JP3496227B2 - Method for producing near-infrared absorbing material powder - Google Patents
Method for producing near-infrared absorbing material powderInfo
- Publication number
- JP3496227B2 JP3496227B2 JP1796593A JP1796593A JP3496227B2 JP 3496227 B2 JP3496227 B2 JP 3496227B2 JP 1796593 A JP1796593 A JP 1796593A JP 1796593 A JP1796593 A JP 1796593A JP 3496227 B2 JP3496227 B2 JP 3496227B2
- Authority
- JP
- Japan
- Prior art keywords
- copper
- absorbing material
- infrared absorbing
- phosphate compound
- cuo
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Disintegrating Or Milling (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は近赤外線吸収材料粉末の
製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing near infrared ray absorbing material powder.
【０００２】[0002]
【従来の技術】従来、物体や画像は肉眼で認識していた
ため、認識しやすい材料とは可視光領域での光を吸収あ
るいは散乱する材料であった。しかし、最近、自動的に
物体や画像を認識する技術が急速に進歩している。そし
て、この画像を認識、読みとるための光源としては、半
導体レーザーが主流になるといわれている。この半導体
レーザーとしては、７００〜１６００ｎｍの波長領域の
ものが、実用化されているが、この波長は近赤外線の領
域であり、肉眼では認識できない。2. Description of the Related Art Conventionally, since an object or an image has been recognized with the naked eye, a material that is easily recognized is a material that absorbs or scatters light in the visible light region. However, recently, a technology for automatically recognizing an object or an image has rapidly advanced. A semiconductor laser is said to become the mainstream as a light source for recognizing and reading this image. As this semiconductor laser, one having a wavelength range of 700 to 1600 nm has been put into practical use, but this wavelength is in the near infrared region and cannot be recognized by the naked eye.
【０００３】可視光を良好に吸収あるいは散乱する物体
や画像でも、必ずしも近赤外光を良好に吸収、散乱する
とはかぎらない。従来の材料では物体や画像がこの近赤
外線領域で認識し難いという課題があった。この課題を
克服する材料として、我々は先に銅含有リン酸化合物が
有効であることを見出している（特願平４−１１５４７
１号）。Even an object or an image which absorbs or scatters visible light well does not always absorb and scatter near infrared light well. The conventional material has a problem that it is difficult to recognize an object or an image in this near infrared region. As a material that overcomes this problem, we have previously found that a copper-containing phosphate compound is effective (Japanese Patent Application No. 4-11547).
No. 1).
【０００４】[0004]
【発明が解決しようとする課題】銅含有リン酸化合物
は、その用途の一例として、粉末にした後、樹脂等と混
練してインク化して使われる。このインクを印刷して使
用する場合、肉眼で認識されずに近赤外線でのみ認識さ
れるような材料が得られれば、種々の新しい用途展開が
期待される。しかし、初めは無色であった粉末が、粉砕
方法によっては微粉砕後に緑味を帯びるという課題があ
った。本発明は、色調を変化させない銅含有リン酸化合
物の粉末の製造方法の提供を目的とする。As an example of its use, a copper-containing phosphate compound is used after being made into powder and then kneaded with a resin or the like to form an ink. When this ink is printed and used, if a material that can be recognized only by near infrared rays without being recognized by the naked eye is obtained, various new applications are expected to develop. However, there was a problem that powder which was initially colorless turned greenish after fine pulverization depending on the pulverization method. An object of the present invention is to provide a method for producing a copper-containing phosphate compound powder that does not change the color tone.
