JP4569244B2 - Surface layer thickness measurement method - Google Patents
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Description
本発明は、ロール型帯電器を始めとする帯電器の表面層の膜厚を測定する方法に関する。 The present invention relates to a method for measuring the film thickness of a surface layer of a charger such as a roll charger.
クリーナレスシステムにおいて用いられる帯電器の表面層をコーティングする時には、膜厚を一定にコントロールする必要がある。従来、この膜厚の制御は、表面コート工程内で一定間隔で抜き取り、コート状態を破壊検査で実施していた。このため、測定したロールに関しては破棄せざるを得ず、無駄が発生していた。また、コート工程の初期段階では、コートが安定せず、ロールを無駄に消費する問題点があった。 When coating the surface layer of a charger used in a cleanerless system, it is necessary to control the film thickness to be constant. Conventionally, this film thickness control has been carried out at regular intervals in the surface coating process, and the coating state has been implemented by destructive inspection. For this reason, the measured roll has to be discarded, and waste has occurred. In addition, at the initial stage of the coating process, there is a problem that the coating is not stable and the roll is consumed wastefully.
具体的に説明すると、表面層を有する帯電ロールは例えば、以下のようにして作製される。まず、金属シャフトの周囲に弾性体層を設ける。その後、弾性体層上に表面層を形成するための表面コート工程に入り、スプレーコートや突き上げ法等により表面層が形成されて、上記帯電ロールが作製される。上記工程では、コート材料（表面層を形成するための塗布液）が作製されてからの時間で、コートされる膜厚に差が発生してしまう。そのため、所望のコート膜厚にするための突き上げ法では、コート開始時にコート液を希釈したり、突き上げスピードを増減させたりして管理している。初期状態での膜厚は管理しやすいが、工程内での管理は困難である。工程内で、膜厚の変化を調査した結果は、図２に示すように、２ロットまでは比較的安定した膜厚を維持しているが、３ロット目で膜厚が急激に低下していることが分かる。コート液を変更すると、４ロット目からは安定した状態を維持できる。３ロット目における膜厚の急激な低下を、非破壊で簡易に確認できれば、工程管理の効率化が図られ、コスト削減にもつながる。 Specifically, the charging roll having the surface layer is produced as follows, for example. First, an elastic body layer is provided around the metal shaft. Thereafter, a surface coating step for forming a surface layer on the elastic body layer is entered, and the surface layer is formed by spray coating, a push-up method or the like, and the charging roll is manufactured. In the above process, a difference occurs in the coated film thickness in the time after the coating material (coating liquid for forming the surface layer) is produced. For this reason, in the push-up method for obtaining a desired coat film thickness, the coating liquid is diluted at the start of coating, or the push-up speed is increased or decreased for management. Although the film thickness in the initial state is easy to manage, it is difficult to manage it in the process. As a result of investigating the change in film thickness within the process, as shown in FIG. 2, a relatively stable film thickness is maintained up to 2 lots, but the film thickness rapidly decreases in the 3rd lot. I understand that. If the coating solution is changed, a stable state can be maintained from the fourth lot. If a rapid decrease in film thickness in the third lot can be easily confirmed non-destructively, process management can be made more efficient, leading to cost reduction.
非破壊で膜厚を測定する方法として、紫外線吸収剤を混入した透明な塗膜が形成された標準試験体の表面に照射した紫外線の反射率と、塗膜の膜厚とから膜厚の検量線図を予め作成しておき、標準試験体と同一組成の透明な塗料を基材表面に塗布して製造した被試験体の表面に紫外線を照射し、紫外線の反射率から先の検量線図を基にして被試験体の膜厚を測定する方法が提案されている（例えば、特許文献１参照）。 As a non-destructive method for measuring the film thickness, the film thickness is calibrated from the reflectivity of the ultraviolet rays irradiated on the surface of the standard specimen on which a transparent coating film mixed with an ultraviolet absorber is formed and the coating film thickness. Prepare a diagram in advance, irradiate the surface of the test specimen manufactured by applying a transparent paint with the same composition as the standard test specimen on the surface of the base material, and calculate the previous calibration curve from the reflectance of the ultraviolet radiation. A method for measuring the film thickness of a device under test has been proposed (for example, see Patent Document 1).
