JP2018012752A - Polishing agent, storage liquid for polishing agent and polishing method - Google Patents
Polishing agent, storage liquid for polishing agent and polishing method Download PDFInfo
- Publication number
- JP2018012752A JP2018012752A JP2016141561A JP2016141561A JP2018012752A JP 2018012752 A JP2018012752 A JP 2018012752A JP 2016141561 A JP2016141561 A JP 2016141561A JP 2016141561 A JP2016141561 A JP 2016141561A JP 2018012752 A JP2018012752 A JP 2018012752A
- Authority
- JP
- Japan
- Prior art keywords
- abrasive
- polishing
- resin
- abrasive grains
- metal material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000005498 polishing Methods 0.000 title claims abstract description 258
- 238000000034 method Methods 0.000 title claims description 42
- 239000007788 liquid Substances 0.000 title claims description 35
- 238000003860 storage Methods 0.000 title claims description 22
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- 239000011347 resin Substances 0.000 claims abstract description 112
- 229920005989 resin Polymers 0.000 claims abstract description 112
- -1 aluminum compound Chemical class 0.000 claims abstract description 97
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 57
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Abstract
Description
本発明は、研磨剤、研磨剤用貯蔵液及び研磨方法に関する。 The present invention relates to an abrasive, a storage solution for an abrasive, and a polishing method.
近年、半導体集積回路(以下、「LSI」という)の高集積化及び高性能化に伴って新たな微細加工技術が開発されている。化学機械研磨(以下、場合により「CMP」という)は、そのような技術の一つであり、LSI製造工程(特に、多層配線形成工程における層間絶縁材料の平坦化、金属プラグ形成、埋め込み配線形成等)において頻繁に利用される技術である。 In recent years, new microfabrication techniques have been developed along with higher integration and higher performance of semiconductor integrated circuits (hereinafter referred to as “LSI”). Chemical mechanical polishing (hereinafter, referred to as “CMP” in some cases) is one such technique, and LSI manufacturing processes (particularly, planarization of interlayer insulating materials, formation of metal plugs, formation of embedded wiring in the multilayer wiring forming process) Etc.) are frequently used.
ところで、各種樹脂は、半導体のパッケージ;絶縁材料(絶縁膜等);配線板(例えばプリント配線基板)、回路基板等の電気電子機器などの多様な用途に用いることが期待されており、樹脂を含む被研磨対象における余分な部分を研磨して除去する場合がある。しかしながら、耐熱性、力学強度、寸法安定性、絶縁特性、エッチング耐性等に優れる樹脂(例えば、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミド)は、研磨して除去することが非常に困難である。これに対し、このような樹脂を除去するため、硬度の高い砥粒を用いて物理的に除去する方法が提案されている(例えば下記特許文献1及び2参照)。 By the way, various resins are expected to be used in various applications such as semiconductor packages; insulating materials (insulating films, etc.); wiring boards (eg, printed wiring boards), circuit boards, etc. In some cases, an excessive portion in the object to be polished is removed by polishing. However, resins having excellent heat resistance, mechanical strength, dimensional stability, insulating properties, etching resistance, etc. (for example, polybenzoxazole, polybenzoxazole precursors and polyimide) are very difficult to polish and remove. is there. On the other hand, in order to remove such a resin, a method of physically removing it using abrasive grains having high hardness has been proposed (see, for example, Patent Documents 1 and 2 below).
上記用途の研磨剤に対しては、樹脂と樹脂以外の配線金属材料(例えば、銅系金属、コバルト系金属等の配線金属;及びバリア金属)とを同時に研磨することが求められる場合がある。一方で、上記従来の方法では、配線金属材料を充分な速度で研磨できないという問題がある。 For the abrasive for the above-mentioned use, it may be required to simultaneously polish a resin and a wiring metal material other than the resin (for example, a wiring metal such as a copper-based metal and a cobalt-based metal; and a barrier metal). On the other hand, the conventional method has a problem that the wiring metal material cannot be polished at a sufficient speed.
本発明は、前記の課題を解決しようとするものであり、高い研磨速度で樹脂と配線金属材料とを除去することが可能な研磨剤を提供することを目的とする。また、本発明は、前記研磨剤を得るための研磨剤用貯蔵液を提供することを目的とする。さらに、本発明は、前記研磨剤を用いた研磨方法を提供することを目的とする。 An object of the present invention is to provide an abrasive capable of removing the resin and the wiring metal material at a high polishing rate. Another object of the present invention is to provide an abrasive storage solution for obtaining the abrasive. Furthermore, this invention aims at providing the grinding | polishing method using the said abrasive | polishing agent.
本発明者らは、鋭意研究を重ねた結果、pHが3.5以下である研磨剤中において、シリカ粒子である第一の砥粒と、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミニウム化合物からなる粒子を除く)である第二の砥粒と、を特定の質量比で用いることで前記課題を解決可能であることを見出した。 As a result of intensive studies, the present inventors have determined that at least one selected from the group consisting of a first abrasive grain that is silica particles, an aluminum compound, and aluminum ions in an abrasive having a pH of 3.5 or less. It has been found that the above-mentioned problem can be solved by using the second abrasive grains, which are particles (excluding particles made of an aluminum compound) attached with a specific mass ratio.
すなわち、本発明に係る樹脂及び配線金属材料研磨用研磨剤は、第一の砥粒、第二の砥粒及び水を含有し、前記第一の砥粒がシリカ粒子であり、前記第二の砥粒が、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミニウム化合物からなる粒子を除く)であり、前記第一の砥粒及び前記第二の砥粒の含有量の質量比が、第一の砥粒:第二の砥粒=20:1〜2:1であり、pHが3.5以下であるものである。 That is, the abrasive for polishing a resin and a wiring metal material according to the present invention contains first abrasive grains, second abrasive grains, and water, and the first abrasive grains are silica particles, The abrasive grains are particles to which at least one selected from the group consisting of an aluminum compound and aluminum ions is attached (excluding particles made of an aluminum compound), and the content of the first abrasive grains and the second abrasive grains Mass ratio is 1st abrasive grain: 2nd abrasive grain = 20: 1-2: 1, and pH is 3.5 or less.
本発明に係る研磨剤によれば、高い研磨速度で樹脂と配線金属材料(例えば、銅系金属、コバルト系金属等の配線金属;及びバリア金属)とを除去することができる。本発明に係る研磨剤によれば、樹脂部と配線金属材料部とを備える基板を研磨する場合においても、樹脂部と配線金属部とを同等の高い速度で研磨することができる。特に、本発明に係る研磨剤によれば、高い研磨速度でポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドを除去することができ、かつ、高い研磨速度で銅配線を除去することができる。 According to the abrasive | polishing agent which concerns on this invention, resin and wiring metal material (For example, wiring metals, such as a copper-type metal and a cobalt-type metal; and a barrier metal) can be removed with a high grinding | polishing rate. According to the abrasive | polishing agent which concerns on this invention, even when grind | polishing the board | substrate provided with a resin part and a wiring metal material part, a resin part and a wiring metal part can be grind | polished at an equivalent high speed. In particular, according to the polishing agent of the present invention, polybenzoxazole, polybenzoxazole precursor and polyimide can be removed at a high polishing rate, and copper wiring can be removed at a high polishing rate.
ところで、ポリイミドを除去するため、強アルカリを用いる方法が提案されている(例えば前記特許文献3参照)。しかしながら、このような方法では、強アルカリを用いるため、人体に対する安全性の面で懸念がある。一方、本発明に係る研磨剤によれば、強アルカリを用いない場合であっても、高い研磨速度で樹脂を除去することができる。 By the way, in order to remove polyimide, a method using a strong alkali has been proposed (for example, see Patent Document 3). However, since such a method uses strong alkali, there is a concern in terms of safety to the human body. On the other hand, according to the polishing agent of the present invention, the resin can be removed at a high polishing rate even when a strong alkali is not used.
また、硬度の高い砥粒を用いる従来の方法では、被研磨面に研磨傷(スクラッチ。研磨後の被研磨面に現れる傷をいう。以下同じ)が多数発生する懸念がある。一方、本発明に係る研磨剤によれば、研磨傷の発生を抑制しつつ高い研磨速度で樹脂及び配線金属材料を除去することができる。 Further, in the conventional method using abrasive grains having high hardness, there is a concern that a large number of polishing scratches (scratches; scratches appearing on the polished surface after polishing; the same applies hereinafter) occur on the polished surface. On the other hand, according to the abrasive | polishing agent which concerns on this invention, resin and a wiring metal material can be removed at a high grinding | polishing speed, suppressing generation | occurrence | production of a grinding | polishing damage | wound.
本発明に係る研磨剤は、エーテル結合を有する水溶性高分子を更に含有してもよい。この場合、更に高い樹脂及び配線金属材料の研磨速度を得ることができる。 The abrasive according to the present invention may further contain a water-soluble polymer having an ether bond. In this case, a higher polishing rate of the resin and the wiring metal material can be obtained.
本発明に係る研磨剤は、絶縁材料研磨抑制剤を更に含有してもよい。この場合、樹脂及び配線金属材料を絶縁材料(樹脂及び配線金属材料を除く)に対して選択的に除去できる。 The abrasive according to the present invention may further contain an insulating material polishing inhibitor. In this case, the resin and the wiring metal material can be selectively removed with respect to the insulating material (excluding the resin and the wiring metal material).
本発明に係る研磨剤は、界面活性剤を更に含有してもよい。この場合、被研磨材料の研磨速度を容易に調整できると共に、研磨傷を容易に低減できる。 The abrasive according to the present invention may further contain a surfactant. In this case, the polishing rate of the material to be polished can be easily adjusted, and polishing scratches can be easily reduced.
本発明に係る研磨剤用貯蔵液は、本発明に係る研磨剤を得るための研磨剤用貯蔵液であって、水で希釈することにより前記研磨剤が得られる。この場合、研磨剤の輸送、保管等に必要なコスト、スペース等が低減できる。 The abrasive storage solution according to the present invention is an abrasive storage solution for obtaining the abrasive according to the present invention, and the abrasive can be obtained by diluting with water. In this case, the cost, space, etc. required for transportation and storage of the abrasive can be reduced.
本発明に係る研磨方法は、本発明に係る研磨剤、又は、本発明に係る研磨剤用貯蔵液を水で希釈して得られる研磨剤を用いて、樹脂及び配線金属材料の少なくとも一部を研磨して除去する工程を備える。このような研磨方法によれば、樹脂及び配線金属材料を高い研磨速度で除去できる。 The polishing method according to the present invention uses at least a part of the resin and the wiring metal material using the abrasive according to the present invention or the abrasive obtained by diluting the storage liquid for abrasive according to the present invention with water. A step of polishing and removing. According to such a polishing method, the resin and the wiring metal material can be removed at a high polishing rate.
本発明に係る研磨方法において、前記樹脂は、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種を含むことが好ましい。 In the polishing method according to the present invention, the resin preferably contains at least one selected from the group consisting of polybenzoxazole, a precursor of polybenzoxazole, and polyimide.
本発明によれば、樹脂と配線金属材料とを高い研磨速度で除去することができる。また、本発明によれば、強アルカリを用いない場合であっても、研磨傷の発生を抑制しつつ高い研磨速度で樹脂及び配線金属材料を除去することができる。特に、本発明によれば、高い研磨速度でポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドを除去することができ、かつ、高い研磨速度で銅配線を除去することができる。 According to the present invention, the resin and the wiring metal material can be removed at a high polishing rate. Further, according to the present invention, even when a strong alkali is not used, the resin and the wiring metal material can be removed at a high polishing rate while suppressing generation of polishing flaws. In particular, according to the present invention, polybenzoxazole, polybenzoxazole precursor and polyimide can be removed at a high polishing rate, and copper wiring can be removed at a high polishing rate.
本発明によれば、樹脂及び配線金属材料の研磨への研磨剤又は研磨剤用貯蔵液の使用を提供することができる。本発明によれば、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種を含む樹脂及び配線金属材料の研磨への研磨剤又は研磨剤用貯蔵液の使用を提供することができる。本発明によれば、樹脂及び配線金属材料を有する基体を化学機械研磨して、樹脂及び配線金属材料の少なくとも一部を除去する研磨への研磨剤又は研磨剤用貯蔵液の使用を提供できる。本発明によれば、絶縁材料(樹脂及び配線金属材料を除く)に対する樹脂及び配線金属材料の選択的研磨への研磨剤又は研磨剤用貯蔵液の使用を提供することができる。本発明は、配線板の樹脂及び配線金属材料の研磨への研磨剤又は研磨剤用貯蔵液の使用を提供することができる。本発明は、回路基板の樹脂及び配線金属材料の研磨への研磨剤又は研磨剤用貯蔵液の使用を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, use of the abrasive | polishing agent or the storage liquid for abrasive | polishing agents for grinding | polishing of resin and wiring metal material can be provided. According to the present invention, there is provided use of a polishing agent or a storage solution for a polishing agent for polishing a resin containing at least one selected from the group consisting of polybenzoxazole, a precursor of polybenzoxazole and polyimide, and a wiring metal material. be able to. ADVANTAGE OF THE INVENTION According to this invention, use of the abrasive | polishing agent or the storage liquid for abrasive | polishing agents can be provided for the grinding | polishing which removes at least one part of resin and a wiring metal material by carrying out chemical mechanical polishing of the base | substrate which has resin and wiring metal material. ADVANTAGE OF THE INVENTION According to this invention, use of the abrasive | polishing agent or the storage liquid for abrasive | polishing agents for the selective grinding | polishing of the resin and wiring metal material with respect to an insulating material (except resin and wiring metal material) can be provided. The present invention can provide the use of an abrasive or a storage solution for an abrasive for polishing a resin of a wiring board and a wiring metal material. The present invention can provide the use of an abrasive or a storage solution for an abrasive to polish a circuit board resin and a wiring metal material.
<定義>
本明細書において「工程」との語には、独立した工程だけでなく、他の工程と明確に区別できないもののその工程の所期の作用が達成される工程が含まれる。
<Definition>
In this specification, the term “process” includes not only an independent process but also a process in which an intended action of the process is achieved although it cannot be clearly distinguished from other processes.
本明細書において「〜」は、その前後に記載される数値をそれぞれ最小値及び最大値として含む範囲を示す。本明細書中に段階的に記載されている数値範囲において、ある段階の数値範囲の上限値又は下限値は、他の段階の数値範囲の上限値又は下限値に置き換えてもよい。本明細書中に記載されている数値範囲において、その数値範囲の上限値又は下限値は、実施例に示されている値に置き換えてもよい。 In the present specification, “to” indicates a range including numerical values described before and after that as a minimum value and a maximum value, respectively. In the numerical ranges described stepwise in the present specification, the upper limit value or lower limit value of a numerical range of a certain step may be replaced with the upper limit value or lower limit value of the numerical range of another step. In the numerical range described in this specification, the upper limit value or the lower limit value of the numerical range may be replaced with the values shown in the examples.
本明細書において「A又はB」とは、A及びBのどちらか一方を含んでいればよく、両方とも含んでいてもよい。 In this specification, “A or B” may include either one of A and B, or may include both.
本明細書において組成物中の各成分の含有量は、組成物中に各成分に該当する物質が複数存在する場合、特に断らない限り、組成物中に存在する当該複数の物質の合計量を意味する。 In the present specification, the content of each component in the composition is the total amount of the plurality of substances present in the composition unless there is a specific notice when there are a plurality of substances corresponding to each component in the composition. means.
本明細書において「研磨速度(Removal Rate)」とは、単位時間あたりに被研磨材料が除去される速度を意味する。 In this specification, “removal rate” means a rate at which a material to be polished is removed per unit time.
本明細書において「研磨剤用貯蔵液をX倍に希釈する」とは、研磨剤用貯蔵液に水等を加えることにより研磨剤を得るに際して、研磨剤の質量が研磨剤用貯蔵液の質量のX倍であるような希釈を意味する。例えば、研磨剤用貯蔵液の質量に対して同質量の水を加えて研磨剤を得ることは、研磨剤用貯蔵液を2倍に希釈することと定義される。 In this specification, “dilute the abrasive stock solution X times” means that when the abrasive is obtained by adding water to the abrasive stock solution, the mass of the abrasive is the mass of the abrasive stock solution. Means a dilution that is X times the. For example, to obtain an abrasive by adding the same amount of water to the mass of the abrasive stock solution is defined as diluting the abrasive stock solution twice.
以下、本発明の実施形態について説明する。 Hereinafter, embodiments of the present invention will be described.
<研磨剤>
本実施形態に係る樹脂及び配線金属材料研磨用研磨剤(以下、単に「研磨剤」という場合がある)は、研磨時に被研磨面に触れる組成物であり、例えばCMP用研磨剤である。
<Abrasive>
The abrasive for polishing a resin and a wiring metal material according to the present embodiment (hereinafter sometimes simply referred to as “abrasive”) is a composition that touches a surface to be polished at the time of polishing, for example, an abrasive for CMP.