【０００５】[0005]
【課題を解決するための手段】本発明は、銅をＣｕＯ、
リン酸をＰ2 Ｏ5 に換算してＣｕＯ／Ｐ2 Ｏ5 のモル比
が０．０５〜４である銅含有リン酸化合物を、水の存在
下で湿式粉砕し、微粉末化する近赤外線吸収材料粉末の
製造方法、及び、銅をＣｕＯ、リン酸をＰ2 Ｏ5 に換算
してＣｕＯ／Ｐ2 Ｏ5 のモル比が０．０５〜４である銅
含有リン酸化合物を、アルミナを使用しない粉砕機で乾
式粉砕し、微粉末化する近赤外線吸収材料粉末の製造方
法、を提供する。According to the present invention, copper is added to CuO,
NIR molar ratio of CuO / P 2 O 5 in terms of the phosphoric acid P 2 O 5 is a copper-containing phosphoric acid compound is 0.05 to 4, and wet grinding in the presence of water, finely powdered A method for producing an absorbing material powder, and a copper-containing phosphate compound having a CuO / P 2 O 5 molar ratio of 0.05 to 4 in which CuO is CuO and phosphoric acid is P 2 O 5 , and alumina is dry milled in not using pulverizer, a method of manufacturing the near-infrared absorbing material powder to be micronized, that provides.
【０００６】本発明において、銅含有リン酸化合物の銅
は近赤外線を良好に吸収する働きをする。銅をＣｕＯ、
リン酸をＰ2 Ｏ5 に換算してＣｕＯ／Ｐ2 Ｏ5 のモル比
で表して、このモル比が０．０５未満の場合は近赤外線
吸収能力が十分でない。また、銅の濃度が高いほど近赤
外線吸収能力が高くなるが、ＣｕＯ／Ｐ2 Ｏ5 のモル比
が４を超えると銅含有リン酸化合物が不安定になる。In the present invention, copper as the copper-containing phosphate compound functions to favorably absorb near infrared rays. CuO for CuO,
Expressed as molar ratio of CuO / P 2 O 5 in terms of the phosphoric acid P 2 O 5, the molar ratio is is not sufficient near infrared absorption capacity of less than 0.05. Although the higher the concentration of copper near infrared absorbing ability may turn high, copper-containing phosphoric acid compound the molar ratio of CuO / P 2 O 5 is more than 4 becomes unstable.
【０００７】銅含有リン酸化合物としては、特に制限は
ないが、近赤外線吸収能力の高い材料としては、リン酸
銅としてメタリン酸銅、ピロリン酸銅、オルトリン酸
銅、銅アパタイト等がある。これら銅含有リン酸塩は、
結晶水を含むものも知られており、一般的に結晶水を含
む化合物は化学的耐久性の面でやや好ましくないが、用
途により使用できる。また、銅含有リン酸化合物として
は、結晶性化合物に制限されずガラス等の非晶質状態の
ものでも使用できる。The copper-containing phosphate compound is not particularly limited, but examples of materials having a high near-infrared absorbing ability include copper metaphosphate, copper metaphosphate, copper orthophosphate, copper apatite and the like. These copper-containing phosphates,
A compound containing water of crystallization is also known. Generally, a compound containing water of crystallization is somewhat unfavorable in terms of chemical durability, but it can be used depending on the application. Further, the copper-containing phosphate compound is not limited to a crystalline compound, and an amorphous compound such as glass can be used.
【０００８】本発明の近赤外線吸収材料粉末の第１の製
造方法、即ち、銅含有リン酸化合物を湿式で粉砕する場
合、水の存在下で湿式粉砕する必要がある。例えば、エ
タノールなどの有機溶媒を用いて粉砕すると、水の存在
下で粉砕した場合に比べて粉末の緑味が強くなる。In the first method for producing the near-infrared absorbing material powder of the present invention, that is, when the copper-containing phosphate compound is wet-milled, it is necessary to wet-mill in the presence of water. For example, when pulverized with an organic solvent such as ethanol, the greenness of the powder becomes stronger than when pulverized in the presence of water.
【０００９】この銅含有リン酸化合物を水を用いて微粉
末化する場合、特に１０μｍ以下の平均粒径に微粉末化
する場合、粉砕機の材質には特に制限はなく、アルミナ
製ボールミル、ジルコニア製ボールミル、樹脂製ボール
ミル、めのう製遊星ミル、各種アクアマイザーなどを、
目標とする微粉末の粒径に応じて適宜使用することがで
きる。When the copper-containing phosphate compound is pulverized with water, particularly when pulverized to an average particle size of 10 μm or less, the material of the crusher is not particularly limited, and a ball mill made of alumina or zirconia is used. Made ball mill, resin ball mill, agate planet mill, various aquamizer, etc.
