JP2006185487A - Method of analyzing organic compound on magnetic recording medium surface, magnetic recording medium manufacturing method using the method, and magnetic recording medium obtained by the method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of analyzing an organic compound by which quantity of the organic compound absorbed to or reacted with inorganic powder on a magnetic recording medium surface can be analyzed simply and surely, and to provide a magnetic recording medium manufacturing method using the analisis method, and the magnetic recording medium obtained by the manufacturing method. <P>SOLUTION: In the method of analyzing the organic compound absorbed or reacting to inorganic powder of a coating layer surface of a coating type magnetic recording medium, in which the coating layer including at least the inorganic powder and binder is formed on a substrate, the absorption of total reflection (ATR) spectrum of the coating layer surface including the absorption wave number being intrinsic to the organic compound to be analyzed is measured by using a Fourier transform infrared spectrophotometer (FT-IO), and the organic compound is analyzed. And the magnetic recording medium is manufactured by providing a process including this analysis method. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for analyzing an organic compound on the surface of a magnetic recording medium, a method for producing a magnetic recording medium using the method, and a magnetic recording medium obtained thereby, and more specifically, an inorganic powder on the surface of the magnetic recording medium. Manufactures an organic compound analysis method that can easily and accurately analyze the amount of organic compounds adsorbed or reacting on the body, a magnetic recording medium excellent in running durability, electromagnetic conversion characteristics, etc. And a magnetic recording medium obtained by the manufacturing method.

A coated product in which a coated layer made of at least an inorganic powder and a binder is provided on a support is used as a magnetic recording medium, for example. Such a coating type magnetic recording medium has been expanded in use for computers or broadcasts, but in these fields, reliability relating to durability and storability is very important. Since the coating type magnetic recording medium comes into contact with the head and the mechanical parts, it is necessary to maintain stable sliding characteristics between them. In order to provide good slidability, compounds such as higher fatty acids and higher fatty acid esters are blended in the magnetic layer and the nonmagnetic layer under the magnetic layer.
Among these compounds, higher fatty acids have a carboxyl group that is an acidic polar group, and this carboxyl group is adsorbed to the basic point of the magnetic substance or inorganic powder, which is great for ensuring relatively low sliding properties. Has contributed. In addition, the surface of the magnetic material or inorganic powder is covered to help improve the dispersibility of the powder.
However, if trace amounts of inorganic cations are present in magnetic materials, inorganic powders, or other blended materials, blended higher fatty acids and inorganic cations when the sample is stored over a long period of time or in a high-temperature, high-humidity atmosphere. May react gradually to produce a fatty acid metal salt. For example, when calcium salt of fatty acid is generated on the surface of the magnetic layer, protrusions are formed on the surface and the electromagnetic conversion characteristics are deteriorated by spacing, and it adheres to the head by running, or it causes dropout and error rate degradation, running. Deteriorates durability and electromagnetic characteristics. In addition, fatty acid iron salt that reacts with a small amount of iron ions and fatty acid has a little stickiness, so it increases the coefficient of friction, causes debris on the tape surface, further causes head dirt and head clogging, and remarkably deteriorates running durability. .
Higher fatty acid esters reduce the coefficient of friction at a relatively high speed, but when adverse conditions such as high temperature and high humidity overlap, fatty acids are produced by hydrolysis, and the produced fatty acids react with trace amounts of inorganic cations as described above. In some cases, a metal salt is produced.
From the above, it is important to suppress the formation of fatty acid metal salts on the surface of the magnetic layer in the development of a coating type magnetic recording medium for computers and broadcasts that requires high reliability. Therefore, a method for evaluating the fatty acid metal salt on the surface layer of the magnetic layer is required.

Fatty acid metal salts present in magnetic recording media are difficult to dissolve in organic solvents, and for separation and detection, acid or alkali such as HCl is reacted to desorb the adsorbed or reacted substance, and extraction is performed. There is a need to do.
In addition, in Patent Document 1, the present inventors reacted a derivatizing agent such as a silylating agent with a compound such as a fatty acid adsorbed or bonded to the inorganic powder, and the resulting derivative was converted to an inorganic powder. A method for analyzing inorganic powder adsorbing compounds separated from the body was proposed. As a result, polar compounds that are strongly adsorbed or reacted with inorganic powder can be separated and detected as derivatives.
However, this method is suitable for the analysis of polar compounds contained in the entire coating layer or magnetic layer, but is not suitable for analyzing the amount of organic compounds present in the coating layer or the surface layer of the magnetic layer that is most relevant to reliability. It is.

Therefore, in Patent Document 2, the present inventors have extracted and removed unadsorbed substances from the support provided with the coating layer with a solvent, and then measured the substance on the surface of the coating layer with an X-ray photoelectron spectrometer (XPS). Next, after adding the derivatization reagent and reacting and removing the adsorbed compound on the surface of the inorganic powder, the substance on the surface of the coating layer is measured with an X-ray photoelectron spectrometer, and adsorbed based on the difference in the measured value before and after the treatment with the derivatizing reagent Alternatively, a method for analyzing an adsorbed compound on the surface of an inorganic powder-containing coating layer for analyzing a compound forming a salt by a chemical reaction was proposed.
This method is very useful as a method for analyzing adsorbed compounds present on the surface of the coated product, particularly the magnetic layer of the magnetic recording medium.
However, this method requires chemical pretreatment, and requires XPS, which is an advanced analyzer, requiring specialized skills and skill, and it takes several days to obtain results. is there.

Japanese Patent Laid-Open No. 11-211712 JP 2001-6163 A

  Accordingly, an object of the present invention is to provide an organic compound analysis method, running durability, electromagnetic conversion characteristics, and the like that can easily and accurately analyze the amount of an organic compound adsorbed or reacted on an inorganic powder on the surface of a magnetic recording medium. It is an object to provide a method for producing an excellent magnetic recording medium using the analysis method and a magnetic recording medium obtained by the production method.

The present invention is as follows.
1) In a method of analyzing an organic compound adsorbed or reacted on an inorganic powder on the surface of a coating layer of a coating type magnetic recording medium provided with a coating layer containing at least an inorganic powder and a binder on a support. Using a Fourier transform infrared spectrophotometer (FT-IR), the total reflection absorption (ATR) spectrum of the coating layer surface including the absorption wave number specific to the organic compound to be analyzed is measured, and the coating layer surface inorganic An organic compound analysis method comprising analyzing an organic compound adsorbed or reacted on a powder.
2) In a method for producing a magnetic recording medium in which a coating layer containing at least a ferromagnetic powder and a binder is provided on a support, an organic to be analyzed using a Fourier transform infrared spectrophotometer (FT-IR) Measuring the total reflection absorption (ATR) spectrum of the coating layer surface including the absorption wave number inherent to the compound, and analyzing the organic compound adsorbed or reacting with the ferromagnetic powder on the coating layer surface. A method for manufacturing a magnetic recording medium.
3) The method for producing a magnetic recording medium according to 2) above, wherein the organic compound to be analyzed is a fatty acid metal salt.
4) A magnetic recording medium manufactured by the method for manufacturing a magnetic recording medium according to 2) or 3) above.
5) The magnetic recording medium as described in 4) above, wherein the index of the amount of the fatty acid metal salt is 0.01 or less.

  According to the present invention, an organic compound adsorbed or reacted on the inorganic powder on the surface of the coating layer, particularly a fatty acid metal salt that forms a salt by reacting with a ferromagnetic powder is converted into a Fourier transform infrared spectrophotometer ( Since it measures based on the total reflection absorption (ATR) spectrum using FT-IR), it does not require any special technique compared to a conventional XPS or surface analyzer such as an Auger electron spectrometer (AES). Easy and accurate analysis. Therefore, if the analysis method of the present invention is used, the amount of the organic compound adsorbed or reacted to the inorganic powder on the surface of the coating layer, particularly the amount of the fatty acid metal salt is below a certain value, running durability, electromagnetic conversion characteristics, etc. Excellent magnetic recording media can be obtained.

In the analysis method of the present invention, an organic compound adsorbed or reacted with an inorganic powder on the surface of a coating layer of a magnetic recording medium is converted into a total reflection absorption spectrum (hereinafter referred to as ATR-FT-) using a Fourier transform infrared spectrophotometer. (Referred to as IR).
A sample to which the analysis method of the present invention is applied is preferably a magnetic recording medium having a magnetic layer formed by dispersing ferromagnetic powder in a binder. The organic compound to be analyzed is not particularly limited as long as it is an organic compound that is adsorbed or reacted with the inorganic powder on the surface of the coating layer.
In the present invention, the coating layer surface is a concept including a coating layer surface layer including a coating layer surface including about 0.1 μm in the thickness direction from the coating layer surface measurable by ATR-FT-IR.
In the present invention, the organic compound adsorbed or reacted on the inorganic powder means a fatty acid metal salt, a fatty acid, or phenylphosphonic acid.
In the present invention, a preferable organic compound to be analyzed includes a fatty acid metal salt that forms a salt by reacting with a ferromagnetic powder.
Hereinafter, the case where the sample to be analyzed is a magnetic recording medium and the organic compound to be analyzed is a fatty acid metal salt will be described.

The Fourier transform infrared spectrophotometer (FT-IR) used in the present invention is widely known in the art and can be appropriately selected from general-purpose products. In addition, ATR-FT-IR in this specification uses Thermo-Nicolet, product name Nexus670, and uses a single reflection horizontal ATR accessory, an incident angle of 60 °, resolution of 1 cm ⁻¹ , and 200 times integration. It is the spectrum obtained by performing.

