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JPH04144937A - Sealing material - Google Patents

Sealing material

Info

Publication number
JPH04144937A
JPH04144937A JP26587390A JP26587390A JPH04144937A JP H04144937 A JPH04144937 A JP H04144937A JP 26587390 A JP26587390 A JP 26587390A JP 26587390 A JP26587390 A JP 26587390A JP H04144937 A JPH04144937 A JP H04144937A
Authority
JP
Japan
Prior art keywords
sealing material
pbo
glass
low
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.)
Pending
Application number
JP26587390A
Other languages
Japanese (ja)
Inventor
Toshiro Yamanaka
俊郎 山中
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Electric Glass Co Ltd
Original Assignee
Nippon Electric Glass Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Electric Glass Co Ltd filed Critical Nippon Electric Glass Co Ltd
Priority to JP26587390A priority Critical patent/JPH04144937A/en
Publication of JPH04144937A publication Critical patent/JPH04144937A/en
Pending legal-status Critical Current

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  • Glass Compositions (AREA)

Abstract

PURPOSE:To obtain a sealing material showing a low coefficient of thermal expansion and excellent fluidity by blending PbO-V2O5-based glass powder with a filler of NaZr2(PO4) type solid solution powder. CONSTITUTION:A sealing material comprising PbO-V2O5-based glass powder and a filler of NaZr2(PO4) type solid solution powder. Glass powder having a composition of 20-50wt.% PbO, 20-50wt.% V2O5, 5-40wt.% TeO2 and 0-8wt.% Al2O3 is used as the glass powder. The solid solution is a substance shown by the formula, the substance forms a solid solution in a wide range and has characteristics of low coefficient of thermal expansion. Since the sealing material has excellent fluidity, the sealing temperature is low, a coefficient of thermal expansion is low, is close to that of alumina, the sealing material is suitable as a sealing material for ceramic packaging using alumina.

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明は、封着材料に関し、より具体的にはアルミナを
使用したセラミックパッケージの気密封着に好適な封着
材料に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a sealing material, and more specifically to a sealing material suitable for hermetically sealing a ceramic package using alumina.

[従来の技術] 従来よりセラミックパッケージの気密封着に使用する封
着材料としては、PbO−8203系の低融点ガラスに
ウイレマイト、コージェライト、ジルコン、酸化すず、
β−ユークリプタイト等の低膨張セラミック粉末のフィ
ラーを混合したものが使用されている。
[Prior Art] Sealing materials conventionally used for hermetically sealing ceramic packages include PbO-8203-based low melting point glass, willemite, cordierite, zircon, tin oxide,
A mixture of a filler of low expansion ceramic powder such as β-eucryptite is used.

近年、セラミックパッケージに集積度の高いICや特殊
な水晶振動子等の熱に敏感な素子を搭載することがあり
、この゛ためセラミックパッケージの封着材料の封着温
度をより下げることが強く望まれているが、PbO−8
20s系の低融点ガラスを用いた封着材料ではこの要求
に応えることが困難である。
In recent years, ceramic packages are sometimes equipped with heat-sensitive elements such as highly integrated ICs and special crystal oscillators.Therefore, there is a strong desire to lower the sealing temperature of the sealing material for ceramic packages. Although it is rare, PbO-8
It is difficult to meet this requirement with a sealing material using 20S type low melting point glass.

このような事情からPbO−8203系ガラスよりも低
い温度で封着可能な低融点ガラスとしてpbo −v2
05系ガラスが開発され、この系のガラスに低膨張セラ
ミック粉末のフィラーを混合してなる封着材料が提案さ
れている。
Due to these circumstances, pbo-v2 is a low-melting glass that can be sealed at a lower temperature than PbO-8203 glass.
05 series glass has been developed, and a sealing material made by mixing this glass with a filler of low expansion ceramic powder has been proposed.