It can be appropriately used depending on the target particle size of the fine powder.
【００１０】本発明の近赤外線吸収材料粉末の第２の製
造方法、即ち、銅含有リン酸化合物を乾式で粉砕する場
合、特に１０μｍ以下の平均粒径に微粉末化する場合、
アルミナを使用しない粉砕機で微粉末化し、アルミナ混
入によるコンタミネーションを防ぐ必要がある。アルミ
ナ製のボールミルを用いて粉砕した場合は、微粉末化後
に緑色になる。アルミナを使用しない粉砕機として、ジ
ルコニア製ボールミル、めのう製遊星ミル、流動層式カ
ウンタージェットミルなどが例示される。The second method for producing the near-infrared ray absorbing material powder of the present invention, that is, when the copper-containing phosphate compound is pulverized by a dry method, particularly when pulverized to an average particle size of 10 μm or less,
It is necessary to pulverize with a crusher that does not use alumina to prevent contamination due to alumina mixing. If ground using an alumina ball mill, ing green after micronization. Examples of the crusher that does not use alumina include a zirconia ball mill, an agate planetary mill, and a fluidized bed counter jet mill.
【００１１】かくして得られた近赤外線吸収材料粉末
は、例えば樹脂等と混練してインクにし、このインクに
より物体に所定の文字、パターン等を印刷する。この文
字、パターンを半導体レーザーで認識する。当然、この
文字、パターンは無色であるため肉眼では認識すること
ができない。The near-infrared absorbing material powder thus obtained is kneaded with, for example, a resin or the like to form an ink, and a predetermined character, pattern or the like is printed on an object with this ink. The letters and patterns are recognized by the semiconductor laser. Naturally, these characters and patterns are colorless and cannot be recognized with the naked eye.
【００１２】[0012]
【実施例】［実施例１］
ＣｕＯ粉末とオルトリン酸とを、ＣｕＯ／Ｐ2 Ｏ5 のモ
ル比が２になるように調合し、２００℃以上の温度で熱
処理し、銅含有リン酸化合物を準備した。この銅含有リ
ン酸化合物３００ｇとイオン交換水３００ｃｃとを２リ
ットル容量のアルミナ製ボールミルに入れ、これを４０
時間、１００ｒｐｍで回転し、湿式粉砕し、スラリーを
得た。得られたスラリーをポリテトラフルオロエチレン
製バットに入れ、乾燥機で１５０℃で１２時間乾燥して
微粉末を得た。得られた粉末の平均粒径は２．８μｍ、
色調は白色であった。EXAMPLES Example 1 CuO powder and orthophosphoric acid were mixed so that the molar ratio of CuO / P 2 O 5 was 2, and heat treated at a temperature of 200 ° C. or higher to give a copper-containing phosphate compound. Got ready. 300 g of this copper-containing phosphoric acid compound and 300 cc of ion-exchanged water were placed in a 2 liter capacity alumina ball mill, and 40
The mixture was rotated at 100 rpm for an hour and wet-milled to obtain a slurry. The obtained slurry was placed in a polytetrafluoroethylene vat and dried in a dryer at 150 ° C. for 12 hours to obtain fine powder. The average particle size of the obtained powder is 2.8 μm,
The color tone was white.
【００１３】［実施例２］
実施例１で準備した銅含有リン酸化合物３００ｇを、流
動層式カウンタージェットミルで１時間、乾式粉砕して
微粉末を得た。得られた粉末の平均粒径は１．５μｍ、
色調は白色であった。Example 2 300 g of the copper-containing phosphate compound prepared in Example 1 was dry pulverized for 1 hour in a fluidized bed counter jet mill to obtain a fine powder. The average particle size of the obtained powder is 1.5 μm,
The color tone was white.
