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WO-2026095056-A1 - OXIDE POWDER

WO2026095056A1WO 2026095056 A1WO2026095056 A1WO 2026095056A1WO-2026095056-A1

Abstract

Disclosed is an oxide powder which contains at least one element that is selected from the group consisting of Cu, Zn, V, Mg, P, and S. The oxide powder has a sphericity of 0.7 to 1.0 inclusive, and has a temperature range in which at least the dimensional change ratio (∆L/L) is less than 0 in a temperature range of 0°C to 200°C inclusive, or a temperature range in which at least the linear expansion coefficient (α) is less than 0 ppm/K in a temperature range of 0°C to 200°C inclusive. The sphericity of the oxide powder may be preferably 0.8 to 1.0 inclusive. The oxide powder can be produced by a method that includes subjecting a starting material powder to a spheroidizing treatment by flame melting or PVD.

Inventors

  • TANAKA, AKINOBU
  • IDE, HITOHIKO
  • MOTONO, RYUJI

Assignees

  • 三井金属株式会社

Dates

Publication Date
20260507
Application Date
20251031
Priority Date
20241101

Claims (15)

  1. An oxide powder comprising at least one element selected from the group consisting of Cu, Zn, V, Mg, P, and S, The sphericity of the oxide powder is 0.7 or more and 1.0 or less. It has a temperature range in which the dimensional change ratio (ΔL/L) is less than 0 in a temperature range of at least 0°C to 200°C, or has a temperature range in which the coefficient of linear expansion (α) is less than 0 ppm/K in a temperature range of at least 0°C to 200°C. Oxide powder.
  2. The oxide powder according to claim 1, comprising at least two elements selected from the group consisting of Cu, Zn, V, Mg, P, and S.
  3. The oxide powder according to claim 2, comprising Zn, Mg, and P.
  4. The oxide powder according to claim 1, comprising at least one powder of an oxide represented by the general formula (1) Zn 2-x Mg x P 2 O 7±δ (wherein part or all of Mg may be substituted with Sr and/or Ca and/or Ba, where 0 ≤ x ≤ 2 and δ is a value determined to satisfy the charge neutrality condition).
  5. The oxide powder according to claim 4, wherein in the general formula (1) Zn 2-x Mg x P 2 O 7±δ , 0.05 ≤ x ≤ 0.5.
  6. The oxide powder according to any one of claims 1 to 5, wherein the sphericity of the oxide powder is 0.8 or more and 1.0 or less.
  7. A resin composition comprising the oxide powder and resin component according to any one of claims 1 to 5.
  8. The resin composition according to claim 7, further comprising a curing agent.
  9. The resin composition according to claim 7, wherein the alpha dose is 0.0200 cph/ cm² or less.
  10. A powder mixture comprising the oxide powder and silica-containing powder or other thermally conductive powder according to any one of claims 1 to 5.
  11. An electronic component encapsulant comprising the resin composition described in claim 7.
  12. An underfill for encapsulating electronic components, comprising the resin composition described in claim 7.
  13. A method for producing an oxide powder according to any one of claims 1 to 5, The process includes: (a) providing raw material powder for spheroidization treatment, and (b) performing spheroidization treatment on the raw material powder obtained in (a) by flame melting or PVD to obtain oxide powder having a spheroidity of 0.7 or more and 1.0 or less. A method for producing oxide powder, wherein step (a) includes any of the following (i) to (iii): (i) To provide a mixed powder, which is a raw material powder for spheroidization treatment, by mixing a raw material compound containing the constituent elements of an oxide powder with a binder; (ii) To provide a raw material powder for spheroidization treatment in the form of a dried powder by mixing a solution containing a raw material compound containing the constituent elements of an oxide powder, allowing it to precipitate, and drying the precipitate; or (iii) To provide a raw material powder for spheroidization treatment in the form of an oxide powder by calcining a mixture of raw material compounds containing the constituent elements of an oxide powder at least once.
  14. The manufacturing method according to claim 13, wherein the flame melting or PVD in step (b) is carried out in a temperature range above the melting point of the raw material powder.
  15. The manufacturing method according to claim 13, further comprising a step of annealing at a temperature range of 100°C to 900°C after step (b).