[発明が解決しようとする問題点コ 先記したようにpbo−v2oIs系ガラスは、低い温
度で封着可能であるが、熱膨張係数をアルミナのそれ(
約70X 10−7/ ”C)に近似させる目的で、こ
のガラスに対して通常のフィラー、すなわちウイレマイ
ト、コージェライト、ジルコン、酸化すず、β−ユーク
リプタイト等の低膨張セラミック粉末のフィラーを混合
すると、熱膨張係数は低下するが、材料の流動性が著し
く損なわれ、低い温度で封着することが困難になるとい
う問題が生じる。
[Problems to be solved by the invention] As mentioned earlier, pbo-v2oIs glass can be sealed at low temperatures, but its thermal expansion coefficient is lower than that of alumina (
For the purpose of approximating approximately 70X 10-7/''C), ordinary fillers, such as fillers of low expansion ceramic powders such as willemite, cordierite, zircon, tin oxide, and β-eucryptite, are mixed with this glass. This causes a problem in that although the coefficient of thermal expansion decreases, the fluidity of the material is significantly impaired, making it difficult to seal at low temperatures.

本発明の目的は、Pb0−v20.系ガラスと低膨張セ
ラミック粉末のフィラーとからなり、熱膨張係数が低く
、且つ良好な流動性を有するため低い温度で封着するこ
とが可能な封着材料を提供することである。
The object of the present invention is that Pb0-v20. It is an object of the present invention to provide a sealing material which is made of glass and a filler of low expansion ceramic powder, has a low coefficient of thermal expansion, and has good fluidity, so that it can be sealed at a low temperature.

口問題点を解決するための手段] 本発明者は、フィラーとして各種の低膨張材料を研究し
ていく中で、NaZr2(PO4)3型固溶体がPbO
−V2O5系ガラスと相性が良く、これを粉末にしてp
bo−v2oe5系ガラス粉末と混合した場合、良好な
流動性を示すことを見い出し、本発明を提案するに到っ
た。
[Means for Solving Problems] While researching various low expansion materials as fillers, the present inventor found that NaZr2(PO4)3 type solid solution was PbO
-Compatible with V2O5 glass, which can be made into powder.
It was discovered that good fluidity is exhibited when mixed with bo-v2oe5-based glass powder, and the present invention was proposed.

すなわち本発明の封着材料は、Pb0−V2O5系ガラ
ス粉末とNaZr2(PO4)3型固溶体粉末のフィラ
ーとからなることを特徴とする。
That is, the sealing material of the present invention is characterized by comprising a Pb0-V2O5 glass powder and a filler of NaZr2(PO4)3 type solid solution powder.

また本発明の封着材料のpbo −V2O5系ガラス粉
末は、重量百分率でPbO20〜50%、V2Ch  
2(1〜50%、TeO□5〜40%、A1□030〜
8%の組成を有することを特徴とする。
Furthermore, the pbo-V2O5 glass powder of the sealing material of the present invention has a weight percentage of PbO20 to 50%, V2Ch
2 (1~50%, TeO□5~40%, A1□030~
It is characterized by having a composition of 8%.

[作用コ 本発明で使用するNaZr2(PO4)+堅固溶体は、
次の一般式で表される物質であり、Xは1価に相当する
元素よりなり、Yは4価に相当する元素よりなり、また
Zは5価に相当する元素よりなる。
[Function] The NaZr2 (PO4) + solid solution used in the present invention is
It is a substance represented by the following general formula, where X is an element corresponding to a monovalent element, Y is an element corresponding to a tetravalent element, and Z is an element corresponding to a pentavalent element.

X  Y2 Z3012 X = Li、Na、に、 ’/2Mg、 ”/2Ca
、’/2Sr、’/4ZrY = Zr、Ti、Sn、
Nb−Na、Ta−Na、V−NaZ = P、Si+
Na この物質は、広範囲に固溶体を形成し、熱膨張係数が低
いという特性を有している。
X Y2 Z3012 X = Li, Na, '/2Mg, '/2Ca
,'/2Sr,'/4ZrY = Zr, Ti, Sn,
Nb-Na, Ta-Na, V-NaZ = P, Si+
Na This material has the characteristics of forming a solid solution over a wide range and having a low coefficient of thermal expansion.

また本発明で使用するPbOV20a系ガラス粉末の成
分を先記のように限定した理由は以下のとおりである。
Further, the reason why the components of the PbOV20a-based glass powder used in the present invention are limited as described above is as follows.

PbOが20%より少ないと370℃以下の温度でガラ
スが充分に流動しなくなり、55%より多いと封着時に
結晶化を起こし、流動しなくなる。
If PbO is less than 20%, the glass will not flow sufficiently at temperatures below 370° C., and if it is more than 55%, crystallization will occur during sealing and the glass will not flow.

