JPH0463135A - Liquid phase synthesis of ceramics - Google Patents
Liquid phase synthesis of ceramicsInfo
- Publication number
- JPH0463135A JPH0463135A JP2169869A JP16986990A JPH0463135A JP H0463135 A JPH0463135 A JP H0463135A JP 2169869 A JP2169869 A JP 2169869A JP 16986990 A JP16986990 A JP 16986990A JP H0463135 A JPH0463135 A JP H0463135A
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- ceramic
- laser light
- source material
- phase synthesis
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 239000007791 liquid phase Substances 0.000 title abstract description 10
- 230000015572 biosynthetic process Effects 0.000 title description 7
- 238000003786 synthesis reaction Methods 0.000 title description 7
- 239000000843 powder Substances 0.000 claims abstract description 46
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 230000001678 irradiating effect Effects 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract 5
- 239000010453 quartz Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000012808 vapor phase Substances 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 238000001308 synthesis method Methods 0.000 description 6
- 229910052755 nonmetal Inorganic materials 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 150000004703 alkoxides Chemical class 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000010923 batch production Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、紫外レーザ光を液相状態にあるセラミック
ス原料に照射して、セラミックス微粉体を製造する方法
に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing ceramic fine powder by irradiating a ceramic raw material in a liquid phase with ultraviolet laser light.
従来のセラミックス微粉体の製造技術は気相合成法と液
相合成法に大別される。気相合成法は金属あるいは非金
属蒸気と反応ガスから気相でセラミックス微粉体を製造
する方法であり、ガス中蒸発法、狭義の気相合成法、気
相酸化法等がある。Conventional techniques for producing fine ceramic powder are broadly divided into vapor phase synthesis and liquid phase synthesis. The vapor phase synthesis method is a method for producing ceramic fine powder in the vapor phase from metal or nonmetal vapor and a reaction gas, and includes evaporation in gas, vapor phase synthesis in a narrow sense, vapor phase oxidation, and the like.
気相合成法の１つであるガス中蒸発法においては、密閉
系の反応装置内部と１０−’ ｌ−−ル以下の高真空に
排気したのち、不活性ガスと酸素、窒素またはアンモニ
ア、メタン系炭化水素等の反応ガスを数十トール導入す
る。そして、あらかじめ反応装置内にセットされた金属
あるいは非金属原料と加熱蒸発させて、反応ガスと反応
させ、微粉体を製造する。この方法によりＺｎＯ１Ａｆ
Ｎ、Ｓｉ：＋Ｎ４、ＢＮ、ＴｉＣ等の微粉セラミックス
が得られる。狭義の気相合成法は、あらかじめ密閉反応
装置内部にセットされた揮発しやすい金属塩化物、水素
化物等を加熱蒸発させ、装置内部に導入された反応ガス
を反応させて微粉体を得る方法である。気相酸化法は揮
発物の塩化物（ＡｊＩＣｆ３、Ｓ ｉ Ｃｌ ａ、Ｔ
ｉ Ｃｌ ａ、ＦｅＣ１ｘ等）の蒸気を酸素で酸化する
ことによって１！、０．、Ｓｔｏｗ、Ｔ ｉ Ｏｚ、Ｆ
ｅｚＯ＝等の微粉体を得る方法である（「粉体と工業」
１９８５年１０月号、Ｐ２５〜３２、（社）日本粉体工
業技術協会編）。In the gas-in-gas evaporation method, which is one of the gas phase synthesis methods, the inside of a closed system reactor is evacuated to a high vacuum of 10-' L or less, and then an inert gas and oxygen, nitrogen or ammonia, or methane are evacuated. Several tens of torr of reactive gas such as hydrocarbons is introduced. Then, it is heated and evaporated with a metal or non-metal raw material set in a reactor in advance and reacted with a reaction gas to produce a fine powder. By this method, ZnO1Af
Fine powder ceramics such as N, Si: +N4, BN, TiC, etc. are obtained. Gas phase synthesis in a narrow sense is a method of heating and evaporating volatile metal chlorides, hydrides, etc. that have been placed inside a closed reaction device in advance, and reacting with the reaction gas introduced into the device to obtain fine powder. be. The gas phase oxidation method uses volatile chlorides (AjICf3, S i Cl a, T
1! by oxidizing the vapor of iCl a, FeC1x, etc.) with oxygen. , 0. , Stow, T i Oz, F.