  In the analysis of the fatty acid metal salt based on ATR-FT-IR in the present invention, information with a detection depth of 0.1 μm is obtained in the magnetic layer using the ferromagnetic inorganic powder. On the other hand, in the analysis by XPS or AES, the detection depth is several nm, and ATR-FT-IR evaluates the depth several tens of times that in the analysis by XPS or AES. However, according to the study by the present inventors, it was found that the amount of fatty acid metal salt obtained from both correlated very well, so that ATR-FT-IR can be used without using expensive XPS or AES. It was possible to analyze the fatty acid metal salt on the surface of the magnetic layer in question more easily and directly.

Carboxylate derived from fatty acid metal salt is antisymmetrical stretching vibration in the vicinity of 1610～1550Cm ^-1, indicating the absorption attributed to the symmetric stretching vibration near 1400 cm ^-1. Therefore, the fatty acid metal salt can be quantified by determining the absorbance of the fatty acid metal salt at the wave number as described above from the obtained ATR-FT-IR.
The magnetic layer in a magnetic recording medium usually contains a vinyl chloride resin, polyurethane, and an isocyanate curing agent in combination as a binder. In particular, the inherent absorption wave number of polyurethane or a curing agent is a fatty acid metal salt. It may overlap. For example, in the case of a polyurethane or a curing agent containing a phenyl group, absorption of the phenyl group is observed in the vicinity of 1600 cm ⁻¹ . Further, the urethane bond has absorption in the vicinity of 1530 cm ⁻¹ . Therefore, the position of the valley having the lowest absorbance between these absorptions, that is, between 1600 and 1530 cm ⁻¹ (including protrusions and shoulders, etc .; the same shall apply hereinafter) can be adopted as the absorbance of the carboxylate.

To quantify the fatty acid metal salt by ATR-FT-IR, specifically, the following steps (1) to (5) can be employed.
(1) A derivatizing reagent is added to the sample, and the fatty acid metal salt, fatty acid, fatty acid ester, and phenylphosphonic acid are removed from the sample to prepare a control sample.
(2) ATR-FT-IR of the control sample is measured.
(3) Separately from (1) and (2), the ATR-FT-IR of the sample is measured without adding a derivatization reagent to the sample.
(4) From the ATR-FT-IR of each of the sample and the control sample, the absorbance of the absorption wave number specific to the fatty acid metal salt (carboxylate) is determined. The derivatization treatment removes fatty acid metal salt, fatty acid, fatty acid ester, and phenylphosphonic acid, but does not affect the absorption of ATR-FT-IR carboxylate.
(5) In the absorption wave number specific to the fatty acid metal salt (carboxylate), the absorbance of the control sample is subtracted from the absorbance of the sample, and the value is used as an index of the amount of the fatty acid metal salt.
According to the study by the present inventors, if the binder composition used for the magnetic recording medium (resin component, curing agent such as polyisocyanate) is the same, even if the other composition and the production process of the medium are different, A similar ATR-FT-IR with a substantially constant baseline is obtained. Therefore, when the binder composition used in the magnetic recording medium is the same, if the ATR-FT-IR of the control sample is present, the ATR-FT-IR of the new sample is measured and is inherent to the fatty acid metal salt (carboxylate). The fatty acid metal salt can be quantified without going through the step (1) of performing the derivatization treatment only by obtaining the difference between the absorbance at the absorption wave number and the absorbance at the baseline. In addition, when a used binder differs, it is preferable to pass through the process of said (1)-(5).

ATR-FT-IR is a change in the binder composition as described above, and the absorption wave number of the fatty acid metal salt (carboxylate) and the baseline at that position vary depending on the overlap with the peak derived from the binder adjacent to the absorption wave number. If so, it is necessary to select an appropriate baseline. When using the polyurethane resin as a binder, it can be the absorbance of the lowest position between the phenyl groups in the vicinity of an ester bond and 1600 cm ^-1 of the polyurethane of 1730 cm ^-1 baseline.

Next, the derivatization process in the step (1) will be described.
Examples of the derivatizing reagent include a silylating agent, an esterifying agent, and an acylating agent, and it is particularly preferable to use a silylating agent. By using a silylating agent, a derivative can be formed by reacting with a fatty acid metal salt having no active hydrogen, which has conventionally been impossible, so that the fatty acid metal salt can be separated and detected.
Examples of silylating agents include N-trimethylsilylimidazole (TMSI), N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA), N, O-bis (trimethylsilyl) acetamide (BSA), N-methyl-N-trimethylsilyltri Fluoroacetamide (MSTFA), N- (trimethylsilyl) dimethylamine (TMSDMA), N- (trimethylsilyl) diethylamine (TMS-DEA), N-methyl-N-trimethylsilylacetamide (MTMSA), trimethylchlorosilane (TMCS), hexamethylenedi Examples include silazane (HMDS), N-methyl-N- (t-butyldimethylsilyl) -trifluoroacetamide (MTBSTFA), and the like. A compound having TMS (trimethylsilyl group) is particularly preferable.

  For derivatization, for example, a part of the magnetic recording medium is taken out, put in a sealable sample bottle, added with hexane and a derivatizing reagent (silylating agent), reacted for an appropriate time, and desorbed from the inorganic powder as a derivative. Let For example, when using TMSI-H agent (HMDS: TMCS: pyridine mixture) manufactured by GL Sciences, the temperature is about 60 ° C. for about 30 minutes. Subsequently, the reaction solution is discarded, and the medium is rinsed with a solvent that does not dissolve the binder, such as ethanol, to remove the derivatized fatty acid metal salt. The ATR-FT-IR of the obtained control sample is measured.

Although the derivatization treatment of the fatty acid metal salt has been described above, the silylating agent can also be suitably used when the organic compound to be analyzed is a compound having active hydrogen other than the fatty acid metal salt.
As described above, the present invention has an effect that a complicated operation such as extraction with HCl, alkali, or polar solvent is unnecessary, and easily and accurately measures an organic compound adsorbed or reacted on an inorganic powder. be able to.

Next, the layer structure of the magnetic recording medium manufactured according to the present invention will be described.
[Support]
The support in the present invention is a nonmagnetic support, and a polyester support (hereinafter simply referred to as polyester) is preferable. Such a polyester is a polyester composed of a dicarboxylic acid and a diol, such as polyethylene terephthalate and polyethylene naphthalate.
The main constituent dicarboxylic acid components include terephthalic acid, isophthalic acid, phthalic acid, 2,6-naphthalenedicarboxylic acid, 2,7-naphthalenedicarboxylic acid, diphenylsulfone dicarboxylic acid, diphenyl ether dicarboxylic acid, diphenylethanedicarboxylic acid, Examples thereof include cyclohexane dicarboxylic acid, diphenyl dicarboxylic acid, diphenyl thioether dicarboxylic acid, diphenyl ketone dicarboxylic acid, and phenylindane dicarboxylic acid.
Examples of the diol component include ethylene glycol, propylene glycol, tetramethylene glycol, cyclohexanedimethanol, 2,2-bis (4-hydroxyphenyl) propane, 2,2-bis (4-hydroxyethoxyphenyl) propane, bis ( 4-Hydroxyphenyl) sulfone, bisphenol fluorene hydroxyethyl ether, diethylene glycol, neopentyl glycol, hydroquinone, cyclohexanediol and the like.
Among the polyesters having these as main constituents, terephthalic acid and / or 2,6-naphthalenedicarboxylic acid as a dicarboxylic acid component and ethylene glycol as a diol component from the viewpoint of transparency, mechanical strength, dimensional stability, etc. And / or a polyester mainly composed of 1,4-cyclohexanedimethanol is preferred.
Among them, a polyester mainly composed of polyethylene terephthalate or polyethylene-2,6-naphthalate, a copolymer polyester composed of terephthalic acid, 2,6-naphthalenedicarboxylic acid and ethylene glycol, and two or more kinds of these polyesters A polyester having a mixture as a main constituent is preferred. Particularly preferred is a polyester having polyethylene-2,6-naphthalate as a main constituent.
The polyester used in the present invention may be biaxially stretched or a laminate of two or more layers.
The polyester may be further copolymerized with other copolymerization components, or may be mixed with other polyesters. Examples of these include the dicarboxylic acid components and diol components mentioned above, or polyesters composed thereof.
In the polyester used in the present invention, an aromatic dicarboxylic acid having a sulfonate group or an ester-forming derivative thereof, a dicarboxylic acid having a polyoxyalkylene group or an ester-forming derivative thereof, in order to make it difficult for delamination during film formation. A diol having a polyoxyalkylene group may be copolymerized.
Of these, 5-sodium sulfoisophthalic acid, 2-sodium sulfoterephthalic acid, 4-sodium sulfophthalic acid, 4-sodium sulfo-2,6-naphthalenedicarboxylic acid, and the like in terms of polyester polymerization reactivity and film transparency. Compounds in which sodium is substituted with other metals (for example, potassium, lithium, etc.), ammonium salts, phosphonium salts, etc., or ester-forming derivatives thereof, polyethylene glycol, polytetramethylene glycol, polyethylene glycol-polypropylene glycol copolymers and their A compound obtained by oxidizing the hydroxy groups at both ends to form a carboxyl group is preferred. The proportion of copolymerization for this purpose is preferably 0.1 to 10 mol% based on the dicarboxylic acid constituting the polyester.
For the purpose of improving heat resistance, a bisphenol compound, a compound having a naphthalene ring or a cyclohexane ring can be copolymerized. The copolymerization ratio is preferably 1 to 20 mol% based on the dicarboxylic acid constituting the polyester.