本実施形態に係る研磨剤は、例えば、樹脂及び配線金属材料を有する基体を研磨して、樹脂及び配線金属材料の少なくとも一部を除去するための研磨剤である。本実施形態に係る研磨剤は、第一の砥粒、第二の砥粒及び水を含有し、前記第一の砥粒がシリカ粒子であり、前記第二の砥粒が、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミニウム化合物からなる粒子を除く)であり、前記第一の砥粒及び前記第二の砥粒の含有量の質量比が、第一の砥粒:第二の砥粒=20:1〜2:1であり、pHが3.5以下であるものである。このような研磨剤によれば、樹脂と配線金属材料とを高い研磨速度で除去することができる。また、本実施形態に係る研磨剤によれば、研磨傷の発生を抑制しつつ高い研磨速度で樹脂及び配線金属材料を除去することができる。本実施形態に係る研磨剤は、絶縁材料(樹脂及び配線金属材料を除く。例えば、酸化珪素等の無機絶縁材料。以下同じ)に対して樹脂及び配線金属材料を選択的に研磨するために用いられてもよい。本実施形態に係る研磨剤は、例えば、配線板又は回路基板の研磨に用いることができる。 The abrasive | polishing agent which concerns on this embodiment is an abrasive | polishing agent for grind | polishing the base | substrate which has resin and wiring metal material, for example, and removes at least one part of resin and wiring metal material. The abrasive | polishing agent which concerns on this embodiment contains a 1st abrasive grain, a 2nd abrasive grain, and water, said 1st abrasive grain is a silica particle, and said 2nd abrasive grain is an aluminum compound and aluminum. It is a particle (excluding particles composed of an aluminum compound) to which at least one selected from the group consisting of ions is attached, and the mass ratio of the content of the first abrasive grain and the second abrasive grain is the first abrasive Grains: second abrasive grains = 20: 1 to 2: 1, and pH is 3.5 or less. According to such an abrasive, the resin and the wiring metal material can be removed at a high polishing rate. Moreover, according to the abrasive | polishing agent which concerns on this embodiment, resin and a wiring metal material can be removed at a high grinding | polishing speed, suppressing generation | occurrence | production of an abrasion flaw. The abrasive according to the present embodiment is used for selectively polishing a resin and a wiring metal material with respect to an insulating material (excluding a resin and a wiring metal material. For example, an inorganic insulating material such as silicon oxide; the same applies hereinafter). May be. The abrasive | polishing agent which concerns on this embodiment can be used for grinding | polishing of a wiring board or a circuit board, for example.
本実施形態に係る研磨剤が、上記効果を奏する理由を、本発明者らは以下のように推測している。アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種のアルミニウム成分が付着した粒子によれば、アルミニウム成分が、ポリベンゾオキサゾール(PBO)、ポリイミド等の化学結合に作用することから、樹脂の研磨速度に優れると考えられる。また、アルミニウム成分が付着した粒子によれば樹脂の高い研磨速度を保ちつつ研磨傷を容易に低減できると考えられる。一方で、シリカ粒子は、配線金属材料の研磨速度に優れると考えられる。したがって、シリカ粒子とアルミニウム成分が付着した粒子とを上記特定量含む研磨液によれば、樹脂と配線金属材料の両方を高い研磨速度で除去することができると考えられる。また、シリカ粒子は、一般的に、pHが3.5以下の研磨剤中で正の電荷を有すると考えられることから、研磨液のpHがこのようなものであると、研磨液中でシリカ粒子が静電的に樹脂及び配線金属材料に作用し、これらの研磨速度が高まり易いと考えられる。したがって、研磨液のpHがこのようなものであると、研磨傷の発生を抑制しつつ、樹脂及び配線金属材料樹脂の高い研磨速度を得易いと考えられる。 The present inventors presume the reason why the abrasive according to the present embodiment has the above effect as follows. According to the particles to which at least one aluminum component selected from the group consisting of an aluminum compound and aluminum ions is attached, the aluminum component acts on chemical bonds such as polybenzoxazole (PBO) and polyimide, so that the polishing rate of the resin It is considered excellent. In addition, it is considered that the particles having the aluminum component attached can easily reduce polishing scratches while maintaining a high resin polishing rate. On the other hand, the silica particles are considered to be excellent in the polishing rate of the wiring metal material. Therefore, it is considered that both the resin and the wiring metal material can be removed at a high polishing rate according to the polishing liquid containing the specific amount of silica particles and particles to which an aluminum component is attached. In addition, since silica particles are generally considered to have a positive charge in an abrasive having a pH of 3.5 or less, if the polishing liquid has such a pH, silica particles in the polishing liquid It is considered that the particles act electrostatically on the resin and the wiring metal material, and the polishing rate thereof tends to increase. Therefore, when the pH of the polishing liquid is such, it is considered that a high polishing rate of the resin and the wiring metal material resin can be easily obtained while suppressing generation of polishing flaws.
(樹脂)
研磨対象である樹脂としては、ポリベンゾオキサゾール(PBO)、PBOの前駆体、ポリイミド(PI)、フェノール樹脂、エポキシ樹脂、アクリル樹脂、メタクリル樹脂、ノボラック樹脂、不飽和ポリエステル、ポリエステル(不飽和ポリエステルを除く)、ポリアミドイミド、ポリアリルエーテル、複素環含有樹脂(前記で例示した樹脂を除く)などが挙げられる。研磨対象は、これらを主成分とした樹脂であってもよい。前記「複素環含有樹脂」としては、ピロール環含有樹脂、ピリジン環含有樹脂、イミダゾール環含有樹脂等が挙げられる。樹脂の形成方法としては、特に制限はないが、蒸着法、スピーンコート法等が挙げられる。樹脂の形状は、特に制限はないが、例えば膜状(樹脂膜)である。これら樹脂の中で、耐熱性、力学強度、寸法安定性、絶縁特性及び、エッチング耐性に優れる観点から、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種が好ましい。
(resin)
As the resin to be polished, polybenzoxazole (PBO), PBO precursor, polyimide (PI), phenol resin, epoxy resin, acrylic resin, methacrylic resin, novolac resin, unsaturated polyester, polyester (unsaturated polyester) Excluded), polyamideimide, polyallyl ether, and heterocyclic-containing resins (excluding the resins exemplified above). The object to be polished may be a resin mainly composed of these. Examples of the “heterocycle-containing resin” include a pyrrole ring-containing resin, a pyridine ring-containing resin, and an imidazole ring-containing resin. The method for forming the resin is not particularly limited, and examples thereof include a vapor deposition method and a spine coating method. The shape of the resin is not particularly limited, but is, for example, a film shape (resin film). Among these resins, at least one selected from the group consisting of polybenzoxazole, a precursor of polybenzoxazole and polyimide is preferable from the viewpoint of excellent heat resistance, mechanical strength, dimensional stability, insulating properties, and etching resistance.
(配線金属材料)
研磨対象である配線金属材料は、例えば、配線材料として用いられる金属材料である。配線金属材料としては、銅系金属、コバルト系金属等の配線金属;タンタル系金属、チタン系金属、マンガン系金属等のバリア金属などが挙げられる。タンタル系金属としては、タンタル、窒化タンタル等が挙げられる。チタン系金属としては、チタン、窒化チタン等が挙げられる。配線金属材料は、銅系金属であることが好ましい。配線金属材料の形状に特に制限はないが、例えば、配線状に形成されたものであってもよい。配線金属材料は、例えば、銅配線であってもよい。
(Wiring metal material)
The wiring metal material to be polished is, for example, a metal material used as a wiring material. Examples of the wiring metal material include wiring metals such as copper metals and cobalt metals; barrier metals such as tantalum metals, titanium metals, and manganese metals. Examples of the tantalum metal include tantalum and tantalum nitride. Examples of the titanium-based metal include titanium and titanium nitride. The wiring metal material is preferably a copper-based metal. Although there is no restriction | limiting in particular in the shape of wiring metal material, For example, what was formed in wiring shape may be sufficient. The wiring metal material may be, for example, a copper wiring.
以下、本実施形態に係る研磨剤に含まれる成分等について詳細に説明する。 Hereinafter, components and the like contained in the abrasive according to this embodiment will be described in detail.
(砥粒)
[第一の砥粒]
本実施形態に係る研磨剤は、第一の砥粒を含有する。当該第一の砥粒は、シリカ粒子である。シリカ粒子を構成するシリカは、例えば、シリカの水酸化物を含んでいてもよい。
(Abrasive grains)
[First abrasive grain]
The abrasive | polishing agent which concerns on this embodiment contains a 1st abrasive grain. The first abrasive grains are silica particles. Silica constituting the silica particles may contain, for example, silica hydroxide.
シリカとしては、コロイダルシリカ、ヒュームドシリカ等が挙げられる。中でも、樹脂及び配線金属材料の高い研磨速度を保ちつつ研磨傷を容易に低減できる観点から、コロイダルシリカが好ましい。これらの観点から、シリカ粒子は、コロイダルシリカを含むことが好ましい。また、シリカ粒子は、コロイダルシリカであってもよい。前記コロイダルシリカとしては、市販品を容易に入手できる。 Examples of silica include colloidal silica and fumed silica. Among these, colloidal silica is preferable from the viewpoint of easily reducing polishing scratches while maintaining a high polishing rate of the resin and the wiring metal material. From these viewpoints, the silica particles preferably contain colloidal silica. The silica particles may be colloidal silica. As said colloidal silica, a commercial item can be obtained easily.
第一の砥粒を構成する材料の修正モース硬度は、12以下が好ましく、10以下がより好ましく、9以下が更に好ましく、8以下が特に好ましい。第一の砥粒の修正モース硬度は、12以下が好ましく、10以下がより好ましく、9以下が更に好ましく、8以下が特に好ましい。 The modified Mohs hardness of the material constituting the first abrasive grains is preferably 12 or less, more preferably 10 or less, still more preferably 9 or less, and particularly preferably 8 or less. The corrected Mohs hardness of the first abrasive is preferably 12 or less, more preferably 10 or less, still more preferably 9 or less, and particularly preferably 8 or less.
シリカの水酸化物等のシリカ粒子の表面は、例えば、アルキル基等で更に変性されていてもよい。シリカ粒子の表面をアルキル基で変性する方法としては、特に制限はないが、例えば、シリカ粒子の表面に存在する水酸基(ヒドロキシル基)と、アルキル基を有するアルコキシシランとを反応させる方法が挙げられる。アルキル基を有するアルコキシシランとしては、特に制限はないが、モノメチルトリメトキシシラン、ジメチルジメトキシシラン、トリメチルモノメトキシシラン、モノエチルトリメトキシシラン、ジエチルジメトキシシラン、トリエチルモノメトキシシラン、モノメチルトリエトキシシラン、ジメチルジエトキシシラン、トリメチルモノエトキシシラン等が挙げられる。反応方法としては、特に制限はなく、例えば、シリカ粒子とアルコキシシランとを含む研磨剤を室温に置いても反応するが、反応を加速するために加熱してもよい。 The surface of silica particles such as silica hydroxide may be further modified with, for example, an alkyl group. The method for modifying the surface of the silica particles with an alkyl group is not particularly limited, and examples thereof include a method of reacting a hydroxyl group (hydroxyl group) present on the surface of the silica particle with an alkoxysilane having an alkyl group. . The alkoxysilane having an alkyl group is not particularly limited, but monomethyltrimethoxysilane, dimethyldimethoxysilane, trimethylmonomethoxysilane, monoethyltrimethoxysilane, diethyldimethoxysilane, triethylmonomethoxysilane, monomethyltriethoxysilane, dimethyl Examples include diethoxysilane and trimethylmonoethoxysilane. There is no restriction | limiting in particular as a reaction method, For example, although it reacts even if it puts the abrasive | polishing agent containing a silica particle and alkoxysilane at room temperature, you may heat in order to accelerate reaction.
第一の砥粒の平均粒径は、充分な機械的研磨力が得られ易く、樹脂及び配線金属材料の更に高い研磨速度が得られる観点から、10nm以上が好ましく、10nmより大きいことがより好ましく、20nm以上が特に好ましい。第一の砥粒の平均粒径は、研磨剤中での良好な分散安定性が得られると共に、研磨により発生する研磨傷の発生数が更に少ない観点から、500nm以下が好ましく、300nm以下がより好ましく、200nm以下が特に好ましい。 The average grain size of the first abrasive grains is preferably 10 nm or more, more preferably larger than 10 nm, from the viewpoint that sufficient mechanical polishing power can be easily obtained and a higher polishing rate of the resin and the wiring metal material can be obtained. 20 nm or more is particularly preferable. The average particle diameter of the first abrasive grains is preferably 500 nm or less, more preferably 300 nm or less, from the viewpoint of obtaining good dispersion stability in the abrasive and further reducing the number of polishing scratches generated by polishing. Preferably, 200 nm or less is particularly preferable.
本明細書において、砥粒の「平均粒径」とは、砥粒の平均二次粒径を意味する。前記平均粒径は、例えば、砥粒を分散させた分散液を動的光散乱式粒度分布計(例えば、COULTER Electronics社製の商品名:COULTER N4 SD)で測定した平均粒径により測定できる。 In this specification, the “average particle diameter” of the abrasive grains means the average secondary particle diameter of the abrasive grains. The average particle diameter can be measured by, for example, an average particle diameter obtained by measuring a dispersion in which abrasive grains are dispersed with a dynamic light scattering particle size distribution meter (for example, trade name: COULTER N4 SD manufactured by COULTER Electronics).
具体的には、平均粒径は、例えば、下記の手順により測定できる。まず、砥粒を分散させた分散液を100μL(Lはリットルを表す。以下同じ。)程度量り取り、砥粒の含有量が0.05質量%前後(測定時透過率(H)が60〜70%である含有量)になるようにイオン交換水で希釈して希釈液を得る。そして、希釈液を動的光散乱式粒度分布計の試料槽に投入し、平均粒径を測ることができる。 Specifically, the average particle diameter can be measured by the following procedure, for example. First, about 100 μL of a dispersion liquid in which abrasive grains are dispersed (L represents liter, the same applies hereinafter), and the content of abrasive grains is around 0.05 mass% (measurement transmittance (H) is 60 to 60%). The diluted solution is obtained by diluting with ion-exchanged water so that the content is 70%. And a dilution liquid can be thrown into the sample tank of a dynamic light scattering type particle size distribution analyzer, and an average particle diameter can be measured.
前記第一の砥粒は、樹脂及び配線金属材料の更に高い研磨速度を得る観点から、一次粒子が平均3粒子未満しか凝集していない粒子が好ましく、一次粒子が平均2粒子未満しか凝集していない粒子がより好ましい。第一の砥粒の会合度の上限は、使用する砥粒の平均一次粒径によって異なり、平均二次粒径が前記で説明した範囲に入っていればよいと考えられる。なお、前記会合度は、平均二次粒径及び平均一次粒径を求め、これらの比(平均二次粒径/平均一次粒径)として得ることができる。 From the viewpoint of obtaining a higher polishing rate of the resin and the wiring metal material, the first abrasive particles are preferably particles in which primary particles are aggregated less than an average of less than 3 particles, and primary particles are aggregated in an average of less than 2 particles. No particles are more preferred. The upper limit of the degree of association of the first abrasive grains varies depending on the average primary particle diameter of the abrasive grains used, and it is considered that the average secondary particle diameter only needs to be within the range described above. The degree of association can be obtained as an average secondary particle size and an average primary particle size and a ratio thereof (average secondary particle size / average primary particle size).
前記平均一次粒径の測定方法としては、公知の透過型電子顕微鏡(例えば、株式会社日立製作所製の商品名:H−7100FA)により測定することができる。例えば、前記電子顕微鏡を用いて粒子の画像を撮影し、所定数の任意の粒子について二軸平均一次粒径を算出し、これらの平均値を求める。粒度分布が広い場合、前記所定数は、平均値が安定する数量とするべきである。第一の砥粒がコロイダルシリカである場合、一般に粒径がそろっているため、測定する粒子数は、例えば20粒子程度でよい。 The average primary particle size can be measured by a known transmission electron microscope (for example, trade name: H-7100FA manufactured by Hitachi, Ltd.). For example, a particle image is taken using the electron microscope, a biaxial average primary particle size is calculated for a predetermined number of arbitrary particles, and an average value thereof is obtained. When the particle size distribution is wide, the predetermined number should be a quantity that stabilizes the average value. When the first abrasive grains are colloidal silica, since the particle diameters are generally uniform, the number of particles to be measured may be about 20 particles, for example.
具体的には、選択した粒子に外接し、その長径が最も長くなるように配置した長方形(外接長方形)を導く。そして、その外接長方形の長径L及び短径Bに基づき、一粒子の二軸平均一次粒径を「(L+B)/2」として算出する。この作業を任意の20粒子に対して実施し、得られた値の平均値を二軸平均一次粒径として用いることができる。この操作はコンピュータプログラムで自動化することもできる。 Specifically, a rectangle (circumscribed rectangle) that circumscribes the selected particle and is arranged so that its major axis is the longest is derived. And based on the major axis L and minor axis B of the circumscribed rectangle, the biaxial average primary particle size of one particle is calculated as “(L + B) / 2”. This operation can be performed on 20 arbitrary particles, and the average value of the obtained values can be used as the biaxial average primary particle size. This operation can also be automated by a computer program.
