JPH0653597B2 - Glass coating method and glass joining method - Google Patents
Glass coating method and glass joining methodInfo
- Publication number
- JPH0653597B2 JPH0653597B2 JP1454590A JP1454590A JPH0653597B2 JP H0653597 B2 JPH0653597 B2 JP H0653597B2 JP 1454590 A JP1454590 A JP 1454590A JP 1454590 A JP1454590 A JP 1454590A JP H0653597 B2 JPH0653597 B2 JP H0653597B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- sheet
- base material
- adhesive
- soluble
- 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
Links
- 239000011521 glass Substances 0.000 title claims description 59
- 238000000034 method Methods 0.000 title claims description 18
- 238000000576 coating method Methods 0.000 title claims description 16
- 239000000463 material Substances 0.000 claims description 18
- 229920005989 resin Polymers 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 16
- 239000000853 adhesive Substances 0.000 claims description 14
- 230000001070 adhesive effect Effects 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 4
- 238000004898 kneading Methods 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910000833 kovar Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003522 acrylic cement Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Landscapes
- Joining Of Glass To Other Materials (AREA)
- Glass Compositions (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明はガラスの微粉末を含有したシートを用いるガラ
スコーティング方法及びガラス接合方法に関するもので
ある。TECHNICAL FIELD The present invention relates to a glass coating method and a glass bonding method using a sheet containing fine glass powder.
（従来の技術） 金属やセラミックス等からなる基材の表面にガラスコー
ティングを施すためには、ガラス粉末とビヒクルとの混
合物をスクリーン印刷法、転写法、スプレー法等の手段
によって基材の表面に載せ、焼成する方法が一般的であ
る。しかしスクリーン印刷法は基材の形状によっては均
一な印刷ができない場合があり、また設備費が高くつく
という問題がある。転写法は設備費は安価でよいが膜厚
が薄く、精度を出しにくいという問題がある。またスプ
レー法は広い面積に適用できるが膜厚のばらつきが大き
く、精度が悪いという問題がある。(Prior Art) In order to apply glass coating to the surface of a base material made of metal or ceramics, a mixture of glass powder and vehicle is applied to the surface of the base material by means of screen printing, transfer, spraying or the like. The method of placing and firing is common. However, the screen printing method has a problem that uniform printing may not be possible depending on the shape of the base material and the equipment cost is high. The transfer method requires low equipment cost, but has a problem that the film thickness is thin and it is difficult to obtain accuracy. Further, although the spray method can be applied to a wide area, there is a problem in that the variation in film thickness is large and the accuracy is poor.
従って高価な設備を必要とせず、均一な膜厚のガラスコ
ーティングを基材の表面に精度良く施すことができるガ
ラスコーティング方法が求められていた。Therefore, there has been a demand for a glass coating method which does not require expensive equipment and is capable of accurately applying a glass coating having a uniform film thickness to the surface of a substrate.
一方、基材の表面に他の部材をガラス接合する方法とし
ては、上記のスクリーン印刷法のほかにプリフォームと
呼ばれるガラスの薄板を基材の表面に載せて焼成する方
法が知られている。しかしこの方法は膜厚を200 μｍ以
下とすることが困難であり、しかも用途に応じて各種の
サイズのものを成形しなければならないという問題があ
る。On the other hand, as a method of glass-bonding another member to the surface of the base material, in addition to the above-mentioned screen printing method, a method of placing a thin glass plate called a preform on the surface of the base material and firing it is known. However, this method has a problem that it is difficult to reduce the film thickness to less than 200 μm, and moreover various sizes must be molded according to the application.
従って任意の膜厚のガラス層により各種形状の部材を容
易にしかも精度よく基材の表面に接合できるガラス接合
方法が求められていた。Therefore, there has been a demand for a glass bonding method capable of bonding members of various shapes to a surface of a base material easily and accurately with a glass layer having an arbitrary thickness.
（発明が解決しようとする課題） 本発明は上記した従来の要望に応え、高価な設備を必要
とせずに均一な膜厚のガラスコーティングを基材の表面
に精度良く施すことができるガラスコーティング方法
と、このガラスコーティング方法を利用して任意の膜厚
のガラス層により各種形状の部材を容易にガラス接合す
ることができるガラス接合方法とを提供することを目的
とするものである。(Problems to be Solved by the Invention) The present invention meets the above-mentioned conventional demands, and a glass coating method capable of accurately applying a glass coating having a uniform film thickness to the surface of a substrate without requiring expensive equipment. It is an object of the present invention to provide a glass bonding method that can easily glass-bond members of various shapes with a glass layer having an arbitrary thickness by using this glass coating method.
