JPS6326302A - Production of ultrafine powder - Google Patents
Production of ultrafine powderInfo
- Publication number
- JPS6326302A JPS6326302A JP17049986A JP17049986A JPS6326302A JP S6326302 A JPS6326302 A JP S6326302A JP 17049986 A JP17049986 A JP 17049986A JP 17049986 A JP17049986 A JP 17049986A JP S6326302 A JPS6326302 A JP S6326302A
- Authority
- JP
- Japan
- Prior art keywords
- water
- high polymer
- metal
- polymer layer
- metal powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 59
- 239000002184 metal Substances 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229920000642 polymer Polymers 0.000 claims abstract description 36
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 238000007740 vapor deposition Methods 0.000 claims abstract description 5
- 238000010298 pulverizing process Methods 0.000 claims abstract 2
- 238000000151 deposition Methods 0.000 claims 1
- 239000003292 glue Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- 229920006267 polyester film Polymers 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 238000001694 spray drying Methods 0.000 abstract description 2
- 238000001771 vacuum deposition Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 11
- 239000003973 paint Substances 0.000 description 7
- 229910001111 Fine metal Inorganic materials 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】 βし猶−ヒの一利２用−分−野 本発明は、超微細金属粉の製造方法乙こ関する。[Detailed description of the invention] Field of use and use of β The present invention relates to a method for producing ultrafine metal powder.
接法ａｖ １１．４扛
微細金属粉の製造方法として、従来、機械的粉砕法、還
元法、噴霧法、粒状化法、電解法等が知られているが、
いずれの方法によっても、平均粒径数十μｍ程度の金属
粉が得られるにすぎず、平均粒径数μＩＴＩ程度又はそ
れ以下の超微細な金属粉を得ることができない。Contact method av 11.4 Mechanical crushing method, reduction method, spraying method, granulation method, electrolytic method, etc. are conventionally known as methods for producing fine metal powder.
With either method, metal powder with an average particle diameter of only about several tens of micrometers can be obtained, and it is not possible to obtain ultrafine metal powder with an average particle diameter of about several micrometers ITI or less.
近年、金属粉を含有する導電性塗料が提案されているが
、」二記のように、従来より知られている金属粉は粒径
が大きいために、ビヒクルに才３シ〕ろ分散性に劣ると
共に、ビヒクルにおりる配合量にも限界があり、更に、
塗料中において金属粉が速やかに沈降し、また、塗膜を
形成した後も、金属粉がビヒクルから分画沈降するので
、高性能の導電性塗膜を形成し難い。In recent years, conductive paints containing metal powders have been proposed, but as mentioned in 2.2, conventionally known metal powders have large particle sizes, making it difficult for vehicles to disperse them. In addition to being inferior, there is a limit to the amount that can be added to the vehicle, and furthermore,
The metal powder quickly settles in the paint, and even after the coating film is formed, the metal powder precipitates fractionally from the vehicle, making it difficult to form a high-performance conductive coating film.
発所麦邂訣夷よｊ堵４に澗遣４に
本発明は、従来の微細金属粉における上記した問題を解
決するためになされたものであって、平均粒径が数μｍ
程度又はそれ以下である超微細金属粉を製造する方法を
提供することを目的とし、特に、粒径が超微細であり、
■つ、分散性にずくれるために、ビヒクル中においても
沈降せず、従って、導電性塗料の製造に好適に用いるこ
とができる超微細金属粉を容易安全且つ低度に製造する
方法を提供することを目的とする。SUMMARY OF THE INVENTION The present invention was made to solve the above-mentioned problems with conventional fine metal powders, and the present invention has been made to solve the above-mentioned problems with conventional fine metal powders.
