Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – From reactant having a halogen atom or oxygen single bonded...
Reexamination Certificate
2000-12-07
2002-10-15
Moore, Margaret G. (Department: 1712)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
From reactant having a halogen atom or oxygen single bonded...
C528S395000, C252S500000
Reexamination Certificate
active
06465603
ABSTRACT:
DESCRIPTION
The invention relates to an electrically conductive inorganic polymer containing at least one metal a) selected from the group consisting of copper, an alkali metal and an alkaline earth metal, and at least one metal b) selected from the group consisting of a metal of the 1
st
, 2
nd
, 4
th
, 5
th
, 6
th
, 7
th
and 8
th
subgroup and the 3
rd
, 4
th
and 5
th
main group of the periodic system starting with atom number 31, an intermediate polymer and a method for producing said inorganic polymer.
Various types of metal alloys and even intermetallic compounds are already known. These, however, are frequently difficult to process further or to produce.
Thus, from JP 62084091, an electrically conductive inorganic polymer is known containing a metal of the 5
th
group. For the production of this polymer, a metal dithiolate complex is thermally decomposed.
The object of the present invention is to provide for an electrically conductive inorganic polymer disposing not only of a high electroconductivity, but also of good mechanical properties and which may easily be further processed.
This object is solved by an electrically conductive inorganic polymer according to the teaching of the claims.
The electrically conductive inorganic polymer according to the present invention, just called polymer in the following, is obtainable by a method comprising three main stages. Is the metal concerned according to the invention copper a), a preliminary stage has then to be carried out, wherein copper carbonate is mixed to form a slurry with an oxide of at least one metal b) with the addition of water. The water is evaporated therefrom by heating. The thereby obtained material may, for example, be pulverized.
The term “copper carbonate” thereby comprises pure copper carbonate, hydrate water-containing copper carbonate and hydroxy carbonate of copper.
In the first main stage of the method for producing the inventive polymer, a carbonate of at least one metal a) with the exception of copper and/or the copper-containing material obtained according to the preliminary stage, is fused with at least one oxide of a metal b).
As metal b) for said metal oxide, a metal is thereby used which is a metal from the 1
st
and 2
nd
, as well as from the 4
th
through 8
th
subgroup and the III
rd
through V
th
main group of the periodic system starting with the atom number 31.
Is copper used as metal a), said oxide of a metal b) may in this case also be a copper oxide or an oxide of another metal b).
When the invention mentions that for the production of the inventive polymer an alkali carbonate and/or an alkaline earth carbonate is/are used, this means in this case that a sole alkali carbonate, a sole alkaline earth carbonate, a compound of several alkali carbonates, a compound of several alkaline earth carbonates or a compound of one or more alkaline earth carbonate(s) or one or more alkaline earth carbonate(s) may be used. And the like applies relative to the metal oxide.
The alkali carbonate and/or alkaline earth carbonate and/or the copper-containing material obtained in the preliminary stage may be fused with an oxide of one, two, three, etc. metals b). The weight ratio between carbonate, respectively of the material from the preliminary stage and the oxide is thereby in the 1
st
stage preferably 25:75 to 60:40. With this range indication, all thereof comprised narrower, or at least integral ranges are characterized and hence disclosed, for example 30:70, 35:65, 38:72, 45:55, 50:50, 53:47 and 58:42.
The melt obtained in the 1
st
main stage, is cooled down slowly in an appropriate manner and then ground, if necessary.
In a 2
nd
main stage the material obtained in the 1
st
main stage is fused with a further oxide of a metal b). Thereby, an oxide having one, two, three or more of the metals b) may be concerned. As metal b), one of the 1
st
, 2
nd
, 4
th
, 5
th
, 6
th
, 7
th
and
8
th
subgroup, as well as of the 3
rd
4
th
and 5
th
main group of the periodic system starting with atom number 31 is used. The indication “starting from atom number 31” thereby relates only to the metals of the main groups.
The material obtained in the 1
st
main stage is preferably used in excess in the 2
nd
main stage. The weight ratio between the material obtained in the 1
st
main stage and the oxide is preferably 60:40 to 70:30 in the 2
nd
main stage.
Appropriately, one heats to a temperature in the 1
st
main stage which is lower than the temperature of the 2
nd
main stage. Preferably, the temperature of the 1
st
main stage is 300 to 850° C., and 700 to 1200° C. in the 2
nd
main stage.
The product obtained subsequent to the 2
nd
main stage is designated as intermediate polymer within the framework of the present documents. Said intermediate polymer may be processed into valuable end products such as will be considered below in more detail.
According to a preferred embodiment, the same metal oxide, respectively the same metal oxides is/are used in the 1
st
and 2
nd
main stage.
As metal b) for the metal oxide serve preferably titanium, vanadium, nickel, gallium, germanium, molybdenum, rhodium, indium, antimony, tellurium, tungsten, rhenium, iridium, thallium, bismuth, copper, gold, silver and zinc.
The melt obtained in the 2
nd
main stage may be allowed to cool down, appropriately slowly. The thereby obtained intermediate polymer may then be pulverized, for example ground, and disposes already of electroconductivity.
This intermediate polymer may then be further processed. It is thereby preferably dissolved in a 3
rd
main stage in an aqueous solvent, for example by means of acids or alkaline solutions, and is then electro-deposited under reduction in an electrolytic cell on an in particular conductive substrate, which is poled as a cathode.
A d.-c. power supply such as a battery or a regulated power supply may serve as the energy source for the operation of said electrolytic cell. The voltage thereby is appropriately in a range of about 1 to 25 V. A voltage in a range between 2 and 12 V revealed to be particularly appropriate. The current density usually is in a range between 1 to 100 mA/cm
2
, further preferred in a range between 1.0 and 35 mA/cm
2
.
The electrolytic solution should not exceed a temperature of +80° C. In general, a reaction temperature in the range between +40° C. and +70° C. revealed to be very advantageous.
With this coating thus deposited on a substrate, the final electrically conductive inorganic polymer is concerned.
The pulverized intermediate polymer such as described above may again be fused and reduced in the 3
rd
main stage according to a further preferred embodiment. For this fusing, as well as for the fusing processes of the 1
st
and 2
nd
main stage, one appropriately employs a suitable crucible, in which the substances and materials to be fused are placed.
The melt of the intermediate polymer for the remainder may not only be obtained in that—such as described above—the intermediate polymer obtained after the 2
nd
main stage is fused again. One may also immediately use the melt obtained in the 2
nd
main stage without prior cooling down of said melt.
The melt of the intermediate polymer is then preferably reduced electrolytically by means of a real gas or by means of a reducing agent having a reduction potential of −0.100 to −0.900 E°inV. With this reduction, polymer crystals separate out from the melt.
For carrying out the electrolysis of the melt from the intermediate polymer, the latter is fused in a crucible at 650 to 900° C. The electrolysis is carried out with direct current, a current density of 10 to 35 mA/cm
2
being preferred. The voltage depends on the melt composition and should be about 0.8 to 3.5 V. As electrodes, those made of graphite or precious metal have proved successful. On these electrodes, more precisely on the cathode, the inventive polymer deposits in the form of crystals. These are then taken out and appropriately washed and dried.
Said reduction may however also be carried out in that just a reducing agent is sub
Bacon & Thomas
Moore Margaret G.
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