cleanliness of the semiconductor substrate.
In particular, the metal contained in the SOI substrate causes a dielectric breakdown of the gate oxide film or a poor reliability in a device such as a DRAM.
これらのような、半導体基板の洗浄としては、フッ酸水溶液を用いたものや（特許文献１参照）、ＲＣＡ洗浄法を用いたものがある。 Such semiconductor substrate cleaning includes those using an aqueous hydrofluoric acid solution (see Patent Document 1) and those using an RCA cleaning method.
しかし、ＳＯＩ基板の一種であるＳＯＱ（Ｓｉｌｉｃｏｎ Ｏｎ Ｑｕａｒｔｚ）基板やＳＯＳ（Ｓｉｌｉｃｏｎ Ｏｎ Ｓａｐｐｈｉｒｅ）基板などの異種の基板を貼り合せたハイブリッド基板では、活性層と支持基板とでは性質が異なるため、洗浄において、片面では汚れが除去されてその再付着が抑制されていても、もう一方の面では汚れが再付着しやすくなって、洗浄による基板の清浄度が十分でないといった問題があった。 However, in a hybrid substrate in which different types of substrates such as an SOI substrate (SOQ (Silicon On Quartz) substrate and SOS (Silicon On Sapphire) substrate) are bonded, the properties of the active layer and the support substrate are different. Even if the dirt is removed on one side and its re-adhesion is suppressed, the dirt tends to re-adhere on the other side, and there is a problem that the cleanliness of the substrate by cleaning is not sufficient.
また、透明絶縁基板である石英基板やサファイア基板を支持基板として用いているため光が透過してしまい、基板表面上のパーティクルを測定する際に用いられる光散乱式パーティクルカウンターでは表面のパーティクルを測定できず、清浄度を確認することができないため、洗浄により汚染物が除去できたかの確認ができないことも問題となる。 In addition, the quartz substrate or sapphire substrate, which is a transparent insulating substrate, is used as a support substrate, so light is transmitted, and the light scattering particle counter used when measuring particles on the substrate surface measures the particles on the surface. In other words, the degree of cleanliness cannot be confirmed, and it is also a problem that it cannot be confirmed whether or not contaminants have been removed by washing.
そこで本発明は、上記問題点に鑑みてなされたものであって、異種の基板同士を貼り合わせることにより表裏面の性質が異なるハイブリッド基板を洗浄する際に、除去された汚染物の再付着を防止することができ、さらには洗浄後の基板の清浄度を間接的に確認できる洗浄方法を提供する。 Therefore, the present invention has been made in view of the above problems, and when the hybrid substrates having different front and back surface properties are bonded to each other by bonding different substrates, the removed contaminants are reattached. Provided is a cleaning method that can be prevented and that can indirectly check the cleanliness of the substrate after cleaning.
上記目的を達成するために、本発明は、活性層となる半導体基板と、該活性層用半導体基板とは異種の支持基板とを貼り合せたハイブリッド基板の洗浄方法であって、少なくとも、洗浄液中で前記ハイブリッド基板の支持基板表面のゼータ電位と反対符号の電位を有するダミー基板と、前記ハイブリッド基板を交互に配置した状態で、前記洗浄液中に浸漬させて洗浄することを特徴とするハイブリッド基板の洗浄方法を提供する（請求項１）。 In order to achieve the above object, the present invention provides a method for cleaning a hybrid substrate in which a semiconductor substrate to be an active layer and a support substrate of a different type from the semiconductor substrate for the active layer are bonded, at least in a cleaning liquid In the hybrid substrate, the dummy substrate having a potential opposite to the zeta potential on the surface of the supporting substrate of the hybrid substrate and the hybrid substrate are alternately arranged and immersed in the cleaning liquid for cleaning. A cleaning method is provided (claim 1).
