EP3542116A1

EP3542116A1 - Arrangement of a furnace and an aggregate of glass particles and method for operating a furnace

Info

Publication number: EP3542116A1
Application number: EP17825747.3A
Authority: EP
Inventors: Rudolf Jussel; Harald Bürke
Original assignee: Ivoclar Vivadent AG
Current assignee: Ivoclar Vivadent AG
Priority date: 2016-11-15
Filing date: 2017-11-14
Publication date: 2019-09-25
Also published as: US20200072552A1; US11808520B2; WO2018091457A1; EP3321621A1

Abstract

The invention relates to an arrangement of a furnace and an aggregate of glass particles, which furnace (10) comprises a pressing stamp (36), a pressure, displacement and/or speed sensor and a control device for controlling a pressing process on the basis of the output signal of the sensor. The sensor detects at least one pressure, location and/or movement parameter of the pressing stamp (36). The pressing stamp (36) acts - optionally via an interposed press piston (28) - on the aggregate of glass particles (32) which are guided in a pressing channel (30) and can be crystallized. The triggering criterion for the process control is a change in at least one movement parameter of the pressing stamp (36) when the aggregate of glass particles (32) is softened, said change being detected by the sensor.

Description

Arrangement of a furnace and a heap of glass particles

and method of operating a furnace

The invention relates to an arrangement of a furnace and a cluster of glass particles, according to the preamble of claim 1, and a method for operating a furnace, according to the preamble of claim 12.

Special ovens such as dental kilns or dental press ovens may be used to make dental restorations of e.g. Ceramic, glass or glass ceramic can be used.

Glass ceramic powders and / or crystallisable glass particles can be used in the production of dental restorations made of glass ceramic, which are preferably pre-heated in a combustion chamber of a kiln or in a press chamber of a press furnace a burning plate is placed.

The glass ceramic powders or glass particles are first heated to a desired viscous state. Finally, during a compression process, these soft glass or glass ceramic particles are pressed under pressure into a solid block or pressed into the mold cavities for dental restoration parts via the cannulated channels of the muffle arranged under the glass or glass ceramic particles until the mold cavities are completely filled.

By another debinding method and another cooling process, dental restoration parts of e.g. Lithium silicate provided.

However, the problem with compaction of the glass particles is that crystallization often occurs before the glass particles are completely densified. This uncontrolled crystallization impedes further densification and results in a loss of strength due to a high level of residual porosity.

In addition, the resulting glass ceramic is inferior, because the uncontrolled crystallization creates an unfavorable critical structure with a broad crystal size distribution. It is therefore desirable that complete densification of the glass particles take place prior to crystallization.

For a successful pressing process of dental glass particles, it is also important to carry out the heating with a precisely defined heating profile.

While the measured temperatures typically relate to the furnace interior temperature and thus not the true temperature of the glass particles, WO 2014/131588 A1 has disclosed a method for detecting the temperature of a blank itself.

In the case of a large pile of glass particles, however, there is a certain temperature gradient within the pile, and even with the said favorable, but also not very inexpensive, solution, the temperature of the pile can typically be detected at one point, but not at all points.

Another problem is that with particularly trained temperature profiles, the dead time of the system muffle / glass particles delays the measured temperature profiles. This depends strongly on the mass of the heap of glass particles and the muffle. Particularly voluminous muffles and a large pile of glass particles would therefore basically have to be operated with even "sharper" heating profiles - ie longer and more exact.

Typically, after the heating, a holding time is inserted, which is intended to compensate for the temperature and in which the hot outer areas of the muffle deliver their heat to the muffle center and thus the heap of glass particles.

However, this hold time significantly increases the press cycle depending on the size of the muffle, which is sometimes not considered acceptable. In addition, depending on the muffle size used, a corresponding control program with suitable temperature profiles and holding times must be selected. Also, the extension of the holding time can not exclude the possibility that the relevant boundary conditions in the process will not be able to affect the result.

Therefore, the invention has for its object to provide an arrangement of a furnace and a cluster of glass particles according to the preamble of claim 1 and a method for operating a furnace according to the preamble of claim 12, which ensures the quality of to be produced dental restoration parts made of glass and independent of the size of a heap of glass particles or the associated muffle a shortened pressing cycle allowed. Included in this is the task of producing a block or blank or other preform made of glass, which serves as a starting material for the production of a dental restoration.

This object is achieved by the claims 1 and 12. Advantageous developments emerge from the subclaims.

According to the invention, a rapid heating of these is carried out before the compaction of the aggregate of glass particles.