（課題を解決するための手段） 上記の課題は、ガラスの微粉末と樹脂バインダとを混練
したシートを、樹脂バインダが水溶性であるときには有
機溶剤易溶性の接着剤を用い、また樹脂バインダが有機
溶剤易溶性であるときには水溶性の接着剤を用いて基材
の表面に接着し、炉内で焼成して基材の表面にガラス層
を形成することを特徴とするガラスコーティング方法に
よって解決される。また上記の課題は、このようにして
形成されたガラス層を利用して基材の表面に他の部材を
接合することを特徴とするガラス接合方法によって解決
される。(Means for Solving the Problem) The above problem is that a sheet obtained by kneading glass fine powder and a resin binder is used, when the resin binder is water-soluble, an adhesive easily soluble in an organic solvent is used, and the resin binder is When it is easily soluble in an organic solvent, it is solved by a glass coating method characterized by adhering to the surface of a substrate with a water-soluble adhesive and baking it in a furnace to form a glass layer on the surface of the substrate. It Further, the above problem can be solved by a glass bonding method, which is characterized in that another member is bonded to the surface of a base material by utilizing the glass layer thus formed.
このように本発明においてはガラスの微粉末と樹脂バイ
ンダとを混練したシートが用いられる。ガラスの微粉末
としては従来からガラス接合用等に用いられてきた低融
点ガラス、ほうろう用フリット等が目的に応じて使用さ
れ、目的によっては結晶化ガラスの微粉末を用いること
もできる。As described above, in the present invention, a sheet obtained by kneading fine glass powder and a resin binder is used. As the fine glass powder, low melting point glass, frit for enamel, etc., which have been conventionally used for joining glass, etc. are used according to the purpose, and fine powder of crystallized glass may be used depending on the purpose.
樹脂バインダは全体をシート化するためのもので、ポリ
ビニルアルコール、カルボキシメチルセルロース、メチ
ルセルロースのような水溶性樹脂や、ポリビニルブチラ
ール、スチレン系樹脂エマルジョン、アクリル系樹脂エ
マルジョン、ブタジエン系樹脂エマルジョンのような有
機溶剤易溶性樹脂が使用される。このほかにフタル酸ジ
ブチルやジエチレングリコールのような可塑剤を少量添
加してもよい。The resin binder is for making the whole into a sheet, and it is a water-soluble resin such as polyvinyl alcohol, carboxymethyl cellulose, or methyl cellulose, or an organic solvent such as polyvinyl butyral, a styrene resin emulsion, an acrylic resin emulsion, or a butadiene resin emulsion. A readily soluble resin is used. In addition to this, a small amount of a plasticizer such as dibutyl phthalate or diethylene glycol may be added.
シート中におけるガラス微粉末の混合比は20〜90重量％
が適当である。こればガラスの混合比が20％未満では均
一なガラスコーティングや十分な接合強度が得られず、
逆に90％を越えると相対的に樹脂バインダが不足してシ
ート化が困難となるためである。またシート全体の厚さ
は50〜400 μｍ程度が好ましい。The mixing ratio of fine glass powder in the sheet is 20 to 90% by weight.
Is appropriate. If the mixing ratio of glass is less than 20%, uniform glass coating and sufficient bonding strength cannot be obtained.
On the other hand, if it exceeds 90%, the resin binder is relatively insufficient and it becomes difficult to form a sheet. The thickness of the entire sheet is preferably about 50 to 400 μm.
第１の発明においては、このようなシートを目的とする
ガラスコーティング面積に合わせて切断したうえで、基
材の表面に接着して焼成が行われる。また第２の発明に
おいてもシートを目的とするガラス接合面積に合わせて
切断し、基材とこれに接合される他の部材との間に接着
して焼成される。このための接着剤としてはシート中の
樹脂バインダが水溶性のものである場合には有機溶剤易
溶性の接着剤を用い、シート中の樹脂バインダが有機溶
剤易溶性のものである場合には水溶性の接着剤を用いる
ものとする。これは接着剤によってシートが溶かされる
ことを防止するためである。In the first invention, such a sheet is cut according to the intended glass coating area and then adhered to the surface of the base material and fired. Also in the second aspect of the invention, the sheet is cut according to the intended glass bonding area, and is bonded and baked between the base material and the other member bonded to the base material. As the adhesive for this, an organic solvent easily soluble adhesive is used when the resin binder in the sheet is water-soluble, and a water-soluble adhesive is used when the resin binder in the sheet is easily soluble in the organic solvent. Use a transparent adhesive. This is to prevent the sheet from being melted by the adhesive.
