Cr-si-n sintered compact, production method therefor, sputtering target, and production method for nitrogen-containing chromium silicide film

Abstract

A Cr-Si-N sintered compact according to the present invention contains chromium, silicon, and nitrogen. The Cr-Si-N sintered compact has a nitrogen content of 1-30 mass% and a silicon content of 20-60 mass%.

Description

Cr-Si-N sintered body, its manufacturing method, sputtering target, and method for manufacturing nitrogen-containing chromium silicide film

[0001] The present disclosure relates to a Cr—Si—N sintered body, a method for producing the same, a sputtering target, and a method for producing a nitrogen-containing chromium silicide film.

[0002] Chromium silicide (CrSi ２ Silicide materials, including silicides such as silicides (SiC, SiO2, SiO3, SiO4, SiO5, SiO6, SiO2, SiO2, SiO2, SiO3), are used as silicide films in semiconductors and solar cells due to their properties. Silicide materials are also used as resistive films in various sensors because their properties can be controlled to either semiconducting or metallic by controlling the crystal phase.

[0003] Sensors with silicide resistive films are used in environments where temperatures fluctuate from room temperature to approximately 150°C, such as in automobiles. To improve detection accuracy in environments where temperatures fluctuate, a silicide film with resistance characteristics that are independent of temperature changes is required.

[0004] For example, in Patent Documents 1 and 2, nitrogen gas is supplied to a CrSi target in addition to argon gas, and the nitrogen gas is used as a reactive gas to form a nitrogen-containing chromium silicide film on a substrate, thereby reducing the temperature coefficient of resistance (hereinafter also referred to as "TCR").

[0005] JP 2010-278479 A JP 2002-367803 A

[0006] However, when nitrogen gas is used as a reactive gas for film formation, the nitrogen gas does not uniformly hit the substrate, making it difficult to form a uniform film on the substrate, and making it difficult to obtain a film with a small TCR.

[0007] The present disclosure aims to provide at least one of a Cr-Si-N-based sintered body that contains chromium, silicon, and nitrogen and that can produce a nitrogen-containing chromium silicide film that has a small TCR and exhibits little change in TCR from room temperature to about 150°C without requiring a reactive gas (nitrogen gas) during film formation, a method for manufacturing the same, a sputtering target, and a method for manufacturing a nitrogen-containing chromium silicide film.

[0008] In this disclosure, we have focused on the composition of a Cr-Si-N sintered body containing chromium, silicon, and nitrogen, and the film obtained from the sintered body, and as a result, we have found a sintered body that, by controlling the nitrogen composition in the sintered body, enables the production of a nitrogen-containing chromium silicide film that has a small TCR and exhibits little change in TCR from room temperature to about 150°C.

[0009] That is, the present invention is as set forth in the claims, and the gist of the present disclosure is as follows. [1] A Cr-Si-N sintered body containing chromium, silicon, and nitrogen, with the nitrogen content being 1 mass % or more and 30 mass % or less and the silicon content being 20 mass % or more and 60 mass % or less. [2] The Cr-Si-N sintered body according to [1] above, containing chromium silicide and one or more selected from the group consisting of chromium nitride and silicon nitride. [3] CrSi, CrSi ２ , Cr ３ Si and Cr ５ Si ３ [4] The Cr-Si-N sintered body according to any one of [1] to [3], which contains at least one selected from the group consisting of: [1], [2], [3], [4], [5], [6], [7], [8], [9],

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[45] ３ Si and Cr ５ Si ３ [6] A method for producing a Cr—Si—N sintered body according to any one of [1] to [5] above, comprising the steps of: mixing an alloy powder of chromium and silicon with a nitrogen-containing compound source containing at least one of chromium and silicon and nitrogen to obtain a mixed powder; and heat-treating the mixed powder by pressurizing and sintering in a vacuum atmosphere. [7] A method for producing a Cr—Si—N sintered body according to [6], wherein the nitrogen-containing compound source is a nitride containing at least one of chromium and silicon. [8] A sputtering target comprising the Cr—Si—N sintered body according to any one of [1] to [5] above. [9] A method for producing a nitrogen-containing chromium silicide film using the Cr—Si—N sintered body according to any one of [1] to [5] above.

[0010] The present disclosure can provide at least one of a Cr-Si-N-based sintered body and a method for producing the same, which contains chromium, silicon, and nitrogen, and which is capable of producing a nitrogen-containing chromium silicide film that has a small TCR and exhibits little change in TCR from room temperature to about 150°C without requiring a reactive gas (nitrogen gas) during film formation.

[0011] 1 is a cross-sectional view showing a sputtering target according to the present disclosure, and FIG. 2 is a cross-sectional view showing an example of a film-coated substrate manufactured by the method for manufacturing a nitrogen-containing chromium silicide film according to the present disclosure.

[0012] The present disclosure will be described in detail below. However, the following description of the configuration requirements is an example of an embodiment of the present disclosure, and the present disclosure is not limited to these contents. Furthermore, the present disclosure includes any combination of the configurations and parameters disclosed in this specification, and also any combination of the upper and lower limits of the values ​​disclosed in this specification.

[0013] [Sintered body] The sintered body of this embodiment is a Cr-Si-N-based sintered body containing chromium, silicon, and nitrogen, characterized in that the nitrogen content is 1% by mass or more and 30% by mass or less, and the silicon content is 20% by mass or more and 60% by mass or less. The sintered body of this embodiment contains nitrogen and silicon in the above-mentioned amounts, so that a nitrogen-containing chromium silicide film having a small TCR and a small change in TCR from room temperature to about 150°C can be produced without requiring a reactive gas (nitrogen gas) during film formation using this sintered body. The sintered body of this embodiment can be used as a sputtering target (hereinafter simply referred to as "target") that can produce a nitrogen-containing chromium silicide film by sputtering.

[0014] This embodiment relates to a Cr—Si—N sintered body. In this embodiment, the Cr—Si—N sintered body refers to a sintered body containing chromium, silicon, and nitrogen as main components, or a sintered body essentially consisting of chromium, silicon, and nitrogen, or may be a sintered body consisting of chromium, silicon, and nitrogen.

