JPS5845161B2 - resistance composition - Google Patents
resistance compositionInfo
- Publication number
- JPS5845161B2 JPS5845161B2 JP51030103A JP3010376A JPS5845161B2 JP S5845161 B2 JPS5845161 B2 JP S5845161B2 JP 51030103 A JP51030103 A JP 51030103A JP 3010376 A JP3010376 A JP 3010376A JP S5845161 B2 JPS5845161 B2 JP S5845161B2
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- composition
- conductive fine
- resistance
- resistor
- 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
Links
- 239000000203 mixture Substances 0.000 title claims description 49
- 239000000843 powder Substances 0.000 claims description 49
- 239000011521 glass Substances 0.000 claims description 25
- 229910021334 nickel silicide Inorganic materials 0.000 claims description 12
- RUFLMLWJRZAWLJ-UHFFFAOYSA-N nickel silicide Chemical compound [Ni]=[Si]=[Ni] RUFLMLWJRZAWLJ-UHFFFAOYSA-N 0.000 claims description 12
- 229910005883 NiSi Inorganic materials 0.000 claims description 6
- 229910005487 Ni2Si Inorganic materials 0.000 claims description 4
- 229910003217 Ni3Si Inorganic materials 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 18
- 239000004020 conductor Substances 0.000 description 16
- 238000000498 ball milling Methods 0.000 description 12
- 239000011230 binding agent Substances 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 229910021332 silicide Inorganic materials 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910005108 Ni3Si2 Inorganic materials 0.000 description 2
- 229910012990 NiSi2 Inorganic materials 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000001293 FEMA 3089 Substances 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000037237 body shape Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Resistance Heating (AREA)
- Adjustable Resistors (AREA)
- Non-Adjustable Resistors (AREA)
Description
【発明の詳細な説明】
本発明は、抵抗組成物、とくに固定抵抗器、可変抵抗器
、混成集積回路用抵抗体あるいは電熱器用発熱体などに
用いられる抵抗組成物に関するもので、詳細（こは、け
い化ニッケルよりなる導電性微粉末とガラスフリットと
を含有することを特徴とするものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a resistance composition, particularly to a resistance composition used for a fixed resistor, a variable resistor, a resistor for a hybrid integrated circuit, a heating element for an electric heater, etc. , which is characterized by containing conductive fine powder made of nickel silicide and glass frit.
従来、精密用固定抵抗器や混成集積回路用抵抗体などに
は、一般にＪＪｕ（Ａｇ）とパラジウム（Ｐｄ）あるい
は酸化ルテニウム（ＲｕＯ□）などの貴金属系の導電性
微粉末とガラスフリットなどからなる抵抗組成物が用い
られている。Conventionally, precision fixed resistors and resistors for hybrid integrated circuits are generally made of JJu (Ag), conductive fine powder of noble metals such as palladium (Pd) or ruthenium oxide (RuO□), and glass frit. A resistive composition is used.
この組成物を用いた抵抗器は、貴金属またはその酸化物
と、ガラスフリットとからなるため、耐熱性、耐電力に
すぐれ、かつ信頼性の高い抵抗器として、一般に知られ
ている。A resistor using this composition is generally known as a resistor that has excellent heat resistance, high power resistance, and high reliability because it is made of a noble metal or its oxide and glass frit.
しかしながら、この抵抗組成物はＡｇ。Ｐｄあるいはル
テニウム（Ｒｕ）などの貴金属、またはその酸化物を用
いているため、価格が非常に高くなり、とくに低い抵抗
値の抵抗組成物は、導電性微粉末を多く必要とするため
、高価となり、民生用などの安価な抵抗器に使用しがた
いのが、大きな欠点である。However, this resistance composition is made of Ag. Because they use noble metals such as Pd or ruthenium (Ru), or their oxides, they are very expensive, and resistor compositions with low resistance values are especially expensive because they require a large amount of conductive fine powder. A major drawback is that it is difficult to use in inexpensive resistors for consumer use.
−・方、貴金属を用いない抵抗組成物には、酸化インジ
ウムや炭化タングステンなどの導電性微粉末とガラスフ
リットとを用いたものが知られている。On the other hand, as resistance compositions that do not use noble metals, there are known resistance compositions that use conductive fine powder such as indium oxide or tungsten carbide and glass frit.
