JPH08296036A - Material for vapor deposition and method for producing molded body thereof - Google Patents
Material for vapor deposition and method for producing molded body thereofInfo
- Publication number
- JPH08296036A JPH08296036A JP10277195A JP10277195A JPH08296036A JP H08296036 A JPH08296036 A JP H08296036A JP 10277195 A JP10277195 A JP 10277195A JP 10277195 A JP10277195 A JP 10277195A JP H08296036 A JPH08296036 A JP H08296036A
- Authority
- JP
- Japan
- Prior art keywords
- sio
- vapor deposition
- mol
- mgo
- transparency
- 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
Landscapes
- Silicon Compounds (AREA)
- Physical Vapour Deposition (AREA)
Abstract
(57)【要約】
【目的】透明性と密着性という相反する特性を兼ね備え
た蒸着膜を形成することができる蒸着用材料およびその
成形体の製造方法を提供する。
【構成】(1) mol%で、一酸化ケイ素( SiO):20〜
90、二酸化ケイ素(SiO2):10〜80から構成される原料
に、酸化マグネシウム( MgO)、酸化ジルコニウム(Zr
02) 、酸化チタニウム(TiO2) および酸化アルミニウム
(Al2O3)のうち1種以上が混合されていることを特徴と
する蒸着用材料。
(2) mol%で、一酸化ケイ素( SiO):20〜90、二酸
化ケイ素(SiO2):10〜80から原料を構成し、さらに酸
化マグネシウム( MgO)、酸化ジルコニウム(Zr02) 、
酸化チタニウム(TiO2) および酸化アルミニウム(Al2O
3)のうち1種以上を混合し、成形ののち 100〜1500℃で
熱処理することを特徴とする蒸着用材料の成形体の製造
方法。(57) [Summary] [Object] To provide a vapor deposition material capable of forming a vapor deposition film having contradictory properties of transparency and adhesion and a method for producing a molded body thereof. [Constitution] (1) mol% silicon monoxide (SiO): 20-
90, silicon dioxide (SiO 2 ): 10 to 80 as raw material, magnesium oxide (MgO), zirconium oxide (Zr
0 2 ), titanium oxide (TiO 2 ), and aluminum oxide (Al 2 O 3 ). (2) In mol%, the raw material is composed of silicon monoxide (SiO): 20 to 90, silicon dioxide (SiO 2 ): 10 to 80, and further, magnesium oxide (MgO), zirconium oxide (Zr0 2 ),
Titanium oxide (TiO 2 ) and aluminum oxide (Al 2 O
3 ) A method for producing a molded body of a vapor deposition material, which comprises mixing at least one of the above, molding, and then heat-treating at 100 to 1500 ° C.
Description
【0001】[0001]
【産業上の利用分野】本発明は、食品包装材料の表面に
形成され、透明性と密着性に優れる酸化ケイ素系薄膜の
蒸着に用いられる蒸着用材料とその成形体の製造方法に
関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vapor deposition material used for vapor deposition of a silicon oxide thin film which is formed on the surface of a food packaging material and is excellent in transparency and adhesion, and a method for producing a molded product thereof. .
【0002】[0002]
【従来の技術】従来から、一酸化ケイ素( SiO)、二酸
化ケイ素(SiO2)などから形成される酸化ケイ素系薄膜
は、電気絶縁用や機械保護用として優れた特性を発揮す
ることからエレクトロニクスや光学の分野で包装材料用
の蒸着薄膜として使用されている。また、酸化ケイ素系
薄膜は食品等の包装用として適する透明性やガスバリア
性も有していることから、最近では食品包装材料の表面
被覆用としても使用されるようになってきた。2. Description of the Related Art Conventionally, a silicon oxide thin film formed of silicon monoxide (SiO), silicon dioxide (SiO 2 ) or the like has excellent characteristics for electrical insulation and mechanical protection, and is therefore used for electronics and It is used as a vapor-deposited thin film for packaging materials in the field of optics. Further, since the silicon oxide thin film has transparency and gas barrier properties suitable for packaging foods and the like, it has recently come to be used also as a surface coating for food packaging materials.
【0003】酸化ケイ素系薄膜を形成する方法として、
一酸化ケイ素の粉末、粒状または塊状のものを蒸着用材
料とし、それを加熱し真空蒸発させて包装材料の表面に
薄膜を蒸着させる方法が周知である。しかし、このとき
形成された一酸化ケイ素蒸着膜の屈折率は 2.0〜 2.2と
比較的高い値であるとともに、膜内の分子構造に多くの
酸素欠陥を有しているので、蒸着膜内で光の吸収、散乱
を起こして蒸着膜は褐色に着色し、透明性は必ずしもよ
くないことが知られている。As a method for forming a silicon oxide thin film,
It is well known to use powder, particles or lumps of silicon monoxide as a vapor deposition material, and heat and vacuum evaporate the vapor to deposit a thin film on the surface of the packaging material. However, the refractive index of the silicon monoxide vapor-deposited film formed at this time is a relatively high value of 2.0 to 2.2, and many oxygen defects are present in the molecular structure in the film. It is known that the vapor-deposited film is colored brown due to absorption and scattering of, and its transparency is not necessarily good.
【0004】一酸化ケイ素蒸着膜の透明性には、蒸着時
の蒸着膜組成のコントロールが大きく影響している。す
なわち、蒸着膜組成をSiOxとして表した場合、xの値が
1に近づくにつれて褐色を呈するようになり、xの値が
2に近づくにつれて透明性が向上する。これを前提とし
て、従来から下記、の方法が提案されている。The transparency of a silicon monoxide vapor deposited film is greatly affected by the control of the vapor deposited film composition during vapor deposition. That is, when the vapor deposition film composition is expressed as SiOx, the color becomes brown as the value of x approaches 1, and the transparency improves as the value of x approaches 2. Based on this, the following methods have been conventionally proposed.
【0005】 酸化ケイ素系混合材料、例えば SiO+
Si2O3+SiO2の混合材料を蒸着用材料として、電子ビー
ム加熱によって真空蒸発させてフィルムの表面に蒸着膜
を形成する方法(特開平2−122924号公報参照)。Silicon oxide-based mixed materials such as SiO +
A method in which a mixed material of Si 2 O 3 + SiO 2 is used as a vapor deposition material and vacuum vaporization is performed by electron beam heating to form a vapor deposition film on the surface of the film (see JP-A-2-122924).
【0006】 金属ケイ素および酸化ケイ素、例えば
SiおよびSiO2を出発原料とし、これらを混合することに
よって蒸着用材料として、加熱によって真空蒸着させて
フィルムの表面にSiOx組成を調整した蒸着膜を形成する
方法(特開昭63−310961号公報、特開昭63−166965号公
報参照)。Metallic silicon and silicon oxide, for example
A method in which Si and SiO 2 are used as starting materials, and a mixture of these is used as a material for vapor deposition to perform vacuum vapor deposition by heating to form a vapor deposition film having an adjusted SiOx composition on the surface of the film (Japanese Patent Laid-Open No. 63-310961). , JP-A-63-166965).
【0007】上記、の方法によれば、 SiO2 の多い
組成をもつ蒸着膜を形成することができるので、所期の
透明性を確保することができる。しかし、蒸着用材料と
して混合したSiO2原料はシリカ系ガラスの形態となって
いるため、フィルム表面との密着性が悪いという問題が
ある。According to the above method, a vapor deposition film having a composition containing a large amount of SiO 2 can be formed, so that the desired transparency can be secured. However, since the SiO 2 raw material mixed as the material for vapor deposition is in the form of silica-based glass, there is a problem that the adhesion to the film surface is poor.