V2O5が、20%より少ないとガラス化が困難となり
、55%より多いと封着時に結晶化を起こし、流動しな
くなる。
If V2O5 is less than 20%, vitrification will be difficult, and if it is more than 55%, crystallization will occur during sealing and will not flow.

Te09が5%より少ないと封着時に結晶化を起こし、
流動しなくなり、40%より多いと溶融ガラスの成形時
に失透する。
If Te09 is less than 5%, crystallization occurs during sealing,
If the amount exceeds 40%, the molten glass will become devitrified during molding.

Al2O3は、失透防止の効果があるが、8%より多い
とガラスの粘度が高くなり、370℃以下の温度で十分
に流動しなくなる。
Al2O3 has the effect of preventing devitrification, but if it exceeds 8%, the viscosity of the glass becomes high and it does not flow sufficiently at temperatures below 370°C.

尚、上記成分以外にも例えば10%以下のZnO1!1
1203 、P2O5や5%以下のCu2O、WO3、
B2O3,5102、Mo2O3、Nb2O6% Fe
2O3、ZrO2、SrO、BaOを含育させることが
可能である。
In addition to the above components, for example, 10% or less of ZnO1!1
1203, P2O5, 5% or less Cu2O, WO3,
B2O3,5102, Mo2O3, Nb2O6% Fe
It is possible to contain 2O3, ZrO2, SrO, and BaO.

[実施例コ 以下、本発明の封着材料を実施例に基づいて説明する。[Example code] Hereinafter, the sealing material of the present invention will be explained based on Examples.

第1表は、本発明のPbO−V205系ガラス粉末を示
すものである。
Table 1 shows the PbO-V205 glass powder of the present invention.

第1表に示したガラス粉末は、鉛丹、五酸化バナジウム
、二酸化テルル、亜鉛華、アルミナ、五酸化ニオブを表
記の組成になるように調合し、白金ルツボに入れ、電気
炉において800 ’Cで1時間溶融した後、薄板状に
成形し、次いでこの成形物をボールミルで粉砕し、20
0メツシユ篩を通過させることによって作製した。
The glass powder shown in Table 1 is prepared by mixing lead red, vanadium pentoxide, tellurium dioxide, zinc white, alumina, and niobium pentoxide to the indicated composition, placing it in a platinum crucible, and heating it in an electric furnace at 80'C. After melting for 1 hour at
0 mesh sieve.

第2表は、本発明のNaZr2(PO4)3型固溶体粉
末のフィラーを示すものである。
Table 2 shows the filler of the NaZr2(PO4)3 type solid solution powder of the present invention.

以下余白 第 表 第2表において試料No 、7のフィラーは、試料No
In Table 2 below, the filler for sample No. 7 is sample No.
.

lのフィラーのZrの1.0を1.0(Nb−Na)で
置換した組成であり、試料NO19のフィラーは試料N
o、1のフィラーのPの0.2を0.2(Si+Na)
で置換した組成である。また試料No、11のフィラー
は、試料No 、7のフィラーのNbの0.5をTaの
0.5で置換した組成である。
The filler of sample No. 19 has a composition in which 1.0 of Zr in the filler of sample No. 1 is replaced with 1.0 (Nb-Na).
o, 0.2 of P of filler 1 is 0.2 (Si+Na)
This is the composition replaced with . Further, the filler of sample No. 11 has a composition in which 0.5 of Nb in the filler of sample No. 7 is replaced with 0.5 of Ta.

第2表の各試料は、原料として炭酸ソーダ、炭酸リチウ
ム、炭酸カリ、炭酸カルシウム、炭酸ストロンチウム、
酸化マグネシウム、ジルコニア、チタニア、シリカ、酸
化すず、五酸化ニオブ、五酸化タンタル、五酸化バナジ
ウム、リン酸アンモニウム、正リン酸よりなるバッチを
湿式混合した後、1300〜1500℃で16時間焼成
し、次いでこの焼成品を粉砕後、20Gメツシユ篩を通
過させて平均粒径を約5ミクロンにしたものである。
Each sample in Table 2 uses soda carbonate, lithium carbonate, potassium carbonate, calcium carbonate, strontium carbonate,
After wet mixing a batch consisting of magnesium oxide, zirconia, titania, silica, tin oxide, niobium pentoxide, tantalum pentoxide, vanadium pentoxide, ammonium phosphate, and orthophosphoric acid, calcining at 1300 to 1500 ° C. for 16 hours, Next, this fired product was pulverized and passed through a 20G mesh sieve to have an average particle size of about 5 microns.

