JPH06263478A - Lead-free low melting point glass - Google Patents
Lead-free low melting point glassInfo
- Publication number
- JPH06263478A JPH06263478A JP6765393A JP6765393A JPH06263478A JP H06263478 A JPH06263478 A JP H06263478A JP 6765393 A JP6765393 A JP 6765393A JP 6765393 A JP6765393 A JP 6765393A JP H06263478 A JPH06263478 A JP H06263478A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- lead
- low melting
- melting point
- sealing
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/122—Silica-free oxide glass compositions containing oxides of As, Sb, Bi, Mo, W, V, Te as glass formers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、電子部品の封止、特
に、蛍光表示管及び半導体パッケージの封着に好適な無
鉛系低融点ガラス、封着用ガラス組成物に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a lead-free low melting point glass and a glass composition for sealing, which are suitable for sealing electronic parts, particularly for sealing fluorescent display tubes and semiconductor packages.
【0002】[0002]
【従来の技術】電子部品の封止、特に、蛍光表示管及び
半導体パッケージの封着をする場合、内部部品への熱の
影響を低減するために、できるだけ低温で封着すること
が必要とされ、一般に500℃以下で封着できる低融点
ガラスが使用されている。現在、これらに使用される低
融点ガラスとして、PbO−B2 O3 、PbO−B2 O
3 −ZnO、PbO−B2 O3 −SiO2 、PbO−B
2 O3 −SiO2 −BaOなどを基本とした鉛を含有す
るガラス粉末に耐火物フィラー粉末を混合させ、被封着
材料の熱膨張係数とほぼ同等となるような、封着材料が
用いられている。これら鉛系低融点ガラスは、鉛の毒性
から環境上問題がある。2. Description of the Related Art In the case of sealing electronic parts, particularly fluorescent display tubes and semiconductor packages, it is necessary to seal them at the lowest possible temperature in order to reduce the influence of heat on internal parts. Generally, a low melting point glass that can be sealed at 500 ° C. or lower is used. Currently, as the low melting point glass used for these, PbO-B 2 O 3, PbO-B 2 O
3 -ZnO, PbO-B 2 O 3 -SiO 2, PbO-B
A sealing material is used, which is a mixture of lead-containing glass powder based on 2 O 3 —SiO 2 —BaO and the like with refractory filler powder and has a thermal expansion coefficient substantially equal to that of the material to be sealed. ing. These lead-based low-melting-point glasses have environmental problems due to the toxicity of lead.
【0003】また、鉛系低融点ガラスは、一般にPbO
の量が多いほど低融点となる。被封着材料の熱影響を低
減するためガラスの封着温度はできるだけ低い方が望ま
しく、ガラス中により多量のPbOが必要となる。この
ため化学的耐久性が悪い、金属鉛が析出するなどの問題
がある。これらの問題を解決すべく、無鉛系低融点ガラ
スの研究、開発が進められている。Lead-based low melting glass is generally PbO.
The higher the amount, the lower the melting point. In order to reduce the heat effect of the material to be sealed, it is desirable that the sealing temperature of the glass is as low as possible, and a larger amount of PbO is required in the glass. Therefore, there are problems such as poor chemical durability and precipitation of metallic lead. In order to solve these problems, research and development of lead-free low melting point glass have been advanced.
【0004】例えば、Na2 O−B2 O3 系等のホウ酸
塩、Na2 O−B2 O3 ーP2 O5系等のリン酸塩、L
i2 O−GeO2 系等のゲルマン酸塩、Ta2 O5 −B
2 O3 系等のタリウム酸塩、Na2 O−MoO3 系等の
モリブデン酸塩、V2 O5 −GeO2 −P2 O5 系等の
バナジン酸塩、テルル酸塩、フッ化物、フツリン酸、カ
ルコゲナイド、オキシカルコゲナイド等の低融点ガラス
が提案されている。For example, Na 2 O--B 2 O 3 type borate, Na 2 O--B 2 O 3 --P 2 O 5 type phosphate, L
i 2 germanate salt of O-GeO 2 system, and the like, Ta 2 O 5 -B
2 O 3 -based thallates, Na 2 O—MoO 3 -based molybdates, V 2 O 5 —GeO 2 —P 2 O 5 -based vanadates, tellurates, fluorides, and fluorine Low melting glass such as acid, chalcogenide, oxychalcogenide, etc. has been proposed.
