JP2570404B2 - Method for producing chromium silicide powder with low content of Na and K - Google Patents
Method for producing chromium silicide powder with low content of Na and KInfo
- Publication number
- JP2570404B2 JP2570404B2 JP63265817A JP26581788A JP2570404B2 JP 2570404 B2 JP2570404 B2 JP 2570404B2 JP 63265817 A JP63265817 A JP 63265817A JP 26581788 A JP26581788 A JP 26581788A JP 2570404 B2 JP2570404 B2 JP 2570404B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- sio
- chromium silicide
- low content
- silicide powder
- 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.)
- Expired - Lifetime
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- Silicon Compounds (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 この発明は、NaおよびＫ含有量のきわめて少ないクロ
ムシリサイド粉末の製造法に関するものであり、上記ク
ロムシリサイド粉末は、Siウエハー上にメモリーおよび
抵抗薄膜などを同時に形成してモノリシツクICなどを製
造するスパツタリング用ターゲツトを製造するための原
料粉末となるものである。Description: TECHNICAL FIELD The present invention relates to a method for producing a chromium silicide powder having a very low Na and K content. It is a raw material powder for producing a sputtering target for producing a monolithic IC or the like by simultaneously forming a thin film or the like.
通常、クロムシリサイド粉末は、Cr粉末とSi粉末とを
Si/Cr（モル比）＝2.0となるように配合し、混合したの
ち、温度:900〜1100℃のH2雰囲気中で焼成してCrSi
2（クロムジシリサイド）を得、これを粉砕してクロム
シリサイド粉末を製造していた。このようにして得られ
たクロムシリサイド粉末は、ホツトプレスすることによ
りターゲツトを作製し、上記ターゲツトを用いてスパツ
タリング法により、例えばモノリシツクICの抵抗薄膜を
製造していた。Usually, chromium silicide powder is composed of Cr powder and Si powder.
Si / Cr were blended so that (molar ratio) = 2.0, were mixed, temperature: 900 to 1100 and fired in an H 2 atmosphere in ° C. CrSi
2 (chromium disilicide) was obtained and pulverized to produce chromium silicide powder. The chromium silicide powder thus obtained was hot-pressed to form a target, and the target was used to produce a resistive thin film of, for example, a monolithic IC by a sputtering method.
ところが、上記従来の技術で述べた方法により製造さ
れたクロムシリサイド粉末には、通常NaおよびＫが含有
されており、このNaおよびＫ含有のクロムシリサイド粉
末を用いて作製したスパツタリング用ターゲツトを使用
して抵抗薄膜を製造すると、その抵抗薄膜にもNaおよび
Ｋイオンが含まれてくる。上記抵抗薄膜にNaおよびＫイ
オンが含まれるとNaおよびＫイオンは抵抗薄膜中を容易
に移動し、抵抗薄膜の絶縁抵抗性を劣化せしめるので好
ましくない。However, the chromium silicide powder produced by the method described in the above-mentioned conventional technology usually contains Na and K, and a sputtering target prepared using the chromium silicide powder containing Na and K is used. When a resistance thin film is manufactured by the above method, the resistance thin film also contains Na and K ions. If Na and K ions are contained in the resistance thin film, the Na and K ions easily move in the resistance thin film and deteriorate the insulation resistance of the resistance thin film, which is not preferable.
したがつて、上記スパツタリング用ターゲツト製造の
ためのクロムシリサイド粉末には、NaおよびＫを含まな
いことが好ましいが、上記クロムシリサイド粉末を製造
するための市販のCr粉末には、通常、NaおよびＫがそれ
ぞれ10〜20ppm程度含まれており、NaおよびＫの少ないC
r粉末を入手することは困難であつた。Therefore, it is preferable that the chromium silicide powder for producing the sputtering target does not contain Na and K. However, the commercially available Cr powder for producing the chromium silicide powder usually contains Na and K. , Each containing about 10 to 20 ppm, and low in Na and K
r It was difficult to obtain powder.
したがつて、通常の製造法により得られたクロムシリ
サイド粉末には、NaおよびＫが含まれることは避けられ
ず、したがつて上記クロムシリサイド粉末を原料粉末と
して得られたスパツタリング用ターゲツトおよびそのタ
ーゲツトを用いて得られた抵抗薄膜にNaおよびＫが含ま
れることは避けられず、絶縁抵抗性の劣化は避けられな
いという問題点があつた。Therefore, it is inevitable that Na and K are contained in the chromium silicide powder obtained by a normal production method, and therefore, the sputtering target obtained by using the chromium silicide powder as a raw material powder and the target thereof However, it is inevitable that Na and K are contained in the resistance thin film obtained by using the method described above, and there is a problem that deterioration of insulation resistance is inevitable.
