JP2018049901A - Resistance paste and resistor produced by firing the same - Google Patents
Resistance paste and resistor produced by firing the same Download PDFInfo
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本発明は、厚膜チップ抵抗器やハイブリッドＩＣなどの抵抗体の材料として使用される抵抗ペースト、特に鉛を含有しない抵抗ペースト及びこれを焼成して作製される抵抗体に関するものである。 The present invention relates to a resistor paste used as a material for resistors such as thick film chip resistors and hybrid ICs, and more particularly to a resistor paste containing no lead and a resistor produced by firing the paste.
従来、電子部品の抵抗体被膜を形成する方法としては、膜形成材料を含む抵抗ペーストを用いて成膜する厚膜方式と膜形成材料をスパッタリング等することで成膜する薄膜方式が一般的に知られている。それらのうち、厚膜方式は抵抗ペーストをセラミック基板上に印刷した後、焼成することで抵抗体を形成するものであり、この方法は成膜に必要な設備が安価で生産性も高いことから、チップ抵抗器やハイブリッドＩＣなどの電子部品が有する抵抗体の製造に広範に利用されている。 Conventionally, as a method for forming a resistor film of an electronic component, a thick film method in which a film is formed using a resistance paste containing a film forming material and a thin film method in which a film forming material is formed by sputtering or the like are generally used. Are known. Among them, the thick film method is to form a resistor by printing a resistor paste on a ceramic substrate and then firing it. This method is inexpensive and has high productivity required for film formation. It is widely used for manufacturing resistors included in electronic components such as chip resistors and hybrid ICs.
上記の厚膜方式に用いる抵抗ペーストは、導電性粒子及びガラスフリット、並びにそれらを印刷に適したペースト状にするための有機ビヒクルから実質的に構成される。導電性粒子としては、二酸化ルテニウム（ＲｕＯ２）やパイロクロア型ルテニウム系酸化物（Ｐｂ２Ｒｕ２Ｏ７−Ｘ、Ｂｉ２Ｒｕ２Ｏ７）が一般に使われている。このように導電性粒子としてＲｕ系酸化物を用いるのは、主に導電性粒子の濃度に対して抵抗値がなだらかに変化するためである。 The resistive paste used in the thick film system is substantially composed of conductive particles and glass frit, and an organic vehicle for making them suitable for printing. As the conductive particles, ruthenium dioxide (RuO 2 ) or pyrochlore-type ruthenium-based oxides (Pb 2 Ru 2 O 7-X , Bi 2 Ru 2 O 7 ) are generally used. The reason why the Ru-based oxide is used as the conductive particles is mainly because the resistance value changes gently with respect to the concentration of the conductive particles.
また、ガラスフリットとしては、ホウケイ酸鉛ガラス（ＰｂＯ−ＳｉＯ２−Ｂ２Ｏ３）やアルミノホウケイ酸鉛ガラス（ＰｂＯ−ＳｉＯ２−Ｂ２Ｏ３−Ａｌ２Ｏ３）など、鉛を多量に含むホウケイ酸鉛系ガラスが使われている。このようにガラスフリットにホウケイ酸鉛系ガラスを用いるのは、Ｒｕ系酸化物との濡れ性が良く、熱膨張係数が基板のそれに近く、焼成時の粘性などが適しているからである。 In addition, as a glass frit, a large amount of lead such as lead borosilicate glass (PbO—SiO 2 —B 2 O 3 ) and lead aluminoborosilicate glass (PbO—SiO 2 —B 2 O 3 —Al 2 O 3 ) is used. Including lead borosilicate glass. The reason why the lead borosilicate glass is used for the glass frit in this way is that it has good wettability with the Ru-based oxide, has a thermal expansion coefficient close to that of the substrate, and has a suitable viscosity during firing.
