JP2020121890A - Impregnation crucible - Google Patents
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- JP2020121890A JP2020121890A JP2019012901A JP2019012901A JP2020121890A JP 2020121890 A JP2020121890 A JP 2020121890A JP 2019012901 A JP2019012901 A JP 2019012901A JP 2019012901 A JP2019012901 A JP 2019012901A JP 2020121890 A JP2020121890 A JP 2020121890A
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- 238000005470 impregnation Methods 0.000 title claims abstract description 55
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 52
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 48
- 239000011148 porous material Substances 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 72
- 238000001035 drying Methods 0.000 claims description 5
- 239000004111 Potassium silicate Substances 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 235000010338 boric acid Nutrition 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 235000019794 sodium silicate Nutrition 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 229910002804 graphite Inorganic materials 0.000 description 11
- 239000010439 graphite Substances 0.000 description 11
- 239000011521 glass Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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Abstract
Description
本発明は含浸坩堝に関する。 The present invention relates to an impregnating crucible.
アルミニウムや銅合金等の非鉄金属の溶解精錬や溶融金属の容器として熱伝導性に優れ、耐熱衝撃に強い黒鉛坩堝が用いられている。
黒鉛坩堝は、熱伝導率が高く、熱膨張率が小さい鱗状黒鉛と、熱伝導率の高い炭化珪素からなる骨材に酸化防止成分としてシリコンやガラス成分を添加した坩堝材料をバインダーカーボンとともに混錬し、成形及び還元焼成して製造される。
BACKGROUND ART A graphite crucible that has excellent thermal conductivity and is resistant to thermal shock is used as a container for melting and refining non-ferrous metals such as aluminum and copper alloys and a molten metal.
The graphite crucible is a kneaded crucible material with binder carbon in which scaly graphite having a high thermal conductivity and a small thermal expansion coefficient and an aggregate made of silicon carbide having a high thermal conductivity are added with silicon and a glass component as an antioxidant component. Then, it is manufactured by molding and reduction firing.
坩堝材料の黒鉛は多孔性であるため機械的強度が十分ではなく、容易に酸化される。黒鉛の酸化が進行すると材質の脆化で黒鉛坩堝に変形や割れを来す。 Since graphite as a crucible material is porous, it has insufficient mechanical strength and is easily oxidized. As the oxidation of graphite progresses, the material becomes brittle and the graphite crucible is deformed or cracked.
そこで、黒鉛の酸化を防止するため、坩堝材料を焼成後、気孔中にガラス成分を含浸させ、表面にガラスを塗布し、焼き付けてガラス化しているが、ガラス成分の浸透は坩堝材料の厚みの２５パーセント程度であった。 Therefore, in order to prevent the oxidation of graphite, after firing the crucible material, the glass component is impregnated in the pores, the surface is coated with glass and baked to vitrify, but the penetration of the glass component depends on the thickness of the crucible material. It was about 25 percent.
黒鉛坩堝の使用中に温度が十分上がらない坩堝上部においては、気孔中のガラス成分が溶融せず、ガラス化した表面であっても溶融しないため、微細な亀裂をエアが通過してしまう。その結果、坩堝材料中の黒鉛の酸化が進行し、黒鉛坩堝の使用寿命が短くなるという問題点がある。
本発明は上記問題点に鑑み、使用寿命の向上した含浸坩堝を提供することを目的とする
In the upper part of the crucible, where the temperature does not rise sufficiently during use of the graphite crucible, the glass component in the pores does not melt, and even the vitrified surface does not melt, so that air passes through the fine cracks. As a result, there is a problem that the graphite in the crucible material is oxidized and the service life of the graphite crucible is shortened.
In view of the above problems, it is an object of the present invention to provide an impregnated crucible having an improved service life.