In the present invention, the method for synthesizing the polyester is not particularly limited, and can be produced according to a conventionally known polyester production method. For example, a direct esterification method in which a dicarboxylic acid component is directly esterified with a diol component. First, a dialkyl ester is used as a dicarboxylic acid component, this is transesterified with the diol component, and this is heated under reduced pressure. A transesterification method of polymerizing by removing excess diol component can be used. At this time, if necessary, a transesterification catalyst or a polymerization reaction catalyst can be used, or a heat-resistant stabilizer can be added.
In addition, anti-coloring agents, antioxidants, crystal nucleating agents, slipping agents, stabilizers, anti-blocking agents, UV absorbers, viscosity modifiers, antifoaming and clearing agents, antistatic agents, pH adjustments in each process during synthesis One or more of various additives such as an agent, a dye, a pigment, and a reaction terminator may be added.

  Further, a filler may be added to the polyester. Examples of the filler include inorganic powders such as spherical silica, colloidal silica, titanium oxide, and alumina, and organic fillers such as crosslinked polystyrene and silicone resin.

  In the present invention, the thickness of the polyester as the support is preferably 3 to 80 μm, more preferably 3 to 50 μm, and particularly preferably 3 to 10 μm. The center line average roughness (Ra) of the support surface is 8 nm or less, more preferably 6 nm or less. This Ra was measured with TOPO-3D manufactured by WYKO.

  In the magnetic recording medium of the present invention, a magnetic layer formed by dispersing ferromagnetic powder in a binder as a coating layer is provided on the nonmagnetic support, and the support and the magnetic layer are provided as necessary. A nonmagnetic layer (lower layer) that is substantially nonmagnetic may be provided between the two.

[Magnetic layer]
The ferromagnetic powder contained in the magnetic layer preferably has a volume of (0.1 to 8) × 10 ⁻¹⁸ ml, more preferably (0.5 to 5) × 10 ⁻¹⁸ ml. By setting it within this range, it is possible to effectively suppress a decrease in magnetic characteristics due to thermal fluctuations, and to obtain good C / N (S / N) while maintaining low noise. Examples of the ferromagnetic powder include ferromagnetic metal powder.
The volume of the ferromagnetic metal powder can be determined as follows.
As for the ferromagnetic metal powder, the volume is determined from the major axis length and minor axis length assuming the shape as a cylinder. As for the size of the magnetic material, an appropriate amount of the magnetic layer is peeled off. N-Butylamine is added to 30 to 70 mg of the peeled magnetic layer, sealed in a glass tube, set in a thermal decomposition apparatus, and heated at 140 ° C. for about 1 day. After cooling, the contents are taken out from the glass tube and centrifuged to separate the liquid and solids. The separated solid is washed with acetone to obtain a powder sample for TEM. This sample is photographed with a Hitachi transmission electron microscope H-9000, and the particles are photographed at a photographing magnification of 100000 times and printed on a photographic paper to obtain a total magnification of 500,000 times to obtain a particle photograph. A target magnetic substance is selected from the particle photograph and placed on an image analyzer KS-400 digitizer manufactured by kontron, and the size of each particle is measured by tracing the outline of the powder. The size of 500 particles is measured, and the measured values are averaged to obtain the average particle size.

<Ferromagnetic metal powder>
The ferromagnetic metal powder used for the magnetic layer in the magnetic recording medium of the present invention is not particularly limited as long as it contains Fe as a main component (including an alloy), but is ferromagnetic with α-Fe as a main component. Alloy powder is preferred. These ferromagnetic powders include Al, Si, S, Sc, Ca, Ti, V, Cr, Cu, Y, Mo, Rh, Pd, Ag, Sn, Sb, Te, Ba, Ta, other than predetermined atoms. It may contain atoms such as W, Re, Au, Hg, Pb, Bi, La, Ce, Pr, Nd, P, Co, Mn, Zn, Ni, Sr, and B. It is preferable that at least one of Al, Si, Ca, Y, Ba, La, Nd, Co, Ni, and B is included in addition to α-Fe, and it is particularly preferable that Co, Al, and Y are included. More specifically, it is preferable that Co is contained in an amount of 10 to 40 atomic%, Fe is contained in an amount of 2 to 20 atomic%, and Y is contained in an amount of 1 to 15 atomic%.

The ferromagnetic metal powder may be previously treated with a dispersant, a lubricant, a surfactant, an antistatic agent or the like, which will be described later. The ferromagnetic metal powder may contain a small amount of water, hydroxide or oxide. The moisture content of the ferromagnetic metal powder is preferably 0.01-2%. It is preferable to optimize the moisture content of the ferromagnetic metal powder depending on the type of the binder. The pH of the ferromagnetic metal powder is preferably optimized depending on the combination with the binder used. The range is usually from 6 to 12, but preferably from 7 to 11. The ferromagnetic powder may contain inorganic ions such as soluble Na, Ca, Fe, Ni, Sr, NH ₄ , SO ₄ , Cl, NO ₂ and NO ₃ . These are preferably essentially absent. If the total of each ion is about 300 ppm or less, the characteristics are not affected. The ferromagnetic powder used in the present invention preferably has fewer pores, and its value is 20% by volume or less, and more preferably 5% by volume or less.

  The crystallite size of the ferromagnetic metal powder is preferably 8 to 20 nm, more preferably 10 to 18 nm, and particularly preferably 12 to 16 nm. This crystallite size is an average value obtained by a Scherrer method from a half-value width of a diffraction peak using an X-ray diffractometer (RINT2000 series manufactured by Rigaku Corporation) under the conditions of a radiation source CuKα1, a tube voltage 50 kV, and a tube current 300 mA. .

The specific surface area by BET method of the ferromagnetic metal powder (S _BET) is preferably less than 30 m ² / g or more 80 m ² / g, more preferably from 50 to 70 m ² / g. Within this range, both good surface properties and low noise can be achieved. The pH of the ferromagnetic metal powder is preferably optimized depending on the combination with the binder used. The range is 4-12, preferably 7-10. The ferromagnetic metal powder may be surface-treated with Al, Si, P, or an oxide thereof as required. The amount thereof is 0.1 to 10% with respect to the ferromagnetic metal powder. When the surface treatment is performed, the adsorption of a lubricant such as a fatty acid is preferably 100 mg / m ² or less. The ferromagnetic metal powder may contain soluble inorganic ions such as Na, Ca, Fe, Ni, and Sr. However, if it is 200 ppm or less, it does not particularly affect the characteristics. Further, the ferromagnetic metal powder used in the present invention preferably has fewer vacancies, and its value is 20% by volume or less, more preferably 5% by volume or less.

The shape of the ferromagnetic metal powder may be needle-like, granular, rice-grained or plate-like as long as the particle volume shown above is satisfied, but it is particularly preferable to use a needle-like ferromagnetic powder. In the case of acicular ferromagnetic metal powder, the acicular ratio is preferably 4-12, more preferably 5-12. The coercive force (Hc) of the ferromagnetic metal powder is preferably 159.2 to 238.8 kA / m (2000 to 3000 Oe), more preferably 167.2 to 230.8 kA / m (2100 to 2900 Oe). . The saturation magnetic flux density is preferably 150 to 300 mT (1500 to 3000 G), and more preferably 160 to 290 mT. The saturation magnetization (σs) is preferably 140 to 170 A · m ² / kg (140 to 170 emu / g), and more preferably 145 to 160 A · m ² / kg. The SFD (switching field distribution) of the magnetic material itself is preferably small and is preferably 0.8 or less. When the SFD is 0.8 or less, the electromagnetic conversion characteristics are good, the output is high, the magnetization reversal is sharp, the peak shift is small, and it is suitable for high-density digital magnetic recording. In order to reduce the Hc distribution, there are methods such as improving the particle size distribution of goethite in the ferromagnetic metal powder, using monodispersed αFe ₂ O ₃ , and preventing sintering between particles.

  As the ferromagnetic metal powder, those obtained by a known production method can be used, and the following methods can be mentioned. Reduction of hydrous iron oxide and iron oxide with anti-sintering treatment using iron or other reducing gas to obtain Fe or Fe-Co particles, reduction of complex organic acid salt (mainly oxalate) and hydrogen A method of reducing with a reactive gas, a method of thermally decomposing a metal carbonyl compound, a method of reducing by adding a reducing agent such as sodium borohydride, hypophosphite or hydrazine to an aqueous solution of a ferromagnetic metal, a metal at a low pressure For example, the powder is obtained by evaporating in an inert gas. The ferromagnetic metal powder thus obtained is subjected to a known slow oxidation treatment. A method of reducing the amount of demagnetization by reducing the hydrous iron oxide and iron oxide with a reducing gas such as hydrogen and controlling the partial pressure, temperature and time of the oxygen-containing gas and inert gas to form an oxide film on the surface. preferable.

<Binder>
The binder (binder) used in the magnetic layer of the present invention is a conventionally known thermoplastic resin, thermosetting resin, reactive resin, or a mixture thereof. Examples of the thermoplastic resin include vinyl chloride, vinyl acetate, vinyl alcohol, maleic acid, acrylic acid, acrylic ester, vinylidene chloride, acrylonitrile, methacrylic acid, methacrylic ester, styrene, butadiene, ethylene, vinyl butyral, vinyl acetal. And polymers or copolymers containing vinyl ether as a constituent unit, polyurethane resins, and various rubber resins.

