JPS637378A - Production of material coated with hyperfine particle metal - Google Patents
Production of material coated with hyperfine particle metalInfo
- Publication number
- JPS637378A JPS637378A JP15072486A JP15072486A JPS637378A JP S637378 A JPS637378 A JP S637378A JP 15072486 A JP15072486 A JP 15072486A JP 15072486 A JP15072486 A JP 15072486A JP S637378 A JPS637378 A JP S637378A
- Authority
- JP
- Japan
- Prior art keywords
- transition metal
- polymer material
- compd
- metal salt
- metal
- 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
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 17
- 239000002184 metal Substances 0.000 title claims abstract description 17
- 239000002245 particle Substances 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 23
- -1 transition metal salt Chemical class 0.000 claims abstract description 19
- 239000002923 metal particle Substances 0.000 claims description 9
- 239000002861 polymer material Substances 0.000 abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- 150000002739 metals Chemical class 0.000 abstract description 3
- 229910052759 nickel Inorganic materials 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 229910052763 palladium Inorganic materials 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 2
- 239000013528 metallic particle Substances 0.000 abstract 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 abstract 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract 1
- 229910052804 chromium Inorganic materials 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 229910052721 tungsten Inorganic materials 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000010419 fine particle Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229920002799 BoPET Polymers 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 150000001728 carbonyl compounds Chemical group 0.000 description 4
- 239000011882 ultra-fine particle Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 1
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- CMMUKUYEPRGBFB-UHFFFAOYSA-L dichromic acid Chemical compound O[Cr](=O)(=O)O[Cr](O)(=O)=O CMMUKUYEPRGBFB-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、電磁特性に優れた超微粒金属で被覆した高分
子材料の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing a polymeric material coated with ultrafine metal particles having excellent electromagnetic properties.
鉄、コバルト、ニッケル等遷移金属の微粒子は、特異な
電磁特性を有するため電子部品材料等へ応用されている
。Fine particles of transition metals such as iron, cobalt, and nickel have unique electromagnetic properties and are used in electronic component materials.
この微粒子を高分子材料の表面に分散付着させて実用材
料とする方法としては、例えば、金属微粒子を塗料に混
ぜて高分子材料表面に塗布したり、無電解メツキによる
金属微粒子の製造時に高分子を存在させてその表面に微
粒子を付着させる方法がある。Methods for making practical materials by dispersing and adhering these fine particles to the surface of polymeric materials include, for example, mixing metal fine particles with paint and applying it to the surface of polymeric materials, or using electroless plating to manufacture polymeric fine particles. There is a method in which fine particles are attached to the surface of the particles.
しかしながら、従来方法では金属微粒子が材料表面で凝
集して塊状に付着し、微粒子の特性が生かされなくなっ
たり、実用上十分な強度で付着保持されなかったり、ま
た、複雑な形状の高分子材料には適用が困難だったり、
あるいは、還元剤等の不純物が混入する等の問題や、求
める程の細かな金属微粒子とならないなどの欠点があっ
た。However, with conventional methods, metal fine particles aggregate on the material surface and adhere in a lump, making it impossible to take advantage of the characteristics of the fine particles, or not being able to adhere and hold them with sufficient strength for practical use. is difficult to apply,
In addition, there are problems such as the contamination of impurities such as reducing agents, and disadvantages such as failure to obtain fine metal particles as desired.
本発明は、かかる問題点の解消を目的にして、高分子材
料表面で遷移金属カルボニル化合物を低温で反応させる
ことにより、この目的を達成し、かつ従来になく超微粒
の金属粒子を材料表面に分散付着させることが出来、こ
れによって優れた電磁特性が得られることを見い出して
為されたものである。The present invention aims to solve these problems by reacting a transition metal carbonyl compound on the surface of a polymeric material at a low temperature, thereby achieving this objective and applying unprecedentedly ultrafine metal particles to the surface of the material. This was done after discovering that it is possible to deposit it in a dispersed manner and that this provides excellent electromagnetic properties.
すなわち、本発明は、［高分子材料の表面において、遷
移金属塩および遷移金属カルボニル化合物を１２０℃以
下で接触し、反応させて平均粒径。That is, the present invention is directed to [a transition metal salt and a transition metal carbonyl compound are brought into contact with each other at 120° C. or lower on the surface of a polymeric material, and reacted to reduce the average particle size.
０．２ミクロン以下の金属粒子を該高分子材料の表面に
分散付着させることを特徴とする超微粒金属で被覆した
材料の製造方法」である。A method for producing a material coated with ultrafine metal particles, which comprises dispersing and adhering metal particles of 0.2 microns or less onto the surface of the polymer material.
