JP7109508B2 - Magnetic tapes, magnetic tape cartridges and magnetic tape devices - Google Patents

Description

The present invention relates to a magnetic tape, a magnetic tape cartridge and a magnetic tape device.

Magnetic recording media include tape-shaped and disk-shaped magnetic recording media, and tape-shaped magnetic recording media, ie, magnetic tapes, are mainly used for storage applications such as data backup.

A magnetic tape is normally housed in a magnetic tape cartridge in a reeled state. Recording and playback of information on a magnetic tape is usually performed by setting a magnetic tape cartridge in a magnetic tape device called a drive, running the magnetic tape inside the magnetic tape device, and connecting the magnetic tape surface (magnetic layer surface) with the magnetic head. It is performed by contacting and sliding. More specifically, recording information on magnetic tape is usually accomplished by recording magnetic signals in the data band of the magnetic tape. A data track is thereby formed in the data band.

2. Description of the Related Art With the enormous increase in the amount of information in recent years, magnetic tapes are required to have a higher recording capacity (higher capacity). As means for increasing the capacity, the width of the data tracks can be narrowed to arrange more data tracks in the width direction of the magnetic tape to increase the recording density.

However, if the width of the data track is narrowed, when the magnetic tape is run in a magnetic tape device (generally called a "drive") and information is recorded and/or reproduced, the positional fluctuation of the magnetic tape causes the magnetic head to move. is difficult to follow the data track accurately, and errors are more likely to occur during recording and/or reproduction. Accordingly, as means for suppressing the occurrence of such errors, in recent years, a system using head tracking servo using a servo signal (hereinafter referred to as a "servo system") has been proposed and put into practical use. (See Patent Document 1, for example).

U.S. Pat. No. 5,689,384

Among servo systems, in a magnetic servo system, a servo pattern (servo signal) is formed on a magnetic layer of a magnetic tape, and the servo pattern is magnetically read to perform head tracking. More details are as follows.
First, the servo head reads the servo pattern formed on the magnetic layer (that is, reproduces the servo signal). The position of the magnetic head within the magnetic tape device is controlled according to the value obtained by reading the servo pattern. As a result, even if the position of the magnetic tape fluctuates when the magnetic tape is transported in the magnetic tape device for recording and/or reproducing information, the accuracy with which the magnetic head follows the data track can be improved. For example, when a magnetic tape is transported in a magnetic tape device to record and/or reproduce information, even if the position of the magnetic tape fluctuates in the width direction with respect to the magnetic head, the servo system can perform head tracking. can control the position of the magnetic head in the width direction of the magnetic tape in the magnetic tape device. Thus, it is possible to accurately record information on the magnetic tape in the magnetic tape device and/or accurately reproduce information recorded on the magnetic tape.

However, in the course of investigations by the present inventors, in a servo system, when head tracking is continued while the magnetic tape is running, the output of the servo signal reproduced by the servo head decreases compared to the initial stage of running (hereinafter referred to as , also referred to as “decrease in servo signal output”). A decrease in the output of the servo signal causes a decrease in accuracy with which the magnetic head follows the data track in the servo system (hereinafter referred to as "head positioning accuracy"). Therefore, in order to more accurately record information on the magnetic tape and/or more accurately reproduce the information recorded on the magnetic tape in the servo system, it is desirable to suppress the output decrease of the servo signal. .

An object of one aspect of the present invention is to provide a magnetic tape in which the output of a servo signal in a servo system is less reduced.

One aspect of the present invention is
A magnetic tape having a magnetic layer comprising a ferromagnetic powder and a binder on a non-magnetic support,
The magnetic layer has a servo pattern,
The absolute value ΔN of the difference between the refractive index Nxy measured in the in-plane direction of the magnetic layer and the refractive index Nz measured in the thickness direction of the magnetic layer (hereinafter also referred to as “ΔN (of the magnetic layer)”). ) is 0.25 or more and 0.40 or less,
Regarding.

In one aspect, the difference (Nxy−Nz) between the refractive index Nxy and the refractive index Nz can be 0.25 or more and 0.40 or less.

In one aspect, the magnetic tape can have a non-magnetic layer containing non-magnetic powder and a binder between the non-magnetic support and the magnetic layer.

In one aspect, the total thickness of the magnetic layer and the non-magnetic layer can be 0.60 μm or less.

In one aspect, the magnetic tape can have a back coat layer containing non-magnetic powder and a binder on the surface of the non-magnetic support opposite to the surface having the magnetic layer.

In one aspect, the servo pattern can be a timing-based servo pattern.

A further aspect of the invention relates to a magnetic tape cartridge containing the above magnetic tape.

A further aspect of the present invention relates to a magnetic tape device including the above magnetic tape and a magnetic head.

According to one aspect of the present invention, it is possible to provide a magnetic tape in which a servo pattern is formed on a magnetic layer and in which a decrease in the output of a servo signal in a servo system is suppressed. Further, according to one aspect of the present invention, it is possible to provide a magnetic tape cartridge and a magnetic tape device containing the above magnetic tape.

An example arrangement of data bands and servo bands is shown. An example of servo pattern arrangement for LTO (Linear-Tape-Open) Ultrium format tape is shown.

[Magnetic tape]
One aspect of the present invention is a magnetic tape having a magnetic layer containing a ferromagnetic powder and a binder on a non-magnetic support, the magnetic layer having a servo pattern, and measuring in the in-plane direction of the magnetic layer. The absolute value ΔN of the difference between the refractive index Nxy measured in the thickness direction of the magnetic layer and the refractive index Nz measured in the thickness direction of the magnetic layer is 0.25 or more and 0.40 or less.
The magnetic tape will be described in more detail below. The following description includes speculations of the inventors. The present invention is not limited by such speculation. Moreover, below, it may demonstrate exemplarily based on drawing. However, the present invention is not limited to the exemplified embodiments.

<Magnetic layer>
(servo pattern)
The magnetic tape has a servo pattern on the magnetic layer. A servo pattern is formed on the magnetic layer by magnetizing a specific position of the magnetic layer with a servo write head. A servo write head is a head that records a servo signal (that is, forms a servo pattern). The shape of the servo pattern and the arrangement on the magnetic layer for enabling head tracking servo are known. A known technique can be applied to the servo pattern of the magnetic layer of the magnetic tape. For example, a timing-based servo method and an amplitude-based servo method are known as head tracking servo methods. The servo pattern that the magnetic layer of the magnetic tape has may be a servo pattern that enables any type of head tracking servo. Also, a servo pattern (that is, a timing-based servo pattern) that enables head tracking servo in the timing-based servo system and a servo pattern that enables head-tracking servo in the amplitude-based servo system are formed on the magnetic layer. good too.

Timing-based servo type head tracking servo will be described below as one specific aspect of the head tracking servo. However, the head tracking servo in the present invention is not limited to the following specific modes.

In the head tracking servo of the timing-based servo method, a plurality of servo patterns of two or more different shapes are formed on the magnetic layer, and the time interval between the two servo patterns of different shapes read by the servo head and the pattern of the same shape. The position of the servo head is recognized based on the time interval between reading the two servo patterns. Based on the position of the servo head thus recognized, the position of the magnetic head in the width direction of the magnetic tape is controlled. In one aspect, the magnetic head whose position is controlled is a magnetic head (reproducing head) that reproduces information recorded on a magnetic tape. ).

FIG. 1 shows an example of arrangement of data bands and servo bands. In FIG. 1, a plurality of servo bands 10 are sandwiched between guide bands 12 on the magnetic layer of the magnetic tape 1 . A plurality of areas 11 sandwiched between two servo bands are data bands. A servo pattern is a magnetized region formed by magnetizing a specific region of a magnetic layer with a servo write head. The area magnetized by the servo write head (the position where the servo pattern is formed) is defined by standards. For example, in the industry standard LTO Ultrium format tape, a plurality of servo patterns inclined with respect to the tape width direction as shown in FIG. 2 are formed on the servo band when the magnetic tape is manufactured. Specifically, in FIG. 2, the servo frame SF on the servo band 10 is composed of a servo subframe 1 (SSF1) and a servo subframe 2 (SSF2). A servo subframe 1 is composed of an A burst (symbol A in FIG. 2) and a B burst (symbol B in FIG. 2). The A burst is composed of servo patterns A1 to A5, and the B burst is composed of servo patterns B1 to B5. On the other hand, servo subframe 2 is composed of a C burst (symbol C in FIG. 2) and a D burst (symbol D in FIG. 2). The C burst is composed of servo patterns C1 to C4, and the D burst is composed of servo patterns D1 to D4. A set of 5 and 4 such 18 servo patterns are arranged in a sub-frame in an arrangement of 5, 5, 4, 4, and are used to identify the servo frame. FIG. 2 shows one servo frame for explanation. Actually, however, in the magnetic layer of the magnetic tape on which head tracking servo of the timing-based servo system is performed, a plurality of servo frames are arranged in the running direction in each servo band. In FIG. 2, arrows indicate the direction of travel. For example, an LTO Ultrium format tape typically has 5000 or more servo frames per meter of tape length in each servo band of the magnetic layer. The servo head sequentially reads servo patterns in a plurality of servo frames while sliding in contact with the surface of the magnetic layer of the magnetic tape conveyed in the magnetic tape device.