【0005】[0005]
【発明が解決しようとする課題】しかし、これら無鉛系
低融点ガラスは、絶縁性、誘電率等の電気的特性、耐水
性、耐酸性等の化学的安定性、ガラスの流動性等の封着
特性、毒性等の問題があり、鉛系低融点ガラスの代りに
使用するに至っていない。本発明は上記課題に鑑みてな
されたもので、電子部品の封止、特に、蛍光表示管及び
半導体パッケージの封着に好適な無鉛系低融点ガラス、
封着用組成物の提供を目的とする。However, these lead-free low-melting-point glasses are sealed with electrical properties such as insulation and dielectric constant, chemical stability such as water resistance and acid resistance, and fluidity of glass. Due to problems with properties and toxicity, it has not been used in place of lead-based low melting point glass. The present invention has been made in view of the above problems, and is a lead-free low-melting glass suitable for sealing electronic components, particularly, sealing fluorescent display tubes and semiconductor packages,
The purpose is to provide a composition for sealing.
【0006】[0006]
【課題を解決するための手段】上記目的を達成するた
め、本発明の無鉛系低融点ガラスは、重量%で V2 O5 20〜45% TeO2 3〜25% MoO 3〜30% B2 O3 1〜13% ZnO 3〜25% BaO 0〜30% TiO2 0〜 5% Al2 O3 0〜 5% Nb2 O5 0〜 7% Ta2 O5 0〜10% の組成からなること、また上記組成のガラス粉末に耐火
物フィラー粉末を10〜50容量%含有させたことを特
徴とする。In order to achieve the above object, the lead-free low melting point glass of the present invention is V 2 O 5 20 to 45% TeO 2 3 to 25% MoO 3 to 30% B 2 in % by weight. O 3 1 to 13% ZnO 3 to 25% BaO 0 to 30% TiO 2 0 to 5% Al 2 O 3 0 to 5% Nb 2 O 5 0 to 7% Ta 2 O 5 0 to 10% The refractory filler powder is contained in the glass powder having the above composition in an amount of 10 to 50% by volume.
【0007】以下、本発明について好ましい態様を挙げ
て詳細に説明する。本発明において組成が前記のように
限定された理由について説明する。V2 O5 は、ガラス
の転移点、軟化点を下げ、また熱膨張係数を小さくする
が、45%(重量%、特記ないかぎり以下同じ。)超で
は再過熱によって失透し流動性が悪化する。またガラス
の絶縁性が低くなる。20%未満では転移点及び軟化点
を下げる効果がほとんどない。The present invention will be described in detail below with reference to preferred embodiments. The reason why the composition is limited as described above in the present invention will be described. V 2 O 5 lowers the glass transition point and softening point, and also lowers the thermal expansion coefficient, but if it exceeds 45% (weight%, the same applies hereafter unless otherwise specified), it devitrifies due to reheating and the fluidity deteriorates. To do. Moreover, the insulating property of glass becomes low. If it is less than 20%, there is almost no effect of lowering the transition point and the softening point.
【0008】TeO2 は、軟化点を低下させ流動性を向
上させるが、25%超ではガラスの安定性が悪くなり、
熱膨張係数が著しく大きくなり、また誘電率が大きくな
る。3%未満ではガラスの転移点及び軟化点を下げる効
果がほとんどない。TeO 2 lowers the softening point and improves the fluidity, but if it exceeds 25%, the stability of the glass deteriorates.
The coefficient of thermal expansion is significantly increased, and the dielectric constant is also increased. If it is less than 3%, there is almost no effect of lowering the glass transition point and softening point.
【0009】MoO3 は、転移点を低下させるが20%
超では再過熱によって失透し流動性が悪化する。3%未
満ではガラスの転移点及び軟化点を下げる効果がほとん
どない。MoO 3 lowers the transition point, but 20%
If it is over, devitrification occurs due to reheating and fluidity deteriorates. If it is less than 3%, there is almost no effect of lowering the glass transition point and softening point.
【0010】B2 O3 は、ガラスを安定化させるが、1
3%超では軟化点が高くなり、ガラスの粘性が大きくな
る。13%未満ではガラスの結晶化傾向が大きくなり、
ガラスが流動しなくなる。B 2 O 3 stabilizes the glass, but 1
If it exceeds 3%, the softening point becomes high and the viscosity of the glass becomes large. If it is less than 13%, the glass tends to crystallize,
The glass will not flow.
【0011】ZnOは、化学的耐久性を向上させ、熱膨
張係数を小さくするが、25%超では軟化点が著しく高
くなる。3%未満ではガラスの結晶化傾向が大きくな
り、ガラスが流動しなくなる。ZnO improves chemical durability and reduces the coefficient of thermal expansion, but if it exceeds 25%, the softening point becomes extremely high. If it is less than 3%, the glass tends to crystallize and the glass does not flow.