[0015] The sintered body of this embodiment contains chromium, silicon, and nitrogen as elements, and has a composition in which the nitrogen content is 1% by mass or more and 30% by mass or less, and the silicon content is 20% by mass or more and 60% by mass or less. The TCR of a film obtained using a sintered body with a nitrogen content outside this range is high. From the viewpoint of reducing the TCR and minimizing the change in TCR, the nitrogen content is preferably 5% by mass or more and 30% by mass or less, more preferably 15% by mass or more and 30% by mass or less, and particularly preferably 20% by mass or more and 30% by mass or less. If the silicon content is less than 20% by mass, the resistivity of the film obtained using the sintered body will be low, while if the silicon content exceeds 60% by mass, the TCR will be high. The silicon content is preferably 30% by mass or more and 55% by mass or less, and more preferably 40% by mass or more and 50% by mass or less. The chromium content can be, for example, 20% by mass or more, 30% by mass or more, or 40% by mass or more, and can be, for example, 70% by mass or less, 60% by mass or less, or 50% by mass or less. Furthermore, the chromium content can be, for example, 20% by mass or more and 70% by mass or less, 30% by mass or more and 60% by mass or less, or 40% by mass or more and 50% by mass or less. The sintered body may contain nitrogen and silicon, with the remainder being chromium.

[0016] The silicon content in the sintered body of this embodiment is the mass ratio (mass %) of silicon to the mass of the sintered body obtained by mass measurement. The mass ratio of silicon contained in the sintered body of this embodiment may be measured by ICP analysis.

[0017] The nitrogen content in the sintered body of this embodiment is the mass ratio (mass %) of nitrogen to the mass of the sintered body. The mass ratio of nitrogen can be measured by a general method used in this technical field, for example, by a combustion-infrared absorption method using a general oxygen / nitrogen analyzer (e.g., a LECO-ON736 oxygen / nitrogen analyzer).

[0018] The chromium content in the sintered body of this embodiment can be determined by subtracting the mass percentage (mass%) of silicon and the mass percentage (mass%) of nitrogen from the mass percentage of the sintered body, assuming that the mass percentage of the sintered body is 100 mass%.

[0019] The chromium, silicon, and nitrogen contained in the sintered body of this embodiment may be in any form, and may be one or more selected from the group consisting of a compound containing at least two of chromium, silicon, and nitrogen, chromium (Cr), and silicon (Si). ２ N) and silicon nitride (Si ３ N ４ ) and chromium silicide, and more preferably chromium silicide and silicon nitride.

[0020] The chromium silicide contained in the sintered body of this embodiment is at least one selected from the group consisting of chromium monosilicide, disilicide, and trisilicide, and further includes CrSi, CrSi ２ , Cr ３ Si and Cr ５ Si ３ and one or more selected from the group consisting of CrSi, Cr ３ Si and Cr ５ Si ３ The sintered body of the present embodiment may contain two or more chromium silicides, such as CrSi, CrSi ２ , Cr ３ Si and Cr ５ Si ３ Preferably, the alloy contains two or more selected from the group consisting of CrSi, Cr ３ Si and Cr ５ Si ３ More preferably, the alloy contains two or more selected from the group consisting of CrSi and Cr ３ Si and Cr ５ Si ３ and more preferably, Cr ３ Si and Cr ５ Si ３ It is particularly preferred that the composition comprises:

[0021] In this embodiment, the crystalline phase contained in the sintered body such as chromium silicide can be identified from its powder X-ray diffraction (hereinafter also referred to as "XRD") pattern. The XRD pattern can be measured using a general XRD device (e.g., RINT Ultima III, manufactured by Rigaku Corporation). The XRD measurement conditions include the following: Acceleration current / voltage: 40 mA / 40 kV Radiation source: CuKα radiation (λ=1.5405 Å) Measurement mode: Continuous scan Scan condition: 2° / min Measurement range: 2θ=20° to 80° Divergence vertical limiting slit: 10 mm Divergence / entrance slit: 1 / 2° Receiving slit: 0.3 mm The crystalline phase of the sintered body can be identified by comparing the obtained XRD pattern with the database of the International Centre for Diffraction Data (ICDD).

[0022] The relative density of the sintered body of this embodiment is preferably 60% or more, and more preferably 70% or more or 80% or more. When the sintered body has such a relative density, cracking of the sintered body or sputtering target is further suppressed. The higher the relative density, the more preferable it is, but it can be 100% or less or less than 100%. The relative density is preferably 60% or more and 100% or less, or 70% or more and less than 100%.

[0023] In this embodiment, the "relative density" refers to the true density (d) [g / cm ３ ] to bulk density (d') [g / cm ３ ] is the proportion [%] of the bulk density d' [g / cm ３ ] is the volume [cm ] measured by Archimedes' method ３ ] and the mass (dry mass) [g] of the sintered body after drying in an air atmosphere at 60°C for 3 hours. The true density is a value calculated from the following formula: d = 1 / {(W １ / M １ ) + (W ２ / M ２ ) + (W ３ / M３ ) + (W ４ / M ４ ) + (W ５ / M ５ ) + (W ６ / M ６ ) + (W ７ / M ７ ) + (W ８ / M ８ )} × 100 In the above formula, d is the true density of the sintered body [g / cm ３ ] and M １ ~M ８ and W １ or W ８ are the amounts of Si, Cr, and Si contained in the sintered body, respectively. ３ N ４ , CrSi, CrSi ２ , Cr ３ Si, Cr ５ Si ３ and Cr ２ The true density of each crystal phase of N [g / cm ３ ], and the mass proportion [mass %] of each crystal phase in the sintered body.

[0024] The true density of each crystal phase may be the value described in the ICDD (Version 2.1502) for each crystal phase. The main true densities are as follows: Si 　　 : 2.33 g / cm ３ Cr 　　 : 7.20 g / cm ３ Si ３ N ４ : 3.19 g / cm ３ CrSi 　　 : 5.36 g / cm ３ CrSi ２　 : 4.98 g / cm ３ Cr ３ Si 　 : 6.46 g / cm ３ Cr ５ Si ３ : 5.87 g / cm ３ Cr ２ N 　 : 6.59 g / cm３ The ICDD numbers of each crystalline phase are 00-026-1481 for Si, 01-077-759 for Cr, and ３ N ４ 01-071-6479, CrSi is 03-065-3298, CrSi ２ 01-072-6184, Cr ３ Si is 01-070-301, Cr ５ Si ３ 01-072-0347 and Cr ２ N is 01-075-4942.