請求項１に記載の発明に係る含浸坩堝は、
成形して還元焼成した坩堝材料の気孔中に酸化防止溶液を含浸させた含浸坩堝であって、
空の含浸槽に前記還元焼成した坩堝材料を入れて含浸槽の内部を減圧する減圧工程と、
減圧した含浸槽に前記酸化防止溶液としてガラス成分の溶液を充填する充填工程と、
酸化防止溶液の溶液を充填した含浸槽の内部を加圧して坩堝材料の気孔中に酸化防止溶液を含浸させる加圧工程と、
気孔中に酸化防止溶液を含浸させた後、含浸槽を大気に開放するとともに、含浸槽から酸化防止溶液の溶液を排出して、坩堝材料を取り出す開放工程を経て製造したことを特徴とする。
The impregnated crucible according to the invention of claim 1
An impregnated crucible in which pores of a crucible material that has been molded and reduction-fired are impregnated with an antioxidant solution,
A decompression step of putting the reduction-fired crucible material in an empty impregnation tank to decompress the inside of the impregnation tank;
A filling step of filling a solution of a glass component as the antioxidant solution in a reduced pressure impregnation tank,
A pressurizing step of pressurizing the inside of the impregnation tank filled with the solution of the antioxidant solution to impregnate the antioxidant solution into the pores of the crucible material,
After the pores are impregnated with the antioxidant solution, the impregnation tank is opened to the atmosphere, the solution of the antioxidant solution is discharged from the impregnation tank, and the crucible material is taken out.
請求項２に記載の発明は、請求項１に記載の含浸坩堝において、
前記開放工程で含浸槽から取り出した坩堝材料を乾燥する乾燥工程と、
前記乾燥させた坩堝材料を前記含浸槽に入れて含浸槽の内部を減圧する再減圧工程と、
減圧した含浸槽に前記酸化防止溶液を充填する再充填工程と、
酸化防止溶液の溶液を充填した含浸槽の内部を加圧して坩堝材料の気孔中に酸化防止溶液を含浸させる再加圧工程と、
気孔中に酸化防止溶液を含浸させた後、含浸槽を大気に開放するとともに、含浸槽から酸化防止溶液の溶液を排出して、坩堝材料を取り出す再開放工程を経て製造したことを特徴とする。
The invention according to claim 2 provides the impregnating crucible according to claim 1,
A drying step of drying the crucible material taken out from the impregnation tank in the opening step,
A re-decompression step of putting the dried crucible material into the impregnation tank and decompressing the inside of the impregnation tank,
A refilling step of filling the reduced pressure impregnation tank with the antioxidant solution,
A re-pressurizing step in which the inside of the impregnation tank filled with the solution of the antioxidant solution is pressurized to impregnate the antioxidant solution into the pores of the crucible material,
After impregnating the pores with the antioxidant solution, the impregnation tank is opened to the atmosphere, the solution of the antioxidant solution is discharged from the impregnation tank, and the crucible material is taken out through a re-opening process. ..
そして、好ましくは、前記ガラス成分として、硼砂、硼酸、ケイ酸ナトリウム、ケイ酸カリウムを使用する。 And, as the glass component, borax, boric acid, sodium silicate, and potassium silicate are preferably used.
請求項１に記載の発明によれば、酸化防止溶液の溶液を充填した含浸槽に坩堝材料を入れて加圧する加圧工程に先行して、空の含浸槽に坩堝材料を入れて減圧し、その後加圧するので、酸化防止溶液が坩堝材料の気孔中に十分浸透する。そのため、酸化防止溶液を坩堝材料の厚みの８０％以上に浸透させることも可能となり、坩堝材料の気孔率を低下させ、坩堝材料の高密度化を図ることができ、強度向上、耐酸化性を向上させることができるので、予めガラス成分を坩堝材質の原料として配合に入れる必要がなくなる。 According to the invention described in claim 1, prior to the pressurizing step of putting the crucible material in the impregnation tank filled with the solution of the antioxidant solution and pressurizing the crucible material, the crucible material is put in the empty impregnation tank to reduce the pressure, Since pressure is applied thereafter, the antioxidant solution sufficiently penetrates into the pores of the crucible material. Therefore, it becomes possible to permeate the antioxidant solution into 80% or more of the thickness of the crucible material, reduce the porosity of the crucible material, and increase the density of the crucible material, thereby improving the strength and oxidation resistance. Since it can be improved, it is not necessary to add a glass component as a raw material for the crucible material to the compound in advance.