このように、本発明の洗浄方法によれば、洗浄により基板から脱離して洗浄液中で遊離している汚染物が、洗浄液中で支持基板表面のゼータ電位と反対符号の電位を有するダミー基板に吸着されて、ハイブリッド基板への汚染物の再付着を防止することができる。特に、支持基板と活性層が異なるゼータ電位を示すような洗浄液中において、遊離した汚染物が一方の面へ吸着されるのを防止することができ、効率良く洗浄を行うことができる。このため、本発明の洗浄方法であれば、洗浄液によるハイブリッド基板の表裏面の性質の違いは考慮する必要が無く、支持基板のゼータ電位の反対符号のダミー基板と、洗浄する基板を交互に配置するのみで汚染物の再付着防止を図ることができるため、使用する洗浄液の選択の幅が広がり、効果的な洗浄を行うことができ、それにより清浄度の高いハイブリッド基板にすることができる。 Thus, according to the cleaning method of the present invention, contaminants that are detached from the substrate by cleaning and released in the cleaning liquid are transferred to the dummy substrate having a potential opposite to the zeta potential of the support substrate surface in the cleaning liquid. By being adsorbed, it is possible to prevent reattachment of contaminants to the hybrid substrate. In particular, in a cleaning solution in which the support substrate and the active layer exhibit different zeta potentials, it is possible to prevent adsorbed contaminants from being adsorbed to one surface, and cleaning can be performed efficiently. For this reason, in the cleaning method of the present invention, there is no need to consider the difference in the properties of the front and back surfaces of the hybrid substrate due to the cleaning liquid, and the dummy substrate having the opposite sign of the zeta potential of the support substrate and the substrate to be cleaned are alternately arranged. Therefore, it is possible to prevent the reattachment of contaminants, so that the range of cleaning liquids to be used can be widened and effective cleaning can be performed, whereby a hybrid substrate with high cleanliness can be obtained.
このとき、前記洗浄されるハイブリッド基板の前記活性層となる半導体基板をシリコン基板とし、前記支持基板を石英基板又はサファイヤ基板とすることが好ましい（請求項２）。
このように、シリコンと石英、サファイヤのような洗浄液によってはゼータ電位の符号が異なり、一方の面へ汚染物が付着しやすいハイブリッド基板の場合でも、本発明の洗浄方法によれば、洗浄液中に遊離した汚染物をダミー基板が吸着し、ハイブリッド基板への汚染物の再付着を効果的に防止することができるため好適である。また、特に汚染物が付着しやすい石英やサファイヤのような絶縁物であっても本発明の洗浄方法を用いれば、汚染物の除去及びその再付着の防止ができるため、高い清浄度に洗浄することができる。
At this time, it is preferable that the semiconductor substrate to be the active layer of the hybrid substrate to be cleaned is a silicon substrate, and the support substrate is a quartz substrate or a sapphire substrate.
Thus, the sign of the zeta potential differs depending on the cleaning liquid such as silicon, quartz, and sapphire, and even in the case of a hybrid substrate in which contaminants are likely to adhere to one surface, according to the cleaning method of the present invention, It is preferable because the dummy substrate adsorbs the released contaminants and effectively prevents the contaminants from reattaching to the hybrid substrate. Moreover, even if it is an insulator such as quartz or sapphire, which easily adheres to contaminants, the cleaning method of the present invention can be used to remove contaminants and prevent their reattachment. be able to.
このとき、前記ダミー基板を、シリコン基板とすることが好ましい（請求項３）。
このように、本発明の洗浄方法に用いるダミー基板としては、洗浄液中でハイブリッド基板の支持基板のゼータ電位と反対符号の電位を有する基板であればよいため、その条件に合致する場合には、汚染源とはならないし比較的安価であるシリコン基板とすることが好ましい。
At this time, the dummy substrate is preferably a silicon substrate.
As described above, the dummy substrate used in the cleaning method of the present invention may be a substrate having a potential opposite to the zeta potential of the support substrate of the hybrid substrate in the cleaning liquid. It is preferable to use a silicon substrate which is not a source of contamination and is relatively inexpensive.