しかし、上記方法では、下地材料に紫外線を反射させる材料である必要があり、一般的なゴム材料が選択できないといった問題がある。また、帯電ロールの表面層のような１０μｍ程度以下の膜厚測定には、不向きである。
以上から、本発明は、上記従来の課題を解決することを目的とする。すなわち、本発明は、非破壊での膜厚測定が可能で、簡便かつ低コストな表面層の膜厚測定方法を提供することを目的とする。 In view of the above, an object of the present invention is to solve the above conventional problems. That is, an object of the present invention is to provide a simple and low-cost method for measuring a film thickness of a surface layer, capable of nondestructive film thickness measurement.
上記目的は下記の本発明により達成される。
すなわち、本発明は、表面層が形成された帯電器の当該表面層の膜厚を測定する方法であって、「白色導電材」としての酸化スズ、または、「導電材」としてのカーボンおよび「白色微粉末」としてのシリカ、酸化チタン、ＰＴＦＥおよびフッ化炭素からなる群から選択される少なくとも１つ、を前記表面層中に含有し、前記表面層中の前記白色微粉末または前記白色導電材の含有量が１０〜４０質量％であり、前記表面層の膜厚が２〜１０μｍであり、下記の方法により作成した検量線をもとにして、前記表面層に光を照射し、その反射濃度から、前記膜厚を算出することを特徴とする表面層の膜厚測定方法である。
−検量線の作成方法−
「白色導電材」または「導電材および白色微粉末」の濃度を一定として表面層を形成するための塗布液を作製し、この塗布液を使用して少なくとも３通りの厚みの表面層を形成し、その後反射濃度計によりそれぞれの反射濃度を測定し、一方で表面層の断面から実際の膜厚を測定し、それぞれの前記反射濃度および前記実際の膜厚から、表面層の膜厚と反射濃度との関係を示す検量線を作成する
The above object is achieved by the present invention described below.
That is, the present invention is a method for measuring the film thickness of the surface layer of the charger on which the surface layer is formed, and includes tin oxide as the “white conductive material” or carbon as the “conductive material ” and “ At least one selected from the group consisting of silica, titanium oxide, PTFE and fluorocarbon as “white fine powder” is contained in the surface layer, and the white fine powder or the white conductive material in the surface layer The surface layer has a thickness of 2 to 10 μm, and based on a calibration curve prepared by the following method, the surface layer is irradiated with light, and its reflection It is a method for measuring a film thickness of a surface layer, wherein the film thickness is calculated from a concentration.
-How to create a calibration curve-
A coating liquid for forming a surface layer is prepared with a constant concentration of “white conductive material” or “conductive material and white fine powder”, and a surface layer having at least three thicknesses is formed using this coating liquid. Then, each reflection density is measured with a reflection densitometer, while the actual film thickness is measured from the cross section of the surface layer, and from the reflection density and the actual film thickness, the film thickness and reflection density of the surface layer are measured. A calibration curve showing the relationship between
本発明によれば、非破壊での膜厚測定が可能で、簡便かつ低コストな表面層の膜厚測定方法を提供することができる。 According to the present invention, a nondestructive film thickness measurement is possible, and a simple and low-cost method for measuring a film thickness of a surface layer can be provided.
本発明の膜厚測定方法は、表面層が形成された帯電器の当該表面層の膜厚を測定する方法である。測定方法としては、表面層に光を照射してその反射濃度を測定し、その測定値から膜厚を算出するものである。特に、表面層の厚さが２〜１０μｍの場合に用いる。 The film thickness measuring method of the present invention is a method for measuring the film thickness of the surface layer of the charger having the surface layer formed thereon. As a measuring method, the surface layer is irradiated with light, its reflection density is measured, and the film thickness is calculated from the measured value. Particularly, it is used when the thickness of the surface layer is 2 to 10 μm.
膜厚の具体的な測定方法としては、まず、各ロットごとに表面層を形成するための塗布液を作製する際に、塗布液中の「白色導電材」または「導電材および白色微粉末」の濃度を一定としておく。そして、この塗布液を使用して、少なくとも３通りの厚みの表面層を形成する。その後、反射濃度計によりそれぞれの反射濃度を測定する。 As a specific method for measuring the film thickness, first, when preparing a coating liquid for forming a surface layer for each lot, the “white conductive material” or “conductive material and fine white powder” in the coating liquid. The concentration of is kept constant. And using this coating liquid, the surface layer of at least 3 types of thickness is formed. Thereafter, each reflection density is measured by a reflection densitometer.