[0025] The mass ratio of each crystalline phase is the mass ratio [mass %] of each crystalline phase determined from the crystalline phase of the sintered body identified using the XRD pattern measured under the above-mentioned conditions and the ratio of the elements (Cr, Si, and N) constituting the sintered body. For example, when the crystalline phases included in the XRD pattern of the sintered body are CrSi, Cr ５ Si ３ and Si ３ N ４ When the composition of the sintered body obtained by composition analysis is X mol % of Cr, Y mol % of Si, and Z mol % of N, the mass percentage [mass %] obtained by multiplying the molar percentage [mol %] calculated by the following formula by the true density of each crystal phase is X=1×M ＣｒＳｉ + 5 x M Ｃｒ５Ｓｉ３ Y = 1 × M ＣｒＳｉ + 3 x M Ｃｒ５Ｓｉ３ + 3 x M Ｓｉ３Ｎ４ Z = 4 x M Ｓｉ３Ｎ４ In the above formula, M ＣｒＳｉ is the molar ratio of CrSi [mol%], M Ｃｒ５Ｓｉ３ is Cr ５ Si ３ The molar ratio [mol%] of M Ｓｉ３Ｎ４ is Si ３ N ４ is the molar ratio [mol %] of

[0026] Furthermore, for example, the true density of the sintered body of this embodiment containing three types of crystalline phases (for example, crystalline phases A, B, and C) can be calculated from the following formula: d = (a + b + c) / ((a / M ａ) + (b / M ｂ ) + (c / M ｃ )) or, d = 1 / ((R ａ / M ａ ) + (R ｂ / M ｂ ) + (R ｃ / M ｃ )) × 100 In the above formula, d is the true density of the sintered body [g / cm ３ ], a, b, and c are the masses [g] of the crystalline phases A, B, and C contained in the sintered body, respectively, and M ａ , M ｂ and M ｃ are the true densities [g / cm 3 ] of the crystalline phases A, B, and C contained in the sintered body, respectively. ３ ] and R ａ , R ｂ and R ｃ are the mass proportions [mass %] of the crystalline phases A, B, and C contained in the sintered body, respectively.

[0027] The sintered body of this embodiment may contain metal elements other than chromium and silicon (hereinafter also referred to as "metal impurities") as long as the effect is exhibited, and may be composed of chromium, silicon, nitrogen, and metal impurities. Examples of metal impurities include one or more metal elements selected from the group consisting of silicon (Si), aluminum (Al), and iron (Fe), or compounds thereof. The total amount of metal impurities may be 5000 ppm by mass or less, 1000 ppm by mass or less, or 500 ppm by mass or less. Examples of the total amount of metal impurities include 0 ppm by mass or more, more than 0 ppm by mass, or 100 ppm by mass or more. Examples of the total amount of metal impurities include 0 ppm by mass or more and 5000 ppm by mass or less, more than 0 ppm by mass to 1000 ppm by mass or less, or 100 ppm by mass or more and 1000 ppm by mass or less.

[0028] The amount of impurities in the sintered body of this embodiment is the mass ratio (ppm by mass) of the amount of impurities relative to the mass of the sintered body of this embodiment obtained by mass measurement. The amount of impurities contained in the sintered body of this embodiment may be measured by GDMS (Glow Discharge Mass Spectrometry) analysis.

[0029] Furthermore, the sintered body of this embodiment may contain oxygen (O) to the extent that the properties when used as a sputtering target are not deteriorated. The oxygen content is preferably 5000 ppm by mass or less. If the oxygen content is 5000 ppm by mass or less, particles derived from insulating oxides can be reduced. The oxygen content of the sintered body of this embodiment is preferably 1000 ppm by mass or less or 500 ppm by mass or less. Ideally, the sintered body of this embodiment does not contain oxygen (oxygen content is 0 ppm by mass), but realistic sintered bodies are thought to contain oxygen. Therefore, the lower limit of the oxygen content of the sintered body of this embodiment can be, for example, more than 0 ppm by mass or 100 ppm by mass or more, and is preferably 100 ppm by mass or more to 5000 ppm by mass or less, or 200 ppm by mass or more to 1000 ppm by mass or less.

[0030] For convenience, the composition of the sintered body of this embodiment is 100 mass % of chromium, silicon, and nitrogen. Therefore, when the sintered body contains at least one of metal impurities and oxygen, the composition of the sintered body of this embodiment may be a composition exceeding 100 mass %.

[0031] The oxygen content in the sintered body of this embodiment is the mass ratio (ppm by mass) of oxygen to the mass of the sintered body. The oxygen content in the sintered body of this embodiment can be measured by analysis using an inert gas fusion-infrared absorption method. A general oxygen / nitrogen analyzer (for example, a LECO-ON736 oxygen / nitrogen analyzer) can be used for the inert gas fusion-infrared absorption method.

[0032] The sintered body of this embodiment may have any shape depending on the purpose, and may have, for example, one or more shapes selected from the group consisting of disk, columnar, plate, rectangular parallelepiped, cubic, polyhedral, and approximately polyhedral. [Sputtering Target] The sintered body of this embodiment can be used for known applications of sintered bodies, particularly chromium silicide sintered bodies, but is preferably used as a sputtering target, and more preferably used as a sintered body for a sputtering target.

[0033] A sputtering target comprising the sintered body of this embodiment (hereinafter also referred to as "the target of this embodiment") may consist of the sintered body of this embodiment, or may be a target comprising a backing plate and the sintered body of this embodiment.

[0034] Hereinafter, the target of this embodiment will be described with reference to FIG. 1, taking as an example a sputtering target including a backing plate and the sintered body of this embodiment.

[0035] 1, the target 100 includes a sintered body 10 and a backing plate 20. The sintered body 10 is formed of the sintered body described above. The backing plate 20 may be made of any material that can conduct electricity and dissipate heat during sputtering, and examples thereof include backing plates made of one or more materials selected from the group consisting of copper (Cu), aluminum (Al), titanium (Ti), and SUS.

[0036] In the target 100 of this embodiment, the sintered body 10 of this embodiment is bonded to a backing plate 20. The sintered body 10 of this embodiment and the backing plate 20 may be bonded directly, or may be bonded via a bonding material 30 as shown in Fig. 1. The bonding material 30 may be a known material, for example, indium (In).

[0037] The shape of the target of this embodiment may be any shape suitable for sputtering, and may be, for example, one or more selected from the group consisting of a plate, a column, and a cylinder.

[0038] In order to increase the film formation area, the area of ​​the sputtering surface of the target in this embodiment is 200 cm ２ Above, 350cm ２ or above 800cm ２ The area of ​​the sputtering surface is preferably 1500 cm or more. ２ or less than 1200 cm ２ For example, it can be 200 cm or less. ２ More than 1500cm ２ Below, 350cm ２ More than 1200cm ２ It is preferable that:

[0039] [Method for producing sintered body] The sintered body of this embodiment may be produced by any method as long as it satisfies the above-mentioned requirements. A preferred production method is a method for producing a Cr-Si-N sintered body, which includes a step of mixing an alloy powder of chromium and silicon with a nitrogen-containing compound source containing at least one of chromium and silicon and nitrogen to obtain a mixed powder, and a heat treatment step of pressure-sintering the mixed powder in a vacuum atmosphere.