【0008】図8は、上記の方法によって Si-SiO2原
料を混合し蒸着用材料として形成した蒸着膜の透明性と
密着性との関係を示す図である。ただし、図の横軸は蒸
着用材料のSi混合比率( mol%)を示し、縦軸は蒸着膜
の透明性の評価基準となる分光光線の透過率を示してい
る。具体的な透明性と密着性の評価要領は後述する。FIG. 8 is a diagram showing the relationship between the transparency and the adhesiveness of a vapor deposition film formed as a vapor deposition material by mixing the Si—SiO 2 raw materials by the above method. However, the horizontal axis of the figure shows the Si mixing ratio (mol%) of the vapor deposition material, and the vertical axis shows the transmittance of the spectral light rays which is the evaluation criterion of the transparency of the vapor deposition film. The specific evaluation procedure of transparency and adhesion will be described later.
【0009】図8から明らかなように、蒸着用材料のSi
mol%を低減して組成中のSiO2を多くすると、透明性を
確保することができるが、密着性が悪化することにな
る。逆にSiO2を減らして密着性を向上させると、今度は
透明性が悪くなって、蒸着膜の透明性と密着性とは相反
した特性を示す。の方法によって形成された蒸着膜も
同様の特性を示すという問題がある。また、上記の、
の方法によって蒸着膜の組成を調整することはかなり
困難であり、さらに SiOとSiO2との蒸気圧に差があり、
すなわちSiO2の蒸気圧が SiOのそれに比較して低圧であ
るため、蒸着時の蒸発速度が制限され生産速度が上がら
ずコスト的にも不利であるという問題もある。As is clear from FIG. 8, the vapor deposition material Si
When the mol% is reduced and the content of SiO 2 in the composition is increased, the transparency can be secured, but the adhesion is deteriorated. On the contrary, when SiO 2 is reduced to improve the adhesion, the transparency becomes worse this time, and the transparency and the adhesion of the deposited film show the contradictory characteristics. There is a problem that the vapor deposition film formed by the above method also exhibits similar characteristics. Also above,
It is quite difficult to adjust the composition of the vapor-deposited film by the method of, and there is a difference in vapor pressure between SiO and SiO 2 ,
That is, since the vapor pressure of SiO 2 is lower than that of SiO 2 , there is a problem in that the evaporation rate at the time of vapor deposition is limited, the production rate does not increase, and there is a cost disadvantage.
【0010】[0010]
【発明が解決しようとする課題】上述の通り、従来の蒸
着用材料を用いて形成された蒸着膜は、食品包装材料用
として必要な透明性と密着性とを同時に具備することが
できず、しかも蒸着時において蒸発速度に制限があり生
産速度が上がらないという製造上の問題がある。As described above, the vapor deposition film formed using the conventional vapor deposition material cannot simultaneously have the transparency and the adhesiveness required for food packaging materials, Moreover, there is a manufacturing problem that the evaporation rate is limited during vapor deposition and the production rate does not increase.
【0011】本発明は、従来の蒸着材料が有していた問
題を克服して、透明性と密着性という相反する特性を兼
ね備えた蒸着膜を形成することができる、食品包装材料
用として好適な蒸着用材料およびその成形体の製造方法
を提供することを目的としている。INDUSTRIAL APPLICABILITY The present invention is suitable for food packaging materials, which can overcome the problems of conventional vapor deposition materials and form a vapor deposition film having contradictory properties of transparency and adhesion. It is an object of the present invention to provide a vapor deposition material and a method for producing a molded body thereof.
【0012】[0012]
【課題を解決するための手段】本発明は、下記(1)の
蒸着用材料および(2)のその製造方法を要旨としてい
る。DISCLOSURE OF THE INVENTION The gist of the present invention is the following vapor deposition material (1) and its production method (2).
【0013】(1) mol%で、一酸化ケイ素( SiO):
20〜90、二酸化ケイ素(SiO2):10〜80から構成される
原料に、酸化マグネシウム( MgO)、酸化ジルコニウム
(Zr02) 、酸化チタニウム(TiO2) および酸化アルミニ
ウム(Al2O3)のうち1種以上が混合されていることを特
徴とする蒸着用材料。(1) In mol%, silicon monoxide (SiO):
20 to 90, silicon dioxide (SiO 2 ): 10 to 80 as raw material, magnesium oxide (MgO), zirconium oxide (Zr0 2 ), titanium oxide (TiO 2 ) and aluminum oxide (Al 2 O 3 ) A material for vapor deposition, characterized in that at least one of them is mixed.
【0014】(2) mol%で、一酸化ケイ素( SiO):
20〜90、二酸化ケイ素(SiO2):10〜80から原料を構成
し、さらに酸化マグネシウム( MgO)、酸化ジルコニウ
ム(Zr02) 、酸化チタニウム(TiO2) および酸化アルミ
ニウム(Al2O3)のうち1種以上を混合し、成形ののち 1
00〜1500℃で熱処理することを特徴とする蒸着用材料の
成形体の製造方法。(2) Silicon monoxide (SiO) at mol%:
20 to 90, silicon dioxide (SiO 2 ): 10 to 80, the raw material is composed of magnesium oxide (MgO), zirconium oxide (Zr0 2 ), titanium oxide (TiO 2 ) and aluminum oxide (Al 2 O 3 ). After mixing one or more of them and molding 1
A method for producing a molded body of a material for vapor deposition, which comprises performing a heat treatment at 00 to 1500 ° C.
【0015】[0015]
【作用】本発明の蒸着用材料は、 SiOおよびSiO2から構
成される原料に、さらに前記以外の金属酸化物として M
gO、ZrO2、TiO2、Al2O3 のうち1種以上が混合されたこ
とを特徴としており、これを用いて形成された酸化ケイ
素系薄膜は透明性および密着性という相反する特性を兼
ね備えたものとなる。The function of the vapor deposition material of the present invention is to use a raw material composed of SiO and SiO 2 and M
One or more of gO, ZrO 2 , TiO 2 , and Al 2 O 3 are mixed, and the silicon oxide thin film formed by using this has both contradictory properties of transparency and adhesion. It becomes a thing.
【0016】酸化ケイ素系薄膜の透明性に関して、前述
の通り、 SiO単体を用いて形成された蒸着膜では分子構
造に多くの酸素欠陥を有しているので、蒸着膜内で光の
吸収、散乱を起こし褐色を呈する。これに対し、 SiOお
よびSiO2を主成分とした上で、さらに金属酸化物として
MgO、ZrO2、TiO2、Al2O3 のうち1種以上を混合するこ
とによって、蒸着膜内の分子構造の酸素欠陥を減少する
ことができ、光の吸収、散乱を抑制することができる。
また、蒸着膜の屈折率を低減することによっても透明性
を改善することができるが、 SiO、SiO2および金属酸化
物の混合比率を調整することで蒸着膜の屈折率を 1.4〜
2.2 の範囲で変化させ得ることも明らかとなった。Regarding the transparency of the silicon oxide thin film, as described above, the vapor deposition film formed by using simple substance of SiO has many oxygen defects in the molecular structure. Occurs and exhibits a brown color. On the other hand, in addition to SiO and SiO 2 as the main components, as a metal oxide
By mixing one or more of MgO, ZrO 2 , TiO 2 , and Al 2 O 3 , oxygen defects in the molecular structure in the deposited film can be reduced, and light absorption and scattering can be suppressed. .
Although it is possible to improve the transparency even by reducing the refractive index of the deposited film, SiO, the refractive index of the deposited film by adjusting the mixing ratio of SiO 2 and metal oxides 1.4
It was also clarified that the range can be changed within 2.2.
【0017】蒸着膜の透明性の評価は、分光光度計によ
って可視光域 (波長 400〜700nm)における分光光線の透
過率を測定することにより行われる。通常、食品包装材
料として使用する場合には、肉眼でほぼ無色と判定され
る分光光線の透過率が78%以上の透明性が基準とされ
る。The transparency of the vapor-deposited film is evaluated by measuring the transmittance of spectral rays in the visible light region (wavelength 400 to 700 nm) with a spectrophotometer. In general, when used as a food packaging material, the standard of transparency is that the spectral light transmittance, which is judged to be almost colorless by the naked eye, is 78% or more.
