DE10119911A1 - Dispersion and/or composition used in production of layers and molded bodies comprises particulate component and catalytic dispersing auxiliary aid - Google Patents
Dispersion and/or composition used in production of layers and molded bodies comprises particulate component and catalytic dispersing auxiliary aidInfo
- Publication number
- DE10119911A1 DE10119911A1 DE10119911A DE10119911A DE10119911A1 DE 10119911 A1 DE10119911 A1 DE 10119911A1 DE 10119911 A DE10119911 A DE 10119911A DE 10119911 A DE10119911 A DE 10119911A DE 10119911 A1 DE10119911 A1 DE 10119911A1
- Authority
- DE
- Germany
- Prior art keywords
- dispersion
- catalytic
- layers
- particulate component
- production
- 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.)
- Ceased
Links
- 239000006185 dispersion Substances 0.000 title claims abstract description 17
- 239000000203 mixture Substances 0.000 title claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 title claims abstract 5
- 238000004519 manufacturing process Methods 0.000 title description 6
- 150000002902 organometallic compounds Chemical class 0.000 claims abstract description 4
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract 2
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims 2
- 230000000593 degrading effect Effects 0.000 claims 2
- 229910001385 heavy metal Inorganic materials 0.000 claims 1
- 150000002739 metals Chemical class 0.000 claims 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000000465 moulding Methods 0.000 description 6
- -1 cyclic alcohols Chemical class 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 125000001190 organyl group Chemical group 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000001962 electrophoresis Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940027983 antiseptic and disinfectant quaternary ammonium compound Drugs 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
- H01J29/86—Vessels; Containers; Vacuum locks
- H01J29/88—Vessels; Containers; Vacuum locks provided with coatings on the walls thereof; Selection of materials for the coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/017—Mixtures of compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2229/00—Details of cathode ray tubes or electron beam tubes
- H01J2229/88—Coatings
- H01J2229/882—Coatings having particular electrical resistive or conductive properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Laminated Bodies (AREA)
Abstract
Description
Die vorliegende Erfindung betrifft den Gegenstand des unabhän gigen Anspruches. Damit befaßt sich die vorliegende Erfindung mit der Herstellung von Schichten und Formkörpern.The present invention relates to the subject of the independent right claim. This is what the present invention is concerned with with the production of layers and moldings.
Als Ausgansmaterial zur Herstellung partikulärer Schichten und/oder Formkörper sind besonders solche System geeignet, bei denen Partikel, aus denen die Schichtsysteme und/oder Formkör per aufgebaut sind, in einer Matrix oder einem Lösungsmittel dispergiert vorliegen. Als Lösungsmittel werden üblicherweise eingesetzt Wasser, aliphatische und/oder cylische Alkohole, Carbonsäureester, Glycolester, Ether, Glycolether, Aromaten, Ketone, Ketonalkohole sowie Derivate und/oder Mischungen die ser Verbindungen.As a starting material for the production of particulate layers and / or moldings are particularly suitable for such systems those particles from which the layer systems and / or molded bodies per are built up in a matrix or a solvent are dispersed. Usually used as solvents used water, aliphatic and / or cyclic alcohols, Carboxylic acid esters, glycol esters, ethers, glycol ethers, aromatics, Ketones, ketone alcohols and derivatives and / or mixtures connections.
Die Schichtqualität wird dabei stark von der Qualität des Dis pergierzustandes der Partikel in der Dispersion beeinflußt. Ein schlechter Dispergierzustand, der oftmals mit dem Vorhan densein von Agglomeraten einhergeht, führt zu Inhomogenitäten im Gefüge der hergestellten Schichten und/oder Formkörper. The layer quality is strongly dependent on the quality of the dis the state of pergier of the particles in the dispersion. A poor state of dispersion, often with the existing the presence of agglomerates leads to inhomogeneities in the structure of the layers and / or moldings produced.
Dies erweist sich als problematisch, wenn die eingesetzten Partikel sehr klein sind, etwa bei Partikelgrößen unter 0,5 µm und/oder Schichten hoher optischer Qualität gewünscht werden. So führt das Vorhandensein von Agglomeraten bei optischen Schichten zu verminderter Transparenz bis hin zur Schichtein trübung.This turns out to be problematic if the used ones Particles are very small, for example with particle sizes below 0.5 µm and / or layers of high optical quality are desired. So the presence of agglomerates leads to optical Layers of reduced transparency right down to the layer turbidity.
