Direct sealing of glass micro-structure

This application is made under 35USC § 119 to the sequence number of the request to submit 30 November 2010 10306318.6 the priority of the European Patent application, on the basis of its content to herein, and all incorporated by reference herein will be the same.

Background Art

The content disclosed in this application mainly relates to a method of manufacturing glass micro-structure, more specifically, relates to the sealing of a plurality of glass layers method of manufacturing glass micro-structure.

Overview

Microfluidic component is a device comprising a micro-reactor, can also be referred to as micro-channel reactor. Micro-reactor is of such a kind of device, dynamic or static target sample is limited and is processed therein. In some cases, the processing relates to the analysis of the chemical reaction. In other cases, the processing as the use of two different reactant of a part of the manufacturing process of the execution. In some other cases, dynamic or static target sample is limited in the micro-reactor, at the same time of the sample and the associated heat exchange between heat exchange fluid. In any case, micro-reactor according to their definition of the size of the channel, usually about 0.1 to 5 mm, preferably 0.5 to 2 millimeters. Micro-channel is the most typical of this kind in the form of limit, and the micro-reactor is typically a continuous flow reactor, rather than batch-type reactor. Micro-channel is relatively small the interior dimensions of the mass transfer and heat transfer rate provides considerable improvement. Furthermore, micro-reactor, compared with the traditional-scale reactor has many advantages, including energy efficiency, the reaction speed, reaction yield, safety, reliability, can be enlarged in scale greatly improved.

There are various techniques used for manufacturing micro-reactor, such as a hot pressing technique. Through hot pressing and hot pressing technology the operation of the mould pattern fossil ink copied to the softened glass is on-chip. After the forming step is a glass and the glass sealing or frit auxiliary sealing, in order to form a complete micro-channel device.

Based on glass material the major advantage of the method is to compare in the usual glass/glass sealing (in 10⁸ to 10⁶ tomari viscosity lower), at a relatively high viscosity (10¹⁰ to 10¹² tomari) achieve strong seal. The method of the glass-based material, can be used to lower than the temperature of the softening point of glass. In this method, it is possible to in the sealing the three-dimensional glass micro-structure at the same time keep the micro-features of the initial geometric shape and size, thereby permitting repetitive fluid properties, such as different reactant and cooling the inside of the channel of the volume and the pressure drop. However, glass material seal requires a large number of additional steps, such as preparation of the frit, uniform deposition of the glass material of the glass material, and the final sintering. Because taking into account the expansion mismatch, chemical compatibility, mechanical resistance, particle size distribution and glass material solution precipitation, these steps each step in the preparation of glass frit composition complicated.

As a result, the glass and the glass directly sealing is desirable, because it saves these process steps, the powder material processing and avoids many of the complex problems associated. Glass and glass seal is in such a temperature of the operation, the viscosity of the glass to allow surface of the tight contact of the seal in order to form the chemical bond. Furthermore, temperature and seal time care must be taken to choose, in order to allow the glass surface tension enables various parts fused together, and to eliminate harmful to the mechanical strength of an acute angle. This firm combination of the softening point of the glass is usually in the vicinity of the temperature; however, in this kind of viscosity, glass flow module may be under the action of the gravity to collapse. Furthermore, the external load (usually 1-2g/cm²) often the use of the upper part of the assembly is applied to the extrusion in order to strengthen the contact between the glass sheets; however, the additional load of the viscosity of the glass structure to accelerate flow and deformation.

Embodiments of the present invention are directed to the elimination of glass micro-structure collapse and deformation, its method is to introduce the side retainer member, absorbing the external or share the weight of the load plate in order to achieve firm and sealing of the glass layer, due to the viscous flow at the same time prevent any not controllable obstructive micro channel deformation, non-stick and under the high temperature of the load plate is adhered to the glass, so as to avoid the collapse of a glass micro-structure and to facilitate surface tension sealing channel joint in a better changes the circle thermal conditions. Regardless of theory, embodiments of the present invention is directed towards improved method of sealing-glass, in the glass and not between the adhesive sheet (such as graphite) side and keep the device for realizing this kind of auxiliary adhesive phenomenon, in order to help direct sealing of glass micro-structure.