このとき、前記洗浄液を、少なくともフッ化水素酸、過酸化水素及びクエン酸が含まれていて、ｐＨが１〜４である溶液とすることができる（請求項４）。
このような洗浄液中では、ハイブリッド基板の活性層と支持基板の種類によってはゼータ電位の符号が異なるため、一方の面に除去された汚染物が再付着しやすくなるが、本発明の洗浄方法によって効果的に再付着を防止でき、また、このような洗浄液は金属汚染物を容易に除去することができ、さらにクエン酸は汚染物の再付着防止効果も有するため、清浄度がより高いハイブリッド基板とすることができる。
At this time, the cleaning liquid may be a solution containing at least hydrofluoric acid, hydrogen peroxide and citric acid and having a pH of 1 to 4.
In such a cleaning liquid, the sign of the zeta potential differs depending on the type of the active layer and the support substrate of the hybrid substrate, so that contaminants removed on one surface are likely to be reattached. Hybrid substrate that can effectively prevent re-adhesion, can easily remove metal contaminants, and citric acid also has the effect of preventing re-adhesion of contaminants. It can be.
このとき、前記洗浄後のダミー基板表面をパーティクル測定して、該測定結果により前記洗浄されたハイブリッド基板の清浄度を確認することが好ましい（請求項５）。
このように、洗浄後のダミー基板表面をパーティクル測定することにより、その測定結果と相関関係にあるハイブリッド基板の清浄度を間接的に測ることができる。また、洗浄するハイブリッド基板の支持基板が透明基板の場合のような、光が透過してパーティクルを直接測定することが困難な基板であっても、上記のように間接的に清浄度を確認することができるため、より確実に所望の清浄度まで洗浄することができる。
At this time, it is preferable to measure particles on the surface of the dummy substrate after the cleaning and confirm the cleanliness of the cleaned hybrid substrate based on the measurement result.
Thus, by measuring particles on the cleaned dummy substrate surface, the cleanliness of the hybrid substrate correlated with the measurement result can be indirectly measured. In addition, even if the substrate to be cleaned is a transparent substrate and the substrate is difficult to directly measure particles through light transmission, the cleanness is indirectly confirmed as described above. Therefore, it can wash | clean to a desired cleanliness more reliably.
以上のように、本発明の洗浄方法によれば、異種基板同士を貼り合わせたハイブリッド基板を洗浄する際に、除去されて洗浄液中に遊離した汚染物を、洗浄液中で支持基板表面のゼータ電位と反対符号の電位を有するダミー基板により吸着させることができる。これにより、ハイブリッド基板の表裏面の性質の違いにより、異なるゼータ電位を示すような場合でも、一方の面への汚染物の付着を効果的に防止することができる。このような本発明の洗浄方法であれば、ハイブリッド基板の表裏面の性質の違いは関係なく、ダミー基板と支持基板のゼータ電位を反対符号のものとし、交互に配置するのみで汚染物の再付着防止を図ることができるため、使用する洗浄液の選択の幅が広がり、効果的な洗浄を行うことができ、それにより清浄度の高いハイブリッド基板にすることができる。また、このような洗浄に用いたダミー基板をパーティクル測定することで、洗浄するハイブリッド基板の支持基板が透明基板であるような直接パーティクル測定するのが困難な場合でも、間接的に清浄度を測ることができるため、より確実に所望の清浄度まで洗浄することができる。 As described above, according to the cleaning method of the present invention, when cleaning a hybrid substrate in which different substrates are bonded to each other, contaminants that have been removed and released into the cleaning liquid are removed from the zeta potential of the support substrate surface in the cleaning liquid. Can be adsorbed by a dummy substrate having a potential opposite to that of. Thereby, even when different zeta potentials are shown due to the difference in the properties of the front and back surfaces of the hybrid substrate, it is possible to effectively prevent contamination from adhering to one surface. With such a cleaning method of the present invention, the zeta potentials of the dummy substrate and the support substrate are of the opposite signs, regardless of the difference in the properties of the front and back surfaces of the hybrid substrate, and the contaminants can be recovered by simply arranging them alternately. Since it is possible to prevent adhesion, the range of selection of the cleaning liquid to be used is widened, and effective cleaning can be performed, whereby a hybrid substrate with high cleanliness can be obtained. In addition, by measuring particles on the dummy substrate used for such cleaning, even if it is difficult to measure particles directly, such as when the supporting substrate of the hybrid substrate to be cleaned is a transparent substrate, the cleanliness is measured indirectly. Therefore, it can wash | clean to a desired cleanliness more reliably.