The purpose of the present invention is to provide a method for producing ultrafine metal powder having a particle size of about
(2) To provide a method for easily, safely and with low production of ultrafine metal powder, which does not settle even in a vehicle due to poor dispersibility and can therefore be suitably used for producing conductive paints. The purpose is to
肌題尭）邂−決ち一隆Δｑ下役
本発明による超微細金属粉の製造方法は、吸水性高分子
層を有する基材シート上に金属蒸着層を形成して、複合
シートを形成する第１］二程、この複合シートを水中に
浸漬して、上記吸水性高分子層を蒸着金属層と共に基材
シートから剥離させ、同時に又は次いで上記吸水性高分
子を水中に溶解させると共に、金属粉を分離させる第２
工程、及びこの金属粉を捕集する第３工程を含むことを
特徴とする。The method for producing ultrafine metal powder according to the present invention involves forming a metal vapor deposition layer on a base sheet having a water-absorbing polymer layer to form a composite sheet. Step 1] Step 2: The composite sheet is immersed in water to peel off the water-absorbing polymer layer together with the vapor-deposited metal layer from the base sheet, and at the same time or subsequently, the water-absorbing polymer layer is dissolved in water, and the metal The second to separate the powder
and a third step of collecting the metal powder.
本発明において、基材シートは、特に限定されるもので
はないが、通常、合成樹脂製のフィルム又はシートが好
適である。かかる基材シートの具体例として、例えば、
ポリエステルフィルムを挙げることができる・
第１工程においては、吸水性高分子層を有するかかる基
材シート上に金属蒸着層を形成して、複合シートを形成
する。即ち、基材シートの片面又は両面に吸水性高分子
を含む糊剤を塗布し、乾燥した後、その上に金属を真空
蒸着させるのである。In the present invention, the base sheet is not particularly limited, but a synthetic resin film or sheet is usually suitable. Specific examples of such base sheets include, for example:
Examples include polyester films.In the first step, a metal vapor deposition layer is formed on such a base sheet having a water-absorbing polymer layer to form a composite sheet. That is, a glue containing a water-absorbing polymer is applied to one or both sides of a base sheet, and after drying, a metal is vacuum-deposited thereon.
上記吸水性高分子としては、既に種々のものが知られて
おり、市販されている。本発明においては、かかる市販
されている吸水性高分子を用いることができるが、特に
、吸水性が高く、且つ、水溶解性にずくれる吸水性高分
子が好適に用いられる。Various types of water-absorbing polymers are already known and commercially available. In the present invention, such commercially available water-absorbing polymers can be used, but water-absorbing polymers that have high water absorption and low water solubility are particularly preferably used.
また、上記糊剤としては、例えば、エマルジョン系糊剤
が適当である。糊剤の塗布厚は、吸水性高分子の吸水性
や水溶解性にもよるが、例えば、乾燥後に５〜２０μｍ
程度であるのが好適である。Moreover, as the above-mentioned glue, for example, an emulsion-based glue is suitable. The coating thickness of the glue depends on the water absorbency and water solubility of the water-absorbing polymer, but for example, it is 5 to 20 μm after drying.
It is preferable that the
吸水性高分子層の上に真空蒸着させる金属層の厚めは、
１０μｍ以下が適当であり、好ましくは１００人乃至５
μｍであり、特に、５００人乃至２μｍ程度が好ましい
。蒸着金属としては、例えば、アルミニウム、銅、ニッ
ケル、クロム、チタン、金、銀、亜鉛、鉛、これらの合
金等を挙げることができるが、これらに限定されるもの
ではない。このような金属の真空蒸着によって、吸水性
高分子層上に極めて微細で均一な粒径及び粒度分布を有
し、形状及び組成も均一である微細金属粉を蒸着させる
ことができる。蒸着金属層の厚みが余りに厚いときｂよ
、粒径数μｍ程度の超微細な金属粉を得ることが困腑で
ある。The thickness of the metal layer vacuum-deposited on the water-absorbing polymer layer is
Appropriately 10 μm or less, preferably 100 to 5
The thickness is preferably about 500 μm to about 2 μm. Examples of the deposited metal include, but are not limited to, aluminum, copper, nickel, chromium, titanium, gold, silver, zinc, lead, and alloys thereof. By such vacuum vapor deposition of metal, fine metal powder having extremely fine and uniform particle size and particle size distribution, and uniform shape and composition can be deposited on the water-absorbing polymer layer. When the thickness of the deposited metal layer is too thick, it is difficult to obtain ultrafine metal powder with a particle size of several μm.