In the head tracking servo of the timing-based servo method, the time interval between reading two servo patterns with different shapes (reproducing servo signals) by the servo head and the time interval between reading two servo patterns with the same type of shape Recognize the position of the servo head. The time interval is usually obtained as the time interval between the peaks of the reproduced waveform of the servo signal. For example, in the embodiment shown in FIG. 2, the servo pattern of burst A and the servo pattern of burst C are servo patterns of the same type, and the servo pattern of burst B and the servo pattern of burst D are servo patterns of the same type. . The A-burst servo pattern and the C-burst servo pattern are servo patterns that differ in shape from the B-burst servo pattern and the D-burst servo pattern. The time interval between the two servo patterns having different shapes read by the servo head is, for example, the interval between the time when one of the servo patterns in the A burst is read and the time when one of the servo patterns in the B burst is read. . The time interval at which the servo head reads two servo patterns having the same shape is, for example, the interval between the time when one of the A burst servo patterns is read and the time when one of the C burst servo patterns is read. be. The head tracking servo of the timing-based servo system is based on the premise that, when the time interval deviates from the set value, the deviation of the time interval is caused by positional fluctuation in the width direction of the magnetic tape. The set value is the time interval when the magnetic tape runs in the width direction without positional fluctuation. In the timing-based servo system, the magnetic head is moved in the width direction according to the degree of deviation from the determined time interval set value. Specifically, the larger the deviation from the set value of the time interval, the larger the widthwise movement of the magnetic head. This point applies not only to the embodiments shown in FIGS. 1 and 2 but also to timing-based servo systems in general.

For example, when a magnetic tape is run in a magnetic tape device using a timing-based servo system and a magnetic signal (information) is recorded or reproduced by a magnetic head, the servo pattern is continuously read by the servo head (servo signal is continuously reproduced). A decline in the output of the servo signal over time results in a decline in the measurement accuracy of the time interval. As a result, the head positioning accuracy decreases as the vehicle continues to run. In a magnetic tape apparatus using a servo system, not limited to a timing-based servo system, if the servo signal output decreases while the servo head continues to read the servo pattern, the head positioning accuracy decreases as the tape continues to run.
With respect to the above points, the present inventor believes that the main cause of the decrease in servo signal output is that the servo write head sequentially forms a plurality of servo patterns on the magnetic layer while sliding in contact with the surface of the magnetic layer of the magnetic tape. It is thought that foreign matter adheres to the servo write head over time. It is presumed that the magnetic force of the formed servo pattern gradually decreases as the servo pattern formation continues, as a result of the deterioration of the servo pattern formation capability of the servo write head due to the influence of the adhering foreign matter. In the magnetic layer having the servo patterns formed in this way, it is considered that the output of the servo signal decreases while the servo pattern continues to be read by the servo head (the servo signal continues to be reproduced). A servo head is a head that reproduces a servo signal (that is, reads a servo pattern).
On the other hand, as a result of diligent studies by the present inventors, it has become clear that such a decrease in servo signal output can be suppressed by setting the ΔN of the magnetic layer to 0.25 or more and 0.40 or less. The speculation of the present inventor regarding this point will be described later.

(ΔN of magnetic layer)
In the present invention and this specification, the absolute value ΔN of the difference between the refractive index Nxy measured in the in-plane direction of the magnetic layer and the refractive index Nz measured in the thickness direction of the magnetic layer is determined by the following method. and
The refractive index in each direction of the magnetic layer is obtained by spectroscopic ellipsometry using a two-layer model. In order to determine the refractive index of the magnetic layer by spectroscopic ellipsometry using the two-layer model, the refractive index value of the portion adjacent to the magnetic layer is used. An example of determining the refractive indices Nxy and Nz of the magnetic layer of a magnetic tape having a layer structure in which a nonmagnetic layer and a magnetic layer are laminated in this order on a nonmagnetic support will be described below. However, the magnetic tape according to one aspect of the present invention can also be a magnetic tape having a layer structure in which a magnetic layer is directly laminated on a non-magnetic support without interposing a non-magnetic layer. For a magnetic tape having such a structure, a two-layer model of a magnetic layer and a non-magnetic support is used to determine the refractive index in each direction of the magnetic layer in the same manner as described below. Also, the incident angle described below is the incident angle when the incident angle in the case of vertical incidence is assumed to be 0°.
(1) Preparation of sample for measurement For a magnetic tape having a backcoat layer on the surface opposite to the surface having the magnetic layer of the non-magnetic support, the backcoat layer of the sample for measurement cut out from the magnetic tape is removed. After that, take measurements. The backcoat layer can be removed by a known method such as dissolving the backcoat layer using a solvent. As a solvent, for example, methyl ethyl ketone can be used. However, any solvent may be used as long as it can remove the back coat layer. After removing the backcoat layer, the surface of the non-magnetic support is roughened by a known method so that light reflected from this surface is not detected during measurement with an ellipsometer. The roughening can be carried out, for example, by polishing the surface of the non-magnetic support with sandpaper after removing the back coat layer. For the measurement sample cut out from the magnetic tape having no back coat layer, the surface of the non-magnetic support opposite to the surface having the magnetic layer is roughened.
Further, the magnetic layer is further removed to expose the surface of the nonmagnetic layer for the following refractive index measurement of the nonmagnetic layer. For the following refractive index measurement of the non-magnetic support, the non-magnetic layer is also removed to expose the surface of the non-magnetic support on the magnetic layer side. Each layer can be removed by known methods as described for the removal of the backcoat layer. The longitudinal direction described below refers to the longitudinal direction of the magnetic tape when the sample for measurement was included in the magnetic tape before it was cut out. This point also applies to other directions described below.
(2) Measurement of Refractive Index of Magnetic Layer Using an ellipsometer, incident light with a beam diameter of 300 μm was irradiated onto the surface of the magnetic layer from the longitudinal direction at incident angles of 65°, 70° and 75°. (phase difference between s-polarized and p-polarized light) and Ψ (amplitude ratio between s-polarized and p-polarized light) are measured. The measurement is performed by changing the wavelength of incident light in the range of 400 to 700 nm in increments of 1.5 nm, and the measured value is obtained for each wavelength.
Using the measured values of Δ and Ψ of the magnetic layer at each wavelength, the refractive index of the non-magnetic layer in each direction determined by the method described below, and the thickness of the magnetic layer, the magnetic layer at each wavelength is calculated by the two-layer model as follows: Find the refractive index of
The 0th layer, which is the substrate of the two-layer model, is a non-magnetic layer, and the first layer is a magnetic layer. A two-layer model is created by considering only the reflection at the interface between the air/magnetic layer and the magnetic layer/non-magnetic layer and assuming that the back reflection of the non-magnetic layer has no effect. The refractive index of the first layer that best matches the obtained measured value is obtained by fitting using the least squares method. As values at a wavelength of 600 nm obtained from the fitting results, the refractive index Nx of the magnetic layer in the longitudinal direction and the refractive index Nz ₁ in the thickness direction of the magnetic layer measured by incident light from the longitudinal direction are obtained.
The same as above except that the direction in which the incident light is incident is the width direction of the magnetic tape. A refractive index Nz ₂ in the thickness direction of the magnetic layer measured by incident light is obtained.
Fitting is performed by the following method.
Generally, it is "complex refractive index n=η+iκ". where η is the real part of the refractive index, κ is the extinction coefficient and i is the imaginary number. The complex permittivity ε=ε1+iε2 (ε1 and ε2 satisfy the Kramers-Kronig relationship) and ε1=η ² -κ ² and ε2= _2ηκ . Let the dielectric constant be ε _x =ε _x 1+iε _x 2, and the complex dielectric constant of Nz ₁ be ε _z1 =ε _z1 1+iε _z1 2.
Let ε _x 2 be one Gaussian, take an arbitrary point with a peak position of 5.8 to 5.1 eV and σ of 4 to 3.5 eV as a starting point, and set the dielectric constant outside the measurement wavelength range (400 to 700 nm). Nx is obtained by putting an offset parameter in and performing least-squares fitting of the measured values. Similarly, ε _z1 2 is obtained by starting from an arbitrary point with a peak position of 3.2 to 2.9 eV and σ of 1.5 to 1.2 eV, placing an offset parameter, and performing least-squares fitting of the measured values. Find Nz ₁ . Ny and Nz ₂ are similarly determined. The refractive index Nxy measured in the in-plane direction of the magnetic layer is obtained as "Nxy=(Nx+Ny)/2". The refractive index Nz measured in the thickness direction of the magnetic layer is obtained as "Nz=(Nz ₁ +Nz ₂ )/2". From the obtained Nxy and Nz, the absolute value ΔN of the difference between them is obtained.
(3) Refractive index measurement of non-magnetic layer Except for the following points, the refractive index of the non-magnetic layer at a wavelength of 600 nm (refractive index in the longitudinal direction, refractive index in the width direction, incident light from the longitudinal direction) and the refractive index in the thickness direction measured by making incident light enter from the width direction).
The wavelength of the incident light is changed in increments of 1.5 nm within the range of 250 to 700 nm.
Using a two-layer model of a non-magnetic layer and a non-magnetic support, the 0th layer, which is the substrate of the two-layer model, is the non-magnetic support and the first layer is the non-magnetic layer. A two-layer model is created by considering only the reflection at the interface between the air/non-magnetic layer and the non-magnetic layer/non-magnetic support, and assuming that there is no influence of the back surface reflection of the non-magnetic support.
In fitting, 7 peaks (0.6 eV, 2.3 eV, 2.9 eV, 3.6 eV, 4.6 eV, 5.0 eV, 6.0 eV) are assumed in the imaginary part (ε2) of the complex permittivity Then, a parameter that offsets the dielectric constant is placed outside the measurement wavelength range (250 to 700 nm).
(4) Measurement of refractive index of non-magnetic support The refractive index of the non-magnetic support at a wavelength of 600 nm (refractive index in the longitudinal direction, refractive index in the width direction, refractive index in the width direction, The refractive index in the thickness direction measured with incident light incident from the longitudinal direction, and the refractive index in the thickness direction measured with incident light incident from the width direction) are the refractive indices of the magnetic layers, except for the following points. Determined similarly to the above method for measurement.
Instead of using a two-layer model, a one-layer model with only surface reflection is used.
The fitting is performed by a Cauchy model (n=A+B/λ ² , n is the refractive index, A and B are constants determined by fitting, and λ is the wavelength).