第3表は、第1表のPbOV2O5系ガラス粉末と第2
表のフィラーとを混合してなる封着材料を示すものであ
る。
Table 3 shows the PbOV2O5 glass powder in Table 1 and the PbOV2O5 glass powder in Table 1.
This shows a sealing material mixed with the filler shown in the table.

以下余白 第3表に示した各試料は、ガラス粉末とフィラーとを表
に示す割合に混合したものであり、熱膨張係数が74〜
79X 10−’/”Cとアルミナのそれに近似してお
り、且つ封着温度も370〜390℃と低い値を示した
Each sample shown in Table 3 below is a mixture of glass powder and filler in the ratio shown in the table, and has a coefficient of thermal expansion of 74 to 74.
79X 10-'/''C, which is close to that of alumina, and the sealing temperature also showed a low value of 370 to 390C.

尚、表中の熱膨張係数は、各試料から所望の大きさの焼
結体を作製した後、それを加工して直径4mm 、長さ
50+++aの円柱状の成形物を作製し、デイラドメー
ター(Dilatometer )によって測定した。
The coefficient of thermal expansion in the table is determined by producing a sintered body of the desired size from each sample, processing it to produce a cylindrical molded product with a diameter of 4 mm and a length of 50 +++ a, and measuring it with a deiradometer. (Dilatometer).

また封着温度は、各試料から外径201111h高さ5
mmのボタンを作製した後、このボタンを加熱して流動
させ、その外径が22mmになった温度を示したもので
ある。
In addition, the sealing temperature was determined from each sample at an outer diameter of 201111h and a height of 5.
After producing a button with a diameter of 22 mm, the button was heated to flow, and the temperature at which the outer diameter of the button became 22 mm is shown.

[発明の効果コ 以上のように本発明の封着材料は、Pb0−v205系
ガラスと、この系のガラスと相性の良いNaZr2(P
O4)3型固溶体粉末のフィラーとからなり、良好な流
動性を有するため封着温度が低く、且つ熱膨張係数も低
く、アルミナのそれに近似しているため、アルミナを使
用したセラミックパッケージの封着材料として好適であ
る。
[Effects of the Invention] As described above, the sealing material of the present invention contains Pb0-v205 glass and NaZr2 (Pb0-v205 glass), which is compatible with this glass type.
O4) It is composed of filler of type 3 solid solution powder and has good fluidity, so the sealing temperature is low and the coefficient of thermal expansion is low, which is similar to that of alumina, so it is suitable for sealing ceramic packages using alumina. Suitable as a material.

Claims (2)

【特許請求の範囲】[Claims] (1)PbO−V_2O_5系ガラス粉末とNaZr_
2(PO_4)_3型固溶体粉末のフィラーとからなる
ことを特徴とする封着材料。
(1) PbO-V_2O_5-based glass powder and NaZr_
2(PO_4)_3 type solid solution powder filler.
(2)PbO−V_2O_5系ガラスが、重量百分率で
PbO20〜55%、V_2O_520〜55%、Te
O_25〜40%、Al_2O_30〜8%の組成を有
することを特徴とする特許請求の範囲第1項記載の封着
材料。
(2) PbO-V_2O_5 glass has a weight percentage of PbO20-55%, V_2O_520-55%, Te
The sealing material according to claim 1, having a composition of O_25 to 40% and Al_2O_30 to 8%.
JP26587390A 1990-10-02 1990-10-02 Sealing material Pending JPH04144937A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP26587390A JPH04144937A (en) 1990-10-02 1990-10-02 Sealing material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP26587390A JPH04144937A (en) 1990-10-02 1990-10-02 Sealing material

Publications (1)

Publication Number Publication Date
JPH04144937A true JPH04144937A (en) 1992-05-19

Family

ID=17423283

Family Applications (1)

Application Number Title Priority Date Filing Date
JP26587390A Pending JPH04144937A (en) 1990-10-02 1990-10-02 Sealing material

Country Status (1)

Country Link
JP (1) JPH04144937A (en)

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