異種の基板を貼り合せたハイブリッド基板の活性層と支持基板とでは、表面電位などの性質が異なるため、洗浄において除去された汚染物の再付着が片面では抑制されていても、もう片方の面では汚染物が再付着しやすく、洗浄を効率的に行うことができないといった問題があった。
この問題を解決するために、本発明者らが以下のような検討を行った。
The active layer of the hybrid substrate with different substrates bonded to the support substrate has different properties such as surface potential, so even if the reattachment of contaminants removed during cleaning is suppressed on one side, the other side However, there is a problem that contaminants are easily reattached and cleaning cannot be performed efficiently.
In order to solve this problem, the present inventors have studied as follows.
異種の基板からなるハイブリッド基板の洗浄において、例えばＳＯＱ基板では、ｐＨが４以下の酸性の洗浄液中において、支持基板であるＳｉＯ２表面と活性層であるＳｉ表面のゼータ電位は反対の符号を有することが多く、このため例えばＲＣＡ洗浄で金属不純物除去のため用いられる塩酸と過酸化水素の混合溶液からなるＳＣ−２洗浄液の酸性溶液中において、支持基板側では汚染物、特に金属が脱離しやすくなる一方、活性層側では吸着しやすくなり、汚染物の除去が困難になる。 In the cleaning of a hybrid substrate made of different types of substrates, for example, in an SOQ substrate, the zeta potentials of the SiO 2 surface as a support substrate and the Si surface as an active layer have opposite signs in an acidic cleaning solution having a pH of 4 or less. For this reason, for example, in an acidic solution of SC-2 cleaning solution composed of a mixed solution of hydrochloric acid and hydrogen peroxide used for removing metal impurities in RCA cleaning, contaminants, particularly metal, are easily detached on the support substrate side. On the other hand, it becomes easy to adsorb on the active layer side, and it becomes difficult to remove contaminants.
また、ｐＨが５以上の洗浄液では、支持基板であるＳｉＯ２表面と活性層であるＳｉ表面のゼータ電位は同符号となることが多いが、例えばＲＣＡ洗浄で不純物除去のために用いられるアンモニア水と過酸化水素の混合溶液からなるＳＣ−１洗浄液では、パーティクル除去効果は有するものの、鉄等の金属はこのようなアルカリ溶液中では酸化物や水酸化物として安定に存在し、ＳＣ−１洗浄液中でＳｉ表面に形成される酸化膜中に取り込まれたりするため、金属除去能力は低い。 In addition, in a cleaning solution having a pH of 5 or more, the zeta potential of the SiO 2 surface serving as the support substrate and the Si surface serving as the active layer often have the same sign. For example, ammonia water used for removing impurities in RCA cleaning SC-1 cleaning solution comprising a mixed solution of hydrogen and hydrogen peroxide has a particle removal effect, but metals such as iron are stably present as oxides and hydroxides in such an alkaline solution, and the SC-1 cleaning solution Among them, the metal removal ability is low because it is taken into the oxide film formed on the Si surface.
上述のような検討の結果、本発明者らは、ハイブリッド基板の洗浄において、洗浄液中で支持基板表面のゼータ電位と反対符号の電位を有するダミー基板を、ハイブリッド基板と交互に配置して洗浄することで、洗浄液中に遊離した汚染物をダミー基板に吸着させて捕集し、ハイブリッド基板への再付着を防止することができることを見出し、さらに、その洗浄後のダミー基板のパーティクル測定によりハイブリッド基板の清浄度を間接的に確認できることを見出し、本発明を完成させた。 As a result of the above-described studies, the inventors cleaned the hybrid substrate by alternately arranging dummy substrates having a potential opposite to the zeta potential on the surface of the supporting substrate in the cleaning liquid. In this way, it is found that the contaminants released in the cleaning liquid can be adsorbed and collected on the dummy substrate and prevented from reattaching to the hybrid substrate, and further, the hybrid substrate can be measured by particle measurement of the dummy substrate after the cleaning. The present inventors have found that the cleanliness can be indirectly confirmed.