According to one embodiment, provides a sealed glass micro-structure the method of the assembly. The method includes providing a base plate as glass micro-structure of the supporting body of the assembly, providing glass micro-structure assembly, which includes one or a plurality of the patterned glass layer on the base plate, and a glass top layer stacked on the one or a plurality of patterned glass layer, wherein the at least one channel formed in the glass top and the one or a plurality of patterned glass layer. The method also includes the upper surface of the glass top layer provides a load on the top plate, so that the top plate close contact with the lower surface of the upper surface of the glass top layer, wherein the top plate is made of non-glass component, and then the base plate providing one or a plurality of side retainer member, adjacent the glass micro-structure assembly, the side retainer member is less than the height of the glass micro-structure assembly defines the height of the uncompressed. Furthermore, the method comprises in heating glass micro-structure and the top plate to the glass sealing temperature at the same time, the load that is in close contact with the glass top plate to compress the glass micro-structure assembly, the glass sealing temperature is a temperature enough to make the glass sliver, wherein the load plate assembly of vertical compression of glass micro-structure in the viscous glass, the contact side of the top plate until the load component of the cage and supported by the support, and under the glass sealing temperature, load the board receives side of the retainer member at the same time, the lower surface of the roof the glass stuck is to be kept on the upper surface of the top layer.

According to another embodiment, the sealing method can further include micro-structure assembly through the glass sealing temperature maintained at about 2 to about 4 hours, to remove an acute angle of at least one channel, wherein the micro-structure of the assembly of the glass of the glass heating increase the surface tension of a micro-structure assembly, so as to make the at least one channel of the smooth at an acute angle.

Combining the following description, the accompanying claims and the attached drawing, will be able to better xie Ben these and other features of the invention, the hand and.

Description of drawings

Although the right end of this specification for and clearly pointed out that for the protection of the invention, may believe that, through the following description of the accompanying drawing, and combining corresponding geographical xie Ben invention will be better, wherein:

Figure 1 is a schematic diagram of in accordance with the present invention one or more of embodiments of the glass micro-structure assembly before sealing;

Figure 2 is a schematic diagram of in accordance with the present invention one or more of the embodiment of a glass micro-structure assembly in the heating to the glass sealing temperature;

Figure 3 is a schematic diagram of in accordance with the present invention one or more of the embodiment of a glass micro-structure assembly under the glass sealing temperature for about 1 hour;

Figure 4 is a schematic diagram of in accordance with the present invention one or more of the embodiment of a glass micro-structure assembly under the glass sealing temperature for about 3 hours;

Figure 5A is micrograph of fig. 1 according to the present invention shown in one or more of the embodiment of a glass micro-structure assembly when heated to the passage in the in the process of glass sealing temperature;

Figure 5B is micrograph of according to the present invention one or more of the channel in the embodiment of the glass sealing temperature through 2 hours after the heat treatment;

Figure 5C according to the present invention is one or a plurality of embodiment of a channel in the glass sealing temperature through 3 hours metallographs after the heat treatment;

Figure 6 is a schematic diagram of in accordance with the invention one or a plurality of embodiments for simultaneously sealing a plurality of glass micro-structure assembly of the heating device.

Detailed description

From time to time will now be described reference to specific embodiments of the features and advantages of the present invention. However, the invention is implemented can be of different forms, and should not be construed as limited to the embodiment described here. On the contrary, provides these embodiments so that the present disclosure is thorough and complete, and will fully to those of skill in the art to express the scope of the invention.

With reference to Figure 1-4 shown sealed glass micro-structure assembly 100 embodiment of the method, the method comprises providing a substrate 200 as glass micro-structure assembly 100 of the support body. Substrate 200 is an optional, because any bottom surface or substrate are applicable, it can include the component of the non-glass, it will not adhere to the glass micro-structure assembly 100 of any layer. Base plate 200 of the component must also be higher than the 1000 [...] temperature durable. In one embodiment, the substrate 200 can include graphite, for example, such as described below is applied to the glass micro-structure assembly 100 of the glass top layer 110 of commercial graphite material.