しか°しながら、これらは、いずれも抵抗組成物を焼成
するとき、窒素などの不活性気圏中で焼成することが必
要で、空気中焼成番こくらべ、焼成がめんどうであり、
かつ焼成コストが大巾に高くなり、また抵抗緒特性も必
ずしも満足できるものではなかった。However, in both of these methods, when firing the resistance composition, it is necessary to fire it in an inert atmosphere such as nitrogen, and firing it in air is cumbersome.
Moreover, the firing cost was significantly increased, and the resistance properties were not necessarily satisfactory.
本発明は、この点の改良に関するものであって、ニッケ
ル（Ｎｉ）とけい素（Ｓｉ）の化合物であるけい化ニッ
ケルよりなる導電性微粉末とガラスフリットとを用いる
ことによって、高性能でかつ安価なグレーズ抵抗体を構
成することのできる抵抗組成物を提供するものである。The present invention relates to an improvement in this point, and uses conductive fine powder made of nickel silicide, which is a compound of nickel (Ni) and silicon (Si), and glass frit to achieve high performance and low cost. The object of the present invention is to provide a resistance composition that can constitute a glazed resistor.
以下、本発明の抵抗組成物について詳細に説明する。Hereinafter, the resistance composition of the present invention will be explained in detail.
導電性微粉末は、Ｎｉと８１の化合物であるけい化ニッ
ケルからなる。The conductive fine powder consists of nickel silicide, which is a compound of Ni and 81.
けい化ニッケルは、Ｎｉ３Ｓｉ ＋ Ｎｉ５Ｓｉ２ 、
Ｎｉ２Ｓｉ ＋ Ｎｉ３Ｓｉ２またはＮｉＳｉの組成
からなる化合物が有用で、これらが混合されていても、
また学独でも有用である。Nickel silicide is Ni3Si + Ni5Si2,
Compounds consisting of the composition Ni2Si + Ni3Si2 or NiSi are useful, even if they are mixed.
It is also useful for independent study.
さらにＮｉＳｉ□の組成からなる化合物が上記組成の化
合物と混合されていても問題はない。Further, there is no problem even if a compound having the composition of NiSi□ is mixed with a compound having the above composition.
導電性微粉末は、ＮｉとＳｉの各微粉末を適当な比率で
混合し、粉末のままか、または円板状に成形した後、真
空中または不活性気圏中において、８００〜１６００℃
の範囲内の温度で熱処理して反応させた後、微粉砕して
つくる。The conductive fine powder is prepared by mixing Ni and Si fine powders in an appropriate ratio, either as a powder or after forming it into a disk shape, and heating it at 800 to 1600°C in a vacuum or in an inert atmosphere.
It is made by heat-treating and reacting at a temperature within the range of , and then pulverizing it.
ＮｉとＳｉの混合比率は、必要なけい化ニッケルの組成
に応じて決定すればよいが、必ずしも化学量論的組成比
に限定するものではない。The mixing ratio of Ni and Si may be determined depending on the required composition of nickel silicide, but is not necessarily limited to a stoichiometric composition ratio.
また熱処理温度は生成するけい化ニッケルの組成、生成
比率ならひに結晶性などに関係する。Furthermore, the heat treatment temperature is related to the composition of the produced nickel silicide, the production ratio, and the crystallinity of the produced nickel silicide.
たとえば、１４００°Ｃ熱処理のものは、１３００’Ｃ
熱処理にくらべ結晶性が高い。For example, those heat treated at 1400°C are heated to 1300'C.
Higher crystallinity than heat treatment.
つぎに、導電材料の製法の一例を詳細に説明する。Next, an example of a method for manufacturing a conductive material will be described in detail.
ＮｉとＳｉの各微粉末を、３：２（原子比）に混合し、
円板状またはブロック状に成形した後、真空中において
１４００℃の温度で熱処理すると、Ｎ １３８１２を主
成分とするけい化ニッケルからなる導電材料が生成する
。Mix fine powders of Ni and Si at a ratio of 3:2 (atomic ratio),
After forming into a disk or block shape, heat treatment is performed at a temperature of 1400° C. in a vacuum to produce a conductive material made of nickel silicide containing N13812 as a main component.