  Examples of thermosetting resins or reactive resins include phenolic resins, epoxy resins, polyurethane curable resins, urea resins, melamine resins, alkyd resins, acrylic reactive resins, formaldehyde resins, silicone resins, and epoxy-polyamide resins. And a mixture of polyester resin and isocyanate prepolymer, a mixture of polyester polyol and polyisocyanate, a mixture of polyurethane and polyisocyanate, and the like. The thermoplastic resin, thermosetting resin and reactive resin are all described in detail in “Plastic Handbook” issued by Asakura Shoten.

  Further, when an electron beam curable resin is used for the magnetic layer, not only the coating film strength is improved and the durability is improved, but also the surface is smoothed and the electromagnetic conversion characteristics are further improved. These examples and their production methods are described in detail in JP-A No. 62-256219.

  The above resins can be used alone or in combination. Among them, it is preferable to use a polyurethane resin, and further, a cyclic structure such as hydrogenated bisphenol A or a polypropylene oxide adduct of hydrogenated bisphenol A, a polyol having an alkylene oxide chain with a molecular weight of 500 to 5000, and a chain extender. A polyurethane resin having a cyclic structure and a molecular weight of 200 to 500 reacted with an organic diisocyanate and having a polar group introduced, or an aliphatic dibasic acid such as succinic acid, adipic acid, or sebacic acid; Fat having no cyclic structure having an alkyl branched side chain such as dimethyl-1,3-propanediol, 2-ethyl-2-butyl-1,3-propanediol, 2,2-diethyl-1,3-propanediol Polyester polyol composed of a group diol and 2 as a chain extender Reaction of an aliphatic diol having a branched alkyl side chain having 3 or more carbon atoms such as ethyl-2-butyl-1,3-propanediol and 2,2-diethyl-1,3-propanediol with an organic diisocyanate compound And a polyurethane resin into which a polar group is introduced, or a cyclic structure such as dimer diol, a polyol compound having a long-chain alkyl chain, and an organic diisocyanate, and a polyurethane resin into which a polar group is introduced are used. Is preferred.

  The average molecular weight of the polar group-containing polyurethane resin used in the present invention is preferably 5,000 to 100,000, and more preferably 10,000 to 50,000. If the average molecular weight is 5,000 or more, it is preferable because the obtained magnetic coating film is not brittle and the physical strength is not lowered, and the durability of the magnetic recording medium is not affected. Further, when the molecular weight is 100,000 or less, the solubility in the solvent does not decrease, and the dispersibility is also good. Further, since the viscosity of the paint at a predetermined concentration does not increase, the workability is good and the handling is easy.

Examples of the polar group contained in the polyurethane resin, for _{example, -COOM, -SO 3 M, -OSO} 3 M, -P = O (OM) 2, -O-P = O (OM) per ₂ (or more, M is a hydrogen atom or an alkali metal base), —OH, —NR ₂ , —N ⁺ R ₃ (R is a hydrocarbon group), an epoxy group, —SH, —CN, etc., and at least one of these polar groups One in which two or more are introduced by copolymerization or addition reaction can be used. Moreover, when this polar group-containing polyurethane-based resin has an OH group, it preferably has a branched OH group from the viewpoint of curability and durability, and preferably has 2 to 40 branched OH groups per molecule. It is more preferable to have 3 to 20 molecules per molecule. The amount of such a polar group is 10 ⁻¹ to 10 ⁻⁸ mol / g, preferably 10 ⁻² to 10 ⁻⁶ mol / g.

  Specific examples of the binder include, for example, VAGH, VYHH, VMCH, VAGF, VAGD, VROH, VYES, VYNC, VMCC, XYHL, XYSG, PKHH, PKHJ, PKHC, PKFE, Nissin Chemical Industry Co., Ltd. MPR-TA, MPR-TA5, MPR-TAL, MPR-TSN, MPR-TMF, MPR-TS, MPR-TM, MPR-TAO, Denki Kagaku 1000W, DX80, DX81, DX82, DX83, 100FD, Japan MR-104, MR-105, MR110, MR100, MR555, 400X-110A manufactured by ZEON Co., Ltd. NIPPOLAN N2301, N2302, N2304 manufactured by Nippon Polyurethane Co., Ltd. Pandex T-5105, T-R3080, T-5201 manufactured by Dainippon Ink, Inc. , Barnock D 400, D-210-80, Crisbon 6109, 7209, Byron UR8200, UR8300, UR-8700, RV530, RV280, Toyobo Co., Ltd. Daiferamin 4020, 5020, 5100, 5300, 9020, 9022, 7020, Mitsubishi Examples include MX5004 manufactured by Kasei Co., Ltd., Sanprene SP-150 manufactured by Sanyo Kasei Co., Ltd., and Saran F310 and F210 manufactured by Asahi Kasei.

The amount of the binder used in the magnetic layer of the present invention is in the range of 5 to 50% by mass, preferably in the range of 10 to 30% by mass with respect to the mass of the ferromagnetic metal powder. When a polyurethane resin is used, it is preferable to use a combination of 2 to 20% by mass and polyisocyanate in a range of 2 to 20% by mass. For example, when head corrosion occurs due to a small amount of dechlorination, polyurethane is used. It is also possible to use only polyurethane or only isocyanate and polyurethane. When using a vinyl chloride resin as the other resin, it is preferably in the range of 5 to 30% by mass. In the present invention, when polyurethane is used, the glass transition temperature is −50 to 150 ° C., preferably 0 to 100 ° C., the breaking elongation is 100 to 2000%, and the breaking stress is 0.49 to 98 MPa (0.05 to 10 kg / mm). ² ) The yield point is preferably 0.49 to 98 MPa (0.05 to 10 kg / mm ² ).

  When the magnetic recording medium used in the present invention is, for example, a floppy disk, it can be composed of two or more layers on both sides of the support. Therefore, the amount of the binder, the amount of vinyl chloride resin, polyurethane resin, polyisocyanate, or other resin in the binder, the molecular weight of each resin forming the magnetic layer, the polar group amount, or the resin described above It is of course possible to change the physical characteristics and the like between the non-magnetic layer and each magnetic layer as required, and rather it should be optimized for each layer, and a known technique relating to a multilayer magnetic layer can be applied. For example, when changing the amount of binder in each layer, it is effective to increase the amount of binder in the magnetic layer in order to reduce scratches on the surface of the magnetic layer. The amount of binder in the magnetic layer can be increased to provide flexibility.

  Examples of the polyisocyanate usable in the present invention include tolylene diisocyanate, 4,4′-diphenylmethane diisocyanate, hexamethylene diisocyanate, xylylene diisocyanate, naphthylene-1,5-diisocyanate, o-toluidine diisocyanate, isophorone diisocyanate, triol. Examples thereof include isocyanates such as phenylmethane triisocyanate, products of these isocyanates and polyalcohols, and polyisocyanates generated by condensation of isocyanates. Commercially available product names of these isocyanates include Coronate L, Coronate HL, Coronate 2030, Coronate 2031, Millionate MR Millionate MTL, Takeda Pharmaceutical Takenate D-102, Takenate D-110N, Takenate. There are D-200, Takenate D-202, Death Module L, Death Module IL, Death Module N, Death Module HL, etc. manufactured by Sumitomo Bayer, and these are used alone or two or more using the difference in curing reactivity. Each layer can be used in combination.

Additives can be added to the magnetic layer in the present invention as necessary. Examples of the additive include an abrasive, a lubricant, a dispersant / dispersion aid, an antifungal agent, an antistatic agent, an antioxidant, a solvent, and carbon black. Examples of these additives include molybdenum disulfide, tungsten disulfide, graphite, boron nitride, graphite fluoride, silicone oil, silicone having a polar group, fatty acid-modified silicone, fluorine-containing silicone, fluorine-containing alcohol, fluorine-containing ester, Polyolefin, polyglycol, polyphenyl ether, phenylphosphonic acid, benzylphosphonic acid, phenethylphosphonic acid, α-methylbenzylphosphonic acid, 1-methyl-1-phenethylphosphonic acid, diphenylmethylphosphonic acid, biphenylphosphonic acid, benzylphenylphosphonic acid , Α-cumylphosphonic acid, toluylphosphonic acid, xylylphosphonic acid, ethylphenylphosphonic acid, cumenylphosphonic acid, propylphenylphosphonic acid, butylphenylphosphonic acid, heptylph Aromatic ring-containing organic phosphonic acids such as enylphosphonic acid, octylphenylphosphonic acid, nonylphenylphosphonic acid and alkali metal salts thereof, octylphosphonic acid, 2-ethylhexylphosphonic acid, isooctylphosphonic acid, isononylphosphonic acid, isodecylphosphonic acid Acids, isoundecyl phosphonic acid, isododecyl phosphonic acid, isohexadecyl phosphonic acid, isooctadecyl phosphonic acid, isoeicosyl phosphonic acid, alkylphosphonic acid and alkali metal salts thereof, phenyl phosphate, benzyl phosphate, phosphoric acid Phenethyl, α-methylbenzyl phosphate, 1-methyl-1-phenethyl phosphate, diphenylmethyl phosphate, biphenyl phosphate, benzylphenyl phosphate, α-cumyl phosphate, toluyl phosphate, xylyl phosphate, ethyl phosphate Phenyl, Li Aromatic phosphates such as cumenyl phosphate, propylphenyl phosphate, butylphenyl phosphate, heptylphenyl phosphate, octylphenyl phosphate, nonylphenyl phosphate, and alkali metal salts thereof, octyl phosphate, 2-ethylhexyl phosphate , Isooctyl phosphate, isononyl phosphate, isodecyl phosphate, isoundecyl phosphate, isododecyl phosphate, isohexadecyl phosphate, isooctadecyl phosphate, isoeicosyl phosphate, and alkali metal salts thereof, alkylsulfonic acid Esters and alkali metal salts thereof, fluorine-containing alkyl sulfates and alkali metal salts thereof, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, butyl stearate, oleic acid, linoleic acid, linolenic acid, Eleiji Monobasic fatty acids that may contain or be branched, such as acids and erucic acids, and their metal salts, or butyl stearate, octyl stearate, amyl stearate, isooctyl stearate Monobasic, which may contain or be branched, containing an unsaturated bond having 10 to 24 carbon atoms, such as octyl myristate, butyl laurate, butoxyethyl stearate, anhydrosorbitan monostearate, anhydrosorbitan tristearate Fatty acid and 1-6 hexahydric alcohol which may contain or be branched including an unsaturated bond having 2 to 22 carbon atoms, alkoxy alcohol or alkylene oxide which may contain or be branched an unsaturated bond having 12 to 22 carbon atoms Mono-fatty acid ester comprising any one of polymer monoalkyl ethers Di-fatty acid esters or polyvalent fatty acid esters, fatty acid amides having 2 to 22 carbon atoms, and aliphatic amines having 8 to 22 carbon atoms can be used. In addition to the above hydrocarbon groups, alkyl groups, aryl groups, and aralkyl groups substituted with nitro groups and groups other than hydrocarbon groups such as halogen-containing hydrocarbons such as F, Cl, Br, CF ₃ , CCl ₃ , and CBr ₃ You may have something.