第一の砥粒における平均粒度分布の標準偏差は、10nm以下が好ましく、5nm以下がより好ましい。平均粒度分布の標準偏差の測定では、例えば、砥粒をCOULTER Electronics社製のCOULTER N4SDに投入し、粒度分布のチャートにより標準偏差の値を得ることができる。 The standard deviation of the average particle size distribution in the first abrasive grains is preferably 10 nm or less, and more preferably 5 nm or less. In the measurement of the standard deviation of the average particle size distribution, for example, the abrasive grains are charged into COULTER N4SD manufactured by COULTER Electronics, and the standard deviation value can be obtained from the particle size distribution chart.
第一の砥粒の含有量は、充分な機械的研磨力が得られ易く、樹脂及び配線金属材料の更に高い研磨速度が得られる観点から、研磨剤の全質量基準で、0.01質量%以上が好ましく、0.1質量%以上がより好ましく、0.5質量%以上が更に好ましい。第一の砥粒の含有量は、研磨剤の粘度上昇を避け易い観点、砥粒の凝集を避け易い観点、研磨傷が低減され易い観点、研磨剤の取り扱いが容易である観点等から、研磨剤の全質量基準で、20質量%以下が好ましく、15質量%以下がより好ましく、10質量%以下が更に好ましい。 The content of the first abrasive grains is 0.01% by mass on the basis of the total mass of the abrasive from the viewpoint that sufficient mechanical polishing power can be easily obtained and a higher polishing rate of the resin and the wiring metal material can be obtained. The above is preferable, 0.1 mass% or more is more preferable, and 0.5 mass% or more is still more preferable. The content of the first abrasive grains is from the viewpoint of easily avoiding an increase in the viscosity of the abrasive, from the viewpoint of easily avoiding the aggregation of abrasive grains, from the viewpoint of easily reducing polishing scratches, and from the viewpoint of easy handling of the abrasive. 20 mass% or less is preferable on the basis of the total mass of the agent, 15 mass% or less is more preferable, and 10 mass% or less is still more preferable.
[第二の砥粒]
本実施形態に係る研磨剤は、第二の砥粒を含有する。第二の砥粒は、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種のアルミニウム成分が付着した粒子(アルミニウム化合物からなる粒子を除く)であり、研磨剤中において前記アルミニウム成分が前記粒子に付着している。すなわち、第二の砥粒は、例えば、アルミニウム化合物以外の粒子に、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種のアルミニウム成分が付着した粒子である。アルミニウム成分は、前記粒子の表面の少なくとも一部に付着していればよい。アルミニウム化合物としては、アルミナ、水酸化アルミニウム等が挙げられる。第二の砥粒は、研磨剤中で正の電荷を有していてもよい。研磨剤がこのような砥粒を含有することにより、研磨傷の発生を抑制しつつ樹脂の高い研磨速度を得ることができる。
[Second abrasive grain]
The abrasive | polishing agent which concerns on this embodiment contains a 2nd abrasive grain. The second abrasive grains are particles to which at least one aluminum component selected from the group consisting of an aluminum compound and aluminum ions is attached (excluding particles made of an aluminum compound), and the aluminum component is added to the particles in an abrasive. It is attached. That is, the second abrasive grains are, for example, particles in which at least one aluminum component selected from the group consisting of an aluminum compound and aluminum ions is attached to particles other than the aluminum compound. The aluminum component may be attached to at least a part of the surface of the particle. Examples of the aluminum compound include alumina and aluminum hydroxide. The second abrasive grain may have a positive charge in the abrasive. When an abrasive | polishing agent contains such an abrasive grain, the high grinding | polishing speed | rate of resin can be obtained, suppressing generation | occurrence | production of an abrasion flaw.
第二の砥粒において、アルミニウム成分が付着する粒子(アルミニウム成分以外の部分。以下、場合により「コア粒子」ともいう)の構成材料としては、シリカ、セリア、セリウムの水酸化物、樹脂及びこれらの変性物からなる群より選ばれる少なくとも一種が挙げられる。コア粒子における前記構成材料の含有量は、コア粒子の全質量を基準として、50質量%以上が好ましく、75質量%以上がより好ましく、90質量%以上が更に好ましく、95質量%以上が特に好ましい。コア粒子は、前記構成材料からなる態様(砥粒の実質的に100質量%が前記構成材料である態様)であってもよい。 In the second abrasive grains, the constituent materials of particles to which the aluminum component adheres (parts other than the aluminum component; hereinafter also referred to as “core particles”) include silica, ceria, cerium hydroxide, resin, and these And at least one selected from the group consisting of the modified products. The content of the constituent material in the core particles is preferably 50% by mass or more, more preferably 75% by mass or more, still more preferably 90% by mass or more, and particularly preferably 95% by mass or more, based on the total mass of the core particles. . The core particle may be in an aspect made of the constituent material (an aspect in which substantially 100% by mass of the abrasive grains is the constituent material).
シリカとしては、コロイダルシリカ、ヒュームドシリカ等が挙げられる。中でも、樹脂及び配線金属材料の高い研磨速度を保ちつつ研磨傷を容易に低減できる観点から、コロイダルシリカが好ましい。前記コロイダルシリカとしては、市販品を容易に入手できる。 Examples of silica include colloidal silica and fumed silica. Among these, colloidal silica is preferable from the viewpoint of easily reducing polishing scratches while maintaining a high polishing rate of the resin and the wiring metal material. As said colloidal silica, a commercial item can be obtained easily.
第二の砥粒に含まれる材料の修正モース硬度は、12以下が好ましく、10以下がより好ましく、9以下が更に好ましく、8以下が特に好ましい。第二の砥粒の修正モース硬度は、12以下が好ましく、10以下がより好ましく、9以下が更に好ましく、8以下が特に好ましい。 The modified Mohs hardness of the material contained in the second abrasive is preferably 12 or less, more preferably 10 or less, still more preferably 9 or less, and particularly preferably 8 or less. The corrected Mohs hardness of the second abrasive is preferably 12 or less, more preferably 10 or less, still more preferably 9 or less, and particularly preferably 8 or less.
前記変性物としては、シリカ、セリア、セリウムの水酸化物等のコア粒子の表面をアルキル基で変性したもの、コア粒子の表面に上記構成材料及びアルミニウム成分以外の粒子を付着させた複合砥粒などが挙げられる。コア粒子の表面をアルキル基で変性する方法としては、特に制限はないが、例えば、コア粒子の表面に存在する水酸基(ヒドロキシル基)と、アルキル基を有するアルコキシシランとを反応させる方法が挙げられる。アルキル基を有するアルコキシシランとしては、特に制限はないが、モノメチルトリメトキシシラン、ジメチルジメトキシシラン、トリメチルモノメトキシシラン、モノエチルトリメトキシシラン、ジエチルジメトキシシラン、トリエチルモノメトキシシラン、モノメチルトリエトキシシラン、ジメチルジエトキシシラン、トリメチルモノエトキシシラン等が挙げられる。反応方法としては、特に制限はなく、例えば、コア粒子とアルコキシシランとを含む研磨剤を室温に置いても反応するが、反応を加速するために加熱してもよい。 Examples of the modified product include silica, ceria, cerium hydroxide and other core particle surfaces modified with an alkyl group, and composite abrasive grains in which particles other than the above-described constituent materials and aluminum components are attached to the core particle surface. Etc. The method of modifying the surface of the core particle with an alkyl group is not particularly limited, and examples thereof include a method of reacting a hydroxyl group (hydroxyl group) present on the surface of the core particle with an alkoxysilane having an alkyl group. . The alkoxysilane having an alkyl group is not particularly limited, but monomethyltrimethoxysilane, dimethyldimethoxysilane, trimethylmonomethoxysilane, monoethyltrimethoxysilane, diethyldimethoxysilane, triethylmonomethoxysilane, monomethyltriethoxysilane, dimethyl Examples include diethoxysilane and trimethylmonoethoxysilane. There is no restriction | limiting in particular as a reaction method, For example, although it reacts even if it puts the abrasive | polishing agent containing a core particle and alkoxysilane at room temperature, you may heat in order to accelerate reaction.
第二の砥粒の平均粒径(平均二次粒径)は、充分な機械的研磨力が得られ易く、樹脂及び配線金属材料の更に高い研磨速度が得られる観点から、10nm以上が好ましく、10nmより大きいことがより好ましく、20nm以上が特に好ましい。第二の砥粒の平均粒径は、研磨剤中での良好な分散安定性が得られると共に、研磨により発生する研磨傷の発生数が更に少ない観点から、500nm以下が好ましく、300nm以下がより好ましく、200nm以下が特に好ましい。平均粒径は、上述した方法と同様の方法により測定できる。 The average particle size (average secondary particle size) of the second abrasive grains is preferably 10 nm or more from the viewpoint that a sufficient mechanical polishing force can be easily obtained and a higher polishing rate of the resin and the wiring metal material can be obtained. It is more preferably larger than 10 nm, particularly preferably 20 nm or more. The average particle size of the second abrasive grains is preferably 500 nm or less, more preferably 300 nm or less, from the viewpoint of obtaining good dispersion stability in the abrasive and further reducing the number of polishing scratches generated by polishing. Preferably, 200 nm or less is particularly preferable. The average particle diameter can be measured by the same method as described above.
第二の砥粒は、樹脂の更に高い研磨速度を得る観点から、一次粒子が平均3粒子未満しか凝集していない粒子が好ましく、一次粒子が平均2粒子未満しか凝集していない粒子がより好ましい。第二の砥粒の会合度の上限は、使用する砥粒の平均一次粒径によって異なり、平均二次粒径が前記で説明した範囲に入っていればよいと考えられる。また、第二の砥粒における平均粒度分布の標準偏差は、10nm以下が好ましく、5nm以下がより好ましい。なお、会合度、平均一次粒径、及び平均粒度分布の標準偏差は、上述した方法と同様の方法により測定できる。平均一次粒径の測定方法において測定する粒子の数は、コア粒子がコロイダルシリカである場合、一般に粒径がそろっているため、例えば20粒子程度でよい。 From the viewpoint of obtaining a higher polishing rate of the resin, the second abrasive is preferably particles in which the primary particles are aggregated less than an average of less than 3 particles, more preferably particles in which the primary particles are aggregated less than an average of less than 2 particles. . The upper limit of the degree of association of the second abrasive grains varies depending on the average primary particle diameter of the abrasive grains used, and it is considered that the average secondary particle diameter only needs to be within the range described above. Further, the standard deviation of the average particle size distribution in the second abrasive grains is preferably 10 nm or less, and more preferably 5 nm or less. The degree of association, the average primary particle size, and the standard deviation of the average particle size distribution can be measured by the same method as described above. When the core particles are colloidal silica, the number of particles to be measured in the average primary particle size measurement method may be about 20 particles, for example, because the particle sizes are generally uniform.
第二の砥粒の含有量は、充分な機械的研磨力が得られ易く、樹脂及び配線金属材料の更に高い研磨速度が得られる観点から、研磨剤の全質量基準で、0.01質量%以上が好ましく、0.1質量%以上がより好ましく、0.5質量%以上が更に好ましい。第二の砥粒の含有量は、研磨剤の粘度上昇を避け易い観点、砥粒の凝集を避け易い観点、研磨傷が低減され易い観点、研磨剤の取り扱いが容易である観点等から、研磨剤の全質量基準で、20質量%以下が好ましく、15質量%以下がより好ましく、10質量%以下が更に好ましい。 The content of the second abrasive is 0.01% by mass based on the total mass of the abrasive from the viewpoint that sufficient mechanical polishing power is easily obtained and a higher polishing rate of the resin and the wiring metal material is obtained. The above is preferable, 0.1 mass% or more is more preferable, and 0.5 mass% or more is still more preferable. The content of the second abrasive grains is determined from the viewpoint of easily avoiding an increase in the viscosity of the abrasive, from the viewpoint of easily avoiding the aggregation of abrasive grains, from the viewpoint of easily reducing polishing scratches, and from the viewpoint of easy handling of the abrasive. 20 mass% or less is preferable on the basis of the total mass of the agent, 15 mass% or less is more preferable, and 10 mass% or less is still more preferable.
[第一の砥粒及び第二の砥粒の含有量の質量比]
第一の砥粒及び第二の砥粒の含有量の質量比は、第一の砥粒:第二の砥粒=20:1〜2:1である。第一の砥粒の含有量に対する第二の砥粒の含有量の質量比(第二の砥粒の総質量/第一の砥粒の総質量))が1/20以上であると、樹脂に対して高い除去速度を得易いと考えられる。一方、第一の砥粒の含有量に対する第二の砥粒の含有量の質量比(第二の砥粒の総質量/第一の砥粒の総質量))が1/2以下であると、配線金属材料に対して高い除去速度を得易いと考えられる。
[Mass ratio of content of first abrasive grain and second abrasive grain]
The mass ratio of the content of the first abrasive grains and the second abrasive grains is first abrasive grains: second abrasive grains = 20: 1 to 2: 1. When the mass ratio of the content of the second abrasive grain to the content of the first abrasive grain (total mass of the second abrasive grain / total mass of the first abrasive grain) is 1/20 or more, the resin It is considered that a high removal rate can be easily obtained. On the other hand, the mass ratio of the content of the second abrasive grains to the content of the first abrasive grains (total mass of the second abrasive grains / total mass of the first abrasive grains) is 1/2 or less. It is considered that a high removal rate can be easily obtained for the wiring metal material.
樹脂及び配線金属材料を更に高い研磨速度で除去する観点から、第一の砥粒及び第二の砥粒の含有量の質量比は、第一の砥粒:第二の砥粒=18:1〜3:1であることが好ましく、第一の砥粒:第二の砥粒=16:1〜3:1であることがより好ましい。 From the viewpoint of removing the resin and the wiring metal material at a higher polishing rate, the mass ratio of the contents of the first abrasive grains and the second abrasive grains is as follows: first abrasive grains: second abrasive grains = 18: 1 Is preferably ˜3: 1, and more preferably 1st abrasive grain: second abrasive grain = 16: 1 to 3: 1.
[砥粒の電位]
砥粒は、研磨剤中で正の電荷を有していてもよい。研磨剤がこのような砥粒を含有することにより、研磨傷の発生を抑制しつつ樹脂の高い研磨速度を得ることができる。
[Abrasive potential]
The abrasive grains may have a positive charge in the abrasive. When an abrasive | polishing agent contains such an abrasive grain, the high grinding | polishing speed | rate of resin can be obtained, suppressing generation | occurrence | production of an abrasion flaw.
樹脂を研磨(CMP等)して除去する場合、pHが3.5以下の研磨剤中で正の電荷を有する砥粒を用いることにより、静電的に砥粒が樹脂に作用することから、樹脂の研磨速度が高くなり易いと考えられる。 When removing the resin by polishing (CMP or the like), by using abrasive grains having a positive charge in an abrasive having a pH of 3.5 or less, the abrasive grains act electrostatically on the resin. It is considered that the resin polishing rate tends to be high.
砥粒が研磨剤中で正の電荷を有しているか否かは、研磨剤における砥粒のゼータ電位を測定することにより判断できる。研磨剤における砥粒のゼータ電位を測定し、数値が0mVを超える場合、砥粒が正の電荷を有していると判断することができる。 Whether or not the abrasive has a positive charge in the abrasive can be determined by measuring the zeta potential of the abrasive in the abrasive. When the zeta potential of the abrasive grains in the abrasive is measured and the numerical value exceeds 0 mV, it can be determined that the abrasive grains have a positive charge.
ゼータ電位は、例えば、ベックマンコールター社製の商品名:DELSA NANO Cで測定できる。ゼータ電位(ζ[mV])は、下記の手順により測定できる。まず、ゼータ電位測定装置において測定サンプルの散乱強度が1.0×104〜5.0×104cps(ここで、「cps」とは、counts per second、すなわち、カウント毎秒を意味し、粒子の計数の単位である)となるように研磨剤を純水で希釈してサンプルを得る。そして、サンプルをゼータ電位測定用セルに入れてゼータ電位を測定する。散乱強度を前記範囲に調整するためには、例えば、砥粒の含有量が1.7〜1.8質量%に調整されるように研磨剤を希釈する。 The zeta potential can be measured by, for example, trade name: DELSA NANO C manufactured by Beckman Coulter. The zeta potential (ζ [mV]) can be measured by the following procedure. First, in the zeta potential measurement device, the scattering intensity of the measurement sample is 1.0 × 10 4 to 5.0 × 10 4 cps (where “cps” means counts per second, that is, counts per second, The sample is obtained by diluting the abrasive with pure water so that Then, the sample is put into a zeta potential measurement cell and the zeta potential is measured. In order to adjust the scattering intensity to the above range, for example, the abrasive is diluted so that the content of abrasive grains is adjusted to 1.7 to 1.8% by mass.
