WO2022202740A1 - 超臨界水利用装置用チタン合金 - Google Patents

超臨界水利用装置用チタン合金 Download PDF

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Publication number
WO2022202740A1
WO2022202740A1 PCT/JP2022/012956 JP2022012956W WO2022202740A1 WO 2022202740 A1 WO2022202740 A1 WO 2022202740A1 JP 2022012956 W JP2022012956 W JP 2022012956W WO 2022202740 A1 WO2022202740 A1 WO 2022202740A1
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based material
sample
test
crucible
supercritical
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English (en)
French (fr)
Japanese (ja)
Inventor
佳明 戸田
仁奈 小畠
元彰 盛田
悠平 間仁田
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National Institute for Materials Science
Tokyo University of Marine Science and Technology NUC
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National Institute for Materials Science
Tokyo University of Marine Science and Technology NUC
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Priority to JP2023509164A priority Critical patent/JPWO2022202740A1/ja
Priority to CN202280025108.9A priority patent/CN117083404A/zh
Publication of WO2022202740A1 publication Critical patent/WO2022202740A1/ja
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium

Definitions

  • the present invention relates to an apparatus for handling supercritical water, and more particularly to a metal material having corrosion resistance, particularly a titanium alloy, which can be applied to an apparatus for handling supercritical water.
  • Supercritical water is in the state of water under high temperature and high pressure, with a temperature of 374.15° C. or higher and a pressure of 22.12 MPa or higher, and has different characteristics from water and steam under atmospheric pressure. Therefore, the oxidation/corrosion phenomenon of metal materials by supercritical water may be different from the oxidation/corrosion phenomenon by water or water vapor. Therefore, it is necessary to improve the corrosion resistance to supercritical water for the members constituting the device for handling supercritical water (hereinafter also referred to as the supercritical water utilization device).
  • Patent document 1 states that pure titanium specified by JIS Classes 1 to 3 or pure titanium specified by ASTM Grades 1 to 4 should be used as materials for containers, pipes, etc. of supercritical water utilization equipment. is disclosed. However, these pure titaniums are allowed to have only a maximum dissolved oxygen content of 0.4% by mass (ASTM Grade 4). In addition, even in pure titanium defined by JIS Class 4, the solid solution oxygen content is 0.4% by mass or less. Advanced refining such as the Kroll method is required to reduce the amount of dissolved oxygen from titanium oxide contained in raw ore and scrap titanium to the above allowable value, and the production of pure titanium is laborious and costly. .
  • Patent Document 2 discloses a titanium-oxygen-based material (Ti- O-based materials) are disclosed.
  • Cited Document 2 does not suggest the corrosion resistance of the rolled plate material of this Ti—O-based material.
  • the present invention expands the applicability of Ti—O-based materials with reduced refining costs by using Ti—O-based materials containing oxygen as a chemical component as materials for devices that handle supercritical water. for the purpose.
  • the Ti—O-based material of the present invention is a Ti—O-based material containing oxygen as a chemical component, the oxygen content being 0.05% by mass or more and 3.0% by mass or less, and the balance being titanium.
  • a crucible containing unavoidable impurities and containing a sample made of the Ti—O-based material or a sample made of pure titanium and an empty crucible containing no sample are placed in a reactor.
  • the weight increment per unit area of the Ti—O-based material sample later is equal to or less than the weight increment per unit area of the pure titanium sample, thereby achieving the above object.
  • the Ti—O-based material is measured from a scanning electron microscope (SEM) image of the cross section of the sample after the supercritical hydroxylation test. It is preferably equal to or less than the thickness of the oxide film of the sample made of pure titanium.
  • the Ti—O-based material preferably has an oxygen content of more than 0.4% by mass and 2.0% by mass or less.
  • the Ti—O-based material more preferably has an oxygen content of 1.0% by mass or more and 2.0% by mass or less.
  • the above supercritical hydroxylation test is In a reactor in which a crucible containing a sample made of the Ti—O-based material or a sample made of pure titanium and an empty crucible containing no sample are installed, the dissolved oxygen content is 0.01 mg / L or less, and the electrical conductivity is 0.01 mg / L or less. Pure water adjusted to 0.08 mS / cm or less is injected, and the reactor is heated to 500 ° C in an electric furnace, and the inside of the reactor is pressurized to a range of 22.12 MPa or more and 23 MPa or less with a high-pressure metering pump to make it supercritical.
  • the pure titanium is specified by JIS or ASTM standards, and is preferably selected from the group consisting of JIS Classes 1 to 4 and ASTM Grades 1 to 4.