[0040] The mixed powder is obtained by a process (hereinafter also referred to as a "mixing process") of mixing an alloy powder of chromium and silicon (hereinafter also referred to as an "alloy powder") with a nitrogen-containing compound source containing at least one of chromium and silicon and nitrogen. The alloy powder is also obtained by a process (hereinafter also referred to as an "alloying process") of heating chromium powder and silicon powder to alloy them. The alloying method may be one or more methods selected from the group consisting of a melting method, a sintering method, a plating method, and a mechanical alloying method, with the melting method being preferred. Examples of the melting method include a quenched ribbon method, an arc melting method, a gas atomization method, a water atomization method, a centrifugal atomization method, and a vacuum atomization method.

[0041] The alloy powder preferably contains a powder obtained by gas atomization (hereinafter also referred to as "gas atomized powder"), and more preferably contains gas atomized powder of chromium and silicon. Powder obtained by gas atomization is composed of spherical particles of about several tens of micrometers, and the particles are composed of a fine crystalline phase. Since gas atomized powder is a powder with a small surface area and composed of fine particles, it can be used as an alloy powder that has a low oxygen content and can produce a sintered body with high strength.

[0042] The gas atomized powder may be, for example, a powder having an average particle size of 5 μm to 100 μm, or a powder having at least one of a spherical and a nearly spherical shape. Further, the gas atomized powder may be a powder composed of polycrystalline particles of chromium silicide, or a powder composed of particles containing polycrystalline chromium silicide of different crystal phases.

[0043] The alloy powder contains at least CrSi ２ In the crystal phase, Si, Cr, CrSi, and Cr ５ Si ３ and CrSi ２ It is more preferable that the crystal phase contains at least one of Si and CrSi, and CrSi ２ It is more preferable that the crystal phase contains

[0044] The conditions for the gas atomization method are arbitrary, but examples include a process temperature for melting chromium and silicon that is higher than the melting temperature. The process temperature is preferably 50°C to 300°C higher than the melting temperature, and more preferably 100°C to 250°C higher than the melting temperature. This results in a molten metal, i.e., a metal in a liquid state. Here, the "melting temperature" refers to the temperature at which precursor materials such as raw material powders or flakes of chromium and silicon melt, and is a value specific to each material. Examples of melting temperatures include 1300°C to 1500°C. Therefore, for example, if the melting temperature is 1400°C, the process temperature should be 1450°C to 1700°C. If the difference between the melting temperature and the process temperature is within the above range, gas atomized powder can be produced with high productivity.

[0045] In the gas atomization method, a precursor that can be used to obtain gas-atomized powder of chromium and silicon to be used as a raw material for the mixed powder is provided. The precursor may be at least one of chromium, silicon, a chromium compound, and a silicon compound, and may be powder, flake, or bulk of chromium and silicon, and is preferably chromium and silicon flake.

[0046] The chromium precursor is preferably high-purity chromium flakes, for example, chromium flakes having a purity of 3N or higher, or 4N or higher. The upper limit of the purity of the chromium flakes is 7N or lower, or 6N or lower.

[0047] The silicon precursor is preferably high-purity silicon flakes, for example, silicon flakes having a lower limit of silicon purity of 3N or more, 4N or more, or 5N or more. The upper limit of the purity of the silicon flakes is 7N or less, or 6N or less.

[0048] In the gas atomization method, the precursor is heated to the above-mentioned processing temperature so as to pass through a gas flow, and the molten metal obtained is dropped into the gas flow, thereby obtaining gas atomized powder.

[0049] The gas flow may be any inert gas, for example, one or more selected from the group consisting of argon, nitrogen and helium, and further argon.

[0050] The pressure of the gas flow (hereinafter also referred to as "gas pressure") may be 1 MPa or more, 4 MPa or more, or 6 MPa or more, and may be 10 MPa or less, or even 9 MPa or less. The gas pressure may be 1 MPa or more and 10 MPa or less, or 4 MPa or more and 9 MPa or less.

[0051] The gas atomization method may be at least one of a crucible type and an electrode type, and is preferably a crucible type. The crucible used in the crucible type gas atomization method is preferably a crucible made of one or more selected from the group consisting of carbon, alumina, magnesia, silicon nitride, zirconia, and boron nitride, or a crucible whose main body is made of one or more selected from the group consisting of carbon, alumina, magnesia, and zirconia and coated with at least one of boron nitride and silicon carbide.

[0052] The nitrogen-containing compound source may be any compound containing at least one of chromium and silicon and nitrogen, and is preferably a nitride of at least one of chromium and silicon, and more preferably at least one of chromium nitride and silicon nitride.

[0053] The starting materials to be subjected to the mixing step may include at least an alloy powder containing either chromium or silicon, and a nitrogen-containing compound source containing the other of silicon and chromium. Particularly preferred starting materials include gas-atomized powders of chromium and silicon, and nitrides of chromium and silicon.

[0054] The mixing method may be any method that can uniformly mix the starting materials, and a mixer such as a V-type mixer or a mixer may be used. The mixing method may be at least either dry mixing or wet mixing, with dry mixing being preferred, and dry mixing using a V-type mixer being more preferred.

[0055] The mixing atmosphere is preferably an atmosphere in which the mixed powder is unlikely to be oxidized, and examples thereof include at least one of a vacuum atmosphere and an inert atmosphere, and further at least one of a nitrogen atmosphere and an argon atmosphere, and further an argon atmosphere.

[0056] The mixing speed may be from 10 to 200 rpm, or from 50 to 100 rpm, and the mixing time may be from 30 minutes to 5 hours, or even from 45 minutes to 3 hours.

[0057] The purity of the mixed powder obtained by the mixing step is preferably 99% or more, and more preferably 99.9% or more. If the mixed powder does not contain many impurities, the impurities are less likely to cause abnormal grain growth, which is a source of particle generation during film formation using the sintered body, in the heat treatment step. The higher the purity of the mixed powder, the more preferable, but examples include a purity of 100% or less. The purity of the mixed powder is preferably 99% or more and 100% or less, or 99.9% or more and less than 100%. <Heat Treatment Step> In the heat treatment step, the mixed powder is pressure-sintered in a vacuum atmosphere. This produces the sintered body of this embodiment. The sintering method is pressure sintering, and specific examples of pressure sintering include one or more selected from the group consisting of hot pressing, hot isostatic pressing (HIP), and spark plasma sintering, with hot pressing being preferred.