  In addition, nonionic surfactants such as alkylene oxide, glycerin, glycidol, and alkylphenol ethylene oxide adducts, cyclic amines, ester amides, quaternary ammonium salts, hydantoin derivatives, heterocyclics, phosphonium or sulfoniums, etc. Amphoteric interfaces such as cationic surfactants, anionic surfactants containing acidic groups such as carboxylic acid, sulfonic acid, and sulfate ester groups, amino acids, aminosulfonic acids, sulfuric or phosphate esters of aminoalcohols, and alkylbetaines An activator or the like can also be used. These surfactants are described in detail in “Surfactant Handbook” (published by Sangyo Tosho Co., Ltd.).

  The above-mentioned lubricant, antistatic agent and the like are not necessarily pure and may contain impurities such as isomers, unreacted materials, side reaction products, decomposition products, oxides, etc. in addition to the main components. These impurities are preferably 30% by mass or less, more preferably 10% by mass or less.

  Specific examples of these additives include, for example, NAF-102, castor oil hardened fatty acid, NAA-42, cation SA, Naimine L-201, Nonion E-208, Anon BF, Anon LG, Takemoto, manufactured by NOF Corporation. Oil and fat: FAL-205, FAL-123, Shin Nippon Chemical Co., Ltd .: NS : BA-41G, Sanyo Kasei Co., Ltd .: Profan 2012E, New Pole PE61, Ionette MS-400 and the like.

In addition, carbon black can be added to the magnetic layer in the present invention as necessary. Examples of carbon black that can be used in the magnetic layer include rubber furnace, rubber thermal, color black, and acetylene black. Specific surface area is 5 to 500 m ² / g, DBP oil absorption is 10 to 400 ml / 100 g, particle size is 5 to 300 mμ, pH is 2 to 10, moisture content is 0.1 to 10%, tap density is 0.1 to 1 g / ml is preferred.

  Specific examples of carbon black used in the present invention include Cabot's BLACKPEARLS 2000, 1300, 1000, 900, 905, 800, 700, VULCAN XC-72, Asahi Carbon Co., Ltd. # 80, # 60, # 55. , # 50, # 35, Mitsubishi Chemical Industries # 2400B, # 2300, # 900, # 1000, # 30, # 40, # 10B, Colombian Carbon Corporation CONDUCTEX SC, RAVEN150, 50, 40, 15, RAVEN -MT-P, Ketchen Black EC manufactured by Japan EC Co., etc. Carbon black may be surface-treated with a dispersant, or may be used after being grafted with a resin, or may be obtained by graphitizing a part of the surface. Carbon black may be dispersed with a binder in advance before being added to the magnetic coating. These carbon blacks can be used alone or in combination. When using carbon black, it is preferable to use 0.1-30 mass% with respect to the mass of a magnetic body. Carbon black functions to prevent the magnetic layer from being charged, reduce the coefficient of friction, impart light-shielding properties, and improve the film strength. These differ depending on the carbon black used. Therefore, these carbon blacks used in the present invention have different types, amounts, and combinations in the magnetic layer and the nonmagnetic layer, and are based on the above-mentioned characteristics such as particle size, oil absorption, conductivity, pH, etc. Of course, it is possible to use them properly according to the purpose, but rather they should be optimized in each layer. For the carbon black that can be used in the magnetic layer of the present invention, for example, “Carbon Black Handbook” edited by Carbon Black Association can be referred to.

  Known organic solvents can be used in the present invention. The organic solvent used in the present invention is an arbitrary ratio of ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, diisobutyl ketone, cyclohexanone, isophorone, tetrahydrofuran, methanol, ethanol, propanol, butanol, isobutyl alcohol, isopropyl alcohol, methyl Alcohols such as cyclohexanol, esters such as methyl acetate, butyl acetate, isobutyl acetate, isopropyl acetate, ethyl lactate, glycol acetate, glycol ethers such as glycol dimethyl ether, glycol monoethyl ether, dioxane, benzene, toluene, xylene, Aromatic hydrocarbons such as cresol and chlorobenzene, methylene chloride, ethylene chloride, carbon tetrachloride, chloroform, ethyl Nkuroruhidorin, chlorinated hydrocarbons such as dichlorobenzene, N, N- dimethylformamide, may be used hexane.

  These organic solvents are not necessarily 100% pure, and may contain impurities such as isomers, unreacted materials, side reaction products, decomposition products, oxides, and moisture in addition to the main components. These impurities are preferably 30% or less, more preferably 10% or less. The organic solvent used in the present invention is preferably the same in the magnetic layer and the nonmagnetic layer. The amount added may be changed. Use non-magnetic layers with high surface tension solvents (cyclohexanone, dioxane, etc.) to increase coating stability. Specifically, the arithmetic average value of the upper layer solvent composition may not fall below the arithmetic average value of the nonmagnetic layer solvent composition. It is essential. In order to improve dispersibility, it is preferable that the polarity is somewhat strong, and it is preferable that 50% or more of a solvent having a dielectric constant of 15 or more is included in the solvent composition. Moreover, it is preferable that a solubility parameter is 8-11.

  These dispersants, lubricants, and surfactants used in the present invention can be properly used in the magnetic layer and further in the nonmagnetic layer described later as needed. For example, of course, the dispersant is not limited to the example shown here, but the dispersant has a property of adsorbing or binding with a polar group, and in the magnetic layer, mainly on the surface of the ferromagnetic metal powder and nonmagnetic. In the layer, it is presumed that the organic phosphorus compound adsorbed or bonded mainly to the surface of the non-magnetic powder with the polar group, for example, is difficult to desorb from the surface of the metal or metal compound. Accordingly, the surface of the ferromagnetic metal powder or the nonmagnetic powder of the present invention is in a state of being coated with an alkyl group, an aromatic group, etc., so that the binder resin component of the ferromagnetic metal powder or nonmagnetic powder is used. The affinity is improved and the dispersion stability of the ferromagnetic metal powder or nonmagnetic powder is also improved. In addition, since the lubricant exists in a free state, fatty acids with different melting points are used in the nonmagnetic layer and magnetic layer to control the bleeding to the surface, and leaching to the surface using esters with different boiling points and polarities. It is conceivable to improve the coating stability by controlling the amount of the surfactant, to improve the lubrication effect by increasing the additive amount of the lubricant in the nonmagnetic layer. All or part of the additives used in the present invention may be added in any step during the production of the coating solution for the magnetic layer or nonmagnetic layer. For example, when mixing with a ferromagnetic powder before the kneading step, when adding at a kneading step with a ferromagnetic powder, a binder and a solvent, when adding at a dispersing step, when adding after dispersing, when adding just before coating, etc. There is.

[Nonmagnetic layer]
Next, detailed contents regarding the nonmagnetic layer will be described. The magnetic recording medium of the present invention can have a nonmagnetic layer containing a binder and a nonmagnetic powder on a support. The nonmagnetic powder that can be used in the nonmagnetic layer may be an inorganic substance or an organic substance. Carbon black or the like can also be used. Examples of the inorganic substance include metals, metal oxides, metal carbonates, metal sulfates, metal nitrides, metal carbides, and metal sulfides.

Specifically, titanium oxide such as titanium dioxide, cerium oxide, tin oxide, tungsten oxide, ZnO, ZrO ₂ , SiO ₂ , Cr ₂ O ₃ , α-alumina, β-alumina having an α conversion of 90 to 100%, γ-alumina, α-iron oxide, goethite, corundum, silicon nitride, titanium carbide, magnesium oxide, boron nitride, molybdenum disulfide, copper oxide, MgCO ₃ , CaCO ₃ , BaCO ₃ , SrCO ₃ , BaSO ₄ , silicon carbide Titanium carbide or the like is used alone or in combination of two or more. Preferable are α-iron oxide and titanium oxide.