導電材料の粉砕は、ステンレススチール棒であら粉砕し
、つぎｌこ、らいかい機で粉砕し、さらにポットにメタ
ノールとともにいれ、ボールミル粉砕をする。The conductive material is crushed using a stainless steel rod, then crushed using a sieve machine, and then placed in a pot with methanol and crushed using a ball mill.
粉砕時間は２４〜２４０時間程度であればよく、必要に
応じてより長時間粉砕してもよい。The pulverization time may be about 24 to 240 hours, and it may be pulverized for a longer time if necessary.
ガラスフリットは、たとえば硼酸（Ｈ３ＢＯ３） ；５
１３重量％、炭酸バノウム（ＢａＣ０３）： ３４．２
重量％、酸化けい素（Ｓ ＋ ０２ ） ； ３．４重
量％、酸化アルミニウム（Ａ１２０３）；６重量％、炭
酸カルシウム（ＣａＣ０３） ：２５５重量％および酸
化マグネシウム（ＭｇＯ）：２．５５重量％を混合し、
アルミするつぼに入れ、１２００℃の温度に加熱して溶
融させ、つぎに、ポットにメタノールとともにいれ、１
０〜２４０時間ボールミル粉砕をして作製する。Glass frit, for example, boric acid (H3BO3);5
13% by weight, banium carbonate (BaC03): 34.2
% by weight, silicon oxide (S+02); 3.4% by weight, aluminum oxide (A1203); 6% by weight, calcium carbonate (CaC03): 255% by weight, and magnesium oxide (MgO): 2.55% by weight. mix,
Put it in an aluminum crucible, heat it to 1200℃ to melt it, then put it in a pot with methanol,
It is produced by ball milling for 0 to 240 hours.
導電性微粉末ならひにガラスフリットの粒径は０．１〜
数μのオーダが良好である。If it is a conductive fine powder, the particle size of Hini glass frit is 0.1~
A value on the order of several microns is good.
なお、ガラスフリットは必ずしも上記組成に限定するも
のではない。Note that the glass frit is not necessarily limited to the above composition.
つぎに、導電性微粉末とガラスフリットを適当な比率で
混合し、印刷適性をす、えるため、たとえばテレピン油
とエチルセルローズとを９：１（重量比）の比率に混合
した有機質粘結剤を添加して、ペースト状の抵抗組成物
を作成する。Next, conductive fine powder and glass frit are mixed in an appropriate ratio, and in order to improve printability, an organic binder containing, for example, turpentine oil and ethyl cellulose is mixed in a ratio of 9:1 (weight ratio). is added to create a paste-like resistance composition.
有機質粘結剤の添力０量は、導電性微粉末とガラスフリ
ットの量１０ｇＧこ対して５ｇが適当であるが、ガラス
フリットの量が多くなるにともない、有機質粘結剤の量
を、やや多くした方が良好である。The appropriate zero additive amount of organic binder is 5 g compared to the 10 g of conductive fine powder and glass frit. However, as the amount of glass frit increases, the amount of organic binder may be slightly increased. The more it is, the better.
このペースト状の抵抗組成物を、２００メツシユのスク
リーンメツシュを用いて、アルミナ磁器基板上にスクリ
ーン印刷し、１２０℃の温度で乾燥させてから、最高温
度７００〜９００℃の範囲内の温度に加熱したトンネル
炉を通して焼成して、グレーズ抵抗体をつくる。This pasty resistive composition was screen printed onto an alumina porcelain substrate using a 200 mesh screen mesh, dried at a temperature of 120°C, and then heated to a maximum temperature within the range of 700-900°C. A glazed resistor is produced by firing through a heated tunnel furnace.
電極としては、抵抗体を印刷し焼成する前に、ＡｇとＰ
ｄとガラスフリットを含むペース１へをスクリーン印刷
し、乾燥後、焼成したＡｇＰｄ電極を用いた。As electrodes, Ag and P are used before printing and firing the resistor.
d and glass frit were screen printed on paste 1, dried and fired, and an AgPd electrode was used.
しかし、ＡｇＰｄ電極のかわりに金電極や釦電極を用い
ても、とくに大きな問題はない。However, there is no particular problem even if a gold electrode or a button electrode is used instead of the AgPd electrode.