また本発明においては、シートの全面を基材に接着する
のではなく数個所を点状または網目状に接着することが
好ましい。これはシートと基材との間に隙間を設けるこ
とにより、焼成時に接着剤が熱分解して発生するガスを
シートの下面から逃がすためであり、全面接着した場合
にはガスがシートの内部において発泡して均一なガラス
コーティング層やガラス接合層を形成しないおそれがあ
る。また全く接着しなければシートはごく薄いものであ
るために基材上から移動してしまうこととなる。In addition, in the present invention, it is preferable that the entire surface of the sheet is not adhered to the base material but that several parts are adhered in a dot shape or a mesh shape. This is because by providing a gap between the sheet and the base material, the gas generated by the thermal decomposition of the adhesive during firing escapes from the lower surface of the sheet. There is a risk of foaming and not forming a uniform glass coating layer or glass bonding layer. If the sheet is not adhered at all, the sheet is very thin and will move from the base material.
このようにシートを基材の表面に点状または網目状に接
着したものを焼成すれば、樹脂バインダが熱分解して飛
散するとともにシート中のガラスの微粉末が溶融して基
材の表面に均一な膜厚のガラスコーティング層が形成さ
れる。また第２の発明によれば、このシートが溶融して
生じたガラス層を利用して基材の表面に他の部材を気密
にガラス接合することができる。When the sheet is adhered to the surface of the base material in a dot-like or mesh-like manner, the resin binder is thermally decomposed and scattered, and the fine glass powder in the sheet is melted to form the surface of the base material. A glass coating layer having a uniform film thickness is formed. According to the second aspect of the invention, the glass layer formed by melting the sheet can be used to hermetically bond other members to the surface of the base material by glass.
本発明に用いられるシートはその膜厚を従来のプリフォ
ームよりも極めて薄く、かつ均一に製造することができ
るので、基材の表面に均一な膜厚のガラスコーティング
を施すことができる。またこのシートは自由な寸法に切
断して用いることができるので、任意の形状の基材の表
面に精度の良いガラスコーティングを施すことができ
る。しかも本発明によれば接着剤によってシートが溶か
されるおそれがなく、また接着剤の熱分解により生じた
ガスがガラスコーティング面やガラス接合面を発泡させ
ることもない。Since the sheet used in the present invention has a film thickness extremely smaller than that of a conventional preform and can be manufactured uniformly, a glass coating having a uniform film thickness can be applied to the surface of the substrate. Further, since this sheet can be cut to a desired size and used, the surface of a base material having an arbitrary shape can be coated with a highly accurate glass coating. Moreover, according to the present invention, there is no fear that the sheet will be melted by the adhesive, and the gas generated by the thermal decomposition of the adhesive does not foam the glass coating surface or the glass bonding surface.
次に本発明の実施例を示す。Next, examples of the present invention will be described.
（実施例） 実施例１ SiO2 67.0％（重量％、以下同じ）、B2O3 22.0 ％、Na2
O 3.5 ％、K2O 4.0％、CaO 1.5 ％、の組成を持ち、
40〜400 ℃における線膨張係数が4.7 ×10-6／℃である
ガラスを325 メッシュ以下に粉砕しガラス粉末を製造し
た。このガラス粉末72部と有機溶剤易溶性樹脂であるポ
リビニルブチラール27部と可塑剤であるフタル酸ジブチ
ル１部とを混練し、膜厚が100 μｍと300 μｍの２種類
のシートを作成した。これらのシートを30mm×30mmの寸
法に切断したうえ、30mm×30mm×0.8 mmt のアルミナ製
の基材の表面にそれぞれ４点接着した。使用した接着材
は水溶性のアクリル系接着剤である。これらの基材をN2
ガス雰囲気中で1000℃×15分間焼成したところ、基材の
表面に膜厚が70μｍと200 μｍの均一なガラスコーティ
ング層が形成された。Example 1 Example 1 SiO 2 67.0% (wt%, the same applies hereinafter), B 2 O 3 22.0%, Na 2
With the composition of O 3.5%, K 2 O 4.0%, CaO 1.5%,
Glass having a coefficient of linear expansion of 4.7 × 10 −6 / ° C. at 40 to 400 ° C. was pulverized to 325 mesh or less to produce glass powder. 72 parts of this glass powder, 27 parts of polyvinyl butyral, which is a resin easily soluble in organic solvents, and 1 part of dibutyl phthalate, which is a plasticizer, were kneaded to prepare two types of sheets having film thicknesses of 100 μm and 300 μm. These sheets were cut into a size of 30 mm × 30 mm, and four points were adhered to each surface of a 30 mm × 30 mm × 0.8 mm t alumina substrate. The adhesive used is a water-soluble acrylic adhesive. N 2
When baked at 1000 ° C. for 15 minutes in a gas atmosphere, a uniform glass coating layer having a film thickness of 70 μm and 200 μm was formed on the surface of the substrate.