そこで、本発明者等は、NaおよびＫ含有量の少ないク
ロムシリサイド粉末を得べく研究を行つた結果、 Cr粉末とSi粉末をSi/Cr＝２（モル比）となるように
配合し混合して得られた混合粉末に、さらにSiO2粉末と
Si粉末の混合粉末を添加し焼成すると、NaおよびＫ含有
量の少ないクロムシリサイド粉末を得ることができると
いう知見を得たのである。Therefore, the present inventors conducted research to obtain a chromium silicide powder having a low content of Na and K, and as a result, blended and mixed Cr powder and Si powder so that Si / Cr = 2 (molar ratio). the mixed powder was collected using a further SiO 2 powder
It has been found that when a mixed powder of Si powder is added and fired, a chromium silicide powder having a low Na and K content can be obtained.
この発明は、かかる知見にもとづいてなされたもので
あつて、 Cr粉末とSi粉末をSi/Cr＝２（モル比）となるように
配合し、混合して得られた混合粉末に、外量で、SiO2粉
末:0.5〜５重量％添加し、さらに上記SiO2粉末と同モル
のSi粉末を添加し混合して得られた混合粉末を、焼成し
たのち粉砕してNaおよびＫ含有量の少ないクロムシリサ
イド粉末を製造する方法に特徴を有するものである。The present invention has been made on the basis of this finding, and a mixture of a Cr powder and a Si powder so that Si / Cr = 2 (molar ratio) is obtained. Then, SiO 2 powder: 0.5 to 5% by weight is added, and a mixed powder obtained by further adding and mixing the same mole of Si powder as the above SiO 2 powder is calcined and then pulverized to reduce the Na and K content. It is characterized by a method for producing a small amount of chromium silicide powder.
NaおよびＫ不純物が焼成中に除去される機構として
は、一般に、SiO2はNaおよびＫを吸収し反応し易い性質
を有するため、焼成中の高温時にCr粉末表面に吸着され
ているNaおよびＫイオンがSiO2中に移動し、さらに高温
になるとNaおよびＫを含むSiO2がSiと反応して昇華性の
SiOになつて飛び出し、その時NaおよびＫもSiOと同時に
系外に除去されるものと推定される。The mechanism by which Na and K impurities are removed during firing is that SiO 2 generally has the property of easily absorbing and reacting with Na and K, and therefore Na and K adsorbed on the surface of the Cr powder at high temperatures during firing. The ions move into the SiO 2 , and at higher temperatures, the SiO 2 containing Na and K reacts with the Si to sublimate
It is presumed that Na and K fly out of the system at the same time as SiO and are removed out of the system.
SiO2とSiとの反応は、 SiO2＋Si→2SiO となるから、SiO2粉末と共に添加されるSi粉末の量は、
SiO2粉末と同モルでなければならない。Since the reaction between SiO 2 and Si is SiO 2 + Si → 2SiO, the amount of Si powder added together with the SiO 2 powder is
Must be the same mole as SiO 2 powder.
外量で添加するSiO2粉末の添加量は、0.5〜５重量％
であり、0.5重量％未満ではNaおよびＫ除去に十分な効
果が得られず、５重量％を越えると焼結体中に残留する
SiO2成分がスパツタリング時に異常放電をおこすので好
ましくない。したがつてSiO2粉末の添加量は0.5〜５重
量％に限定されるが、Si粉末の添加量は、SiO2粉末と同
モルである必要からSi粉末:1.0〜10重量％と定めた。The amount of SiO 2 powder added in an external amount is 0.5 to 5% by weight
If it is less than 0.5% by weight, a sufficient effect for removing Na and K cannot be obtained, and if it exceeds 5% by weight, it remains in the sintered body.
This is not preferable because the SiO 2 component causes abnormal discharge during sputtering. Although the Addition Amount of connexion SiO 2 powder is limited to 0.5 to 5 wt%, the amount of Si powder, Si powder from necessarily SiO 2 powder and the mole: 1.0 to 10 was defined as wt%.
つぎに、この発明を実施例にもとづいて具体的に説明
する。Next, the present invention will be specifically described based on embodiments.
市販の平均粒径:100μｍのCr粉末、平均粒径:50μｍ
のSi粉末および平均粒径:10μｍのSiO2粉末を用意し
た。Commercial average particle size: Cr powder of 100 μm, average particle size: 50 μm
And an average particle size of 10 μm SiO 2 powder were prepared.
上記Cr粉末にはNaおよびＫがそれぞれ20ppm含まれて
おり、Si粉末にはNaおよびＫの含有量は1ppm以下であつ
た。The Cr powder contained 20 ppm each of Na and K, and the Si powder contained 1 ppm or less of Na and K.
上記Cr粉末とSi粉末とを、それぞれ、 Cr粉末:48.1重量％、 Si粉末:51.9重量％、 となるように配合し、さらに外量で SiO2粉末:3重量％、 Si粉末:1.5重量％、 を加えてＶコンで混合し、温度:1100℃、H2気流中、１
時間保持の条件で焼成したのち、温度:1430℃、10分間
保持し、ついで冷した。上記温度:1430℃で10分間保
持したのは、SiO2＋Si→2SiOの反応を促進させるためで
ある。The above-mentioned Cr powder and Si powder were blended so that Cr powder: 48.1% by weight and Si powder: 51.9% by weight, respectively, and further, SiO 2 powder: 3% by weight, Si powder: 1.5% by weight , And mixed with a V-con, at a temperature of 1100 ° C. in a stream of H 2 ,
After calcination under the condition of holding for a time, the temperature was kept at 1430 ° C. for 10 minutes, and then cooled. The temperature was kept at 1430 ° C. for 10 minutes in order to promote the reaction of SiO 2 + Si → 2SiO.