The nucleation of the crystallizable glass particles begins depending on the material in the transformation region Tg (also referred to as "transformation point Tg") of the glass particles and has its maximum velocity during the increase in temperature at a temperature range about 50 ° C over the transformation range Tg of the glass particles (Tg + 50 ° C). As the temperature continues to increase, the rate of nucleation slows down. The compaction speed of the glass particles is measured in a temperature range e.g. increased between 50 ° C over the transformation range Tg of the glass particles (Tg + 50 ° C) and 100 ° C over the transformation range Tg of the glass particles (Tg + 100 ° C) with increasing temperature.

In this connection, according to the invention, by rapidly heating the glass particles from approximately the transformation range Tg, the glass particles are heated to a temperature range e.g. 70 ° C above the transformation range (Tg + 70 ° C) only a few germs (to the extent desired) formed. It is favorable that in the compaction according to the example from the temperature range - 70 ° C over the transformation range Tg (Tg + 70 ° C) - result due to the few germs and a few glass crystals.

This ensures that the further compaction is no longer prevented by the unwanted and uncontrolled crystallization (strong).

Surprisingly, the parameters for the compression process can be determined independently of the amount of glass particles, the material of the glass particles and the size of the muffle.

In a preferred embodiment, it is provided that after the compression process, the compacted debris of the glass particles can be cooled immediately. Because with a further increase in the temperature - subsequent to the above-mentioned example - over the "Tg + 100 ° G" range slows the speed of compaction of the glass particles, while accelerating the rate of crystallization. In this case, the invention by a controlled temperature or after the compaction immediate cooling of the glass particles further diminished the crystal growth.

According to the invention, it is particularly favorable that the inherent physical parameters of glass particles can now be used as a criterion for the first time with the invention. This represents a significant advance over the typical and hitherto widespread kilns and blast furnaces where only one temperature sensor is used inside the furnace. In contrast, in the case of the better solution according to WO 2014/131588 A1, the surface of the dental restoration part to be produced is checked. However, even with a large mass of dental glass particles, there is a temperature gradient and the size of the debris also accounts for the temperature difference between inside and outside. Another disadvantage of the previously known solution is that additional and costly measurement technology must be attached to the device.

Typically, in a muffle, there is a temperature gradient that, with its isotherms, is substantially bell-shaped as viewed in three-dimensional view, with the lowest at the bottom center of the pile and the highest at the top of the pile at the bottom of the pile Temperature exists. According to the invention, glass particle parameters are now used on the side surfaces of the heap as a triggering criterion for the process control, in a surprisingly sophisticated manner, wherein the softening of the glass particles are evaluated in their entirety.

For the process control includes the start of the pressing process, at which start the furnace temperature, the pressure in a combustion chamber of the furnace and a pressing force of the ram are controlled by the control device. In addition, this includes the end of the pressing process or the beginning of a cooling process subsequent to the pressing process, in which end or beginning the pressing force of the press ram by the control device, in particular reduced to zero, and the furnace temperature by the control device, in particular by switching off the furnace and / or the opening of the furnace hood, is reduced.

For example, the decrease in press speed can be used as a triggering criterion for the shutdown of the furnace. In the pressing operation, when the pressing speed detected by the sensor is decreased, it is close to zero or less than 5%, in particular less than 2%, of the maximum pressing speed of the press die, the furnace shutdown criterion is satisfied, which means that automatically or manually the pressing process should be terminated and the cooling process should be started. In addition, the back pressure on the ram due to the heating of the glass particles and the investment material in the lower part can be measured by a pressure sensor and used as a trigger criterion for the process control. For example, the pressing process should be started when the detected back pressure remains constant within a predetermined time to a predetermined level.

In addition, the location of the ram can be detected by a location sensor and used as a triggering criterion for the process control. For example, the oven should be switched off when the location of the ram almost does not change during the pressing process within a predetermined time.

Before heating, the heap of glass particles according to the invention from different starting glasses is first filled into the pressing channel of the furnace where it forms gradients, in particular color and / or translucency gradients, so that the dental restoration parts to be produced have desired gradients which match the oral situation of a patient.

The gradients correspond to at least one gradual layer-wise and / or one continuous change of a physical property of the cluster of glass particles.

In a further preferred embodiment, the heap of glass particles consists of different colored glass particles and / or at least one type of glass, which is colored differently with pigments. Pigments include, among others, colored pigments, cloudy pigments and fluorescent pigments.

The use of pigments is particularly suitable at relatively low process temperatures. At higher process temperatures such pigments are chemically or thermally not stable in the respective glass matrix and would partially or completely decompose.

In a further preferred embodiment, the heap of glass particles consists of glasses with different contents of nucleating agents. As a result, after controlled crystallization, a block with different crystal sizes and / or different strengths in different areas may result. For example, in a manufactured dental restoration in dentine a larger crystal size can be realized with a softer material with low translucency and in the melting range a fine crystalline structure with high hardness, high wear resistance and high translucency. In a further preferred embodiment, the heap of glass particles consists of glasses with different densities. A particularly soft, elastic region, which is suitable for the reproduction of dentin with low hardness, is possible by controlled generation of residual porosity.