上記の抵抗ペーストでは、成膜後の抵抗体の特性を改善するため、各種添加剤を含有させることが昔から行われている。例えば特許文献１には、酸化ルテニウム、酸化鉛、酸化珪素、及び酸化アルミニウムを含む粉砕物を有機ビヒクルに対して添加剤として酸化スズ（ＳｎＯ２）を所定量含有させることで、焼成により得られる抵抗体の抵抗温度係数の絶対値と電流ノイズとを小さくする技術が開示されている。 In the above-described resistance paste, various additives have been included for a long time in order to improve the characteristics of the resistor after film formation. For example, in Patent Document 1, a pulverized product containing ruthenium oxide, lead oxide, silicon oxide, and aluminum oxide is obtained by firing by adding a predetermined amount of tin oxide (SnO 2 ) as an additive to the organic vehicle. A technique for reducing the absolute value of the resistance temperature coefficient of the resistor and the current noise is disclosed.
近年、環境保護に配慮して電子部品では鉛フリー化が進められており、抵抗ペーストにおいても鉛フリー化が求められている。また、上記した抵抗ペーストを材料にして作製される電子部品等はますます小型化、高性能化する傾向にあり、これに伴い抵抗ペーストには抵抗値を高くしても電流ノイズの小さい抵抗体を作製できるものが求められている。 In recent years, lead-free electronic components have been promoted in consideration of environmental protection, and lead-free solder pastes are also required. In addition, electronic components made from the above-mentioned resistance paste are becoming smaller and higher performance, and as a result, resistance pastes have low current noise even if the resistance value is increased. There is a demand for a material that can be used.
本発明は上記の状況に鑑みてなされたものであり、高い抵抗値を有しながら電流ノイズを小さく抑えることが可能な電気的特性に優れた鉛フリーの厚膜抵抗体を形成することができる鉛フリーの抵抗ペーストを提供することを目的とする。 The present invention has been made in view of the above situation, and can form a lead-free thick film resistor excellent in electrical characteristics capable of suppressing current noise while having a high resistance value. An object is to provide a lead-free resistance paste.
本発明者は、上記目的を達成可能な鉛フリーの抵抗ペーストについて検討を重ねた結果、抵抗ペーストに特定の添加剤を含有させることによって、導電性粒子にルテニウムを含む鉛フリーの酸化物を用いると共に、ガラスフリットにも鉛フリーのものを用いる場合であっても良好な電気的特性を有する抵抗体を作製できることを見出し、本発明を完成するに至った。 As a result of repeated studies on a lead-free resistance paste capable of achieving the above object, the present inventor uses a lead-free oxide containing ruthenium in conductive particles by including a specific additive in the resistance paste. At the same time, it has been found that a resistor having good electrical characteristics can be produced even when a lead-free glass frit is used, and the present invention has been completed.
即ち、本発明が提供する抵抗ペーストは、二酸化ルテニウムからなる導電性粒子と、鉛を含まないガラスフリットと、有機ビヒクルと、添加剤とで実質的に構成される抵抗ペーストであって、前記添加剤として酸化スズ換算量で０.１〜１.８質量％の有機スズ化合物を含んでいることを特徴としている。 That is, the resistance paste provided by the present invention is a resistance paste substantially composed of conductive particles made of ruthenium dioxide, glass frit containing no lead, an organic vehicle, and an additive. It is characterized by containing 0.1 to 1.8% by mass of an organic tin compound in terms of tin oxide as an agent.
本発明によれば、鉛による環境汚染を引き起こすことなく、高い抵抗値を有しながら電流ノイズを小さく抑えることが可能な電気的特性に優れた厚膜抵抗体を作製できる抵抗ペーストを提供することができる。 According to the present invention, there is provided a resistance paste capable of producing a thick film resistor excellent in electrical characteristics capable of suppressing current noise to a low level while having a high resistance value without causing environmental pollution due to lead. Can do.