請求項２に記載の発明によれば、減圧工程、充填工程、加圧工程及び開放工程を経て酸化防止溶液を気孔中に含浸させた坩堝材料を乾燥した後、再度、減圧工程、充填工程、加圧工程及び開放工程を実施するのでより一層、酸化防止溶液を厚みの奥深くまで浸透させることができる。 According to the invention described in claim 2, after drying the crucible material having the pores impregnated with the antioxidant solution through the depressurizing step, the filling step, the pressurizing step and the opening step, the depressurizing step, the filling step, Since the pressurizing step and the releasing step are carried out, the antioxidant solution can be further penetrated deep into the thickness.
以下に本発明を図面に基づき説明する。図１には鱗状黒鉛と炭化珪素からなる骨材に酸化防止成分を添加し、バインダーカーボンとともに混錬し、成形及び還元焼成した坩堝材料の気孔中に酸化防止溶液を含浸させる含浸坩堝の製造工程の一実施例が示されている。 The present invention will be described below with reference to the drawings. FIG. 1 shows a manufacturing process of an impregnated crucible in which an antioxidant component is added to an aggregate composed of scaly graphite and silicon carbide, kneaded together with binder carbon, and the pores of a crucible material formed and reduced and fired are impregnated with an antioxidant solution An example of is shown.
当該製造工程は、含浸槽１１と酸化防止溶液の溶液１２を溜める溶液タンク１３を使用し、含浸槽１１と溶液タンク１３が管路１４で接続され、含浸槽は加熱・冷却ジャケット１５で包まれている。
溶液タンク１３には酸化防止溶液として硼砂、硼酸、ケイ酸ナトリウム、ケイ酸カリウムのいずれかの水溶液が充填されている。
In the manufacturing process, the
The
製造工程は、空の含浸槽１１に還元焼成した坩堝材料１０を入れて含浸槽１１の内部を減圧する減圧工程（Ａ）と、減圧した含浸槽１１に溶液タンク１３から管路１４を通して酸化防止溶液の溶液１２を充填する充填工程（Ｂ）と、酸化防止溶液の溶液１２を充填した含浸槽１１の内部を加圧して坩堝材料１０の気孔中に酸化防止溶液を含浸させる加圧工程（Ｃ）と、含浸槽１１で気孔中に酸化防止溶液を含浸させた後、含浸槽１１を大気に開放するとともに、含浸槽１１から管路１４を通して酸化防止溶液の溶液１２を溶液タンク１３に戻し、含浸槽１１から坩堝材料１０を取り出す開放工程（Ｄ）からなる。
しかして本実施例の減圧工程（Ａ）では真空度１５ｋＰａ以下まで減圧している。また、加圧工程（Ｂ）では０．５ＭＰａ以上に加圧している。
The manufacturing process includes a decompression step (A) in which the reduced and fired
However, in the depressurizing step (A) of this embodiment, the degree of vacuum is reduced to 15 kPa or less. In the pressurizing step (B), the pressure is 0.5 MPa or more.
上述した製造工程により酸化防止溶液を含浸させた坩堝材料１０で製造した含浸坩堝の物性調査の結果を表１に示す。
Table 1 shows the results of the physical property investigation of the impregnated crucible manufactured from the
使用後品は未含浸の使用後品に比べると、上端は酸化の影響により、気孔率の上昇、嵩比重の低下、固定炭素の低下が確認されるが、強度の低下は確認されない。
胴部、底部については気孔率の低下、嵩比重の上昇、強度の上昇が確認できる。
The post-use product has a higher porosity, a lower bulk specific gravity, and a lower fixed carbon due to the effect of oxidation at the upper end than the non-impregnated post-use product, but the strength is not confirmed.
Regarding the body and bottom, a decrease in porosity, an increase in bulk specific gravity, and an increase in strength can be confirmed.
