JPH01201076A - Production of sintered compact having heat resistance and corrosion resistance - Google Patents
Production of sintered compact having heat resistance and corrosion resistanceInfo
- Publication number
- JPH01201076A JPH01201076A JP63249785A JP24978588A JPH01201076A JP H01201076 A JPH01201076 A JP H01201076A JP 63249785 A JP63249785 A JP 63249785A JP 24978588 A JP24978588 A JP 24978588A JP H01201076 A JPH01201076 A JP H01201076A
- Authority
- JP
- Japan
- Prior art keywords
- cr3c2
- tic
- sintering
- tin
- sintered compact
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000007797 corrosion Effects 0.000 title claims abstract description 13
- 238000005260 corrosion Methods 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000010304 firing Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 8
- 230000035939 shock Effects 0.000 abstract description 8
- 229910003470 tongbaite Inorganic materials 0.000 abstract description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052718 tin Inorganic materials 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 abstract 3
- 229910033181 TiB2 Inorganic materials 0.000 abstract 3
- 229910034327 TiC Inorganic materials 0.000 abstract 3
- 229910007948 ZrB2 Inorganic materials 0.000 abstract 3
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 abstract 3
- 229910003465 moissanite Inorganic materials 0.000 abstract 2
- 229910010271 silicon carbide Inorganic materials 0.000 abstract 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- -1 nickel or cobalt Chemical class 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009760 electrical discharge machining Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、耐熱耐食性焼結体の製造方法に関するもので
ある。本発明によって得られた焼結体は、加熱炉、均熱
炉などの工業用炉や溶融金属に対し優れた耐食性を備え
ているため熱電対の保護管等での使用が期待されるもの
である。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing a heat-resistant and corrosion-resistant sintered body. The sintered body obtained by the present invention has excellent corrosion resistance against industrial furnaces such as heating furnaces and soaking furnaces, and against molten metal, so it is expected to be used in thermocouple protection tubes, etc. be.
Ｃｒ、、Ｃｚ系セラミック材料は、従来、金属のニッケ
ルやコバルトで結合焼結したものや、各種酸化物、窒化
物、硼化物、炭化物、リン化物を焼結助剤として焼結し
たものが提案されている。そして、焼結助剤の添加量は
０．５〜１０重量％で焼成温度は１５００℃以下とされ
ている
（特開昭５９−１０７０５８号公報）。Conventionally, Cr, Cz-based ceramic materials have been proposed by bonding and sintering with metals such as nickel or cobalt, or by sintering with various oxides, nitrides, borides, carbides, and phosphides as sintering aids. has been done. The amount of the sintering aid added is 0.5 to 10% by weight, and the firing temperature is 1500° C. or lower (Japanese Patent Application Laid-Open No. 107058/1983).
しかしながら、耐食性が優れているだけでは実用上問題
が有り、耐熱衝撃性、耐摩耗性、高温強度等の物性が良
好であることが要求される。Ｃｒ５Ｃｚ系セラミツクで
これらの条件を全て満すものは無く、本発明はこれらの
点を全て改善したものである。これ迄に１つの改善例と
してＣｒ、Ｃ２の耐熱衝撃性を高めるために各種ウィス
カー、ファイバーを混入することが示されているが充分
な効果が得られていない。However, simply having excellent corrosion resistance is problematic in practice, and good physical properties such as thermal shock resistance, abrasion resistance, and high-temperature strength are required. There is no Cr5Cz ceramic that satisfies all of these conditions, and the present invention improves all of these points. Up to now, as an example of improvement, it has been shown that various whiskers and fibers are mixed in to improve the thermal shock resistance of Cr and C2, but sufficient effects have not been obtained.
耐熱衝撃性が良くないのはＣｒ５Ｃｚの熱膨張率が大き
いためであるので、これを改善するためには複合材をあ
る程度以上添加して本質的にＭｉ織を変える必要がある
。本発明は複合材の添加と焼成温度を従来より高くする
ことによって物性の改良に成功したものである。The thermal shock resistance is not good because Cr5Cz has a large coefficient of thermal expansion, so in order to improve this, it is necessary to add a certain amount of composite material to essentially change the Mi weave. The present invention has succeeded in improving the physical properties by adding a composite material and increasing the firing temperature than before.