このようにして、吸水性高分子層の上に金属を蒸着させ
たシートは、次に、第２工程において、水中に浸漬させ
ることによって、水が上記蒸着金属層を透過するためで
あるとみられるが、吸水性高分子層は基材シートから容
易に且つ速やかに剥離し、これと同時に又は通常、速や
かに吸水性高分子が水中で膨潤溶解し、その結果、蒸着
金属層は微粉状に水中に浮遊する。This seems to be because the sheet with the metal vapor-deposited on the water-absorbing polymer layer is then immersed in water in the second step, allowing water to pass through the vapor-deposited metal layer. However, the water-absorbing polymer layer peels off easily and quickly from the base sheet, and at the same time, or usually, the water-absorbing polymer swells and dissolves in water, and as a result, the vapor-deposited metal layer peels off from the base sheet in the form of fine powder. Floating on.
尚、このように、吸水性高分子層の上に金属を蒸着させ
たシー］・を水中に浸漬させ、吸水性高分子層を基材シ
ーＩ・から剥離させる際に、必要に応して、ブラシ等の
適宜の手段にて、蒸着金属層を摩擦し、吸水性高分子層
の基材シートからの剥離と、金属粉の吸水性高分子から
の剥離浮遊を促進させてもよい。In this way, when immersing the sheet with metal vapor-deposited on the water-absorbing polymer layer in water and peeling off the water-absorbing polymer layer from the base sheet I, if necessary, The vapor-deposited metal layer may be rubbed with an appropriate means such as a brush to promote the separation of the water-absorbing polymer layer from the base sheet and the separation and floating of the metal powder from the water-absorbing polymer.
本発明の方法においては、吸水性高分子層の上に金属を
１着させた後、このシートを速やかに水中に浸漬するの
が好ましい。この場合、蒸着金属は急冷され、吸水性高
分子層上の蒸着金属は極めて微細な球状のままであり、
相互に融着しないので、吸水性高分子が水に溶解したと
き、極めて微細な金属粉を得ることができる。In the method of the present invention, it is preferable to place one layer of metal on the water-absorbing polymer layer and then immediately immerse the sheet in water. In this case, the deposited metal is rapidly cooled, and the deposited metal on the water-absorbing polymer layer remains in an extremely fine spherical shape.
Since they do not fuse with each other, extremely fine metal powder can be obtained when the water-absorbing polymer is dissolved in water.
本発明の方法によれば、第３工程として、水中に浮遊す
る金属粉を濾過、遠心沈降等の方法にて水から分離し、
ケーキとした後、所要量の酸化防止剤と分散剤を含有す
る水中に上記金属粉を再び分散浮遊させ、湿式粉砕した
後、噴霧乾燥すれば、本発明による超微細金属粉を得る
ことができる。According to the method of the present invention, as the third step, metal powder floating in the water is separated from the water by a method such as filtration or centrifugal sedimentation,
After forming a cake, the metal powder is dispersed and suspended again in water containing the required amount of antioxidant and dispersant, wet-pulverized, and then spray-dried to obtain the ultrafine metal powder according to the present invention. .
但し、金属粉を捕集した後の乾燥方法は、噴霧乾燥に限
定されるものではない。However, the drying method after collecting the metal powder is not limited to spray drying.