[0058] The treatment temperature (heat treatment temperature) in the heat treatment step is preferably 1350°C or higher and 1800°C or lower. If the treatment temperature is 1350°C or higher, cracks in the sintered body are less likely to occur. If the treatment temperature is 1800°C or lower, melting of the sintered body can be suppressed. Furthermore, if the treatment temperature is within the above range, the density of the resulting sintered body is more likely to be improved. The treatment temperature is preferably 1375°C or higher or 1400°C or higher. The upper limit of the treatment temperature can be, for example, 1700°C or lower or 1600°C or lower, and is preferably 1375°C or higher and 1700°C or lower, or 1400°C or higher and 1600°C or lower.

[0059] The upper limit of the pressure for the pressure firing is, for example, 50 MPa or less or 40 MPa or less, and the lower limit is, for example, 10 MPa or more or 20 MPa or more, and 10 MPa or more and 50 MPa or less, or 20 MPa or more and 40 MPa or less is preferred.

[0060] The temperature increase rate and the temperature decrease rate are not particularly limited and can be appropriately determined in consideration of the volume of the firing furnace, the size and shape of the sintered body, etc. Examples of the temperature increase rate include 100°C / hour or more or 150°C / hour or more, and 300°C / hour or less or 250°C / hour or less.

[0061] The heat treatment time may be adjusted appropriately depending on the performance of the heat treatment furnace, and may be, for example, from 1 hour to 5 hours. The heat treatment time may further be set to 1.5 hours to 3.5 hours. Setting the heat treatment time to 1 hour or more suppresses temperature variations in the firing furnace and the hot press mold, making it easier to obtain a sintered body with a uniform structure. Setting the heat treatment time to 5 hours or less makes it easier to manufacture a sintered body with industrial productivity.

[0062] The atmosphere in the heat treatment step may be a vacuum atmosphere (also called a "vacuum reduced pressure atmosphere"). Firing in a vacuum atmosphere makes it easier to obtain a sintered body having a composition equivalent to that of the raw alloy powder. Here, "vacuum" refers to a pressure state of 1 atmosphere or less, and "vacuum atmosphere" refers to an atmosphere in which the pressure is 1 atmosphere or less.

[0063] [Film Formation Method] The target of this embodiment can be used in a method for producing a nitrogen-containing chromium silicide film using the target. The film is formed by a sputtering method. Specifically, the film (nitrogen-containing chromium silicide film) obtained from the target of this embodiment is a sputtered film, that is, a nitrogen-containing chromium silicide film deposited on a substrate. In other words, a substrate 201 having a nitrogen-containing chromium silicide film 202, a so-called film-coated substrate 200, can be produced by a sputtering method using the target of this embodiment (see FIG. 2).

[0064] Any film manufacturing method (film formation method) can be used, but examples include a film manufacturing method under the following conditions. This allows for the production of a film, further a thin film, or even a sputtered film. Magnetic field strength: 1000 Gauss (directly above the target, horizontal component) Substrate-target distance: 90 mm Substrate temperature: Room temperature (25°C) Introduced gas: Argon The sputtering method may be at least one selected from the group consisting of DC sputtering, RF sputtering, AC sputtering, DC magnetron sputtering, RF magnetron sputtering, and ion beam sputtering. In terms of being able to form a film uniformly and at high speed on a large-area substrate, the sputtering method is preferably DC magnetron sputtering or RF magnetron sputtering.

[0065] The power density in the sputtering method was 0.6 W / cm ２ or more than 1.0 W / cm ２ or more, and 10 W / cm ２ or less than 7.5 W / cm ２ For example, the power density is 0.6 W / cm or less. ２ At a power density of 10 W / cm or more, the film formation rate is increased and productivity is not likely to decrease. ２ If the power density is 0.6 W / cm or less, the load on the target is small and the occurrence of defects in the target during sputtering deposition is suppressed. ２ More than 10W / cm ２ Preferably, 1.0 W / cm or less２ More than 7.5W / cm ２ The following is more preferred:

[0066] The substrate used for sputtering deposition may be one or more selected from the group consisting of a glass substrate, a sapphire substrate and an alumina substrate, with a glass substrate being preferred.

[0067] It is preferable to heat-treat the film after deposition. Although the film after deposition is amorphous, heat-treating it is thought that the crystallinity in microregions, such as the generation of crystalline domains, changes. This can reduce the TCR of the nitrogen-containing chromium silicide film. The temperature of the heat treatment can be appropriately set depending on the composition of the nitrogen-containing chromium silicide film, and examples of the temperature include 800°C or less, or 700°C or less. Examples of the lower limit of the heat treatment temperature include 150°C or more, 200°C or more, 300°C or more, or 500°C or more. By setting the heat treatment temperature to 800°C or less, the production efficiency of the nitrogen-containing chromium silicide film is less likely to decrease. On the other hand, if the heat treatment temperature is 150°C or more, the TCR of the nitrogen-containing chromium silicide film is likely to decrease. Examples of the heat treatment temperature include 150°C or more and 800°C or less, or 200°C or more and 700°C or less.

[0068] The heat treatment time may be adjusted appropriately depending on the size and quantity of the films to be treated and the performance of the heat treatment furnace, and may be, for example, from 0.5 hours to 10 hours.

[0069] The heat treatment is preferably carried out in an oxygen-free atmosphere. The oxygen-free atmosphere is an atmosphere that does not contain oxygen, and specifically includes, for example, at least one selected from the group consisting of a vacuum atmosphere, an argon atmosphere, and a nitrogen atmosphere. A vacuum atmosphere is more preferable, and a vacuum atmosphere of 10 Pa or less is even more preferable.