According to the invention, non-ideal starting conditions from previous process steps such as a correct preheating temperature or preheating time of the muffle are taken into account or corrected or compensated.

The heap of glass particles is - long before the pressing process - on the ram - typically via the interposition of a plunger, for example, Al ₂ 0 ₃ , pressurized. On its upper end face now acts a force and a pressure that is absorbed by its underside, but partly also to an elastic deformation of the glass particles - but in (very) small extent - leads. In any case, this force and the deformation is sufficient to make the arrangement of the glass particles, which is loose after insertion in the muffle, firmer and more stable.

The muffle mass typically has a comparatively low coefficient of thermal expansion, for example, 3 x 10 ^-6 / K, while the glass particles of, for example lithium silicate have a significantly higher thermal expansion coefficient of for example 10 x 10 ^"6 / K.

Glass particles have a coefficient of thermal expansion of, for example, 10 or 10.5 × 10 ^-6 / K below the so-called glass transition region. Although the coefficient of thermal expansion clearly increases when the so-called phase transition of the second order is exceeded, for example to 14.5 × 10 ^-6 / K, due to the softening of the glass particles, the shape of the glass particles also changes in particular but also to enter the Anstiftkanäle for the dental restoration cavities after the pile of glass particles has now become viscous.This represents a significant overcompensation of the increasing coefficient of thermal expansion.

In this regard, considering the parameters of the movement of the ram, micro-pulses are observed which, due to the thermal expansion of the ram, plunger, glass particles and surrounding muffle, cause little and momentary movement between the upper or near-end of the lump of the glass particle and the muffle play. It is particularly favorable that thereby the time course of the thermal expansion as a result of the heating of the introduced Systems consisting of muffle, intermediate plunger and in particular the heap of glass particles can be detected. In a further advantageous embodiment, it is provided that the control device determines the beginning of the press independently of the temperature measured by the temperature sensor as a function of the termination of the micro-pulses.

In a further advantageous embodiment, it is provided that the control device starts the press start based on an increase in the measured time duration between two consecutive micro-pulses above a predetermined threshold.

In a further advantageous embodiment, it is provided that the control device lowers the heating power to a nominal value as the time duration between two successive micro-pulses increases over a predetermined, in particular second threshold value.

According to the invention, the time profile of the micro-pulses is evaluated and a tripping criterion for the process control is established either at the termination of the micro-pulses of the movement parameters of the glass particles and / or upon detection of a predetermined number of micro-pulses and / or by evaluating the time interval between the micro-pulses.

With the invention, e.g. Determine and set the optimal start of pressing, thus bringing the total time spent on the press cycle close to optimum.

According to the invention, the triggering criterion for the actual pressing process is monitored by the movement parameters, and the occurrence of short-term micromotion is monitored and used as a criterion. It is understood that the micro-movements are directed against the pressing direction, due to the thermal expansion of the entire system ram / plunger / glass particles / muffle / combustion chamber shell.

The pressing punch moves during the heating of the glass particles by a predetermined amount against the pressing direction, which is in particular less than 1 mm and particularly preferably between 0.3 and 0.5 mm.

For detecting the micro-motion, which is basically a micro-pulse of a motion parameter, a displacement sensor or a speed sensor is primarily suitable. The resolution should be at least 0.01 mm or a corresponding speed size, preferably 50 μπι per second. Otherwise, that is, for example, when the pressing force is applied via a stepper motor with a non-elastic or low elastic drive train, the realization of a force sensor or pressure sensor as a sensor for the detection of microimps is possible. Alternatively, a pure displacement measurement, possibly at a pressing force close to zero, is possible.

The amplitude and frequency of the micro-pulses of course depends on physical parameters, for example on the material of the glass particles to be pressed, the investment material used, the temperature, but also, for example, the applied pressing force or its regulation.

The thermal expansion counteracting the pressing force is essentially composed of the thermal expansion of the press ram, of the pressing piston, of the glass particles, and of the muffle below the glass particles. The insulation area of the furnace below the combustion chamber floor is also warmed up a bit and expands accordingly.

The fact that the pressing ram is in contact with the interposed pressing piston and thus also with the upper end of the cluster of the glass particles, preferably under a contact pressure, can be exploited in a particularly favorable manner. The pressing force can be transmitted without time delay, as well as the backward movement in the material expansion of the glass particles. The control device for the control of the pressing process not only detects this, but also controls the further course of the temperature-time profile.

Due to the high thermal insulation of the furnace is typically outside and thus at the supporting points, which are responsible for closing the furnace, at least in relation to hot combustion chamber considered practically cold, typically between room temperature and 50 ° C, so that there existing Heating is relatively low.