Es ist daher üblich, Dispergierhilfsmittel einzusetzen, um bei den zur Herstellung von Schichten und/oder Formkörper verwen deten Dispersionen einen guten Dispergierzustand zu gewährlei sten. Die Qualität der Dispersion ist dabei von Wahl und Menge des eingesetzten Dispergierhilfsmittels abhängig.It is therefore common to use dispersing aids in order to use the to produce layers and / or moldings to ensure good dispersions sten. The quality of the dispersion depends on the choice and quantity dependent on the dispersing agent used.
Als Dispergierhilfsmittel werden eingesetzt sowohl anorgani sche als auch organische Verbindungen, wobei insbesondere or ganische Tenside als oligomere oder polymere Verbindungen Ein satz finden, die sich mit einer Vielzahl von Lösungsmitteln und/oder unterschiedlichen Partikeln mit guten Ergebnissen kombinieren lassen. Gleichfalls finden als Dispergierhilfen niedermolekulare und/oder monomere Substanzen Einsatz, z. B. Carbonsäuren und/oder deren Derivate, Amine, quaternäre Ammo niumverbindungen sowie sonstige organische Basen, Organophos phate und/oder -pyrrophosphate.Dispersants are used both inorganic cal as well as organic compounds, in particular or ganic surfactants as oligomeric or polymeric compounds Find a set that works with a variety of solvents and / or different particles with good results let combine. Also find as dispersing aids Use of low molecular weight and / or monomeric substances, e.g. B. Carboxylic acids and / or their derivatives, amines, quaternary ammo nium compounds and other organic bases, organophos phate and / or pyrrophosphate.
Wenn die Schichtherstellung, die mit üblichen Verfahren erfol gen kann, wie z. B. Spin- und/oder Dipcoating, Drucken, Elek trophorese, Sprühen und/oder Aufrakeln), bzw. die Formköprer herstellung abgeschlossen ist, die gleichfalls mit üblichen Verfahren erfolgen kann wie z. B. Schlickerguß, Spritzguß, Ex trusion, Elektrophorese und/oder Foliengießen, haben die Dis pergiermittel ihren Zweck erfüllt. Sie dürfen dann die Schicht- oder Formkörpereigenschaften nicht beeinträchtigen und werden daher oftmals entfernt. If the layer production is carried out using the usual methods conditions such. B. spin and / or dip coating, printing, elec trophoresis, spraying and / or doctoring), or the molded body manufacturing is complete, also with usual Procedures can take place such. B. slip molding, injection molding, Ex trusion, electrophoresis and / or film casting, have the Dis Powdering agent serves its purpose. You can then Do not impair layer or molded body properties and are therefore often removed.
Dies kann, z. B. bei der Herstellung von Keramikkörpern, durch eine Temperaturbehandlung erfolgen, nach welcher etwaige Dis pergierhilfsmittel weitgehend entfernt sind. Dazu werden aber in der Regel Temperaturen benötigt, die dispergierhilfsmittel abhängig deutlich über 500°C liegen können.This can e.g. B. in the production of ceramic bodies, by a temperature treatment, after which any dis Pouring aids are largely removed. To do so As a rule, temperatures are required for the dispersing agents depending on the temperature can be significantly higher than 500 ° C.
Dies ist dann problematisch, wenn keine sehr hohen Temperatu ren eingesetzt werden können oder sollen. Ein Beispiel stellt etwa die Beschichtung von Kathodenstrahlröhren mit ITO (Indi um-Zinn-Oxid) dar. Hier ist einerseits zur Erzielung der ge wünschten Leitfähigkeiten eine besonders hohe Dichte ge wünscht, die eine weitgehende Entfernung der Dispergierhilfs mittel erfordert, andererseits ist eine hohe Temperatur hier für aber im Prozeß nicht anwendbar. Die Wahl der Dispergier hilfsmittel ist dadurch stark eingeschränkt und es gilt, hier noch geeignete Dispergiermittel zu finden.This is problematic if the temperature is not very high Ren can or should be used. An example provides for example the coating of cathode ray tubes with ITO (Indi um tin oxide). Here, on the one hand, to achieve the ge desired conductivities a particularly high density desires extensive removal of the dispersing aid medium required, on the other hand there is a high temperature here but not applicable in the process. The choice of dispersants Aid is severely limited by this and it applies here to find suitable dispersants.