In the Figure 1 embodiment, the glass micro-structure assembly 100 for each layer of the stack, in order to promote the sealing of the glass micro-structure assembly 100 to the glass surface of the close contact of the. Glass micro-structure assembly 100 can include is arranged on the substrate 200 on the one or a plurality of patterned glass layer 120. With reference to Figure 1, the patterned glass layer 120 has a plurality of settings on the patterned glass layer 120 on the upper surface of the projection and the lower surface of the. Furthermore, glass micro-structure assembly 100 can also include stacking in the one or a plurality of patterned glass layer 120 on the glass top layer 110. Although the showing in Figure 1 of the glass top layer 110 has a flat upper surface and a lower surface, however, it could be imagined that, on the upper surface and the lower surface can also be patterned, similar to the patterned glass layer 120. However, if the glass top layer 110 is patterned on the upper surface, it must remain in the glass top layer 110 on the whole surface of the top supporting board 300 close contact with the lower surface of. This close contact with the detailed description below.

Once again reference fig. 1, glass micro-structure assembly 100 also includes the base plate 200 by its contact with and support of the glass bottom layer 140. As shown, one or a plurality of patterned glass layer 120 can be stacked in the glass bottom layer 140 is. In the Figure 1 embodiment, the glass bottom layer 140 in its upper surface and a lower surface defining a substantially flat cross-section; however, with the glass top layer 110 the same, can be thought of, glass bottom layer 140 is also patterned. Nevertheless, the glass bottom layer 140 is an optional, therefore, can be thought of the patterned glass layer 120 directly over the base plate 200 or other suitable substrate.

Reference again to Figure 1, the glass top layer 110 and one or a plurality of patterned glass layer 120 to form a stacked arrangement of at least one of the glass top layer 110 and one or a plurality of patterned glass layer 120 between the channel 150. Furthermore, a plurality of patterned glass layer 120 stack can also be formed on the patterned glass layer 120 between the channel 150. Furthermore, the glass bottom layer 140 and one or a plurality of patterned glass layer 120 can be formed between the at least one channel 150. Channel 150 formed in the sealing process and shaping in the following will be described in more detail.

In order to obtain the desired glass micro-structure product, properly aligning glass micro-structure assembly 100 of a layer stack is beneficial. With reference to Figure 1 of the embodiment, the patterned glass layer 120 through the surface of the tenon-and-mortise positioning system is precisely aligned with, the technical field of this is the familiar ordinary technical personnel. As shown, a patterned glass layer 120 a tenon 122 inserted into another patterned layer 120 of the mortice 121 in, in order to ensure proper alignment. Can be thought of, other engagement or coupling mechanism, for example, negative and positive coupling mechanism, is also suitable for the promotion of glass micro-structure assembly 100 each layer of the proper alignment. As shown in Figure 1 before some of the layers of the contact point between the layers, in the 20 the lower glass micro-structure assembly [...] 100 exists between each layer of up to about 200 the  m, or about 20-100 the gap   m.

Glass micro-structure assembly 100 of the glass can include various components, for example, glass, glass-ceramic material, borosilicate glass, silicon dioxide, or a combination thereof. Suitable commercial material may include Eagle And All of these were made by the Corning Company of production (  Incorporated Coming). Can be thought of, glass and other materials such as ceramic (for example, silicon carbide), metal and metal alloy (such as nickel, molybdenum, tungsten) can be used for the combination of glass micro-structure assembly 100 of each layer. According to all of the described alternative method of the embodiment, can also be the filling material, such as various refractory material powder, is added to or included in the component in the glass, for example by any suitable means of adjusting the mechanical or thermal properties of the glass.

Furthermore, as shown in Figure 1, the load the top plate 300 is set up in the glass top layer 110 on the upper surface of, the top plate 300 close contact with the lower surface of the glass top layer 110 of the upper surface. In this text, "close contact" said glass top layer 110 of the load and the entire upper surface of top plate 300 is contacted with the lower surface of the, in the sealing process so that no gap on the interface. The top plate 300 is made of non-glass component, the component at the room temperature will not be adhered or attached to the glass. As shown in Figure 1 is shown in the embodiment, load top plate 300 has a substantially flat lower surface, the glass top layer 110 has a substantially flat upper surface; however, can be thought of as, these surfaces can be the still maintain close contact of the complementary surface of the patterning.