[0070] The present disclosure will be described below with reference to examples. However, the present disclosure is not limited to these examples. (Relative Density) The relative density (%) of the sintered body was calculated in accordance with JIS R 1634, using the following formula, where the bulk density (d') of the sintered body is the ratio of the true density (d) of the sintered body to the bulk density (d') of the sintered body: Relative density [%] = (d' / d) × 100 Bulk density d' of sintered body [g / cm ３ ] is the volume [cm ] measured by Archimedes' method ３ The true density was calculated from the dry mass [g] of the sintered body after drying at 60°C for 3 hours. The true density was calculated from the following formula: d = 1 / {(W １ / M １ ) + (W ２ / M ２ ) + (W ３ / M ３ ) + (W ４ / M ４ ) + (W ５ / M ５ ) + (W ６ / M ６ ) + (W ７ / M ７ ) + (W ８ / M ８ )} × 100 In the above formula, d is the true density of the sintered body [g / cm ３ ] and M １ ~M ８ and W １ or W ８ are the amounts of Si, Cr, and Si contained in the sintered body, respectively. ３ N ４ , CrSi, CrSi ２ , Cr ３ Si, Cr ５ Si ３ and Cr ２ The true density of each crystal phase of N [g / cm ３ ], and the mass percentage [mass %] of each crystal phase in the sintered body. The true density of each crystal phase was the value described in the ICDD (Version 2.1502) for each crystal phase. Si 　　 : 2.33 g / cm ３ Cr 　　 : 7.20 g / cm ３ Si ３N ４ : 3.19 g / cm ３ CrSi 　　 : 5.36 g / cm ３ CrSi ２　 : 4.98 g / cm ３ Cr ３ Si 　 : 6.46 g / cm ３ Cr ５ Si ３ : 5.87 g / cm ３ Cr ２ N 　 : 6.59 g / cm ３ In addition, the true density d [g / cm 3 ] of the sintered body of the present embodiment in the three types of crystal phases (crystal phases A, B, and C) ３ ] is the mass of crystalline phase A contained in the sintered body, a [g], the mass of crystalline phase B, the mass of crystalline phase C, and the true density M ａ [g / cm ３ ], M ｂ [g / cm ３ ] and M ｃ [g / cm ３ ] was used to calculate the value from the following formula: d = (a + b + c) / ((a / M ａ ) + (b / M ｂ ) + (c / M ｃ The chromium, silicon, and nitrogen contents of the sintered body were calculated using the following formula: Chromium content = 100 × (a Ｃｒ +b Ｃｒ ) / (a ​​+ b + c) Silicon content = 100 × (a Ｓｉ +c Ｓｉ ) / (a ​​+ b + c) Nitrogen content = 100 × (b Ｎ +c Ｎ ) / (a ​​+ b + c) In the above formula, a is the mass [g] of chromium silicide contained in the sintered body, b is the mass [g] of chromium nitride contained in the sintered body, c is the mass [g] of silicon nitride contained in the sintered body, a Ｃｒ is the mass of chromium contained in chromium silicide [g], a Ｓｉis the mass of silicon contained in chromium silicide [g], b Ｃｒ is the mass of chromium contained in chromium nitride [g], b Ｎ is the mass of nitrogen contained in chromium nitride [g], c Ｓｉ is the mass of silicon contained in silicon nitride [g], c Ｎ is the mass [g] of nitrogen contained in silicon nitride. Chromium silicide is CrSi, CrSi ２ , Cr ３ Si and Cr ５ Si ３ Chromium nitride is at least one of Cr ２ N, and silicon nitride is Si ３ N ４ is.

[0071] The crystalline phase contained in the sintered body was identified from the powder X-ray diffraction (hereinafter also referred to as "XRD") pattern. An XRD device (device name: RINT Ultima III, manufactured by Rigaku Corporation) was used to obtain the XRD pattern of the sintered body by the following measurements. Acceleration current / voltage: 40 mA / 40 kV Radiation source: CuKα radiation (λ=1.5405 Å) Measurement mode: Continuous scan Scan conditions: 2° / min Measurement range: 2θ=20° to 80° Divergence vertical limiting slit: 10 mm Divergence / entrance slit: 1 / 2° Receiving slit: 0.3 mm The crystalline phase of the sintered body was identified by comparing the obtained XRD pattern with the ICDD database.

[0072] (TCR) Using an 8403-type AC / DC Hall measurement system (manufactured by Toyo Corporation), the resistivity R (R ３０ ~R １５０ ) was measured, and the resistivity R (μΩ cm) and R ３０ The TCR was calculated from the resistance (μΩ·cm) and each temperature T (°C) using the following formula in the range of 40°C to 150°C: TCR (ppm / °C) = (R - R ３０ ) / (R３０ ×(T-30))×10 ６ (Difference Between Maximum and Minimum TCR Values) The difference between the maximum and minimum TCR values ​​in the range of 40° C. to 150° C. obtained above was determined.

[0073] (Film Composition) The composition of the nitrogen-containing chromium silicide film was measured using an accelerated particle analyzer (device name: RBS-400 analytical end station, manufactured by Eurofins EAG). The film-coated substrate was processed so that the surface had a square shape of 10 mm x 10 mm (thickness: 0.7 mm), and the measurement was performed using the following method. Measurement method: RBS method (Rutherford backscattering spectroscopy)

[0074] Example 1: 48% by mass of chromium flakes (purity: 4N, particle size: 3 mm) and 52% by mass of silicon flakes (purity: 5N, particle size: 10 mm) were placed in a carbon crucible, and the chromium flakes and silicon flakes were melted at a processing temperature of 1650°C to obtain a molten metal of chromium and silicon. The molten metal was then dripped through an argon gas flow at a gas pressure of 7 MPa, and a chromium silicide alloy powder was obtained by a gas atomization method. The obtained chromium silicide alloy powder contained CrSi ２ The chromium silicide alloy powder and silicon nitride powder (product name: α-Si) were then mixed together so that the chromium silicide alloy powder was 81 mass % and the silicon nitride powder was 19 mass %. ３ N ４ , manufactured by Yeamin Co., Ltd.) were dry mixed for 1 hour at 60 rpm using a V-type mixer in an argon atmosphere to obtain a Cr—Si—N alloy powder containing 39 mass % of chromium, 54 mass % of silicon, and 7 mass % of nitrogen.

[0075] Next, the Cr-Si-N alloy powder was placed in a carbon mold (press die: diameter 15.2 cm) and sintered by hot pressing under the following conditions to obtain a sintered body of this example: Firing method: hot pressing Heating rate: 200°C / hour Heating atmosphere: vacuum atmosphere Firing atmosphere: vacuum atmosphere Firing temperature: 1400°C Firing pressure: 40 MPa Firing time: 3 hours This resulted in a disk-shaped sintered body of this example measuring 15.2 cm in diameter and 7 mm thick.

[0076] From the results of the XRD measurement, the sintered body of this example has a CrSi crystal phase. ２ and Si ３ N ４ It was confirmed that the sintered body of this example was a Cr—Si—N sintered body containing CrSi ２ 81% by mass, and Si ３ N ４ The sintered body contained 19 mass % of chromium, 39 mass % of silicon, 54 mass % of silicon, and 7 mass % of nitrogen.

[0077] The resulting sintered body was bonded to a backing plate to obtain a sputtering target.