なお、抵抗組成物を磁器基板上に印刷する必要のない場
合、たとえば、体形の場合では、有機質粘結剤はとくに
必要ではない。Note that when there is no need to print the resistive composition on the ceramic substrate, for example, in the case of a body shape, the organic binder is not particularly necessary.
このときは、導電性微粉末とガラスフリットの混合物の
みで、この混合物に少量の水を添加して成形し、高温に
加熱することによって抵抗体を作製することができる。At this time, a resistor can be produced using only a mixture of conductive fine powder and glass frit by adding a small amount of water to the mixture, molding it, and heating it to a high temperature.
以下、実施例について説明する。Examples will be described below.
実施例 Ｉ
ＮｉとＳｉの各微粉末を５：２（原子比）に混合し、円
板状に成形した後、真空中において１４００’Ｃの温度
で２時間、熱処理してＮ ｉ５ Ｓ ｉ２を主成分とす
るけい化ニッケルからなる導電材料を作製した。Example I Ni and Si fine powders were mixed at a ratio of 5:2 (atomic ratio), formed into a disk shape, and then heat treated in vacuum at a temperature of 1400'C for 2 hours to form N i5 S i2. We created a conductive material consisting of nickel silicide as the main component.
この導電材料を微粉砕して導電性微粉末を作製した。This conductive material was pulverized to produce conductive fine powder.
つきに、導電性微粉末とガラスフリットとを第１表に示
す割合で配合し、有機質粘結剤を添加して、抵抗組成物
を作製した。At the same time, conductive fine powder and glass frit were blended in the proportions shown in Table 1, and an organic binder was added to prepare a resistance composition.
この抵抗組成物を、アルミナ磁器基板上に、２００メツ
シユのスクリーンメツシュを用いて、スクリーン印刷し
、１２０℃で乾燥させてから、最高温度８５０°Ｃに加
熱したトンネル炉を通して焼成し、抵抗体を作製した。This resistor composition was screen printed on an alumina porcelain substrate using a 200-mesh screen mesh, dried at 120°C, and fired through a tunnel furnace heated to a maximum temperature of 850°C. was created.
焼成後の膜厚は約１５μであった。The film thickness after firing was about 15μ.
２５°Ｃ（こおける面積抵抗値、２５°Ｃと１２５℃の
温度間で測定した抵抗温度係数を第１−表に示す。Table 1 shows the sheet resistance value at 25°C (temperature coefficient of resistance measured between 25°C and 125°C).
負荷寿命特性は、１２を、周囲温度７０°Ｃで、■ 除去をくりかえし、１００ ５ ｍ Ｗ／ ｍｔ７ｔの負荷電力 ５時間印加、０．５時間 ０時間経過したときの＊ 本抵抗値変化で評価した結果、 て、±１％以内であった。The load life characteristics are 12 at an ambient temperature of 70°C, ■ Repeat removal, 100 Load power of 5 mW/mt7t Applied for 5 hours, 0.5 hours *When 0 hours have passed* As a result of evaluating this resistance value change, It was within ±1%.
ずべての試料に゛つい
なお、試料１〜４は、４８時間ボールミル粉砕をして得
た導電性微粉末を使用したものであり、試料５は、２５
時間ボールミル粉砕をして得た導電性微粉末を使用した
ものである。Regarding all the samples, samples 1 to 4 used conductive fine powder obtained by ball milling for 48 hours, and sample 5 used conductive fine powder obtained by ball milling for 48 hours.
It uses conductive fine powder obtained by time ball mill grinding.
実施例 ２
ＮｉとＳｉの各微粉末を３：２（原子比）に混合し、円
板状に成形した後、真空中において１４００℃の温度で
熱処理して、Ｎｉ３Ｓｉ２を主成分とするけい化ニッケ
ルからなる導電材料を作製した。Example 2 Fine powders of Ni and Si were mixed at a ratio of 3:2 (atomic ratio), formed into a disk shape, and then heat treated in a vacuum at a temperature of 1400°C to form a silicide containing Ni3Si2 as the main component. A conductive material made of nickel was fabricated.
この導電材料を微粉砕して導電性微粉末を作製した。This conductive material was pulverized to produce conductive fine powder.