In addition to room temperature on the glass will not be adhered to, should also be a component of the top plate at a temperature higher than 1000 the durable under [...] of the temperature of the. In one embodiment, the top plate 300 includes graphite. Optionally, the graphite top plate 300 in the graphite top plate 300 is arranged on the lower surface of the substantially free of carbonaceous soot or dust. In one commercial embodiment, the top plate 300 by the mechanical machining or grinding to the standard of the 50  m/300 mm   Ref2020 Mersen the smoothness of the production of graphite, wherein the lower surface of the graphite usually limits the roughness is 0.3 (grinding) to 3 the (mechanical processing)  m RMS (root mean square value). Graphite top plate can contain minor partial surface degradation, such as scratches or oxidation inclined, however, these small defect does not affect the adhesion phenomenon as described below. These minor local effect in the sealing cycle is only copied to the viscous glass. Can be thought of, the top plate 300 can include various load and surface area. Specifically, the top plate is 300 is significantly greater than the weight of the weight of the glass micro-structure assembly. For example, the top plate 300 can reach as high as about the weight of 5000g, or about from 500 to 3000g, or from about 2500 to about 2700g, or about 2600 g. Moreover, the top plate 300 can also be the surface area of change according to the requirements. In one embodiment, the top plate 300 has about 250 × 300 mm size.

Reference again to Figure 1, one or a plurality of side retainer member 400 also can be arranged on the base plate 200 is, and with the glass micro-structure assembly 100 adjacent. In Figure 1 in a pre-sealing device, side retainer member 400 D with height, is less than the uncompressed glass micro-structure assembly 100 limits the height H1. Side retainer member 400 D is set as the height of the sealing process of the glass micro-structure the height of the required product. Side retainer member 400 D and uncompressed height of the height of H1 can be changes in the difference between the. In one exemplary embodiment, the difference is about 300 the  m. Can be thought of, the kind of rigid heat stable material suitable for use as a side holder member 400, for example, metal, ceramic or alloy. In one embodiment, side retainer member 400 comprises alumina. Optionally, side keeper member 400 can be coated with a non-stick powder, for example, boron nitride, in order to prevent the side holder member 400 is adhered to a glass micro-structure assembly 100 on the glass.

As described throughout herein, side keeper member 400 can be the glass sealing process provides many benefits. Bound set aside theory, side retainer member 400 help to prevent the micro-structure in the sealed period with the passage of time without being subject to the control of. Side retainer member 400 allows the use of a relatively high sealing load, at the same time prevent the sealing load in the thermal cycle the negative impact of the 2nd part. So a heavy load will normally be completely grind under such high temperature glass fluid module. However, the heavy load are favorable in sealing operation, it can be through the deformation of the glass plate becomes flat and through the softened glass is the highest deformation or penetration of the other surface is the elimination of any difference in height, between the glass layer, the glass top layer and 110 and the top plate 300 the close contact between the. Once the side of the supporting component of the load, the glass plate adhered to the upper part of the top plate 300 is, as described in more detail below. Furthermore, by omitting additional complicated steps, such as preparation of the frit, glass material of the glass material is evenly deposited and sintered, side retainer member 400 is described below in conjunction with the temporary adhesion simplify the glass-glass sealing process.

Figure 2 has shown the glass micro-structure assembly 100 the initial compression. In Figure 2 is shown in a compression stage of the, base plate 200, the top plate 300, glass micro-structure assembly 100 and the side holder member 400 is heated to the glass sealing temperature. In this text, "glass sealing temperature" is defined to be sufficient to make the temperature of the glass is provided with a viscosity. As mentioned above, glass material is viscous flow of the glass-glass seal necessary. In one embodiment, the glass sealing temperature than the glass in the microstructured assembly with low softening temperature glass of about 5 to about 50 the [...]. For example, the glass sealing temperature is from about 980 to about 1035 the [...] , or of from about 1000 to about 1020 the [...] , or about 1010 the [...]. In the glass sealing temperature is lower, the viscosity of the glass is about 10⁶ to about 10⁹ tomari, 10⁷ to about 10⁸ tomari, or about 10^7.5 tomari.