前記ゼータ電位は、樹脂及び配線金属材料の更に高い研磨速度、及び、良好な保存安定性が得られる観点から、20mV以上が好ましく、25mV以上がより好ましく、30mV以上が更に好ましく、35mV以上が特に好ましい。前記ゼータ電位の上限は、特に制限はないが、例えば100mV以下である。 The zeta potential is preferably 20 mV or more, more preferably 25 mV or more, further preferably 30 mV or more, and particularly preferably 35 mV or more from the viewpoint of obtaining a higher polishing rate of the resin and the wiring metal material and good storage stability. preferable. The upper limit of the zeta potential is not particularly limited, but is 100 mV or less, for example.
(水)
本実施形態に係る研磨剤は、水を含有する。水は、他の成分の分散媒、又は、溶媒として用いられる。水としては、他の成分の作用を阻害することを防止するために不純物を可能な限り含有しないものが好ましい。具体的には、水としては、イオン交換樹脂にて不純物イオンを除去した後にフィルタを通して異物を除去した純水、超純水及び蒸留水が好ましい。
(water)
The abrasive | polishing agent which concerns on this embodiment contains water. Water is used as a dispersion medium or solvent for other components. The water is preferably one containing as little impurities as possible in order to prevent the action of other components from being inhibited. Specifically, the water is preferably pure water, ultrapure water, or distilled water from which foreign ions are removed through a filter after removing impurity ions with an ion exchange resin.
(添加剤)
本実施形態に係る研磨剤は、第一及び第二の砥粒並びに水以外の成分として添加剤を含有することができる。添加剤は、研磨剤中の砥粒の分散性の向上、研磨剤の化学的安定性の向上、研磨速度の向上等の目的で用いることができる。添加剤としては、pH調整剤、防食剤、酸化剤、エーテル結合を有する水溶性高分子、有機溶媒、絶縁材料研磨抑制剤、界面活性剤、消泡剤、キレート剤等が挙げられる。研磨剤中の添加剤の含有量は、研磨剤の特性を損なわない範囲で任意に決定できる。
(Additive)
The abrasive | polishing agent which concerns on this embodiment can contain an additive as components other than the 1st and 2nd abrasive grain and water. The additive can be used for the purpose of improving the dispersibility of the abrasive grains in the abrasive, improving the chemical stability of the abrasive, and improving the polishing rate. Examples of the additive include a pH adjuster, an anticorrosive, an oxidizing agent, a water-soluble polymer having an ether bond, an organic solvent, an insulating material polishing inhibitor, a surfactant, an antifoaming agent, and a chelating agent. The content of the additive in the abrasive can be arbitrarily determined as long as the characteristics of the abrasive are not impaired.
[研磨剤のpH及びpH調整剤]
本実施形態に係る研磨剤のpHは、研磨傷の発生を抑制しつつ高い研磨速度で樹脂及び配線金属材料を除去する観点及び砥粒の凝集が抑制され易い観点から、3.5以下である。研磨剤のpHは、樹脂及び配線金属材料の研磨速度が更に向上する観点、及び、砥粒の凝集が更に抑制され、砥粒の良好な分散安定性が得られる観点から、3.5未満が好ましく、3.4以下がより好ましく、3.3以下が更に好ましく、3.1以下が特に好ましい。研磨剤のpHは、充分な機械的研磨力が得られ易く、樹脂及び配線金属材料の研磨速度が更に向上する観点から、1.5以上が好ましく、1.8以上がより好ましい。これらの観点から、研磨剤のpHは、1.5〜3.5が好ましく、1.8〜3.3がより好ましく、1.8〜3.1が特に好ましい。pHは液温25℃におけるpHと定義する。
[Abrasive pH and pH adjuster]
The pH of the abrasive according to the present embodiment is 3.5 or less from the viewpoint of removing the resin and the wiring metal material at a high polishing rate while suppressing the generation of polishing flaws and from the viewpoint of easily suppressing the aggregation of abrasive grains. . The pH of the abrasive is less than 3.5 from the viewpoint of further improving the polishing rate of the resin and the wiring metal material, and from the viewpoint of further suppressing the aggregation of the abrasive grains and obtaining good dispersion stability of the abrasive grains. Preferably, 3.4 or less is more preferable, 3.3 or less is further preferable, and 3.1 or less is particularly preferable. The pH of the abrasive is preferably 1.5 or more, more preferably 1.8 or more, from the viewpoint that sufficient mechanical polishing power can be easily obtained and the polishing rate of the resin and the wiring metal material is further improved. From these viewpoints, the pH of the abrasive is preferably 1.5 to 3.5, more preferably 1.8 to 3.3, and particularly preferably 1.8 to 3.1. The pH is defined as the pH at a liquid temperature of 25 ° C.
研磨剤のpHは、一般的なガラス電極を用いたpHメーターによって測定できる。具体的には、例えば、株式会社堀場製作所の商品名:Model(F−51)を使用できる。例えば、フタル酸塩pH標準液(pH:4.01)と、中性リン酸塩pH標準液(pH:6.86)と、ホウ酸塩pH標準液(pH:9.18)とをpH標準液として用い、pHメーターを3点校正した後、pHメーターの電極を研磨剤に入れて、2min以上経過して安定した後の値を測定することによりpHの測定値を得ることができる。このとき、標準緩衝液及び研磨剤の液温は、例えば25℃である。 The pH of the abrasive can be measured by a pH meter using a general glass electrode. Specifically, for example, trade name: Model (F-51) manufactured by HORIBA, Ltd. can be used. For example, phthalate pH standard solution (pH: 4.01), neutral phosphate pH standard solution (pH: 6.86), and borate pH standard solution (pH: 9.18) The pH value can be obtained by using the standard solution and calibrating the pH meter at three points, and then measuring the value after the pH meter electrode is placed in an abrasive and stabilized for 2 minutes or more. At this time, the liquid temperature of the standard buffer and the abrasive is, for example, 25 ° C.
本実施形態に係る研磨剤は、pH調整剤(pH調整剤成分)を含有していてもよい。pH調整剤を用いることにより、研磨剤のpHを容易に調整することができる。また、pH調整剤は配線金属材料との錯体を形成易いことから、pH調整剤を用いることにより、配線金属材料の研磨速度が更に向上すると考えられる。pH調整剤としては、酸成分、塩基成分(例えば、アンモニア等の弱塩基成分)などが挙げられる。 The abrasive according to the present embodiment may contain a pH adjuster (pH adjuster component). By using a pH adjuster, the pH of the abrasive can be easily adjusted. Moreover, since the pH adjuster can easily form a complex with the wiring metal material, it is considered that the polishing rate of the wiring metal material is further improved by using the pH adjusting agent. Examples of the pH adjuster include an acid component and a base component (for example, a weak base component such as ammonia).
pH調整剤はpHを調整しつつ、酸化剤等により酸化された配線金属材料(配線金属、バリア金属等)の溶解を促進し、研磨速度を更に向上させる観点から、酸成分を含むことが好ましい。酸成分としては、有機酸成分、無機酸成分等が挙げられる。 The pH adjuster preferably contains an acid component from the viewpoint of promoting the dissolution of the wiring metal material (wiring metal, barrier metal, etc.) oxidized by the oxidizing agent or the like while adjusting the pH, and further improving the polishing rate. . Examples of the acid component include an organic acid component and an inorganic acid component.
有機酸成分としては、有機酸(アミノ酸を除く)、有機酸エステル、有機酸塩、アミノ酸等が挙げられる。有機酸としては、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、2−メチル酪酸、n−ヘキサン酸、3,3−ジメチル酪酸、2−エチル酪酸、4−メチルペンタン酸、n−ヘプタン酸、2−メチルヘキサン酸、n−オクタン酸、2−エチルヘキサン酸、安息香酸、グリコール酸、サリチル酸、グリセリン酸、シュウ酸、マロン酸、コハク酸、3−メチルフタル酸、4−メチルフタル酸、3−アミノフタル酸、4−アミノフタル酸、3−ニトロフタル酸、4−ニトロフタル酸、グルタル酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、イソフタル酸、リンゴ酸、酒石酸、クエン酸、p−トルエンスルホン酸、p−フェノールスルホン酸、メチルスルホン酸、乳酸、イタコン酸、安息香酸、マレイン酸、キナルジン酸、アジピン酸、ピメリン酸等が挙げられる。有機酸エステルとしては、前記有機酸のエステル等が挙げられる。有機酸塩としては、前記有機酸のアンモニウム塩、アルカリ金属塩、アルカリ土類金属塩、ハロゲン化物等が挙げられる。 Examples of the organic acid component include organic acids (excluding amino acids), organic acid esters, organic acid salts, amino acids and the like. Examples of organic acids include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, 3-methylphthalic acid, 4-methylphthalic acid, 3-aminophthalic acid Acid, 4-aminophthalic acid, 3-nitrophthalic acid, 4-nitrophthalic acid, glutaric acid, adipic acid, pimelic acid, maleic acid, phthalic acid, isophthalic acid, malic acid, tartaric acid, citric acid, p-toluenesulfonic acid, p -Phenolsulfonic acid, methylsulfonic acid, lactic acid, itaconic acid, benzoic acid, maleic acid, quinaldic acid, adipic acid, pimelin Etc. The. Examples of the organic acid ester include esters of the organic acid. Examples of the organic acid salt include ammonium salts, alkali metal salts, alkaline earth metal salts and halides of the organic acids.
無機酸成分としては、無機酸、当該無機酸のアンモニウム塩、過硫酸アンモニウム、硝酸アンモニウム、塩化アンモニウム、クロム酸等が挙げられる。無機酸としては、塩酸、硫酸、硝酸等が挙げられる。 Examples of the inorganic acid component include inorganic acids, ammonium salts of the inorganic acids, ammonium persulfate, ammonium nitrate, ammonium chloride, and chromic acid. Examples of the inorganic acid include hydrochloric acid, sulfuric acid, nitric acid and the like.
例えば、被研磨対象(被研磨基板等)が、集積回路用素子を含むシリコン基板である場合、アルカリ金属、アルカリ土類金属、ハロゲン化物等による汚染は望ましくないため、前記酸成分の塩としてはアルカリ金属塩、アルカリ土類金属塩又はハロゲン化物以外の塩が好ましい。 For example, when the object to be polished (substrate to be polished) is a silicon substrate including an integrated circuit element, contamination with alkali metal, alkaline earth metal, halide, etc. is not desirable. Salts other than alkali metal salts, alkaline earth metal salts or halides are preferred.
酸成分としては、実用的な研磨速度を維持しつつ、エッチング速度を効果的に抑制できる観点から、マロン酸、リンゴ酸、酒石酸、クエン酸、サリチル酸、アジピン酸、フタル酸、グリコール酸、及びコハク酸からなる群より選ばれる少なくとも一種が好ましい。 The acid component includes malonic acid, malic acid, tartaric acid, citric acid, salicylic acid, adipic acid, phthalic acid, glycolic acid, and succinic acid from the viewpoint of effectively suppressing the etching rate while maintaining a practical polishing rate. At least one selected from the group consisting of acids is preferred.
pH調整剤は、一種を単独で、又は、二種以上を組み合わせて使用できる。 A pH adjuster can be used individually by 1 type or in combination of 2 or more types.
pH調整剤の含有量は、樹脂及び配線金属材料の更に高い研磨速度を得易い観点から、研磨剤の全質量を基準として、0.001質量%以上が好ましく、0.002質量%以上がより好ましく、0.005質量%以上が更に好ましい。pH調整剤の含有量は、エッチングを抑制し被研磨面の荒れを低減し易い観点から、研磨剤の全質量を基準として、20質量%以下が好ましく、10質量%以下がより好ましく、5質量%以下が更に好ましい。これらの観点から、pH調整剤の含有量は、研磨剤の全質量を基準として、0.001〜20質量%が好ましく、0.002〜10質量%がより好ましく、0.005〜5質量%が更に好ましい。 The content of the pH adjuster is preferably 0.001% by mass or more and more preferably 0.002% by mass or more based on the total mass of the abrasive from the viewpoint of easily obtaining a higher polishing rate of the resin and the wiring metal material. Preferably, 0.005 mass% or more is more preferable. The content of the pH adjuster is preferably 20% by mass or less, more preferably 10% by mass or less, and more preferably 5% by mass, based on the total mass of the abrasive, from the viewpoint of suppressing etching and reducing roughness of the polished surface. % Or less is more preferable. From these viewpoints, the content of the pH adjusting agent is preferably 0.001 to 20% by mass, more preferably 0.002 to 10% by mass, based on the total mass of the abrasive, and 0.005 to 5% by mass. Is more preferable.
[防食剤]
本実施形態に係る研磨剤は、防食剤(防食剤成分、金属防食剤)を含有してもよい。防食剤は配線金属(銅系及びコバルト系金属等)に対して保護膜を形成することで、配線金属の過剰な腐食(エッチング)を抑制して被研磨面の荒れを低減し易くすることができる。
[Anticorrosive]
The abrasive according to this embodiment may contain an anticorrosive agent (anticorrosive component, metal anticorrosive agent). The anticorrosive agent forms a protective film against the wiring metal (copper-based and cobalt-based metal, etc.), thereby suppressing excessive corrosion (etching) of the wiring metal and making it easy to reduce the roughness of the surface to be polished. it can.
防食剤としては特に制限はなく、金属材料に対する防食作用を有する化合物として従来公知の成分がいずれも使用可能である。防食剤としては、具体的には、トリアゾール化合物、ピリジン化合物、ピラゾール化合物、ピリミジン化合物、イミダゾール化合物、グアニジン化合物、チアゾール化合物、テトラゾール化合物、トリアジン化合物、及びヘキサメチレンテトラミンからなる群より選ばれる少なくとも一種を用いることができる。ここで「化合物」とは、その骨格を有する化合物の総称であり、例えば「トリアゾール化合物」とは、トリアゾール骨格を有する化合物を意味する。 There is no restriction | limiting in particular as an anticorrosive agent, Any conventionally well-known component can be used as a compound which has the anticorrosive action with respect to a metal material. Specifically, the anticorrosive agent is at least one selected from the group consisting of triazole compounds, pyridine compounds, pyrazole compounds, pyrimidine compounds, imidazole compounds, guanidine compounds, thiazole compounds, tetrazole compounds, triazine compounds, and hexamethylenetetramine. Can be used. Here, “compound” is a general term for compounds having the skeleton, and for example, “triazole compound” means a compound having a triazole skeleton.
トリアゾール化合物としては、例えば、1,2,3−トリアゾール、1,2,4−トリアゾール、3−アミノ−1H−1,2,4−トリアゾール、ベンゾトリアゾール(BTA)、1−ヒドロキシベンゾトリアゾール、1−ジヒドロキシプロピルベンゾトリアゾール、2,3−ジカルボキシプロピルベンゾトリアゾール、4−ヒドロキシベンゾトリアゾール、4−カルボキシ−1H−ベンゾトリアゾール、4−カルボキシ−1H−ベンゾトリアゾールメチルエステル(1H−ベンゾトリアゾール−4−カルボン酸メチル)、4−カルボキシ−1H−ベンゾトリアゾールブチルエステル(1H−ベンゾトリアゾール−4−カルボン酸ブチル)、4−カルボキシ−1H−ベンゾトリアゾールオクチルエステル(1H−ベンゾトリアゾール−4−カルボン酸オクチル)、5−ヘキシルベンゾトリアゾール、(1,2,3−ベンゾトリアゾリル−1−メチル)(1,2,4−トリアゾリル−1−メチル)(2−エチルヘキシル)アミン、トリルトリアゾール、ナフトトリアゾール、ビス[(1−ベンゾトリアゾリル)メチル]ホスホン酸、3H−1,2,3−トリアゾロ[4,5−b]ピリジン−3−オール、1H−1,2,3−トリアゾロ[4,5−b]ピリジン、1−アセチル−1H−1,2,3−トリアゾロ[4,5−b]ピリジン、3−ヒドロキシピリジン、1,2,4−トリアゾロ[1,5−a]ピリミジン、1,3,4,6,7,8−ヘキサヒドロ−2H−ピリミド[1,2−a]ピリミジン、2−メチル−5,7−ジフェニル−[1,2,4]トリアゾロ[1,5−a]ピリミジン、2−メチルサルファニル−5,7−ジフェニル−[1,2,4]トリアゾロ[1,5−a]ピリミジン、及び2−メチルサルファニル−5,7−ジフェニル−4,7−ジヒドロ−[1,2,4]トリアゾロ[1,5−a]ピリミジンが挙げられる。なお、トリアゾール骨格と、それ以外の骨格とを一分子中に有する化合物は、トリアゾール化合物に分類されるものとする。 Examples of the triazole compound include 1,2,3-triazole, 1,2,4-triazole, 3-amino-1H-1,2,4-triazole, benzotriazole (BTA), 1-hydroxybenzotriazole, 1 -Dihydroxypropylbenzotriazole, 2,3-dicarboxypropylbenzotriazole, 4-hydroxybenzotriazole, 4-carboxy-1H-benzotriazole, 4-carboxy-1H-benzotriazole methyl ester (1H-benzotriazole-4-carboxylic acid) Acid methyl), 4-carboxy-1H-benzotriazole butyl ester (1H-benzotriazole-4-carboxylate butyl), 4-carboxy-1H-benzotriazole octyl ester (1H-benzotriazole-4-carboxylate) Octyl bonate), 5-hexylbenzotriazole, (1,2,3-benzotriazolyl-1-methyl) (1,2,4-triazolyl-1-methyl) (2-ethylhexyl) amine, tolyltriazole, Naphthotriazole, bis [(1-benzotriazolyl) methyl] phosphonic acid, 3H-1,2,3-triazolo [4,5-b] pyridin-3-ol, 1H-1,2,3-triazolo [ 4,5-b] pyridine, 1-acetyl-1H-1,2,3-triazolo [4,5-b] pyridine, 3-hydroxypyridine, 1,2,4-triazolo [1,5-a] pyrimidine 1,3,4,6,7,8-hexahydro-2H-pyrimido [1,2-a] pyrimidine, 2-methyl-5,7-diphenyl- [1,2,4] triazolo [1,5- a] Pyri Gin, 2-methylsulfanyl-5,7-diphenyl- [1,2,4] triazolo [1,5-a] pyrimidine, and 2-methylsulfanyl-5,7-diphenyl-4,7-dihydro- [1,2,4] triazolo [1,5-a] pyrimidine. A compound having a triazole skeleton and another skeleton in one molecule is classified as a triazole compound.