Here, it is assumed that the heating surrounds the cylindrical combustion chamber in a conventional manner as a ring heating and heated by convection and heat radiation mainly the muffle, but also of course located therein heap of glass particles and optionally the plunger, typically in a few minutes to several 100 ° C. In typical press furnaces, the wall thickness of the thermal insulation is five centimeters or less and is thus in the range of the diameter of the muffle or below. The heating in the drive train of plunger, ram, glass particles and investment material in the lower part and possibly the burner plate and surrounding parts generates a back pressure on the press drive.

According to the invention, it is possible to work during the detection of the triggering criterion according to the invention with the same pressing force as during the actual pressing.

However, it is preferable to choose an auxiliary pressing force between three and fifty percent of the nominal pressing force, since this is already sufficient to produce the desired movement hysteresis.

It is also possible to keep the pressing force immediately after the delivery of the press ram to the plunger - and thus indirectly to the bulk of the glass particles - for a short time to a comparatively high value to ensure a stable investment of the bulk material of the glass particles in the muffle and then a Presskraftnachregelung make.

Another consideration relevant to the accuracy of the measurements taken is the provision of the oven vacuum prior to taking the measurement. Due to the furnace vacuum, the seals between the furnace hood and the furnace underside, or for example between the furnace hood and an approachable firing table, are compressed to the predetermined extent. The compression may well be in the range of several millimeters and would falsify the measurement result if the negative pressure during the pre-press, ie during the detection of the triggering criterion, would be built up.

If, for whatever reason, during this time no complete negative pressure, as desired during the pressing cycle, is to be provided, at least care must be taken that the negative pressure in the furnace interior remains constant during this pre-pressing time.

Typically, however, assuming sufficient tightness of the furnace, the underpressure can already be established within a considerably shorter than the required heating time of the furnace, for example within 1 to 2 minutes.

In a further preferred embodiment, it is provided that in the pressing process, if a vobestimmter part of the heap of glass particles is heated and compressed, the negative pressure can be reduced by, for example, a whole or partial ventilation of the combustion chamber. If subsequently another area of the glass particles is also densified, then there will be in the gaps between the glass particles this Enclosed area of air and thus prevents a complete consolidation of this area. This results, for example, in a block with different densities.

According to a further preferred embodiment, a force control is provided for the press drive. Due to the heating and thus during the thermal expansion of the drive train (including the bulk of the glass particles) must be a readjustment, z. B. when exceeding a predetermined force. With a correspondingly good setting of this Nachregelcharaktstik a qualitatively and quantitatively well interpretable number of micro-pulses can be realized. During the heating of the glass particles in the still solid state of matter, the distance between the micro-pulses and / or the interval between intervals at which a readjustment of the force takes place increases exponentially.

For example, an end of the series of micro-impulses can be used as a triggering criterion, approximated by the absence of a pulse, for example, for more than 30 seconds.

However, it is possible to quickly count the number of pulses and determine the trigger criterion based on this. Furthermore, it is also possible to use the measure of the time difference between two successive pulses as a triggering criterion.

In a further preferred embodiment, it is provided that after the pressing process, a crystallization program is started to form controlled, homogeneous glass crystals, but not the unwanted crystal growth as in the compression process. This results, for example, a block of lithium metasilicate.

Preferably, in the crystallization program, the ram no longer exerts pressure. Too long pressing could lead to unwanted or inhomogeneous crystallization.

The crystallization program is preferred in a temperature range between the transformation range Tg and about 80 ° C over the transformation range Tg of the glass particles (Tg + 80 ° C), in particular between 40 ° C over the transformation range Tg (Tg + 40 ° C) and about 60 ° C over the transformation range Tg of the glass particles (Tg + 60 ° C) made. At this temperature range, nucleation of the cluster of glass particles takes place. A subsequent increase in temperature to 60 ° C to 1 60 ° C above Tg causes a controlled crystallization. An even higher temperature for crystallization is possible, but would unnecessarily wear out the mold. In a further preferred embodiment, it is provided that after the pressing process and / or after the crystallization program, a cooling process and / or a demolding process is or are started. In the case of a dental restoration to be produced, a plaster-based dental investment material in a muffle is preferably used, which investment material has two advantages over high-temperature-resistant phosphate-bonded investment materials. On the one hand, the surface quality and thus the imaging accuracy is better. On the other hand, the devesting is easier.

In the case that an ingot or a milling block is cooled and demolded immediately after the pressing process, this can be checked for any errors, because this is glassy transparent.

In a further preferred embodiment, it is provided that a reusable muffle is used for a dental restoration or dental restorations to be produced.

In a further preferred embodiment, it is provided that at the end of all processes results in a block of lithium silicate with nucleating agents.