Das Ziel der vorliegenden Erfindung besteht darin, Neues für die gewerbliche Anwendung bereitzustellen.The aim of the present invention is to create something new for to provide the commercial application.
Das Ziel wird erreicht mit den Merkmalen des unabhängigen An spruches.The goal is achieved with the characteristics of the independent contractor award.
Damit sieht die Erfindung zunächst vor, daß bei einer Disper sion und/oder Zusammensetzung zur Herstellung einer Dispersion mit einem partikulären Bestandteil und einem Dispergierhilfs mittel ein katalytisch Dispergierhilfsmittel abbauender Be standteil enthalten ist.The invention thus initially provides that in a disper sion and / or composition for the preparation of a dispersion with a particulate component and a dispersing aid medium a catalytically dispersing auxiliary part is included.
Die Erfindung geht damit einen grundlegend anderen Weg als die Selektion eines besonderen Dispergierhilfsmittels und vermei det so die Nachteile durch die stark beschränkte Wahl leicht entfernbarer Dispergierhilfsmittel, indem vorgeschlagen wird, das oder die Dispergierhilfsmittel einfach katalytisch abzu bauen.The invention thus goes a fundamentally different way than that Selection of a special dispersing agent and avoid so the disadvantages due to the very limited choice easily removable dispersing aid by suggesting to simply catalytically remove the dispersing agent or agents to build.
Es hat sich überraschend gezeigt, daß dies, obwohl wenigstens eine zusätzliche Substanz verwendet wird, die ja die entste henden Schichten und/oder Formkörper in ihrer Funktionalität beeinträchtigen könnte, zu wesentlich verbesserten Ergebnissen führt. So wurde gefunden, daß sich mit der Erfindung auch bei niederen Temperaturen transparente, elektrisch besonders gut leitende ITO (SnO2/In2O3) herstellen lassen. Dies wird auf die verbesserten Kontaktstellen und besseren Übergänge zwischen einzelnen ITO-Partikeln zurückgeführt. Ob und wieweit hier verbleibende metallisch leitende Reste der Metallorganyle selbst die Leitfähigkeit an den Partikelgrenzen selbst erhö hen, ist unklar; daß dies der Fall ist, wird aber nicht ausge schlossen. Jedenfalls führt aber der Zusatz der Metallorganyle zu wesentlichen und unerwarteten Verbesserungen der Schichten, obwohl die Metallorganyle selbst nicht leiten, und zwar selbst bei den eingesetzten, niedrigen Prozeßtemperaturen von z. B. 200°C nicht.It has surprisingly been found that, although at least one additional substance is used, which could impair the functionality of the resulting layers and / or moldings, this leads to significantly improved results. It was found, for example, that the invention can be used to produce transparent ITO (SnO 2 / In 2 O 3 ) which is particularly electrically conductive even at low temperatures. This is attributed to the improved contact points and better transitions between individual ITO particles. It is unclear whether and to what extent remaining metallically conductive residues of the metal organyls themselves increase the conductivity at the particle boundaries; that this is the case is not excluded. In any case, the addition of the metal organyles leads to significant and unexpected improvements in the layers, although the metal organyles themselves do not conduct, even at the low process temperatures of z. B. 200 ° C not.
Es hat sich als ausreichend erwiesen, einen Anteil von unter 2 Gewichtsprozent metallorganischer Verbindungen einzusetzen. Bevorzugt ist eine Menge unter 1 Gewichtsprozent.It has proven to be sufficient to have a share of less than 2 Use weight percent of organometallic compounds. An amount below 1 percent by weight is preferred.
Die Erfindung wird im folgenden beispielhaft beschrieben.The invention is described below by way of example.
Eine ethanolische Dispersion mit 2 Gew.-% ITO mit einer Teilchen größe unter 0,2 µm wird mit 6 Gewichtsprozent einer Carbonsäure bezogen auf ITO dispergiert und durch Spincoating auf ein Borosilikatglas zu einer Dicke von ca. 100 nm aufgetragen. Nach Antrocknung wird als Verkratzschutz eine Lösung eines hydroli sierbaren Si-Alkoholates über spincoating zur Nachbeschichtung aufgetragen. Dann wird das doppelt beschichtete Substrat für 30 min bei 180°C ausgeheizt. Nach Abkühlen wird die Leitfähig keit zu 70 kΩ bestimmt.An ethanolic dispersion with 2 wt .-% ITO with one particle Size under 0.2 microns with 6 percent by weight of a carboxylic acid based on ITO dispersed and by spin coating on a Borosilicate glass applied to a thickness of approximately 100 nm. To Drying is a solution of a hydroli as scratch protection Si-alcoholates that can be used via spin coating for re-coating applied. Then the double coated substrate for Baked at 180 ° C for 30 min. After cooling, the conductivity becomes determined to 70 kΩ.
