Methods for producing titanium hydride powder, slurry, and active metal brazing filler metal

Abstract

The present invention provides a method for producing titanium hydride powder suitable for use in active metal brazing filler metals, titanium hydride powder, a slurry, and an active metal brazing filler metal. [Solution] The method for producing titanium hydride powder of this invention is a method for producing titanium hydride powder containing TiH2 and used in active metal brazing materials, and includes a milling step in which a raw material powder containing TiH2 is wet-milled, and the titanium hydride powder obtained after the wet milling has a 90% particle size D90 of 7.00 μm or less as measured by laser diffraction / scattering method.

Description

[Technical Field]

[0001] This invention relates to a method for producing titanium hydride powder containing TiH2. ,vinegar Rally Manufacturing method , and active metal brazing material Manufacturing method It is related to. [Background technology]

[0002] For example, small nodules generated when crushing titanium sponge blocks obtained by reducing titanium tetrachloride with metallic magnesium, and cutting chips and other scrap generated when cutting ingots or slabs made by melting and casting the crushed titanium sponge, may be subjected to the hydrodehydrogenation process (the so-called HDH process).

[0003] In the hydrogenation-dehydrogenation method, the small pieces or scraps are heated in a hydrogen gas atmosphere to be hydrogenated and embrittled, and then crushed to a predetermined particle size to produce titanium hydride powder. The titanium hydride powder is then heated in a vacuum as a dehydrogenation treatment to produce titanium powder (pure titanium powder).

[0004] The titanium hydride powder obtained by the hydrogenation-dehydrogenation method before dehydrogenation contains TiH2, which is a metal hydride, and can be used for various purposes other than the production of titanium powder by the hydrogenation-dehydrogenation method described above. Related techniques include those described in Patent Documents 1 to 3, for example.

[0005] Patent Document 1 states, "We have discovered that fine titanium particles suitable for paste can be produced by continuing to mechanically pulverize titanium hydride powder produced by hydrogen pulverization or titanium metal powder produced using this as a raw material in a pulverizer, leading to the completion of the present invention." It also goes on to describe a titanium-based powder for paste characterized by an average particle size of 20 μm or less, a d90 of 22.50 μm or less, and particle size distribution parameters α and β satisfying the following relationship: 0.6<β / α<1.0 (1), where α = (d90 - d50) / d50, and β = (d50 - d10) / d50 (d10, d50, and d90 are the particle sizes corresponding to 10%, 50%, and 90% of the integrated weight in the cumulative particle size distribution of the titanium powder)." Regarding the above-mentioned "mechanical pulverization," Patent Document 1 states, "Because the titanium hydride extracted from the reaction vessel is highly disintegrable, it is preferable to pulverize and size-regulate it using a known crusher. The pulverization atmosphere is preferably atmospheric pressure or an inert gas atmosphere." Patent Document 1 also describes examples and comparative examples in which the "d90" is from "20.32" μm to "58.33" μm.

[0006] Patent Document 2 describes a method for producing titanium powder by a hydrogenation-dehydrogenation method, characterized in that titanium hydride is pulverized to an average particle size of 10 μm or less and the dehydrogenation temperature is set to 300 to 600°C.

[0007] Patent Document 3 describes "a titanium hydride powder produced by a process of hydrogen embrittlement of sponge titanium produced by the Kroll process, characterized in that the average particle size is 30 μm or less, the proportion of powder with particle sizes of 5 μm or less is 10% by weight or less, the oxygen content is 0.15% or less, and the chlorine content is 0.05% by weight or less." [Prior art documents] [Patent documents]

[0008] [Patent Document 1] Patent No. 5898761 [Patent Document 2] Japanese Patent Application Publication No. 3-122205 [Patent Document 3] Japanese Patent Application Publication No. 10-195504 Summary of the Invention [Problem to be solved by the invention]

[0009] Incidentally, active metal brazing filler metals used to join ceramic materials and metal materials, which are difficult to join with ordinary brazing filler metals, sometimes contain Ti, and titanium hydride powder is sometimes used for this.