以下、本発明の洗浄方法について、実施態様の一例として、図１を参照しながら詳細に説明するが、本発明はこれに限定されるものではない。
図１は、本発明の実施態様の一例として洗浄カセットに基板を配置した状態を示す概略図である。
Hereinafter, although the washing | cleaning method of this invention is demonstrated in detail, referring FIG. 1 as an example of an embodiment, this invention is not limited to this.
FIG. 1 is a schematic view showing a state in which a substrate is arranged in a cleaning cassette as an example of an embodiment of the present invention.
本発明の洗浄方法では、図１に示すように、活性層３とそれとは異種の支持基板２を貼り合わせたハイブリッド基板５と、洗浄液中でハイブリッド基板５の支持基板３表面のゼータ電位と反対符号の電位を有するダミー基板４を、洗浄カセット１に交互に配置した状態で収納し、これを洗浄液中に浸漬させて洗浄する。
In the cleaning method of the present invention, as shown in FIG. 1, the
このように、本発明の洗浄方法によれば、表裏面が異なる性質を有するハイブリッド基板の洗浄において、特に、洗浄液によっては表裏面でゼータ電位が反対符号を示す場合でも、支持基板とゼータ電位が反対符号のダミー基板をハイブリッド基板と交互に配置するため、ダミー基板が汚染物を吸着して捕集材の働きをし、効果的に洗浄を行うことができる。 Thus, according to the cleaning method of the present invention, in the cleaning of the hybrid substrate having different properties on the front and back surfaces, the support substrate and the zeta potential are different even when the zeta potential shows opposite signs on the front and back surfaces depending on the cleaning liquid. Since the dummy substrates with the opposite signs are alternately arranged with the hybrid substrate, the dummy substrates can adsorb contaminants and act as a trapping material, so that cleaning can be performed effectively.
このような本発明の洗浄方法を適用できるハイブリッド基板５の種類、サイズとしては特に限定されず、目的により適宜選択できるが、種類としては、例えば活性層３となる半導体基板をシリコン基板とし、支持基板２を石英基板又はサファイヤ基板としたハイブリッド基板が好ましい。
このようなハイブリッド基板は、酸性の洗浄液中において活性層と支持基板でゼータ電位が反対符号を示すことが多く、この場合でも本発明によれば、除去された汚染物はダミー基板により吸着されるため、一方の面への汚染物の再付着を防止することができ、本発明の洗浄方法を適用するには好適である。
The type and size of the hybrid substrate 5 to which the cleaning method of the present invention can be applied are not particularly limited and can be appropriately selected depending on the purpose. For example, the semiconductor substrate to be the
In such a hybrid substrate, the zeta potential of the active layer and the support substrate often shows opposite signs in an acidic cleaning solution. Even in this case, according to the present invention, the removed contaminants are adsorbed by the dummy substrate. Therefore, it is possible to prevent the reattachment of contaminants on one surface, which is suitable for applying the cleaning method of the present invention.
このとき、ダミー基板４としても、洗浄液中でハイブリッド基板の支持基板表面のゼータ電位と反対符号の電位を有するものであれば、特に限定されないが、例えばシリコン基板とすることが好ましい。シリコン基板であれば、きわめて清浄なものを比較的安価で入手できるため好適である。
また、このダミー基板４としては、低欠陥の基板であることが好ましい。低欠陥であれば、洗浄後の清浄度の確認の際に、洗浄時にどれだけの汚染物が付着したかをより正確に把握できる。
At this time, the dummy substrate 4 is not particularly limited as long as it has a potential opposite to the zeta potential on the surface of the support substrate of the hybrid substrate in the cleaning liquid. A silicon substrate is preferable because a very clean substrate can be obtained at a relatively low cost.
The dummy substrate 4 is preferably a low defect substrate. If the defect is low, it is possible to more accurately grasp how much contaminants have adhered during cleaning when checking the cleanliness after cleaning.