The present inventor speculates as follows about the reason why the magnetic tape described above can suppress the decrease in output of the servo signal.
As described above, as the servo write head contacts and slides on the surface of the magnetic layer of the magnetic tape to sequentially form a plurality of servo patterns on the magnetic layer, foreign matter may adhere to the servo write head. As a result, as the servo pattern continues to be read by the servo head (the servo signal continues to be reproduced), the output of the servo signal decreases.
With respect to the above points, the present inventor believes that ΔN obtained by the above method can be a value that can serve as an indicator of the state of existence of ferromagnetic powder in the surface region of the magnetic layer. This ΔN is presumed to be affected by various factors such as the orientation of the ferromagnetic powder in the magnetic layer, the presence of the binder, and the density distribution of the ferromagnetic powder. A magnetic layer having a ΔN of 0.25 or more and 0.40 or less by controlling various factors is considered to have a high strength on the surface of the magnetic layer and is unlikely to be scraped off even when it slides against the servo write head. As a result, the present inventor speculates that it is possible to suppress the adherence of shavings generated by scraping the surface of the magnetic layer to the servo write head as foreign matter, which contributes to the suppression of the decrease in the output of the servo signal. . However, this is only speculation, and the present invention is not limited to the above speculation.

ΔN of the magnetic layer of the magnetic tape is 0.25 or more and 0.40 or less. From the viewpoint of further suppressing the output decrease of the servo signal, ΔN is preferably 0.25 or more and 0.35 or less. Specific aspects of means for adjusting ΔN will be described later.

ΔN is the absolute value of the difference between Nxy and Nz. Nxy is the refractive index measured in the in-plane direction of the magnetic layer, and Nz is the refractive index measured in the thickness direction of the magnetic layer. In one aspect, Nxy>Nz, and in another aspect, Nxy<Nz. From the viewpoint of the electromagnetic conversion characteristics of the magnetic tape, it is preferable that Nxy>Nz. It is more preferable to be 0.35 or less.

Various means for adjusting ΔN described above will be described later.

(ferromagnetic powder)
Ferromagnetic powders commonly used in the magnetic layers of various magnetic recording media can be used as the ferromagnetic powder contained in the magnetic layer. It is preferable to use ferromagnetic powder having a small average particle size from the viewpoint of improving the recording density of the magnetic recording medium. From this point of view, ferromagnetic powder having an average particle size of 50 nm or less is preferably used as the ferromagnetic powder, and ferromagnetic powder having an average particle size of 40 nm or less is more preferably used. On the other hand, from the viewpoint of magnetization stability, the average particle size of the ferromagnetic powder is preferably 5 nm or more, more preferably 10 nm or more, and even more preferably 15 nm or more.

A preferred specific example of the ferromagnetic powder is hexagonal ferrite powder. For details of the hexagonal ferrite powder, for example, paragraphs 0012 to 0030 of JP-A-2011-225417, paragraphs 0134-0136 of JP-A-2011-216149, paragraphs 0013-0030 of JP-A-2012-204726 and Paragraphs 0029 to 0084 of JP-A-2015-127985 can be referred to.

A preferred specific example of the ferromagnetic powder is metal powder. For details of the metal powder, for example, paragraphs 0137 to 0141 of JP-A-2011-216149 and paragraphs 0009-0023 of JP-A-2005-251351 can be referred to.

A preferred specific example of the ferromagnetic powder is ε-iron oxide powder. As a method for producing ε-iron oxide powder, a method of producing from goethite, a reverse micelle method, and the like are known. All of the above manufacturing methods are known. Also, a method for producing ε-iron oxide powder in which a part of Fe is substituted with substitution atoms such as Ga, Co, Ti, Al, and Rh is described in J. Am. Jpn. Soc. Powder Metallurgy Vol. 61 Supplement, No. S1, pp. S280-S284, J.P. Mater. Chem. C, 2013, 1, pp. 5200-5206 and the like. However, the method for producing the ε-iron oxide powder that can be used as the ferromagnetic powder in the magnetic layer is not limited.

In the present invention and this specification, unless otherwise specified, the average particle size of various powders such as ferromagnetic powder is a value measured by the following method using a transmission electron microscope.
The powder is photographed with a transmission electron microscope at a magnification of 100,000 times and printed on photographic paper at a total magnification of 500,000 times to obtain a photograph of the particles constituting the powder. The particles of interest are selected from the photograph of the particles obtained, and the contours of the particles are traced with a digitizer to measure the size of the particles (primary particles). Primary particles refer to individual particles without agglomeration.
The above measurements are performed on 500 randomly selected particles. The arithmetic mean of the particle sizes of the 500 particles thus obtained is taken as the average particle size of the powder. As the transmission electron microscope, for example, Hitachi's H-9000 transmission electron microscope can be used. Further, the particle size can be measured using known image analysis software such as Carl Zeiss image analysis software KS-400. Unless otherwise specified, the values related to the size of the powder such as the average particle size shown in the examples below are obtained using a Hitachi transmission electron microscope H-9000 as a transmission electron microscope, and Carl Zeiss image analysis software KS- as image analysis software. 400 is the value measured.

As a method for collecting a sample powder from a magnetic recording medium for particle size measurement, for example, the method described in paragraph 0015 of JP-A-2011-048878 can be employed.

In the present invention and this specification, unless otherwise specified, the size of the particles constituting the powder (particle size) is the shape of the particles observed in the above particle photographs.
(1) In the case of needle-like, spindle-like, columnar (however, the height is greater than the maximum major diameter of the bottom surface), etc., the length of the major axis constituting the particle, that is, the major axis length,
(2) In the case of a plate-like or columnar shape (where the thickness or height is smaller than the maximum major diameter of the plate surface or bottom surface), it is expressed by the maximum major diameter of the plate surface or bottom surface,
(3) If the shape is spherical, polyhedral, unspecified, etc., and if the major axis of the particle cannot be specified from the shape, it is represented by the equivalent circle diameter. The equivalent circle diameter is obtained by the circular projection method.

In addition, the average acicular ratio of the powder is obtained by measuring the length of the minor axis of the particles in the above measurement, that is, the minor axis length, and obtaining the value of (long axis length / minor axis length) of each particle. It refers to the arithmetic mean of the values obtained for the particles. Here, unless otherwise specified, the minor axis length is the length of the minor axis constituting the particle in the case of (1) in the definition of the particle size, and the thickness or height in the case of (2). In the case of (3), since there is no distinction between the major axis and the minor axis, (long axis length/short axis length) is regarded as 1 for convenience.
Unless otherwise specified, when the particle shape is specific, for example, in the case of the definition (1) of the particle size, the average particle size is the average major axis length, and in the case of the definition (2), the average particle size is Average plate diameter. In the case of the same definition (3), the average particle size is the average diameter (also referred to as average particle size or average particle size).

In one aspect, the ferromagnetic particles constituting the ferromagnetic powder contained in the magnetic layer can have a plate-like shape. Ferromagnetic powder composed of plate-like ferromagnetic particles is hereinafter referred to as plate-like ferromagnetic powder. The average platelet ratio of the platelet-like ferromagnetic powder can preferably range from 2.5 to 5.0. The average tabular ratio is the arithmetic mean of (maximum length/thickness or height) in the definition (2) above. As the average tabular ratio increases, the orientation treatment tends to increase the uniformity of the orientation state of the ferromagnetic particles constituting the tabular ferromagnetic powder, and the value of ΔN tends to increase.

Also, the activation volume can be used as an index of the particle size of the ferromagnetic powder. An "activation volume" is a unit of magnetization reversal. The activation volume described in the present invention and this specification is measured using a vibrating sample magnetometer at a magnetic field sweep speed of 3 minutes and 30 minutes at the coercive force Hc measurement part in an environment of an ambient temperature of 23 ° C. ± 1 ° C. , and is a value obtained from the following relational expression between Hc and activation volume V. The activation volume shown in the examples below is a value obtained by performing measurement using a vibrating sample magnetometer manufactured by Toei Kogyo Co., Ltd.
Hc=2Ku/Ms{1−[(kT/KuV)ln(At/0.693)] ^1/2 }
[In the above formula, Ku: anisotropy constant, Ms: saturation magnetization, k: Boltzmann constant, T: absolute temperature, V: activation volume, A: spin precession frequency, t: magnetic field reversal time]
From the viewpoint of improving the recording density, the activated volume of the ferromagnetic powder is preferably 2500 nm ³ or less, more preferably 2300 nm ³ or less, and even more preferably 2000 nm ³ or less. On the other hand, from the viewpoint of magnetization stability, the activated volume of the ferromagnetic powder is preferably, for example, 800 nm ³ or more, more preferably 1000 nm ³ or more, and even more preferably 1200 nm ³ or more.