つぎｌこ、導電性微粉末とガラスフリツ＊トとを第２表
に示す割合で配合し、有機質粘結剤を添加して、抵抗組
成物を作製した。Next, conductive fine powder and glass frit were blended in the proportions shown in Table 2, and an organic binder was added to prepare a resistance composition.
この抵抗組成物を、実施例１と同様にして、アルミナ磁
器基板上に印刷し、乾燥後焼成して、抵抗体を作製した
。This resistor composition was printed on an alumina ceramic substrate in the same manner as in Example 1, dried and fired to produce a resistor.
２５℃における面積抵抗値、２５℃と１２５℃の温度間
で測定した抵抗温度係数を第２表に示す。Table 2 shows the sheet resistance value at 25°C and the temperature coefficient of resistance measured between 25°C and 125°C.
負荷寿命特性は、１２５ ｍＷ／ｍｌｔの負荷電力を周
囲温度７０℃で１．５時間印加、０．５時間除去をくり
かえし、１．０００時間経過したときの抵抗値変化で評
価した結果、すべての試料について、±１％以内であっ
た。The load life characteristics were evaluated by applying a load power of 125 mW/mlt at an ambient temperature of 70°C for 1.5 hours and removing it for 0.5 hours, and evaluating the resistance value change after 1,000 hours. For the samples, it was within ±1%.
なお、試料６〜８は、２４時間ボールミル粉砕して得た
導電性微粉末を使用したものであり、試料９〜１１は、
１２０時間ボールミル粉砕をして、また試料１２は、２
４０時間ボールミル粉砕をおして得た導電性微粉末を使
用したものである。In addition, samples 6 to 8 used conductive fine powder obtained by ball milling for 24 hours, and samples 9 to 11 used
After ball milling for 120 hours, sample 12
A conductive fine powder obtained by ball milling for 40 hours was used.
実施例 ３
ＮｉとＳｉの各微粉末を３：２（原子比）に混合し、ブ
ロック状０こ成形した後、真空中において、８００℃の
温度で熱処理して、Ｎｉ３ｓｔ２を主成分とするけい化
ニッケルからなる導電材料を作製した。Example 3 Ni and Si fine powders were mixed at a ratio of 3:2 (atomic ratio), formed into a block shape, and then heat-treated at a temperature of 800°C in a vacuum to form a silicone material containing Ni3st2 as the main component. A conductive material made of nickel oxide was fabricated.
この導電材料を微粉砕して、導電性微粉末を作製した。This conductive material was finely pulverized to produce conductive fine powder.
つぎに、導電性微粉末とガラスフリットを第３表に示す
割合で配合し、有機質粘結剤を添加して、抵抗組成物を
作成した。Next, conductive fine powder and glass frit were blended in the proportions shown in Table 3, and an organic binder was added to prepare a resistance composition.
この抵抗組成物を、実施例１と同様にして、アルミナ磁
器基本板上に印刷し、乾燥後、焼威し、抵抗体を作製し
た。This resistor composition was printed on an alumina porcelain basic board in the same manner as in Example 1, dried, and burned to produce a resistor.
２５°Ｃにおける面積抵抗値、２５℃と１２５℃の温度
間で測定した抵抗温度係数を第３表に示す。Table 3 shows the sheet resistance value at 25°C and the temperature coefficient of resistance measured between 25°C and 125°C.
負荷寿命特性は、実施例１と同様Ｏこして測定した結果
、すべての試料について、抵抗値変化率は、±１％以内
であった。The load life characteristics were measured using O strain as in Example 1, and the resistance change rate was within ±1% for all samples.
なお、試料１３〜１５は、１２０時間ボールミル粉砕し
て得た導電性微粉末を用いた。For samples 13 to 15, conductive fine powder obtained by ball milling for 120 hours was used.
実施例 ４
ＮｉとＳｉの各微粉末を２：１（原子比）に混合し、フ
ロック状に成形した後、真空中において、１４００℃の
温度で熱処理して、Ｎｉ２Ｓｉを主成分とするけい化ニ
ッケルからなる導電材料を作製した。Example 4 Fine powders of Ni and Si were mixed at a ratio of 2:1 (atomic ratio), formed into a floc, and then heat treated in a vacuum at a temperature of 1400°C to form a silicide containing Ni2Si as the main component. A conductive material made of nickel was fabricated.