【0018】蒸着時の密着性に関して、蒸着膜が形成さ
れるフィルム、例えばプラスチックフィルムの熱膨張係
数はSiO2の熱膨張係数に比べると非常に大きく、プラス
チックフィルムの表面にSiO2の薄膜を形成すると、真空
蒸着時の熱応力によって剥離、亀裂、反り、クラックな
どが発生して、薄膜の密着性は著しく悪化する。しか
し、蒸着用材料にSiO2の他に SiOおよび金属酸化物とし
て MgO、ZrO2、TiO2、Al2O3 のうち1種以上を混合させ
ることによって、蒸着膜の熱膨張係数を大きくすること
ができ、蒸着時の密着性を向上させることができる。[0018] For adhesion during deposition, films deposited film is formed, for example, the thermal expansion coefficient of the plastic film is very large compared to the coefficient of thermal expansion of SiO 2, forming a SiO 2 thin film on the surface of the plastic film Then, peeling, cracks, warpage, cracks, and the like occur due to thermal stress during vacuum deposition, and the adhesion of the thin film is significantly deteriorated. However, by increasing the thermal expansion coefficient of the vapor deposition film by mixing SiO 2 as the vapor deposition material and at least one of MgO, ZrO 2 , TiO 2 , and Al 2 O 3 as the metal oxide in addition to SiO 2 . It is possible to improve the adhesion during vapor deposition.
【0019】蒸着膜の密着性の評価は、薄膜に粘着テー
プを貼り、瞬時に剥がすテストを同一場所で10回繰り返
して、そのときの剥離状況を観察して行われている。通
常、食品包装材料として使用する場合には、10回繰り返
して剥がしても全く剥離が見られない程度の密着性を確
保する必要がある。The adhesion of the vapor-deposited film is evaluated by applying an adhesive tape to the thin film and repeating the instant peeling test 10 times at the same place, and observing the peeling condition at that time. Usually, when used as a food packaging material, it is necessary to secure the adhesion to the extent that no peeling is observed even after peeling 10 times.
【0020】本発明の蒸着用材料では、 SiOおよびSiO2
以外の金属酸化物として MgO、ZrO2、TiO2、Al2O3 を使
用することを特徴としている。しかし、これらの金属酸
化物を過剰に混合すると金属酸化物自体の表面エネルギ
ーが大きいため、表面エネルギーが小さいプラスチック
フィルムとの密着性が悪化することになる。また、出発
原料の SiOとSiO2の混合比率によっては、金属酸化物を
混合しても密着性や透明性が改善されない場合もある。
後述の実施例において、食品包装材料として要求される
密着性や透明性を満たすことができる出発原料での SiO
とSiO2の混合比率および金属酸化物の混合量を説明す
る。In the vapor deposition material of the present invention, SiO and SiO 2
It is characterized by using MgO, ZrO 2 , TiO 2 , and Al 2 O 3 as metal oxides other than. However, when these metal oxides are excessively mixed, the surface energy of the metal oxide itself is large, so that the adhesion with a plastic film having a small surface energy is deteriorated. Further, depending on the mixing ratio of the starting materials SiO and SiO 2 , the adhesion and the transparency may not be improved even if the metal oxide is mixed.
In the examples described below, SiO in the starting material that can satisfy the adhesiveness and transparency required for food packaging materials
The mixing ratio of SiO 2 and SiO 2 and the amount of metal oxide mixed will be described.
【0021】蒸着用材料の形態が粉末状のままでは、成
膜時に粉末が飛散し、蒸着膜の特性を劣化させる恐れが
あるので、蒸着用材料は成形体とするのが望ましい。If the vapor deposition material is in the form of powder, the powder may scatter during film formation and deteriorate the characteristics of the vapor deposition film. Therefore, the vapor deposition material is preferably formed into a compact.
【0022】本発明の成形体の製造方法は、 SiOおよび
SiO2から構成される出発原料に、さらに金属酸化物とし
て MgO、ZrO2、TiO2、Al2O3 のうち1種以上を混合し、
成形ののち熱処理することを特徴としている。出発原料
は、蒸着用材料としての焼結性および真空蒸着における
蒸発性を確保するためには微粉末が適しており、成形性
を考慮して粉末の粒径は 0.1〜30μm の範囲とするのが
望ましい。The method for producing a molded article of the present invention comprises SiO and
A starting material composed of SiO 2 is further mixed with at least one of MgO, ZrO 2 , TiO 2 , and Al 2 O 3 as a metal oxide,
It is characterized by heat treatment after molding. As the starting material, fine powder is suitable to secure sinterability as a material for vapor deposition and vaporization in vacuum vapor deposition, and the particle size of the powder should be in the range of 0.1 to 30 μm in consideration of formability. Is desirable.
【0023】出発原料と金属酸化物粉末との混合は、慣
用されているボールミル等の手段を用いてもよく、その
方法は特に限定されない。成形には、プレス成形機等を
用いる方法が適用できる。成形時に使用されるバインダ
ーとしては通常は水が用いられるが、より強固な成形体
を必要とする場合には、ケイ酸エチル、ケイ酸メチル等
のケイ酸化合物、またはポリビニルアルコール等の有機
系化合物を用いることが望ましい。成形バインダーとし
て水を用いる場合には成形後に 200℃程度の乾燥処理で
水分除去ができるが、ケイ酸化合物または有機系化合物
をバインダーとして使用する場合には、これらの除去が
必要となるため 500〜 600℃で数時間の加熱処理が必要
となる。The starting material and the metal oxide powder may be mixed by a commonly used means such as a ball mill, and the method is not particularly limited. A method using a press molding machine or the like can be applied to the molding. Water is usually used as the binder used at the time of molding, but when a stronger molded body is required, ethyl silicate, a silicic acid compound such as methyl silicate, or an organic compound such as polyvinyl alcohol is used. Is preferred. When water is used as a molding binder, water can be removed by a drying treatment at about 200 ° C after molding, but when a silicic acid compound or an organic compound is used as a binder, these must be removed. Heat treatment at 600 ° C for several hours is required.
【0024】成形後の熱処理温度は 100〜1500℃とする
のが望ましい。熱処理温度が 100℃未満であると、乾燥
に長時間を要することになる。一方、熱処理温度が1500
℃を超えると溶融焼結の問題が生じるとともに、蒸着材
料が緻密化して蒸発速度を高めることが困難になる。さ
らに、蒸着材料の取扱いや蒸発速度の確保を考慮するな
らば、熱処理温度は 900〜1100℃の範囲にするのがさら
に望ましい。The heat treatment temperature after molding is preferably 100 to 1500 ° C. When the heat treatment temperature is lower than 100 ° C, it takes a long time to dry. On the other hand, the heat treatment temperature is 1500
If the temperature exceeds ℃, the problem of melting and sintering will occur, and the vapor deposition material will become densified, making it difficult to increase the evaporation rate. Further, considering the handling of the vapor deposition material and the securing of the evaporation rate, the heat treatment temperature is more preferably in the range of 900 to 1100 ° C.
【0025】[0025]
【実施例】本発明の蒸着材料およびその製造方法の作
用、効果を、実施例1から実施例7に基づいて説明す
る。EXAMPLE The operation and effect of the vapor deposition material and the method for producing the same of the present invention will be described based on Examples 1 to 7.
【0026】(実施例1)SiOおよびSiO2から構成され
る出発原料に、金属酸化物として MgOを混合して蒸着用
材料を製造する場合を説明する。Example 1 A case where a starting material composed of SiO and SiO 2 is mixed with MgO as a metal oxide to produce a vapor deposition material will be described.