すなわち、本発明は、ＺｒＢ、、ＴｉＢ、、Ｔｉｃ。 That is, the present invention relates to ZrB, TiB, Tic.
ＳｉＣ及びＴｉＮから選ばれた１種以上が０．５〜５０
重量％で残部が実質的にＣｒ、Ｃ，である混合物を温度
１６００℃以上で焼成することを特徴とする耐熱耐食性
焼結体の製造方法である。One or more selected from SiC and TiN is 0.5 to 50
This is a method for producing a heat-resistant and corrosion-resistant sintered body, which is characterized by firing a mixture whose weight percentage is essentially Cr and C at a temperature of 1600° C. or higher.
以下、さらに詳しく本発明について説明する。The present invention will be explained in more detail below.
複合材としてＺｒＢ、、ＴｉＢ、、ＴｉＣ，ＳｉＣ％
ＴｉＮを選んだ理由は、これらがＣｒ、Ｃ，の焼結性
を促進する効果を有するだけでなく、耐食性、耐熱衝撃
性、硬度、強度、破壊靭性を高める働きをするからであ
る。ZrB, , TiB, , TiC, SiC% as composite material
The reason for choosing TiN is that it not only has the effect of promoting the sinterability of Cr, C, but also works to improve corrosion resistance, thermal shock resistance, hardness, strength, and fracture toughness.
本発明に用いるＣｒａＣ２は純度９９％以上、平均粒径
５μｍ以下特に１μＩ以下が好ましく、同様に複合材の
ＺｒＢｚ、ＴｉＢｚ、ＴｉＣ，ＳｉＣ、ＴｉＮについて
も純度９９％以上、平均粒径１０μ糟以下特に５μｍ以
下が好ましい。CraC2 used in the present invention preferably has a purity of 99% or more and an average particle size of 5 μm or less, particularly 1 μI or less. Similarly, the composite materials ZrBz, TiBz, TiC, SiC, and TiN also have a purity of 99% or more and an average particle size of 10 μm or less, especially The thickness is preferably 5 μm or less.
通常、これらの微粉末の混合物はそれぞれの微粉末を均
一に混合する事により得られるが、同時に粉砕混合して
も良い。混合物の粒度としては平均粒径１０μｍ以下好
ましくは１μｍ以下である。Usually, a mixture of these fine powders is obtained by uniformly mixing the respective fine powders, but they may also be pulverized and mixed at the same time. The average particle size of the mixture is 10 μm or less, preferably 1 μm or less.
粉砕方法としては湿式、乾式が採用される。Wet and dry crushing methods are used.
本発明の焼結体は前記混合物を真空中、アルゴン、ヘリ
ウム、窒素などの中性あるいは還元性の雰囲気下でホッ
トプレス法かプレス成型後常圧焼結法によって得ること
ができる。炭化クロム系セラミックの焼成温度は、従来
１５００℃以下が良いとされていたが、本発明では１６
００℃以上の焼成温度が必要であることを見い出したも
のである。焼成時間については３０分〜ｌＯ時間程度で
あるが、原料組成、原料粒度により適宜選択される。ま
た焼結方法としては常圧焼結、ホップレス焼結さらにＨ
Ｉ Ｐ法も有効である。The sintered body of the present invention can be obtained by hot-pressing the above-mentioned mixture in vacuum or in a neutral or reducing atmosphere such as argon, helium, nitrogen, etc., or by press-molding and then pressureless sintering. Conventionally, the firing temperature of chromium carbide-based ceramics was considered to be 1500°C or lower, but in the present invention, the firing temperature is 1600°C or lower.
It has been discovered that a firing temperature of 00°C or higher is required. The firing time is approximately 30 minutes to 10 hours, and is appropriately selected depending on the raw material composition and raw material particle size. Sintering methods include normal pressure sintering, hopless sintering, and H
The IP method is also effective.