  The shape of the nonmagnetic powder may be any of acicular, spherical, polyhedral and plate shapes. The crystallite size of the nonmagnetic powder is preferably 4 nm to 1 μm, and more preferably 40 to 100 nm. A crystallite size in the range of 4 nm to 1 μm is preferred because it does not become difficult to disperse and has a suitable surface roughness. The average particle size of these non-magnetic powders is preferably 5 nm to 2 μm. However, if necessary, non-magnetic powders having different average particle sizes may be combined, or even a single non-magnetic powder may have a wide particle size distribution. It can also have an effect. The average particle size of the particularly preferred nonmagnetic powder is 10 to 200 nm. The range of 5 nm to 2 μm is preferable because the dispersion is good and the surface roughness is suitable.

The specific surface area of the nonmagnetic powder is 1 to 100 m ² / g, preferably 5 to 70 m ² / g, and more preferably 10 to 65 m ² / g. A specific surface area in the range of 1 to 100 m ² / g is preferred because it has a suitable surface roughness and can be dispersed with a desired amount of binder. The oil absorption using dibutyl phthalate (DBP) is 5 to 100 ml / 100 g, preferably 10 to 80 ml / 100 g, and more preferably 20 to 60 ml / 100 g. The specific gravity is 1 to 12, preferably 3 to 6. The tap density is 0.05 to 2 g / ml, preferably 0.2 to 1.5 g / ml. When the tap density is in the range of 0.05 to 2 g / ml, there are few particles to be scattered, the operation is easy, and there is a tendency that it is difficult to adhere to the apparatus. The pH of the nonmagnetic powder is preferably 2 to 11, but is particularly preferably between 6 and 9. When the pH is in the range of 2 to 11, the friction coefficient does not increase due to high temperature, high humidity, or liberation of fatty acids. The moisture content of the nonmagnetic powder is 0.1 to 5% by mass, preferably 0.2 to 3% by mass, and more preferably 0.3 to 1.5% by mass. A water content in the range of 0.1 to 5% by mass is preferable because the dispersion is good and the viscosity of the paint after dispersion is stable. The ignition loss is preferably 20% by mass or less, and the ignition loss is preferably small.

When the nonmagnetic powder is an inorganic powder, the Mohs hardness is preferably 4-10. If the Mohs hardness is in the range of 4 to 10, durability can be ensured. The nonmagnetic powder has a stearic acid adsorption amount of 1 to 20 μmol / m ² , more preferably ² to 15 μmol / m ² . The heat of wetting of the nonmagnetic powder into water at 25 ° C. is preferably in the range of 200 to 600 erg / cm ² (200 to 600 mJ / m ² ). Moreover, the solvent which exists in the range of this heat of wetting can be used. The amount of water molecules on the surface at 100 to 400 ° C. is suitably 1 to 10 / 100Å. The pH of the isoelectric point in water is preferably between 3 and 9. It is preferable that Al ₂ O ₃ , SiO ₂ , TiO ₂ , ZrO ₂ , SnO ₂ , Sb ₂ O ₃ and ZnO are present on the surface of these nonmagnetic powders by surface treatment. Particularly preferred for dispersibility are Al ₂ O ₃ , SiO ₂ , TiO ₂ , and ZrO ₂ , but more preferred are Al ₂ O ₃ , SiO ₂ , and ZrO ₂ . These may be used in combination or may be used alone. Further, a surface-treated layer co-precipitated according to the purpose may be used, or a method of treating the surface layer with silica after first treating with alumina, or vice versa may be employed. The surface treatment layer may be a porous layer depending on the purpose, but it is generally preferable that the surface treatment layer is homogeneous and dense.

  Specific examples of the non-magnetic powder used in the non-magnetic layer of the present invention include, for example, Showa Denko Nanotite, Sumitomo Chemical HIT-100, ZA-G1, Toda Kogyo DPN-250, DPN-250BX, DPN-245, DPN-270BX, DPB-550BX, DPN-550RX, Ishihara Sangyo Titanium oxide TTO-51B, TTO-55A, TTO-55B, TTO-55C, TTO-55S, TTO-55D, SN-100, MJ -7, α-iron oxide E270, E271, E300, STT-4D, STT-30D, STT-30, STT-65C manufactured by Titanium Industry, MT-100S, MT-100T, MT-150W, MT-500B manufactured by Teika T-600B, T-100F, T-500HD, etc. are mentioned. FINEX-25, BF-1, BF-10, BF-20, ST-M, Dowa Mining DEFIC-Y, DEFIC-R, Nippon Aerosil AS2BM, TiO2P25, Ube Industries 100A, 500A, Titanium Industry Y-LOP manufactured and what baked it are mentioned. Particularly preferred nonmagnetic powders are titanium dioxide and α-iron oxide.

Carbon black can be mixed in the nonmagnetic layer together with nonmagnetic powder to lower the surface electrical resistance, reduce the light transmittance, and obtain a desired micro Vickers hardness. The micro-Vickers hardness of the nonmagnetic layer is generally 25~60kg / mm ² (245~588MPa), preferably in order to adjust the head contact, a 30~50kg / mm ² (294~490MPa), thin film hardness meter ( Using a HMA-400 manufactured by NEC, measurement can be performed using a diamond triangular pyramid needle having a ridge angle of 80 degrees and a tip radius of 0.1 μm at the tip of the indenter. It is standardized that the light transmittance is generally 3% or less for absorption of infrared rays having a wavelength of about 900 nm, for example, 0.8% or less for a VHS magnetic tape. For this purpose, rubber furnace, rubber thermal, color black, acetylene black and the like can be used.

Non specific surface area of the carbon black used in the magnetic layer is 100 to 500 m ² / g, preferably 150~400m ² / g, DBP oil absorption of the present invention are 20 to 400 ml / 100 g, preferably 30 to 200 ml / 100 g . The particle size of carbon black is 5 to 80 nm, preferably 10 to 50 nm, and more preferably 10 to 40 nm. Carbon black preferably has a pH of 2 to 10, a water content of 0.1 to 10%, and a tap density of 0.1 to 1 g / ml.

  Specific examples of carbon black that can be used in the non-magnetic layer of the present invention include BLACKPEARLS 2000, 1300, 1000, 900, 800, 880, 700, VULCAN XC-72, manufactured by Mitsubishi Kasei Kogyo Co., Ltd. 3050B, # 3150B, # 3250B, # 3750B, # 3950B, # 950, # 650B, # 970B, # 850B, MA-600, Columbia Carbon's CONDUCTEX SC, RAVEN8800, 8000, 7000, 5750, 5250, 3500, 2100 2000, 1800, 1500, 1255, 1250, Ketjen Black EC manufactured by Akzo Corporation, and the like.

  Carbon black may be surface-treated with a dispersant, or may be grafted with a resin, or may be obtained by graphitizing a part of the surface. Moreover, before adding carbon black to a coating material, you may disperse | distribute with a binder beforehand. These carbon blacks can be used in a range not exceeding 50% by mass with respect to the inorganic powder and in a range not exceeding 40% of the total mass of the nonmagnetic layer. These carbon blacks can be used alone or in combination. The carbon black that can be used in the nonmagnetic layer of the present invention can be referred to, for example, “Carbon Black Handbook” edited by Carbon Black Association.

  Further, an organic powder can be added to the nonmagnetic layer according to the purpose. Examples of such organic powder include acrylic styrene resin powder, benzoguanamine resin powder, melamine resin powder, and phthalocyanine pigment, but polyolefin resin powder, polyester resin powder, polyamide resin powder, polyimide resin, and the like. Resin powder and polyfluorinated ethylene resin can also be used. As the production method, those described in JP-A Nos. 62-18564 and 60-255827 can be used.

  As the binder resin, lubricant, dispersant, additive, solvent, dispersion method and the like of the nonmagnetic layer, those of the magnetic layer can be applied. In particular, with respect to the binder resin amount, type, additive, and dispersant addition amount and type, known techniques relating to the magnetic layer can be applied.

  The magnetic recording medium of the present invention may be provided with an undercoat layer. By providing the undercoat layer, the adhesive force between the support and the magnetic layer or the nonmagnetic layer can be improved. As the undercoat layer, a polyester resin that is soluble in a solvent is used.

[Layer structure]
In the thickness structure of the magnetic recording medium used in the present invention, the preferable thickness of the support is 3 to 80 μm. When an undercoat layer is provided between the support and the nonmagnetic layer or the magnetic layer, the thickness of the undercoat layer is 0.01 to 0.8 μm, preferably 0.02 to 0.6 μm.

  The thickness of the magnetic layer is optimized depending on the saturation magnetization amount, head gap length, and recording signal band of the magnetic head to be used, but is generally 10 to 150 nm, preferably 20 to 120 nm, and more preferably. Is 30 to 100 nm, particularly preferably 30 to 80 nm. Further, the thickness variation rate of the magnetic layer is preferably within ± 50%, and more preferably within ± 40%. There may be at least one magnetic layer, and the magnetic layer may be separated into two or more layers having different magnetic characteristics, and a configuration related to a known multilayer magnetic layer can be applied.

  The thickness of the nonmagnetic layer of the present invention is 0.5 to 2.0 μm, preferably 0.8 to 1.5 μm, and more preferably 0.8 to 1.2 μm. The non-magnetic layer of the magnetic recording medium of the present invention exhibits its effect if it is substantially non-magnetic. For example, even if it contains a small amount of magnetic material as an impurity or intentionally, This shows the effect of the invention and can be regarded as substantially the same configuration as the magnetic recording medium of the invention. Note that “substantially the same” means that the residual magnetic flux density of the nonmagnetic layer is 10 mT or less or the coercive force is 7.96 kA / m (100 Oe) or less, and preferably has no residual magnetic flux density and coercive force. Means.