本発明方法によって、超微粒金属が良く分散し、かつ実
用十分な強度で付着保持された高分子材料が低温での反
応で簡便に得られる。By the method of the present invention, a polymer material in which ultrafine metal particles are well dispersed and adhered and held with sufficient strength for practical use can be easily obtained by reaction at a low temperature.
かかる方法は、粒状、繊維状、板状のほか、複雑な形状
の高分子材料にも適用することができる。This method can be applied to polymer materials having complex shapes as well as particles, fibers, and plates.
得られた被覆材料は、金属粒子が超微粒子で均質に分散
されているため優れた電磁特性を有し、導電材料、磁性
材料、光学材料等への応用に存用である。The obtained coating material has excellent electromagnetic properties because the metal particles are homogeneously dispersed as ultrafine particles, and is useful for applications such as conductive materials, magnetic materials, and optical materials.
〔作 用〕
本発明で使用される高分子材料は、有機系および無機系
高分子材料であり、粉末状、繊維状、板状等のいかなる
形状の高分子材料にも適用できる。[Function] The polymeric materials used in the present invention are organic and inorganic polymeric materials, and can be applied to polymeric materials in any shape such as powder, fiber, plate, etc.
具体的には、バルブ、綿などの天然高分子；ポリオレフ
ィン、ポリアミドなどの熱可塑性樹脂；エポキシ樹脂、
不飽和ポリエステル等の熱硬化性樹脂；グラファイト、
炭素繊維等の炭素材料などがある。Specifically, natural polymers such as valves and cotton; thermoplastic resins such as polyolefins and polyamides; epoxy resins,
Thermosetting resins such as unsaturated polyester; graphite,
Examples include carbon materials such as carbon fiber.
また、本発明で用いる遷移金属塩は、例えばＣｕ。Further, the transition metal salt used in the present invention is, for example, Cu.
Ｎｉ、Ｇｏ、Ｐｄ、Ｆｅ等の金属の塩であり、中でもＮ
ｉ、Ｐｄの塩が好ましい。Salts of metals such as Ni, Go, Pd, Fe, etc. Among them, N
i, Pd salts are preferred.
さらに、本発明で用いる遷移金属カルボニル化合物は、
Ｆｅ、 Ｎｉ＋ Ｃｏ＋ Ｗ＋ Ｍｏ、 Ｃｒ等の金属
のカルボニル化合物である。これらは併用しても差し支
えない。Furthermore, the transition metal carbonyl compound used in the present invention is
It is a carbonyl compound of a metal such as Fe, Ni+ Co+ W+ Mo, or Cr. These may be used in combination.
次に、上記の遷移金属塩および遷移金属カルボニル化合
物を高分子材料の表面で接触、反応させるには、−般に
は次の方法が好適である。Next, the following method is generally suitable for bringing the above transition metal salt and transition metal carbonyl compound into contact and reacting on the surface of the polymeric material.
先ず、高分子材料の表面に遷移金属塩を付着せしめるが
、付着に先立ち、必要に応じて高分子材料表面に酸化処
理を行なう。この酸化処理は、たとえば硫酸酸性の重ク
ロム酸カリ溶液などで処理することにより行なわれる。First, a transition metal salt is deposited on the surface of a polymeric material, but prior to the deposition, the surface of the polymeric material is oxidized if necessary. This oxidation treatment is carried out, for example, by treatment with a sulfuric acid acidic potassium dichromate solution.
この高分子材料を、塩化第１錫の塩酸酸性水溶液に浸漬
したのち、遷移金属塩の塩酸酸性水溶液に浸漬すること
によって表面に遷移金属塩を付着せしめる。This polymeric material is immersed in an acidic hydrochloric acid aqueous solution of tinnous chloride, and then immersed in an acidic hydrochloric acid aqueous solution of a transition metal salt to adhere the transition metal salt to the surface.
次いで、遷移金属塩の付着された高分子材料を金属カル
ボニル化合物と接触させて金属カルボニル化合物を熱分
解する。Next, the polymeric material to which the transition metal salt is attached is brought into contact with the metal carbonyl compound to thermally decompose the metal carbonyl compound.
この熱分解時の温度は、１２０℃以下、好ましくは１０
０℃以下にすることが重要である。The temperature during this thermal decomposition is 120°C or less, preferably 10°C or less.
It is important to keep the temperature below 0°C.
温度が１２０℃超過では高分子材料表面以外の反応器壁
などにも分解金属が析出したり、副反応による炭素が不
純物として生成したり、また、金属の平均粒子径も０．
２ミクロン（μ）より大となってしまう。If the temperature exceeds 120°C, decomposed metals may precipitate on the walls of the reactor other than on the surface of the polymer material, carbon may be produced as impurities due to side reactions, and the average particle size of the metal may also be 0.