ピリジン化合物としては、例えば、8−ヒドロキシキノリン、プロチオナミド、2−ニトロピリジン−3−オール、ピリドキサミン、ニコチンアミド、イプロニアジド、イソニコチン酸、ベンゾ[f]キノリン、2,5−ピリジンジカルボン酸、4−スチリルピリジン、アナバシン、4−ニトロピリジン−1−オキシド、ピリジン−3−酢酸エチル、キノリン、2−エチルピリジン、キノリン酸、アレコリン、シトラジン酸、ピリジン−3−メタノール、2−メチル−5−エチルピリジン、2−フルオロピリジン、ペンタフルオロピリジン、6−メチルピリジン−3−オール、及びピリジン−2−酢酸エチルが挙げられる。 Examples of the pyridine compound include 8-hydroxyquinoline, prothionamide, 2-nitropyridin-3-ol, pyridoxamine, nicotinamide, iproniazide, isonicotinic acid, benzo [f] quinoline, 2,5-pyridinedicarboxylic acid, 4- Styrylpyridine, anabasine, 4-nitropyridine-1-oxide, pyridine-3-ethyl acetate, quinoline, 2-ethylpyridine, quinolinic acid, arecoline, citrazic acid, pyridine-3-methanol, 2-methyl-5-ethylpyridine 2-fluoropyridine, pentafluoropyridine, 6-methylpyridin-3-ol, and ethyl pyridine-2-acetate.
ピラゾール化合物としては、例えば、ピラゾール、1−アリル−3,5−ジメチルピラゾール、3,5−ジ(2−ピリジル)ピラゾール、3,5−ジイソプロピルピラゾール、3,5−ジメチル−1−ヒドロキシメチルピラゾール、3,5−ジメチル−1−フェニルピラゾール、3,5−ジメチルピラゾール、3−アミノ−5−ヒドロキシピラゾール、4−メチルピラゾール、N−メチルピラゾール、3−アミノピラゾール、及び3−アミノピラゾールが挙げられる。 Examples of the pyrazole compound include pyrazole, 1-allyl-3,5-dimethylpyrazole, 3,5-di (2-pyridyl) pyrazole, 3,5-diisopropylpyrazole, 3,5-dimethyl-1-hydroxymethylpyrazole. 3,5-dimethyl-1-phenylpyrazole, 3,5-dimethylpyrazole, 3-amino-5-hydroxypyrazole, 4-methylpyrazole, N-methylpyrazole, 3-aminopyrazole, and 3-aminopyrazole It is done.
ピリミジン化合物としては、ピリミジン、1,3−ジフェニル−ピリミジン−2,4,6−トリオン、1,4,5,6−テトラヒドロピリミジン、2,4,5,6−テトラアミノピリミジンサルフェイト、2,4,5−トリヒドロキシピリミジン、2,4,6−トリアミノピリミジン、2,4,6−トリクロロピリミジン、2,4,6−トリメトキシピリミジン、2,4,6−トリフェニルピリミジン、2,4−ジアミノ−6−ヒドロキシルピリミジン、2,4−ジアミノピリミジン、2−アセトアミドピリミジン、2−アミノピリミジン、4−アミノピラゾロ[3,4−d]ピリミジン等が挙げられる。 Pyrimidine compounds include pyrimidine, 1,3-diphenyl-pyrimidine-2,4,6-trione, 1,4,5,6-tetrahydropyrimidine, 2,4,5,6-tetraaminopyrimidine sulfate, 2, 4,5-trihydroxypyrimidine, 2,4,6-triaminopyrimidine, 2,4,6-trichloropyrimidine, 2,4,6-trimethoxypyrimidine, 2,4,6-triphenylpyrimidine, 2,4 -Diamino-6-hydroxylpyrimidine, 2,4-diaminopyrimidine, 2-acetamidopyrimidine, 2-aminopyrimidine, 4-aminopyrazolo [3,4-d] pyrimidine and the like.
イミダゾール化合物としては、例えば、1,1’−カルボニルビス−1H−イミダゾール、1,1’−オキサリルジイミダゾール、1,2,4,5−テトラメチルイミダゾール、1,2−ジメチル−5−ニトロイミダゾール、1,2−ジメチルイミダゾール、1−(3−アミノプロピル)イミダゾール、1−ブチルイミダゾール、1−エチルイミダゾール、1−メチルイミダゾール、及びベンズイミダゾールが挙げられる。 Examples of the imidazole compound include 1,1′-carbonylbis-1H-imidazole, 1,1′-oxalyldiimidazole, 1,2,4,5-tetramethylimidazole, and 1,2-dimethyl-5-nitroimidazole. 1,2-dimethylimidazole, 1- (3-aminopropyl) imidazole, 1-butylimidazole, 1-ethylimidazole, 1-methylimidazole, and benzimidazole.
グアニジン化合物としては、例えば、1,1,3,3−テトラメチルグアニジン、1,2,3−トリフェニルグアニジン、1,3−ジ−o−トリルグアニジン、及び1,3−ジフェニルグアニジンが挙げられる。 Examples of the guanidine compound include 1,1,3,3-tetramethylguanidine, 1,2,3-triphenylguanidine, 1,3-di-o-tolylguanidine, and 1,3-diphenylguanidine. .
チアゾール化合物としては、例えば、2−メルカプトベンゾチアゾール、及び2,4−ジメチルチアゾールが挙げられる。 Examples of the thiazole compound include 2-mercaptobenzothiazole and 2,4-dimethylthiazole.
テトラゾール化合物としては、例えば、テトラゾール、5−メチルテトラゾール、5−アミノ−1H−テトラゾール、及び1−(2−ジメチルアミノエチル)−5−メルカプトテトラゾールが挙げられる。 Examples of the tetrazole compound include tetrazole, 5-methyltetrazole, 5-amino-1H-tetrazole, and 1- (2-dimethylaminoethyl) -5-mercaptotetrazole.
トリアジン化合物としては、例えば、3,4−ジヒドロ−3−ヒドロキシ−4−オキソ−1,2,4−トリアジンが挙げられる。 Examples of the triazine compound include 3,4-dihydro-3-hydroxy-4-oxo-1,2,4-triazine.
前記防食剤は一種を単独で、又は二種以上を組み合わせて使用できる。 The said anticorrosive agent can be used individually by 1 type or in combination of 2 or more types.
前記防食剤の含有量は、被研磨膜に対して更に高い研磨速度を得易い観点から、研磨剤の総質量に対し、0.001質量%以上であることが好ましく、0.01質量%以上であることがより好ましく、0.02質量%以上であることが更に好ましい。同様の観点から、前記防食剤の含有量は、研磨剤の総質量に対し、10質量%以下であることが好ましく、5.0質量%以下であることがより好ましく、0.5質量%以下であることが更に好ましい。前記防食剤の含有量は、研磨剤の総質量に対し、例えば、0.001質量%〜10質量%であってもよく、0.01質量%〜5.0質量%であってもよく、0.02質量%〜0.5質量%であってもよい。 The content of the anticorrosive is preferably 0.001% by mass or more and 0.01% by mass or more with respect to the total mass of the abrasive from the viewpoint of easily obtaining a higher polishing rate for the film to be polished. It is more preferable that it is 0.02% by mass or more. From the same viewpoint, the content of the anticorrosive is preferably 10% by mass or less, more preferably 5.0% by mass or less, and 0.5% by mass or less with respect to the total mass of the abrasive. More preferably. The content of the anticorrosive may be, for example, 0.001% by mass to 10% by mass, or 0.01% by mass to 5.0% by mass with respect to the total mass of the abrasive, 0.02 mass%-0.5 mass% may be sufficient.
防食剤としては、銅系及びコバルト系金属等の配線金属に対して保護膜を形成することで配線金属のエッチングを抑制して被研磨面の荒れを低減し易くする効果を好適に得る観点から、トリアゾール化合物、ピリジン化合物、イミダゾール化合物、テトラゾール化合物、トリアジン化合物及びヘキサメチレンテトラミンからなる群より選択される少なくとも一種が好ましく、トリアゾール化合物、3−ヒドロキシピリジン、ベンズイミダゾール、5−アミノ−1H−テトラゾール、3,4−ジヒドロ−3−ヒドロキシ−4−オキソ−1,2,4−トリアジン及びヘキサメチレンテトラミンからなる群より選ばれる少なくとも一種がより好ましく、トリアゾール化合物が更に好ましい。トリアゾール化合物としては、3H−1,2,3−トリアゾロ[4,5−b]ピリジン−3−オール、1−ヒドロキシベンゾトリアゾール、1H−1,2,3−トリアゾロ[4,5−b]ピリジン、及びベンゾトリアゾールからなる群より選ばれる少なくとも一種が好ましい。 As an anticorrosive agent, from the viewpoint of suitably obtaining the effect of suppressing the etching of the wiring metal and easily reducing the roughness of the surface to be polished by forming a protective film on the wiring metal such as copper-based and cobalt-based metals. , At least one selected from the group consisting of triazole compounds, pyridine compounds, imidazole compounds, tetrazole compounds, triazine compounds and hexamethylenetetramine is preferred, triazole compounds, 3-hydroxypyridine, benzimidazole, 5-amino-1H-tetrazole, At least one selected from the group consisting of 3,4-dihydro-3-hydroxy-4-oxo-1,2,4-triazine and hexamethylenetetramine is more preferable, and a triazole compound is still more preferable. Examples of the triazole compound include 3H-1,2,3-triazolo [4,5-b] pyridin-3-ol, 1-hydroxybenzotriazole, 1H-1,2,3-triazolo [4,5-b] pyridine. And at least one selected from the group consisting of benzotriazole is preferred.
本実施形態に係る研磨剤において、防食剤の含有量に対する酸成分の含有量の質量比(酸成分/防食剤)は、エッチング速度と研磨速度を良好に制御する観点から、10/1〜1/5の範囲であることが好ましく、7/1〜1/5の範囲であることがより好ましく、5/1〜1/5の範囲であることが更に好ましく、5/1〜1/1の範囲であることが特に好ましい。 In the abrasive according to this embodiment, the mass ratio of the content of the acid component to the content of the anticorrosive (acid component / anticorrosive) is 10/1 to 1 from the viewpoint of favorably controlling the etching rate and the polishing rate. / 5 is preferable, 7/1 to 1/5 is more preferable, 5/1 to 1/5 is further preferable, and 5/1 to 1/1 is preferable. A range is particularly preferred.
[酸化剤]
本実施形態に係る研磨剤は、酸化剤(酸化剤成分、金属酸化剤)を含有してもよい。研磨剤が酸化剤を含有することにより、金属材料(配線金属、バリア金属等。例えば金属層)の表面が酸化され、研磨速度を更に向上させることができると考えられる。前記酸化剤は、特に制限はなく、通常用いられる酸化剤から適宜選択することができる。酸化剤としては、過酸化水素、ペルオキソ硫酸塩、硝酸、過ヨウ素酸カリウム、次亜塩素酸、オゾン水等が挙げられ、これらの中でも過酸化水素が好ましい。酸化剤は、一種を単独で、又は、二種以上を組み合わせて使用できる。
[Oxidant]
The abrasive according to this embodiment may contain an oxidant (oxidant component, metal oxidant). It is considered that when the polishing agent contains an oxidizing agent, the surface of the metal material (wiring metal, barrier metal, etc., for example, a metal layer) is oxidized, and the polishing rate can be further improved. There is no restriction | limiting in particular in the said oxidizing agent, It can select suitably from the oxidizing agent used normally. Examples of the oxidizing agent include hydrogen peroxide, peroxosulfate, nitric acid, potassium periodate, hypochlorous acid, and ozone water. Among these, hydrogen peroxide is preferable. An oxidizing agent can be used individually by 1 type or in combination of 2 or more types.
酸化剤の含有量は、金属の酸化が不充分となり金属材料の研磨速度が低下することを防ぎ易い観点から、研磨剤の総質量に対し、0.01質量%以上が好ましく、0.02質量%以上がより好ましく、0.05質量%以上が更に好ましい。酸化剤の含有量は、被研磨面に荒れが生じることを容易に抑制できる共にディッシングを小さく抑え易い観点から、研磨剤の総質量に対し、5質量%以下が好ましく、3質量%以下がより好ましい。これらの観点から、酸化剤の含有量は、研磨剤の総質量に対し、例えば、0.01質量%〜5質量%であってもよい。なお、過酸化水素水のように、一般に水溶液として入手できる酸化剤を用いる場合、当該水溶液中に含まれる酸化剤の含有量が研磨剤において前記範囲になるように、酸化剤の含有量を調整できる。 The content of the oxidizing agent is preferably 0.01% by mass or more based on the total mass of the polishing agent from the viewpoint of easily preventing the metal from being oxidized insufficiently and reducing the polishing rate of the metal material, and 0.02% by mass. % Or more is more preferable, and 0.05 mass% or more is still more preferable. The content of the oxidizing agent is preferably 5% by mass or less, more preferably 3% by mass or less with respect to the total mass of the abrasive, from the viewpoint that it is possible to easily suppress the occurrence of roughness on the surface to be polished and to easily suppress dishing. preferable. From these viewpoints, the content of the oxidizing agent may be, for example, 0.01% by mass to 5% by mass with respect to the total mass of the abrasive. In addition, when using an oxidizing agent that is generally available as an aqueous solution, such as hydrogen peroxide, the content of the oxidizing agent is adjusted so that the content of the oxidizing agent contained in the aqueous solution is within the above range in the abrasive. it can.
[エーテル結合を有する水溶性高分子]
本実施形態に係る研磨剤は、エーテル結合を有する水溶性高分子を含有してもよい。エーテル結合を有する水溶性高分子を研磨剤が含有することにより、樹脂及び配線金属材料の更に高い研磨速度を得ることができる。
[Water-soluble polymer having an ether bond]
The abrasive according to this embodiment may contain a water-soluble polymer having an ether bond. When the abrasive contains a water-soluble polymer having an ether bond, a higher polishing rate of the resin and the wiring metal material can be obtained.
エーテル結合を有する水溶性高分子としては、エーテル結合を有し、水に溶解又は混和可能な高分子であれば特に制限はないが、ポリエーテル、モノエーテル化合物等が挙げられる。エーテル結合を有する水溶性高分子は、樹脂及び配線金属材料の研磨速度が向上し易い観点から、ポリエーテルであることが好ましい。 The water-soluble polymer having an ether bond is not particularly limited as long as it is a polymer having an ether bond and is soluble or miscible in water, and examples thereof include polyethers and monoether compounds. The water-soluble polymer having an ether bond is preferably a polyether from the viewpoint of easily improving the polishing rate of the resin and the wiring metal material.