The ferromagnetic powder content (filling rate) in the magnetic layer is preferably in the range of 50 to 90 mass %, more preferably in the range of 60 to 90 mass %. A component of the magnetic layer other than the ferromagnetic powder is at least a binder and may optionally include one or more additional additives. A high filling rate of the ferromagnetic powder in the magnetic layer is preferable from the viewpoint of improving the recording density.

(binder, curing agent)
The magnetic tape is a coated magnetic tape, and contains a binder in the magnetic layer. A binder is one or more resins. Resins may be homopolymers or copolymers. Binders contained in the magnetic layer include polyurethane resins, polyester resins, polyamide resins, vinyl chloride resins, acrylic resins obtained by copolymerizing styrene, acrylonitrile, methyl methacrylate, etc., cellulose resins such as nitrocellulose, epoxy resins, phenoxy resins, A resin selected from polyvinyl acetal, polyvinyl butyral, and other polyvinyl alkylal resins can be used alone, or a plurality of resins can be mixed and used. Preferred among these are polyurethane resins, acrylic resins, cellulose resins and vinyl chloride resins. These resins can also be used as binders in the non-magnetic layer and/or backcoat layer, which will be described later. Paragraphs 0029 to 0031 of JP-A-2010-24113 can be referred to for the above binders. The binder may also be a radiation-curable resin such as an electron beam-curable resin. Regarding the radiation curable resin, paragraphs 0044 to 0045 of JP-A-2011-048878 can be referred to.
The weight-average molecular weight of the resin used as the binder can be, for example, 10,000 or more and 200,000 or less. The weight average molecular weight in the present invention and the specification is a value obtained by converting a value measured by gel permeation chromatography (GPC) into polystyrene. The following conditions can be mentioned as measurement conditions. The weight average molecular weight shown in the examples below is a value obtained by converting the value measured under the following measurement conditions into polystyrene.
GPC device: HLC-8120 (manufactured by Tosoh Corporation)
Column: TSK gel Multipore HXL-M (manufactured by Tosoh Corporation, 7.8 mmID (Inner Diameter) × 30.0 cm)
Eluent: Tetrahydrofuran (THF)

In one aspect, a binder containing an acidic group can be used as the binder. The term "acidic group" as used in the present invention and the specification includes a group capable of dissociating into an anion by releasing H ⁺ in water or a solvent containing water (aqueous solvent) and a salt form thereof. . Specific examples of the acidic group include, for example, a sulfonic acid group, a sulfate group, a carboxyl group, a phosphoric acid group, and salt forms thereof. For example, the salt form of a sulfonic acid group (--SO ₃ H) means a group represented by --SO ₃ M, where M represents an atom capable of becoming a cation in water or an aqueous solvent (such as an alkali metal atom). means. This point also applies to the salt forms of the various groups described above. Examples of binders containing acidic groups include resins containing at least one acid group selected from the group consisting of sulfonic acid groups and salts thereof (eg, polyurethane resins, vinyl chloride resins, etc.). However, the resin contained in the magnetic layer is not limited to these resins. Also, in the binder containing acidic groups, the acidic group content can be, for example, in the range of 20 to 500 eq/ton. Note that eq is equivalent and is a unit that cannot be converted into SI units. The content of various functional groups such as acidic groups contained in the resin can be determined by a known method according to the type of functional group. The value of ΔN tends to increase with the use of a binder with a higher acid group content. The binder can be used in the magnetic layer-forming composition in an amount of, for example, 1.0 to 30.0 parts by mass, preferably 1.0 to 30.0 parts by mass, per 100.0 parts by mass of the ferromagnetic powder. An amount of 20.0 parts by weight can be used. The value of ΔN tends to increase as the amount of binder used relative to the ferromagnetic powder increases.

Curing agents can also be used with resins that can be used as binders. The curing agent can be, in one aspect, a thermosetting compound which is a compound in which a curing reaction (crosslinking reaction) proceeds by heating, and in another aspect, a photocuring compound in which a curing reaction (crosslinking reaction) proceeds by light irradiation. can be a chemical compound. The curing agent can be contained in the magnetic layer in a state where at least a portion of it reacts (crosslinks) with other components such as a binder as the curing reaction progresses during the process of forming the magnetic layer. In this respect, when the composition used for forming other layers contains a curing agent, the same applies to layers formed using this composition. Preferred curing agents are thermosetting compounds, preferably polyisocyanates. For details of the polyisocyanate, paragraphs 0124 to 0125 of JP-A-2011-216149 can be referred to. The curing agent is contained in the composition for forming the magnetic layer in an amount of, for example, 0 to 80.0 parts by weight per 100.0 parts by weight of the binder, and preferably 50.0 to 80.0 parts by weight from the viewpoint of improving the strength of the magnetic layer. Parts by weight amounts can be used.

(Additive)
The magnetic layer contains ferromagnetic powder and a binder, and optionally one or more additives. Examples of additives include the curing agents described above. Additives that can be contained in the magnetic layer include nonmagnetic powders, lubricants, dispersants, dispersing aids, antifungal agents, antistatic agents, antioxidants, carbon black, and the like. Commercially available additives can be appropriately selected and used according to desired properties. For example, regarding lubricants, paragraphs 0030 to 0033, 0035 and 0036 of JP-A-2016-126817 can be referred to. The non-magnetic layer may contain a lubricant. Paragraphs 0030, 0031, 0034, 0035 and 0036 of JP-A-2016-126817 can be referred to for lubricants that can be contained in the non-magnetic layer. Regarding the dispersant, paragraphs 0061 and 0071 of JP-A-2012-133837 can be referred to. A dispersant may be contained in the non-magnetic layer. For the dispersant that can be contained in the non-magnetic layer, see paragraph 0061 of JP-A-2012-133837.

The magnetic layer preferably contains one or more non-magnetic powders. Examples of non-magnetic powders include non-magnetic powders (hereinafter referred to as "protrusion-forming agents") that can function as protrusion-forming agents that form moderately protruding protrusions on the surface of the magnetic layer. The protrusion-forming agent is a component that can contribute to controlling the frictional properties of the magnetic layer surface of the magnetic tape. The magnetic layer may also contain a non-magnetic powder that can function as an abrasive (hereinafter referred to as "abrasive"). The magnetic layer of the magnetic tape preferably contains at least one of a projection-forming agent and an abrasive, more preferably both.

As the protrusion-forming agent, various non-magnetic powders generally used as protrusion-forming agents can be used. These may be powders of inorganic substances or powders of organic substances. In one aspect, the particle size distribution of the projection-forming agent is preferably monodisperse with a single peak, rather than polydisperse with multiple peaks, from the viewpoint of uniforming frictional properties. From the standpoint of availability of monodisperse particles, the non-magnetic powder contained in the magnetic layer is preferably inorganic powder (inorganic powder). Examples of the inorganic powder include powders of inorganic oxides such as metal oxides, metal carbonates, metal sulfates, metal nitrides, metal carbides, and metal sulfides. is preferred. The projection-forming agent is more preferably colloidal particles, more preferably inorganic oxide colloidal particles. From the standpoint of availability of monodisperse particles, the inorganic oxide colloidal particles are more preferably colloidal silica (silica colloidal particles). In the present invention and the specification, the term "colloidal particles" means at least methyl ethyl ketone, cyclohexanone, toluene or ethyl acetate, or at least one mixed solvent containing two or more of the above solvents at an arbitrary mixing ratio per 100 mL of organic solvent. It refers to particles which, when added to 1 g, are capable of dispersing rather than settling to provide a colloidal dispersion. For colloidal particles, the average particle size is the value determined by the method described as a method for measuring the average particle size in paragraph 0015 of JP-A-2011-048878. In another aspect, the projection-forming agent is also preferably carbon black.

The average particle size of the projection-forming agent is, for example, 30-300 nm, preferably 40-200 nm.

On the other hand, the abrasive is preferably a non-magnetic powder with a Mohs hardness of over 8, more preferably a non-magnetic powder with a Mohs hardness of 9 or more. The maximum Mohs hardness is 10 for diamond. Specifically, alumina ( _Al2O3 ) _, silicon carbide, boron carbide ₍ B4C), _SiO2 , TiC, chromium oxide ( _Cr2O3 ) _, cerium oxide, zirconium oxide ₍ ZrO2), iron oxide , diamond, etc. Among them, alumina powder such as α-alumina and silicon carbide powder are preferable. Regarding the particle size of the abrasive, the specific surface area, which is an index of the particle size, is, for example, 14 m ² /g or more, preferably 16 m ² /g or more, more preferably 18 m ² /g or more. Also, the specific surface area of the abrasive can be, for example, 40 m ² /g or less. The specific surface area is a value determined by a nitrogen adsorption method (also called a BET (Brunauer-Emmett-Teller) one-point method). In the following, the specific surface area determined by such a method is also referred to as the BET specific surface area.