【0012】BaOは、ガラスを安定化させるが、30
%超では軟化点が高くなり、ガラスが流動しなくなる。BaO stabilizes the glass, but
If it exceeds%, the softening point becomes high and the glass does not flow.
【0013】TiO2 は、5%超ではガラスの結晶化傾
向が大きくなり、ガラスが流動しなくなる。If TiO 2 exceeds 5%, the glass tends to crystallize and the glass does not flow.
【0014】Al2 O3 は、化学的耐久性を向上させ、
熱膨張係数を小さくするが、5%超ではガラスの結晶化
傾向が大きくなり、ガラスが流動しなくなる。Al 2 O 3 improves the chemical durability,
Although the coefficient of thermal expansion is reduced, if it exceeds 5%, the tendency of the glass to crystallize increases and the glass does not flow.
【0015】Nb2 O5 は、ガラスを安定化させるが、
7%超では軟化点が高くなり、ガラスが流動しなくな
る。Nb 2 O 5 stabilizes the glass,
If it exceeds 7%, the softening point becomes high and the glass does not flow.
【0016】Ta2 O5 は、ガラスを安定化させるが、
10%超では軟化点が高くなり、ガラスが流動しなくな
る。Ta 2 O 5 stabilizes the glass,
If it exceeds 10%, the softening point becomes high and the glass does not flow.
【0017】本発明において、上記組成は、V2 O5 2
0〜45%、TeO2 3〜25%、MoO3 3〜30
%、B2 O3 1〜13%、ZnO 3〜25%、BaO
0〜30%、TiO2 0〜5%、Al2 O3 0〜5
%、Nb2 O5 0〜7%、Ta2O5 0〜10%が好ま
しく、この組成範囲にあるガラスは、作業温度範囲が、
400〜500℃と従来の鉛系低融点ガラスと同等の温
度特性を持っている。また、 絶縁性、 誘電率等の電気特
性も同等であり、 しかもPbOを含んでいないため化学
的安定性が著しくよい。In the present invention, the above composition is V 2 O 5 2
0-45%, TeO 2 3-25%, MoO 3 3-30
%, B 2 O 3 1 to 13%, ZnO 3 to 25%, BaO
0-30%, TiO 2 0-5%, Al 2 O 3 0-5
%, Nb 2 O 5 0~7% , Ta 2 O 5 0~10% is preferred, glass in this composition range, the working temperature range,
It has a temperature characteristic of 400 to 500 ° C., which is equivalent to that of conventional lead-based low melting point glass. Also, the electrical properties such as insulation and dielectric constant are the same, and since PbO is not contained, the chemical stability is remarkably good.
【0018】本発明の無鉛系低融点ガラスは、従来から
の低融点ガラスと同じ方法で製造できる。すなわち、V
2 O5 、TeO2 、MoO3 、B2 O3 、ZnO、Ba
O、TiO2 、Al2 O3 、Nb2 O5 、Ta2 O5 を
与える原料を上記割合を満足するように配合し、加熱し
て溶融した後、金型に流しこみガラスブロックを製造す
る。粉末とする場合は、例えば、ボールミル等を用いて
粉砕する。The lead-free low melting point glass of the present invention can be manufactured by the same method as the conventional low melting point glass. That is, V
2 O 5 , TeO 2 , MoO 3 , B 2 O 3 , ZnO, Ba
Raw materials that give O, TiO 2 , Al 2 O 3 , Nb 2 O 5 , and Ta 2 O 5 are blended so as to satisfy the above ratio, heated and melted, and then cast into a mold to produce a glass block. . When it is made into a powder, for example, it is pulverized by using a ball mill or the like.
【0019】本発明に用いる耐火物フィラー粉末には、
例えばコージェライト、β−ユークリプタイト、β−ス
ポジューメン、ケイ酸亜鉛から選ばれた一種又は二種以
上の粉末を用いるのが好ましく、その粒径は1〜10μ
m程度が好ましく、その配合量は、ガラス粉末と耐火物
フィラーとの合計に対して10〜50容量%であること
が好ましい。The refractory filler powder used in the present invention includes:
For example, it is preferable to use one or more kinds of powder selected from cordierite, β-eucryptite, β-spodumene and zinc silicate, and the particle size thereof is 1 to 10 μm.
m is preferable, and the blending amount thereof is preferably 10 to 50% by volume based on the total amount of the glass powder and the refractory filler.