このとき、本発明で用いられる洗浄液としては、特に限定されないが、例えば塩酸やフッ化水素酸と過酸化水素などの酸性の洗浄液、特には、少なくともフッ化水素酸、過酸化水素及びクエン酸からなり、溶液のｐＨが１〜４である洗浄液とすることができる。
例えばＳＯＱ基板やＳＯＳ基板においては、酸性溶液中で、活性層のシリコンは負の表面電位を、支持基板の石英やサファイアは正の表面電位を持つことが多い。そのため、酸性溶液中において正の電位を有する金属酸化物等の汚染物が存在すると、支持基板側からは脱離しやすくなるが活性層側に吸着しやすくなり、汚染物の除去効率が低下してしまう。
このような場合でも、本発明の洗浄方法によれば、交互に配置されたダミー基板が洗浄液中に遊離する汚染物を吸着して、ハイブリッド基板への再付着が防止されるため、上記のような洗浄液を用いて、金属汚染物を除去しながら、その再付着を防止することができ、ハイブリッド基板の清浄度をより高くすることができる。
At this time, the cleaning liquid used in the present invention is not particularly limited, but an acidic cleaning liquid such as hydrochloric acid, hydrofluoric acid and hydrogen peroxide, in particular, at least from hydrofluoric acid, hydrogen peroxide and citric acid. Thus, the cleaning liquid having a pH of 1 to 4 can be obtained.
For example, in an SOQ substrate or SOS substrate, in an acidic solution, silicon in the active layer often has a negative surface potential, and quartz or sapphire in the support substrate often has a positive surface potential. Therefore, if there is a contaminant such as a metal oxide having a positive potential in the acidic solution, it tends to be detached from the support substrate side but easily adsorbed to the active layer side, and the contaminant removal efficiency is reduced. End up.
Even in such a case, according to the cleaning method of the present invention, the dummy substrates arranged alternately absorb the contaminants released in the cleaning liquid and prevent reattachment to the hybrid substrate. With this cleaning solution, it is possible to prevent re-deposition while removing metal contaminants, and to increase the cleanliness of the hybrid substrate.
さらに、これらのような酸性の洗浄液の中でも鉄等の金属汚染除去効果が高いフッ化水素酸に、酸化剤として過酸化水素を加えることで、汚染物の除去効率をより高めることができ、ここにクエン酸に代表されるキレート効果を有する試薬を加えることで、脱離した汚染物の基板表面への再付着をさらに抑制することができるため、汚染物の除去効果をより高めることができる。 Furthermore, by adding hydrogen peroxide as an oxidizing agent to hydrofluoric acid, which has a high metal contamination removal effect such as iron, among these acidic cleaning liquids, the removal efficiency of contaminants can be further increased. By adding a reagent having a chelate effect typified by citric acid, it is possible to further suppress the reattachment of the desorbed contaminants to the substrate surface, so that the contaminant removal effect can be further enhanced.
この洗浄液の組成比としては、特に限定されず、被洗浄基板の種類や汚染度に応じ適宜選択することができ、必要に応じて界面活性剤等を添加しても良い。また洗浄液への浸漬時間は特に制限されないが、洗浄効果やスループットを考慮すると３分〜６０分であることが好ましい。 The composition ratio of the cleaning liquid is not particularly limited and can be appropriately selected according to the type of the substrate to be cleaned and the degree of contamination. A surfactant or the like may be added as necessary. The immersion time in the cleaning liquid is not particularly limited, but is preferably 3 minutes to 60 minutes in consideration of the cleaning effect and throughput.