Also, from the viewpoint that the projection-forming agent and the abrasive can better exhibit their respective functions, the content of the projection-forming agent in the magnetic layer is preferably set to: It is 1.0 to 4.0 parts by mass, more preferably 1.5 to 3.5 parts by mass. On the other hand, the abrasive content in the magnetic layer is preferably 1.0 to 20.0 parts by mass, more preferably 3.0 to 15.0 parts by mass, per 100.0 parts by mass of the ferromagnetic powder. parts, more preferably 4.0 to 10.0 parts by mass.

Examples of additives that can be used in a magnetic layer containing an abrasive include dispersants described in paragraphs 0012 to 0022 of JP-A-2013-131285, which improve the dispersibility of the abrasive in the composition for forming the magnetic layer. It can be mentioned as a dispersing agent for

<Nonmagnetic layer>
Next, the nonmagnetic layer will be explained. The above magnetic tape may have a magnetic layer directly on a non-magnetic support, or may have a non-magnetic layer containing non-magnetic powder and a binder between the non-magnetic support and the magnetic layer. good. The non-magnetic powder used in the non-magnetic layer may be inorganic powder or organic powder. Carbon black or the like can also be used. Examples of inorganic substances include metals, metal oxides, metal carbonates, metal sulfates, metal nitrides, metal carbides, and metal sulfides. These non-magnetic powders are commercially available and can be produced by known methods. For details, paragraphs 0146 to 0150 of Japanese Patent Application Laid-Open No. 2011-216149 can be referred to. For carbon black that can be used in the non-magnetic layer, see paragraphs 0040 to 0041 of JP-A-2010-24113. The content (filling rate) of the non-magnetic powder in the non-magnetic layer is preferably in the range of 50 to 90 mass %, more preferably in the range of 60 to 90 mass %.

Other details such as binders and additives for the non-magnetic layer can be applied to known techniques for non-magnetic layers. In addition, for example, the type and content of the binder, the type and content of the additive, and the like can be applied to known techniques related to magnetic layers.

The non-magnetic layer of the magnetic tape is intended to include non-magnetic powder as well as a substantially non-magnetic layer containing a small amount of ferromagnetic powder, for example as an impurity or intentionally. Here, the substantially non-magnetic layer means that the residual magnetic flux density of this layer is 10 mT or less, the coercive force is 7.96 kA/m (100 Oe) or less, or the residual magnetic flux density is 10 mT or less. and a coercive force of 7.96 kA/m (100 Oe) or less. The non-magnetic layer preferably has no residual magnetic flux density and no coercive force.

<Nonmagnetic support>
Next, the non-magnetic support will be described. As the non-magnetic support (hereinafter also simply referred to as "support"), biaxially stretched polyethylene terephthalate, polyethylene naphthalate, polyamide, polyamide-imide, aromatic polyamide and the like are known. Among these, polyethylene terephthalate, polyethylene naphthalate and polyamide are preferred. These supports may be previously subjected to corona discharge, plasma treatment, easy adhesion treatment, heat treatment, or the like.

<Back coat layer>
The magnetic tape can also have a back coat layer containing non-magnetic powder and a binder on the surface of the non-magnetic support opposite to the surface having the magnetic layer. The backcoat layer preferably contains one or both of carbon black and inorganic powder. The binder contained in the backcoat layer and the various additives that can be optionally contained can be applied to the known techniques relating to the backcoat layer, and the known techniques relating to the formulation of the magnetic layer and/or the non-magnetic layer can be applied. can also For example, paragraphs 0018 to 0020 of JP-A-2006-331625 and US Pat. .

<Various thicknesses>
In order to increase the recording capacity per roll of the magnetic tape cartridge, it is desirable to lengthen the total length of the magnetic tape that can be accommodated in one roll of the magnetic tape cartridge. For that purpose, it is required to make the magnetic tape thinner (hereinafter referred to as "thinning"). As one means for reducing the thickness of a magnetic tape, for a magnetic tape having a nonmagnetic layer and a magnetic layer in this order on a nonmagnetic support, the total thickness of the nonmagnetic layer and the magnetic layer should be reduced. is mentioned. When the magnetic tape has a non-magnetic layer between the non-magnetic support and the magnetic layer, the total thickness of the non-magnetic layer and the magnetic layer should be 0.60 μm or less from the viewpoint of thinning the magnetic tape. is preferable, and 0.50 μm or less is more preferable. Also, the total thickness of the nonmagnetic layer and the magnetic layer can be, for example, 0.10 μm or more, or 0.20 μm or more. According to the study of the present inventor, it was found that a magnetic tape having a thin total thickness of the non-magnetic layer and the magnetic layer tends to cause a decrease in the output of the servo signal. On the other hand, in a magnetic tape having a thin total thickness of the non-magnetic layer and the magnetic layer, by setting the ΔN of the magnetic layer to 0.25 or more and 0.40 or less, it is possible to suppress the decrease in the output of the servo signal.
The thickness of the nonmagnetic support of the magnetic tape is preferably 3.00 to 4.50 μm.
The thickness of the magnetic layer can be optimized according to the saturation magnetization amount of the magnetic head to be used, the head gap length, the recording signal band, and the like. The thickness of the magnetic layer is generally 0.01 μm to 0.15 μm, preferably 0.02 μm to 0.12 μm, more preferably 0.03 μm to 0.10 μm from the viewpoint of high-density recording. . At least one magnetic layer is required, and the magnetic layer may be separated into two or more layers having different magnetic properties, and a configuration relating to a known multi-layered magnetic layer can be applied. The thickness of the magnetic layer when separated into two or more layers is the total thickness of these layers.
The thickness of the nonmagnetic layer is, for example, 0.10 to 0.55 μm, preferably 0.10 to 0.50 μm.
The thickness of the backcoat layer is preferably 0.90 μm or less, more preferably in the range of 0.10 to 0.70 μm.
The total thickness of the magnetic tape is preferably 6.00 μm or less, more preferably 5.70 μm or less, and more preferably 5.50 μm or less from the viewpoint of improving the recording capacity per roll of the magnetic tape cartridge. is more preferred. On the other hand, the total thickness of the magnetic tape is preferably 1.00 μm or more from the viewpoint of ease of handling (handling property) of the magnetic tape.

The thickness of each layer and the non-magnetic support can be determined by exposing a section in the thickness direction of the magnetic tape by a known technique such as an ion beam or a microtome, and then examining the exposed section with a scanning transmission electron microscope (STEM). ) shall be obtained by observing the cross section. For a specific example of the method for measuring the thickness, it is possible to refer to the description of the method for measuring the thickness in Examples described later.

<Manufacturing process>
(Preparation of each layer-forming composition)
The process of preparing a composition for forming a magnetic layer, a non-magnetic layer or a backcoat layer usually includes at least a kneading process, a dispersing process, and a mixing process provided before or after these processes as required. Each step may be divided into two or more stages. The components used for preparing each layer-forming composition may be added at the beginning or in the middle of any step. As the solvent, one or more of various solvents commonly used in the production of coating type magnetic recording media can be used. Regarding the solvent, for example, paragraph 0153 of JP-A-2011-216149 can be referred to. Alternatively, individual components may be added in two or more steps. For example, the binder may be dividedly added in the kneading step, the dispersing step, and the mixing step for viscosity adjustment after dispersion. Conventionally known manufacturing techniques can be used in various steps to manufacture the magnetic tape. In the kneading step, it is preferable to use a kneader having a strong kneading force such as an open kneader, a continuous kneader, a pressure kneader or an extruder. For details of these kneading processes, reference can be made to Japanese Patent Application Laid-Open Nos. 1-106338 and 1-79274. A known disperser can be used. Alternatively, the ferromagnetic powder and the abrasive can be dispersed separately. More specifically, separate dispersion is a step of mixing an abrasive liquid containing an abrasive and a solvent (but substantially free of ferromagnetic powder) with a magnetic liquid containing ferromagnetic powder, a solvent and a binder. This is a method of preparing a composition for forming a magnetic layer through The above-mentioned "substantially free of ferromagnetic powder" means that no ferromagnetic powder is added as a constituent of the abrasive liquid, and a trace amount of ferromagnetic powder is unintentionally mixed as an impurity. shall be allowed to exist. Regarding ΔN, there is a tendency that the longer the dispersion time of the magnetic liquid, the larger the value of ΔN. This is because the longer the dispersion time of the magnetic liquid, the higher the dispersibility of the ferromagnetic powder in the coating layer of the composition for forming the magnetic layer, and the uniformity of the orientation state of the ferromagnetic particles constituting the ferromagnetic powder by the orientation treatment. This is thought to be because there is a tendency for the Also, the value of ΔN tends to increase as the dispersion time for mixing and dispersing the various components of the composition for forming a non-magnetic layer increases. The dispersion time of the magnetic liquid and the dispersion time of the composition for forming the non-magnetic layer may be set so as to achieve a ΔN of 0.25 or more and 0.40 or less.
Filtration may be performed by a known method at any stage of preparing each layer-forming composition. Filtration can be performed, for example, by filter filtration. As a filter used for filtration, for example, a filter having a pore size of 0.01 to 3 μm (eg, glass fiber filter, polypropylene filter, etc.) can be used.