  • the weight increment per unit area of the sample made of the Ti—O-based material and the sample made of pure titanium was determined by roughly polishing the entire surface of the sample to be subjected to the supercritical hydroxylation test with water-resistant abrasive paper. After adjusting the surface roughness to a degree, the length, width, and thickness of each sample are measured with a micrometer to the nearest 1 ⁇ m, and the total surface area of each sample is calculated, After degreasing and washing the samples, place the samples one by one in a crucible and dry them in a dryer, then weigh the weight of each sample with an electronic balance to the nearest 0.1 mg, Weigh the empty crucible dried in the dryer with an electronic balance to the nearest 0.1 mg, After the test, the crucible containing the sample and the empty crucible are weighed to the nearest 0.1 mg with an electronic balance, It is preferably calculated by dividing the value obtained by subtracting the weight increase of the empty crucible from the weight difference of each sample weighed together with the crucible before and after the
  • the Ti—O-based material may be produced by a method selected from the group consisting of casting, additive manufacturing, sintering, rolling, forging, drawing, and extrusion.
  • the Ti—O-based material may be a cast material, an additive manufacturing material, or a sintered material, and is preferably a cast material.
  • One aspect of the present invention provides a supercritical water utilization apparatus using the Ti—O-based material.
  • a casting material for supercritical water utilization equipment using the Ti—O-based material is provided.
  • another aspect of the present invention provides use of the Ti—O-based material in a supercritical water utilization apparatus.
  • oxygen which has been recognized as a harmful component in terms of corrosion resistance in conventional titanium alloy materials, is effectively used as an alloying element, and a Ti—O-based material with reduced refining costs can be used in supercritical water. It can be used as a material for equipment.
  • FIG. 2 is a diagram showing a SEM image of a cross section of each test piece after a supercritical hydroxylation test in Test 1 of Example.
  • the Ti—O-based material of the present invention is a Ti—O-based material containing oxygen as a chemical component, and a crucible containing a sample made of the Ti—O-based material or a sample made of pure titanium and a sample not containing the sample.
  • the weight increase per unit area of the sample made of the Ti—O-based material after the test is equal to the weight increase per unit area of the sample made of pure titanium. is less than or equal to the weight increment of
  • the pure titanium to be subjected to the supercritical hydroxylation test is specified by JIS or ASTM standards, and is preferably selected from the group consisting of JIS Classes 1 to 4 and ASTM Grades 1 to 4.
  • the Ti—O-based material of the present invention has a corrosion resistance to supercritical water equivalent to or higher than that of pure titanium defined by JIS or ASTM standards, so it can be used as a member constituting a supercritical water utilization device. suitable for use.
  • the Ti—O-based material of the present invention has a thickness of the oxide film of the sample made of the Ti—O-based material measured from a scanning electron microscope (SEM) image of the cross section of the sample after the supercritical hydroxylation test.
  • the thickness is preferably equal to or less than the thickness of the oxide film of the sample made of pure titanium.
  • a Ti—O-based material that satisfies both the weight increment per unit area of the sample after the test and the thickness of the oxide film is more suitable for use as a member constituting a supercritical water utilization apparatus.
  • the thickness of the oxide film of the sample made of Ti—O-based material and the sample made of pure titanium after the supercritical hydroxylation test is different in the scanning electron microscope (SEM) image of the cross section of the target sample.
  • SEM scanning electron microscope
  • At least a sample made of a Ti—O-based material or a sample made of pure titanium to be tested can be exposed to supercritical water for a certain period of time in a crucible installed in a reactor.
  • any test equipment and test conditions can be set. Specific test examples will be described in the examples described later, but preferred embodiments are, for example, as follows.
  • the time for exposing the sample contained in the crucible in the reactor to supercritical water is not particularly limited, and may be, for example, 50.0 hours or 50.0 hours or more. Also, the time condition of less than 50.0 hours may be set according to the characteristics of the supercritical water utilization equipment to which the target Ti—O-based material is applied. In the examples described later, as representative examples, test examples in which the time for exposing the sample contained in the crucible in the reactor to supercritical water was set to 50.0 hours, 25.0 hours, and 1.75 hours will be described. do.
  • a sample made of a Ti—O-based material or a sample made of pure titanium is exposed to supercritical water for a certain period of time in a crucible placed in a reactor.
  • the subcritical region is necessarily passed through in the process of achieving the supercritical state, so the sample subjected to the test is exposed to subcritical water for a certain period of time.
  • the sample to be tested is also exposed to constant high-temperature and high-pressure water or steam for a certain period of time.
  • the Ti—O-based material of the present invention exhibits corrosion resistance to supercritical water, more specifically, corrosion resistance to supercritical water at a temperature of 374.15° C. or higher and 500° C. or lower and a pressure of 22.12 MPa or higher and 23 MPa or lower.