Once again reference Figure 2, glass micro-structure assembly 100 is heated, load top plate 300 vertical compression glass micro-structure assembly 100 in the viscous glass. Compression reducing the glass micro-structure assembly 100 height, in Figure 1 the height of the uncompressed H1 to fig. 2 of the height of the slightly compressed H2. In one exemplary embodiment, side retainer member 400 D and the height of the slightly compressed height H2 is about the difference between the the 200  m. Because of this kind of slight compression, glass micro-structure assembly 100 between the glass layer is no longer any clearance, because the surface to be sealed contact with each other.

Figure 3 shows the compression stage, among them the load top plate 300 compressed glass micro-structure assembly 100, the supporting board 300 contact side keeper member 400 and is received by the support. At this time, glass micro-structure assembly 100 and the side holder member 400 that the height of the same. Because the top plate 300 contact side keeper member 400, substantially no load is applied to the glass micro-structure assembly 100 on. When the temperature in the glass seal, because side keeper member 400 absorbing the weight, glass micro-structure assembly 100 without further reduce the height of the. If there is no side keeper member 400, under the same load, glass micro-structure assembly 100 will further decrease in the height of the, channel 150 will be further flattened. Figure 3 the compression phase shown in the glass micro-structure assembly 100 under the glass sealing temperature is maintained for a period of about 30 minutes to about 2 hours, or about 1 hour of time.

Furthermore, the top plate 300 by a load side of the keeper member 400 at the same time absorbed by the, viscosity of the glass becomes low enough, glass micro-structure assembly 100 the surface tension of the glass in the channel 150 becomes round, as shown in Figure 5A and 5B illustrated. Figure 5A has shown the Figure 2 the illustrative display of when the heating to the glass sealing temperature of the channel 150 there are many sharp edges, for example, channel 150 of the 45 [...] bevel 152 and acute-angled sealing joint 154. Sealing joint 154, because glass micro-structure assembly 100 of the two stack formed by the connection of the glass layer.

Fig. 4 shows glass micro-structure assembly 100 to maintain the glass sealing temperature for a time sufficient so that the channel 150 of the rounding at an acute angle. For example, this can be through the glass micro-structure assembly 100 to maintain the glass seal temperature and corresponding the glass viscosity of about 2 to about 4 hours, or about 3 hours to achieve. An acute angle in the channel of the micro-reactor is disadvantageous, because an acute angle in the reactor will increase little turbulence in a flow of the fluid, and to weaken the mechanical strength of the micro-reactor.

Reference to Figure 3 and 4, even in the load the top plate 300 by the side of the weight of the keeper member 400 to support the rear or share, load the top plate 300 is still maintained and the glass layer 110 close contact. Specifically, the inventor has surprisingly found that, under the glass sealing temperature, supporting board 300 is side keeper member 400 at the same time supported by the, load top plate 300 adhered to the lower surface of the glass top layer 110 on the upper surface.

Not bound by theory, the temporary adhesive is micro-structure of the glass when the glass is viscous, and glass top layer 110 with the load on the upper surface of the top plate 300 when the close contact with the lower surface of the. Keep the glass top layer 110 and load the top plate 300 in the glass between the close proximity of the sealing temperature is conducive to adhesion, it utilizes the penetration load top plate 300 on the microporous or the surface of any surface defects (such as scratches) adhesion of glass. If the glass top layer 110 and the load on the upper surface of the top plate 300 between the lower surface of the close contact is not achieved (for example, because the top plate 300 on the lower surface of the soot or carbon deposit), adhesion may be hindered. Furthermore, this kind of temporary adhesion effect observed at the room temperature of is, therefore, in order to realize this kind of adhesion effect, it is necessary to by heating to glass sliver of the glass sealing temperature.