(Coating process)
The magnetic layer can be formed, for example, by directly coating the magnetic layer-forming composition on the non-magnetic support, or by sequentially or simultaneously coating the magnetic layer-forming composition with the non-magnetic layer-forming composition. The backcoat layer can be formed by coating a composition for forming a backcoat layer on the opposite side of the non-magnetic support from the side having the magnetic layer (or the side on which the magnetic layer is to be provided later). Also, the coating process for forming each layer can be divided into two or more steps. For example, in one aspect, the composition for forming the magnetic layer can be applied in two or more steps. In this case, the drying treatment may or may not be performed between the two stages of the coating process. Also, the orientation treatment may or may not be performed between the two stages of the coating process. For details of coating for forming each layer, paragraph 0066 of JP-A-2010-231843 can also be referred to. In addition, a known technique can be applied to the drying process after applying each layer-forming composition. As for the composition for forming the magnetic layer, a coating layer formed by applying the composition for forming the magnetic layer (hereinafter also referred to as "coating layer of the composition for forming the magnetic layer" or simply "coating layer"). The value of ΔN tends to increase as the drying temperature decreases. The drying temperature can be, for example, the ambient temperature at which the drying process is performed, and may be set so as to achieve a ΔN of 0.25 or more and 0.40 or less.

(Other processes)
For various other steps for manufacturing the magnetic tape, paragraphs 0067 to 0070 of JP-A-2010-231843 can be referred to.
For example, the coating layer of the composition for forming the magnetic layer is preferably subjected to orientation treatment while the coating layer is in a wet state. From the viewpoint of the ease of achieving a ΔN of 0.25 or more and 0.40 or less, the orientation treatment involves arranging a magnet so that a magnetic field is applied perpendicularly to the surface of the coating layer of the composition for forming the magnetic layer. It is preferable to carry out by (that is, vertical alignment treatment). The strength of the magnetic field during the orientation treatment may be set so as to achieve a ΔN of 0.25 or more and 0.40 or less. When the magnetic layer-forming composition is coated in two or more steps, it is preferable to perform the orientation treatment at least after the final coating step, and more preferably to perform the vertical orientation treatment. For example, when a magnetic layer is formed by a two-step coating process, after the first coating process, a drying process is performed without performing an orientation treatment, and then the coating layer formed in the second coating process is orientation treatment can be applied. Various known techniques including those described in paragraph 0052 of JP-A-2010-24113 can be applied to the alignment treatment. For example, the vertical alignment treatment can be performed by a known method such as a method using opposed magnets with different polarities. In the orientation zone, the drying speed of the coating layer can be controlled by the temperature and air volume of the drying air and/or the conveying speed of the magnetic tape in the orientation zone. Also, the coated layer may be pre-dried before being conveyed to the orientation zone.
Further, calendering can be performed at any stage after drying the coated layer of the composition for forming the magnetic layer. For conditions of calendar processing, for example, paragraph 0026 of Japanese Patent Application Laid-Open No. 2010-231843 can be referred to. The value of ΔN tends to increase as the calender temperature (the surface temperature of the calender rolls) increases. The calendar temperature may be set so as to achieve a ΔN of 0.25 or more and 0.40 or less.

(Formation of servo pattern)
The magnetic tape has a servo pattern on the magnetic layer. The details of the servo patterns are as described above. For example, FIG. 1 shows an arrangement example of a region (servo band) in which a timing base servo pattern is formed and a region (data band) sandwiched between two servo bands. An example placement of a timing-based servo pattern is shown in FIG. However, the arrangement shown in each drawing is an example, and the servo patterns, servo bands, and data bands may be arranged according to the system of the magnetic tape device (drive). Also, the shape and arrangement of the timing base servo pattern are described in, for example, US Pat. No. 5,689,384, FIG. 4, FIG. 5, FIG. 6, FIG. 9, FIG. 17, FIG. 20 or the like can be applied.

A servo pattern can be formed by magnetizing specific regions of a magnetic layer with a servo write head mounted on a servo writer. The area magnetized by the servo write head (the position where the servo pattern is formed) is defined by standards. As the servo writer, a commercially available servo writer or a known servo writer can be used. For the configuration of the servo writer, for example, known techniques such as those described in Japanese Patent Application Laid-Open No. 2011-175687, US Pat. No. 5,689,384, US Pat.

As described above, the magnetic tape according to one aspect of the present invention can be obtained. A magnetic tape is usually housed in a magnetic tape cartridge, and the magnetic tape cartridge is loaded into a magnetic tape device.

[Magnetic tape cartridge]
One aspect of the present invention relates to a magnetic tape cartridge including the above magnetic tape.

A magnetic tape cartridge generally contains a magnetic tape wound on a reel inside a cartridge body. The reel is rotatably provided inside the cartridge body. As magnetic tape cartridges, a single reel type magnetic tape cartridge having one reel inside the cartridge body and a dual reel type magnetic tape cartridge having two reels inside the cartridge body are widely used. When a single-reel magnetic tape cartridge is loaded into a magnetic tape device (drive) for recording and/or reproducing information (magnetic signals) on the magnetic tape, the magnetic tape is pulled out from the magnetic tape cartridge and driven into the drive. It is wound on the reel on the side. A magnetic head is arranged in the magnetic tape transport path from the magnetic tape cartridge to the take-up reel. The magnetic tape is fed out and taken up between the magnetic tape cartridge side reel (supply reel) and the drive side reel (take-up reel). During this time, information is recorded and/or reproduced by contact and sliding between the magnetic head and the surface of the magnetic layer of the magnetic tape. On the other hand, a twin-reel magnetic tape cartridge has both a supply reel and a take-up reel inside the magnetic tape cartridge. The magnetic tape cartridge may be either a single-reel type magnetic tape cartridge or a twin-reel type magnetic tape cartridge. The magnetic tape cartridge may include the magnetic tape according to one aspect of the present invention, and other known techniques can be applied.

[Magnetic tape device]
One aspect of the present invention relates to a magnetic tape device including the above magnetic tape and a magnetic head.

In the present invention and in this specification, the term "magnetic tape device" means a device capable of at least one of recording information on a magnetic tape and reproducing information recorded on the magnetic tape. Such devices are commonly called drives. The magnetic tape device may be a sliding type magnetic tape device. A sliding type device refers to a device in which the surface of the magnetic layer and the magnetic head are brought into contact with each other and slide when recording information on the magnetic tape and/or reproducing the recorded information.

The magnetic head included in the magnetic tape device can be a recording head capable of recording information on the magnetic tape, and a reproducing head capable of reproducing information recorded on the magnetic tape. can also In one aspect, the magnetic tape device can include both a recording head and a reproducing head as separate magnetic heads. In another aspect, the magnetic head included in the magnetic tape may have a configuration in which both the recording element and the reproducing element are provided in one magnetic head. As a reproducing head, a magnetic head (MR head) including a magnetoresistive (MR) element as a reproducing element capable of reading information recorded on a magnetic tape with high sensitivity is preferable. Various known MR heads can be used as the MR head. A magnetic head for recording and/or reproducing information may also include a servo pattern reading element. Alternatively, the magnetic tape device may include a magnetic head (servo head) having a servo pattern reading element as a separate head from the magnetic head for recording and/or reproducing information.

The details of the magnetic tape mounted on the magnetic tape device are as described above. Such magnetic tapes have servo patterns. Therefore, when a magnetic signal is recorded on the data band by the magnetic head to form a data track and/or the recorded signal is reproduced, the servo pattern is read by the servo head while the servo pattern is read by the servo head. Tracking allows the magnetic head to follow the data tracks with high accuracy.

For details of the head tracking servo of the timing-based servo method, known techniques such as those described in US Pat. No. 5,689,384, US Pat. No. 6,542,325, and US Pat. Further, for the details of the head tracking servo of the amplitude-based servo method, known techniques such as US Pat. No. 5,426,543 and US Pat. No. 5,898,533 can be applied.

A commercially available magnetic tape device is usually equipped with a magnetic head according to the standard. In addition, commercially available magnetic tape devices are usually equipped with a servo control mechanism for enabling head tracking in a standardized servo system. A magnetic tape device according to one aspect of the present invention can be configured by, for example, incorporating the magnetic tape according to one aspect of the present invention into a commercially available magnetic tape device.

The present invention will be described below based on examples. However, the present invention is not limited to the embodiments shown in the examples. "Parts" and "%" described below indicate "mass parts" and "mass%" unless otherwise specified. In addition, the processes and evaluations described below were performed in an environment with an ambient temperature of 23° C.±1° C. unless otherwise specified.

1. Preparation of magnetic tape [Example 1]
<Preparation of abrasive liquid>
3.0 parts of 2,3-dihydroxynaphthalene (manufactured by Tokyo Kasei Co., Ltd.) is added to 100.0 parts of alumina powder (HIT-80 manufactured by Sumitomo Chemical Co., Ltd.) having a gelatinization rate of about 65% and a BET specific surface area of 20 m ² /g. 31.3 parts of a 32% solution (solvent is a mixed solvent of methyl ethyl ketone and toluene) of SO ₃ Na group-containing polyester polyurethane resin (UR-4800 (SO ₃ Na group: 0.08 meq/g) manufactured by Toyobo Co., Ltd.); 570.0 parts of a mixed solvent of methyl ethyl ketone and cyclohexanone (1:1 (mass ratio)) was mixed as a solvent, and dispersed for 5 hours with a paint shaker in the presence of zirconia beads. After dispersion, the dispersion liquid and the beads were separated by a mesh to obtain an alumina dispersion.