Wie vor, aber mit 3% Carbonsäure. Nach Abkühlen wird die Leit fähigkeit zu 30 kΩ bestimmt.As before, but with 3% carboxylic acid. After cooling, the guide ability determined to 30 kΩ.
Wie vor, aber mit 1% Carbonsäure. Nach Abkühlen wird die Leit fähigkeit zu 10,3 kΩ bestimmt.As before, but with 1% carboxylic acid. After cooling, the guide ability determined to 10.3 kΩ.
Eine Dispersion wie in Beispiel 3 wird hergestellt, aber es werden zusätzlich 0,2 Gew.-% eines Zirkonalkoholates zugesetzt. Dann werden Schichten wie unter 1 damit hergestellt. Nach Ab kühlen wird die Leitfähigkeit zu 7,5 kΩ bestimmt. Derartige Leitfähigkeit von solchen ITO-Schichten waren zuvor nicht er zielbar, insbesondere nicht bei transparenten ITO-Schichten.A dispersion as in Example 3 is made, but it an additional 0.2% by weight of a zirconium alcoholate is added. Then layers as in 1 are produced with it. After Ab cool the conductivity is determined to be 7.5 kΩ. such Conductivity of such ITO layers was not previously there targetable, especially not with transparent ITO layers.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10119911A DE10119911A1 (en) | 2001-03-15 | 2001-06-22 | Dispersion and/or composition used in production of layers and molded bodies comprises particulate component and catalytic dispersing auxiliary aid |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10112885 | 2001-03-15 | ||
| DE10119911A DE10119911A1 (en) | 2001-03-15 | 2001-06-22 | Dispersion and/or composition used in production of layers and molded bodies comprises particulate component and catalytic dispersing auxiliary aid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE10119911A1 true DE10119911A1 (en) | 2002-10-02 |
Family
ID=7677821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE10119911A Ceased DE10119911A1 (en) | 2001-03-15 | 2001-06-22 | Dispersion and/or composition used in production of layers and molded bodies comprises particulate component and catalytic dispersing auxiliary aid |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE10119911A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008041377A1 (en) | 2008-08-20 | 2010-02-25 | Evonik Degussa Gmbh | Dispersion, useful for preparing film, which is useful e.g. in optoelectronics, and microelectronics, comprises indium tin oxide particles, alkyloxacarboxylic acid, a thermoplastic binder e.g. polyvinyl butyral, and solvent e.g. alcohols |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4435376A1 (en) * | 1993-10-05 | 1995-04-27 | Dainippon Toryo Kk | Composition for the formation of conductive films |
-
2001
- 2001-06-22 DE DE10119911A patent/DE10119911A1/en not_active Ceased
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4435376A1 (en) * | 1993-10-05 | 1995-04-27 | Dainippon Toryo Kk | Composition for the formation of conductive films |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102008041377A1 (en) | 2008-08-20 | 2010-02-25 | Evonik Degussa Gmbh | Dispersion, useful for preparing film, which is useful e.g. in optoelectronics, and microelectronics, comprises indium tin oxide particles, alkyloxacarboxylic acid, a thermoplastic binder e.g. polyvinyl butyral, and solvent e.g. alcohols |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| OP8 | Request for examination as to paragraph 44 patent law | ||
| 8181 | Inventor (new situation) |
Free format text: NASS, RUEDIGER, DR., 66292 RIEGELSBERG, DE BURGARD, DETLEF, 66333 VOELKLINGEN, DE |
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| 8127 | New person/name/address of the applicant |
Owner name: NANOGATE ADVANCED MATERIALS GMBH, 66121 SAARBRUECKEN |
|
| 8127 | New person/name/address of the applicant |
Owner name: AIR PRODUCTS AND CHEMICALS, INC., ALLENTOWN, PA., |
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| 8128 | New person/name/address of the agent |
Representative=s name: J?NSSON, H., DIPL.-CHEM. DR.RER.NAT., PAT.-ANW., 5 |
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| 8131 | Rejection |