[0078] The resulting sputtering target was used to form a nitrogen-containing chromium silicide film by sputtering under the following conditions: Apparatus: DC magnetron sputtering apparatus (manufactured by ULVAC, Inc.) Magnetic field strength: 1000 Gauss (directly above the target, horizontal component) Substrate-target distance: 90 mm Substrate temperature: room temperature (approximately 25°C) Introduced gas: argon Substrate used: glass substrate (manufactured by Corning Eagle XG Inc.) Thickness: 0.8 mm Power density: 200 W (2.5 W / cm ２The resulting film was heat-treated under the following conditions to produce a nitrogen-containing chromium silicide film of this example: Heat treatment temperature: 400°C Heat treatment time: 60 minutes Heat treatment atmosphere: vacuum atmosphere The nitrogen-containing chromium silicide film of this example had a Cr content of 27.9 atom %, a Si content of 58.6 atom %, a N content of 11.8 atom %, and a H content of 1.7 atom %.

[0079] Example 2: 20% by mass of chromium flakes (purity: 4N, particle size: 3 mm) and 80% by mass of silicon flakes (purity: 5N, particle size: 10 mm) were placed in a carbon crucible, and the chromium flakes and silicon flakes were melted at a processing temperature of 1600°C to obtain a molten metal of chromium and silicon. The molten metal was then dripped through an argon gas flow at a gas pressure of 7 MPa, and a chromium silicide alloy powder was obtained by a gas atomization method. The chromium silicide alloy powder contained Si and CrSi. ２ The chromium silicide alloy powder and silicon nitride powder (product name: α-Si) were then mixed together to form a mixture of 41 mass % chromium silicide alloy powder, 28 mass % silicon nitride powder, and 31 mass % chromium nitride powder. ３ N ４ , manufactured by Yeamin Co., Ltd.) and chromium nitride powder (product name: Cr ２ N, manufactured by Treibacher) was dry mixed for 1 hour at 60 rpm using a V-type mixer under an argon atmosphere to obtain a Cr—Si—N alloy powder containing 36 mass % chromium, 49 mass % silicon, and 15 mass % nitrogen.

[0080] Next, the Cr-Si-N alloy powder was placed in a carbon mold (press die: diameter 15.2 cm) and sintered by hot pressing under the following conditions to obtain a sintered body of this example: Firing method: hot pressing Heating rate: 200°C / hour Heating atmosphere: vacuum atmosphere Firing atmosphere: vacuum atmosphere Firing temperature: 1450°C Pressure: 40 MPa Firing time: 3 hours This resulted in a disk-shaped sintered body measuring 15.2 cm in diameter and 7 mm thick.

[0081] From the results of the XRD measurement, the sintered body of this example was found to be CrSi ２ , CrSi and Si ３ N ４ From the results of the XRD measurement, it was confirmed that the sintered body of this example was a Cr—Si—N sintered body containing CrSi ２ 57% by mass, CrSi 31% by mass, and Si ３ N ４ The sintered body contained 12 mass % of chromium, 36 mass % of silicon, 49 mass % of silicon, and 15 mass % of nitrogen.

[0082] A nitrogen-containing chromium silicide film was formed under the same conditions as in Example 1, except that the heat treatment temperature was changed to 520°C.

[0083] The nitrogen-containing chromium silicide film of this example had a Cr content of 25 atom %, a Si content of 55 atom %, a N content of 19 atom %, and a H content of 1 atom %.

[0084] Example 3 60 mass% of chromium flakes (purity: 4N, particle size: 3 mm) and 40 mass% of silicon flakes (purity: 5N, particle size: 10 mm) were placed in a carbon crucible, and the chromium flakes and silicon flakes were melted at a processing temperature of 1600°C to obtain a molten metal of chromium and silicon. Thereafter, a gas atomization method was used in which the molten metal was dropped through an argon gas flow at a gas pressure of 7 MPa to obtain a chromium silicide alloy powder. The chromium silicide alloy powder was composed of CrSi, CrSi ２ The chromium silicide alloy powder was then mixed with silicon nitride powder (product name: α-Si ) in a ratio of 25 mass % chromium silicide alloy powder, 56 mass % silicon nitride powder, and 19 mass % chromium nitride powder. ３ N ４ , manufactured by Yeamin Co., Ltd.) and chromium nitride powder (product name: Cr ２N, manufactured by Treibacher) were dry mixed for 1 hour at 60 rpm using a V-type mixer under an argon atmosphere to obtain a Cr—Si—N alloy powder containing 32 mass % of chromium, 43 mass % of silicon, and 25 mass % of nitrogen.

[0085] Next, the Cr-Si-N alloy powder was placed in a carbon mold (press die: diameter 15.2 cm) and sintered by hot pressing under the following conditions to obtain the sintered body of this example: Firing furnace: hot press furnace Heating rate: 200°C / hour Heating atmosphere: vacuum atmosphere Firing atmosphere: vacuum atmosphere Firing temperature: 1450°C Pressure: 40 MPa Firing time: 3 hours This resulted in a disk-shaped sintered body with a diameter of 15.2 cm and a thickness of 7 mm, free from microcracks.

[0086] From the results of the XRD measurement, it was found that the sintered body of this example contained Cr ３ Si, Cr ５ Si ３ and Si ３ N ４ From the results of the XRD measurement, it was confirmed that the sintered body of this example was a Cr—Si—N based sintered body consisting of Cr ３ 31% by mass of Si, Cr ５ Si ３ 7 mass% and Si ３ N ４ The sintered body contained 62 mass % of chromium, 32 mass % of silicon, 43 mass % of silicon, and 25 mass % of nitrogen.

[0087] A nitrogen-containing chromium silicide film was formed under the same conditions as in Example 1, except that the film was formed under the same conditions as in Example 1 and the heat treatment temperature was set to 610°C.

[0088] Example 4: 20% by mass of chromium flakes (purity: 4N, particle size: 3 mm) and 80% by mass of silicon flakes (purity: 5N, particle size: 10 mm) were placed in a carbon crucible, and the chromium flakes and silicon flakes were melted at a processing temperature of 1600°C to obtain a molten metal of chromium and silicon. A chromium silicide alloy powder was then obtained by a gas atomization method in which the molten metal was dropped through an argon gas flow at a gas pressure of 7 MPa. The chromium silicide alloy powder contained Si, CrSi ２ The gas atomized powder and chromium nitride powder (product name: Cr ２ N, manufactured by Treibacher) were dry mixed for 1 hour at 60 rpm using a V-type mixer under an argon atmosphere to obtain a Cr—Si—N powder containing 50 mass % chromium, 45 mass % silicon, and 5 mass % nitrogen.