【００１４】［実施例３］
実施例１で準備した銅含有リン酸化合物１００ｇを、め
のう製遊星ミルで２時間、乾式粉砕して微粉末を得た。
得られた粉末の平均粒径は３μｍ、色調は白色であっ
た。Example 3 100 g of the copper-containing phosphate compound prepared in Example 1 was dry pulverized for 2 hours with an agate planetary mill to obtain a fine powder.
The obtained powder had an average particle size of 3 μm and a white color tone.
【００１５】［比較例１］
実施例１で準備した銅含有リン酸化合物３００ｇとエタ
ノール３００ｃｃとを２リットル容量のアルミナ製ボー
ルミルに入れ、これを４０時間、１００ｒｐｍで回転
し、湿式粉砕しスラリーを得た。得られたスラリーをロ
ータリーエバポレーターを用いて乾燥して微粉末を得
た。得られた粉末の平均粒径は２．７μｍ、色調は緑色
であった。Comparative Example 1 300 g of the copper-containing phosphate compound prepared in Example 1 and 300 cc of ethanol were placed in a 2 liter capacity alumina ball mill, which was rotated for 40 hours at 100 rpm and wet pulverized to form a slurry. Obtained. The obtained slurry was dried using a rotary evaporator to obtain a fine powder. The obtained powder had an average particle size of 2.7 μm and a color tone of green.
【００１６】［比較例２］
実施例１で準備した銅含有リン酸化合物３００ｇを２リ
ットル容量のアルミナ製ボールミルに入れた。これを８
０時間、１００ｒｐｍで回転し、乾式粉砕して微粉末を
得た。得られた粉末の平均粒径は３．５μｍ、色調は緑
色であった。COMPARATIVE EXAMPLE 2 300 g of the copper-containing phosphate compound prepared in Example 1 was placed in a 2 liter capacity alumina ball mill. This 8
It was rotated at 100 rpm for 0 hours and dry-ground to obtain a fine powder. The obtained powder had an average particle diameter of 3.5 μm and a color tone of green.
【００１７】[0017]
【発明の効果】本発明によれば、無色の近赤外吸収材料
粉末が製造されるため、肉眼で認識されず、近赤外光を
吸収する半導体レーザー光源を用いたシステムにより物
体、画像として良好に認識できる材料を効率的に供する
ことができる。According to the present invention, since a colorless near-infrared absorbing material powder is produced, it is not recognized by the naked eye and a system using a semiconductor laser light source that absorbs near-infrared light is used as an object or an image. Good recognizable materials can be provided efficiently.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭60−131815（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C01B 25/37 C09K 3/00 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References JP-A-60-131815 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) C01B 25/37 C09K 3/00
Claims (4)
ＣｕＯ／Ｐ2 Ｏ5 のモル比が０．０５〜４である銅含有
リン酸化合物（Ｃｕ 3 （ＰＯ 4 ） 2 ・Ｃｕ（ＯＨ） 2 は除
く）を、水の存在下で湿式粉砕し、微粉末化する近赤外
線吸収材料粉末の製造方法。1. A copper-containing phosphate compound (Cu 3 (PO 4 ) 2 ) having a CuO / P 2 O 5 molar ratio of 0.05 to 4 in terms of CuO for copper and P 2 O 5 for phosphoric acid. · Cu (OH) 2 is divided
A method for producing a near-infrared absorbing material powder, which comprises:
ＣｕＯ／Ｐ2 Ｏ5 のモル比が０．０５〜４である銅含有
リン酸化合物（Ｃｕ 3 （ＰＯ 4 ） 2 ・Ｃｕ（ＯＨ） 2 は除
く）を、アルミナを使用しない粉砕機で乾式粉砕し、微
粉末化する近赤外線吸収材料粉末の製造方法。2. A copper-containing phosphate compound (Cu 3 (PO 4 ) 2 having a molar ratio of CuO / P 2 O 5 of 0.05 to 4 in terms of CuO for copper and P 2 O 5 for phosphoric acid. · Cu (OH) 2 is divided
A method for producing a powder of near-infrared absorbing material, which comprises pulverizing (p.