【0020】耐火物フィラー粉末を低融点ガラス粉末に
混合するのは、その熱膨張係数を被封着物のそれと同じ
くするためと、強度を向上させるためであるが、10容
量%未満ではその効果があらわれず、50容量%超で
は、ガラスの流動性が著しく悪くなり、被封着物を気密
的に封着できなくなる。耐火物フィラーの製造法は、特
に限定されないが、例えば、各組成を与える原料を所定
の割合で混合し、焼成、粉砕して製造される。The refractory filler powder is mixed with the low melting point glass powder in order to make its coefficient of thermal expansion the same as that of the material to be sealed and to improve the strength. If it does not appear and exceeds 50% by volume, the fluidity of the glass is significantly deteriorated and the adherend cannot be hermetically sealed. The method for producing the refractory filler is not particularly limited, but, for example, it is produced by mixing raw materials giving each composition in a predetermined ratio, firing and pulverizing.
【0021】ガラス粉末と、耐火物フィラー粉末との混
合方法は、どのような方法によってもよく、例えば、ガ
ラスブロックをボールミルで粉砕する際に、耐火物フィ
ラーを加えて、粉砕、混合を同時に行ってもよく、それ
ぞれを所定の大きさの粉末とした後、混合してもよい。Any method may be used for mixing the glass powder and the refractory filler powder. For example, when the glass block is crushed by a ball mill, the refractory filler is added, and the crushing and mixing are performed at the same time. Alternatively, each may be mixed into a powder having a predetermined size.
【0022】このようにして製造された本発明の無鉛系
低融点ガラス、封着用ガラス組成物は、従来のものと同
様な方法により、電子部品の封着に用いることができ
る。例えば、半導体のパッケージの封着をする場合、封
着用ガラス組成物と有機バインダーとを混合した後、半
導体のパッケージの封着すべき部分に付着させ、加熱し
て、封着用ガラス組成物を溶融させるとともに、有機バ
インダーを飛散させることにより、パッケージを封着す
る。The lead-free low melting point glass and glass composition for sealing of the present invention thus produced can be used for sealing electronic parts by a method similar to the conventional one. For example, in the case of sealing a semiconductor package, after mixing the glass composition for sealing and an organic binder, it is attached to a portion of the semiconductor package to be sealed and heated to melt the glass composition for sealing. At the same time, the package is sealed by scattering the organic binder.
【0023】[0023]
【実施例】V2 O5 、TeO2 、MoO3 、B2 O3 、
ZnO、BaO、TiO2 、Al2 O3 、Nb2 O5 、
Ta2 O5 を表1に示す重量割合で配合し、白金ルツボ
に入れ、1000〜1200℃の電気炉中で1時間加熱
して溶融させた後、急冷して板状に成形し、板状のガラ
スブロックを得た。ついで、このガラスブロックをボ−
ルミルにて粉砕してガラス粉末を得た(実施例1〜5、
比較例1〜2)。これらのガラスについて特性を測定し
た結果を表1に示す。EXAMPLES V 2 O 5 , TeO 2 , MoO 3 , B 2 O 3 ,
ZnO, BaO, TiO 2 , Al 2 O 3 , Nb 2 O 5 ,
Ta 2 O 5 was blended in a weight ratio shown in Table 1, put in a platinum crucible, heated in an electric furnace at 1000 to 1200 ° C. for 1 hour to be melted, and then rapidly cooled to be formed into a plate shape. I got a glass block. Then, this glass block
Glass powder was obtained by crushing with a rumill (Examples 1 to 5,
Comparative Examples 1-2). The results of measuring the properties of these glasses are shown in Table 1.
【0024】得られたガラス粉末に、表2に示す耐火物
フィラ−粉末を、表2に示す容量割合で混合し、封着用
ガラス組成物を得た(実施例6〜8、比較例3)。これ
らについて特性を測定した結果を表2に示す。The glass powder obtained was mixed with the refractory filler powder shown in Table 2 in a volume ratio shown in Table 2 to obtain glass compositions for sealing (Examples 6 to 8 and Comparative Example 3). . The results of measuring the characteristics of these are shown in Table 2.
【0025】表1、表2に示した特性の測定方法は、以
下の通りである。 1)ガラス転移点、軟化点:ガラスを粉末とし、示差熱
分析装置を用いて、昇温速度10℃/分でそれぞれの温
度を測定。 2)熱膨張係数:ガラスを5mmφ×20mmに加工し
て、示差膨張計により昇温速度10℃/分で、30℃〜
250℃までの平均熱膨張係数を測定。The methods for measuring the characteristics shown in Tables 1 and 2 are as follows. 1) Glass transition point, softening point: Glass was used as powder and each temperature was measured at a temperature rising rate of 10 ° C./min using a differential thermal analyzer. 2) Coefficient of thermal expansion: Glass is processed into 5 mmφ × 20 mm, and the temperature is raised by a differential expansion meter at a temperature rising rate of 10 ° C./min from 30 ° C.