  • corrosion resistance to supercritical water more specifically, corrosion resistance to supercritical water at a temperature of 374.15° C. or higher and 500° C. or lower and a pressure of 22.12 MPa or higher and 23 MPa or lower.
  • subcritical water that is, subcritical water
  • water or steam under conditions of temperature and pressure higher than normal temperature and pressure could be.
  • the Ti—O-based material of the present invention having such properties can be used not only as a member that constitutes a supercritical water utilization device, but also as a member that constitutes a device that handles subcritical water. Since it can be useful as a component for equipment that handles water or steam under temperature and pressure conditions, it is expected that the availability of Ti—O-based materials with reduced refining costs will be further expanded. is.
  • the Ti—O-based material of the present invention contains a certain amount of oxygen (O) as a chemical component, with the balance being titanium and unavoidable impurities.
  • the oxygen content may be 0.4% by mass or less, which corresponds to pure titanium specified by JIS or ASTM standards, but it takes time and effort to prepare the material. In terms of cost, an excessively small amount may not be practically desirable.
  • the solid solution oxygen content of pure titanium defined by JIS or ASTM standards is up to 0.4% by mass (JIS Class 4, ASTM Grade 4). In O-based materials, the oxygen content may be greater than 0.4% by mass.
  • the oxygen content is 0.01% by mass or more and 10.0% by mass or less, preferably 0.03% by mass or more and 7.5% by mass or less, more preferably 0.03% by mass or more and 7.5% by mass or less. 05% by mass or more and 5.0% by mass or less, more preferably 0.05% by mass or more and 3.0% by mass or less, even more preferably 0.4% by mass or more and 2.0% by mass or less, and More preferably, it is 1.0% by mass or more and 2.0% by mass or less.
  • the Ti—O-based material of the present invention having such a component composition can be produced using conventional metal material production and processing methods.
  • Manufacturing and processing methods applicable to the Ti—O-based material of the present invention include, but are not limited to, casting, additive manufacturing, sintering, rolling, forging, drawing, and extrusion. Among them, casting, additive manufacturing, and sintering are preferable, and casting is more preferable from a practical viewpoint.
  • the Ti—O-based material according to one embodiment of the present invention is produced using a casting method, whereby the Ti—O-based material of the present invention is produced as a cast material, and using the cast material, Casting materials for supercritical water utilization equipment can be produced. These casting materials can be suitably used as members constituting a supercritical water utilization apparatus.
  • Ti—O-based material As a chemical component, it contains 0.05%, 1.0%, 2.0%, 3.0%, 4.0%, and 5.0% oxygen in mass%, and the balance is titanium and unavoidable Ingots of six types of Ti—O-based materials containing impurities were melted. In the following, in order to distinguish each Ti—O-based material, Ti-0.05% O, Ti-1.0% O, Ti-2.0% O, Ti Also referred to as Ti-3.0%O, Ti-4.0%O, and Ti-5.0%O.
  • a strip-shaped test piece having a length of 20 mm, a width of 10 mm, and a thickness of 2 mm was cut out as a sample for the supercritical hydroxylation test. All test pieces were adjusted to have the same degree of surface roughness. The length, width and thickness of each specimen were then measured with a micrometer to the nearest 1 ⁇ m to calculate the total surface area of each specimen.
  • test pieces After degreasing and washing the test pieces, they were placed one by one in an alumina crucible with a diameter of 26 mm and a depth of 19 mm, and dried in a dryer. Thereafter, the weight of each test piece together with the crucible was weighed to the nearest 0.1 mg using an electronic balance.
  • an empty crucible containing no test piece was also dried with a dryer and weighed to the nearest 0.1 mg with an electronic balance.
  • a crucible containing a test piece and an empty crucible not containing a test piece were placed in a reactor made of Hastelloy C276 and having a volume of 2.8 L. Pure water adjusted to 08 mS/cm or less was injected. Then, the reactor was heated to 500° C. in an electric furnace, and the inside of the reactor was pressurized to about 23 MPa by a high-pressure metering pump to achieve a supercritical state.
  • the temperature inside the reactor was lowered and the pressure was reduced, and after replacement with argon gas, the crucible containing the test piece and the test piece were not contained.
  • the empty crucible was removed and weighed to the nearest 0.1 mg on an electronic balance.
  • the weight increment per unit area was calculated by dividing the value obtained by subtracting the weight increase of the empty crucible from the weight difference of each test piece weighed together with the crucible before and after the above test by the total surface area of each test piece.
  • the weight increment per unit area of each test piece was 16.55 ⁇ g/mm 2 (Ti-0.05% O), 15.37 ⁇ g/mm 2 (Ti-1.0% O), 14.03 ⁇ g. /mm 2 (Ti-2.0% O), 16.55 ⁇ g/mm 2 (Ti-3.0% O), 38.29 ⁇ g/mm 2 (Ti-4.0% O), and 62.65 ⁇ g/mm mm 2 (Ti-5.0% O).