以下、本発明の抵抗ペーストの実施形態について説明する。この本発明の実施形態の抵抗ペーストに用いる二酸化ルテニウムの形態については特に制限はなく、一般的な製法で得られる酸化物を使用することができる。ただし、焼成により形成される厚膜抵抗体の抵抗値のばらつきや電流ノイズをできるだけ抑えるため、当該厚膜抵抗体中の導電パスを微細にするのが望ましく、そのためには酸化物の粒子のＢＥＴ径による平均粒径が１.０μｍ以下であるのが望ましい。 Hereinafter, embodiments of the resistance paste of the present invention will be described. There is no restriction | limiting in particular about the form of ruthenium dioxide used for the resistance paste of this embodiment of this invention, The oxide obtained by a general manufacturing method can be used. However, in order to suppress the variation in resistance value and current noise of the thick film resistor formed by firing as much as possible, it is desirable to make the conductive path in the thick film resistor finer. It is desirable that the average particle diameter by diameter is 1.0 μm or less.
上記抵抗ペーストを構成するガラスフリットは、鉛を含まないものであれば特にその組成に制限はない。例えば、ホウケイ酸ガラス、アルミノホウケイ酸ガラス、ホウケイ酸アルカリ土類ガラス、ホウケイ酸アルカリガラス、ホウケイ酸亜鉛ガラス、ホウケイ酸ビスマスガラスなどを用いることができる。前述したように、厚膜抵抗体中の導電パスを微細にして該厚膜抵抗体の抵抗値のばらつきや電流ノイズをできるだけ抑えるため、ガラスフリットのレーザー回折式粒度分布測定によるＤ５０（メジアン径）は５μｍ以下であることが好ましい。 If the glass frit which comprises the said resistance paste does not contain lead, there will be no restriction | limiting in particular in the composition. For example, borosilicate glass, aluminoborosilicate glass, borosilicate alkaline earth glass, borosilicate alkali glass, borosilicate zinc glass, borosilicate bismuth glass, or the like can be used. As described above, D50 (median diameter) measured by laser diffraction particle size distribution measurement of glass frit to minimize the conductive path in the thick film resistor and suppress variations in resistance value and current noise of the thick film resistor as much as possible. Is preferably 5 μm or less.
上記抵抗ペーストを構成する有機ビヒクルは、抵抗ペーストに通常使用されているものであってよく、例えば、エチルセルロース、ブチラール、アクリルなどの樹脂をターピネオール、ブチルカルビトールアセテートなどの溶剤に溶解したものが好適に用いられる。 The organic vehicle constituting the resistance paste may be one normally used for the resistance paste, for example, a resin obtained by dissolving a resin such as ethyl cellulose, butyral, or acrylic in a solvent such as terpineol or butyl carbitol acetate. Used for.
上記抵抗ペーストは、更に添加剤として有機スズ化合物を酸化スズ換算量で０.１質量％以上１.８質量％以下含有している。添加剤としての有機スズ化合物の種類については特に制限はなく、例えばオクチル酸第一スズ、ジブチルスズジアセテ−ト等を用いることができる。一般的に酸化スズは、焼成により形成される抵抗体の抵抗値を上昇させて電流ノイズを小さくする働きを有しているものの、酸化スズ粉の状態で添加しただけではその働きが不十分になりやすい。これに対して、上記の通り有機スズ化合物を添加することにより抵抗値を良好に上昇させることが可能になる。有機スズ化合物の含有量を抵抗ペーストに対して酸化スズ換算量で０.１質量％以上１.８質量％以下とするのは、０.１質量％未満では電流ノイズを小さくする効果が十分得られないからである。逆に、１.８質量％を超えると抵抗値が高くなり過ぎて、電流ノイズを小さくする効果が十分得られなくなるおそれがある。 The resistance paste further contains an organic tin compound as an additive in an amount of 0.1% by mass to 1.8% by mass in terms of tin oxide. There is no restriction | limiting in particular about the kind of organotin compound as an additive, For example, a stannous octylate, dibutyltin diacetate, etc. can be used. In general, tin oxide has the function of reducing the current noise by increasing the resistance value of the resistor formed by firing, but its function is insufficient only by adding it in the state of tin oxide powder. Prone. On the other hand, it becomes possible to raise a resistance value favorably by adding an organotin compound as mentioned above. The content of the organic tin compound is 0.1% by mass or more and 1.8% by mass or less in terms of tin oxide based on the resistance paste. If the content is less than 0.1% by mass, the effect of reducing current noise is sufficiently obtained. Because it is not possible. On the other hand, if it exceeds 1.8% by mass, the resistance value becomes too high, and the effect of reducing the current noise may not be obtained sufficiently.