本実施例に係る含浸坩堝の製造工程によれば、酸化防止溶液の溶液１２を充填した含浸槽１１に坩堝材料１０を入れて加圧する加圧工程（Ｂ）に先行して、空の含浸槽１１に坩堝材料１０を入れて減圧し、その後加圧するので、酸化防止溶液が坩堝材料１０の気孔中に十分浸透する。そのため、酸化防止溶液を坩堝材料１０の厚みの８０％以上浸透させることも可能となり、坩堝材料１０の気孔率を低下させ、坩堝材料１０の高密度化を図ることができるので、含浸坩堝の使用寿命が大きく向上する。
According to the manufacturing process of the impregnated crucible according to this example, the empty impregnation tank is preceded by the pressurizing step (B) in which the
上記実施例では、減圧工程（Ａ）、充填工程（Ｂ）、加圧工程（Ｃ）及び開放工程（Ｄ）を各１回実施するが、開放工程で取り出した坩堝材料を乾燥した後、減圧工程（Ａ）、充填工程（Ｂ）、加圧工程（Ｃ）及び開放工程（Ｄ）を再度実施することにより、より一層酸化防止溶液を坩堝材料１０の厚みの奥深くまで含浸させることができる。その場合、先の製造工程で使用した酸化防止溶液の溶液１２とは異なる酸化防止溶液の溶液を使用することもできる。
In the above example, the depressurizing step (A), the filling step (B), the pressurizing step (C), and the releasing step (D) are performed once, but after the crucible material taken out in the releasing step is dried, the depressurizing step is performed. By performing the step (A), the filling step (B), the pressurizing step (C), and the opening step (D) again, the antioxidant solution can be further impregnated deeper into the thickness of the
１０…坩堝材料
１１…含浸槽
１２…酸化防止溶液の溶液
１３…溶液タンク
10... Crucible
Claims (4)
空の含浸槽に前記還元焼成した坩堝材料を入れて含浸槽の内部を減圧する減圧工程と、
減圧した含浸槽に前記酸化防止溶液の溶液を充填する充填工程と、
酸化防止溶液の溶液を充填した含浸槽の内部を加圧して坩堝材料の気孔中に酸化防止溶液を含浸させる加圧工程と、
気孔中に酸化防止溶液を含浸させた後、含浸槽を大気に開放するとともに、含浸槽から酸化防止溶液の溶液を排出して、坩堝材料を取り出す開放工程を経て製造したことを特徴とする含浸坩堝。 An impregnated crucible in which pores of a crucible material that has been molded and reduction-fired are impregnated with an antioxidant solution,
A decompression step of putting the reduction-fired crucible material in an empty impregnation tank to decompress the inside of the impregnation tank;
A filling step of filling the reduced pressure impregnation tank with a solution of the antioxidant solution,
A pressurizing step of pressurizing the inside of the impregnation tank filled with the solution of the antioxidant solution to impregnate the antioxidant solution into the pores of the crucible material,
After impregnating the pores with the antioxidant solution, the impregnation tank is opened to the atmosphere, the solution of the antioxidant solution is discharged from the impregnation tank, and the manufacturing process is carried out through an opening step of taking out the crucible material. crucible.
前記乾燥させた坩堝材料を前記含浸槽に入れて含浸槽の内部を減圧する再減圧工程と、
減圧した含浸槽に前記酸化防止溶液を充填する再充填工程と、
酸化防止溶液の溶液を充填した含浸槽の内部を加圧して坩堝材料の気孔中に酸化防止溶液を含浸させる再加圧工程と、
気孔中に酸化防止溶液を含浸させた後、含浸槽を大気に開放するとともに、含浸槽から酸化防止溶液の溶液を排出して、坩堝材料を取り出す再開放工程を経て製造したことを特徴とする請求項１に記載の含浸坩堝。 A drying step of drying the crucible material taken out from the impregnation tank in the opening step,
A re-decompression step of putting the dried crucible material into the impregnation tank and decompressing the inside of the impregnation tank,
A refilling step of filling the reduced pressure impregnation tank with the antioxidant solution,
A re-pressurizing step in which the inside of the impregnation tank filled with the solution of the antioxidant solution is pressurized to impregnate the antioxidant solution into the pores of the crucible material,
After impregnating the pores with the antioxidant solution, the impregnation tank is opened to the atmosphere, the solution of the antioxidant solution is discharged from the impregnation tank, and the crucible material is taken out through a re-opening process. The impregnated crucible according to claim 1.
The impregnating crucible according to claim 2, wherein a solution of an antioxidant solution different from the solution of the antioxidant solution filled in the filling step is filled in the impregnation tank.
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