【0027】SiOとSiO2を粉砕し平均粒径を約20μm と
して、これらをSiOmol%が0、10、20、40、60、80、90
および100mol%となるように混合し8種類の混合比率か
らなる出発原料を作製した。その出発原料に平均粒径21
μm の MgO粉末を添加して MgO mol%が出発原料に対し
(出発原料を100mol%として)0、5、20、30および35
mol%となるように混合した。成形バインダーとして少
量の水を添加後、圧力500kg/cm2で成形して、直径10m
m、厚さ1mmの成形体を得た。その後、成形体を120℃で
15時間乾燥ののち、1000℃で2時間熱処理して蒸着材料
を製造した。SiO and SiO 2 were pulverized to have an average particle size of about 20 μm, and the SiO mol% was 0, 10, 20, 40, 60, 80, 90.
And 100 mol% were mixed to prepare a starting material composed of 8 kinds of mixing ratios. The starting material has an average particle size of 21
Add μm of MgO powder to make MgO mol% 0, 5, 20, 30 and 35 relative to the starting material (100% starting material).
It mixed so that it might become mol%. After adding a small amount of water as a molding binder, mold at a pressure of 500 kg / cm 2 and have a diameter of 10 m.
A molded body with m and a thickness of 1 mm was obtained. Then, the molded body at 120 ℃
After drying for 15 hours, heat treatment was performed at 1000 ° C. for 2 hours to manufacture a vapor deposition material.
【0028】上記蒸着用材料を電子ビーム加熱によって
圧力10-5Torrの雰囲気中で蒸発させ、厚さ12μm のポリ
エチレンテレフタレートフィルムの表面に 500Åの薄膜
を蒸着させた。薄膜の透明度の評価は、分光光度計を用
いて分光光線の透過率で判定した。また、薄膜の密着性
の評価は薄膜に粘着テープを貼り、瞬時に剥がすテスト
を同一場所で10回繰り返すことによって行い、剥離が生
じない場合を密着性良好とし、剥離が発生する場合を密
着性不良とした。The above vapor deposition material was evaporated by electron beam heating in an atmosphere having a pressure of 10 -5 Torr to deposit a thin film of 500 Å on the surface of a polyethylene terephthalate film having a thickness of 12 μm. The transparency of the thin film was evaluated by the transmittance of the spectroscopic light using a spectrophotometer. In addition, the adhesion of the thin film is evaluated by sticking an adhesive tape on the thin film and repeating the instant peeling test 10 times at the same place.If the peeling does not occur, the adhesiveness is good, and if the peeling occurs, the adhesiveness is evaluated. It was bad.
【0029】図1は、実施例1( SiO-SiO2-MgO 系原料
を混合して蒸着用材料を製造した場合)における透明性
と密着性の関係を示す図である。図の横軸には出発原料
の混合比率をSiOmol%で表示し、図中のパラメーターと
してMgO の混合量を出発原料料全体(SiO-SiO2を100mol
%として)に対する mol%で示している。FIG. 1 is a diagram showing the relationship between transparency and adhesion in Example 1 (when a material for vapor deposition was manufactured by mixing SiO—SiO 2 —MgO 2 -based raw materials). The horizontal axis of the figure shows the mixing ratio of the starting materials in SiO mol%, and the mixing amount of MgO as the parameter in the figure is the total starting material (100 mol of SiO-SiO 2
%)).
【0030】図1から明らかなように、蒸着用材料を S
iO単体から製造した場合(図中のSiO :100mol%、MgO
:0mol %) または SiOとSiO2を混合した出発原料の
みから製造した場合(図中のMgO :0mol %) に比べ、
さらに金属酸化物として MgOを混合することによって、
透明性と密着性を改善することができる。しかし、出発
原料に対する MgOの混合比率を増加させ過ぎると、ポリ
エチレンテレフタレートフィルムとの密着性が悪化す
る。As is clear from FIG. 1, the vapor deposition material is S
When manufactured from iO alone (SiO 2 in the figure: 100 mol%, MgO
: 0 mol%) or compared with the case where it is produced only from a starting material in which SiO and SiO 2 are mixed (MgO: 0 mol% in the figure),
Furthermore, by mixing MgO as a metal oxide,
The transparency and adhesion can be improved. However, if the mixing ratio of MgO to the starting material is increased too much, the adhesion with the polyethylene terephthalate film deteriorates.
【0031】前述の通り、食品包装材料として使用する
場合には、透明性は透過率78%以上を確保し、密着性が
良好でなければならない。そのため、金属酸化物として
MgOを混合する場合には、出発原料の混合比率は SiO m
ol%で20〜90 mol%とする必要がある。また、 MgOの混
合比率に関しては、その混合比率を増加させ過ぎると密
着性が悪化することから MgO mol%は5〜30 mol%とす
るのがよい。As described above, when used as a food packaging material, the transparency must ensure a transmittance of 78% or more, and the adhesion must be good. Therefore, as a metal oxide
When mixing MgO, the mixing ratio of the starting materials is SiO m
It is necessary to be 20 to 90 mol% in ol%. Regarding the mixing ratio of MgO, if the mixing ratio is excessively increased, the adhesiveness deteriorates, so MgO mol% is preferably 5 to 30 mol%.
【0032】(実施例2)SiOおよびSiO2から構成され
る出発原料に、金属酸化物としてZr02を混合して蒸着用
材料を製造する場合を説明する。[0032] (Example 2) starting material composed of SiO and SiO 2, illustrating a case of producing the deposition material by mixing Zr0 2 as the metal oxide.
【0033】実施例1と同様に、8種類の混合比率から
なる出発原料を作製した。その出発原料に平均粒径18μ
m のZr02粉末を添加してZr02 mol%が出発原料に対し
0、5、20、25および30 mol%となるように混合し、成
形ののち熱処理して蒸着用材料を製造した。このときの
成形および熱処理条件は実施例1と同様とした。この蒸
着用材料を供試材として実施例1と同様の条件でポリエ
チレンテレフタレートフィルムの表面に 500Åの薄膜を
蒸着した。In the same manner as in Example 1, starting materials having 8 kinds of mixing ratios were prepared. The average particle size of the starting material is 18μ
Zr0 2 powder of m 2 was added and mixed so that Zr0 2 mol% was 0, 5, 20, 25 and 30 mol% with respect to the starting material, and after molding, heat treatment was performed to manufacture a vapor deposition material. The molding and heat treatment conditions at this time were the same as in Example 1. Using this evaporation material as a test material, a thin film of 500 Å was evaporated on the surface of a polyethylene terephthalate film under the same conditions as in Example 1.
【0034】図2は、実施例2( SiO-SiO2-ZrO2系原料
を混合して蒸着用材料を製造した場合)における透明性
と密着性の関係を示す図である。実施例1と同様に、出
発原料にZr02を混合することによって透明性と密着性を
改善できることが分かる。FIG. 2 is a diagram showing the relationship between transparency and adhesion in Example 2 (when a material for vapor deposition was manufactured by mixing SiO—SiO 2 —ZrO 2 -based raw materials). As in Example 1, it can be seen that transparency and adhesion can be improved by mixing ZrO 2 with the starting material.
【0035】図2から、金属酸化物としてZr02を混合す
る場合には、出発原料の混合比率はSiO mol%で20〜90
mol%とする必要がある。また、Zr02の混合比率に関し
ては、その混合比率を増加させ過ぎると密着性が悪化す
ることからZr02 mol%は5〜25 mol%とするのがよい。From FIG. 2, when ZrO 2 is mixed as the metal oxide, the mixing ratio of the starting materials is 20 to 90 in terms of SiO mol%.
Must be mol%. Further, regarding the mixing ratio of Zr0 2 , if the mixing ratio is excessively increased, the adhesiveness deteriorates, so Zr0 2 mol% is preferably set to 5 to 25 mol%.