The temporary adhesion is a glass sealing process provides many advantages. For example, glass top layer 110 and the upper surface of the top plate 300 the adhesion of the under surface of the sealing can be at a relatively high temperature and relatively low viscosity to achieve, without losing glass micro-structure assembly 100 required external (outer) and internal (fluid properties) geometrical shape. As described in more detail below, at a relatively high temperature and relatively low degree of viscosity lower sealing the channel becomes round, and to provide improved mechanical performance, such as glass micro-structure assembly 100 the internal pressure resistance. Furthermore, temporary adhere to the glass micro-structure operable in the production of the product of the glass sealing temperature and glass viscosity range, without losing geometry control.

The top plate 300 and a glass top layer 110 according to the adhesion between the material of each layer changes and processing conditions. For example and non-limiting, adhesion has been observed 10N used for 160 × 260 nm or 180 × 200 mm of the contact surface. This invention intends to use the greater than 10N of adhesion.

Glass micro-structure assembly 100 of the channel 150 becomes round to fig. 4 and fig. 5C after the best level shown, glass micro-structure assembly 100 is cooled to form a glass micro-reactor product. Here can use various cooling rate and the cooling time. In one embodiment, glass micro-structure assembly was 4 to about 6 hours is cooled to the room temperature. After cooling, the top plate 300 and glass micro-structure assembly 100 between the interaction of no obvious, thus the top plate 300 can be repeatedly used for other glass micro-structure assembly 100 the sealing.

Embodiment

Figure 5A-5C microscopic picture shows the passage in the sealing process 150 of rounded process. In the experiment from the micrograph, wherein Coming   3D microstructure at about 1010 the sealing temperature of glass [...] is sealed. Glass micro-structure in the 3 hours from room temperature to in the 1010 [...]. Using 1700g graphite top and alumina side retainer. After the heat sealing, the glass micro-structure 6 hours of cooling to room temperature. When heated to a temperature in the process of glass sealing temperature, as shown in Figure 5A illustrated, the load applied to the impact of the sealing and the temperature of the trigger, but not enough to make the sealing joint 154 and 45° bevel 152 becomes round. 1 hour later, as shown in Figure 5B shown, glass surface tension makes the channel 150 to become round the acute-angle portion. In particular, 45° bevel basic removing; however, an acute angle of a sealing joint 154 left. At this time, the internal pressure resistance of the line is equal to or lower than 30 bar. 3 hours later, as shown in Figure 5C illustrated, sealing joint 154 acute angle is no longer visible, and the internal pressure resistance is improved to 70 to 100 between the two sides. If the sealing process is extended to, for example, 6 hours, will not produce other benefits. In fact, a continuous time will adversely reduce the channel 150 height, reducing the internal volume. Therefore, there is a the best sealing duration, long enough in order to make the surface tension can cause channel profile becomes round, but will not increase the glass micro-structure assembly 100 collapse or depression, this will cause the undesirable reduction of the internal volume of the circuit.

Can be thought of various heating devices can be used for the heating process. With reference to Figure 6 embodiment, a plurality of glass micro-structure assembly 100 can at the same time is sealed. As shown, in that in one of the many sealing manner, heating device 500 can include a multi-stage radiation heating assembly, the assembly has two lower support plate 600 and a top plate 700. As shown, heating device 500 in the glass micro-structure assembly 100 comprises a radiating element the opposite sides, in order to provide a uniform heating. Top plate 700 preventably the above glass micro-structure assembly sample with the following glass micro-structure assembly of the top of the sample subjected to the different compared with the radiation heating process.

Unless otherwise defined, the use herein of all technical and scientific terms of the present invention in the field of the technology of the commonly understood by the ordinary technical personnel the same meaning. In herein the terminology used in the description is used for only the particular embodiment described, and was not intended to limiting. In the specification and in the attached claims the use of the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context otherwise specified.

Unless otherwise indicated, the specification and claims the expression of the use of the amount of the component or attribute all digital, such as molecular weight, the reaction conditions should be understood as such as in all cases is modified by the word "about". Therefore, unless otherwise indicated, in the specification and the claim in the book attribute the value of the divisor, according to the present invention in the mode of execution of the seek to obtain the performance of required change. Although limit the invention and a wide range of the value range of the parameter is the approximate, but in a particular embodiment, the report of the value as precisely as possible. The ordinary technicians in this field will understand, any numerical value includes determining the value inherent to the use of the measuring technology of a certain error.