前記ポリエーテルとしては、多糖類、ポリアルキレングリコール、ポリグリセリン、ポリオキシプロピレンポリグリセリルエーテル、ポリオキシエチレンポリグリセリルエーテル、グリセリン脂肪族エステル、ジグリセリン脂肪族エステル、芳香族グリコールエーテル、脂肪族グリコールエーテル、エステル系グリコールエーテル、酸化プロピレン付加物、没食子酸配糖体、フェノール類の配糖体、ポリフェノール類の配糖体、糖のエステル化合物、イソステアリン酸ポリオキシエチレングリセリル、トリイソステアリン酸ポリオキシエチレングリセリル、1,4−ジ(2−ヒドロキシエトキシ)ベンゼン、2,2−ビス(4−ポリオキシエチレン−オキシフェニル)プロパン、2,2−ビス(4−ポリオキシプロピレンオキシフェニル)プロパン、エチレングルコールモノフェニルエーテル、ジエチレングルコールモノフェニルエーテル、ポリオキシアルキレンモノフェニルエーテル、プロピレングルコールモノフェニルエーテル、ポリオキシプロピレンモノメチルフェニルエーテル、ポリエチレングルコールモノメチルエーテル、ペンタエリスリトールポリオキシエチレンエーテル、エチレングリコールモノアリルエーテル、ポリオキシエチレンモノアリルエーテル、ジメチロールヘプタンEO付加物、ジグリセリン脂肪族エステル、アルキルグルコシド等が挙げられる。本明細書において、「多糖類」とは、特に断らない限り、グリコシド結合によって重合度2以上重合した物質として定義される。 Examples of the polyether include polysaccharide, polyalkylene glycol, polyglycerin, polyoxypropylene polyglyceryl ether, polyoxyethylene polyglyceryl ether, glycerin aliphatic ester, diglycerin aliphatic ester, aromatic glycol ether, aliphatic glycol ether, ester Glycol ether, propylene oxide adduct, gallic acid glycoside, phenol glycoside, polyphenol glycoside, sugar ester compound, polyoxyethylene glyceryl isostearate, polyoxyethylene glyceryl triisostearate, 1 , 4-di (2-hydroxyethoxy) benzene, 2,2-bis (4-polyoxyethylene-oxyphenyl) propane, 2,2-bis (4-polyoxypropyleneoxyphenyl) propyl Bread, ethylene glycol monophenyl ether, diethylene glycol monophenyl ether, polyoxyalkylene monophenyl ether, propylene glycol monophenyl ether, polyoxypropylene monomethyl phenyl ether, polyethylene glycol monomethyl ether, pentaerythritol polyoxyethylene ether, Examples include ethylene glycol monoallyl ether, polyoxyethylene monoallyl ether, dimethylol heptane EO adduct, diglycerin aliphatic ester, and alkyl glucoside. In the present specification, “polysaccharide” is defined as a substance polymerized by a glycosidic bond with a polymerization degree of 2 or more unless otherwise specified.
多糖類としては、スクロース、ラクツロース、ラクトース、トレハロース、マルトース、セロビオース、コージビオース、ニゲロース、イソマルトース、イソトレハロース、ネオトレハロース、ソホロース、ラミナリビオース、ゲンチビオース、ツラノース、マルツロース、パラチノース、ゲンチオビウロース、マンノビオース、メリビオース、メリビウロース、ネオラクトース、ガラクトスクロース、シラビオース、ルチノース、ルチヌロース、ビシアノース、キシロビオース、プリメベロース、トレハロサミン、マルチトール、セロビオン酸、ラクトサミン、ラクトースジアミン、ラクトビオン酸、ラクチトール、ヒアロビウロン酸、スクラロース、ニゲロトリオース、マルトトリオース、メレジトース、マルトトリウロース、ラフィノース、ケストース、ニストース、ニゲロテトラオース、スタキオース、アミロース、デキストラン、デキストリン、マルトデキストリン、クラスターデキストリン、シクロアワオドリン、ラミナラン、カロース、PGA、ペクチン、グルコマンナン、ジェランガム、カードラン、サイリウム、ローカストビーンガム、プルラン、アルギン酸、タマリンド、カラギーナン、CMC、キサンタンガム、アラビアガム、グァーガム、ペクチン、大豆多糖類、フルクタン、グリコーゲン、α−シクロデキストリン、β−シクロデキストリン、γ−シクロデキストリン、イソマルトオリゴ糖、ガラクトオリゴ糖、キシロオリゴ糖、大豆オリゴ糖、ニゲロオリゴ糖、乳果オリゴ糖、フラクトオリゴ糖等が挙げられる。 Polysaccharides include sucrose, lactulose, lactose, trehalose, maltose, cellobiose, cordobiose, nigerose, isomaltose, isotrehalose, neotrehalose, sophorose, laminaribiose, gentibiose, tulanose, maltulose, palatinose, gentiobiose, mannobiose , Melibiose, melibiurose, neolactose, galactosucrose, silabiose, rutinose, rutinose, vicyanose, xylobiose, primeverose, trehalosamine, maltitol, cellobionic acid, lactosamine, lactosediamine, lactobionic acid, lactitol, hyalobiuronic acid, sucralose, nigerotriose Maltotriose, melezitose, maltotriurose, rafino , Kestose, nystose, nigerotetraose, stachyose, amylose, dextran, dextrin, maltodextrin, cluster dextrin, cycloawaodrine, laminaran, callose, PGA, pectin, glucomannan, gellan gum, curdlan, psyllium, locust bean gum , Pullulan, alginic acid, tamarind, carrageenan, CMC, xanthan gum, gum arabic, guar gum, pectin, soy polysaccharide, fructan, glycogen, α-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, isomaltoligosaccharide, galactooligosaccharide, Xylooligosaccharides, soybean oligosaccharides, nigerooligosaccharides, dairy oligosaccharides, fructooligosaccharides and the like can be mentioned.
α−グルコース重合物としては、アミロース、デキストラン、デキストリン、マルトデキストリン、クラスターデキストリン、α−シクロデキストリン、β−シクロデキストリン、γ−シクロデキストリン、マルトース、イソマルトース、マルトトリオース、スタキオース等が挙げられる。 Examples of the α-glucose polymer include amylose, dextran, dextrin, maltodextrin, cluster dextrin, α-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, maltose, isomaltose, maltotriose, stachyose and the like.
[有機溶媒]
本実施形態に係る研磨剤は、有機溶媒を含有してもよい。研磨剤が有機溶媒を含有することにより、樹脂及び配線金属材料の研磨速度及び研磨剤の濡れ性を更に向上させることができる。有機溶媒としては、特に制限はないが、20℃で液状の溶媒が好ましい。100gの水(20℃)に対する有機溶媒の溶解度は、研磨剤を高濃縮化する観点から、30g以上が好ましく、50g以上がより好ましく、100g以上が更に好ましい。有機溶媒は、一種を単独で、又は、二種以上を組み合わせて使用できる。
[Organic solvent]
The abrasive according to this embodiment may contain an organic solvent. When the abrasive contains an organic solvent, the polishing rate of the resin and the wiring metal material and the wettability of the abrasive can be further improved. Although there is no restriction | limiting in particular as an organic solvent, A liquid solvent is preferable at 20 degreeC. From the viewpoint of highly concentrating the abrasive, the solubility of the organic solvent in 100 g of water (20 ° C.) is preferably 30 g or more, more preferably 50 g or more, and even more preferably 100 g or more. An organic solvent can be used individually by 1 type or in combination of 2 or more types.
有機溶媒としては、炭酸エステル類、ラクトン類、グリコール類、グリコール類の誘導体等が挙げられる。炭酸エステル類としては、エチレンカーボネート、プロピレンカーボネート、ジメチルカーボネート、ジエチルカーボネート、メチルエチルカーボネート等が挙げられる。ラクトン類としては、ブチロラクトン、プロピオラクトン等が挙げられる。グリコール類としては、エチレングリコール、プロピレングリコール、ジエチレングリコール、ジプロピレングリコール、トリエチレングリコール、トリプロピレングリコール等が挙げられる。グリコール類の誘導体としては、グリコールモノエーテル類、グリコールジエーテル類等が挙げられる。グリコールモノエーテル類としては、エチレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールモノメチルエーテル、ジプロピレングリコールモノメチルエーテル、トリエチレングリコールモノメチルエーテル、トリプロピレングリコールモノメチルエーテル、エチレングリコールモノエチルエーテル、プロピレングリコールモノエチルエーテル、ジエチレングリコールモノエチルエーテル、ジプロピレングリコールモノエチルエーテル、トリエチレングリコールモノエチルエーテル、トリプロピレングリコールモノエチルエーテル、エチレングリコールモノプロピルエーテル、プロピレングリコールモノプロピルエーテル、ジエチレングリコールモノプロピルエーテル、ジプロピレングリコールモノプロピルエーテル、トリエチレングリコールモノプロピルエーテル、トリプロピレングリコールモノプロピルエーテル、エチレングリコールモノブチルエーテル、プロピレングリコールモノブチルエーテル、ジエチレングリコールモノブチルエーテル、ジプロピレングリコールモノブチルエーテル、トリエチレングリコールモノブチルエーテル、トリプロピレングリコールモノブチルエーテル等が挙げられる。グリコールジエーテル類としては、エチレングリコールジメチルエーテル、プロピレングリコールジメチルエーテル、ジエチレングリコールジメチルエーテル、ジプロピレングリコールジメチルエーテル、トリエチレングリコールジメチルエーテル、トリプロピレングリコールジメチルエーテル、エチレングリコールジエチルエーテル、プロピレングリコールジエチルエーテル、ジエチレングリコールジエチルエーテル、ジプロピレングリコールジエチルエーテル、トリエチレングリコールジエチルエーテル、トリプロピレングリコールジエチルエーテル、エチレングリコールジプロピルエーテル、プロピレングリコールジプロピルエーテル、ジエチレングリコールジプロピルエーテル、ジプロピレングリコールジプロピルエーテル、トリエチレングリコールジプロピルエーテル、トリプロピレングリコールジプロピルエーテル、エチレングリコールジブチルエーテル、プロピレングリコールジブチルエーテル、ジエチレングリコールジブチルエーテル、ジプロピレングリコールジブチルエーテル、トリエチレングリコールジブチルエーテル、トリプロピレングリコールジブチルエーテル等が挙げられる。有機溶媒としては、表面張力が低い観点から、グリコール類、及び、グリコール類の誘導体からなる群より選ばれる少なくとも一種が好ましく、表面張力が更に低い観点から、グリコールモノエーテル類がより好ましい。 Examples of the organic solvent include carbonate esters, lactones, glycols, and derivatives of glycols. Examples of the carbonic acid esters include ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, and methyl ethyl carbonate. Examples of lactones include butyrolactone and propiolactone. Examples of glycols include ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, triethylene glycol, and tripropylene glycol. Examples of the derivatives of glycols include glycol monoethers and glycol diethers. As glycol monoethers, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, diethylene glycol monomethyl ether, dipropylene glycol monomethyl ether, triethylene glycol monomethyl ether, tripropylene glycol monomethyl ether, ethylene glycol monoethyl ether , Propylene glycol monoethyl ether, diethylene glycol monoethyl ether, dipropylene glycol monoethyl ether, triethylene glycol monoethyl ether, tripropylene glycol monoethyl ether, ethylene glycol monopropyl ether, propylene glycol monopropyl ether, polyethylene Glycol monopropyl ether, dipropylene glycol monopropyl ether, triethylene glycol monopropyl ether, tripropylene glycol monopropyl ether, ethylene glycol monobutyl ether, propylene glycol monobutyl ether, diethylene glycol monobutyl ether, dipropylene glycol monobutyl ether, triethylene glycol mono Examples include butyl ether and tripropylene glycol monobutyl ether. As glycol diethers, ethylene glycol dimethyl ether, propylene glycol dimethyl ether, diethylene glycol dimethyl ether, dipropylene glycol dimethyl ether, triethylene glycol dimethyl ether, tripropylene glycol dimethyl ether, ethylene glycol diethyl ether, propylene glycol diethyl ether, diethylene glycol diethyl ether, dipropylene glycol Diethyl ether, triethylene glycol diethyl ether, tripropylene glycol diethyl ether, ethylene glycol dipropyl ether, propylene glycol dipropyl ether, diethylene glycol dipropyl ether, dipropylene glycol dipropyl ether, trie Glycol dipropyl ether, tripropylene glycol dipropyl ether, ethylene glycol dibutyl ether, propylene glycol dibutyl ether, diethylene glycol dibutyl ether, dipropylene glycol dibutyl ether, triethylene glycol dibutyl ether, tripropylene glycol dibutyl ether and the like. As the organic solvent, at least one selected from the group consisting of glycols and derivatives of glycols is preferable from the viewpoint of low surface tension, and glycol monoethers are more preferable from the viewpoint of lower surface tension.
有機溶媒の含有量は、樹脂及び配線金属材料に対する研磨剤の濡れ性が低下することを抑制する観点から、研磨剤の全質量基準で、0.500質量%以上が好ましく、1.000質量%以上がより好ましい。有機溶媒の含有量は、分散安定性に優れる観点から、研磨剤の全質量基準で、20.000質量%以下が好ましく、15.000質量%以下がより好ましく、10.000質量%以下が更に好ましい。 The content of the organic solvent is preferably 0.500% by mass or more and 1.000% by mass based on the total mass of the abrasive from the viewpoint of suppressing the wettability of the abrasive to the resin and the wiring metal material. The above is more preferable. From the viewpoint of excellent dispersion stability, the content of the organic solvent is preferably 20.000% by mass or less, more preferably 15.000% by mass or less, and further preferably 10.000% by mass or less, based on the total mass of the abrasive. preferable.
[絶縁材料研磨抑制剤]
本実施形態に係る研磨剤は、絶縁材料の研磨を抑制する成分として、絶縁材料研磨抑制剤(絶縁材料研磨抑制剤成分。例えば無機絶縁膜研磨抑制剤)を含有してもよい。研磨剤が絶縁材料研磨抑制剤を含有することにより、絶縁材料の研磨速度を抑制し、樹脂及び配線金属材料を絶縁材料に対して選択的に除去できる。
[Insulating material polishing inhibitor]
The abrasive according to this embodiment may contain an insulating material polishing inhibitor (insulating material polishing inhibitor component, for example, an inorganic insulating film polishing inhibitor) as a component that suppresses polishing of the insulating material. When the polishing agent contains the insulating material polishing inhibitor, the polishing rate of the insulating material can be suppressed, and the resin and the wiring metal material can be selectively removed with respect to the insulating material.
絶縁材料研磨抑制剤としては、例えば、アリルアミン系重合体が挙げられる。本明細書において「アリルアミン系重合体」とは、アリルアミン系化合物を含む単量体を重合して得られる構造単位を有する重合体として定義される。本明細書において「アリルアミン系化合物」とは、アリル基及びアミノ基を有する化合物として定義される。アリルアミン系重合体は、アリルアミン系化合物のみを重合して得られる構造単位を有していてもよく、アリルアミン系化合物と、アリルアミン系化合物以外の化合物とを共重合して得られる構造単位を有していてもよい。 Examples of the insulating material polishing inhibitor include allylamine polymers. In the present specification, the “allylamine polymer” is defined as a polymer having a structural unit obtained by polymerizing a monomer containing an allylamine compound. In this specification, an “allylamine compound” is defined as a compound having an allyl group and an amino group. The allylamine polymer may have a structural unit obtained by polymerizing only an allylamine compound, and has a structural unit obtained by copolymerizing an allylamine compound and a compound other than the allylamine compound. It may be.
絶縁材料研磨抑制剤は、一種を単独で、又は、二種以上を組み合わせて使用できる。 The insulating material polishing inhibitor can be used alone or in combination of two or more.
絶縁材料研磨抑制剤(アリルアミン系重合体等)の重量平均分子量(Mw)は、絶縁材料の研磨速度を抑制し易い観点から、500以上が好ましく、800以上がより好ましく、1000以上が更に好ましい。絶縁材料研磨抑制剤(アリルアミン系重合体等)の重量平均分子量は、粘度が過剰に高くなることが抑制されて良好な保存安定性が得られる観点から、300000以下が好ましく、200000以下がより好ましく、150000以下が更に好ましい。絶縁材料研磨抑制剤(アリルアミン系重合体等)の重量平均分子量は、ゲル浸透クロマトグラフィー(GPC:Gel Permeation Chromatography)を用いて、以下の条件で測定できる。
[条件]
試料:20μL
標準ポリエチレングリコール:ポリマー・ラボラトリー社製標準ポリエチレングリコール(分子量:106、194、440、600、1470、4100、7100、10300、12600、23000)
検出器:昭和電工株式会社製、RI−モニター、商品名「Syodex―RI SE−61」
ポンプ:株式会社日立製作所製、商品名「L−6000」
カラム:昭和電工株式会社製、商品名「GS−220HQ」、「GS−620HQ」をこの順番で連結して使用
溶離液:0.4mol/Lの塩化ナトリウム水溶液
測定温度:30℃
流速:1.00mL/min
測定時間:45min。
The weight average molecular weight (Mw) of the insulating material polishing inhibitor (allylamine polymer or the like) is preferably 500 or more, more preferably 800 or more, and still more preferably 1000 or more, from the viewpoint of easily suppressing the polishing rate of the insulating material. The weight average molecular weight of the insulating material polishing inhibitor (allylamine-based polymer or the like) is preferably 300000 or less, more preferably 200000 or less, from the viewpoint of suppressing the viscosity from becoming excessively high and obtaining good storage stability. 150,000 or less is more preferable. The weight average molecular weight of an insulating material polishing inhibitor (such as an allylamine polymer) can be measured under the following conditions using gel permeation chromatography (GPC).
[conditions]
Sample: 20 μL
Standard polyethylene glycol: Standard polyethylene glycol manufactured by Polymer Laboratory (molecular weight: 106, 194, 440, 600, 1470, 4100, 7100, 10300, 12600, 23000)
Detector: Showa Denko Co., Ltd., RI-monitor, product name “Syodex-RI SE-61”
Pump: Hitachi, Ltd., trade name “L-6000”
Column: Showa Denko Co., Ltd., trade names “GS-220HQ” and “GS-620HQ” connected in this order and used Eluent: 0.4 mol / L sodium chloride aqueous solution Measurement temperature: 30 ° C.