This is a method to obtain fine powder such as ezO= ("Powder and Industry"
October 1985 issue, pages 25-32, edited by Japan Powder Technology Association).
気相合成法による微粉体製造は、いずれの方法でも金属
あるいは非金属原料を１０００°Ｃ以上もの高温で蒸発
させ、反応ガスと反応させる必要がある。Regardless of the method used to produce fine powder by vapor phase synthesis, it is necessary to evaporate a metal or nonmetal raw material at a high temperature of 1000° C. or higher and react it with a reaction gas.
加熱熱源の種類により分類すると、主なものとして燃焼
プロセス、プラズマプロセス、レーザプロセス、電気炉
加熱プロセスがある。When classified by type of heating heat source, the main ones are combustion process, plasma process, laser process, and electric furnace heating process.
一方、液相合成法には液相において金属アルコキシドの
加水分解によって微粉体を製造するアルコキシド法があ
る（「化学装置」、１９８８年１１月号、Ｐ２４〜２９
）。On the other hand, among the liquid phase synthesis methods, there is an alkoxide method in which fine powder is produced by hydrolysis of metal alkoxide in the liquid phase ("Kagaku Kippatsu", November 1988 issue, pp. 24-29).
).
気相合成法においては、加熱プロセスの違いによって粉
体製造条件は大きく異なるが、すべての方法において粉
体製造に先立ち、金属あるいは非金属原料を密閉反応装
置を開放して反応装置内にバッチ的にセラする必要があ
る。これはプロセスの工業化上、装置の大型化あるいは
製品の大量製造、コストダウン等に対して重大な欠点と
なる。In the gas phase synthesis method, the powder production conditions differ greatly depending on the heating process, but in all methods, prior to powder production, metal or nonmetal raw materials are placed in a batchwise manner in a closed reactor by opening the reactor. It is necessary to clean it up. This is a serious drawback when it comes to industrializing the process, increasing the size of equipment, mass manufacturing products, and reducing costs.
さらに揮発性化合物は大気中で不安定であり、生成する
微粉体は金属あるいは非金属の加熱温度、反応混合ガス
のガス圧、流速等に強く影響される。Further, volatile compounds are unstable in the atmosphere, and the fine powder produced is strongly influenced by the heating temperature of the metal or nonmetal, the gas pressure of the reaction mixture, the flow rate, etc.
一方、液相合成法の場合には、炭化物、窒化物などの微
粉体は高温のプロセスを必要とするためアルコキシド法
では製造できない。また、液相アルコキシド法も気相合
成法と同様、微粉体の製造過程はバッチプロセスである
。On the other hand, in the case of liquid phase synthesis, fine powders such as carbides and nitrides cannot be produced using the alkoxide method because they require high-temperature processes. Further, in the liquid phase alkoxide method as well as in the gas phase synthesis method, the manufacturing process of fine powder is a batch process.
この発明は上記のような問題点を解決するためになされ
たもので、セラミック微粉体を連続的に大量に製造でき
るとともに同一反応状態を維持して均質なセラミック微
粉体を容易に製造できる方法を提供することを目的とし
ている。This invention was made in order to solve the above-mentioned problems, and provides a method that can continuously produce large quantities of ceramic fine powder and maintain the same reaction state to easily produce homogeneous ceramic fine powder. is intended to provide.
〔課題を解決するための手段］
上記課題は、溶媒中に溶解状態にあるセラミックス原料
に紫外レーザ光を照射することを特徴とするセラミック
ス微粉体製造方法によって解決される。[Means for Solving the Problems] The above problems are solved by a ceramic fine powder production method characterized by irradiating a ceramic raw material dissolved in a solvent with an ultraviolet laser beam.