本発明の方法は、ハツチ式にても連続式にても実施する
ことができる。例えば、連続した長尺の基材シートを用
いて、連続的にこれに糊剤を塗布乾燥し、引き続いてそ
の上に金属を真空蒸着し、次いで、水中に浸漬すれば、
超微細金属粉を得ることができる。The method of the invention can be carried out in a hatched or continuous manner. For example, if a continuous long base material sheet is used, a glue is continuously applied to it and dried, then a metal is vacuum-deposited thereon, and then immersed in water.
Ultrafine metal powder can be obtained.
対（２）処理
本発明の方法によって得られる金属粉は、吸水性高分子
層上に真空蒸着にて超微細な金属粉からなる層を形成さ
せた後、上記吸水性高分子層を溶解させ、上記蒸着金属
を微粉状に分離させる。従って、このようにして得られ
る金属粉は、極めて微細であって、平均粒径が数μｍで
あり、粒度分布も著しく狭く、しかも、球形に近い形状
を有し、そのため、二次凝集も少ない。Pair (2) Processing The metal powder obtained by the method of the present invention is obtained by forming a layer of ultrafine metal powder on a water-absorbing polymer layer by vacuum evaporation, and then dissolving the water-absorbing polymer layer. , the vapor-deposited metal is separated into fine powder. Therefore, the metal powder obtained in this way is extremely fine, with an average particle size of several micrometers, a significantly narrow particle size distribution, and a nearly spherical shape, and therefore has little secondary agglomeration. .
従って、本発明による超微細金属粉は、例えば、ビヒク
ル中における分散性にすくれ、また、ビヒクル中に多量
に分散させるごとができるので、導電性塗料に用いるの
に好適である。例えば、従来、ニッケル粉末を含有する
導電性塗料が用いられており、これによれば、膜厚３０
μｍ以上の塗膜によって導電性を達成しているが、本発
明による超微細金属粉を含む導電性塗料によれば、通常
、１０μｍ以下の乾燥膜厚にてずくれた導電性を有する
導電性塗料を得ることができる。Therefore, the ultrafine metal powder according to the present invention has excellent dispersibility in a vehicle, and can be dispersed in a large amount in a vehicle, so that it is suitable for use in conductive paints. For example, conventionally, conductive paint containing nickel powder has been used, and according to this, the film thickness is 30
Conductivity is achieved by a coating film with a thickness of 10 μm or more, but the conductive paint containing ultrafine metal powder according to the present invention usually has a conductivity with a dry film thickness of 10 μm or less. You can get paint.
また、本発明の方法は、従来の方法に比べて簡単であり
ながら、従来、困難であった粒径数μｍ程度の超微細金
属粉を容易に且つ低度に得ることができ、しかも、処理
の多くは水の存在下に行なわれるので、金属粉の酸化を
防止することができると共に、発火や爆発の危険がなく
、安全性にずくれる。更に、基材シートは繰り返して用
いることができる。In addition, although the method of the present invention is simpler than conventional methods, it is possible to easily obtain ultrafine metal powder with a particle size of several μm, which has been difficult in the past. Since most of the process is carried out in the presence of water, it is possible to prevent the metal powder from oxidizing, and there is no risk of fire or explosion, which improves safety. Furthermore, the base sheet can be used repeatedly.
去１副寸
以下に実施例を挙げて本発明を説明するが、本発明はこ
れら実施例により何ら限定されるものではない。The present invention will be described below with reference to Examples, but the present invention is not limited to these Examples in any way.
幅１ｍ、厚み１２μｍのポリエステルフィルム上にグラ
ビア印刷機にて吸水性高分子を含む糊剤を乾燥厚み１０
μｍに塗布し、１２０°Ｃの温度に加熱乾燥した後、こ
の吸水性高分子層の上に連続式真空蒸着装置を用いて、
アルミニウムを厚み１μｍに真空蒸着さ−Ｕだ。A glue containing a water-absorbing polymer was applied using a gravure printing machine onto a polyester film with a width of 1 m and a thickness of 12 μm to a dry thickness of 10 μm.