[0010] In this case, it has been newly discovered that finely divided titanium hydride powder is desirable to increase the reactivity of Ti in the active metal brazing filler metal with the joined materials, such as ceramic materials, and to increase the wettability between the active metal brazing filler metal and the joined materials.

[0011] However, common milling methods, such as the "mechanical milling" under "atmospheric pressure or an inert gas atmosphere" described in Patent Document 1, can be difficult to achieve for extremely finely milling titanium hydride powder to a particle size below a predetermined size. Even if milling were possible, the specific surface area of ​​the active particle surface of the titanium hydride powder increases significantly during milling, which can lead to reaction with oxygen in the atmosphere and the resulting oxidation heat, potentially resulting in ignition. Even if ignition does not occur after milling, a relatively thick oxide layer may form due to the increase in material temperature, potentially resulting in insignificant improvement in wettability when used in an active metal brazing material. For these reasons, it is undesirable to mill titanium hydride powder using only dry milling.

[0012] One object of the present invention is to provide a method for producing titanium hydride powder that can be suitably used for active metal brazing filler metals. ,vinegar Rally Manufacturing method , and active metal brazing material Manufacturing method Another object of the present invention is to provide a titanium hydride powder having a relatively small particle size while reducing the risk of fire. [Means for solving the problem]

[0013] The method for producing titanium hydride powder of the present invention is a method for producing titanium hydride powder containing TiH2 and used in active metal brazing filler metals, and includes a milling step in which a raw material powder containing TiH2 is wet-milled, and the titanium hydride powder obtained after the wet-milling has a 90% particle size D90 of 7.00 μm or less as measured by a laser diffraction / scattering method, and the milling step further includes dry-milling, in which the raw material powder that has been subjected to the dry-milling is wet-milled, and the raw material powder obtained by the dry-milling is subjected to a 90% particle size D90 of 7.00 μm or less as measured by a laser diffraction / scattering method. Ruhei The average particle size D50 is adjusted to be 10 μm or more and 15 μm or less.

[0015] In the pulverization step, The wet grinding may include: The raw material powder, a liquid, and a grinding medium are placed in a grinding container, and the grinding container is rotated to perform wet grinding, thereby obtaining a slurry containing the titanium hydride powder and the liquid.

[0016] In this case, the pulverization step The wet grinding In this case, the rotation speed of the grinding container can be set to 200 rpm to 250 rpm, and the grinding time can be set to 60 minutes to 100 minutes.

[0017] The pulverization step The wet grinding In this case, the ratio of the mass of the liquid to the total mass of the raw material powder and the liquid can be set to 0.6 to 0.9.

[0025] Slurry of the present invention Manufacturing method Any of the above titanium hydride powders and liquid Including the body To produce a slurry It is something.

[0026] The above slurry The manufacturing method Preferably, the mass ratio of the liquid in the slurry is 0.6 to 0.9.

[0027] The active metal brazing material of this invention Manufacturing method is one of the above a method for producing titanium hydride powder, Contains titanium hydride powder The company manufactures active metal brazing materials. It is something. [Effects of the Invention]

[0028] Titanium hydride powder of the present invention Titanium hydride powder produced by the method can be suitably used for active metal brazing materials. DETAILED DESCRIPTION OF THE INVENTION

[0029] Hereinafter, an embodiment of the present invention will be described in detail.

[0030] (titanium hydride powder) The titanium hydride powder according to one embodiment of the present invention contains TiH2 and is used in active metal brazing filler metals.

[0031] Active metal brazing, which uses an active metal brazing filler metal, is often applied to joining ceramic materials or ceramic materials to metal materials, and is also referred to as the active-metal method. In active metal brazing, the titanium contained in the titanium hydride powder in the active metal brazing filler metal reacts with nitrogen, oxygen, and other elements in the materials to be joined to form compounds, which significantly reduce interfacial energy and improve wettability between the active metal brazing filler metal and the materials to be joined. This method is therefore applicable to materials that are difficult to join with conventional brazing filler metals. If the active metal already contains a certain amount of oxygen, the aforementioned wettability improvement effect can be reduced. However, using titanium hydride powder containing TiH2 is expected to suppress the oxidation of titanium and the incorporation of oxygen during the joining process compared to metallic titanium powder.