このようにして得られたCrSi2焼成体を解砕および粉
砕してCrSi2粉末を製造し、この粉末のNaおよびＫ含有
量を測定したところ、Na:0.5ppm、K:0.1ppmであつた。The thus obtained CrSi 2 fired body was crushed and pulverized to produce a CrSi 2 powder, and the Na and K contents of the powder were measured. As a result, Na: 0.5 ppm and K: 0.1 ppm were obtained. .
このCrSi2粉末に、さらに半導体Siチツプを加え、CrS
i2.7組成に調整した後、ボールミルにより混合、粉砕を
行い、得られた粉末を温度:1300℃、150kg/cm2で真空ホ
ツトプレスすることにより相対密度:99.3％のターゲツ
ト素材を得ることができた。A semiconductor Si chip is further added to this CrSi 2 powder,
After adjusting the composition to 2.7 , the mixture was mixed and pulverized by a ball mill, and the obtained powder was subjected to vacuum hot pressing at a temperature of 1300 ° C. and 150 kg / cm 2 to obtain a target material having a relative density of 99.3%. .
市販のNaおよびＫ含有Cr粉末を用いて、NaおよびＫ含
有量の極めて少ないクロムシリサイド粉末を製造するこ
とができるので安価なNaおよびＫ含有量の極めて少ない
クロムシリサイドターゲツトを得ることができ、このタ
ーゲツトを用いて製造するモノリシツクIC等に形成され
る抵抗薄膜もNaおよびＫ含有量が極めて少なく、絶縁抵
抗性のすぐれたものが得られるという効果がある。Using a commercially available Cr powder containing Na and K, a chromium silicide powder having an extremely low Na and K content can be produced, so that an inexpensive chromium silicide target having an extremely low Na and K content can be obtained. A resistive thin film formed on a monolithic IC or the like manufactured using a target also has an effect that the content of Na and K is extremely small and a film having excellent insulation resistance can be obtained.
Claims (2)
るように配合し混合して得られた混合粉末を焼成してク
ロムシリサイド粉末を製造する方法において、 上記混合粉末に、さらにSiO2粉末と上記SiO2粉末と同モ
ルのSi粉末からなる混合粉末を添加混合したのち焼成す
ることを特徴とするNaおよびＫ含有量の少ないクロムシ
リサイド粉末の製造法。1. A method for producing a chromium silicide powder by firing a mixed powder obtained by blending and mixing Si powder and Cr powder in a molar ratio of Si / Cr = 2; further preparation of small chromium silicide powder having Na and K content and firing After adding and mixing mixed powder of SiO 2 powder and the SiO 2 powder with the same moles of Si powder.
粉末とCr粉末の混合粉末に対して、外量で SiO2粉末:0.5〜５重量％、 Si粉末:1.0〜10重量％、 添加することを特徴とする請求項１記載のNaおよびＫ含
有量の少ないクロムシリサイド粉末の製造法。2. The amount of the SiO 2 powder and the Si powder to be added is as follows:
2. The Na and K contents according to claim 1, wherein SiO 2 powder: 0.5 to 5% by weight and Si powder: 1.0 to 10% by weight are added to the mixed powder of the powder and the Cr powder. Of chromium silicide powder with low content.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63265817A JP2570404B2 (en) | 1988-10-21 | 1988-10-21 | Method for producing chromium silicide powder with low content of Na and K |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63265817A JP2570404B2 (en) | 1988-10-21 | 1988-10-21 | Method for producing chromium silicide powder with low content of Na and K |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02111614A JPH02111614A (en) | 1990-04-24 |
| JP2570404B2 true JP2570404B2 (en) | 1997-01-08 |
Family
ID=17422469
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63265817A Expired - Lifetime JP2570404B2 (en) | 1988-10-21 | 1988-10-21 | Method for producing chromium silicide powder with low content of Na and K |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2570404B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020099644A1 (en) * | 2018-11-16 | 2020-05-22 | Kanthal Ab | New process for manufacturing a chromium alloyed molybdenum silicide portion of a heating element |
| JP2020203821A (en) * | 2018-11-22 | 2020-12-24 | 東ソー株式会社 | Cr-Si SINTERED BODY |
| CN112144024B (en) * | 2020-09-14 | 2022-12-02 | 浙江最成半导体科技有限公司 | Chromium silicide target material and preparation method thereof |
-
1988
- 1988-10-21 JP JP63265817A patent/JP2570404B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02111614A (en) | 1990-04-24 |
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