The oven of the present invention includes any heating device that provides thermal energy.

The glass particles of the present invention mainly refer to glass powder, glass granules and glass sand, but are not limited thereto. All industrially applicable glass particles, in particular those for the production of dental restoration parts, are within the scope of the present invention.

Further advantages, details and features will become apparent from the following description of an embodiment of the invention with reference to the drawings.

Show it:

1 shows a section through the combustion chamber of a furnace according to the invention in a

embodiment;

Fig. 2 is a graph of the speed of the ram and other physical quantities plotted against time; and

Fig. 3 is a diagrammatic representation of the rate of nucleation, densification and crystal growth plotted against temperature. In Fig. 1, an inventive furnace 10, which is particularly suitable for the production of dental restoration parts, shown in a relevant for the invention section.

A combustion chamber 12 is surrounded by a heating device 14, shown schematically, with a helically extending heating screen, which is shielded by a quartz glass 16 as a protective device. Large-volume heat insulation elements 18 surround the combustion chamber 12 on all sides, ie also downwards, even if this is not apparent from Fig. 1.

The bottom of the combustion chamber 12 is formed by a burner plate 20, the recesses 22 for receiving the muffle 24, and graduated in different sizes, in the illustrated embodiment in two sizes.

The combustion chamber 12 has a roof cone 26 which centrally increases the combustion chamber to the top. In this area, a part of a plunger 28 is received, which is inserted in a press channel 30, adjacent to a heap of glass particles 32 of lithium silicate, which is completely received in the muffle 24 in the press channel 30 and in the illustrated embodiment, color and translucency gradients forms.

The plunger may be made of any suitable material, such as Al ₂ 0 _3i boron nitride, graphite and / or investment itself.

In a ram passage a punch 36 is guided, which is driven by a drive device and is able to exert pressure on the ram 28 and thus indirectly on the pile of glass particles 32.

For the operation of the stove this is now opened first. A muffle preheated, for example, to 850 ° C. in a so-called preheating furnace, into which a cold heap of glass particles 32 and a cold pressing piston 28 have already been introduced, are placed centrally on the firing plate 20. The recess 22 fits in its dimensions exactly to the associated muffle 24, so that the muffle 24 is exactly central. The furnace hood is closed and a vacuum source sucks the air present in the combustion chamber 12 and in the thermal insulation elements until a negative pressure is created.

Gaskets are provided between a furnace base and the firing hood of the furnace, which are compressed by the build-up of the negative pressure. The build-up of the negative pressure takes place in one to two minutes, and during the entire following pressing cycle the negative pressure is kept constant, for example by a pressure regulator. the negative pressure source, or by running the corresponding suction pump.

As soon as the heap of glass particles 32 is introduced into the muffle 24, the heating of the glass particles 32, which have a much lower mass relative to the muffle 24, begins. The pile of glass particles thereby expands, the preheating temperature being well below the softening temperature. The thermal expansion coefficient of the muffle 24, so the investment material used for the formation of the muffle, is significantly lower than the coefficient of thermal expansion of the bulk of the glass particles, but also of the plunger and the press ram, the punch can for example also consist of Al ₂ 0 ₃ or, for example, steel.

In the exemplary embodiment illustrated here, the coefficient of thermal expansion of the muffle is 3 × 10 -6 / K and that of the respective glass particles is approximately 10 × 10 -6 / K, and that of the press ram 8 × 10 -6 / K.

In the thermal expansion in the axial direction considered here, the thermal expansions L ₀ add up when heated. The total thermal expansion L _{0 ges} is:

^L tot = ^L 0 ^{+ L} 0 o EBM aggregate ^{+ L} 0 ^L 0 Aloxkolben press stamp

In this case, the pressing ram 36 must be taken into account only insofar as it is heated, that is to say in the region of the heat-insulating elements 18 adjacent to the combustion chamber.

The opposite end of the punch 36, which is connected to the drive device, is significantly less hot, for example below 100 ° C.

The temperature gradient of the ram 36 is particularly high when a ram, for example, Al ₂ 0 ₃ is used; when using a metallic ram, an additional heat-insulating cylinder can be installed in the ram. l_o EB means the axial length of the muffle or embedding mass below the press channel 30.

In the considered embodiment of the furnace, the hot plate 20 is only superficially warm and already comparatively cool in the lower region. However, this does not apply if a so-called foot heating of a combustion chamber is realized, that is, if below the burner plate 20, a further heating is provided. In this embodiment the additional thermal expansion in the local area must be added to the above total thermal expansion.

To determine the axial displacement of the ram 36 by the thermal expansion, is of l_o _ges the thermal expansion of the furnace itself withdraw upon heating. It should be noted, however, that typically the seal and the closing force of the furnace are realized far out, and that thermal expansion is typically limited to the range between room temperature and a temperature below 100 ° C, for example 60 ° C; the heat-insulating elements 18, which become very hot at least inside, exert no axial force, but lie loosely in the furnace.