[0032] On the other hand, the properties of titanium hydride powder that can enhance the reactivity between Ti in an active metal brazing filler metal and the materials to be joined have not been fully investigated. The inventors, however, believed that if titanium hydride powder with a sufficiently small particle size is used in an active metal brazing filler metal, compounds (such as titanium oxides and nitrides) will be formed uniformly at the joining interface between the Ti in the active metal brazing filler metal and the materials to be joined, thereby improving the joinability of active metal brazing. This is thought to be because the small particle size increases the number of titanium hydride powder particles per unit volume of the active metal brazing filler metal, reducing the density difference of the titanium hydride powder within the brazing filler metal. In addition, the large specific surface area facilitates the formation of compounds with a relatively uniform size in a uniform manner during the reaction.

[0033] More specifically, the titanium hydride powder of this embodiment has a 90% particle size D90 of 7.00 μm or less, preferably 6.50 μm or less, as measured by a laser diffraction / scattering method. If the 90% particle size D90 is greater than 7.00 μm, the specific surface area will be small, resulting in insufficient reactivity with the workpiece during active metal brazing. If the 90% particle size D90 is too small, the powder will be prone to agglomeration, potentially resulting in substantial coarsening. The 90% particle size of the titanium hydride powder is preferably 5.80 μm to 6.40 μm, more preferably 5.90 μm to 6.30 μm.

[0034] Wet milling, as described below, tends to make it easier to obtain titanium hydride powder with a small 90% particle size D90, as described above. Dry milling often does not allow for significant refinement due to limitations on the particle size that can be classified after milling. Furthermore, titanium hydride powder produced through wet milling tends to have the particle size and particle size distribution described below.

[0035] The maximum particle size of the titanium hydride powder measured by laser diffraction / scattering method is preferably 11.00 μm or less, and more preferably 10.50 μm or less. If the maximum particle size is small, the generation of coarse particles during active metal brazing is suppressed, and mechanical properties such as joint strength after joining are stabilized. The maximum particle size of the titanium hydride powder may be, for example, 9.00 μm or more, typically 10.00 μm or more.

[0036] Furthermore, for the titanium hydride powder, the 10% particle size D10, average particle size D50, and 90% particle size measured by laser diffraction / scattering method are preferably such that the larger of the value obtained by subtracting the 10% particle size D10 from the average particle size D50 (D50-D10) and the value obtained by subtracting the average particle size D50 from the 90% particle size D90 (D90-D50) is 3.00 μm or less, and even more preferably 2.00 μm or less. A small difference between the average particle size D50 and the 10% particle size D10, or between the 90% particle size D90 and the average particle size D50, indicates that the particle size distribution of the titanium hydride powder is sharp. When the larger of these differences is small as described above, relatively small particles are uniformly generated during active metal brazing, which is thought to further stabilize the mechanical properties. The difference between the average particle size D50 and the 10% particle size D10, and the difference between the 90% particle size D90 and the average particle size D50 may be, for example, 0.5 μm or more, typically 1.0 μm or more.

[0037] Furthermore, the titanium hydride powder preferably has a volume ratio of particles with a particle diameter of 6.00 μm or more of 14.00% or less. This prevents the generation of coarse titanium-containing particles during active metal brazing, thereby suppressing the resulting decrease in reactivity with the joined materials. In this case, for example, when joining ceramic or metallic circuit boards using an active metal brazing material, the overall or partial thickness of the joining layer formed with the active metal brazing material can be prevented from increasing due to the generation of coarse titanium-containing particles. A smaller number of coarse particles and a larger number of fine particles increases the surface area, thereby increasing the contact area with the ceramic or metallic material, resulting in the formation of more titanium compounds such as nitrides at the interface, further enhancing brazing strength. Therefore, it is desirable to have fewer particles with a particle diameter of 6.00 μm or more, and their volume ratio is preferably 14.00% or less, and more preferably 13.00% or less. The volume ratio of particles of the titanium hydride powder having a particle size of 6.00 μm or more may be, for example, 1.0% or more, typically 3.0% or more.