本発明のＺｒＢｚ 、ＴｉＢｚ、 ＴｉＣ、ＳｉＣ、Ｔ
ｉＮの少なくとも１種以上からなる複合材の添加量は０
．５〜５０重景％である。０．５重量％未満では焼結性
、強度、硬度などの面で充分でなく、一方、５０重量％
をこえてはＣｒ、Ｃ２本来の性質が損われる。ZrBz, TiBz, TiC, SiC, T of the present invention
The amount of the composite material containing at least one type of iN is 0.
．． The ratio is 5 to 50%. If it is less than 0.5% by weight, it is not sufficient in terms of sinterability, strength, hardness, etc.;
Exceeding this will damage the original properties of Cr and C2.
これら複合材の効果としては、焼結性の向上とＣｒ３Ｃ
，の微細な結晶を析出させることによって高強度、高靭
性化するだけでなく複合材固有の性質である高融点、高
硬度、高耐食性等の性能を付与できるものである。本発
明の複合材の組み合せにより特性の異った焼結体を製造
することも可能である。The effects of these composite materials include improved sinterability and Cr3C
By precipitating fine crystals of . It is also possible to produce sintered bodies with different characteristics by combining the composite materials of the present invention.
炭化クロムにはＣｒ５Ｃｔ以外にＣｒｔＣ＊、ＣｒａＣ
等が知られているが、これらを本発明に用いることもで
きる。In addition to Cr5Ct, chromium carbide also contains CrtC* and CraC.
etc. are known, but these can also be used in the present invention.
実施例１
純度９９％以上のＣｒ：＋Ｃｚ粉末（平均粒径４〜５μ
ｍ）とＺｒＢｚ、 ＴｉＢｚ、ＴＩＣ％ ＳｉＣ％ Ｔ
ｉＮの各粉末（平均粒径３〜４μｌ１１）の１種以上を
所定量計量後ボールミル混合した後ＣＩ Ｐ （２，７
ｔｏｎ ／ｃｄ、３分間）成型し、真空雰囲気下におい
て所定の温度、時間で常圧焼結した。得られた焼結体の
物性を表−１に示す。実験隘１〜８は比較例、実験阻９
〜２２は本発明例である。Example 1 Cr:+Cz powder with a purity of 99% or more (average particle size 4-5μ
m) and ZrBz, TiBz, TIC% SiC% T
After weighing a predetermined amount of one or more types of iN powders (average particle size 3 to 4 μl11) and mixing them in a ball mill, CI P (2,7
ton/cd for 3 minutes) and sintered under normal pressure at a predetermined temperature and time in a vacuum atmosphere. Table 1 shows the physical properties of the obtained sintered body. Experiments 1 to 8 are comparative examples, experiment number 9
-22 are examples of the present invention.
なお、表に示した物性は次のようにして測定した。The physical properties shown in the table were measured as follows.
（１１耐熱衝撃性は、急冷強度測定法で求めた。供試体
は３ Ｘ ４ Ｘ ４ Ｑ 龍の曲げ強度試験片を用い
、電気炉内で所定の温度で加熱し、一定時間（１時間）
保持後炉の下に設置しである０℃の水中へ降下させて試
験片を急冷した。その試験片の曲げ強度を測定し強度が
低下したときの加熱温度と水の温度（０℃）との差をΔ
Ｔとした。(11 Thermal shock resistance was determined by the quenching strength measurement method. The specimen was a 3 x 4 x 4 Q dragon bending strength test piece, heated at a predetermined temperature in an electric furnace, and then heated for a certain period of time (1 hour).
After holding, the test piece was placed under the furnace and lowered into water at 0°C to quench the test piece. Measure the bending strength of the test piece and calculate the difference between the heating temperature and the water temperature (0℃) when the strength decreases by Δ
It was set as T.