Under axial here is the axis 40 of the ram 36 to understand that passes centrally through both the plunger and the pile of glass particles 32 and the muffle 24 and the burner plate 20 therethrough; All parts are formed circular symmetrical in the illustrated embodiment.

In Fig. 2, a plurality of curves are plotted on the same graph, the abscissa being time. These values include the following values:

The temperature curve 51 shows the regulated temperature in the combustion chamber of the furnace.

The pressure curve 52 shows the pressure in the interior of the furnace.

The speed curve 53 shows the speed of the ram 36 or the associated drive device.

The zero point of the ordinate is offset in height and the velocity values in μηη / min are entered on the right.

The applied pressing force is entered in the pressing force curve 54.

As can be seen from Fig. 2, the furnace 10 is already preheated at the beginning considered, to about 550 ° C. The heating is still switched on. At the time about 70 seconds from the beginning of the heating is carried out, the target temperature in the considered embodiment is about 580 ° C. After 10 seconds at about 80 seconds, with the local peak of the speed of the punch 36 is rapidly introduced into the press channel 30 until the ram, plunger and the pile of glass particles rest on each other. The press die 36 exerts a constant pressure of approximately 100 N on the heap of glass particles 32. As can be seen from the pressure curve 52, the pressure in the furnace decreases rapidly within the first 40 seconds and is 100 mbar at 70 seconds. At the latest at 240 seconds, the final pressure of 50 mbar has been reached. This is kept constant during the entire pressing cycle.

From 70 seconds to about 115 seconds, the speed of the ram 36 is zero, as shown in FIG. At just over 115 seconds, a micro-pulse 60 according to the invention develops at a negative speed. This corresponds to a thermal expansion L _{0 ges} , as explained with reference to FIG. 1. The micro-pulse has a size of about 500 pm / min and a duration of less than one second, depending on the quality of the press force control - although this is not clear from Fig. 2 based on the embodiment shown here.

The upper end of the heap of the glass particles 32 slips a bit upward, contrary to the effect of the pressing pressure according to the press curve 54, and falls in a short time due to the softening of the glass particles again. At the time of about 135 seconds, the next micro-pulse 62 occurs. This is followed by further micro-pulses 64, 66, 68 and 70 at 150, 170, 195 and 225 seconds, while the subsequent period remains micro-pulse-free up to 250 seconds.

In the illustrated embodiment, according to the invention, the pressing process is triggered by the detection of a number of micro-pulses predetermined according to experience when the number of micro-pulses according to FIG. 2 reaches six.

This means according to the invention that the glass particles 32 have become micro-plastic or viscous; the further thermal expansion is pulse-free. This fact is evaluated according to the invention as an indication that the heap of glass particles has reached the actual desired temperature for the preparation of the pressing process.

For the detection of the micro-pulses, it is basically possible to perform a speed detection, a path detection or a press force detection, depending on the resolution of the available sensors and depending on the elasticity of the drive. In experiments in connection with the embodiment in question here, a speed detection has been found to be the most advantageous, but also a path detection is basically possible.

Although FIG. 2 does not show the entire heating time period of the cluster of glass particles until the beginning of compaction, it is to be noted here that, according to the invention, considerably faster heating is carried out than in the prior art. This produces a controlled, small amount of germs. From the time of 250 seconds on, the compaction process begins until approximately 660 seconds. The compression now reaches its maximum speed at about 470 seconds.

In a preferred embodiment, it is provided that immediately after the compression process, a cooling program is started to prevent the otherwise occurring at higher temperature crystal growth.

In a further preferred embodiment, it is provided that after the compression process, a crystallization program is started so that the desired, homogeneous and finer crystal structure results.

In a further preferred embodiment, provision is made for a cooling program and / or a crystallization program and / or a demoulding program and / or a cleaning program to be carried out after the compression process.

This results, for example, a block of lithium metasilicate glass ceramic or lithium silicate glass with nucleating agents.

In Fig. 3, three curves 72, 74, 76 are plotted in a diagram, wherein the abscissa is the temperature. The velocity curves 72, 74, 76, each with a plurality of triangles, circles and squares for discriminating each other, show at various temperatures the rate of nucleation, densification and crystal growth of the glass particles of lithium silicate.

The zero point of the abscissa - ie the temperature - is here offset in height and corresponds to the transformation range Tg of glasses of lithium silicate, which is about 450 ° C. In the transformation region Tg, the viscosity η of the glass particles of lithium silicate is about 10exp13.2 poise and the micro-pulses have ready, as long as the thermal expansion of the bulk of the glass particles is compensated by microplastic deformation at the contact points of the glass particles and the viscosity η a height of Reached 10exp14.5 poise.