【0036】(実施例3)SiOおよびSiO2から構成され
る出発原料に、金属酸化物としてTiO2を混合して蒸着用
材料を製造する場合を説明する。[0036] (Example 3) starting material composed of SiO and SiO 2, illustrating a case of producing the deposition material by mixing TiO 2 as the metal oxide.
【0037】8種類の混合比率からなる出発原料に平均
粒径2μm のTiO2粉末を添加してTiO2 mol%が出発原料
に対し0、5、20、30および 35mol%となるように混合
し、成形ののち熱処理して蒸着用材料を製造した。その
後、この蒸着用材料を供試材としてポリエチレンテレフ
タレートフィルムの表面に 500Åの薄膜を蒸着した。TiO 2 powder having an average particle size of 2 μm was added to a starting material composed of 8 kinds of mixing ratios and mixed so that TiO 2 mol% was 0, 5, 20, 30 and 35 mol% with respect to the starting material. After forming, a heat treatment was performed to manufacture a vapor deposition material. Then, a thin film of 500 Å was deposited on the surface of the polyethylene terephthalate film by using this deposition material as a test material.
【0038】その他の条件は実施例1の場合と同様であ
る。Other conditions are the same as those in the first embodiment.
【0039】図3は、実施例3( SiO-SiO2-TiO2系原料
を混合して蒸着用材料を製造した場合)における透明性
と密着性の関係を示す図である。図3から明らかなよう
に、金属酸化物としてTiO2を混合する場合には、出発原
料の混合比率は SiO mol%で20〜90 mol%とする必要が
ある。またTiO2の混合比率に関しては、その混合比率を
増加させ過ぎると密着性が悪化することから、TiO2 mol
%は5〜30 mol%とするのがよい。FIG. 3 is a diagram showing the relationship between transparency and adhesion in Example 3 (when a vapor deposition material was produced by mixing SiO—SiO 2 —TiO 2 -based raw materials). As is clear from FIG. 3, when TiO 2 is mixed as the metal oxide, the mixing ratio of the starting materials must be 20 to 90 mol% in terms of SiO mol%. Also with respect to the mixing ratio of TiO 2, since the mixing adhesion to the ratio excessively increases to deteriorate, TiO 2 mol
% Is preferably 5 to 30 mol%.
【0040】(実施例4)SiOおよびSiO2から構成され
る出発原料に、金属酸化物として Al2O3を混合して蒸着
用材料を製造する場合を説明する。Example 4 A case will be described in which a starting material composed of SiO and SiO 2 is mixed with Al 2 O 3 as a metal oxide to produce a vapor deposition material.
【0041】8種類の混合比率からなる出発原料に平均
粒径24μm の Al2O3粉末を添加してAl2O3 mol%が出発
原料に対し0、5、20、40および45 mol%となるように
混合し、成形ののち熱処理して蒸着用材料を製造した。
その後、この蒸着用材料を供試材としてポリエチレンテ
レフタレートフィルムの表面に 500Åの薄膜を蒸着し
た。その他の条件は実施例1の場合と同様である。Al 2 O 3 powder having an average particle size of 24 μm was added to a starting material composed of 8 kinds of mixing ratios to obtain Al 2 O 3 mol% of 0, 5, 20, 40 and 45 mol% based on the starting material. After mixing, the mixture was molded and then heat-treated to produce a vapor deposition material.
Then, a thin film of 500 Å was deposited on the surface of the polyethylene terephthalate film by using this deposition material as a test material. Other conditions are the same as those in the first embodiment.
【0042】図4は、実施例4( SiO-SiO2-Al2O3 系原
料を混合して蒸着用材料を製造した場合)における透明
性と密着性の関係を示す図である。図4から、金属酸化
物として Al2O3を混合する場合には、出発原料の混合比
率は SiO mol%で20〜90 mol%とする必要がある。ま
た、Al2O3 の混合比率に関しては、その混合比率を増加
させ過ぎると密着性が悪化することから、 Al2O3 mol%
は5〜40 mol%とするのがよい。FIG. 4 is a diagram showing the relationship between transparency and adhesion in Example 4 (when a vapor deposition material was produced by mixing SiO—SiO 2 —Al 2 O 3 -based raw materials). From FIG. 4, when Al 2 O 3 is mixed as the metal oxide, the mixing ratio of the starting materials needs to be 20 to 90 mol% in terms of SiO mol%. Regarding the mixing ratio of Al 2 O 3 , if the mixing ratio is increased too much, the adhesion will deteriorate, so Al 2 O 3 mol%
Is preferably 5 to 40 mol%.
【0043】(実施例5)SiOおよびSiO2から構成され
る出発原料に、金属酸化物として MgOと Al2O3との等モ
ル混合物を混合して蒸着用材料を製造する場合を説明す
る。(Example 5) A case where a vapor deposition material is manufactured by mixing an equimolar mixture of MgO and Al 2 O 3 as a metal oxide with a starting material composed of SiO and SiO 2 will be described.
【0044】8種類の混合比率からなる出発原料に平均
粒径21μm の MgOと平均粒径24μmの Al2O3との等モル
混合物を mol%が出発原料に対し0、5、20、30および
35 mol%となるように混合し、成形ののち熱処理して蒸
着用材料を製造した。その後、この蒸着用材料を供試材
としてポリエチレンテレフタレートフィルムの表面に50
0Åの薄膜を蒸着した。その他の条件は実施例1の場合
と同様である。Equimolar mixture of MgO having an average particle size of 21 μm and Al 2 O 3 having an average particle size of 24 μm was added to a starting material composed of 8 kinds of mixing ratios in an amount of 0, 5, 20, 30 and
The mixture was mixed so as to be 35 mol%, heat-treated after molding, and a vapor deposition material was manufactured. After that, this evaporation material was used as a test material on the surface of the polyethylene terephthalate film.
A 0Å thin film was deposited. Other conditions are the same as those in the first embodiment.
【0045】図5は、実施例5( SiO-SiO2-MgO-Al2O3
系原料を混合して蒸着用材料を製造した場合)における
透明性と密着性の関係を示す図である。図5から明らか
なように、金属酸化物として MgOと Al2O3との等モル混
合物を混合する場合には、出発原料の混合比率は SiO m
ol%で20〜90 mol%とする必要がある。また、 MgOとAl
2O3との等モル混合物の混合比率に関しては、その混合
比率を増加させ過ぎると密着性が悪化することから、5
〜30 mol%とするのがよい。FIG. 5 shows Example 5 (SiO-SiO 2 -MgO-Al 2 O 3
It is a figure which shows the relationship of transparency and adhesiveness in the case of manufacturing a vapor deposition material by mixing a system raw material. As is clear from FIG. 5, when an equimolar mixture of MgO and Al 2 O 3 is mixed as the metal oxide, the mixing ratio of the starting materials is SiO m.
It is necessary to be 20 to 90 mol% in ol%. Also, MgO and Al
Regarding the mixing ratio of the equimolar mixture with 2 O 3 , if the mixing ratio is excessively increased, the adhesion will be deteriorated.
It is recommended to set it to ~ 30 mol%.
【0046】(実施例6)SiOおよびSiO2から構成され
る出発原料に、金属酸化物として MgOと Al2O3とTiO2と
の40:30:30 mol%混合物を混合して蒸着用材料を製造す
る場合を説明する。Example 6 A starting material composed of SiO and SiO 2 was mixed with a 40:30:30 mol% mixture of MgO, Al 2 O 3 and TiO 2 as a metal oxide to form a vapor deposition material. The case of manufacturing is explained.