[0038] The above-mentioned 10% particle size D10, average particle size D50, 90% particle size D90, and maximum particle size, as well as the volume ratio of particles having a predetermined particle size, can each be measured using a particle size distribution analyzer (Laser Scattering Particle Size Distribution Analyzer LA-960 (laser diffraction / scattering method)) manufactured by Horiba, Ltd.

[0039] Titanium hydride powder contains TiH2, and typically consists mostly of TiH2. The TiH2 content of titanium hydride powder can be confirmed by analyzing its hydrogen concentration using an inert gas fusion-thermal conductivity method. The hydrogen content in titanium hydride powder may be 3.0 mass% or more and 4.0 mass% or less. When titanium is completely hydrogenated and can no longer contain any more hydrogen, the hydrogen content of titanium hydride powder may be 4.0 mass% or less, typically 3.0 mass% or more and 4.0 mass% or less.

[0040] Titanium hydride powder may contain impurities such as Fe, Si, Mn, Mg, Cl, N, and / or O, each in a content of 0.1 mass% or less. It may also contain other impurities in amounts below the detection limit. The presence and content of impurities can be confirmed by ICP atomic emission spectroscopy (Fe, Si, Mn, Mg), silver nitrate titration (Cl), ammonia distillation separation amidosulfuric acid titration (N), and inert gas fusion-infrared absorption spectroscopy (O).

[0041] (slurry) The slurry contains the titanium hydride powder and a liquid. The liquid may be water (tap water, industrial water, distilled water, purified water, ion-exchanged water, pure water, ultrapure water, etc.) or an organic solvent with a viscosity similar to that of water. The slurry may also contain other components or elements.

[0042] The slurry referred to here may be the slurry taken out from the wet-milling apparatus after wet-milling by the manufacturing method described below. In this case, the liquid used in the wet-milling may correspond to the liquid in the slurry.

[0043] By adding titanium hydride powder to the slurry, the risk of fire can be reduced even if the particles are extremely fine, as described above. Therefore, the slurry containing titanium hydride powder is easy to handle.

[0044] The mass proportion of the liquid in the slurry (when the liquid is water, this means the water content; calculated by liquid mass / (liquid mass+titanium hydride powder mass)) is preferably 0.6 to 0.9, and more preferably 0.75 to 0.85. If the mass proportion of the liquid is too low, the viscosity of the slurry increases, making it difficult to pulverize. If the mass proportion of the liquid is too high, the frequency of collisions between the powder and media decreases, making it difficult to pulverize.

[0045] (active metal brazing filler metal) The titanium hydride powder is used in an active metal brazing material for use in active metal brazing. At least a part of the active metal brazing material may contain the titanium hydride powder.

[0046] Active metal brazing materials are typically used for joining ceramic materials, such as circuit boards, to metal materials by active metal brazing. Examples of ceramic materials include oxide-based, nitride-based, and carbide-based ceramics, specifically Al2O3, SiC, Si3N4, AlN, and ZrO2. Examples of metal materials include Cu.

[0047] Active metal brazing filler metals are sometimes in powder or sheet form, but as an example, they may be in paste form. Paste-form active metal brazing filler metals may contain, in addition to the titanium hydride powder, an organic substance such as an organic solvent, and may be, for example, a powder containing titanium hydride powder dispersed in an organic solvent. Powders other than titanium hydride powder that may be contained in active metal brazing filler metals include silver powder and copper powder. Titanium hydride powder may be mixed into such powders as an additive.