この導電材料を微粉砕して、導電性微粉末を作製した。This conductive material was finely pulverized to produce conductive fine powder.
つぎに、導電性微粉末とガラスフリ木ットを第４表に示
す割合で配合し、有機質粘結剤を添加して抵抗組成物を
作製した。Next, conductive fine powder and glass fried wood were blended in the proportions shown in Table 4, and an organic binder was added to prepare a resistance composition.
この抵抗組成物を、実施例１と同様にして、アルミナ磁
器基板上に印刷し、乾燥後、焼成し、抵抗体を作製した
。This resistor composition was printed on an alumina ceramic substrate in the same manner as in Example 1, dried, and fired to produce a resistor.
２５°Ｃにおける面積抵抗値、２５°Ｃと１２５℃の温
度間で測定した抵抗温度係数を第４表に示す。Table 4 shows the sheet resistance value at 25°C and the temperature coefficient of resistance measured between 25°C and 125°C.
負荷寿命特性は、実施例１と同様にして測定した結果、
すべての試料について、抵抗値変化率は、±１％以内で
あった。The load life characteristics were measured in the same manner as in Example 1, and the results were as follows:
For all samples, the resistance value change rate was within ±1%.
なお、試料１６〜１８は、２４時間ボールミル粉砕し、
試料１９〜２１は、１６８時間ボールミル粉砕し、試ｔ
」２２〜２４は、２１６時間ボールミル粉砕し、試料２
５は、２４０時間ボールミル粉砕をおこなって得た導電
性微粉末を用いた。In addition, samples 16 to 18 were ball milled for 24 hours,
Samples 19 to 21 were ball milled for 168 hours and tested
”22 to 24 were ball milled for 216 hours and sample 2
In No. 5, conductive fine powder obtained by ball milling for 240 hours was used.
実施例 ５
ＮｉとＳｉの各微粉末を１：１（原子比）に混合し、ブ
ロック状に成形した後、真空中において、１４００℃の
温度で熱処理して、ＮｉＳｉを主成分とするけい化ニッ
ケルからなる導電材料を作製した。Example 5 Ni and Si fine powders were mixed at a ratio of 1:1 (atomic ratio), formed into a block shape, and then heat-treated in a vacuum at a temperature of 1400°C to form a silicide containing NiSi as the main component. A conductive material made of nickel was fabricated.
この導電材料を、あら粉砕し、つぎに、らいかい機粉砕
し、さらに２４時間ボールミル粉砕をおこなって、導電
性微粉末を作製した。This conductive material was roughly pulverized, then pulverized in a miller, and further pulverized in a ball mill for 24 hours to produce a conductive fine powder.
つぎＧこ、＊導電性微粉末とガラスフリットを第５表に
示す割合で配合し、有機質粘結剤を雄刃［ルて抵抗組成
物を作製した。Next, conductive fine powder and glass frit were blended in the proportions shown in Table 5, and an organic binder was added to the mixture to prepare a resistance composition.
この抵抗組成物を、実施例１と同様にして、アルミナ磁
器基板−Ｌに印刷し、乾燥後、焼成して抵抗体を作製し
た。This resistor composition was printed on an alumina ceramic substrate-L in the same manner as in Example 1, dried, and fired to produce a resistor.
２５℃における面積抵抗値、２５°Ｃと１２５℃の温度
間で測定した抵抗温度係数を第５表１こ示す。Table 5 shows the sheet resistance value at 25°C and the temperature coefficient of resistance measured between 25°C and 125°C.
負荷寿命特性は、実施例１と同様にして測定した結果、
すべての試料ζこついて、抵抗値変化率は、±１％以内
であった。The load life characteristics were measured in the same manner as in Example 1, and the results were as follows:
For all samples ζ, the resistance value change rate was within ±1%.
実施例 ６
ＮｉとＳｉの各微粉末を３：２．８（原子比）ｃコ混合
し、ブ爾ツク状に成形した後、真空中において１４００
８Ｃの温度で熱処理して、Ｎ ｌ ３ Ｓ ｉ２とＮｉ
Ｓｉを主成分とするけい化ニッケルからなる導電材料を
作製した。Example 6 Fine powders of Ni and Si were mixed at a ratio of 3:2.8 (atomic ratio), formed into a book shape, and heated to 1400°C in a vacuum.