【0047】8種類の混合比率からなる出発原料に平均
粒径21μm の MgOと平均粒径24μmの Al2O3と平均粒径
2μm のTiO2との40:30:30 mol%混合物を mol%が出発
原料に対し0、5、20、30および35 mol%となるように
混合し、成形ののち熱処理して蒸着用材料を製造した。
その後、この蒸着用材料を供試材としてポリエチレンテ
レフタレートフィルムの表面に 500Åの薄膜を蒸着し
た。その他の条件は実施例1の場合と同様である。40:30:30 mol% mixture of MgO having an average particle size of 21 μm, Al 2 O 3 having an average particle size of 24 μm and TiO 2 having an average particle size of 2 μm was used as a starting material consisting of 8 kinds of mixing ratios. Was mixed with the starting material so as to be 0, 5, 20, 30 and 35 mol%, molded and heat treated to produce a material for vapor deposition.
Then, a thin film of 500 Å was deposited on the surface of the polyethylene terephthalate film by using this deposition material as a test material. Other conditions are the same as those in the first embodiment.
【0048】図6は、実施例6( SiO-SiO2-MgO-Al2O3-
TiO2系原料を混合して蒸着用材料を製造した場合)にお
ける透明性と密着性の関係を示す図である。図6から、
金属酸化物として MgOと Al2O3とTiO2との40/30/30 mol
%混合物を混合する場合には、出発原料の混合比率は S
iO mol%で20〜90 mol%とする必要がある。また、 MgO
と Al2O3とTiO2との40/30/30 mol%混合物の混合比率に
関しては、その混合比率を増加させ過ぎると密着性が悪
化することから、5〜30 mol%とするのがよい。FIG. 6 shows Example 6 (SiO-SiO 2 -MgO-Al 2 O 3-
It is a diagram showing the adhesion relationship between transparency in case of producing the deposition material by mixing TiO 2 system material). From FIG.
40/30/30 mol of MgO, Al 2 O 3 and TiO 2 as metal oxide
% When the mixture is mixed, the mixing ratio of the starting materials is S
iO mol% needs to be 20 to 90 mol%. Also, MgO
And Al with respect to the second mixing ratio of O 3 and 40/30/30 mol% mixture of TiO 2, since the adhesion too increase its mixing ratio is deteriorated, it is preferable to 5 to 30 mol% .
【0049】なお、出発原料に金属酸化物として2種以
上の混合物を混合して蒸着用材料を製造する場合として
実施例5および実施例6を示したが、他の金属酸化物を
2種以上混合する場合であっても、その混合物の混合比
率は実施例5、実施例6に示す範囲内であれば、透明性
と密着性が十分確保できることを確認している。Although Example 5 and Example 6 are shown as the case of manufacturing a material for vapor deposition by mixing a mixture of two or more kinds of metal oxides as a starting material, two or more kinds of other metal oxides are shown. Even in the case of mixing, it has been confirmed that transparency and adhesion can be sufficiently ensured as long as the mixing ratio of the mixture is within the range shown in Examples 5 and 6.
【0050】(実施例7)SiOおよびSiO2から構成され
る出発原料に金属酸化物として MgOを混合して蒸着用材
料を製造する場合に、成形体に施される熱処理温度が蒸
着時の蒸発特性に及ぼす影響を調査した。(Example 7) When a starting material composed of SiO and SiO 2 is mixed with MgO as a metal oxide to produce a material for vapor deposition, the heat treatment temperature applied to the compact is evaporation during vapor deposition. The effect on properties was investigated.
【0051】SiOとSiO2を粉砕し平均粒径を約20μm と
し、SiO が60 mol%、SiO2が40 mol%の比率で構成され
る出発原料を作製したのち、平均粒径21μm の MgO粉末
を添加して MgO mol%が出発原料に対し20 mol%になる
ように混合した。成形バインダーとして少量の水を添加
後、圧力 500kg/cm2で成形して、直径10mm、厚さ1mmの
成形体を得た。その後、成形体を 100℃〜1580℃の範囲
内で熱処理温度を変化させて、大気中で2時間加熱して
蒸着材料を製造した。SiO and SiO 2 were crushed to have an average particle size of about 20 μm, and a starting material composed of SiO 2 in an amount of 60 mol% and SiO 2 in an amount of 40 mol% was prepared. Was added and mixed so that MgO mol% was 20 mol% with respect to the starting material. After adding a small amount of water as a molding binder, molding was performed at a pressure of 500 kg / cm 2 to obtain a molded body having a diameter of 10 mm and a thickness of 1 mm. Then, the heat treatment temperature of the molded body was changed within the range of 100 ° C. to 1580 ° C., and the molded body was heated in the atmosphere for 2 hours to manufacture a vapor deposition material.
【0052】製造された蒸着材料の蒸着時の蒸発速度を
評価するため、蒸着材料を真空熱天秤で10℃/minで昇温
して、圧力10-5Torrの条件で温度1250℃に2時間保持
し、このときの蒸着材料の蒸発率を測定した。蒸着材料
の蒸発率は、昇温前後の重量を計量して求められ、(昇
温前の重量−昇温後の重量)/(昇温前の重量)で示さ
れる。In order to evaluate the evaporation rate of the produced vapor deposition material during vapor deposition, the vapor deposition material was heated with a vacuum thermobalance at 10 ° C./min, and the temperature was 1250 ° C. for 2 hours under the pressure of 10 −5 Torr. It was held and the evaporation rate of the vapor deposition material at this time was measured. The evaporation rate of the vapor deposition material is determined by weighing the weight before and after temperature rise, and is represented by (weight before temperature rise-weight after temperature rise) / (weight before temperature rise).
【0053】図7は、成形体の熱処理温度と蒸着材料の
蒸発率の関係を示した図である。図7から明らかなよう
に、熱処理温度が上昇すると、粒成長にともなって蒸着
材料の比表面積が低下するので、蒸着時の蒸発率が小さ
くなる。特に熱処理温度が1500℃を超えると、著しく蒸
発率が低下し、蒸発速度が制限される。一方、熱処理温
度が 100℃未満では、乾燥に長時間を要する。したがっ
て、成形体の熱処理温度は、 100〜1500℃の範囲にする
のが望ましい。また、熱処理温度が 900℃未満では、成
形体が十分に固化しないのでその取扱いに注意を要する
ことから、成形体の熱処理温度は 900〜1100℃の範囲に
するのがさらに望ましい。FIG. 7 is a diagram showing the relationship between the heat treatment temperature of the compact and the evaporation rate of the vapor deposition material. As is clear from FIG. 7, when the heat treatment temperature rises, the specific surface area of the vapor deposition material decreases with grain growth, so the evaporation rate during vapor deposition decreases. Especially when the heat treatment temperature exceeds 1500 ° C., the evaporation rate is remarkably reduced, and the evaporation rate is limited. On the other hand, if the heat treatment temperature is less than 100 ° C, it takes a long time to dry. Therefore, it is desirable that the heat treatment temperature of the molded body is in the range of 100 to 1500 ° C. Further, if the heat treatment temperature is lower than 900 ° C, the molded body will not be sufficiently solidified, and therefore care must be taken in its handling. Therefore, the heat treatment temperature of the molded body is more preferably in the range of 900 to 1100 ° C.
【0054】実施例では、金属酸化物として MgOを混合
して蒸着用材料を製造する場合について説明したが、他
にZr02、TiO2およびAl2O3 のうち1種以上を混合する場
合であっても同様であることを確認している。In the examples, the case where MgO is mixed as the metal oxide to produce the vapor deposition material has been described. However, in the case where at least one of Zr0 2 , TiO 2 and Al 2 O 3 is mixed, I have confirmed that it is the same even if there is.
【0055】[0055]
【効果】本発明の蒸着用材料を用いれば、透明性と密着
性のいずれにも優れ食品包装材料に適する蒸着膜を形成
することができる。さらに本発明の製造方法によれば、
取扱いが容易で蒸発率も高い前記の蒸着材料の成形体を
製造することができる。[Effect] By using the vapor deposition material of the present invention, it is possible to form a vapor deposition film excellent in both transparency and adhesiveness and suitable for food packaging materials. Furthermore, according to the manufacturing method of the present invention,
A molded body of the above vapor deposition material that is easy to handle and has a high evaporation rate can be manufactured.