[0048] Active metal brazing is sometimes performed by placing an active metal brazing material on one of the workpieces by coating or other means, sandwiching the active metal brazing material between the two workpieces, and then heating them in a vacuum. During this process, the organic solvent in the paste-like active metal brazing material evaporates, other powders melt, and Ti reacts with components of the workpieces (e.g., Al2O3) to form compounds (e.g., Al-Ti-O), chemically bonding the active metal brazing material and the workpieces. In the case of the active metal brazing material containing titanium hydride powder of the above-mentioned embodiment, the titanium hydride powder, which is distributed relatively uniformly and densely on the target surfaces, uniformly forms compounds of similar size. This increases the effective reactivity between Ti and the workpieces, which is thought to improve the bond strength between the workpieces using the active metal brazing material.

[0049] (Manufacturing method) In producing the titanium hydride powder described above, a raw material powder containing TiH2 can be subjected to a milling process including wet milling.

[0050] To obtain the raw material powder to be subjected to the pulverization step, the titanium raw material can be subjected to the steps up to the dehydrogenation step in the hydrodehydrogenation process. In other words, the raw material powder is obtained before the dehydrogenation step during the hydrodehydrogenation process. Below, a method for obtaining the raw material powder during the hydrodehydrogenation process will be described in detail, but the raw material powder is not limited to that obtained by this method.

[0051] In the hydrodehydrogenation process, a titanium raw material is first subjected to a hydrogenation step. Examples of titanium raw materials that can be used include small pieces generated when crushing titanium sponge blocks, and cutting chips or other scrap generated when cutting ingots or slabs produced by melting and casting the titanium sponge obtained by crushing. The titanium sponge blocks are produced by reducing titanium tetrachloride with metallic magnesium and consist primarily of Ti.

[0052] In the hydrogenation process, the titanium raw material is heated to a temperature of, for example, 500°C or higher, and hydrogen gas is supplied to the titanium raw material. This causes the titanium raw material to absorb hydrogen, generating TiH2, which becomes the hydrogenation raw material. In the final titanium hydride powder, much of the titanium is combined with hydrogen, so an increase in oxygen content is suppressed even if the powder is fine. As a result, when used in active metal brazing, the occurrence of problems such as a decrease in wettability due to oxygen is suppressed. Furthermore, in this embodiment, ignition of the titanium hydride powder is suppressed, and an increase in oxygen content due to ignition can also be suppressed.

[0053] The hydrogenation raw material may then be subjected to a crushing process and a classification process. A crushing device equipped with an impact crushing rotor or an air classifier equipped with a classification rotor may be used. Air classification is advantageous because it can classify powder in a relatively fine range and also because it can finely adjust the classification point. This process results in a raw material powder. When titanium powder is to be produced, the raw material powder is subjected to a dehydrogenation process.

[0054] The milling process for the raw material powder includes wet milling, in which the raw material powder is milled in a liquid. Wet milling can significantly reduce the risk of fire when the raw material powder is milled into extremely fine particles such as the titanium hydride powder mentioned above. Liquids used in wet milling include water (tap water, industrial water, distilled water, purified water, ion-exchanged water, pure water, ultrapure water, etc.) and organic solvents with a viscosity similar to that of water.

[0055] Wet milling can be performed using a wet milling device that grinds raw material powder with media, such as a wet ball mill or bead mill. In this case, the raw material powder is placed in a drum-shaped or other milling container of the wet milling device together with liquid and milling media, and the container is rotated to wet mill the raw material powder. For example, the rotation speed of the milling container may be 200 rpm to 250 rpm, and the milling time may be 60 to 100 minutes. The mass ratio of the liquid to the total weight of the raw material powder and liquid placed in the milling container may be 0.6 to 0.9. An example of such a device is the "Pivot Mill PM-20" manufactured by Sugiyama Heavy Industries, Ltd.

[0056] In addition, wet milling may use a wet milling device such as a water jet that applies an impact force to the raw material powder by spraying a pressurized liquid containing the raw material powder. This is because excessive pulverization can be suppressed by adjusting the spray pressure, and the raw material powder can be easily refined to the desired small particle size. Furthermore, wet milling devices that apply an impact force to the raw material powder by spraying a pressurized liquid can suppress contamination by the media material.