Measure the average coefficient of thermal expansion up to 250 ° C.
【0026】3)体積抵抗:ガラスを50mm×50m
m×3mmに加工して、金を蒸着し電極を形成した後、
絶縁計で室温90Vの条件で測定。 4)誘電率:ガラスを50mm×50mm×3mmに加
工して、金を蒸着し電極を形成した後、ブリッジ法で室
温、1MHzの条件で測定。3) Volume resistance: 50 mm × 50 m of glass
After processing into m × 3 mm and depositing gold to form electrodes,
Measured at room temperature 90V with an insulation meter. 4) Dielectric constant: Measured under the conditions of room temperature and 1 MHz by the bridge method after processing glass into 50 mm × 50 mm × 3 mm and depositing gold to form electrodes.
【0027】5)耐水性:ガラスを10mm×10mm
×10mmに加工して、95℃の蒸留水に1時間放置
し、重量減を測定。 6)流動性:各粉末試料を、その比重に相当する重量を
採取し、12.5mmφの円柱状に加圧成形した後、板
ガラス上にのせ430℃で10分間熱処理した後、その
直径を測定。18mm以上であれば良好と判定。5) Water resistance: Glass 10 mm × 10 mm
It was processed into × 10 mm and left in distilled water at 95 ° C for 1 hour, and the weight loss was measured. 6) Flowability: Each powder sample was sampled in a weight corresponding to its specific gravity, pressure-molded into a column of 12.5 mmφ, heat-treated at 430 ° C. for 10 minutes on a plate glass, and then its diameter was measured. . 18 mm or more is judged to be good.
【0028】[0028]
【表1】 [Table 1]
【0029】[0029]
【表2】 [Table 2]
【0030】表1より、本発明の低融点ガラスは、比較
例1の鉛系低融点ガラスとほぼ同じ熱特性、電気特性を
持ち、さらに耐水性が著しくよいことがわかる。また公
知の無鉛系低融点ガラスである比較例2と比較しても電
気的特性、耐水性が著しくよいことがわかる。表2よ
り、耐火物フィラ−を含有させた封着用組成物は、従来
の鉛系封着用組成物と同等の特性が得られることがわか
る。It can be seen from Table 1 that the low melting point glass of the present invention has almost the same thermal characteristics and electrical characteristics as the lead-based low melting point glass of Comparative Example 1 and has significantly excellent water resistance. It is also found that the electrical characteristics and water resistance are remarkably excellent even when compared with the known lead-free low melting point glass, Comparative Example 2. From Table 2, it can be seen that the sealing composition containing the refractory filler has characteristics equivalent to those of the conventional lead-based sealing composition.
【0031】[0031]
【発明の効果】本発明の無鉛系低融点ガラス、封着用ガ
ラス組成物は、作業温度範囲が400〜500℃と従来
の鉛系低融点ガラスと同等であり、鉛を含んでいないた
め、毒性等の環境上問題がなく、化学的安定性もよい。
したがって、本発明の無鉛系低融点ガラス、封着用ガラ
ス組成物は、電子部品の封止、特に、蛍光表示管及び半
導体パッケージの封着に好適である。The lead-free low-melting glass and glass composition for sealing of the present invention has a working temperature range of 400 to 500 ° C., which is equivalent to that of conventional low-melting glass of lead and does not contain lead. It has no environmental problems such as the above, and has good chemical stability.
Therefore, the lead-free low melting point glass and glass composition for sealing of the present invention are suitable for sealing electronic parts, particularly for sealing fluorescent display tubes and semiconductor packages.
Claims (2)
ィラー粉末を10〜50容量%含有させたことを特徴と
する封着用ガラス組成物。2. A glass composition for sealing, characterized in that the powder of the low melting point glass according to claim 1 contains 10 to 50% by volume of a refractory filler powder.
Priority Applications (1)
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JP06765393A JP3339647B2 (en) | 1993-03-03 | 1993-03-03 | Lead-free low melting glass and sealing glass composition |
Applications Claiming Priority (1)
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---|---|---|---|
JP06765393A JP3339647B2 (en) | 1993-03-03 | 1993-03-03 | Lead-free low melting glass and sealing glass composition |
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JPH06263478A true JPH06263478A (en) | 1994-09-20 |
JP3339647B2 JP3339647B2 (en) | 2002-10-28 |
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JP06765393A Expired - Fee Related JP3339647B2 (en) | 1993-03-03 | 1993-03-03 | Lead-free low melting glass and sealing glass composition |
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