<Preparation of Composition for Forming Magnetic Layer>
(Magnetic liquid)
Plate-shaped ferromagnetic hexagonal barium ferrite powder 100.0 parts (activation volume: 1600 nm ³ , average plate ratio: 3.5)
SO ₃ Na group-containing polyurethane resin See Table 1 Weight average molecular weight: 70,000 SO ₃ Na group content: See Table 1 Cyclohexanone 150.0 parts Methyl ethyl ketone 150.0 parts (abrasive liquid)
6.0 parts of alumina dispersion prepared above (silica sol (protrusion forming agent liquid))
Colloidal silica (average particle size: 100 nm) 2.0 parts Methyl ethyl ketone 1.4 parts (other components)
Stearic acid 2.0 parts Butyl stearate 2.0 parts Polyisocyanate (Coronate (registered trademark) manufactured by Tosoh Corporation) 2.5 parts (finishing additive solvent)
Cyclohexanone 200.0 parts Methyl ethyl ketone 200.0 parts

(Preparation method)
The magnetic liquid was prepared by dispersing the various components of the above magnetic liquid in a batch-type vertical sand mill using beads as a dispersing medium. Zirconia beads (bead diameter: see Table 1) were used as the beads, and the beads were dispersed for the time shown in Table 1 (magnetic fluid bead dispersion time).
The magnetic liquid thus obtained, the above-mentioned abrasive liquid, silica sol, other components, and finishing additive solvent are mixed and dispersed in beads for 5 minutes, and then treated with a batch type ultrasonic device (20 kHz, 300 W) for 0.5 minutes (ultrasonic dispersion) was performed. Thereafter, filtration was performed using a filter having a pore size of 0.5 μm to prepare a composition for forming a magnetic layer.

<Preparation of composition for forming non-magnetic layer>
Of the various components of the non-magnetic layer-forming composition below, components other than stearic acid, butyl stearate, cyclohexanone, and methyl ethyl ketone were dispersed in beads using a batch-type vertical sand mill (dispersion media: zirconia beads (bead diameter : 0.1 mm), dispersion time: see Table 1) to obtain a dispersion. The remaining ingredients were then added to the resulting dispersion and stirred with a dissolver stirrer. Next, the resulting dispersion was filtered using a filter (pore size 0.5 μm) to prepare a composition for forming a non-magnetic layer.

Non-magnetic inorganic powder: α-iron oxide 100.0 parts Average particle size (average major axis length): 0.15 μm
Average acicular ratio: 7
BET specific surface area: 52 m ² /g
Carbon black 20.0 parts Average particle size: 20 nm
Electron beam-curable vinyl chloride copolymer 13.0 parts Electron beam-curable polyurethane resin 6.0 parts Stearic acid 1.0 parts Butyl stearate 1.0 parts Cyclohexanone 300.0 parts Methyl ethyl ketone 300.0 parts

<Preparation of Composition for Forming Backcoat Layer>
Of the various components of the composition for forming a backcoat layer described below, components other than stearic acid, butyl stearate, polyisocyanate and cyclohexanone were kneaded and diluted in an open kneader to obtain a mixture. After that, the resulting mixed solution is subjected to a horizontal bead mill, using zirconia beads with a bead diameter of 1.0 mm, at a bead filling rate of 80% by volume and a rotor tip peripheral speed of 10 m / sec, with a residence time of 2 minutes per pass. , and 12 passes of distributed processing were performed. The remaining ingredients were then added to the resulting dispersion and stirred with a dissolver stirrer. Next, the resulting dispersion was filtered using a filter (pore size: 1.0 μm) to prepare a composition for forming a backcoat layer.

Non-magnetic inorganic powder: α-iron oxide 80.0 parts Average particle size (average major axis length): 0.15 μm
Average acicular ratio: 7
BET specific surface area: 52 m ² /g
Carbon black 20.0 parts Average particle size: 20 nm
Vinyl chloride copolymer 13.0 parts Sulfonic acid group-containing polyurethane resin 6.0 parts Phenylphosphonic acid 3.0 parts Methyl ethyl ketone 155.0 parts Stearic acid 3.0 parts Butyl stearate 3.0 parts Polyisocyanate 5.0 parts Cyclohexanone 355.0 parts

<Production of magnetic tape>
After the composition for forming a non-magnetic layer was coated on a polyethylene naphthalate support and dried, it was irradiated with an electron beam at an acceleration voltage of 125 kV and an energy of 40 kGy to form a non-magnetic layer.
A coating layer was formed by coating the composition for forming a magnetic layer on the surface of the formed non-magnetic layer so that the thickness after drying was 50 nm. While this coating layer was in a wet state, it was subjected to the magnetic layer formation and orientation shown in Table 1 using opposing magnets of different poles in an atmosphere at the atmospheric temperature (magnetic layer drying temperature) shown in Table 1. A strong magnetic field was applied perpendicularly to the surface of the coating layer to perform vertical orientation treatment and drying treatment, thereby forming a magnetic layer.
After that, the composition for forming a backcoat layer was coated on the surface of the support opposite to the surface on which the non-magnetic layer and the magnetic layer were formed, and dried.
Then, using calender rolls composed only of metal rolls, the conditions were a calendering speed of 80 m/min, a linear pressure of 300 kg/cm (294 kN/m), and a calender temperature (surface temperature of the calender rolls) shown in Table 1. Surface smoothing treatment (calendering) was performed below.
After that, heat treatment was performed for 36 hours in an environment with an ambient temperature of 70°C. After heat treatment, the tape is slit to a width of 1/2 inch (1 inch is 0.0254 meters) and attached to a device equipped with a slit product feeder and take-up device so that the nonwoven fabric and razor blade are pressed against the surface of the magnetic layer. The surface of the magnetic layer was cleaned with a cleaning device.
With the magnetic layer of the magnetic tape obtained above demagnetized, a servo pattern having an arrangement and shape conforming to the LTO Ultrium format was formed on the magnetic layer by a servo write head mounted on a servo testing machine. As a result, a magnetic tape having a data band, a servo band, and a guide band arranged in accordance with the LTO Ultrium format on the magnetic layer and having a servo pattern arranged and shaped in accordance with the LTO Ultrium format on the servo band was obtained. . A total of 5,000,000 servo frames having A, B, C and D bursts are formed on this magnetic tape in the arrangement shown in FIG. The servo testing machine has a servo write head and a servo head. This servo tester was also used in the evaluations described later.
Through the above steps, the magnetic tape of Example 1 having the timing base servo pattern formed on the magnetic layer was produced.

[Examples 2 and 4, Comparative Examples 1 to 5]
A magnetic tape was produced in the same manner as in Example 1, except that various items shown in Table 1 were changed as shown in Table 1.
In Table 1, the magnetic tapes were produced without performing orientation treatment on the coating layer of the composition for forming the magnetic layer in the comparative examples described as "no orientation treatment" in the "formation and orientation of magnetic layer" column.

[Example 3]
After the formation of the non-magnetic layer, the composition for forming the magnetic layer was coated on the surface of the non-magnetic layer so that the thickness after drying was 50 nm to form a first coating layer. This first coating layer was passed through an atmosphere at the atmospheric temperature (magnetic layer drying temperature) shown in Table 1 without application of a magnetic field to form a first magnetic layer (without orientation treatment).
Thereafter, a magnetic layer-forming composition was coated on the surface of the first magnetic layer so as to have a thickness of 50 nm after drying to form a second coating layer. While this second coating layer was in a wet state, it was measured in Table 1 using opposing magnets of opposite poles in an atmosphere at the ambient temperature (magnetic layer drying temperature) shown in the column "Formation and Orientation of Magnetic Layer" in Table 1. A magnetic field of the indicated intensity was applied in the direction perpendicular to the surface of the second coating layer to perform vertical orientation treatment and drying treatment, thereby forming a second magnetic layer.
A magnetic tape was produced in the same manner as in Example 1, except that the multi-layered magnetic layer was formed as described above.

[Comparative Example 6]
After the formation of the non-magnetic layer, the composition for forming the magnetic layer was coated on the surface of the non-magnetic layer so that the thickness after drying was 50 nm to form a first coating layer. While this first coating layer was in a wet state, it was dried in the atmosphere at the ambient temperature (drying temperature of the magnetic layer) shown in Table 1 using opposed magnets with opposite poles. A magnetic field having the strength described in 1 was applied in a direction perpendicular to the surface of the first coating layer to perform vertical orientation treatment and drying treatment, thereby forming a first magnetic layer.
Thereafter, a magnetic layer-forming composition was coated on the surface of the first magnetic layer so as to have a thickness of 50 nm after drying to form a second coating layer. This second coating layer was passed through an atmosphere at the atmospheric temperature (magnetic layer drying temperature) shown in Table 1 without application of a magnetic field to form a second magnetic layer (without orientation treatment).
A magnetic tape was produced in the same manner as in Example 1, except that the multi-layered magnetic layer was formed as described above.