Description

Oxide powder This invention relates to a novel oxide powder having a spherical particle shape. Furthermore, it relates to a resin composition and powder mixture containing the spherical oxide powder. Moreover, it relates to a method for producing the spherical oxide powder. In recent years, in technological fields requiring high precision, such as highly advanced electronic and optical equipment, fuel cells, and sensors, there has been a strong demand for controlling and suppressing the thermal expansion of solid materials. In particular, when constructing precision equipment such as semiconductor devices that require nanometer-level precision by combining multiple materials, differences in the thermal expansion coefficients between materials can lead to serious problems such as misalignment, interfacial delamination, disconnection, warping, and cracking. Therefore, technologies for highly precise control of thermal expansion are required. While many materials expand with increasing temperature, it is also known that there are rare negative thermal expansion materials that have the property of decreasing in volume with increasing temperature. As one technique for controlling the thermal expansion of precision instruments, a technique that controls the overall thermal expansion coefficient of an instrument is attracting attention, for example, by adding a negative thermal expansion material to a matrix material (resin, glass, metal, etc.) with a large positive thermal expansion coefficient, in combination with a material with a low positive thermal expansion coefficient (e.g., silica) as needed. Examples of negative thermal expansion materials include β-eucryptite, zirconium tungstate ( ZrW₂O ₸ ), zirconium tungstate phosphate ( Zr₂WO₄ ( PO₄ ) ₂ ), ZnxCd₁ -x ( CN) ₂ , manganese nitride, and bismuth nickel iron oxide. For example, Patent Document 1 reports a method for synthesizing a negative thermal expansion material Zr(1-x ) XxW2O8 (where X is a substitution element for zirconium Zr, 0≦x＜＜1), characterized by mixing a raw material in a stoichiometric ratio such that the sum of tungsten trioxide WO3 in a molar ratio of 2 with zirconium oxide ZrO2 and a substitution element X corresponding to the substitution amount x is in a molar ratio of 1 , forming a powder with a polarized particle size distribution consisting of small particles with a particle size within a predetermined range and large particles with a particle size within a predetermined range, and then placing the raw material powder into a desired mold and sintering it. Patent Document 1 states that this synthesis method has the effect of being able to synthesize large, high-density heat-shrinkable ceramics without press molding the raw material powder. In addition to Patent Document 1, development is underway on new negative thermal expansion materials with various compositions and properties, as well as methods for manufacturing them. Figure 1 is an SEM image of the oxide powder 1 obtained in Example 1.Figure 2 is an SEM image of the oxide powder 3 obtained in Example 3.Figure 3 is an SEM image of the raw material powder of Comparative Example 1.Figure 4 is a graph showing the paste viscosity at different shear rates for the examples and comparative examples. <Oxide powder> The oxide powder of the present invention is An oxide powder comprising at least one element selected from the group consisting of Cu, Zn, V, Mg, P, and S, The sphericity of the oxide powder is 0.7 or more and 1.0 or less. The oxide powder has a temperature range in which the dimensional change ratio (ΔL/L) is less than 0 in a temperature range of at least 0°C to 200°C, or a temperature range in which the coefficient of linear expansion (α) is less than 0 ppm/K in a temperature range of at least 0°C to 200°C. The oxide powder may contain at least one element selected from the group consisting of Cu, Zn, V, Mg, P, and S (hereinafter referred to as "Element A" for simplicity), which may encompass any combination of two or more of these elements. In oxide powders, when element A contains only one element, it may be Cu alone, Zn alone, V alone, Mg alone, P alone, or S alone. In oxide powders, when element A includes a combination of two elements, it may be a combination of Cu/Zn, Cu/V, Cu/Mg, Cu/P, Cu/S, Zn/V, Zn/Mg, Zn/P, Zn/S, V/Mg, V/P, V/S, Mg/P, Mg/S, or P/S. In oxide powders, when element A includes a combination of three elements, one of the following combinations can be selected: Cu/Zn/V, Cu/Zn/Mg, Cu/Zn/P, Cu/Zn/S, Cu/V/Mg, Cu/V/P, Cu/V/S, Cu/Mg/P, Cu/Mg/S, Cu/P/S, Zn/V/Mg, Zn/V/P, Zn/V/S, Zn/Mg/P, Zn/Mg/S, Zn/P/S, V/Mg/P, V/Mg/S, V/P/S, or Mg/P/S. In an oxide powder according to a preferred embodiment, element A may contain Zn, Mg, and P as a combination of three elements. It is more preferable that element A consists of Zn, Mg, and P. In oxide powders, when element A encompasses a combination of four elements, one of the following combinations can be selected: Cu/Zn/V/M