It becomes larger than 2 microns (μ).
上記の反応は、気相および触媒を使用した液相でも行な
える。液相で行なう場合は、トルエン、デカンなどの不
活性溶媒中に金属カルボニル化合物を溶解し、この溶液
に高分子材料を浸漬して分解反応を行なわせることがで
きる。The above reactions can be carried out in the gas phase and also in the liquid phase using catalysts. When carrying out the decomposition reaction in a liquid phase, the metal carbonyl compound can be dissolved in an inert solvent such as toluene or decane, and the polymeric material can be immersed in this solution to carry out the decomposition reaction.
生成した超微粒子金属の酸化を防ぐために、必要に応じ
て酸化防止処理を行なう。これに有効な酸化防止剤はシ
ランカップリング剤である。シランカップリング剤の具
体例としてはビニルトリエトキシシラン、γ−メタクリ
ロキシプコビルトリメトキシシランなどのビニル系シラ
ン化合物；γ−アミノプロビルトリエトキシシラン、Ｎ
−フェニル−γ−アミノプロピルトリメトキシシランな
どのアミノ系シラン化合物；γ−グリシドキシプロビル
メチルジェトキシシランなどのエポキシ系シラン化合物
がある。これらのなかではアミノ系シランカップリング
剤が特に有効である。In order to prevent the generated ultrafine metal particles from oxidizing, anti-oxidation treatment is performed as necessary. An effective antioxidant for this purpose is a silane coupling agent. Specific examples of silane coupling agents include vinyl silane compounds such as vinyltriethoxysilane and γ-methacryloxypcobyltrimethoxysilane; γ-aminoprobyltriethoxysilane, N
-Phenyl-γ-aminopropyltrimethoxysilane and other amino-based silane compounds; and γ-glycidoxypropylmethyljethoxysilane and other epoxy-based silane compounds. Among these, amino-based silane coupling agents are particularly effective.
酸化防止処理方法は、シランカップリング剤を気相また
は液相で前記の超微粒子金属被覆材料に５０〜１５０℃
にて接触させることで行なうことができる。The oxidation prevention treatment method involves applying a silane coupling agent to the ultrafine metal coating material in the gas phase or liquid phase at 50 to 150°C.
This can be done by contacting the
実施例１
厚さ１００μのポリエチレンテレフタレート（ＰＥＴ）
フィルムの表面を予め重クロム酸溶液（ＫｚＣｒ２（ｈ
５０ ｇ Ｓ？ａ硫酸４００ｍｌ、水６ Ｑ ０ｍ１
）で室温下に酸化処理し、次いで塩化第一錫溶液（Ｓｎ
Ｃｆｆｚ １００ ｇ、、ＨＣｊ２５０ｍｊ！、水Ｉｌ
）、塩化パラジウム溶液（ｐａｃｘ ２０．５ ｇ 、
濃塩酸１０ｍ１、水４１）に順次浸漬し、最後に５０
℃で３時間乾燥して遷移金属処理を行なった。Example 1 Polyethylene terephthalate (PET) with a thickness of 100μ
The surface of the film was coated with a dichromic acid solution (KzCr2(h
50g S? a Sulfuric acid 400ml, water 6Q 0ml
) at room temperature, and then oxidized with a stannous chloride solution (Sn
Cffz 100 g,,HCj250mj! , water Il
), palladium chloride solution (pacx 20.5 g,
Sequentially immersed in 10ml of concentrated hydrochloric acid, 41ml of water, and finally 50ml of water.
It was dried at ℃ for 3 hours and subjected to transition metal treatment.
次に、Ｆｅ（Ｃｏ）ｓのトルエン５重世％溶液に上記処
理したＰＥＴフィルムを浸漬し、６０℃で３０分間加熱
した。この結果、該フィルムに分解したＦｅの超微粒子
が担持された。次いで、このフィルムをγ−アミノプロ
ピルトリエトキシシランのトルエン１重量％溶液に浸漬
し、８０℃で１時間加熱して担持Ｆｅの酸化防止処理を
行なった。Next, the above-treated PET film was immersed in a 5% solution of Fe(Co)s in toluene and heated at 60° C. for 30 minutes. As a result, ultrafine particles of decomposed Fe were supported on the film. Next, this film was immersed in a 1% by weight solution of γ-aminopropyltriethoxysilane in toluene and heated at 80° C. for 1 hour to prevent the supported Fe from oxidizing.