2. Various Evaluations (1) Thickness of Non-Magnetic Support and Each Layer The thicknesses of the magnetic layer, non-magnetic layer, non-magnetic support and back coat layer of each magnetic tape produced were measured by the following methods. As a result of the measurement, various thicknesses were the values shown in Table 1.
The thicknesses of the magnetic layer, non-magnetic layer and non-magnetic support measured here were used to calculate the refractive index below.
(i) Preparation of sample for cross-sectional observation According to the method described in paragraphs 0193 to 0194 of JP-A-2016-177851, including the entire region in the thickness direction from the magnetic layer side surface to the backcoat layer side surface of the magnetic tape. A sample for cross-sectional observation was prepared.
(ii) Thickness measurement The produced sample was observed by STEM, and an STEM image was taken. This STEM image is a STEM-HAADF (High-Angle Annular Dark Field) image taken at an acceleration voltage of 300 kV and an imaging magnification of 450,000 times. The image was taken so as to include the entire area in the thickness direction. In the STEM image thus obtained, a straight line connecting both ends of a line representing the surface of the magnetic layer was determined as a reference line representing the surface of the magnetic layer on the side of the magnetic layer. The straight line connecting the two ends of the line segment is, for example, an STEM image when an STEM image is taken such that the magnetic layer side of the sample for cross-sectional observation is positioned above the image and the backcoat layer side is positioned below the image. is a straight line connecting the intersection of the left side of the image (having a rectangular or square shape) and the line segment and the intersection of the right side of the STEM image and the line segment. Similarly, the reference line representing the interface between the magnetic layer and the non-magnetic layer, the reference line representing the interface between the non-magnetic layer and the non-magnetic support, the reference line representing the interface between the non-magnetic support and the back coat layer, the magnetic tape A reference line representing the backcoat layer side surface of was determined.
The thickness of the magnetic layer was determined as the shortest distance from a randomly selected point on the reference line representing the magnetic layer side surface of the magnetic tape to the reference line representing the interface between the magnetic layer and the non-magnetic layer. Similarly, the thicknesses of the non-magnetic layer, the non-magnetic support and the back coat layer were determined.

(2) ΔN of the magnetic layer
In the following, M-2000U manufactured by Woollam was used as an ellipsometer. The creation and fitting of the two-layer model or the one-layer model were performed using WVASE32 manufactured by Woollam as analysis software.
(i) Refractive index measurement of non-magnetic support A sample for measurement was cut out from each magnetic tape. An unused cloth is impregnated with methyl ethyl ketone, and this cloth is used to wipe off the backcoat layer of the measurement sample to expose the surface of the non-magnetic support. The surface was roughened with sandpaper so that it would not be detected in meter measurements.
Thereafter, an unused cloth was impregnated with methyl ethyl ketone, and the cloth was used to wipe off the magnetic layer and non-magnetic layer of the measurement sample. By attaching the measurement sample, the surface of the non-magnetic support exposed by removing the magnetic layer and the non-magnetic layer (hereinafter referred to as the "magnetic layer side surface of the non-magnetic support") faces upward. placed on a silicon wafer.
Using an ellipsometer, incident light was incident on the surface of the magnetic layer side of the non-magnetic support of the measurement sample on the silicon wafer, and Δ and ψ were measured as described above. Using the obtained measured value and the thickness of the non-magnetic support obtained in (2) above, the refractive index of the non-magnetic support (refractive index in the longitudinal direction, refractive index in the width direction, refractive index in the longitudinal direction, refractive index in the The refractive index in the thickness direction measured by incident light from the direction and the refractive index in the thickness direction measured by incident light incident from the width direction) were obtained.
(ii) Refractive index measurement of non-magnetic layer A sample for measurement was cut out from each magnetic tape. An unused cloth is impregnated with methyl ethyl ketone, and the cloth is used to wipe off the backcoat layer of the measurement sample to expose the non-magnetic support surface. The surface was roughened with sandpaper so that it would not be detected in the ellipsometer measurement.
Thereafter, an unused cloth is impregnated with methyl ethyl ketone, and the surface of the magnetic layer of the measurement sample is lightly wiped off with the cloth to remove the magnetic layer to expose the surface of the non-magnetic layer. A sample for measurement was placed on a silicon wafer.
The non-magnetic layer surface of the measurement sample on this silicon wafer is measured using an ellipsometer, and the refractive index of the non-magnetic layer (refractive index in the longitudinal direction, refractive index in the width direction, , the refractive index in the thickness direction measured with incident light incident from the longitudinal direction, and the refractive index in the thickness direction measured with incident light incident from the width direction) were determined.
(iii) Refractive Index Measurement of Magnetic Layer A sample for measurement was cut out from each magnetic tape. An unused cloth is impregnated with methyl ethyl ketone, and the cloth is used to wipe off the backcoat layer of the measurement sample to expose the non-magnetic support surface. The surface was roughened with sandpaper so that it would not be detected in the ellipsometer measurement.
Thereafter, a measurement sample was placed on a silicon wafer in the same manner as in (i) above.
The magnetic layer surface of the measurement sample on this silicon wafer was measured using an ellipsometer, and spectroscopic ellipsometry was used to determine the refractive index of the magnetic layer (refractive index Nx in the longitudinal direction, refractive index Nx in the width direction, The refractive index Ny, the refractive index Nz ₁ in the thickness direction measured by incident light from the longitudinal direction, and the refractive index Nz ₂ in the thickness direction measured by incident light incident from the width direction were obtained. Nxy and Nz were obtained from the obtained values, and the absolute value ΔN of the difference between them was obtained. For both the magnetic tapes of Examples and Comparative Examples, the obtained Nxy was a value larger than Nz (that is, Nxy>Nz).

(3) Vertical Squareness Ratio (SQ)
The vertical squareness ratio of the magnetic tape is the squareness ratio measured in the vertical direction of the magnetic tape. The "perpendicular direction" described in relation to the squareness ratio means the direction orthogonal to the surface of the magnetic layer. For each magnetic tape of Examples and Comparative Examples, an external magnetic field was applied to the magnetic tape at a maximum external magnetic field of 1194 kA / m ( 15 kOe) and a scanning speed of 4.8 kA/m/sec (60 Oe/sec) to obtain the vertical squareness ratio. The measured value is a value after demagnetization correction, and is obtained by subtracting the magnetization of the sample probe of the vibrating sample magnetometer as background noise. In one aspect, the vertical squareness ratio of the magnetic tape is preferably 0.60 or more and 1.00 or less, more preferably 0.65 or more and 1.00 or less. Also, in one aspect, the perpendicular squareness ratio of the magnetic tape can be, for example, less than or equal to 0.90, less than or equal to 0.85, or less than or equal to 0.80, or even greater than these values.

(4) Servo Signal Output Decrease The magnetic tape on which the timing-based servo pattern was formed was attached to a servo testing machine. In the servo testing machine, while the magnetic layer surface of the running magnetic tape and the servo head are brought into contact with each other and slid, the servo pattern from the first servo frame formed on the magnetic tape by the servo head to the final 5, Servo patterns were sequentially read (servo signal reproduction) up to the servo pattern of the 000,000th servo frame. Let A be the arithmetic mean of the signal outputs obtained in the 1st to 100th servo frames, and let B be the arithmetic mean of the signal outputs obtained in the 4,999,900th to 5,000,000th servo frames, The amount of output decrease (unit: %) of the servo signal was calculated as "[(B−A)/A]×100".

The above results are shown in Table 1 (Tables 1-1 and 1-2).

From the results shown in Table 1, in the magnetic tapes of Examples 1 to 4, in which the ΔN of the magnetic layer is within the range described above, the decrease in servo signal output is suppressed as compared with the magnetic tapes of Comparative Examples 1 to 6. It can be confirmed that there is
The squareness ratio is generally known as an index of the state of existence of ferromagnetic powder in the magnetic layer. However, as shown in Table 1, even magnetic tapes having the same vertical squareness ratio have different ΔN values (for example, Examples 3 and 4 and Comparative Example 6). The present inventor believes that this indicates that ΔN is a value affected by other factors in addition to the state of existence of the ferromagnetic powder in the magnetic layer.

One aspect of the present invention is useful in the technical field of magnetic tapes for high density recording.

Claims (9)

A magnetic tape having a magnetic layer containing ferromagnetic powder on a non-magnetic support,
the magnetic layer has a servo pattern,
The magnetic tape has a total thickness of 1.00 μm or more and 6.00 μm or less,
A magnetic tape, wherein a difference , Nxy-Nz, between a refractive index Nxy measured in the in-plane direction of the magnetic layer and a refractive index Nz measured in the thickness direction of the magnetic layer is 0.25 or more and 0.40 or less. 2. The magnetic tape according to claim 1 , comprising a non-magnetic layer containing non-magnetic powder between said non-magnetic support and said magnetic layer. 3. The magnetic tape according to claim 2 , wherein the total thickness of said magnetic layer and said non-magnetic layer is 0.60 [mu]m or less. 4. The magnetic tape according to any one of claims 1 to 3 , further comprising a back coat layer containing a non-magnetic powder on the surface of the non-magnetic support opposite to the surface having the magnetic layer. The magnetic tape of any one of claims 1-4 , wherein the servo pattern is a timing-based servo pattern. The magnetic tape according to any one of claims 1 to 5 , wherein the magnetic tape has a total thickness of 1.00 µm or more and 5.70 µm or less. The magnetic tape according to any one of claims 1 to 6 , wherein the magnetic tape has a total thickness of 1.00 µm or more and 5.50 µm or less. A magnetic tape cartridge containing the magnetic tape according to any one of claims 1 to 7 . A magnetic tape device comprising the magnetic tape according to any one of claims 1 to 7 and a magnetic head.

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