また、一方で、表面層の断面からマイクロスコープなどにより膜厚を測定して実際の膜厚を測定しておく。そして、上記それぞれの反射濃度および実際の膜厚から、表面層の膜厚と反射濃度との関係を示す検量線を作成する。この検量線をもとにして、上記塗布液をその後使用した場合に、反射濃度を測定するだけで、非破壊かつ非接触で表面層の膜厚を算出するができる。そのため、コストダウンを図ることができる。また、計測が非破壊で非接触なため容易であり、時間もかからないというメリットもある。 On the other hand, the actual film thickness is measured by measuring the film thickness from a cross section of the surface layer with a microscope or the like. Then, a calibration curve showing the relationship between the film thickness of the surface layer and the reflection density is created from each of the reflection densities and the actual film thicknesses. Based on this calibration curve, when the coating solution is subsequently used, the thickness of the surface layer can be calculated in a non-destructive and non-contact manner simply by measuring the reflection density. Therefore, cost reduction can be achieved. In addition, there is an advantage that measurement is easy because it is non-destructive and non-contact, and does not take time.
既述のように、表面層中には、「白色導電材」または「導電材および白色微粉末」を含有させる。これらを含有させることで、反射濃度の測定が可能となる。 As described above, the surface layer contains “white conductive material” or “conductive material and white fine powder”. By containing these, the reflection density can be measured.
白色導電材としては、導電処理した酸化スズを使用する。酸化スズは、表面層中での分散性がよく、帯電ロールの表面層に含有させた場合に、良好な材料特性を発揮し得る点でも好適だからである。 As the white conductive material, to use a conductive-treated acid dregs's. This is because tin oxide has good dispersibility in the surface layer and is preferable in that it can exhibit good material properties when contained in the surface layer of the charging roll.
また、白色導電材の代わりに、導電材および白色微粉末を使用することもできる。白色微粉末は反射濃度の測定に必要となり、導電材は帯電装置の帯電特性を得るために必要となる。 Moreover, a conductive material and white fine powder can also be used instead of a white conductive material. The white fine powder is necessary for measuring the reflection density, and the conductive material is necessary for obtaining the charging characteristics of the charging device.
白色微粉末としては、シリカ、酸化チタン、ＰＴＦＥおよびフッ化炭素からなる群から選択される少なくとも１つを使用し、高い分散性を得る観点から、シリカまたは酸化チタンを使用することがより好ましい。 The fine white powder, silica, titanium oxide, using at least one is selected from the group consisting of PTFE and fluorocarbon, in view of obtaining high dispersibility, it is more preferably used silica or titanium oxide.
また、導電材としては、カーボンを使用し、表面層中に１０〜３０質量％含有させることが好ましい。カーボンには、ケッチェンブラック、サーマルブラック、アセチレンブラック、黒鉛等が使用可能である。ケッチェンブラックは、給油性が高く導電性に優れた特性を有しており、サーマルブラックは給油性が小さくゴム補強性が強い特性を有している。これらの導電性カーボンは、単独でも使用可能であるが、特にケッチェンブラックとサーマルブラックとを併用すると、半導電性領域での抵抗値の急激な変化を抑えることができ、比較的少量の使用で半導電性領域でのバラツキの少ない導電性化が可能である。 Moreover, as a electrically conductive material, it is preferable to use carbon and to make it contain 10-30 mass% in a surface layer. As the carbon, ketjen black, thermal black, acetylene black, graphite and the like can be used. Ketjen Black has high oil supply properties and excellent electrical conductivity, and thermal black has low oil supply properties and strong rubber reinforcement properties. These conductive carbons can be used alone, but when ketjen black and thermal black are used in combination, a rapid change in resistance value in the semiconductive region can be suppressed, and a relatively small amount can be used. Thus, it is possible to achieve conductivity with little variation in the semiconductive region.
表面層中の白色微粉末または白色導電材の含有量は、１０〜４０質量％であり、２０〜３０質量％であることがより好ましい。 The content of fine white powder or a white conductive material in the surface layer, Ri 10-40% by mass, and more preferably 20 to 30 wt%.