上記した本発明の実施形態の抵抗ペーストの製造法は特に制約がなく、ロールミルなどの市販の混練装置に、上記した抵抗ペーストの構成成分の所定量を秤量して装入し、混練することで作製することができる。その際、導電性粒子とガラスフリットの混合割合は、質量基準による導電性粒子／ガラスフリットの比で５／９５〜５０／５０程度であるのが好ましい。また、抵抗体の作製法も特に制約がなく、上記した本発明の実施形態の抵抗ペーストを材料として用いて従来と同様の方法で形成することができる。例えば、上記した抵抗ペーストをアルミナ基板などの通常の基板上にスクリーン印刷法などにより塗布し、乾燥した後、ベルト炉などを用いて８００〜９００℃程度のピーク温度で焼成することによって、鉛フリーの抵抗体を形成することができる。 The method for producing the resistance paste of the above-described embodiment of the present invention is not particularly limited, and a predetermined amount of the components of the resistance paste described above is weighed into a commercially available kneading apparatus such as a roll mill, and kneaded. Can be produced. At that time, the mixing ratio of the conductive particles and the glass frit is preferably about 5/95 to 50/50 in terms of the ratio of the conductive particles / glass frit on a mass basis. Further, the method for manufacturing the resistor is not particularly limited, and the resistor can be formed by the same method as the conventional one using the resistor paste of the embodiment of the present invention as a material. For example, the above-described resistance paste is applied to a normal substrate such as an alumina substrate by screen printing or the like, dried, and then fired at a peak temperature of about 800 to 900 ° C. using a belt furnace or the like, thereby lead-free. Can be formed.
尚、本発明の実施形態の抵抗ペーストは、上記した必須成分の他に、厚膜抵抗体の電気的特性を調整するために従来から通常使用されている例えば分散剤、可塑剤などの種々の添加剤を必要に応じて添加してもよい。 In addition to the essential components described above, the resistor paste according to the embodiment of the present invention is conventionally used in various ways such as dispersants and plasticizers that are conventionally used to adjust the electrical characteristics of thick film resistors. You may add an additive as needed.
導電性粒子、ガラスフリット、有機ビヒクル、及び添加剤を様々な配合割合で混合して複数の抵抗ペースト試料を調製し、それらを各々焼成することで厚膜抵抗体を形成し、その電気的特性について評価した。具体的には、導電性粒子には水酸化ルテニウムを焙焼することによって作製したＢＥＴ径４０ｎｍのＲｕＯ２粉末を用意した。ガラスフリットには一般的な方法で混合、溶融、急冷、粉砕することによって作製した１０質量％ＳｒＯ−４３質量％ＳｉＯ２−１６質量％Ｂ２Ｏ３−４質量％Ａｌ２Ｏ３−２０質量％ＺｎＯ−７質量％Ｎａ２Ｏの組成を有するレーザー回折式粒度分布測定によるＤ５０が１.９μｍのガラスフリットを用意した。 Conductive particles, glass frit, organic vehicle, and additives are mixed at various blending ratios to prepare multiple resistor paste samples, which are then fired to form thick film resistors and their electrical properties Was evaluated. Specifically, RuO 2 powder having a BET diameter of 40 nm prepared by roasting ruthenium hydroxide was prepared as the conductive particles. For glass frit, 10 mass% SrO-43 mass% SiO 2 -16 mass% B 2 O 3 -4 mass% Al 2 O 3 -20 mass produced by mixing, melting, quenching, and pulverizing by a general method. A glass frit having a composition of% ZnO-7 mass% Na 2 O and having a D50 of 1.9 μm as measured by laser diffraction particle size distribution was prepared.