実施例２ 実施例１に記した膜厚の異なる２種類のシートを用い
て、第１図に示されるとおりの圧力センサのガラス封着
を行った。図中、(1)は40〜400 ℃における線膨張係数
が3.3 ×10-6／℃のシリコンチップ、(2)は40〜400 ℃
における線膨張係数が2.9 ×10-6／℃の結晶化ガラス製
の基台、(3)は40〜400 ℃における線膨張係数が4.9 ×1
0-6／℃のコバール合金（29％Ni−17％Co−54％Fe）か
らなるステム台座、(4)は同じコバール合金製のピンで
ある。Example 2 Using two types of sheets having different film thicknesses described in Example 1, a pressure sensor as shown in FIG. 1 was glass-sealed. In the figure, (1) is a silicon chip with a linear expansion coefficient of 3.3 × 10 -6 / ° C at 40 to 400 ℃, (2) is 40 to 400 ℃.
Base made of crystallized glass with a linear expansion coefficient of 2.9 × 10 -6 / ℃, (3) has a linear expansion coefficient of 4.9 × 1 at 40 to 400 ℃
A stem pedestal made of Kovar alloy (29% Ni-17% Co-54% Fe) of 0 -6 / ° C. (4) is a pin made of the same Kovar alloy.
ステム台座(3)と基台(2)との間のガラス接合は、両者間
の線膨張係数の差が大きいので膜厚が100 μｍのシート
(5)を外径3.0 mm、内径0.6 mmに打ち抜いたものを用
い、ステム台座(3)とピン(4)との間のガラス接合はガラ
ス体積を多くするため膜厚が300 μｍのシート(6)を用
いて行った。接着剤及び加熱条件は実施例１と同様であ
る。この結果、各部材は精度良く気密シールされ、プリ
フォームを使用していた従来のガラス接合方法に比較し
て接合強度約20％向上した。The glass joint between the stem pedestal (3) and the base (2) has a large difference in linear expansion coefficient between them, so a sheet with a film thickness of 100 μm
Using (5) punched out with an outer diameter of 3.0 mm and an inner diameter of 0.6 mm, the glass bonding between the stem pedestal (3) and the pin (4) increases the glass volume, so a sheet with a thickness of 300 μm ( 6). The adhesive and heating conditions are the same as in Example 1. As a result, each member was hermetically sealed with high accuracy, and the bonding strength was improved by about 20% as compared with the conventional glass bonding method using the preform.
（発明の効果） 以上に説明したとおり、第１の発明によれば特別の設備
を必要とせずに均一な膜厚のガラスコーティング層を基
材の表面に精度良くかつ容易に施すことができる。また
第２の発明によれば各種形状の部材を精度良くかつ容易
にガラス接合することができる。(Effects of the Invention) As described above, according to the first invention, a glass coating layer having a uniform film thickness can be accurately and easily applied to the surface of a substrate without requiring special equipment. Further, according to the second aspect of the present invention, members of various shapes can be glass-bonded accurately and easily.
よって本発明は従来の問題点を一掃したガラスコーティ
ング方法及びガラス接合方法として、産業の発展に寄与
するところは極めて大である。Therefore, the present invention, as a glass coating method and a glass joining method that eliminates the conventional problems, has a great contribution to the industrial development.
第１図は実施例２の方法により接合された圧力センサを
示す断面図である。 (5)、(6)：シート。FIG. 1 is a sectional view showing a pressure sensor joined by the method of the second embodiment. (5), (6): Sheet.
Claims (2)
たシートを、樹脂バインダが水溶性であるときには有機
溶剤易溶性の接着剤を用い、また樹脂バインダが有機溶
剤易溶性であるときには水溶性の接着剤を用いて基材の
表面に接着し、炉内で焼成して基材の表面にガラス層を
形成することを特徴とするガラスコーティング方法。1. A sheet obtained by kneading fine glass powder and a resin binder is used with an adhesive which is easily soluble in an organic solvent when the resin binder is water-soluble, and is water-soluble when the resin binder is easily soluble in an organic solvent. A glass coating method, which comprises using the adhesive of claim 1 to adhere to the surface of a substrate and firing in a furnace to form a glass layer on the surface of the substrate.
ラス層を利用して基材の表面に他の部材を接合すること
を特徴とするガラス接合方法。2. A glass bonding method, wherein another member is bonded to the surface of a base material by using the glass layer formed by the method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1454590A JPH0653597B2 (en) | 1990-01-23 | 1990-01-23 | Glass coating method and glass joining method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1454590A JPH0653597B2 (en) | 1990-01-23 | 1990-01-23 | Glass coating method and glass joining method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03218951A JPH03218951A (en) | 1991-09-26 |
| JPH0653597B2 true JPH0653597B2 (en) | 1994-07-20 |
Family
ID=11864127
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1454590A Expired - Lifetime JPH0653597B2 (en) | 1990-01-23 | 1990-01-23 | Glass coating method and glass joining method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0653597B2 (en) |
-
1990
- 1990-01-23 JP JP1454590A patent/JPH0653597B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03218951A (en) | 1991-09-26 |
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