Flow rate: 1.00 mL / min
Measurement time: 45 min.
絶縁材料研磨抑制剤の含有量は、絶縁材料の研磨速度を抑制し易い観点から、研磨剤の全質量基準で、0.001質量%以上が好ましく、0.003質量%以上がより好ましく、0.004質量%以上が更に好ましく、0.005質量%以上が特に好ましい。絶縁材料研磨抑制剤の含有量は、樹脂及び配線金属材料の研磨速度が低下することを抑制し易く、絶縁材料に対する樹脂及び配線金属材料の研磨速度比を高く保持し易い観点から、研磨剤の全質量基準で、0.400質量%以下が好ましく、0.300質量%以下がより好ましく、0.200質量%以下が更に好ましく、0.100質量%以下が特に好ましい。 The content of the insulating material polishing inhibitor is preferably 0.001% by mass or more, more preferably 0.003% by mass or more, based on the total mass of the abrasive, from the viewpoint of easily suppressing the polishing rate of the insulating material. 0.004 mass% or more is more preferable, and 0.005 mass% or more is particularly preferable. The content of the insulating material polishing inhibitor is easy to suppress a decrease in the polishing rate of the resin and the wiring metal material, and from the viewpoint of easily maintaining a high polishing rate ratio of the resin and the wiring metal material to the insulating material. Based on the total mass, it is preferably 0.400% by mass or less, more preferably 0.300% by mass or less, still more preferably 0.200% by mass or less, and particularly preferably 0.100% by mass or less.
砥粒の全質量に対する絶縁材料研磨抑制剤の質量比(絶縁材料研磨抑制剤/砥粒)は、樹脂及び配線金属材料を絶縁材料に対して選択的に除去し易い観点から、0.002以上が好ましく、0.003以上がより好ましく、0.005以上が更に好ましい。砥粒の全質量に対する絶縁材料研磨抑制剤の質量比は、樹脂及び配線金属材料を高い研磨速度で除去し易い観点から、0.400以下が好ましく、0.300以下がより好ましく、0.200以下が更に好ましい。 The mass ratio of the insulating material polishing inhibitor to the total mass of the abrasive grains (insulating material polishing inhibitor / abrasive grains) is 0.002 or more from the viewpoint of easily removing the resin and the wiring metal material from the insulating material. Is preferable, 0.003 or more is more preferable, and 0.005 or more is more preferable. The mass ratio of the insulating material polishing inhibitor to the total mass of the abrasive grains is preferably 0.400 or less, more preferably 0.300 or less, and more preferably 0.200 from the viewpoint of easily removing the resin and the wiring metal material at a high polishing rate. The following is more preferable.
[界面活性剤]
研磨剤は、界面活性剤(界面活性剤成分)を含有していてもよい。研磨剤が界面活性剤を含有することにより、被研磨材料の研磨速度を容易に調整できると共に、研磨傷を容易に低減できる。
[Surfactant]
The abrasive may contain a surfactant (surfactant component). When the polishing agent contains a surfactant, the polishing rate of the material to be polished can be easily adjusted and polishing scratches can be easily reduced.
界面活性剤としては、水溶性陰イオン性界面活性剤、水溶性非イオン性界面活性剤、水溶性陽イオン性界面活性剤等が挙げられる。水溶性陰イオン性界面活性剤としては、ラウリル硫酸アンモニウム、ポリオキシエチレンラウリルエーテル硫酸アンモニウム、アルキルリン酸エステル塩、ポリオキシエチレンアルキルエーテルリン酸塩、ラウロイルサルコシン塩等が挙げられる。水溶性非イオン性界面活性剤としては、ポリオキシエチレンラウリルエーテル、ポリエチレングリコールモノステアレート等が挙げられる。水溶性陽イオン性界面活性剤としては、ヘキサデシルトリメチルアンモニウム塩、ミリスチルトリメチルアンモニウム塩、ラウリルトリメチルアンモニウム塩、ステアリルトリメチルアンモニウム塩、セチルトリメチルアンモニウム塩、ステアリルトリメチルアンモニウム塩、ジステアリルジメチルアンモニウム塩、アルキルベンジルジメチルアンモニウム塩、アルキルベンジルジメチルアンモニウム塩、ココナットアミンアセテート、ステアリルアミンアセテート等が挙げられる。これらの中でも、界面活性剤としては、水溶性陰イオン性界面活性剤が好ましい。特に、共重合成分としてアンモニウム塩又はテトラメチルアンモニウム塩を用いて得られた高分子分散剤等の水溶性陰イオン性界面活性剤の少なくとも一種を使用することがより好ましい。界面活性剤は、一種を単独で、又は、二種以上を組み合わせて使用できる。界面活性剤の含有量は、研磨剤の全質量基準で例えば0.0001〜0.1質量%である。 Examples of the surfactant include a water-soluble anionic surfactant, a water-soluble nonionic surfactant, and a water-soluble cationic surfactant. Examples of the water-soluble anionic surfactant include ammonium lauryl sulfate, polyoxyethylene lauryl ether ammonium sulfate, alkyl phosphate ester salt, polyoxyethylene alkyl ether phosphate, lauroyl sarcosine salt and the like. Examples of the water-soluble nonionic surfactant include polyoxyethylene lauryl ether and polyethylene glycol monostearate. Water-soluble cationic surfactants include hexadecyl trimethyl ammonium salt, myristyl trimethyl ammonium salt, lauryl trimethyl ammonium salt, stearyl trimethyl ammonium salt, cetyl trimethyl ammonium salt, stearyl trimethyl ammonium salt, distearyl dimethyl ammonium salt, alkylbenzyl Examples thereof include dimethylammonium salt, alkylbenzyldimethylammonium salt, coconutamine acetate, stearylamine acetate and the like. Among these, as the surfactant, a water-soluble anionic surfactant is preferable. In particular, it is more preferable to use at least one water-soluble anionic surfactant such as a polymer dispersant obtained by using an ammonium salt or a tetramethylammonium salt as a copolymerization component. Surfactant can be used individually by 1 type or in combination of 2 or more types. The content of the surfactant is, for example, 0.0001 to 0.1% by mass based on the total mass of the abrasive.
(その他)
研磨剤に含まれる各成分の配合方法及び研磨剤の希釈方法は、特に制限はなく、例えば、翼式攪拌機による攪拌、又は、超音波分散等で各成分を分散又は溶解させることができる。水に対する各成分の混合順序は限定されない。
(Other)
The blending method of each component contained in the abrasive and the dilution method of the abrasive are not particularly limited. For example, each component can be dispersed or dissolved by stirring with a blade-type stirrer or ultrasonic dispersion. The mixing order of each component with respect to water is not limited.
本実施形態に係る研磨剤は、砥粒と、水とを少なくとも含む一液式研磨剤として保存してもよく、スラリ(第一の液)と、添加液(第二の液)とを有する複数液式研磨剤として保存してもよい。複数液式研磨剤では、スラリと添加液とを混合して前記研磨剤となるように前記研磨剤の構成成分がスラリと添加液とに分けられる。スラリは、例えば、第一の砥粒、第二の砥粒及び水を少なくとも含む。添加液は、例えば、水を少なくとも含む。防食剤、酸化剤、pH調整剤、エーテル結合を有する水溶性高分子、有機溶媒、絶縁材料研磨抑制剤、界面活性剤、消泡剤、キレート剤等の添加剤は、スラリ及び添加液のうち添加液に含まれることが好ましい。なお、研磨剤の構成成分は、三液以上に分けて保存してもよい。 The abrasive according to this embodiment may be stored as a one-part abrasive containing at least abrasive grains and water, and has a slurry (first liquid) and an additive liquid (second liquid). It may be stored as a multi-liquid abrasive. In a multi-liquid type abrasive | polishing agent, the structural component of the said abrasive | polishing agent is divided into a slurry and an additive liquid so that slurry and an additive liquid may be mixed and it may become the said abrasive | polishing agent. The slurry includes, for example, at least a first abrasive grain, a second abrasive grain, and water. The additive liquid contains at least water, for example. Additives such as anticorrosives, oxidants, pH adjusters, water-soluble polymers with ether bonds, organic solvents, insulating material polishing inhibitors, surfactants, antifoaming agents, chelating agents, etc. It is preferable to be contained in the additive solution. The constituents of the abrasive may be stored in three or more liquids.
複数液式研磨剤においては、研磨直前又は研磨時にスラリ及び添加液が混合されて研磨剤が調製されてもよい。複数液式研磨剤におけるスラリと添加液とをそれぞれ研磨定盤上へ供給し、研磨定盤上においてスラリ及び添加液が混合されて得られる研磨剤を用いて被研磨面を研磨してもよい。 In the multi-liquid abrasive, the slurry and additive liquid may be mixed immediately before or during polishing to prepare the abrasive. The slurry and additive liquid in the multi-liquid type abrasive may be respectively supplied onto the polishing surface plate, and the surface to be polished may be polished using an abrasive obtained by mixing the slurry and the additive liquid on the polishing surface plate. .
<研磨剤用貯蔵液>
本実施形態に係る研磨剤用貯蔵液は、前記研磨剤を得るための貯蔵液であり、研磨剤用貯蔵液を水で希釈することにより前記研磨剤が得られる。研磨剤用貯蔵液は、水の量を使用時よりも減じて保管されており、使用前又は使用時に水で希釈されて前記研磨剤として用いられる。研磨剤用貯蔵液は、水の含有量が前記研磨剤よりも少ない点で前記研磨剤と異なっている。希釈倍率は、例えば1.5倍以上である。
<Abrasive stock solution>
The storage solution for abrasive | polishing agent which concerns on this embodiment is a storage solution for obtaining the said abrasive | polishing agent, and the said abrasive | polishing agent is obtained by diluting the storage solution for abrasive | polishing agents with water. The abrasive stock solution is stored with the amount of water reduced compared to the time of use, and is diluted with water before use or at the time of use and used as the abrasive. The abrasive stock solution is different from the abrasive in that the water content is less than that of the abrasive. The dilution factor is, for example, 1.5 times or more.
<研磨方法>
本実施形態に係る研磨方法は、研磨剤を用いて樹脂及び配線金属材料の少なくとも一部を研磨(CMP等)して除去する研磨工程を備えている。前記研磨工程では、樹脂及び配線金属材料を含む被研磨面を研磨することができる。前記研磨工程では、研磨剤を用いて、樹脂及び配線金属材料を有する基体を研磨して前記樹脂及び配線金属材料の少なくとも一部を除去することができる。基体は、例えば、表面に凹部及び凸部を有する基板上に形成された樹脂及び配線金属材料を有してもよい。基体は、例えば、配線板又は回路基板であってよい。本実施形態に係る研磨方法は、研磨工程の前に、樹脂及び配線金属材料を有する基体を用意する工程を備えていてもよい。前記樹脂は、ポリベンゾオキサゾール、ポリベンゾオキサゾールの前駆体及びポリイミドからなる群より選ばれる少なくとも一種を含むことが好ましい。
<Polishing method>
The polishing method according to the present embodiment includes a polishing step in which at least a part of the resin and the wiring metal material is removed by polishing (CMP or the like) using an abrasive. In the polishing step, the surface to be polished containing the resin and the wiring metal material can be polished. In the polishing step, at least a part of the resin and the wiring metal material can be removed by polishing a substrate having the resin and the wiring metal material using an abrasive. The base body may have, for example, a resin and a wiring metal material formed on a substrate having concave and convex portions on the surface. The substrate may be, for example, a wiring board or a circuit board. The polishing method according to the present embodiment may include a step of preparing a substrate having a resin and a wiring metal material before the polishing step. The resin preferably contains at least one selected from the group consisting of polybenzoxazole, a precursor of polybenzoxazole, and polyimide.
前記研磨工程は、一液式研磨剤を用いて、樹脂及び配線金属材料の少なくとも一部を研磨して除去する工程であってもよく、複数液式研磨剤におけるスラリと添加液とを混合して得られる研磨剤を用いて、樹脂及び配線金属材料の少なくとも一部を研磨して除去する工程であってもよく、研磨剤用貯蔵液を水で希釈して得られる研磨剤を用いて樹脂及び配線金属材料の少なくとも一部を研磨して除去する工程であってもよい。 The polishing step may be a step of polishing and removing at least a part of the resin and the wiring metal material using a one-component abrasive, and the slurry in the multiple-component abrasive and the additive solution are mixed. It may be a step of polishing and removing at least a part of the resin and the wiring metal material using the obtained abrasive, and the resin using the abrasive obtained by diluting the stock solution for abrasive with water. And a step of polishing and removing at least a part of the wiring metal material.
研磨工程では、樹脂及び配線金属材料に加えて絶縁材料を備える基体を研磨してもよい。この場合、研磨工程では、例えば、樹脂及び配線金属材料(配線金属、バリア金属等)を研磨して絶縁材料が露出したときに研磨が停止されてもよい。また、研磨工程では、樹脂、配線金属材料(配線金属、バリア金属等)及び必要に応じ絶縁材料を含む被研磨面の少なくとも一部を研磨することによりこれらの材料を同時に研磨してもよい。 In the polishing step, a substrate including an insulating material in addition to the resin and the wiring metal material may be polished. In this case, in the polishing step, for example, the polishing may be stopped when the resin and the wiring metal material (wiring metal, barrier metal, etc.) are polished and the insulating material is exposed. In the polishing step, these materials may be simultaneously polished by polishing at least a part of the surface to be polished including resin, wiring metal material (wiring metal, barrier metal, etc.) and, if necessary, an insulating material.
複数液式研磨剤を用いる場合、本実施形態に係る研磨方法は、研磨工程の前に、複数液式研磨剤におけるスラリと添加液とを混合して研磨剤を得る研磨剤調製工程を備えていてもよい。研磨剤用貯蔵液を用いる場合、本実施形態に係る研磨方法は、研磨工程の前に、研磨剤用貯蔵液を水で希釈して研磨剤を得る研磨剤調製工程を備えていてもよい。 When a multi-liquid abrasive is used, the polishing method according to the present embodiment includes an abrasive preparation step of obtaining an abrasive by mixing the slurry and additive liquid in the multi-liquid abrasive before the polishing step. May be. When using the storage solution for abrasive | polishing agent, the grinding | polishing method which concerns on this embodiment may be equipped with the abrasive | polishing agent preparation process which dilutes the storage liquid for abrasive | polishing agent with water before a grinding | polishing process.
研磨工程では、例えば、基体の被研磨面を研磨定盤の研磨布(研磨パッド)に押しあて、被研磨面と研磨布との間に研磨剤を供給して、基体の裏面(被研磨面と反対の面)に所定の圧力を加えた状態で、基体を研磨定盤に対して相対的に動かすことにより被研磨面を研磨することができる。 In the polishing step, for example, the surface to be polished of the substrate is pressed against the polishing cloth (polishing pad) of the polishing surface plate, and an abrasive is supplied between the surface to be polished and the polishing cloth, so that the back surface of the substrate (surface to be polished) The surface to be polished can be polished by moving the substrate relative to the polishing surface plate while applying a predetermined pressure to the surface opposite to the surface.
研磨装置としては、例えば、回転数を変更可能なモータ等が取り付けてあると共に研磨布を貼り付け可能な定盤と、基体を保持するホルダーとを有する一般的な研磨装置を使用できる。研磨布としては、特に制限はないが、一般的な不織布、発泡ポリウレタン、多孔質フッ素樹脂等が使用できる。研磨条件に特に制限はないが、基体が飛び出さないように定盤の回転速度は200回/min以下の低回転が好ましい。例えば、研磨している間、研磨布には研磨剤をポンプ等で連続的に供給する。研磨剤の供給量に制限はないが、研磨布の表面が常に研磨剤で覆われると共に、研磨の進行により生じる生成物が連続的に排出されることが好ましい。 As the polishing apparatus, for example, a general polishing apparatus having a surface plate to which a motor capable of changing the number of rotations and the like, and a polishing cloth can be attached, and a holder for holding the substrate can be used. Although there is no restriction | limiting in particular as abrasive cloth, A general nonwoven fabric, a polyurethane foam, a porous fluororesin, etc. can be used. The polishing conditions are not particularly limited, but the rotation speed of the surface plate is preferably a low rotation of 200 times / min or less so that the substrate does not jump out. For example, during polishing, an abrasive is continuously supplied to the polishing cloth with a pump or the like. Although there is no restriction | limiting in the supply amount of an abrasive | polishing agent, It is preferable that the surface of an abrasive cloth is always covered with an abrasive | polishing agent and the product produced by progress of grinding | polishing is discharged | emitted continuously.