セラミックス原料は紫外レーザ光透過性の溶媒に可溶の
ものである。このセラミックス原料には、セラミック微
粉末が、シリカの場合には各種シリケート類、例えばテ
トラエチルシリケー）（Ｓｉ（ｏｃ２ｕｓ）４） 、酸
化ケイ系（ＳｉＯ２）、サイアロン（ＳｉＡｊ！ＯＮ）
、シリカ等を使用することができる。The ceramic raw material is soluble in a solvent that transmits ultraviolet laser light. This ceramic raw material includes fine ceramic powder, and in the case of silica, various silicates, such as tetraethyl silicate (Si(oc2us)4), silicon oxide (SiO2), and sialon (SiAj!ON).
, silica, etc. can be used.
セラミック微粉末がアルミナの場合には、セラミックス
原料としてアルミナ等を使用することができる。セラミ
ック微粉末が酸化アルミニウム（ＡｆｆｉＺ０３）又は
粉末混合試料としてＡ ｌ ｚＯｓ Ｗ（ｈ等を使用
することができる。When the ceramic fine powder is alumina, alumina or the like can be used as the ceramic raw material. The ceramic fine powder can be aluminum oxide (AffiZ03) or the powder mixture sample can be Al zOs W (h, etc.).
溶媒は紫外レーザ光透過性で、かつ前記セラミックス原
料を溶解しうるものが選択される。例えば、メタノール
、ヘキサン、エーテル、シクロヘキサンを使用でき、テ
トラエチルシリケートにはメタノールやエーテル、Ａｆ
、Ｏ，にはメタノール、ヘキサン、シクロヘキサン等を
使用できる。The solvent is selected to be transparent to ultraviolet laser light and capable of dissolving the ceramic raw material. For example, methanol, hexane, ether, cyclohexane can be used, and tetraethyl silicate has methanol, ether, Af
, O, may be methanol, hexane, cyclohexane, or the like.
セラミックス原料は常法により溶媒に溶解すればよく、
例えば撹拌、加熱等の手段を利用できる。Ceramic raw materials can be dissolved in a solvent using a conventional method.
For example, means such as stirring and heating can be used.
濃度は限定されない。The concentration is not limited.
使用するレーザ光は、ＡｒＦ、ＫｒＦ、ＸｅＣｌ１等の
レーザガスを使用する紫外レーザ光（エキシマレーザ）
が適している。The laser beam used is an ultraviolet laser beam (excimer laser) that uses laser gas such as ArF, KrF, and XeCl1.
is suitable.
レーザ光照射中に酸素、窒素またはアンモニア、メタン
系炭化水素等の反応ガスをセラミック原料と伴に同時に
反応器に供給してもよい。ガスを供給、すなわち、ガス
を調整することにより、酸化物あるいは窒化物セラミッ
クスが得られやすくなる。特に、生じる酸化物などは酸
化の程度が最も進んだ構造のものとなる。During the laser beam irradiation, a reactive gas such as oxygen, nitrogen, ammonia, or methane-based hydrocarbons may be simultaneously supplied to the reactor together with the ceramic raw material. By supplying the gas, that is, adjusting the gas, oxide or nitride ceramics can be easily obtained. In particular, the oxides and the like that are produced have a structure in which the degree of oxidation is the most advanced.
本発明による製造プロセスの一例の概要を第１図に示す
。FIG. 1 shows an outline of an example of the manufacturing process according to the present invention.
石英ガラス製等の紫外レーザ光に対して、透明な反応器
２に紫外レーザ光源４からのレーザ光を外部から照射す
る。当該反応器２に液相溶解状態のセラミックス原料を
原料供給部１から連続的に供給し、レーザ光によりそこ
で微粉体を製造する。A transparent reactor 2 made of quartz glass or the like is irradiated with laser light from an ultraviolet laser light source 4 from the outside. Ceramic raw materials in a liquid-phase dissolved state are continuously supplied to the reactor 2 from the raw material supply section 1, and fine powder is manufactured there using laser light.