添加剤にはオクチル酸第一スズ（有機スズＡ）、ジブチルスズジアセテ−ト（有機スズＢ）、及びＳｎＯ２を用意し、有機ビヒクルにはエチルセルロースとターピネオールを主成分とするものを用意した。これらＲｕＯ２粉末、ガラスフリット、添加剤、及び有機ビヒクルを様々な配合割合となるように秤量し、三本ロールミルで混練した。これにより試料１〜８の抵抗ペーストを作製した。 As additives, stannous octylate (organotin A), dibutyltin diacetate (organotin B), and SnO 2 were prepared, and an organic vehicle containing ethylcellulose and terpineol as main components was prepared. These RuO 2 powder, glass frit, additive, and organic vehicle were weighed so as to have various blending ratios and kneaded by a three-roll mill. This produced the resistance paste of samples 1-8.
次に、各試料の抵抗ペーストに対して、ＡｇＰｄペーストを用いて電極間距離１ｍｍの２つの電極が形成されたアルミナ基板を用意し、該アルミナ基板上において上記両電極を接続するように抵抗ペーストを幅１ｍｍにスクリ−ン印刷し、１５０℃で１０分間乾燥した後、ベルト炉にてピーク温度８５０℃で９分間焼成した。このようにして作製した厚膜抵抗体の電気的特性（抵抗値、電流ノイズ）を測定した。この電気的特性の測定結果を、使用した抵抗ペーストの組成と共に下記表１に示す。尚、抵抗値はＫＥＩＴＨＬＥＹ社製のＭｏｄｅｌ２００１Ｍｕｌｔｉｍｅｔｅｒを用いて４端子法にて測定し、電流ノイズはＱｕａｎ−Ｔｅｃｈ社製のノイズメーターＭｏｄｅｌ３１５Ｃを用いて１／１０Ｗ印加で測定した。 Next, an alumina substrate on which two electrodes having an interelectrode distance of 1 mm are formed using AgPd paste is prepared for the resistance paste of each sample, and the two electrodes are connected on the alumina substrate. Was screen printed to a width of 1 mm, dried at 150 ° C. for 10 minutes, and then fired in a belt furnace at a peak temperature of 850 ° C. for 9 minutes. The electrical characteristics (resistance value, current noise) of the thick film resistor thus fabricated were measured. The measurement results of the electrical characteristics are shown in Table 1 below together with the composition of the resistance paste used. The resistance value was measured by a four-terminal method using a Model 2001 Multimeter manufactured by KEITHLEY, and the current noise was measured by applying 1/10 W using a noise meter Model 315C manufactured by Quan-Tech.
上記表１においてほぼ同程度の抵抗値を有する試料１と試料５、試料２及び４と試料６〜７、及び試料３と試料８をそれぞれ比較することで分かるように、安価なＲｕＯ２からなる導電性粒子と鉛フリーのガラスフリットとを用いて厚膜抵抗体を形成した場合においても、添加剤としてオクチル酸第一スズ又はジブチルスズジアセテ−トを本発明が規定する範囲内で添加することによって、これら有機スズを加えないか又は従来から用いられているＳｎＯ２を添加剤として含有させる場合に比べて電流ノイズを小さくできることが分かる。
In Table 1 above, as can be seen by comparing Sample 1 and Sample 5, Samples 2 and 4, Samples 6-7, and Sample 3 and Sample 8 having substantially the same resistance value, each is made of inexpensive RuO 2. Even when a thick film resistor is formed using conductive particles and lead-free glass frit, stannous octylate or dibutyltin diacetate should be added within the range specified by the present invention as an additive. Thus, it can be seen that the current noise can be reduced as compared with the case where these organotins are not added or SnO 2 conventionally used is added as an additive.
Claims (5)
A method for producing a lead-free resistor, wherein the resistor is produced by firing the resistor paste according to claim 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7367547B2 (en) | 2020-01-31 | 2023-10-24 | 住友金属鉱山株式会社 | Thick film resistor composition, thick film resistor paste, and thick film resistor |
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