求項１に記載の近赤外線吸収材料粉末の製造方法。 3. A contract in which the copper-containing phosphate compound is in an amorphous state.
The method for producing a near-infrared absorbing material powder according to claim 1.
求項２に記載の近赤外線吸収材料粉末の製造方法。 4. A contract in which the copper-containing phosphate compound is in an amorphous state.
The method for producing a near-infrared absorbing material powder according to claim 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1796593A JP3496227B2 (en) | 1993-01-08 | 1993-01-08 | Method for producing near-infrared absorbing material powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1796593A JP3496227B2 (en) | 1993-01-08 | 1993-01-08 | Method for producing near-infrared absorbing material powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06206714A JPH06206714A (en) | 1994-07-26 |
| JP3496227B2 true JP3496227B2 (en) | 2004-02-09 |
Family
ID=11958457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1796593A Expired - Fee Related JP3496227B2 (en) | 1993-01-08 | 1993-01-08 | Method for producing near-infrared absorbing material powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3496227B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1261787C (en) | 2003-03-10 | 2006-06-28 | 京瓷株式会社 | Camera device |
-
1993
- 1993-01-08 JP JP1796593A patent/JP3496227B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06206714A (en) | 1994-07-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0992455B1 (en) | Ultraviolet-screening zinc oxide excellent in transparency and composition containing the same | |
| AU743389B2 (en) | Fine hollow powder,thin flaky titanium oxide powder obtained by pulverization of the fine hollow powder and processes for producing the same | |
| US6077341A (en) | Silica-metal oxide particulate composite and method for producing silica agglomerates to be used for the composite | |
| DE69923666T2 (en) | CLEANING OF CERIUM OXIDE FOR POLISHING, METHOD FOR THE PRODUCTION THEREOF, AND METHOD OF POLISHING THEREOF | |
| US5911921A (en) | Non-stoichiometric ytterbium phosphate powder of low infrared reflectivity | |
| US5049309A (en) | Titania sol | |
| DE69918220T2 (en) | Ultraviolet light absorbers | |
| JPH11193354A (en) | Silica-coated zinc oxide particle, its preparation, and composition containing it | |
| EP0596442A1 (en) | Ultraviolet-shielding agent, method for the preparation thereof and cosmetic composition compounded therewith | |
| US5989331A (en) | TiO2 slurry stabilization | |
| US8642174B2 (en) | Near-infrared-absorbing particles, process for their production, dispersion, and article thereof | |
| JPH0661457B2 (en) | Oil dispersion and method for producing the same | |
| JPH05213618A (en) | Zinc oxide particle dispersed matter | |
| JPH09188517A (en) | Iron-containing superfine zinc oxide, its production and use | |
| JP3496227B2 (en) | Method for producing near-infrared absorbing material powder | |
| KR20080011425A (en) | Degradable zinc oxide powder and process for production thereof | |
| JP3550705B2 (en) | Near infrared absorbing material | |
| JPH06207161A (en) | Improved near infrared light absorbing material and ink using the same | |
| WO1996030448A1 (en) | Zinc oxide-coated body pigment and cosmetic material containing the same | |
| KR100618083B1 (en) | Invisible-Light Absorption Material and Ink and Manufacturing Method of the same | |
| US5738718A (en) | Zinc oxide-containing spherical silica and process for its production | |
| KR940006240B1 (en) | Process for preparing pigmentary copper phthalo cyanine | |
| US7115164B2 (en) | Preparation of yellow pigments | |
| JPH06306349A (en) | Near-infrared-absorbing material | |
| DE1905879B2 (en) | Process for the production of manganese activated zinc phosphate phosphors |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081128 Year of fee payment: 5 |
|
| LAPS | Cancellation because of no payment of annual fees |