【図1】実施例1( SiO-SiO2-MgO 系原料を混合して蒸
着用材料を製造した場合)における透明性と密着性の関
係を示す図である。FIG. 1 is a diagram showing the relationship between transparency and adhesion in Example 1 (when a vapor deposition material is manufactured by mixing SiO—SiO 2 —MgO 3 -based raw materials).
【図2】実施例2( SiO-SiO2-ZrO2系原料を混合して蒸
着用材料を製造した場合)における透明性と密着性の関
係を示す図である。FIG. 2 is a diagram showing a relationship between transparency and adhesion in Example 2 (when a vapor deposition material is manufactured by mixing SiO—SiO 2 —ZrO 2 -based raw materials).
【図3】実施例3( SiO-SiO2-TiO2系原料を混合して蒸
着用材料を製造した場合)における透明性と密着性の関
係を示す図である。FIG. 3 is a diagram showing the relationship between transparency and adhesion in Example 3 (when a vapor deposition material is manufactured by mixing SiO—SiO 2 —TiO 2 based raw materials).
【図4】実施例4( SiO-SiO2-Al2O3 系原料を混合して
蒸着用材料を製造した場合)における透明性と密着性の
関係を示す図である。FIG. 4 is a diagram showing a relationship between transparency and adhesion in Example 4 (when a vapor deposition material is manufactured by mixing SiO—SiO 2 —Al 2 O 3 -based raw materials).
【図5】実施例5( SiO-SiO2-MgO-Al2O3 系原料を混合
して蒸着用材料を製造した場合)における透明性と密着
性の関係を示す図である。FIG. 5 is a diagram showing a relationship between transparency and adhesion in Example 5 (when a material for vapor deposition is manufactured by mixing SiO—SiO 2 —MgO—Al 2 O 3 -based raw materials).
【図6】実施例6( SiO-SiO2-Al2O3-TiO2系原料を混合
して蒸着用材料を製造した場合)における透明性と密着
性の関係を示す図である。FIG. 6 is a diagram showing a relationship between transparency and adhesion in Example 6 (when a material for vapor deposition is manufactured by mixing SiO—SiO 2 —Al 2 O 3 —TiO 2 -based raw materials).
【図7】成形体の熱処理温度と蒸着材料の蒸発率の関係
を示した図である。Si-SiO2原料を混合し蒸着用材料と
して形成した蒸着膜の透明性と密着性との関係を示す図
である。FIG. 7 is a diagram showing a relationship between a heat treatment temperature of a molded body and an evaporation rate of a vapor deposition material. FIG. 3 is a diagram showing a relationship between transparency and adhesion of a vapor deposition film formed as a vapor deposition material by mixing Si—SiO 2 raw materials.
【図8】Si-SiO2原料を混合し蒸着用材料として形成し
た蒸着膜の透明性と密着性との関係を示す図である。FIG. 8 is a diagram showing a relationship between transparency and adhesion of a vapor deposition film formed as a vapor deposition material by mixing Si—SiO 2 raw materials.
Claims (2)
0、二酸化ケイ素(SiO2):10〜80から構成される原料
に、酸化マグネシウム( MgO)、酸化ジルコニウム(Zr
02) 、酸化チタニウム(TiO2) および酸化アルミニウム
(Al2O3)のうち1種以上が混合されていることを特徴と
する蒸着用材料。1. A mol% of silicon monoxide (SiO): 20-9.
0, silicon dioxide (SiO 2 ): 10 to 80 as a raw material, magnesium oxide (MgO), zirconium oxide (Zr
0 2 ), titanium oxide (TiO 2 ), and aluminum oxide (Al 2 O 3 ).
0、二酸化ケイ素(SiO2):10〜80から原料を構成し、
さらに酸化マグネシウム( MgO)、酸化ジルコニウム
(Zr02)、酸化チタニウム(TiO2) および酸化アルミニ
ウム(Al2O3)のうち1種以上を混合し、成形ののち 100
〜1500℃で熱処理することを特徴とする蒸着用材料の成
形体の製造方法。2. Silicon monoxide (SiO): 20-9 in mol%.
0, silicon dioxide (SiO 2 ): The raw material is composed of 10 to 80,
Furthermore, one or more kinds of magnesium oxide (MgO), zirconium oxide (Zr0 2 ), titanium oxide (TiO 2 ) and aluminum oxide (Al 2 O 3 ) are mixed, and after molding, 100
A method for manufacturing a molded body of a material for vapor deposition, which comprises heat treatment at a temperature of up to 1500 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10277195A JP3725200B2 (en) | 1995-04-26 | 1995-04-26 | Vapor deposition material and method for producing molded article thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10277195A JP3725200B2 (en) | 1995-04-26 | 1995-04-26 | Vapor deposition material and method for producing molded article thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08296036A true JPH08296036A (en) | 1996-11-12 |
| JP3725200B2 JP3725200B2 (en) | 2005-12-07 |
Family
ID=14336433
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10277195A Expired - Fee Related JP3725200B2 (en) | 1995-04-26 | 1995-04-26 | Vapor deposition material and method for producing molded article thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3725200B2 (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008195992A (en) * | 2007-02-09 | 2008-08-28 | Dainippon Printing Co Ltd | Raw material powder of evaporation source material for ion plating, evaporation source material for ion plating and manufacturing method thereof, gas barrier sheet and manufacturing method thereof |
| JP2009024253A (en) * | 2007-06-20 | 2009-02-05 | Dainippon Printing Co Ltd | Raw material powder of evaporation source material for ion plating, evaporation source material for ion plating and manufacturing method thereof, gas barrier sheet and manufacturing method thereof |
| JP2009215125A (en) * | 2008-03-12 | 2009-09-24 | Shin Etsu Chem Co Ltd | Silicon oxide sintered compact for film vapor deposition, method for producing the same, and method for producing silicon oxide vapor deposition film |
| EP1892313A4 (en) * | 2005-06-16 | 2010-01-27 | Osaka Titanium Technologies Co | Silicon monoxide vapor deposition material and process for producing the same |
| JP2010018445A (en) * | 2008-07-08 | 2010-01-28 | Shin-Etsu Chemical Co Ltd | Pellet body for film vapor deposition, method for producing the same, and method for producing silicon oxide vapor-deposited film |
| JP2012087390A (en) * | 2010-10-21 | 2012-05-10 | Toppan Printing Co Ltd | Vapor deposition material |
| JP2012122128A (en) * | 2010-02-16 | 2012-06-28 | Mitsubishi Materials Corp | Vapor deposition material for forming thin film, and thin film sheet and laminated sheet provided with the thin film |
| JP2012132085A (en) * | 2010-03-04 | 2012-07-12 | Mitsubishi Materials Corp | Deposition material for forming thin film, thin-film sheet having the thin film, and laminated sheet |
| WO2020137990A1 (en) * | 2018-12-26 | 2020-07-02 | Agc株式会社 | Vapor deposition material, method for manufacturing substrate having underlayer thereon, and method for manufacturing substrate having water-repellent and oil-repellent layer thereon |
| WO2020137999A1 (en) * | 2018-12-26 | 2020-07-02 | Agc株式会社 | Vapor deposition material, and methods for manufacturing substrate having underlayer thereon and substrate having water-repellent and oil-repellent layer thereon using same |
| CN113227439A (en) * | 2018-12-26 | 2021-08-06 | Agc株式会社 | Vapor deposition material, method for producing substrate with base layer, and method for producing substrate with water-and oil-repellent layer |
| CN113260463B (en) * | 2018-12-26 | 2023-09-22 | Agc株式会社 | Base material with water-repellent and oil-repellent layer, evaporation material and method for manufacturing base material with water-repellent and oil-repellent layer |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4771544B2 (en) * | 2006-11-28 | 2011-09-14 | 株式会社大阪チタニウムテクノロジーズ | Method for producing SiO sintered body |
-
1995
- 1995-04-26 JP JP10277195A patent/JP3725200B2/en not_active Expired - Fee Related
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1892313A4 (en) * | 2005-06-16 | 2010-01-27 | Osaka Titanium Technologies Co | Silicon monoxide vapor deposition material and process for producing the same |
| JP2008195992A (en) * | 2007-02-09 | 2008-08-28 | Dainippon Printing Co Ltd | Raw material powder of evaporation source material for ion plating, evaporation source material for ion plating and manufacturing method thereof, gas barrier sheet and manufacturing method thereof |