ハイブリッド基板を上記洗浄液に浸漬後、ＲＣＡ洗浄を続けて行うことができる。この場合も、ダミー基板を交互に配置しておくことでハイブリッド基板を高清浄度に洗浄することができる。ＲＣＡ洗浄においては例えば洗浄液としてＳＣ−１（ＮＨ４ＯＨ＋Ｈ２Ｏ２＋Ｈ２Ｏ）及びＳＣ−２（ＨＣｌ＋Ｈ２Ｏ２＋Ｈ２Ｏ）を用い、これらの洗浄液と純水への浸漬を交互に行うことができる。ＳＣ−１溶液及びＳＣ−２溶液の組成は適宜選択できる。また目的に応じ、ＳＣ−１溶液とＳＣ−２溶液に加えて硫酸等の洗浄液も適宜使用することができる。また純水のかわりに、オゾン水や水素水といった機能水を使用しても良い。 After the hybrid substrate is immersed in the cleaning solution, the RCA cleaning can be continued. Also in this case, the hybrid substrate can be cleaned with high cleanliness by arranging the dummy substrates alternately. In RCA cleaning, for example, SC-1 (NH 4 OH + H 2 O 2 + H 2 O) and SC-2 (HCl + H 2 O 2 + H 2 O) are used as cleaning liquids, and these cleaning liquids and immersion in pure water are alternately performed. be able to. The composition of the SC-1 solution and the SC-2 solution can be appropriately selected. In addition to the SC-1 solution and the SC-2 solution, a cleaning solution such as sulfuric acid can be appropriately used depending on the purpose. Functional water such as ozone water or hydrogen water may be used instead of pure water.
以上のように、本発明の洗浄方法により洗浄されたハイブリッド基板５の清浄度を確認するため、洗浄後のダミー基板４表面をパーティクル測定して、その測定結果により、洗浄されたハイブリッド基板５の清浄度を確認することができる。
このように、洗浄されたハイブリッド基板の清浄度を、ダミー基板表面のパーティクル測定の結果により間接的に確認することができる。これは、洗浄後のダミー基板のパーティクル数は洗浄されたハイブリッド基板と比例関係が見られるからである。これにより、特に透明基板等のような光が透過してパーティクル測定が困難な基板の清浄度を正確に簡便な方法で確認することができ、より確実に所望の清浄度にすることができる。
As described above, in order to check the cleanliness of the hybrid substrate 5 cleaned by the cleaning method of the present invention, the surface of the dummy substrate 4 after cleaning is subjected to particle measurement, and the measurement result of the cleaned hybrid substrate 5 The cleanliness can be confirmed.
In this way, the cleanliness of the cleaned hybrid substrate can be indirectly confirmed from the result of particle measurement on the surface of the dummy substrate. This is because the number of particles on the dummy substrate after cleaning is proportional to the cleaned hybrid substrate. Thereby, the cleanliness of a substrate that is particularly difficult to measure particles due to the transmission of light such as a transparent substrate can be confirmed accurately by a simple method, and the desired cleanliness can be achieved more reliably.
以下、本発明を実施例、比較例によりさらに具体的に説明するが、本発明はこれに限定されない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further more concretely, this invention is not limited to this.
（実施例）
活性層をシリコン、支持基板を石英として貼り合せたハイブリッド基板（ＳＯＱ基板）とダミー基板としてシリコン基板を、洗浄カセットに交互に配置した状態で収納した。
１％フッ化水素酸、２％過酸化水素水及び２％クエン酸を混合したｐＨが１〜２の洗浄液に上記ハイブリッド基板及びダミー基板を洗浄カセットごと３０分浸漬し、純水リンス後、乾燥を行った。なお、この洗浄液中ではシリコン（ダミー基板）と石英（支持基板）はゼータ電位が反対符号であった。
(Example)
A hybrid substrate (SOQ substrate) bonded with silicon as the active layer and quartz as the support substrate and a silicon substrate as a dummy substrate were housed alternately in the cleaning cassette.
Immerse the hybrid substrate and dummy substrate in a cleaning solution with a pH of 1-2 mixed with 1% hydrofluoric acid, 2% hydrogen peroxide, and 2% citric acid for 30 minutes together with the cleaning cassette, rinse with pure water, and dry Went. In this cleaning solution, zeta potentials of silicon (dummy substrate) and quartz (support substrate) had opposite signs.
（比較例１）
活性層をシリコン、支持基板を石英として貼り合せたハイブリッド基板（ＳＯＱ基板）とダミー基板としてシリコン基板を、洗浄カセットに交互に配置した状態で収納した。
ｐＨが２〜３である２％クエン酸の洗浄液に上記ハイブリッド基板及びダミー基板を３０分浸漬し、純水リンス後、乾燥を行った。なお、この洗浄液中ではシリコン（ダミー基板）と石英（支持基板）はゼータ電位が同符号であった。
(Comparative Example 1)
A hybrid substrate (SOQ substrate) bonded with silicon as the active layer and quartz as the support substrate and a silicon substrate as a dummy substrate were housed alternately in the cleaning cassette.