  • Ti-0.05% O is pure titanium corresponding to JIS Class 1 or ASTM Grade 1 from its oxygen content.
  • the Ti—O-based material having a content of 0% by mass or less has a weight increment per unit area of the test piece after the supercritical hydroxylation test, which is less than or equal to the weight increment per unit area of the test piece made of pure titanium. confirmed.
  • each test piece after the above test was observed (analyzed) by an optical microscope, SEM/EDX (scanning electron microscope/energy dispersive X-ray analyzer), and XRD (X-ray diffractometer). .
  • FIGS. 1(a) to (f) are respectively Ti-0.05% O, Ti-1.0% O, Ti-2.0% O, Ti-3.0% O, Ti-4.0 1 is a diagram showing SEM images of the cross section of each test piece after a supercritical hydroxylation test for % O and Ti-5.0% O.
  • FIG. The scale bar shown in FIG. 1(a) is 4 ⁇ m, and FIGS. 1(b)-(f) have similar magnifications.
  • the approximate range of the portion corresponding to the oxide film is indicated by double-headed arrows for easy understanding.
  • the thickness of the oxide film of each test piece measured from two different fields of view of the SEM images of FIGS. Average value is 10.3 ⁇ m (Ti-0.05% O), 9.02 ⁇ m (Ti-1.0% O), 10.3 ⁇ m (Ti-2.0% O), 11.6 ⁇ m ( Ti-3.0% O), 20.1 ⁇ m (Ti-4.0% O), and 17.1 ⁇ m (Ti-5.0% O).
  • the Ti—O-based material having an oxygen content of 0.05% by mass or more and 2.0% by mass or less has a weight increase per unit area of the test piece after the supercritical hydroxylation test, from pure titanium
  • the thickness of the oxide film of the test piece after the supercritical hydroxylation test is equal to or less than the thickness of the oxide film of the test piece made of pure titanium.
  • titanium-oxygen-based materials containing a certain amount of oxygen as an alloying element in titanium alloy materials can have corrosion resistance to supercritical water, and the corrosion resistance is defined by JIS or ASTM standards. It has been found that it can be comparable to, or even better than, pure titanium used. This means that not only the Ti—O-based material having the same oxygen content as that of pure titanium, but also the upper limit of 0.4% by mass of solid solution oxygen content specified by the JIS or ASTM standards for pure titanium. This means that the Ti—O-based material exceeding the above can also be used as a member constituting a supercritical water utilization apparatus.
  • the weight increment per unit area of the test piece after the above test was 11.09 ⁇ g/mm 2 (Ti-0.05% O) and 7.85 ⁇ g/mm 2 (Ti-1.0% O), Compared to Ti-0.05% O, Ti-1.0% O showed a smaller weight increase per unit area of the test piece after the supercritical hydroxylation test.
  • 9Cr steel and carbon steel are 15 ⁇ g/mm 2 or more and 30 ⁇ g/mm 2 or more, respectively, and the results obtained with Ti-0.05% O and Ti-1.0% O are It was significantly smaller than the known 9Cr steel, and the difference with carbon steel was clear.
  • titanium-oxygen-based material containing a certain amount of oxygen as an alloy element by adjusting the oxygen content, can be used as a member exposed to supercritical water for a time shorter than 50.0 hours. was suggested to be useful.
  • the weight increment per unit area of the test piece after the above test was 5.69 ⁇ g/mm 2 (Ti-0.05% O) and 4.24 ⁇ g/mm 2 (Ti-1.0% O), Compared to Ti-0.05% O, Ti-1.0% O showed a smaller weight increase per unit area of the test piece after the supercritical hydroxylation test.
  • titanium-oxygen materials containing a certain amount of oxygen as an alloying element can be useful as members exposed to supercritical water for about 2.0 hours by adjusting the oxygen content. gender was suggested.
  • oxygen which has been recognized as a harmful component in terms of corrosion resistance, is effectively used as an alloying element to reduce refining costs. Since it can be used as a material for equipment to be handled, it is possible to provide a material for supercritical water utilization equipment at a low cost, and it is expected to expand the industrial applicability of supercritical water.

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PCT/JP2022/012956 2021-03-26 2022-03-22 超臨界水利用装置用チタン合金 Ceased WO2022202740A1 (ja)

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JP2014506293A (ja) * 2010-12-22 2014-03-13 サンドビック インテレクチュアル プロパティー アクティエボラーグ キャスティングによるナノ双晶形成チタン材料の作製方法
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