製造された微粉体は溶媒とともに反応器３から流出し、
遠心濾過等の固液分離器３によって回収される。固液分
離器３で分離された未反応の原料液は原料供給部１にリ
サイクルされる。生成する微粉体の粒径等は照射する紫
外レーザ光の光強度、照射時間、レーザ光波長などをコ
ントロールすることにより、制御することが可能である
。微粉体の製造条件としては、反応温度：常温〜３００
°Ｃ１反応圧カニ常圧、レーザ出カニ１００〜３００
（ｍＪ／パルス〕、レーザ発振数：５〜１００〔Ｈ２〕
、レーザ光照射時間：ｌ〜６０ （＋５ｉｎ）などの条
件が望ましい。The produced fine powder flows out from the reactor 3 together with the solvent,
It is recovered by a solid-liquid separator 3 such as centrifugal filtration. The unreacted raw material liquid separated by the solid-liquid separator 3 is recycled to the raw material supply section 1. The particle size etc. of the fine powder to be produced can be controlled by controlling the light intensity, irradiation time, laser light wavelength, etc. of the ultraviolet laser light to be irradiated. The manufacturing conditions for the fine powder include reaction temperature: room temperature to 300°C.
°C1 reaction pressure normal pressure, laser output crab 100-300
(mJ/pulse), number of laser oscillations: 5 to 100 [H2]
, laser beam irradiation time: 1 to 60 (+5 inches).
尚、本発明の方法はバッチ方式にて実施することも可能
であることはいうまでもない。It goes without saying that the method of the present invention can also be carried out in a batch manner.
本発明の方法で得られるセラミック微粉体は粒径が２〜
１０ｎ程度、特に３〜５ｉ！ｍ程度にすることができ、
しかも均質品を得ることができる。The ceramic fine powder obtained by the method of the present invention has a particle size of 2 to 2
About 10n, especially 3-5i! It can be made about m,
Moreover, a homogeneous product can be obtained.
このセラミックス微粉体の製造方法は、従来の気相合成
法が熱エネルギーによって金属あるいは非金属セラミッ
クス原料を加熱蒸発させ反応させる点に比較し、紫外レ
ーザ光の持つ強力な光量子エネルギーを利用して微粉体
を合成している。This method of producing fine ceramic powder uses the powerful photon energy of ultraviolet laser light to produce fine powder, unlike the conventional vapor phase synthesis method, which uses thermal energy to heat and evaporate metal or non-metallic ceramic raw materials to react. Synthesizing the body.
液相状態にあるセラミックス原料を１００″Ｃ前後に加
熱し紫外レーザ光を照射することで紫外レーザ光の非常
に強い量子エネルギーを得て、例えば５ｔ−Ｈなどの結
合が切断され微粉末を得ることができる。By heating the ceramic raw material in the liquid phase to around 100"C and irradiating it with ultraviolet laser light, the extremely strong quantum energy of the ultraviolet laser light is obtained, and bonds such as 5t-H are severed to obtain fine powder. be able to.
第１図に示す装置を用いた。 The apparatus shown in FIG. 1 was used.
フッ化水素酸７０〜９０容量部とクロロベンゼン３０〜
１０容量部の混合液１００重量部を溶媒として、シリカ
１０重量部およびアルミナ１０重量部をセラミックス原
料として溶解させた原料液に、ＫｒＦレーザ（レーザ光
波長２４８ｎ■）を照射し、シリカを主成分としたセラ
ミックス微粉体を製造した。実験条件を以下に示す。70-90 parts by volume of hydrofluoric acid and 30-90 parts by volume of chlorobenzene
A raw material solution prepared by dissolving 10 parts by weight of a mixed solution of 10 parts by volume as a solvent and 10 parts by weight of silica and 10 parts by weight of alumina as ceramic raw materials is irradiated with a KrF laser (laser light wavelength 248 nm) to dissolve silica as the main component. A fine ceramic powder was produced. The experimental conditions are shown below.