[Production method]
The step of producing the magnetic layer coating liquid for the magnetic recording medium used in the present invention comprises at least a kneading step, a dispersing step, and a mixing step provided before and after these steps. Each process may be divided into two or more stages. All raw materials such as ferromagnetic metal powder, non-magnetic powder, binder, carbon black, abrasive, antistatic agent, lubricant, and solvent used in the present invention may be added at the beginning or middle of any step. In addition, individual raw materials may be added in two or more steps. For example, polyurethane may be divided and added in a kneading step, a dispersing step, and a mixing step for adjusting the viscosity after dispersion. In order to achieve the object of the present invention, a conventional known manufacturing technique can be used as a partial process. In the kneading step, it is preferable to use a kneading force such as an open kneader, a continuous kneader, a pressure kneader, or an extruder. When using a kneader, magnetic powder or non-magnetic powder and all or a part of the binder (however, preferably 30% or more of the total binder) and 100 parts by mass of the magnetic material are kneaded in the range of 15 to 500 parts by mass. It is processed. Details of these kneading treatments are described in JP-A-1-106338 and JP-A-1-79274. Further, glass beads can be used to disperse the magnetic layer solution and the nonmagnetic layer solution. Such glass beads are preferably zirconia beads, titania beads, and steel beads, which are high specific gravity dispersion media. The particle diameter and filling rate of these dispersion media are optimized. A well-known thing can be used for a disperser.

  In the method for producing a magnetic recording medium of the present invention, for example, a magnetic layer is applied to the surface of a support under running so as to have a predetermined film thickness. Here, a plurality of magnetic layer coating solutions may be applied sequentially or simultaneously, and a nonmagnetic layer coating solution and a magnetic layer coating solution may be applied sequentially or simultaneously. The coating machine for applying the above magnetic coating solution or non-magnetic layer coating solution includes air doctor coat, blade coat, rod coat, extrusion coat, air knife coat, squeeze coat, impregnation coat, reverse roll coat, transfer roll coat, gravure coat Kiss coat, cast coat, spray coat, spin coat, etc. can be used. As for these, for example, “Latest Coating Technology” (May 31, 1983) issued by General Technology Center Co., Ltd. can be referred to.

  In the case of a magnetic tape, the magnetic layer coating solution is subjected to magnetic field orientation treatment in the longitudinal direction using a cobalt magnet or a solenoid on the ferromagnetic metal powder contained in the magnetic layer coating solution. In the case of a disk, a sufficiently isotropic orientation may be obtained even without non-orientation without using an orientation device, but known random methods such as alternately arranging cobalt magnets obliquely and applying an alternating magnetic field with a solenoid. It is preferable to use an alignment device. In the case of a ferromagnetic metal powder, the isotropic orientation is generally preferably in-plane two-dimensional random, but can also be three-dimensional random with a vertical component. Further, isotropic magnetic characteristics can be imparted in the circumferential direction by using a well-known method such as a counter-polarized magnet and making it vertically oriented. In particular, when performing high density recording, vertical alignment is preferable. Moreover, circumferential orientation can also be achieved using spin coating.

  It is preferable that the drying position of the coating film can be controlled by controlling the temperature, air volume, and coating speed of the drying air, the coating speed is preferably 20 m / min to 1000 m / min, and the temperature of the drying air is preferably 60 ° C. or higher. Also, moderate pre-drying can be performed before entering the magnet zone.

After drying, the coating layer is usually subjected to a surface smoothing treatment. For the surface smoothing process, for example, a super calendar roll or the like is used. By performing the surface smoothing treatment, voids generated by the removal of the solvent during drying disappear and the filling rate of the ferromagnetic metal powder in the magnetic layer is improved, so that a magnetic recording medium having high electromagnetic conversion characteristics can be obtained. Can do. As the calendering roll, a heat-resistant plastic roll such as epoxy, polyimide, polyamide, polyamideimide or the like is used. Moreover, it can also process with a metal roll.
The magnetic recording medium of the present invention has a surface having extremely excellent smoothness with a center surface average roughness of 0.1 to 4 nm, preferably 1 to 3 nm at a cutoff value of 0.25 mm. preferable. As the method, for example, as described above, a magnetic layer formed by selecting a specific ferromagnetic metal powder and a binder is subjected to the calendar treatment. As calendering conditions, the temperature of the calendar roll is in the range of 60 to 100 ° C., preferably in the range of 70 to 100 ° C., particularly preferably in the range of 80 to 100 ° C., and the pressure is 100 to 500 kg / cm (98 to 490 kN). / M), preferably 200 to 450 kg / cm (196 to 441 kN / m), particularly preferably 300 to 400 kg / cm (294 to 392 kN / m). Is preferably carried out by

  The obtained magnetic recording medium can be cut into a desired size using a cutting machine or the like. The cutting machine is not particularly limited, but is preferably provided with a plurality of pairs of rotating upper blades (male blades) and lower blades (female blades). The slitting speed, the meshing depth, and the upper blade (male blade) are appropriately selected. The peripheral speed ratio (upper blade peripheral speed / lower blade peripheral speed) of the blade and the lower blade (female blade), the continuous use time of the slit blade, and the like are selected.

[Physical properties]
The saturation magnetic flux density of the magnetic layer of the magnetic recording medium used in the present invention is preferably 100 to 300 mT. The coercive force (Hr) of the magnetic layer is preferably 143.3 to 318.4 kA / m (1800 to 4000 Oe), more preferably 159.2 to 278.6 kA / m (2000 to 3500 Oe). The coercive force distribution is preferably narrow, and SFD and SFDr are 0.6 or less, more preferably 0.2 or less.

The friction coefficient with respect to the head of the magnetic recording medium used in the present invention is 0.50 or less, preferably 0.3 or less in the range of temperature -10 to 40 ° C. and humidity 0 to 95%. The surface resistivity is preferably 10 ⁴ to 10 ¹² Ω / sq of the magnetic surface, and the charging position is preferably within −500 V to +500 V. The elastic modulus at 0.5% elongation of the magnetic layer is preferably 0.98 to 19.6 GPa (100 to 2000 kg / mm ² ) in each in-plane direction, and the breaking strength is preferably 98 to 686 MPa (10 to 70 kg). / Mm ² ), the elastic modulus of the magnetic recording medium is preferably 0.98 to 14.7 GPa (100 to 1500 kg / mm ² ) in each in-plane direction, and the residual spread is preferably 0.5% or less, 100 ° C. The thermal shrinkage at any of the following temperatures is preferably 1% or less, more preferably 0.5% or less, and most preferably 0.1% or less.

The glass transition temperature of the magnetic layer (maximum point of loss elastic modulus measured by dynamic viscoelasticity measured at 110 Hz) is preferably 50 to 180 ° C, and that of the nonmagnetic layer is preferably 0 to 180 ° C. The loss elastic modulus is preferably in the range of 1 × 10 ⁷ to 8 × 10 ⁸ Pa (1 × 10 ⁸ to 8 × 10 ⁹ dyne / cm ² ), and the loss tangent is preferably 0.2 or less. If the loss tangent is too large, adhesion failure is likely to occur. These thermal characteristics and mechanical characteristics are preferably almost equal within 10% in each in-plane direction of the medium.

The residual solvent contained in the magnetic layer is preferably 100 mg / m ² or less, more preferably 10 mg / m ² or less. The porosity of the coating layer is preferably 30% by volume or less, more preferably 20% by volume or less for both the nonmagnetic layer and the magnetic layer. The porosity is preferably small in order to achieve high output, but it may be better to ensure a certain value depending on the purpose. For example, in the case of a disk medium in which repeated use is important, a larger void ratio is often preferable for running durability.

The maximum height SR _max of the magnetic layer is 0.5 μm or less, the ten-point average roughness SRz is 0.3 μm or less, the center plane peak height SRp is 0.3 μm or less, and the center plane valley depth SRv is 0.3 μm or less. The center surface area ratio SSr is preferably 20 to 80%, and the average wavelength Sλa is preferably 5 to 300 μm. These can be easily controlled by controlling the surface properties with the filler of the support or the surface of the calendered roll. The curl is preferably within ± 3 mm.

  When the magnetic recording medium of the present invention is composed of a nonmagnetic layer and a magnetic layer, these physical characteristics can be changed between the nonmagnetic layer and the magnetic layer according to the purpose. For example, the elastic modulus of the magnetic layer can be increased to improve running durability, and at the same time, the elastic modulus of the nonmagnetic layer can be made lower than that of the magnetic layer to improve the contact of the magnetic recording medium with the head.