From Fig. 3 it can be seen that a nucleation of glasses of lithium silicate in the temperature range between 460 to 530 ° C, ie between 10 ° C over the transformation range Tg of the glass particles (Tg + 10 ° C) and 80 ° C over the transformation range Tg of Glass particles (Tg + 80 ° C), a compression of these in the temperature range between 500 to 580 ° C, ie between 50 ° C over the transformation range Tg of the glass particles (Tg + 50 ° C) and 130 ° C over the transformation range Tg of the glass particles ( Tg + 130 ° C), a crystal growth of these in the temperature range between 510 to 610 ° C, ie between see about 60 ° C over the transformation range Tg of the glass particles (Tg + 60 ° C) and 160 ° C over the transformation range Tg of the glass particles (Tg + 160 ° C) takes place.

These three temperature ranges overlap, and in each of these temperature ranges there is a maximum rate of nucleation (at approximately 500 ° C), a maximum rate of compaction (at approximately 550 ° C), and a maximum rate of crystal growth (at approx. 580 ° C).

In order to form only a few germs (to the desired extent) before and during compaction so that complete compaction is not strongly prevented by the germs, a rapid heating, for example within three minutes, of 460 ° C. (Tg + 10 ° C.) is achieved according to the invention ) to 520 ° C (Tg + 70 ° C) corresponding to the temperature point 78 in FIG. 3.

At the temperature point 78, both nucleation and crystal growth have a relatively low velocity while the rate of densification is relatively high. According to the invention, therefore, this temperature point 78 is utilized. By rapid heating to the temperature point 78 as few germs and glass crystals are formed before and during compression.

In addition to the optimum temperature point 78, the end temperature for rapid heating may be another predetermined temperature between 500 ° C (Tg + 50 ° C) and 530 ° C (Tg + 80 ° C), which corresponds at least to the dilatometric softening of the glass particles and in which the viscosity of the glass particles η is at least 10exp11, 5 poise.

Claims

Patent Application Claims:

1 . Arrangement of a furnace and a heap of glass particles, which furnace

(10) a plunger (36), a pressure, displacement and / or velocity sensor and a control device for controlling a pressing operation based on the output signal of the sensor, wherein the sensor at least one pressure, location, and / or movement parameters of the press ram (36) detected, wherein the ram (36) - optionally via an intermediate plunger (28) - on the pile of glass particles (32) acts, which are guided in a press channel (30) and crystallizable, and wherein the Tripping criterion for the process control is detected via the sensor change of at least one movement parameter of the press ram (36) at softening of the bulk of glass particles (32).

2. The arrangement of a furnace and a cluster of glass particles according to claim 1, characterized in that the process control controls the start of the pressing process, at which start the furnace temperature, the pressure in a combustion chamber (12) of the furnace (10) and a pressing force of the press ram (36) are controlled by the control device, and that the process control controls the end of the pressing operation, at which end the pressing force of the ram (36) by the control device, in particular to zero, reduces and the oven temperature by the control device, in particular by switching off the Oven (10), is reduced.

3. Arrangement of a furnace and a cluster of glass particles according to claim 1, characterized in that the heap of glass particles (32) in the press channel (30) gradients, in particular color and / or translucency gradients, forms.

4. Arrangement of a furnace and a heap of glass particles according to claim

1 or 3, characterized in that the gradients correspond to at least one gradual layer-wise and / or a continuous change of a physical property of the cluster of glass particles.

5. Arrangement of a furnace and a heap of glass particles according to one of claims 1, 3 and 4, characterized in that the heap of glass particles (32) of different colored glass particles and / or at least one type of glass, which is colored differently with pigments, and / or consists of glasses with different contents of nucleating agents and / or with different densities.

6. Arrangement of a furnace and a cluster of glass particles according to one of the preceding claims, characterized in that the triggering criterion for the start of the pressing operation, the termination of micro-pulses (60, 62, 64, 66, 68, 70) of the movement parameter and / or Number and / or their time interval is.

7. Arrangement of a furnace and a cluster of glass particles according to one of the preceding claims, characterized in that the ikroimpulse (60, 62. 64, 66, 68, 70) a short-term and small movement between the heap of glass particles (32) and the Play muffle (24).

8. Arrangement of a furnace and a cluster of Glaspartikein according to any one of the preceding claims, characterized in that the control device, the number of micro-pulses (60, 62, 64, 66, 68, 70) of the movement parameters and / or their distance and / or their Changes in the distance and / or their size recorded and used for process control.

9. The arrangement of a furnace and a cluster of glass particles according to any one of the preceding claims, characterized in that the triggering criterion for the end of the pressing operation, the decrease in the pressing speed to a value close to zero or a value of less than 5%, in particular less than 2% , which is maximum pressing speed of the punch (36).