実験条件
反応器２は紫外レーザ光に対して透明な石英ガラス製反
応器を使用した。Experimental Conditions Reactor 2 was a quartz glass reactor transparent to ultraviolet laser light.
実験結果
セラミック微粉体組成（％）
第２図にレーザ光発振数と微粉体生成量、第３図に反応
器加熱温度と微粉体生成量の関係、そして第４図に微粉
体の粒径分布を示す。Experimental results Ceramic fine powder composition (%) Figure 2 shows the relationship between the number of laser beam oscillations and the amount of fine powder produced, Figure 3 shows the relationship between the reactor heating temperature and the amount of fine powder produced, and Figure 4 shows the particle size distribution of the fine powder. shows.
尚、第２図の記号は下記の条件を示している。Note that the symbols in FIG. 2 indicate the following conditions.
〔発明の効果］
以上のように、この発明によれば均質なセラミックス微
粉体を大量に連続的に製造することができる。[Effects of the Invention] As described above, according to the present invention, homogeneous ceramic fine powder can be continuously produced in large quantities.
第１図は本発明の方法の実施に利用される装置の一例を
ブロックフローダイヤグラムで表わしたものである。第
２図、第３図は実施例による微粉末生成量とレーザ光発
振数、反応器加熱温度の関係を示したグラフである。第
４図は実施例で製造された微粉体の粒径分布を示したグ
ラフである。FIG. 1 is a block flow diagram illustrating an example of an apparatus utilized in carrying out the method of the present invention. FIGS. 2 and 3 are graphs showing the relationship between the amount of fine powder produced, the number of laser beam oscillations, and the reactor heating temperature according to Examples. FIG. 4 is a graph showing the particle size distribution of the fine powder produced in Examples.
Claims (2)
レーザ光を照射することを特徴とするセラミックス微粉
体製造方法。(1) A method for producing fine ceramic powder, which comprises irradiating a ceramic raw material dissolved in a solvent with ultraviolet laser light.
のセラミックス原料を連続的に供給することを特徴とす
る請求項（１）記載のセラミックス微粉体製造方法。(2) The method for manufacturing fine ceramic powder according to claim (1), characterized in that the ceramic raw material in a molten state is continuously supplied to a manufacturing device that is irradiating ultraviolet laser light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2169869A JPH0463135A (en) | 1990-06-29 | 1990-06-29 | Liquid phase synthesis of ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2169869A JPH0463135A (en) | 1990-06-29 | 1990-06-29 | Liquid phase synthesis of ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0463135A true JPH0463135A (en) | 1992-02-28 |
Family
ID=15894462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2169869A Pending JPH0463135A (en) | 1990-06-29 | 1990-06-29 | Liquid phase synthesis of ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0463135A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005049213A1 (en) * | 2003-11-20 | 2005-06-02 | Hamamatsu Photonics K.K. | Microparticle, process for producing microparticle and production apparatus |
-
1990
- 1990-06-29 JP JP2169869A patent/JPH0463135A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005049213A1 (en) * | 2003-11-20 | 2005-06-02 | Hamamatsu Photonics K.K. | Microparticle, process for producing microparticle and production apparatus |
| JPWO2005049213A1 (en) * | 2003-11-20 | 2007-11-29 | 浜松ホトニクス株式会社 | Fine particles, method for producing fine particles, and production apparatus |
| CN100423847C (en) * | 2003-11-20 | 2008-10-08 | 浜松光子学株式会社 | Microparticle, process for producing microparticle and production apparatus |
| JP4545690B2 (en) * | 2003-11-20 | 2010-09-15 | 浜松ホトニクス株式会社 | Fine particle production method and production apparatus |
| US7938344B2 (en) | 2003-11-20 | 2011-05-10 | Hamamatsu Photonics K.K. | Microparticles, microparticle production method, and microparticle production apparatus |
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