μm, and after heating and drying at a temperature of 120°C, a continuous vacuum evaporation device was used on this water-absorbing polymer layer.
Aluminum is vacuum-deposited to a thickness of 1 μm.
このようにして得たシートを水槽に連続的に導き、浸漬
し、基材シートから吸水性高分子層と蒸着金属層を剥離
させ、吸水性高分子を水に熔解させて、水中に浮遊して
いる金属粉を捕集した。The sheet thus obtained is continuously introduced into a water tank and immersed, the water-absorbing polymer layer and the vapor-deposited metal layer are peeled off from the base sheet, and the water-absorbing polymer is dissolved in water so that it floats in the water. metal powder was collected.
酸化防止剤及び分散剤を適宜量を含む水中に上記金属粉
を再び分散させ、ポットミルにて１５分分間式粉砕した
後、脱水乾燥して、平均粒径約２μｍの超微細アルミニ
ウム粉を得た。The metal powder was redispersed in water containing appropriate amounts of antioxidant and dispersant, milled in a pot mill for 15 minutes, and then dehydrated and dried to obtain ultrafine aluminum powder with an average particle size of about 2 μm. .
Claims (3)
層を形成して、複合シートを形成する第１工程、この複
合シートを水中に浸漬して、上記吸水性高分子層を蒸着
金属層と共に基材シートから剥離させ、同時に又は次い
で上記吸水性高分子を水中に溶解させると共に、金属粉
を水中に浮遊させる第２工程、及びこの金属粉を捕集す
る第３工程を含むことを特徴とする超微細金属粉の製造
方法。(1) First step of forming a composite sheet by forming a metal vapor deposition layer on a base sheet having a water-absorbing polymer layer, immersing this composite sheet in water and vapor-depositing the water-absorbing polymer layer. A second step of peeling the metal layer together with the base sheet, simultaneously or subsequently dissolving the water-absorbing polymer in water, and suspending the metal powder in the water; and a third step of collecting the metal powder. A method for producing ultrafine metal powder characterized by:
特許請求の範囲第１項記載の超微細金属粉の製造方法。(2) The method for producing ultrafine metal powder according to claim 1, which comprises wet-pulverizing the collected metal powder.
ことを特徴とする特許請求の範囲第１項記載の超微細金
属粉の製造方法。(3) The method for producing ultrafine metal powder according to claim 1, wherein the collected metal powder is wet-pulverized and then spray-dried.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17049986A JPS6326302A (en) | 1986-07-18 | 1986-07-18 | Production of ultrafine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17049986A JPS6326302A (en) | 1986-07-18 | 1986-07-18 | Production of ultrafine powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6326302A true JPS6326302A (en) | 1988-02-03 |
Family
ID=15906091
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17049986A Pending JPS6326302A (en) | 1986-07-18 | 1986-07-18 | Production of ultrafine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6326302A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008063605A (en) * | 2006-09-06 | 2008-03-21 | Ulvac Japan Ltd | Method for forming nanometal particle and nanoorder wiring |
| JP2011156520A (en) * | 2010-02-04 | 2011-08-18 | Sumitomo Metal Mining Co Ltd | Method of classifying metal fine powder |
| JP2014040644A (en) * | 2012-08-23 | 2014-03-06 | Oike Ind Co Ltd | Method for producing inorganic fine particles |
-
1986
- 1986-07-18 JP JP17049986A patent/JPS6326302A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008063605A (en) * | 2006-09-06 | 2008-03-21 | Ulvac Japan Ltd | Method for forming nanometal particle and nanoorder wiring |
| JP2011156520A (en) * | 2010-02-04 | 2011-08-18 | Sumitomo Metal Mining Co Ltd | Method of classifying metal fine powder |
| JP2014040644A (en) * | 2012-08-23 | 2014-03-06 | Oike Ind Co Ltd | Method for producing inorganic fine particles |
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