[0057] Examples of wet milling devices that spray pressurized liquid containing raw material powder include those that spray pressurized liquid containing raw material powder from multiple nozzles (e.g., two nozzles) and collide them to apply impact force to the raw material powder, and those that spray pressurized liquid containing raw material powder from nozzles and collide it with media to apply impact force to the raw material powder. An example of the former is the "Starburst 10" manufactured by Sugino Machine Co., Ltd., and an example of the latter is the "Starburst Mini (HJP-25001V2)" manufactured by Sugino Machine Co., Ltd.

[0058] When such a wet-type grinding device is used in the grinding step, the injection pressure of the pressurized liquid is preferably 200 MPa to 250 MPa. If the injection pressure is too low, the grinding force may be insufficient and pulverization may not proceed well, while if the injection pressure is too high, excessive grinding may occur, increasing cohesion and resulting in an increase in the amount of substantial coarse particles.

[0059] Furthermore, when a wet milling device that sprays a pressurized liquid containing the raw material powder is used in the milling process, it is preferable to mill the raw material powder using the wet milling device 1 to 5 times. If the number of milling cycles is too few, the target particle size may not be achieved, while if the number of milling cycles is too many, there is a concern that excessive milling will increase cohesion and result in an increase in the number of substantial coarse particles.

[0060] The raw material powder used for wet milling preferably has a small particle size, for example, an average particle size D50 measured by laser diffraction / scattering method of 30 μm or less, particularly 10 μm to 15 μm. This shortens the time from the start of processing to reaching the target particle size. Since wet milling is performed on such small-particle-size raw material powder, if it is necessary to adjust the particle size of the raw material powder before wet milling, dry milling can be performed. The milling process may include dry milling and wet milling in this order. For dry milling, for example, a mill equipped with an impact milling rotor, which mills the raw material by colliding with a rotating rotor, may be used. After dry milling, classification may be performed before wet classification. The raw material powder's particle size is further reduced by wet milling. Achieving a relatively small average particle size D50 through dry milling facilitates the production of titanium hydride powder with a sufficiently small 90% particle size D90 after wet milling. Classification after wet milling is not necessarily required.

[0061] When wet-pulverization in the pulverization step is completed, titanium hydride powder having a predetermined small particle size is obtained. In some cases, it is preferable to remove the titanium hydride powder together with the liquid from the wet-pulverization apparatus and then form a slurry containing the liquid and titanium hydride powder. This effectively reduces the risk of the titanium hydride powder catching fire. [Example]

[0062] Next, a titanium hydride powder according to the present invention was produced as a prototype, which will be described below, although the description here is for illustrative purposes only and is not intended to be limiting.

[0063] The cutting chips generated during the machining of titanium ingots were subjected to a hydrogenation process using a hydrogenation-dehydrogenation method, a crushing process, and a classification process to obtain raw powder containing TiH2. This raw powder was then subjected to a crushing process that included dry crushing and wet crushing in this order to produce titanium hydride powder.

[0064] For wet milling, a wet milling device (Pivot Mill PM-20 manufactured by Sugiyama Heavy Industries Co., Ltd.) was used, which rotates the milling container and mills the raw material powder in the liquid inside by bringing it into contact with the milling media. The wet milling conditions were changed as shown in Table 1.

[0065] The particle size distribution of the raw material powder and titanium hydride powder was measured using a particle size distribution analyzer (Laser Scattering Particle Size Distribution Analyzer LA-960 (laser diffraction / scattering method)) manufactured by Horiba, Ltd. The 10% particle size D10, average particle size D50, and 90% particle size D90 were determined for each of the raw material powder and titanium hydride powder. The maximum particle size, D50-D10, D90-D50, and volume ratio of particles with a particle size of 6.00 μm or more were also determined for the titanium hydride powder. The results are shown in Table 2. The hydrogen content of the titanium hydride powder was measured using a hydrogen analyzer (RHEN602) manufactured by LECO Japan LLC. The results are shown in Table 2.