After heat treatment at a temperature of 8C, N l 3 S i2 and Ni
A conductive material made of nickel silicide containing Si as a main component was produced.
この導電材料をあら粉砕し、らいかい機粉砕し、さらに
２４時間ボールミル粉砕をおこなって、導電性微粉末を
作製した。This conductive material was roughly pulverized, pulverized in a miller, and further pulverized in a ball mill for 24 hours to produce a conductive fine powder.
つぎに、導電性微粉末とガラスフリットを第６表（こ示
＊す割合で配合し、廟機質粘結材を添カロして抵抗組成
物を作製した。Next, conductive fine powder and glass frit were blended in the proportions shown in Table 6 (*), and a material binder was added to prepare a resistance composition.
この抵抗組成物を、実施例１と同様にして、アルミナ磁
器基板上Ｇこ印刷し、乾燥後、焼成して抵抗体を作製し
た。This resistor composition was printed on an alumina ceramic substrate in the same manner as in Example 1, dried, and fired to produce a resistor.
２５℃における面積抵抗値、２５’Ｃと１２５°Ｃの温
度間で測定した抵抗温度係数を第６表に示す。Table 6 shows the sheet resistance value at 25°C and the temperature coefficient of resistance measured between 25'C and 125°C.
負荷寿命特性は、実施例１−と同様にして測定した結果
、すべての試料について、抵抗値変化率は±１％以内で
あった。The load life characteristics were measured in the same manner as in Example 1. As a result, the rate of change in resistance value was within ±1% for all samples.
実施例 ７
２４時間ボールミル粉砕して作製したＮｉＳｉからなる
導電性微粉末と、１２０時間ボールミル粉砕して作製し
たＮ １３Ｓ ｉからなる導電性微粉末と、ガラスフリ
ットとを、第７表に示す割合で配合し、有機質粘結剤を
雄刃Ｏして抵抗組成物を作製した。Example 7 Conductive fine powder made of NiSi prepared by ball milling for 24 hours, conductive fine powder made of N 13S i prepared by ball milling for 120 hours, and glass frit in the proportions shown in Table 7. A resistance composition was prepared by adding an organic binder to the mixture.
この抵抗組成物を、実施例１と同様にして、アルミナ磁
器基板上σこ印刷し、乾燥後、焼成して抵抗体を作製し
た。This resistor composition was printed on an alumina ceramic substrate in the same manner as in Example 1, dried, and fired to produce a resistor.
２５°Ｃ（こおける面積抵抗値、２５℃と１２５°Ｃの
温度間で測定した抵抗温度係数を第７表に示す。Table 7 shows the sheet resistance value at 25°C (temperature coefficient of resistance measured between 25°C and 125°C).
負荷寿命特性は、実施例１と同様にして測定した結果、
すべての試料について、抵抗値変化率は±１％以内であ
る。The load life characteristics were measured in the same manner as in Example 1, and the results were as follows:
For all samples, the resistance value change rate is within ±1%.
実施例 ８
２４時間ボールミル粉砕して作製したＮ ｉ５ Ｓ ｉ
２からなる導電性微粉末と、１５時間ボールミル粉砕し
て作製したＮｉＳｉ２からなる導電性微粉末と、ガラス
フリットとを、第８表に示す割合で配合し、有機質粘結
剤を添加して抵抗組成物を作製した。Example 8 N i5 S i produced by ball milling for 24 hours
Conductive fine powder consisting of NiSi2, conductive fine powder consisting of NiSi2 prepared by ball milling for 15 hours, and glass frit were blended in the proportions shown in Table 8, and an organic binder was added to form a resistive powder. A composition was prepared.
この抵抗組成物を、実施例］と同様にして、アル中ミナ
磁器基板−［に印刷し、乾燥後、焼成して抵抗体を作製
した。This resistor composition was printed on an alumina ceramic substrate in the same manner as in Example, dried, and fired to produce a resistor.
２５°Ｃにおける面積抵抗値、２５°Ｃと１２５℃の温
度間で測定した抵抗温度係数を第８表に示す。Table 8 shows the sheet resistance value at 25°C and the temperature coefficient of resistance measured between 25°C and 125°C.