研磨布の表面状態を常に同一にして研磨を行うために、本実施形態に係る研磨方法は、研磨工程の前に研磨布のコンディショニング工程を備えることが好ましい。例えば、ダイヤモンド粒子のついたドレッサを用いて、少なくとも水を含む液で研磨布のコンディショニングを行うことができる。本実施形態に係る研磨方法は、研磨工程後に、基体洗浄工程を備えることが好ましい。研磨終了後の基体は、流水中でよく洗浄後、スピンドライ等を用いて、基体上に付着した水滴を払い落としてから、乾燥させることが好ましい。また、市販の洗浄液を基体表面に流しつつ、ポリビニルアルコール系樹脂でできたブラシを回転させながら、当該ブラシを基体に一定の圧力で押し付けて基体上の付着物を除去する、公知の洗浄方法により洗浄した後に乾燥させることがより好ましい。 In order to perform polishing with the surface state of the polishing cloth always the same, the polishing method according to the present embodiment preferably includes a conditioning process of the polishing cloth before the polishing process. For example, using a dresser with diamond particles, the polishing pad can be conditioned with a liquid containing at least water. The polishing method according to this embodiment preferably includes a substrate cleaning step after the polishing step. The substrate after polishing is preferably washed in running water, and then dried after removing water droplets adhering to the substrate using spin drying or the like. In addition, while a commercially available cleaning liquid is poured on the surface of the substrate, a brush made of polyvinyl alcohol resin is rotated, and the brush is pressed against the substrate with a certain pressure to remove deposits on the substrate by a known cleaning method. It is more preferable to dry after washing.
本実施形態に係る研磨剤によれば、樹脂及び配線金属材料を有する基体を研磨して、樹脂及び配線金属材料の少なくとも一部を除去できる。このような特長を利用した用途としては、例えば、再配線工程に使われる樹脂及び配線金属材料研磨用途が挙げられる。 According to the abrasive | polishing agent which concerns on this embodiment, the base | substrate which has resin and wiring metal material can be grind | polished, and at least one part of resin and wiring metal material can be removed. As an application using such a feature, for example, a resin and wiring metal material polishing application used in a rewiring process can be cited.
樹脂の研磨速度は、研磨時間を短縮する観点から、200nm/min以上が好ましく、300nm/min以上がより好ましく、500nm/min以上が更に好ましく、1000nm/min以上が特に好ましい。樹脂の研磨速度は、樹脂の凹部の過剰な研磨が進むことが抑制されて平坦性が更に向上する観点、及び、研磨時間を調整することが容易である観点から、5000nm/min以下が好ましく、3000nm/min以下がより好ましい。 From the viewpoint of shortening the polishing time, the resin polishing rate is preferably 200 nm / min or more, more preferably 300 nm / min or more, still more preferably 500 nm / min or more, and particularly preferably 1000 nm / min or more. The polishing rate of the resin is preferably 5000 nm / min or less from the viewpoint that the excessive polishing of the concave portion of the resin is suppressed and the flatness is further improved, and the polishing time is easy to adjust. 3000 nm / min or less is more preferable.
配線金属材料の研磨速度は、研磨時間を短縮する観点から、200nm/min以上が好ましく、250nm/min以上がより好ましく、300nm/min以上が更に好ましい。配線金属材料の研磨速度は、研磨後の樹脂との表面高さを揃え易い観点から、2000nm/min以下が好ましく、1000nm/min以下がより好ましい。 From the viewpoint of shortening the polishing time, the polishing rate of the wiring metal material is preferably 200 nm / min or more, more preferably 250 nm / min or more, and further preferably 300 nm / min or more. The polishing rate of the wiring metal material is preferably 2000 nm / min or less, more preferably 1000 nm / min or less, from the viewpoint of easily aligning the surface height with the resin after polishing.
以下、実施例により本発明を更に詳しく説明するが、本発明の技術的思想を逸脱しない限り、本発明はこれらの実施例に限定されるものではない。例えば、研磨剤の材料及びその配合比率は、本実施例記載の種類及び比率以外でも構わないし、研磨対象の組成及び構造も、本実施例記載以外の組成及び構造でも構わない。 EXAMPLES Hereinafter, although an Example demonstrates this invention in more detail, this invention is not limited to these Examples, unless it deviates from the technical idea of this invention. For example, the material of the abrasive and the blending ratio thereof may be other than the types and ratios described in this example, and the composition and structure of the polishing target may be other than those described in this example.
<研磨剤の調製>
(実施例1)
第一の砥粒としてコロイダルシリカ1(コロイダルシリカ、平均粒径:60nm)を、第二の砥粒としてコロイダルシリカにアルミニウム化合物(水酸化アルミニウム)が付着した砥粒(平均粒径:100nm、以下、「修飾砥粒1」ともいう)を、それぞれ準備した。
<Preparation of abrasive>
Example 1
Colloidal silica 1 (colloidal silica, average particle diameter: 60 nm) as the first abrasive grains, and abrasive grains (average particle diameter: 100 nm, below) with the aluminum compound (aluminum hydroxide) attached to the colloidal silica as the second abrasive grains , Also referred to as “modified abrasive grains 1”).
コロイダルシリカ1(第一の砥粒)5.00質量部に、修飾砥粒1(第二の砥粒)0.30質量部、有機溶媒として有機溶媒1(プロピレングルコールモノメチルエーテルアセテート)5.00質量部、防食剤としてBTA0.20質量部、pH調整剤としてリンゴ酸、超純水X質量部、及び酸化剤として過酸化水素を添加することで研磨剤100質量部を得た。修飾砥粒1は、コロイダルシリカの全質量に対して分散剤として酢酸を5.0質量%含むコロイダルシリカ分散液を用いて供給した。なお、超純水の配合量(X質量部)は、研磨剤が100質量部になるよう計算して調整した。また、過酸化水素は、過酸化水素水(濃度:30質量%)を用いて供給し、過酸化水素水としての配合量を1.05質量部とした。 4. 5.00 parts by mass of colloidal silica 1 (first abrasive), 0.30 parts by mass of modified abrasive 1 (second abrasive), and organic solvent 1 (propylene glycol monomethyl ether acetate) as an organic solvent 00 parts by mass, BTA 0.20 parts by mass as an anticorrosive, malic acid, ultrapure water X parts by mass as a pH adjuster, and hydrogen peroxide as an oxidizing agent were added to obtain 100 parts by mass of an abrasive. The modified abrasive grain 1 was supplied using a colloidal silica dispersion containing 5.0% by mass of acetic acid as a dispersant with respect to the total mass of the colloidal silica. In addition, the compounding quantity (X mass part) of ultrapure water was adjusted and calculated so that an abrasive | polishing agent might be 100 mass parts. Moreover, hydrogen peroxide was supplied using hydrogen peroxide water (concentration: 30 mass%), and the compounding amount as hydrogen peroxide water was 1.05 parts by mass.
(実施例2〜8、比較例1〜4)
第一及び第二の砥粒、有機溶媒、防食剤、酸化剤及びpH調整剤の種類並びに含有量を表1及び表2のとおりに変更した以外は、実施例1と同様の方法で研磨剤を調製した。表1及び表2の各成分の量は、研磨剤の全質量を基準とした含有量(単位:質量%)である。
(Examples 2-8, Comparative Examples 1-4)
Abrasives in the same manner as in Example 1 except that the types and contents of the first and second abrasive grains, organic solvent, anticorrosive, oxidizing agent and pH adjuster were changed as shown in Tables 1 and 2. Was prepared. The amount of each component in Table 1 and Table 2 is the content (unit: mass%) based on the total mass of the abrasive.
表1及び表2中、第一の砥粒としてのコロイダルシリカ2は、平均粒径70nmのコロイダルシリカであり、修飾砥粒2はコロイダルシリカにアルミニウム化合物(水酸化アルミニウム)が付着した平均粒径30nmの砥粒である。また、有機溶媒2はプロピレングリコールモノプロピルエーテルである。 In Tables 1 and 2, colloidal silica 2 as the first abrasive grains is colloidal silica having an average particle diameter of 70 nm, and modified abrasive grains 2 have an average particle diameter in which an aluminum compound (aluminum hydroxide) is attached to the colloidal silica. 30 nm abrasive grains. The organic solvent 2 is propylene glycol monopropyl ether.
<研磨剤のpH測定>
研磨剤のpHを下記の条件で測定した。結果を表1及び表2に示す。
測定温度:25±5℃
測定装置:株式会社堀場製作所の商品名:Model(F−51)
測定方法:フタル酸塩pH標準液(pH:4.01)と、中性リン酸塩pH標準液(pH:6.86)と、ホウ酸塩pH標準液(pH:9.18)とをpH標準液として用い、pHメーターを3点校正した後、pHメーターの電極を研磨剤に入れて、2min以上経過して安定した後のpHを前記測定装置により測定した。
<Measurement of pH of abrasive>
The pH of the abrasive was measured under the following conditions. The results are shown in Tables 1 and 2.
Measurement temperature: 25 ± 5 ° C
Measuring device: Product name of Horiba, Ltd .: Model (F-51)
Measurement method: phthalate pH standard solution (pH: 4.01), neutral phosphate pH standard solution (pH: 6.86), and borate pH standard solution (pH: 9.18) After the pH meter was calibrated at three points using the pH standard solution, the pH meter electrode was placed in an abrasive and the pH after stabilizing for 2 minutes or more was measured with the measuring device.
<ゼータ電位の測定>
研磨剤中における砥粒のゼータ電位を下記のとおり測定した。ゼータ電位測定装置としては、ベックマンコールター社製の商品名:DELSA NANO Cを用いた。ゼータ電位測定装置において測定サンプルの散乱強度が1.0×104〜5.0×104cpsとなるように研磨剤を純水で希釈してサンプルを得た。その後、得られたサンプルをゼータ電位測定用セルに入れてゼータ電位を測定した。全ての実施例において、砥粒の表面は、研磨剤中において正に帯電していた。
<Measurement of zeta potential>
The zeta potential of the abrasive grains in the abrasive was measured as follows. As the zeta potential measuring device, trade name: DELSA NANO C manufactured by Beckman Coulter, Inc. was used. The sample was obtained by diluting the abrasive with pure water so that the scattering intensity of the measurement sample was 1.0 × 10 4 to 5.0 × 10 4 cps in a zeta potential measurement device. Thereafter, the obtained sample was put in a cell for measuring zeta potential, and zeta potential was measured. In all examples, the surface of the abrasive grains was positively charged in the abrasive.
<研磨特性の評価>
(研磨速度の評価)
被研磨膜を有する基体として、厚み8000nmのポリイミド膜(PI膜)をシリコン基板上に形成して得られた基体と、厚み1000nmの銅膜(Cu膜)をシリコン基板上に形成して得られた基体と、厚み1000nmのTEOS(テトラエトキシシラン、オルトケイ酸テトラエチル)膜をシリコン基板上に形成して得られた基体とを用いた。
<Evaluation of polishing characteristics>
(Evaluation of polishing rate)
As a substrate having a film to be polished, a substrate obtained by forming a polyimide film (PI film) with a thickness of 8000 nm on a silicon substrate and a copper film (Cu film) with a thickness of 1000 nm are obtained on a silicon substrate. The base obtained by forming a TEOS (tetraethoxysilane, tetraethyl orthosilicate) film having a thickness of 1000 nm on a silicon substrate was used.
前記で調製した研磨剤を用いて、下記研磨条件にて60秒間被研磨膜を化学機械研磨した。なお、TEOS膜の研磨は、実施例1〜8において行った。 Using the polishing agent prepared above, the film to be polished was subjected to chemical mechanical polishing for 60 seconds under the following polishing conditions. The TEOS film was polished in Examples 1-8.
[研磨条件]
研磨装置:片面用研磨機(アプライドマテリアルズ製、商品名:Reflexion LK)
研磨布:スウェード状発泡ポリウレタン樹脂製研磨布
定盤回転数:123回/min
ヘッド回転数:117回/min
研磨圧力:21kPa
研磨剤の供給量:300mL/min
[Polishing conditions]
Polishing device: single-side polishing machine (Applied Materials, trade name: Reflexion LK)
Polishing cloth: Polishing cloth made of suede foam polyurethane resin Surface plate rotation speed: 123 times / min
Head rotation speed: 117 times / min
Polishing pressure: 21 kPa
Abrasive supply amount: 300 mL / min
前記研磨条件で研磨した基体の被研磨面にスポンジブラシ(ポリビニルアルコール系樹脂製)を押し付け、蒸留水を被研磨面に供給しながら基体とスポンジブラシとを回転させ、60秒間洗浄した。次に、スポンジブラシを取り除き、基体の被研磨面に蒸留水を60秒間供給した。最後に、基体を高速で回転させることで蒸留水を弾き飛ばして基体を乾燥させた。 A sponge brush (made of polyvinyl alcohol resin) was pressed against the surface to be polished of the substrate polished under the above polishing conditions, and the substrate and the sponge brush were rotated while supplying distilled water to the surface to be polished, and washed for 60 seconds. Next, the sponge brush was removed, and distilled water was supplied to the polished surface of the substrate for 60 seconds. Finally, the substrate was dried by spinning off the distilled water by rotating the substrate at a high speed.
研磨速度は、研磨前後における被研磨膜の膜厚を測定して得られる膜厚差から算出した。PI膜及びTEOS膜の膜厚の測定には、膜厚測定装置(大日本スクリーン製造株式会社製、商品名:ラムダエース、VL−M8000LS)を用いた。銅膜の膜厚の測定には、金属膜厚測定装置(日立国際電気株式会社製、商品名:VR−120/08S)を用いた。研磨速度の測定結果を表1及び表2に示す。 The polishing rate was calculated from the difference in film thickness obtained by measuring the film thickness of the film to be polished before and after polishing. A film thickness measuring device (Dainippon Screen Mfg. Co., Ltd., trade name: Lambda Ace, VL-M8000LS) was used to measure the film thickness of the PI film and TEOS film. A metal film thickness measuring device (manufactured by Hitachi Kokusai Electric Co., Ltd., trade name: VR-120 / 08S) was used for measuring the film thickness of the copper film. Tables 1 and 2 show the measurement results of the polishing rate.
表1及び表2に示されるとおり、実施例及び比較例を比較すると、シリカ粒子である第一の砥粒と、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミニウム化合物からなる粒子を除く)である第二の砥粒とを、第一の砥粒:第二の砥粒=20:1〜2:1の質量比で用い、pHが3.5以下である研磨剤を用いることで、樹脂及び配線金属材料の高い研磨速度が得られることがわかる。 As shown in Table 1 and Table 2, when Examples and Comparative Examples are compared, the first abrasive grains that are silica particles and particles to which at least one selected from the group consisting of an aluminum compound and an aluminum ion adheres (aluminum compound) Polishing with a pH of 3.5 or less, using a second abrasive grain that is a first abrasive grain: second abrasive grain = 20: 1 to 2: 1. It can be seen that a high polishing rate of the resin and the wiring metal material can be obtained by using the agent.
Claims (7)
前記第一の砥粒がシリカ粒子であり、
前記第二の砥粒が、アルミニウム化合物及びアルミニウムイオンからなる群より選ばれる少なくとも一種が付着した粒子(アルミニウム化合物からなる粒子を除く)であり、
前記第一の砥粒及び前記第二の砥粒の含有量の質量比が、第一の砥粒:第二の砥粒=20:1〜2:1であり、
pHが3.5以下である、樹脂及び配線金属材料研磨用研磨剤。 Containing first abrasive grains, second abrasive grains and water,
The first abrasive grains are silica particles;
The second abrasive grains are particles to which at least one selected from the group consisting of an aluminum compound and aluminum ions is attached (excluding particles consisting of an aluminum compound),
The mass ratio of the contents of the first abrasive grains and the second abrasive grains is first abrasive grains: second abrasive grains = 20: 1 to 2: 1,
Polishing agent for polishing resin and wiring metal material having pH of 3.5 or less.
水で希釈することにより前記研磨剤が得られる、研磨剤用貯蔵液。 An abrasive stock solution for obtaining the abrasive according to any one of claims 1 to 4,
A storage solution for abrasives, which is obtained by diluting with water.
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JP2007273910A (en) * | 2006-03-31 | 2007-10-18 | Fujifilm Corp | Polishing composition liquid |
JP2009279720A (en) * | 2008-05-23 | 2009-12-03 | Jgc Catalysts & Chemicals Ltd | Particle-dispersed fluid for polishing, and manufacturing method thereof |
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WO2020141804A1 (en) * | 2018-12-31 | 2020-07-09 | 주식회사 동진쎄미켐 | Chemical-mechanical polishing particle and polishing slurry composition comprising same |
JP7404393B2 (en) | 2018-12-31 | 2023-12-25 | ドンジン セミケム カンパニー リミテッド | Chemical mechanical polishing particles and polishing slurry compositions containing the same |
WO2020196542A1 (en) * | 2019-03-27 | 2020-10-01 | 株式会社フジミインコーポレーテッド | Polishing composition, polishing method, and method for producing substrate |
US20220055180A1 (en) * | 2019-03-27 | 2022-02-24 | Fujimi Incorporated | Polishing composition, polishing method, and method for producing substrate |
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WO2023181810A1 (en) * | 2022-03-23 | 2023-09-28 | 株式会社フジミインコーポレーテッド | Polishing composition and polishing method using same |
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