本発明者らの実験によると、上記範囲とすることで、特に高い測定精度が得られることが確認された。すなわち、白色導電材として酸化スズを使用し、表面層中の含有量を質量部で５部から６０部として表面コート条件を振って膜厚を変更し、反射濃度と膜厚との検量線を作成したところ、５重量部の場合、白色導電材が少なく、所望の膜厚２μｍから８μｍの膜厚で計測可能ではあるが、反射濃度の濃いところでの測定になるため測定精度に多少のバラツキが見られることがあった。また、６０部の場合では、２μｍから３μｍの膜厚で、反射濃度と膜厚との検量線が得られたが、３μｍを超える膜厚では、濃度がばらついてしまうことがあった。一方で、２μｍから１０μｍの膜厚で特に精度よく計測可能だったのは、１０〜４０質量部（質量％）の範囲であった。 According to the experiments by the present inventors, it was confirmed that particularly high measurement accuracy can be obtained by setting the above range. That is, tin oxide is used as the white conductive material, the film thickness is changed by changing the surface coating conditions with the content in the surface layer from 5 parts to 60 parts by mass, and a calibration curve between the reflection density and the film thickness is obtained. As a result, in the case of 5 parts by weight, the white conductive material is small and measurement is possible with a desired film thickness of 2 μm to 8 μm. However, since the measurement is performed at a high reflection density, there is some variation in measurement accuracy. It was sometimes seen. In the case of 60 parts, a calibration curve between the reflection density and the film thickness was obtained with a film thickness of 2 μm to 3 μm. However, when the film thickness exceeded 3 μm, the concentration might vary. On the other hand, it was in the range of 10 to 40 parts by mass (% by mass) that the film thickness of 2 to 10 μm could be measured particularly accurately.
白色微粉末または白色導電材の体積平均粒径は、０．０１〜３μｍとすることが好ましく、０．０１〜０．０３とすることが好ましい。０．０１〜３μｍとすることで、均一な分散が出来き、同じ膜厚でも反射濃度が均一になるため、測定の精度が向上するといった利点が得られる。 The volume average particle size of the white fine powder or the white conductive material is preferably 0.01 to 3 μm, and preferably 0.01 to 0.03. By setting the thickness to 0.01 to 3 μm, uniform dispersion can be achieved, and the reflection density becomes uniform even with the same film thickness, so that an advantage of improving measurement accuracy can be obtained.
反射濃度を測定する際に照射する光は、ハロゲンランプから発生されるような白色光を使用することができる。また、市販の光学濃度計（例えば、Ｘ−Ｒｉｔｅ社製のＸ−Ｒｉｔｅ ４０４）を使用して、反射濃度を測定することができる。 White light generated from a halogen lamp can be used as the light to be irradiated when measuring the reflection density. The reflection density can be measured using a commercially available optical densitometer (for example, X-Rite 404 manufactured by X-Rite).
本発明を以下の実施例により具体的に説明するが、本発明はこれに限定されるものではない。 The present invention will be specifically described with reference to the following examples, but the present invention is not limited thereto.
［検量線の作成］
帯電器として、以下のような帯電ロールを作製した。まず、エピクロロヒドリンゴムを金属シャフト（ステンレス製）に被覆しロール状に研磨して、金属シャフトの外周に弾性体層を形成した。
[Create calibration curve]
As a charger, the following charging roll was produced. First, epichlorohydrin rubber was coated on a metal shaft (made of stainless steel) and polished into a roll to form an elastic layer on the outer periphery of the metal shaft.
ナイロン樹脂に白色導電材（酸化スズ：体積平均粒径０．０２μｍ）を２０質量％混合した塗布液を調製した。この塗布液を、膜厚が１．５μｍとなるように弾性体上に、突き上げ法により塗布した。１４０℃、１５分から２０分乾燥させて表面層を形成し、帯電ロールを製造した。 A coating solution was prepared by mixing 20% by mass of a white conductive material (tin oxide: volume average particle size 0.02 μm) with nylon resin. This coating solution was applied on the elastic body by a push-up method so that the film thickness became 1.5 μm. A surface layer was formed by drying at 140 ° C. for 15 to 20 minutes to produce a charging roll.