The hybrid substrate and the dummy substrate were immersed in a 2% citric acid cleaning solution having a pH of 2 to 3 for 30 minutes, rinsed with pure water, and then dried. In this cleaning solution, silicon (dummy substrate) and quartz (support substrate) have the same zeta potential.
（比較例２）
活性層をシリコン、支持基板を石英として貼り合せたハイブリッド基板（ＳＯＱ基板）とダミー基板としてシリコン基板を、洗浄カセットに交互に配置した状態で収納した。
１％フッ化水素酸及び２％過酸化水素水を混合したｐＨが１〜２の洗浄液に上記ハイブリッド基板及びダミー基板を３０分浸漬し、純水リンス後、乾燥を行った。なお、この洗浄液中ではシリコン（ダミー基板）と石英（支持基板）はゼータ電位が同符号であった。
(Comparative Example 2)
A hybrid substrate (SOQ substrate) bonded with silicon as the active layer and quartz as the support substrate and a silicon substrate as a dummy substrate were housed alternately in the cleaning cassette.
The hybrid substrate and the dummy substrate were immersed in a cleaning solution having a pH of 1 to 2 in which 1% hydrofluoric acid and 2% hydrogen peroxide water were mixed for 30 minutes, rinsed with pure water, and then dried. In this cleaning solution, silicon (dummy substrate) and quartz (support substrate) have the same zeta potential.
洗浄後に、ダミー基板であるシリコン基板表面のパーティクル数を、表面検査装置を用いて測定すると、実施例の場合は０．１９μｍ以上のパーティクル数が平均１５個であった。
一方、比較例１、２の場合は０．１９μｍ以上のパーティクル数が平均３７個、４２個であった。
After cleaning, when the number of particles on the surface of the silicon substrate, which is a dummy substrate, was measured using a surface inspection apparatus, the number of particles of 0.19 μm or more was an average of 15 in the case of the example.
On the other hand, in Comparative Examples 1 and 2, the average number of particles of 0.19 μm or more was 37 and 42.
また、洗浄後のＳＯＱ基板の活性層表面のＦｅ濃度を全反射蛍光Ｘ線ウェーハ表面分析装置を用いて調べると、実施例では検出下限以下であった。
一方、比較例１では１．６×１０１０ａｔｏｍ／ｃｍ２、比較例２では１．１×１０１０ａｔｏｍ／ｃｍ２であった。
以上より、本発明の洗浄方法によれば、パーティクルと金属汚染の低減を効果的に達成できていることがわかる。これらの結果を表１に示した。
Further, when the Fe concentration on the surface of the active layer of the cleaned SOQ substrate was examined using a total reflection fluorescent X-ray wafer surface analyzer, it was below the lower limit of detection in the examples.
On the other hand, it was 1.6 × 10 10 atoms / cm 2 in Comparative Example 1 and 1.1 × 10 10 atoms / cm 2 in Comparative Example 2.
From the above, it can be seen that the cleaning method of the present invention can effectively reduce particles and metal contamination. These results are shown in Table 1.
なお、本発明は、上記実施形態に限定されるものではない。上記実施形態は、例示であり、本発明の特許請求の範囲に記載された技術的思想と実質的に同一な構成を有し、同様な作用効果を奏するものは、いかなるものであっても本発明の技術的範囲に包含される。 The present invention is not limited to the above embodiment. The above-described embodiment is an exemplification, and the present invention has substantially the same configuration as the technical idea described in the claims of the present invention, and any device that exhibits the same function and effect is the present invention. It is included in the technical scope of the invention.
１…洗浄カセット、 ２…支持基板、 ３…活性層、
４…ダミー基板、 ５…ハイブリッド基板。
1 ... cleaning cassette, 2 ... support substrate, 3 ... active layer,
4 ... dummy substrate, 5 ... hybrid substrate.
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