[0089] Next, this Cr—Si—N powder was placed in a carbon mold (press die: diameter 15.2 cm) and fired by hot pressing under the following conditions to obtain the sintered body of this example: Firing furnace: hot press furnace Heating rate: 200°C / hour Heating atmosphere: vacuum atmosphere Firing atmosphere: vacuum atmosphere Firing temperature: 1450°C Pressure: 40 MPa Firing time: 3 hours This resulted in a disk-shaped sintered body with a diameter of 15.2 cm and a thickness of 7 mm, free from microcracks.

[0090] From the results of the XRD measurement, the sintered body of this example was found to be composed of CrSi, CrSi ２ and Si ３ N ４ From the results of the XRD analysis, it was confirmed that the sintered body of this example was a Cr—Si—N sintered body consisting of 45 mass % CrSi and 50 mass % CrSi. ２ 42% by mass, and Si ３ N ４The sintered body contained 13 mass % of chromium, 50 mass % of silicon, 45 mass % of silicon, and 5 mass % of nitrogen.

[0091] A nitrogen-containing chromium silicide film was formed under the same conditions as in Example 1, except that the heat treatment temperature was changed to 370°C.

[0092] Example 5 5% by mass of chromium flakes (purity: 4N, particle size: 3 mm) and 95% by mass of silicon flakes (purity: 5N, particle size: 10 mm) were placed in a carbon crucible, and the chromium flakes and silicon flakes were melted at a processing temperature of 1600°C to obtain a molten metal of chromium and silicon. Thereafter, a gas atomization method was used in which the molten metal was dropped through an argon gas flow at a gas pressure of 7 MPa to obtain a chromium silicide alloy powder. The chromium silicide alloy powder contained Si, CrSi ２ Thereafter, the Cr-Si alloy powder and silicon nitride powder (product name: α-Si) were mixed together so that the chromium silicide alloy powder was 23 mass %, the silicon nitride powder was 38 mass %, and the chromium nitride powder was 39 mass %. ３ N ４ , manufactured by Yeamin Co., Ltd.) and chromium nitride powder (product name: Cr ２ N, manufactured by Treibacher) was dry mixed for 1 hour at 60 rpm using a V-type mixer under an argon atmosphere to obtain a Cr—Si—N alloy powder containing 36 mass % chromium, 44 mass % silicon, and 20 mass % nitrogen.

[0093] Next, the Cr-Si-N alloy powder was placed in a carbon mold (press die: diameter 15.2 cm) and sintered by hot pressing under the following conditions to obtain the sintered body of this example: Firing furnace: hot press furnace Heating rate: 200°C / hour Heating atmosphere: vacuum atmosphere Firing atmosphere: vacuum atmosphere Firing temperature: 1450°C Pressure: 40 MPa Firing time: 3 hours This resulted in a disk-shaped sintered body with a diameter of 15.2 cm and a thickness of 7 mm, free from microcracks.

[0094] From the results of the XRD measurement, the sintered body of this example is composed of CrSi, Cr ５ Si ３ and Si ３ N ４ From the results of the XRD analysis, it was confirmed that the sintered body of this example was a Cr—Si—N-based sintered body consisting of 26 mass % CrSi and 10 mass % Cr. ５ Si ３ 25 mass% of Si ３ N ４ The sintered body contained 49 mass % of chromium, 36 mass % of silicon, 44 mass % of silicon, and 20 mass % of nitrogen.

[0095] A nitrogen-containing chromium silicide film was formed under the same conditions as in Example 1, except that the heat treatment temperature was changed to 580°C.

[0096] Comparative Example 1: A CrSi alloy containing 42% by mass of chromium and 58% by mass of silicon was prepared in the same manner as in Example 1. ２ A chromium silicide alloy powder having a crystalline phase consisting of Cr and Si was obtained.

[0097] A chromium silicide sintered body was obtained in the same manner as in Example 1, except that the chromium silicide alloy powder was directly sintered by hot pressing, the sintering temperature was set to 1250° C., and the pressure was set to 15 MPa.

[0098] From the results of the XRD measurement, the sintered body of this comparative example was CrSi ２From the results of the XRD measurement and the composition analysis by ICP, the sintered body of this comparative example was identified as a Cr—Si sintered body (a sintered body of chromium silicide) consisting of CrSi ２ The sintered body contained 87 mass % of Fe and 13 mass % of Si, 42 mass % of chromium, and 58 mass % of silicon.

[0099] A chromium silicide film was formed under the same conditions as in Example 1, except that the heat treatment temperature was changed to 230°C.

[0100] The evaluation results of the examples and comparative examples are shown in Table 1.

[0101] From the examples and comparative examples, it was confirmed that the film obtained by depositing a Cr-Si-N sintered body has a lower TCR maximum value - TCR minimum value. Furthermore, from Examples 1 to 5, it was confirmed that the resistivity of the obtained film increases with an increase in the nitrogen content of the target. The entire contents of the specification, claims, drawings, and abstract of Japanese Patent Application No. 2024-30924, filed on March 1, 2024, are hereby incorporated by reference as the disclosure of the specification of the present disclosure.

[0102] 10...sintered body, 20...backing plate, 30...bonding material, 100...sputtering target, 200...film-coated substrate, 201...substrate, 202...nitrogen-containing chromium silicide film.

Claims

1. A Cr-Si-N sintered body containing chromium, silicon, and nitrogen, with the nitrogen content being 1% by mass or more and 30% by mass or less, and the silicon content being 20% ​​by mass or more and 60% by mass or less.

2. The Cr-Si-N sintered body according to claim 1, which contains chromium silicide and at least one selected from the group consisting of chromium nitride and silicon nitride.

3. CrSi, CrSi ２ , Cr ３ Si and Cr ５ Si ３ 3. The Cr-Si-N sintered body according to claim 1, comprising one or more selected from the group consisting of:

4. A Cr-Si-N sintered body according to any one of claims 1 to 3, wherein the nitrogen content is 15% by mass or more and 30% by mass or less.

5. Cr ３ Si and Cr ５ Si ３ The Cr-Si-N sintered body according to claim 3, comprising:

6. A method for producing a Cr-Si-N sintered body according to any one of claims 1 to 5, comprising the steps of: mixing an alloy powder of chromium and silicon with a nitrogen-containing compound source containing at least one of chromium and silicon and nitrogen to obtain a mixed powder; and heat treating the mixed powder by pressure-sintering it in a vacuum atmosphere.

7. The method for producing a Cr-Si-N sintered body according to claim 6, wherein the nitrogen-containing compound source is a nitride containing at least one of chromium and silicon.

8. A sputtering target comprising the sintered body according to any one of claims 1 to 5.

9. A method for producing a nitrogen-containing chromium silicide film, using the sintered body according to any one of claims 1 to 5.

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