[0066] The above wet grinding yielded a slurry containing titanium hydroxide powder, and the titanium hydride powder in the slurry was subjected to an alumina plate bonding test according to the procedure described below. (1) A slurry containing approximately 0.1 g of titanium hydride powder, the mass of which was calculated in advance, was dropped onto a 15 x 15 x 1.5 mm alumina plate placed on a SUS tray, and the water was dried in a dryer at approximately 80°C. (2) An alumina plate of the same size as (1) was placed on top of the alumina plate on which titanium hydride powder had been spread, and a quartz plate was placed on top of that. (3) Several quartz plates were stacked on top of the quartz plate for height adjustment, and a titanium plate weighing approximately 130 g was placed on top of them as a weight to obtain a test sample. (4) The obtained test samples were subjected to heat treatment at 800° C. for 90 minutes in a vacuum atmosphere of 10 Pa or less. (5) After the heat treatment, the test samples were checked to see if the alumina plates could be joined together. (6) Regarding the bonding of the test samples after the heat treatment, a shear test was conducted in which one end face of the stacked alumina plates was fixed and a 5 kg weight was placed on the other end face (area: 15 mm × 1.5 mm) and a shear load was applied horizontally to the bonded surfaces to check for damage. If the bonded alumina plates peeled off or the solidified test powder was damaged and could not be used for the thermal conductivity measurement described below, the result was judged as "fail."

[0067] Test samples of the titanium hydride powder were prepared in the same manner as in the alumina plate bonding test, and their thermal conductivity was measured in accordance with the US standard ASTM E 1530. The results are shown in Table 2. The measurement device used was a steady-state thermal conductivity measuring device (GH-1, manufactured by Advance Riko Co., Ltd.) The test sample was prepared as an alumina plate measuring 25 × 25 × 1.5 mmt, and the net amount of test powder used was approximately 0.1 g.

[0068] In Examples 1 to 3, the 90% particle diameter D90 of the titanium hydride powder was sufficiently small, resulting in high thermal conductivity of the test samples. On the other hand, in Comparative Examples 1 to 10 and 12, the 90% particle diameter D90 of the titanium hydride powder was large, resulting in low thermal conductivity of the test samples, although bonding was possible. In Comparative Example 11, bonding was not possible.

[0069] [Table 1]

[0070] [Table 2]

[0071] The above results suggest that certain titanium hydride powders may be suitable for use as active metal brazing filler metals.

Claims

1. TiH 2 A method for producing a titanium hydride powder for use in an active metal brazing material, comprising: TiH 2 A grinding step including wet grinding a raw material powder containing the 90% particle size D90 of the titanium hydride powder obtained after the wet milling method as measured by a laser diffraction / scattering method is 7.00 μm or less; The pulverization step further includes dry pulverization, and the raw material powder that has been subjected to the dry pulverization is subjected to the wet pulverization. The method for producing titanium hydride powder comprises adjusting the raw material powder by the dry pulverization so that the average particle diameter D50 measured by a laser diffraction / scattering method is 10 μm or more and 15 μm or less.

2. 2. The method for producing titanium hydride powder according to claim 1, wherein in the milling step, the raw material powder, a liquid, and milling media are placed in a milling container, and the milling container is rotated to perform wet milling, thereby obtaining a slurry containing the titanium hydride powder and the liquid.

3. 3. The method for producing titanium hydride powder according to claim 2, wherein the wet grinding in the grinding step is carried out with the grinding container rotating at a speed of 200 rpm to 250 rpm for a grinding time of 60 minutes to 100 minutes.

4. 3. The method for producing titanium hydride powder according to claim 2, wherein in the wet pulverization in the pulverization step, the ratio of the mass of the liquid to the total mass of the raw material powder and the liquid is 0.6 to 0.

9.

5. The method for producing a titanium hydride powder according to any one of claims 1 to 4, A method for producing a slurry comprising producing a slurry containing the titanium hydride powder and a liquid.

6. 6. The method for producing a slurry according to claim 5, wherein the mass ratio of the liquid in the slurry is 0.6 to 0.

9.

7. The method for producing a titanium hydride powder according to any one of claims 1 to 4, A method for producing an active metal brazing filler metal, which comprises producing an active metal brazing filler metal containing the titanium hydride powder.

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