この帯電ロールの反射濃度をＸ−Ｒｉｔｅ社製の「Ｘ−Ｒｉｔｅ ４０４」（センサ部分の開口は、φ３．４ｍｍ）により測定したところ、１．３であった。また、この帯電ロールの表面層部分を含む一部を切り取り、マイクロスコープにより表面層の厚みを測定したところ、１．５μｍであった。 When the reflection density of this charging roll was measured by “X-Rite 404” (opening of the sensor portion was φ3.4 mm) manufactured by X-Rite, it was 1.3. Further, a part of the charging roll including the surface layer portion was cut out, and the thickness of the surface layer was measured with a microscope.
表面層の膜厚を４μｍ，５μｍ，８μｍとし、それぞれの反射濃度を上記と同じようにして測定したところ、反射濃度と膜厚との間で線形関係が見られ、図１のような検量線が得られた。 When the thickness of the surface layer was set to 4 μm, 5 μm, and 8 μm and the respective reflection densities were measured in the same manner as described above, a linear relationship was found between the reflection density and the film thickness, and a calibration curve as shown in FIG. was gotten.
［実際のラインでの評価］
検量線を作成する際に使用した塗布液を使用し、種々の膜厚（２〜１０μｍの範囲）の表面層を形成し、帯電ロールを作製した。それぞれの帯電ロールの表面層について、上記検量線の作成と同様に反射濃度を測定し、その測定値から膜厚を算出したところ、図１に示すように、当該測定値が検量線上にほぼ正確にのっていることが確認できた。
[Evaluation on actual line]
Using the coating solution used when preparing the calibration curve, surface layers having various film thicknesses (range of 2 to 10 μm) were formed to prepare charging rolls. With respect to the surface layer of each charging roll, the reflection density was measured in the same manner as in the preparation of the calibration curve, and the film thickness was calculated from the measured value. As shown in FIG. I was able to confirm that
以上から、予め、膜厚と反射濃度との関係を示す検量線を作成しておき、その検量線に基づいて、反射濃度を測定することで、非破壊かつ非接触で、容易に膜厚の測定が可能となることが確認できた。これにより、表面層を形成するための工程管理が低コストかつ容易になるいえる。 From the above, a calibration curve showing the relationship between the film thickness and the reflection density is prepared in advance, and the reflection density is measured based on the calibration curve, so that the film thickness can be easily measured in a non-destructive and non-contact manner. It was confirmed that measurement was possible. Thereby, it can be said that the process management for forming the surface layer becomes low-cost and easy.
Claims (1)
白色導電材としての酸化スズ、または、導電材としてのカーボンおよび白色微粉末としてのシリカ、酸化チタン、ＰＴＦＥおよびフッ化炭素からなる群から選択される少なくとも１つ、を前記表面層中に含有し、
前記表面層中の前記白色微粉末または前記白色導電材の含有量が１０〜４０質量％であり、
前記表面層の膜厚が２〜１０μｍであり、
下記の方法により作成した検量線をもとにして、前記表面層に光を照射し、その反射濃度から、前記膜厚を算出することを特徴とする表面層の膜厚測定方法。
−検量線の作成方法−
「白色導電材」または「導電材および白色微粉末」の濃度を一定として表面層を形成するための塗布液を作製し、この塗布液を使用して少なくとも３通りの厚みの表面層を形成し、その後反射濃度計によりそれぞれの反射濃度を測定し、一方で表面層の断面から実際の膜厚を測定し、それぞれの前記反射濃度および前記実際の膜厚から、表面層の膜厚と反射濃度との関係を示す検量線を作成する。 A method of measuring the film thickness of the surface layer of the charger on which the surface layer is formed,
Tin oxide as a white conductive material or a silica as carbon and a fine white powder as the conductive material, at least one selected from the group consisting of titanium oxide, PTFE and fluorocarbon, was contained in the surface layer ,
The content of the white fine powder or the white conductive material in the surface layer is 10 to 40% by mass,
The surface layer has a thickness of 2 to 10 μm,
A method for measuring a film thickness of a surface layer, which comprises irradiating the surface layer with light based on a calibration curve prepared by the following method and calculating the film thickness from the reflection density.
-How to create a calibration curve-
A coating liquid for forming a surface layer is prepared with a constant concentration of “white conductive material” or “conductive material and white fine powder”, and a surface layer having at least three thicknesses is formed using this coating liquid. Then, each reflection density is measured with a reflection densitometer, while the actual film thickness is measured from the cross section of the surface layer, and from the reflection density and the actual film thickness, the film thickness and reflection density of the surface layer are measured. Create a calibration curve showing the relationship between
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