負荷寿命特性は、実施例１と同様にして測定した結果、
すべての試料について、抵抗値変化率は±１％以内であ
る。The load life characteristics were measured in the same manner as in Example 1, and the results were as follows:
For all samples, the resistance value change rate is within ±1%.
以上、実施例から明らかなように、本発明のけい化ニッ
ケルからなる導電性微粉末と、ガラスフリットとを含有
する抵抗組成物を用いた抵抗体は、低い抵抗値のものが
容易に得られること、負荷寿命特性など抵抗緒特性が優
れていること、金属けい化物ならひにガラスからなるた
め不燃性であること、空気中で焼成して抵抗体を作製す
ることができ、またＡｇやＰ ｄ 、 ＲｕＯ２などか
らなる貴金属系の抵抗組成物にくらべて、非常ｌこ安価
であることなどの多くの利点を有するものである。As is clear from the examples above, a resistor using a resistive composition containing a conductive fine powder of nickel silicide of the present invention and a glass frit can easily have a low resistance value. In addition, metal silicides have excellent resistance characteristics such as load life characteristics, are nonflammable because they are made of glass, and can be fired in air to produce resistors. It has many advantages, such as being much cheaper than noble metal-based resistance compositions made of d, RuO2, etc.
したがって、混成集積回路用抵抗体や抵抗ネットワーク
だけでなく、電力用や一般用の各種固定抵抗器や可変抵
抗器や電熱器用発熱体さらには、とくに低い抵抗値のも
のは、一種の導体としても使用することができるなど、
その用途は広い。Therefore, in addition to resistors and resistance networks for hybrid integrated circuits, various fixed resistors and variable resistors for electric power and general use, heating elements for electric heaters, and those with particularly low resistance values can also be used as a kind of conductor. can be used, etc.
Its uses are wide.
また、本発明において使用目的に応じてそれ（こ適した
特性の抵抗器を得るため、さらに他の成分を追加導入す
ることができるのは言うまでもないことである。It goes without saying that in the present invention, other components can be added in order to obtain a resistor with suitable characteristics depending on the purpose of use.
Claims (1)
リットとを含有し、前記導電性微粉末と前記ガラスフリ
ットとの重量比率が２０：８０から７５ ： ２５の範
囲内にあることを特徴とする抵抗組成物。 ２、特許請求の範囲第１項の記載において、前記導電性
微粉末がＮｉ３Ｓｉ ＋ Ｎｉ５Ｓｉ２ 、Ｎｉ２Ｓｉ
ｒＮｉ３Ｓｉ２およびＮｉＳｉから選択されたひとつ
からなることを特徴とする抵抗組成物。 ３ 特許請求の範囲第１項の記載において、前記導電性
微粉末がＮｉ３Ｓｉ 、Ｎｉ５Ｓｉ２ ＋ Ｎｉ２Ｓｉ
＋Ｎ １３８１２１ Ｎ ＋ Ｓ ＋およびＮｉＳｉ
２から選択された少なくとも２種からなることを特徴と
する抵抗組成物。[Claims] 1. Contains a conductive fine powder made of nickel silicide and a glass frit, and the weight ratio of the conductive fine powder and the glass frit is in the range of 20:80 to 75:25. A resistive composition comprising: 2. Claim 1 states that the conductive fine powder is Ni3Si + Ni5Si2, Ni2Si
A resistive composition comprising one selected from rNi3Si2 and NiSi. 3. In claim 1, the conductive fine powder is Ni3Si, Ni5Si2 + Ni2Si.
+N 138121 N + S + and NiSi
1. A resistance composition comprising at least two selected from the group consisting of:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP51030103A JPS5845161B2 (en) | 1976-03-18 | 1976-03-18 | resistance composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP51030103A JPS5845161B2 (en) | 1976-03-18 | 1976-03-18 | resistance composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS52112796A JPS52112796A (en) | 1977-09-21 |
| JPS5845161B2 true JPS5845161B2 (en) | 1983-10-07 |
Family
ID=12294435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP51030103A Expired JPS5845161B2 (en) | 1976-03-18 | 1976-03-18 | resistance composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5845161B2 (en) |
-
1976
- 1976-03-18 JP JP51030103A patent/JPS5845161B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS52112796A (en) | 1977-09-21 |
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