According to the present invention, the magnetic recording medium obtained as described above is analyzed for ATR-FT-IR, for example, to analyze a fatty acid metal salt formed by reacting with a ferromagnetic metal powder of a magnetic layer. Can do. As mentioned above, fatty acid metal salts such as calcium salts of fatty acids form protrusions on the surface of the magnetic layer and degrade the electromagnetic conversion characteristics by spacing, and adhere to the head by running, or dropout and error rate degradation Cause deterioration of running durability and electromagnetic conversion characteristics. Therefore, in the present invention, for example, the conditions under which a fatty acid metal salt is rapidly generated are forcibly created, and after placing the obtained magnetic recording medium, the amount of the fatty acid metal salt is analyzed, and the fatty acid metal salt is analyzed. If the salt formation exceeds a certain value, the type and amount of components of the magnetic layer can be reset appropriately, or the fatty acid metal salt can be wiped off by the wiping process to improve running durability and electromagnetic conversion characteristics. Deterioration can be prevented in advance.
Therefore, in the method for producing a magnetic recording medium of the present invention, the step of analyzing the organic compound adsorbed or reacting with the ferromagnetic powder on the surface of the coating layer may be performed after any step of the step of producing the magnetic recording medium. However, it is preferred that an ATR-FT-IR measurement at least after the final stage is included. In the ATR-FT-IR measurement at the final stage, when the amount of fatty acid metal salt set is exceeded, it is excluded from product shipment and the composition and processing conditions of the magnetic recording medium in each manufacturing process are reviewed. Thus, a magnetic recording medium having a constant quality can always be manufactured.
The index of the amount of fatty acid metal salt on the magnetic layer surface determined by ATR-FT-IR is 0.01 or less, preferably 0.007 or less, more preferably 0.004 or less.
In the present invention, examples of means for controlling the amount of the fatty acid metal salt include, but are not limited to, the following means.
(1) To reduce the amount of salt-forming atoms such as Y contained in the ferromagnetic metal powder.
(2) Reduce vinyl chloride resin and suppress fatty acid generation from hydrolysis from fatty acid esters. Also, reduce the amount of hydrolyzable fatty acid ester used.
(3) To reduce the amount of fatty acid used.
(4) Use a surface treating agent for ferromagnetic powder such as phenylphosphonic acid.
(5) The tape surface is wiped off by a magnetic tape surface treatment such as wiping.

EXAMPLES Hereinafter, although an Example demonstrates this invention, this invention is not limited to the following example.
In addition, the display of "part" in an Example shows "mass part".

(Example 1)
Magnetic layer composition 100 parts of ferromagnetic metal powder (shown in Table 1) was pulverized with an open kneader for 10 minutes, then vinyl chloride resin (MR-110 manufactured by Nippon Zeon Co., Ltd.) 10 parts polyurethane (UR-8300 manufactured by Toyobo Co., Ltd.) 6 parts ( Solids)
40 parts of methyl ethyl ketone / cyclohexanone = 1/1 were added and kneaded for 60 minutes.
Then
α-Al ₂ O ₃ (average particle size 0.2 μm) 10 parts Carbon black (average particle size 80 nm) 2 parts Methyl ethyl ketone / cyclohexanone = 1/200 parts were added and dispersed in a sand mill for 120 minutes.
4 parts of polyisocyanate (solid content)
(Japan Polyurethane Coronate 3041)
Stearic acid (described in Table 1)
Fatty acid ester (described in Table 1) 1 part Toluene 50 parts was added and stirred and mixed for 20 minutes.
Then, it filtered using the filter which has an average hole diameter of 1 micrometer, and prepared the magnetic coating material.

Nonmagnetic layer composition The following components were each kneaded with a kneader and then dispersed using a sand mill. To the obtained dispersion, 3 parts of polyisocyanate (Coronate L manufactured by Nippon Polyurethane Co., Ltd.) is added, 40 parts of methyl ethyl ketone and cyclohexanone mixed solution are added, and the mixture is filtered using a filter having an average pore size of 1 μm, and a nonmagnetic layer A forming coating solution was prepared.
Nonmagnetic powder αFe ₂ O ₃ hematite 80 parts Average long axis length: 0.15μm
Specific surface area by BET method: 58m ² / g
Average needle ratio: 7.5
Carbon black (Mitsubishi Carbon Co., Ltd.) 20 parts Average primary particle size: 16nm
DBP oil absorption: 80ml / 100g
pH: 8.0
Specific surface area by BET method: 250m ² / g
Volatile content: 1.5%
12 parts of vinyl chloride copolymer MR-110 made by Nippon Zeon
Polyester polyurethane resin 12 parts Toyobo UR-8200
Stearic acid 2 parts Methyl ethyl ketone 150 parts Cyclohexane 50 parts Toluene 50 parts

Polyethylene terephthalate (PET) support having a thickness of 10 μm so that the thickness after drying of the obtained magnetic coating is 0.1 μm and the thickness after drying of the non-magnetic coating is 1.5 μm The surface is coated with an extrusion coating head, the magnetic coating is undried, magnetic field orientation is performed with a 300 mT (3000 gauss) magnet, and the following back solution is dried to a thickness of 0.5 μm. The coating was dried so that Thereafter, a five-step calendering process (speed 100 m / min, linear pressure 294 kN / m (300 kg / cm), temperature 90 ° C.) using a combination of a metal roll and a heat-resistant plastic roll was performed.
Thereafter, it was slit to a width of ½ mm to produce a magnetic tape.

(Back liquid composition)
Carbon black (particle size 18 nm) 100 parts Nitrocellulose (HIG1 / 2 manufactured by Asahi Kasei Co., Ltd.) 60 parts Polyurethane (UR-8300 manufactured by Toyobo Co., Ltd.) 60 parts Polyisocyanate (Coronate L manufactured by Nippon Polyurethane Co., Ltd.) 20 parts Methyl ethyl ketone 1000 parts Toluene 1000 parts

(Examples 2 to 10)
Change the type of ferromagnetic metal powder, the amount of stearic acid, and the type of higher fatty acid ester as shown in Table 1 below, or set the storage conditions for the magnetic tape of Example 1 or 2 as shown in Table 1 below. A magnetic tape was produced in the same manner as in Example 1 except that the production of the fatty acid metal salt was promoted.

(Example 11)
The tape of Example 6 after production was subjected to wiping using a raised polyester cloth.

(Quantification of fatty acid metal salts present on the surface of the magnetic layer)
Place 3 cm of magnetic tape in a Bayer bottle, 10 ml of n-hexane to remove unadsorbed fatty acids not forming metal salt, and 0 TMSI-H agent from GL Sciences for derivatization treatment. .3 ml was added, and derivatization reaction was performed by heating at 60 ° C. for 1 hour. The reacted magnetic tape was removed and rinsed well with ethanol to obtain a control sample. The ATR-FT-IR of this control sample was measured. Separately from this, ATR-FT-IR of a sample which is the same magnetic tape as described above was measured. Obtain the difference between the absorbance at wavenumber (1550 cm ⁻¹ ) corresponding to the absorption of carboxylate and the absorbance at 1630 cm ⁻¹ without absorption, and use it as the absorbance of the sample. Was used as an indicator of the amount of fatty acid metal salt. For comparison, the surface of the magnetic layer before and after the derivatization treatment was measured by AES.

ATR-FT-IR is measured using Thermo-Nicolet, product name Nexus 670, with a single reflection horizontal ATR accessory, incident angle 60 °, resolution 1 cm ⁻¹ , 200 times integration. It was.
For the AES measurement, a product name μ-AES PHI660 manufactured by ULVAC-PHI was used to determine the strength of Fe and C, and the ratio (ΔC / Fe) was calculated.

Measurement of friction coefficient To contact the magnetic tape and stainless steel pole (SUS420J) with 50g tension (T1) (wrapping angle 180 °) and run the magnetic tape at a speed of 3.0cm / sec under this condition. The required tension (T2) was measured. The measurement was performed in an environment of 23 ° C. and 70% RH, and the measured value of the first pass was adopted. The measurement at the 100th pass was also performed.
Based on this measured value, the friction coefficient (μ) of the magnetic tape was obtained by the following formula.
μ = (1 / π) × ln (T2 / T1)

Evaluation of head contamination Using a digital beta cam VTR DVW-A500 model manufactured by Sony Corporation, a 732m long magnetic tape was run at 20 ° C in a 50% RH environment, running 1 volume 2 passes continuously 25 volumes. The state of head contamination was evaluated from the following viewpoints.
No dirt: ◎, dirt somewhat: ◯, dirt: △, dirt in head gap: x
The results are shown in Table 2.

From Table 2, the amount of fatty acid metal salt by ATR-FT-IR and the value of fatty acid metal salt by AES are well correlated. By measuring ATR-FT-IR, the surface of the magnetic layer can be measured easily and accurately. It was found that fatty acid metal salts can be evaluated.
Further, from Table 2, it was confirmed that the greater the amount of fatty acid metal salt, the higher the coefficient of friction and the more dirty the head after running. This is presumably because the fatty acid metal salt formed on the surface of the magnetic layer increases the coefficient of friction and causes head contamination.
In addition, the amount of fatty acid metal salt on the surface of the magnetic layer of the magnetic recording medium is 0.01 or less, more preferably 0.007 or less, and more preferably 0. It turns out that it is 004 or less.

Claims (5)

  In a method for analyzing an organic compound adsorbed or reacted on an inorganic powder on the surface of a coating layer of a coating type magnetic recording medium provided with a coating layer containing at least an inorganic powder and a binder on a support, Fourier transform is performed. Using an infrared spectrophotometer (FT-IR), the total reflection absorption (ATR) spectrum of the coating layer surface including the absorption wave number specific to the organic compound to be analyzed is measured, and the inorganic powder on the coating layer surface An organic compound analysis method, comprising: analyzing an organic compound adsorbed or reacted on the organic compound.   In a method for manufacturing a magnetic recording medium, wherein a coating layer containing at least a ferromagnetic powder and a binder is provided on a support, a Fourier transform infrared spectrophotometer (FT-IR) is used to convert an organic compound to be analyzed. Measuring the total reflection absorption (ATR) spectrum of the coating layer surface including a specific absorption wave number, and analyzing an organic compound adsorbed or reacting with the ferromagnetic powder on the coating layer surface. A method of manufacturing a magnetic recording medium.   The method for producing a magnetic recording medium according to claim 2, wherein the organic compound to be analyzed is a fatty acid metal salt.   A magnetic recording medium manufactured by the method for manufacturing a magnetic recording medium according to claim 2.   The magnetic recording medium according to claim 4, wherein an index of the amount of the fatty acid metal salt is 0.01 or less.