電子顕微鏡による表面の形態観察により、ＰＥＴフィル
ム表面に平均粒径０．０８μの球状超微粒子Ｆｅが均一
に分散して担持されていたのが判明した。Observation of the surface morphology using an electron microscope revealed that spherical ultrafine particles Fe with an average particle size of 0.08 μm were uniformly dispersed and supported on the PET film surface.
得られた担持ＰＥＴフィルムについて、振動試料型磁力
計により磁気特性を測定した。その結果は第１表の通り
。The magnetic properties of the obtained supported PET film were measured using a vibrating sample magnetometer. The results are shown in Table 1.
実施例２
実施例１において、ＰＥＴフィルムの代わりに炭素繊維
を用いた以外は実施例１と同様にして酸化防止処理まで
済ませた超微粒Ｆｅ担持炭素繊維を得た。Example 2 Ultrafine Fe-supported carbon fibers were obtained in the same manner as in Example 1 except that carbon fibers were used instead of the PET film, including the antioxidant treatment.
このものの電子顕微鏡観察により、炭素繊維表面に平均
粒径０．１μの球状超微粒子Ｆｅが均一に分散して担持
されていたのが判明した。Electron microscopic observation of this material revealed that spherical ultrafine particles Fe with an average particle size of 0.1 μm were uniformly dispersed and supported on the carbon fiber surface.
また、このものの磁気特性は第１表の通りであった。The magnetic properties of this product were as shown in Table 1.
比較例１
実施例１において、遷移金属塩処理を行なっていないＰ
ＥＴフィルムを用いた以外は実施例１と同様にしてＦｅ
（Ｃｏ） ｓの接触反応を行なった。Comparative Example 1 P that was not subjected to transition metal salt treatment in Example 1
Fe was prepared in the same manner as in Example 1 except that the ET film was used.
A catalytic reaction of (Co)s was carried out.
結果は、該フィルム表面に分解Ｆｅは認められなかった
。As a result, no decomposed Fe was observed on the surface of the film.
比較例２
実施例ＩのＦｅ （ＣＯ） ｓの接触反応において、分
解温度を１３０℃に変更した外は、実施例１と同様に実
施した。Comparative Example 2 The same procedure as in Example 1 was carried out except that the decomposition temperature in the catalytic reaction of Fe (CO) s in Example I was changed to 130°C.
この結果、ＰＥＴフィルム表面および該フィルム表面以
外の反応器壁にも分解Ｆｅが生成した。As a result, decomposed Fe was generated on the PET film surface and on the reactor wall other than the film surface.
ＰＥＴフィルム表面の分解Ｆｅは、平均粒径０．８μの
球状微粒子であった。また、このものの磁気特性は第１
表の通りであった。The decomposed Fe on the surface of the PET film was spherical fine particles with an average particle size of 0.8 μm. Also, the magnetic properties of this material are the first
It was as shown in the table.
第１表Table 1
Claims (1)
カルボニル化合物を１２０℃以下で接触し、反応させて
平均粒径０．２ミクロン以下の金属粒子を該高分子材料
の表面に分散付着させることを特徴とする超微粒金属で
被覆した材料の製造方法。A transition metal salt and a transition metal carbonyl compound are brought into contact with each other at a temperature of 120°C or lower on the surface of a polymeric material, and the metal particles having an average particle size of 0.2 microns or less are dispersed and adhered to the surface of the polymeric material. A method for producing a material coated with a characteristic ultrafine metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15072486A JPS637378A (en) | 1986-06-27 | 1986-06-27 | Production of material coated with hyperfine particle metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15072486A JPS637378A (en) | 1986-06-27 | 1986-06-27 | Production of material coated with hyperfine particle metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS637378A true JPS637378A (en) | 1988-01-13 |
Family
ID=15503022
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15072486A Pending JPS637378A (en) | 1986-06-27 | 1986-06-27 | Production of material coated with hyperfine particle metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS637378A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5599083A (en) * | 1993-12-17 | 1997-02-04 | Mort; Christopher H. J. | Projection apparatus |
| JP2008524010A (en) * | 2004-12-17 | 2008-07-10 | インテグラン・テクノロジーズ・インコーポレーテッド | Articles containing fine-grained metal and polymer materials |
-
1986
- 1986-06-27 JP JP15072486A patent/JPS637378A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5599083A (en) * | 1993-12-17 | 1997-02-04 | Mort; Christopher H. J. | Projection apparatus |
| JP2008524010A (en) * | 2004-12-17 | 2008-07-10 | インテグラン・テクノロジーズ・インコーポレーテッド | Articles containing fine-grained metal and polymer materials |
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