10. Arrangement of a furnace and a cluster of glass particles according to one of the preceding claims, characterized in that the control device detects a backward movement of the press ram (36) corresponding to the thermal expansion of the cluster of glass particles (32) via the sensor and the triggering criterion for the start of the Pressing operation is an end of the backward movement and / or the beginning of a forward movement and / or a defined time after a change of movement parameters of the press ram (36).

11. Arrangement of a furnace and a heap of glass particles according to one of the preceding claims, characterized in that the sensor below the softening temperature of the heap of glass particles (32) counteracts the pressing force thermal expansion of the muffle (24), optionally the plunger (28) of the press ram (36) and the heap of glass particles (32), in particular the accumulated thermal expansion of these detected.

12. The arrangement of a furnace and a cluster of glass particles according to any one of the preceding claims, characterized in that the sensor of the softening of the cluster of glass particles (32) corresponding decreasing counterforce due to thermal expansion coefficients or due to differences between thermal expansion coefficients of the control device fed, said determines a further course of the process to a time after the time of detection of the softening of the cluster of glass particles (32).

13. Arrangement of a furnace and a cluster of glass particles according to any one of the preceding claims, characterized in that the control device the press ram (36) before the actual pressing process - optionally via the intermediate plunger (28) - to the pile of glass particles (32) applies and the thermal expansion of the heap of glass particles (32) - detected according to a movement of the press ram (36) against the pressing direction - and the absence of further thermal expansion or in the softening the decreasing counterforce as a particular additional triggering criterion.

14. Arrangement of a furnace and a cluster of glass particles according to one of the preceding claims, characterized in that the control device the Pressstempei (36) exert a pressing force or a pressing pressure on the heap of glass particles (32), even before the heap of glass particles (32) is softened.

15. Arrangement of a furnace and a cluster of glass particles according to one of the preceding claims, characterized in that based on the movement parameter detected by the sensor, the pressing pressure exerted by the pressing die (36) and / or the temperature of a temperature sensor, the or Combustion chamber (12) is mounted, the control device detects the type and material of the cluster of glass particles (32) - based on predetermined signatures - and based on the pressing process controls.

16. Arrangement of a furnace and a cluster of glass particles according to any one of the preceding claims, characterized in that during the detection of the movement parameter of the ram (36) a constant force or a predetermined profile following force on the pile of glass particles (32) - optionally via the interposed pressing piston (28) - exercises and the movement parameter is detected after the ram (36) - optionally on the plunger (28)

- At the pile of glass particles (32) is applied.

17. The arrangement of a furnace and a cluster of glass particles according to any one of the preceding claims, characterized in that the pressing die (36) moves during the heating of the cluster of glass particles (32) by a predetermined amount, in particular less than 1 mm and especially preferably between 0.3 and 0.5 mm.

18. A method for operating a furnace based on a control device for controlling a pressing operation, wherein a pressure, displacement and / or speed sensor detects at least one pressure, location, and / or movement parameters of a ram (36), and wherein the Control device controls the pressing operation based on an output signal of the sensor, wherein during the pressing process, the pressing punch (36) - optionally via an intermediate plunger (28) - on a heap of glass particles (32) acts and exerts pressure, which heap of glass particles (32) in a pressing channel (30) of a muffle (24) is introduced, and wherein the triggering criterion for the process control is a change of at least one movement parameter of the press ram (36) detected by the sensor, corresponding to the softening of the lump of glass particles (32).

19. The method according to claim 12, characterized in that after the termination of micro-pulses (60, 62, 64, 66, 68, 70) of the motion parameter, the frequency glass particles (32) within ten minutes, in particular within five minutes, preferably within three minutes to a predetermined temperature is heated, which corresponds to at least the dilatometric softening of the heap of glass particles.

20. The method according to claim 18 or 19, characterized in that after the pressing process, a crystallization program is started, wherein the press ram (36) no longer exerts pressure.

21. Method according to one of claims 18 to 20, characterized in that in the temperature range between the transformation region or transformation point Tg of the cluster of glass particles and 100 ° C over the transformation range Tg (Tg + 1 00 ° C), in particular between 30 ° C over the Transformation range Tg (Tg + 30 ° C) and 80 ° C over the transformation range Tg (Tg + 80 ° C), a nucleation of the cluster of glass particles (32) takes place.

22. The method according to any one of claims 18 to 21, characterized in that after the pressing process and / or after the crystallization program, a cooling process and / or a demolding process is started or, in particular a gypsum-based dental investment material used in a muffle (24) becomes.

23. The method according to any one of claims 18 to 22, characterized in that at the end of the process, a block of lithium metasilicate and / or lithium silicate with nucleating agents results.