| JP2009024253A (en) * | 2007-06-20 | 2009-02-05 | Dainippon Printing Co Ltd | Raw material powder of evaporation source material for ion plating, evaporation source material for ion plating and manufacturing method thereof, gas barrier sheet and manufacturing method thereof |
| JP2009215125A (en) * | 2008-03-12 | 2009-09-24 | Shin Etsu Chem Co Ltd | Silicon oxide sintered compact for film vapor deposition, method for producing the same, and method for producing silicon oxide vapor deposition film |
| US7998263B2 (en) | 2008-03-12 | 2011-08-16 | Shin-Etsu Chemical Co., Ltd. | Sintered silicon oxide for film vapor deposition, its production method, and method for producing silicon oxide vapor deposition film |
| US8066806B2 (en) | 2008-03-12 | 2011-11-29 | Shin-Etsu Chemical Co., Ltd. | Sintered silicon oxide for film vapor deposition, its production method, and method for producing silicon oxide vapor deposition film |
| JP2010018445A (en) * | 2008-07-08 | 2010-01-28 | Shin-Etsu Chemical Co Ltd | Pellet body for film vapor deposition, method for producing the same, and method for producing silicon oxide vapor-deposited film |
| JP2012122128A (en) * | 2010-02-16 | 2012-06-28 | Mitsubishi Materials Corp | Vapor deposition material for forming thin film, and thin film sheet and laminated sheet provided with the thin film |
| JP2012132085A (en) * | 2010-03-04 | 2012-07-12 | Mitsubishi Materials Corp | Deposition material for forming thin film, thin-film sheet having the thin film, and laminated sheet |
| JP2012087390A (en) * | 2010-10-21 | 2012-05-10 | Toppan Printing Co Ltd | Vapor deposition material |
| WO2020137990A1 (en) * | 2018-12-26 | 2020-07-02 | Agc株式会社 | Vapor deposition material, method for manufacturing substrate having underlayer thereon, and method for manufacturing substrate having water-repellent and oil-repellent layer thereon |
| WO2020137999A1 (en) * | 2018-12-26 | 2020-07-02 | Agc株式会社 | Vapor deposition material, and methods for manufacturing substrate having underlayer thereon and substrate having water-repellent and oil-repellent layer thereon using same |
| CN113227439A (en) * | 2018-12-26 | 2021-08-06 | Agc株式会社 | Vapor deposition material, method for producing substrate with base layer, and method for producing substrate with water-and oil-repellent layer |
| CN113227440A (en) * | 2018-12-26 | 2021-08-06 | Agc株式会社 | Vapor deposition material, substrate with base layer using same, and method for producing substrate with water-and oil-repellent layer |
| CN113227441A (en) * | 2018-12-26 | 2021-08-06 | Agc株式会社 | Vapor deposition material, method for producing substrate with base layer, and method for producing substrate with water-and oil-repellent layer |
| JPWO2020137990A1 (en) * | 2018-12-26 | 2021-11-18 | Agc株式会社 | A method for manufacturing a vapor-deposited material, a base material with a base layer, and a method for manufacturing a base material with a water-repellent and oil-repellent layer. |
| JPWO2020137993A1 (en) * | 2018-12-26 | 2021-11-18 | Agc株式会社 | A method for manufacturing a vapor-deposited material, a base material with a base layer, and a method for manufacturing a base material with a water-repellent and oil-repellent layer. |
| JPWO2020137999A1 (en) * | 2018-12-26 | 2021-11-18 | Agc株式会社 | A method for manufacturing a vapor-deposited material, a base material with a base layer, and a base material with a water-repellent oil-repellent layer using the same. |
| CN113260463B (en) * | 2018-12-26 | 2023-09-22 | Agc株式会社 | Base material with water-repellent and oil-repellent layer, evaporation material and method for manufacturing base material with water-repellent and oil-repellent layer |
| CN113227440B (en) * | 2018-12-26 | 2023-10-20 | Agc株式会社 | Vapor deposition material and method for manufacturing base material with base layer and base material with water-repellent and oil-repellent layer using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3725200B2 (en) | 2005-12-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH08296036A (en) | Material for vapor deposition and method for producing molded body thereof | |
| JP3836163B2 (en) | Method for forming high refractive index film | |
| CA1096715A (en) | Heat-reflecting glass pane and a process for the production thereof | |
| EP2123612B1 (en) | Wear resistant coatings and tiles and methods of making same | |
| BE1005853A5 (en) | Ceramic titanate aluminum production method thereof. | |
| US5137779A (en) | Glass-ceramic article decorated with ceramic color | |
| JP4964584B2 (en) | Use of vapor deposition materials to produce high refractive index optical layers, vapor deposition materials, and methods of preparing the vapor deposition materials | |
| JPH0667019A (en) | Antireflection layer and its production | |
| US3663244A (en) | High durability lead titanate-containing enamel for glass ceramics | |
| US20220306526A1 (en) | Thermochromic materials | |
| JP2008057045A (en) | Oxide sintered sputtering target | |
| US4004935A (en) | Glazing compositions for ceramic articles | |
| JP3314542B2 (en) | Low order titanium oxide powder | |
| CN113336450A (en) | Antireflection film, preparation method thereof and optical element | |
| JP5095994B2 (en) | Vapor deposition material for producing high refractive index optical layers | |
| JP2946569B2 (en) | Composition for forming high heat resistant high refractive index composite oxide thin film | |
| JPH0428858A (en) | Production of vapor deposition material | |
| CN115921863A (en) | Coating material, composite oxide film, preparation method and optical product | |
| GB2029861A (en) | A heat reflecting pane and a method of manufacturing the same | |
| EP3561006A1 (en) | Glitter pigment, pigment-containing composition, and pigment-containing coated object | |
| JP5533049B2 (en) | Vapor deposition material and method for producing the same | |
| JP2004002202A (en) | Target and its manufacturing method | |
| JP6800446B2 (en) | Optical film and its manufacturing method | |
| CN120303223A (en) | Glass article and method of manufacturing the same | |
| JPS623782B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A131 | Notification of reasons for refusal |
Effective date: 20040113 Free format text: JAPANESE INTERMEDIATE CODE: A131 |
|
| A521 | Written amendment |
Effective date: 20040309 Free format text: JAPANESE INTERMEDIATE CODE: A523 |
|
| A521 | Written amendment |
Effective date: 20040325 Free format text: JAPANESE INTERMEDIATE CODE: A523 |
|
| A131 | Notification of reasons for refusal |
Effective date: 20050614 Free format text: JAPANESE INTERMEDIATE CODE: A131 |
|
| A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20050627 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Effective date: 20050920 Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20050921 |
|
| R150 | Certificate of patent (=grant) or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 3 Free format text: PAYMENT UNTIL: 20080930 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080930 Year of fee payment: 3 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 6 Free format text: PAYMENT UNTIL: 20110930 |
|
| LAPS | Cancellation because of no payment of annual fees |