（２）耐食性は、３Ｘ４Ｘ４０ｍの試験片を４５０℃、
１時間Ａｒ雰囲気下で鉛の溶湯に浸漬しその侵食量から
判定した。侵食量は腐食部分、スケール等を削り落した
後の重量減少とした。(2) Corrosion resistance was determined by testing a 3x4x40m test piece at 450°C.
It was immersed in molten lead in an Ar atmosphere for 1 hour and judged from the amount of corrosion. The amount of erosion was defined as the weight loss after removing corroded parts, scale, etc.
〇−異状なし、△−やや侵食、×−かなり侵食（３）相
対密度はアルキメデス法で測定した。〇-No abnormality, △-Slight erosion, ×-Significant erosion (3) Relative density was measured by Archimedes method.
本発明例（実験隘９〜２２）は、比較例（実験隘１〜８
）に比べて耐熱衝撃性と耐食性が共に優れていることが
わかる。The inventive examples (experimental positions 9 to 22) are the comparative examples (experimental positions 1 to 8).
), it can be seen that both thermal shock resistance and corrosion resistance are superior.
実施例２
実施例１の実験ＮｃＬ１３について焼成温度を変えて相
対密度を求めた。その結果を表−２に示す。Example 2 Regarding experiment NcL13 of Example 1, the relative density was determined by changing the firing temperature. The results are shown in Table-2.
実験陽２３〜２５は比較例、実験ＮｔＸ２６〜２７は本
発明例である。これより焼成温度としては、１６００°
Ｃ以上が必要であることがわかる。Experiments Nos. 23 to 25 are comparative examples, and Experiments NtX 26 to 27 are examples of the present invention. From this, the firing temperature is 1600°
It can be seen that C or higher is required.
表−２
〔発明の効果〕
本発明によって得られた耐熱耐食性焼結体は、高強度、
高耐食、耐熱衝撃性、導電性等に優れているので、熱電
対の保護管、金属加工用ダイス、ヒーター、温度センサ
ー等の幅広い分野で使用することができる。また、金属
と同様に放電加工ができるので複雑形状品にも容易に対
応することができる。Table 2 [Effects of the invention] The heat-resistant and corrosion-resistant sintered body obtained by the present invention has high strength,
Because it has excellent corrosion resistance, thermal shock resistance, and electrical conductivity, it can be used in a wide range of fields such as thermocouple protection tubes, metal processing dies, heaters, and temperature sensors. Furthermore, since it can be subjected to electrical discharge machining in the same way as metal, it can be easily manufactured into products with complex shapes.
特許出願人 電気化学工業株式会社Patent applicant Denki Kagaku Kogyo Co., Ltd.
Claims (1)
Ｎから選ばれた１種以上が０．５〜５０重量％で残部が
実質的にＣｒ＿３Ｃ＿２である混合物を温度１６００℃
以上で焼成することを特徴とする耐熱耐食性焼結体の製
造方法。1. ZrB_2, TiB_2, TiC, SiC and Ti
A mixture containing 0.5 to 50% by weight of one or more selected from N and the remainder being substantially Cr_3C_2 was heated at a temperature of 1600°C.
A method for producing a heat-resistant and corrosion-resistant sintered body, which is characterized by firing in the above manner.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63249785A JPH0625035B2 (en) | 1987-10-06 | 1988-10-05 | Method for producing heat-resistant and corrosion-resistant sintered body |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62-250727 | 1987-10-06 | ||
| JP25072787 | 1987-10-06 | ||
| JP63249785A JPH0625035B2 (en) | 1987-10-06 | 1988-10-05 | Method for producing heat-resistant and corrosion-resistant sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01201076A true JPH01201076A (en) | 1989-08-14 |
| JPH0625035B2 JPH0625035B2 (en) | 1994-04-06 |
Family
ID=26539487
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63249785A Expired - Lifetime JPH0625035B2 (en) | 1987-10-06 | 1988-10-05 | Method for producing heat-resistant and corrosion-resistant sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0625035B2 (en) |
-
1988
- 1988-10-05 JP JP63249785A patent/JPH0625035B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0625035B2 (en) | 1994-04-06 |
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